data_(NNTBS)DyI(THF)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H54 Dy Fe I N2 O2 Si2' _chemical_formula_weight 876.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Dy' 'Dy' -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.098(5) _cell_length_b 11.619(5) _cell_length_c 16.156(10) _cell_angle_alpha 101.744(7) _cell_angle_beta 91.826(6) _cell_angle_gamma 118.257(4) _cell_volume 1776.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 3.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5446 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24706 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 30.62 _reflns_number_total 10016 _reflns_number_gt 8047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2, 2013' _computing_cell_refinement 'SAINT V8.32B (Bruker AXS Inc., 2013' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013' _computing_structure_solution 'SHELXS-2013 (Sheldrick 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+11.0114P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10016 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.74689(2) 0.48575(3) 0.241488(16) 0.03472(9) Uani 1 1 d . . . Fe1 Fe 1.03581(7) 0.46929(7) 0.24591(4) 0.02519(15) Uani 1 1 d . A . Si2 Si 0.95474(18) 0.81567(17) 0.19515(10) 0.0367(3) Uani 1 1 d . . . N1 N 0.7356(5) 0.3253(5) 0.3001(3) 0.0461(14) Uani 1 1 d . A . N2 N 0.9146(4) 0.6560(5) 0.2025(3) 0.0301(9) Uani 1 1 d . A . O1 O 0.6734(4) 0.3446(4) 0.1011(2) 0.0353(8) Uani 1 1 d . A . O2 O 0.7687(7) 0.6237(6) 0.3789(4) 0.0807(12) Uani 1 1 d . A . C1 C 0.5639(7) 0.2047(7) 0.0809(4) 0.0556(18) Uani 1 1 d . . . H1A H 0.5033 0.1888 0.1258 0.067 Uiso 1 1 calc R A . H1B H 0.6034 0.1434 0.0764 0.067 Uiso 1 1 calc R . . C2 C 0.4845(10) 0.1814(10) -0.0024(5) 0.092(4) Uani 1 1 d . A . H2A H 0.4788 0.1028 -0.0439 0.111 Uiso 1 1 calc R . . H2B H 0.3894 0.1630 0.0050 0.111 Uiso 1 1 calc R . . C3 C 0.5551(9) 0.3002(10) -0.0332(6) 0.086(3) Uani 1 1 d . . . H3A H 0.4939 0.3392 -0.0390 0.103 Uiso 1 1 calc R A . H3B H 0.5802 0.2773 -0.0900 0.103 Uiso 1 1 calc R . . C4 C 0.6786(8) 0.3970(8) 0.0267(4) 0.0559(19) Uani 1 1 d . A . H4A H 0.7621 0.4091 0.0007 0.067 Uiso 1 1 calc R . . H4B H 0.6818 0.4854 0.0428 0.067 Uiso 1 1 calc R . . C5 C 0.8881(10) 0.6689(10) 0.4401(5) 0.0807(12) Uani 1 1 d . . . H5A H 0.9699 0.6880 0.4106 0.097 Uiso 1 1 calc R A . H5B H 0.8732 0.5975 0.4697 0.097 Uiso 1 1 calc R . . C6 C 0.9127(10) 0.7924(10) 0.5031(6) 0.0807(12) Uani 1 1 d . A . H6A H 0.9496 0.7966 0.5608 0.097 Uiso 1 1 calc R . . H6B H 0.9763 0.8750 0.4856 0.097 Uiso 1 1 calc R . . C7 C 0.7765(10) 0.7728(10) 0.4993(5) 0.0807(12) Uani 1 1 d . . . H7A H 0.7808 0.8618 0.5095 0.097 Uiso 1 1 calc R A . H7B H 0.7330 0.7306 0.5455 0.097 Uiso 1 1 calc R . . C8 C 0.6855(10) 0.6840(10) 0.4134(5) 0.0807(12) Uani 1 1 d . A . H8A H 0.5932 0.6149 0.4211 0.097 Uiso 1 1 calc R . . H8B H 0.6745 0.7382 0.3768 0.097 Uiso 1 1 calc R . . C9 C 0.8642(6) 0.3329(5) 0.2920(3) 0.0369(13) Uani 1 1 d . A . C10 C 0.9008(6) 0.2669(5) 0.2195(3) 0.0366(12) Uani 1 1 d . . . H10A H 0.8417 0.2138 0.1669 0.044 Uiso 1 1 calc R A . C11 C 1.0382(7) 0.2936(6) 0.2389(4) 0.0446(14) Uani 1 1 d . A . H11A H 1.0864 0.2605 0.2025 0.054 Uiso 1 1 calc R . . C12 C 1.0911(7) 0.3790(7) 0.3230(4) 0.0456(15) Uani 1 1 d . . . H12A H 1.1811 0.4128 0.3526 0.055 Uiso 1 1 calc R A . C13 C 0.9871(7) 0.4050(6) 0.3550(3) 0.0422(14) Uani 1 1 d . A . H13A H 0.9966 0.4611 0.4093 0.051 Uiso 1 1 calc R . . C14 C 1.0210(5) 0.6238(5) 0.2048(3) 0.0241(9) Uani 1 1 d . A . C15 C 1.0411(5) 0.5349(5) 0.1373(3) 0.0261(9) Uani 1 1 d . . . H15A H 0.9798 0.4829 0.0852 0.031 Uiso 1 1 calc R A . C16 C 1.1658(5) 0.5374(6) 0.1607(3) 0.0318(11) Uani 1 1 d . A . H16A H 1.2035 0.4890 0.1270 0.038 Uiso 1 1 calc R . . C17 C 1.2251(5) 0.6250(6) 0.2434(4) 0.0334(11) Uani 1 1 d . . . H17A H 1.3101 0.6461 0.2746 0.040 Uiso 1 1 calc R A . C18 C 1.1354(5) 0.6757(5) 0.2717(3) 0.0286(10) Uani 1 1 d . A . H18A H 1.1488 0.7342 0.3258 0.034 Uiso 1 1 calc R . . C21 C 0.6041(10) 0.0505(8) 0.3366(4) 0.076(2) Uani 1 1 d . . . C24 C 0.5657(9) -0.0123(8) 0.2403(4) 0.076(2) Uani 1 1 d . A . H24A H 0.5430 -0.1070 0.2287 0.114 Uiso 1 1 calc R . . H24B H 0.6440 0.0368 0.2115 0.114 Uiso 1 1 calc R . . H24C H 0.4853 -0.0069 0.2187 0.114 Uiso 1 1 calc R . . C25 C 1.0493(8) 0.9453(7) 0.2978(4) 0.0489(16) Uani 1 1 d . A . H25A H 0.9930 0.9216 0.3435 0.073 Uiso 1 1 calc R . . H25B H 1.0671 1.0338 0.2914 0.073 Uiso 1 1 calc R . . H25C H 1.1374 0.9485 0.3123 0.073 Uiso 1 1 calc R . . C26 C 0.7884(9) 0.8132(10) 0.1690(6) 0.072(2) Uani 1 1 d . A . H26A H 0.7263 0.7754 0.2097 0.108 Uiso 1 1 calc R . . H26B H 0.7450 0.7575 0.1109 0.108 Uiso 1 1 calc R . . H26C H 0.8066 0.9054 0.1726 0.108 Uiso 1 1 calc R . . C27 C 1.0637(7) 0.8723(6) 0.1082(3) 0.0414(14) Uani 1 1 d . A . C28 C 1.2071(7) 0.8858(7) 0.1270(4) 0.0471(15) Uani 1 1 d . . . H28A H 1.2635 0.9232 0.0839 0.071 Uiso 1 1 calc R A . H28B H 1.1967 0.7967 0.1254 0.071 Uiso 1 1 calc R . . H28C H 1.2525 0.9460 0.1838 0.071 Uiso 1 1 calc R . . C29 C 1.0876(9) 1.0111(7) 0.1026(4) 0.059(2) Uani 1 1 d . . . H29A H 1.1383 1.0367 0.0549 0.088 Uiso 1 1 calc R A . H29B H 1.1417 1.0777 0.1560 0.088 Uiso 1 1 calc R . . H29C H 0.9983 1.0078 0.0932 0.088 Uiso 1 1 calc R . . C30 C 0.9900(9) 0.7705(7) 0.0215(4) 0.058(2) Uani 1 1 d . . . H30A H 1.0466 0.8007 -0.0231 0.086 Uiso 1 1 calc R A . H30B H 0.8999 0.7639 0.0079 0.086 Uiso 1 1 calc R . . H30C H 0.9764 0.6818 0.0246 0.086 Uiso 1 1 calc R . . I1 I 0.47497(11) 0.4864(2) 0.19523(16) 0.0512(5) Uani 0.528(7) 1 d P A 1 Si1 Si 0.6115(5) 0.2431(4) 0.3597(2) 0.0324(8) Uani 0.528(7) 1 d P A 1 C19 C 0.670(2) 0.3219(16) 0.4768(8) 0.067(5) Uani 0.528(7) 1 d P A 1 H19A H 0.6751 0.4103 0.4905 0.101 Uiso 0.528(7) 1 calc PR A 1 H19B H 0.7618 0.3330 0.4923 0.101 Uiso 0.528(7) 1 calc PR A 1 H19C H 0.6044 0.2638 0.5090 0.101 Uiso 0.528(7) 1 calc PR A 1 C20 C 0.4473(14) 0.2386(15) 0.3340(11) 0.053(3) Uani 0.528(7) 1 d P A 1 H20A H 0.4620 0.3309 0.3468 0.079 Uiso 0.528(7) 1 calc PR A 1 H20B H 0.3802 0.1869 0.3682 0.079 Uiso 0.528(7) 1 calc PR A 1 H20C H 0.4119 0.1957 0.2731 0.079 Uiso 0.528(7) 1 calc PR A 1 C22 C 0.7051(14) 0.0618(15) 0.3818(10) 0.053(4) Uani 0.528(7) 1 d P A 1 H22A H 0.7020 -0.0257 0.3714 0.079 Uiso 0.528(7) 1 calc PR A 1 H22B H 0.7006 0.0918 0.4423 0.079 Uiso 0.528(7) 1 calc PR A 1 H22C H 0.7915 0.1281 0.3670 0.079 Uiso 0.528(7) 1 calc PR A 1 C23 C 0.4526(14) -0.0206(12) 0.3780(8) 0.046(3) Uani 0.528(7) 1 d P A 1 H23A H 0.4240 -0.1153 0.3752 0.069 Uiso 0.528(7) 1 calc PR A 1 H23B H 0.3805 -0.0156 0.3448 0.069 Uiso 0.528(7) 1 calc PR A 1 H23C H 0.4666 0.0283 0.4377 0.069 Uiso 0.528(7) 1 calc PR A 1 I1A I 0.46247(17) 0.4424(4) 0.2238(2) 0.0617(8) Uani 0.472(7) 1 d P A 2 Si1A Si 0.6520(4) 0.2123(5) 0.3677(3) 0.0331(10) Uani 0.472(7) 1 d P A 2 C19A C 0.7372(18) 0.2823(19) 0.4829(9) 0.058(5) Uani 0.472(7) 1 d P A 2 H19D H 0.8275 0.2865 0.4872 0.087 Uiso 0.472(7) 1 calc PR A 2 H19E H 0.6786 0.2237 0.5176 0.087 Uiso 0.472(7) 1 calc PR A 2 H19F H 0.7497 0.3732 0.5038 0.087 Uiso 0.472(7) 1 calc PR A 2 C20A C 0.4804(15) 0.2027(18) 0.3619(13) 0.056(4) Uani 0.472(7) 1 d P A 2 H20D H 0.4349 0.1666 0.3023 0.084 Uiso 0.472(7) 1 calc PR A 2 H20E H 0.4921 0.2931 0.3835 0.084 Uiso 0.472(7) 1 calc PR A 2 H20F H 0.4233 0.1432 0.3966 0.084 Uiso 0.472(7) 1 calc PR A 2 C22A C 0.7664(17) 0.0388(15) 0.3565(9) 0.044(3) Uani 0.472(7) 1 d P A 2 H22D H 0.7431 -0.0562 0.3425 0.066 Uiso 0.472(7) 1 calc PR A 2 H22E H 0.8073 0.0802 0.4167 0.066 Uiso 0.472(7) 1 calc PR A 2 H22F H 0.8329 0.0862 0.3204 0.066 Uiso 0.472(7) 1 calc PR A 2 C23A C 0.5195(16) -0.0585(15) 0.3827(10) 0.051(4) Uani 0.472(7) 1 d P A 2 H23D H 0.5316 -0.1372 0.3623 0.076 Uiso 0.472(7) 1 calc PR A 2 H23E H 0.4214 -0.0851 0.3711 0.076 Uiso 0.472(7) 1 calc PR A 2 H23F H 0.5513 -0.0230 0.4444 0.076 Uiso 0.472(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01736(11) 0.04213(16) 0.02946(13) -0.00887(9) 0.00212(8) 0.00959(10) Fe1 0.0223(3) 0.0255(4) 0.0225(3) 0.0032(2) -0.0007(2) 0.0088(3) Si2 0.0435(9) 0.0442(9) 0.0295(7) -0.0010(6) -0.0030(6) 0.0315(8) N1 0.030(2) 0.044(3) 0.027(2) -0.0028(19) 0.0073(18) -0.007(2) N2 0.024(2) 0.041(3) 0.0264(19) -0.0002(17) 0.0000(15) 0.0205(19) O1 0.0295(19) 0.036(2) 0.0254(17) -0.0019(14) -0.0049(14) 0.0084(16) O2 0.076(2) 0.079(2) 0.0561(19) -0.0214(17) 0.0124(17) 0.028(2) C1 0.048(4) 0.045(4) 0.041(3) 0.001(3) -0.014(3) 0.002(3) C2 0.065(5) 0.086(7) 0.054(5) 0.019(4) -0.027(4) -0.018(5) C3 0.062(5) 0.092(7) 0.059(5) 0.022(5) -0.029(4) 0.004(5) C4 0.051(4) 0.055(4) 0.034(3) 0.008(3) -0.011(3) 0.007(3) C5 0.076(2) 0.079(2) 0.0561(19) -0.0214(17) 0.0124(17) 0.028(2) C6 0.076(2) 0.079(2) 0.0561(19) -0.0214(17) 0.0124(17) 0.028(2) C7 0.076(2) 0.079(2) 0.0561(19) -0.0214(17) 0.0124(17) 0.028(2) C8 0.076(2) 0.079(2) 0.0561(19) -0.0214(17) 0.0124(17) 0.028(2) C9 0.043(3) 0.026(3) 0.023(2) 0.0057(18) 0.002(2) 0.002(2) C10 0.046(3) 0.023(2) 0.028(2) 0.0047(19) 0.002(2) 0.008(2) C11 0.061(4) 0.031(3) 0.041(3) 0.007(2) -0.001(3) 0.023(3) C12 0.052(4) 0.043(3) 0.041(3) 0.013(3) -0.007(3) 0.023(3) C13 0.049(3) 0.038(3) 0.023(2) 0.006(2) -0.005(2) 0.009(3) C14 0.020(2) 0.023(2) 0.026(2) 0.0054(17) 0.0038(16) 0.0088(18) C15 0.024(2) 0.033(3) 0.022(2) 0.0081(18) 0.0060(17) 0.014(2) C16 0.022(2) 0.034(3) 0.037(3) 0.004(2) 0.0085(19) 0.014(2) C17 0.019(2) 0.034(3) 0.044(3) 0.007(2) 0.002(2) 0.011(2) C18 0.020(2) 0.027(2) 0.030(2) 0.0031(18) -0.0013(17) 0.0070(19) C21 0.080(4) 0.051(3) 0.035(2) 0.010(2) -0.005(2) -0.017(3) C24 0.080(4) 0.051(3) 0.035(2) 0.010(2) -0.005(2) -0.017(3) C25 0.077(5) 0.047(4) 0.029(3) -0.002(2) 0.004(3) 0.040(4) C26 0.060(5) 0.091(6) 0.084(6) 0.013(5) -0.001(4) 0.056(5) C27 0.065(4) 0.032(3) 0.027(2) 0.002(2) -0.001(2) 0.027(3) C28 0.053(4) 0.040(3) 0.051(4) 0.019(3) 0.019(3) 0.022(3) C29 0.097(6) 0.043(4) 0.040(3) 0.006(3) -0.003(4) 0.039(4) C30 0.093(6) 0.044(4) 0.028(3) 0.003(2) 0.000(3) 0.031(4) I1 0.0261(4) 0.0650(8) 0.0740(9) 0.0248(6) 0.0078(4) 0.0284(5) Si1 0.0344(19) 0.0277(17) 0.0284(14) 0.0079(11) 0.0086(13) 0.0094(14) C19 0.078(12) 0.053(9) 0.026(6) 0.006(5) 0.012(7) -0.003(8) C20 0.034(7) 0.049(8) 0.077(10) 0.033(7) 0.030(7) 0.014(6) C22 0.040(7) 0.052(8) 0.057(8) 0.031(7) -0.001(6) 0.009(6) C23 0.045(7) 0.030(6) 0.044(6) 0.018(5) 0.002(5) 0.000(5) I1A 0.0312(5) 0.0827(14) 0.0802(12) 0.0123(10) 0.0032(6) 0.0384(7) Si1A 0.0234(18) 0.033(2) 0.0281(16) -0.0021(14) 0.0096(13) 0.0052(15) C19A 0.049(9) 0.059(11) 0.029(6) 0.001(6) 0.011(6) 0.000(8) C20A 0.030(7) 0.049(9) 0.088(13) 0.022(8) 0.019(7) 0.017(7) C22A 0.052(9) 0.047(8) 0.034(6) 0.015(6) 0.006(6) 0.024(7) C23A 0.046(8) 0.039(8) 0.047(8) 0.005(6) 0.017(6) 0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 N2 2.207(5) . ? Dy1 N1 2.212(6) . ? Dy1 O1 2.366(4) . ? Dy1 O2 2.389(5) . ? Dy1 C14 2.839(5) . ? Dy1 C9 2.869(6) . ? Dy1 I1A 2.9457(17) . ? Dy1 I1 3.089(2) . ? Dy1 Fe1 3.3006(15) . ? Fe1 C16 2.023(5) . ? Fe1 C12 2.030(6) . ? Fe1 C17 2.031(5) . ? Fe1 C11 2.034(6) . ? Fe1 C13 2.042(6) . ? Fe1 C10 2.042(5) . ? Fe1 C15 2.043(5) . ? Fe1 C18 2.049(5) . ? Fe1 C9 2.099(5) . ? Fe1 C14 2.109(5) . ? Si2 N2 1.722(5) . ? Si2 C26 1.866(7) . ? Si2 C25 1.869(6) . ? Si2 C27 1.898(7) . ? N1 C9 1.399(8) . ? N1 Si1 1.718(6) . ? N1 Si1A 1.810(7) . ? N2 C14 1.399(6) . ? O1 C4 1.445(7) . ? O1 C1 1.454(7) . ? O2 C5 1.434(11) . ? O2 C8 1.462(11) . ? C1 C2 1.488(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.430(12) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.446(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.479(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.416(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.533(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C13 1.442(8) . ? C9 C10 1.443(8) . ? C10 C11 1.415(9) . ? C10 H10A 0.9500 . ? C11 C12 1.422(9) . ? C11 H11A 0.9500 . ? C12 C13 1.412(10) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C18 1.437(6) . ? C14 C15 1.442(7) . ? C15 C16 1.408(7) . ? C15 H15A 0.9500 . ? C16 C17 1.418(8) . ? C16 H16A 0.9500 . ? C17 C18 1.422(7) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C21 C22 1.257(16) . ? C21 C24 1.529(9) . ? C21 C23A 1.532(15) . ? C21 Si1A 1.649(10) . ? C21 C23 1.714(16) . ? C21 C22A 1.892(19) . ? C21 Si1 2.152(11) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.528(9) . ? C27 C28 1.537(10) . ? C27 C30 1.538(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? Si1 C20 1.830(16) . ? Si1 C19 1.868(14) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? Si1A C20A 1.853(16) . ? Si1A C19A 1.888(16) . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Dy1 N1 134.73(17) . . ? N2 Dy1 O1 93.34(15) . . ? N1 Dy1 O1 93.64(16) . . ? N2 Dy1 O2 92.5(2) . . ? N1 Dy1 O2 90.8(2) . . ? O1 Dy1 O2 166.56(19) . . ? N2 Dy1 C14 28.87(14) . . ? N1 Dy1 C14 106.45(17) . . ? O1 Dy1 C14 90.34(13) . . ? O2 Dy1 C14 100.56(18) . . ? N2 Dy1 C9 106.87(16) . . ? N1 Dy1 C9 28.39(17) . . ? O1 Dy1 C9 90.89(15) . . ? O2 Dy1 C9 99.0(2) . . ? C14 Dy1 C9 78.22(15) . . ? N2 Dy1 I1A 120.39(15) . . ? N1 Dy1 I1A 104.86(17) . . ? O1 Dy1 I1A 83.10(10) . . ? O2 Dy1 I1A 83.50(17) . . ? C14 Dy1 I1A 148.34(14) . . ? C9 Dy1 I1A 132.58(15) . . ? N2 Dy1 I1 107.30(12) . . ? N1 Dy1 I1 117.96(14) . . ? O1 Dy1 I1 79.60(10) . . ? O2 Dy1 I1 87.11(17) . . ? C14 Dy1 I1 134.85(11) . . ? C9 Dy1 I1 144.95(12) . . ? I1A Dy1 I1 13.54(5) . . ? N2 Dy1 Fe1 68.09(11) . . ? N1 Dy1 Fe1 67.36(14) . . ? O1 Dy1 Fe1 89.10(10) . . ? O2 Dy1 Fe1 104.31(17) . . ? C14 Dy1 Fe1 39.28(10) . . ? C9 Dy1 Fe1 39.00(11) . . ? I1A Dy1 Fe1 168.69(7) . . ? I1 Dy1 Fe1 167.65(5) . . ? C16 Fe1 C12 114.5(3) . . ? C16 Fe1 C17 41.0(2) . . ? C12 Fe1 C17 99.6(3) . . ? C16 Fe1 C11 98.2(3) . . ? C12 Fe1 C11 41.0(2) . . ? C17 Fe1 C11 112.7(3) . . ? C16 Fe1 C13 153.1(2) . . ? C12 Fe1 C13 40.6(3) . . ? C17 Fe1 C13 120.8(2) . . ? C11 Fe1 C13 68.7(3) . . ? C16 Fe1 C10 117.5(2) . . ? C12 Fe1 C10 68.4(3) . . ? C17 Fe1 C10 150.2(2) . . ? C11 Fe1 C10 40.6(3) . . ? C13 Fe1 C10 68.3(2) . . ? C16 Fe1 C15 40.5(2) . . ? C12 Fe1 C15 152.5(3) . . ? C17 Fe1 C15 68.3(2) . . ? C11 Fe1 C15 119.1(2) . . ? C13 Fe1 C15 166.2(2) . . ? C10 Fe1 C15 109.4(2) . . ? C16 Fe1 C18 68.8(2) . . ? C12 Fe1 C18 119.3(2) . . ? C17 Fe1 C18 40.8(2) . . ? C11 Fe1 C18 150.9(2) . . ? C13 Fe1 C18 111.0(2) . . ? C10 Fe1 C18 168.3(2) . . ? C15 Fe1 C18 68.3(2) . . ? C16 Fe1 C9 157.2(2) . . ? C12 Fe1 C9 68.5(3) . . ? C17 Fe1 C9 161.0(2) . . ? C11 Fe1 C9 68.8(3) . . ? C13 Fe1 C9 40.7(2) . . ? C10 Fe1 C9 40.8(2) . . ? C15 Fe1 C9 128.8(2) . . ? C18 Fe1 C9 131.2(2) . . ? C16 Fe1 C14 68.4(2) . . ? C12 Fe1 C14 158.8(2) . . ? C17 Fe1 C14 68.2(2) . . ? C11 Fe1 C14 159.2(2) . . ? C13 Fe1 C14 130.0(2) . . ? C10 Fe1 C14 130.5(2) . . ? C15 Fe1 C14 40.62(19) . . ? C18 Fe1 C14 40.40(18) . . ? C9 Fe1 C14 117.7(2) . . ? C16 Fe1 Dy1 120.37(15) . . ? C12 Fe1 Dy1 125.0(2) . . ? C17 Fe1 Dy1 124.57(16) . . ? C11 Fe1 Dy1 122.5(2) . . ? C13 Fe1 Dy1 85.9(2) . . ? C10 Fe1 Dy1 82.44(19) . . ? C15 Fe1 Dy1 80.30(13) . . ? C18 Fe1 Dy1 85.85(14) . . ? C9 Fe1 Dy1 59.32(18) . . ? C14 Fe1 Dy1 58.47(12) . . ? N2 Si2 C26 107.4(4) . . ? N2 Si2 C25 112.2(3) . . ? C26 Si2 C25 108.4(4) . . ? N2 Si2 C27 113.4(2) . . ? C26 Si2 C27 107.8(4) . . ? C25 Si2 C27 107.5(3) . . ? C9 N1 Si1 130.6(5) . . ? C9 N1 Si1A 107.6(5) . . ? Si1 N1 Si1A 23.26(14) . . ? C9 N1 Dy1 102.9(3) . . ? Si1 N1 Dy1 125.1(4) . . ? Si1A N1 Dy1 148.2(4) . . ? C14 N2 Si2 118.5(3) . . ? C14 N2 Dy1 101.5(3) . . ? Si2 N2 Dy1 138.0(2) . . ? C4 O1 C1 108.8(4) . . ? C4 O1 Dy1 122.0(4) . . ? C1 O1 Dy1 122.9(4) . . ? C5 O2 C8 109.8(6) . . ? C5 O2 Dy1 118.4(5) . . ? C8 O2 Dy1 131.6(5) . . ? O1 C1 C2 105.8(6) . . ? O1 C1 H1A 110.6 . . ? C2 C1 H1A 110.6 . . ? O1 C1 H1B 110.6 . . ? C2 C1 H1B 110.6 . . ? H1A C1 H1B 108.7 . . ? C3 C2 C1 107.9(6) . . ? C3 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? C3 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C2 C3 C4 109.0(7) . . ? C2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? C2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? O1 C4 C3 107.2(6) . . ? O1 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? O1 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? O2 C5 C6 109.4(8) . . ? O2 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O2 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C7 C6 C5 100.2(7) . . ? C7 C6 H6A 111.7 . . ? C5 C6 H6A 111.7 . . ? C7 C6 H6B 111.7 . . ? C5 C6 H6B 111.7 . . ? H6A C6 H6B 109.5 . . ? C6 C7 C8 113.1(7) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O2 C8 C7 100.0(8) . . ? O2 C8 H8A 111.8 . . ? C7 C8 H8A 111.8 . . ? O2 C8 H8B 111.8 . . ? C7 C8 H8B 111.8 . . ? H8A C8 H8B 109.5 . . ? N1 C9 C13 127.5(5) . . ? N1 C9 C10 127.2(5) . . ? C13 C9 C10 105.3(6) . . ? N1 C9 Fe1 130.3(4) . . ? C13 C9 Fe1 67.5(3) . . ? C10 C9 Fe1 67.5(3) . . ? N1 C9 Dy1 48.7(3) . . ? C13 C9 Dy1 117.3(4) . . ? C10 C9 Dy1 111.1(4) . . ? Fe1 C9 Dy1 81.68(18) . . ? C11 C10 C9 109.5(5) . . ? C11 C10 Fe1 69.4(3) . . ? C9 C10 Fe1 71.7(3) . . ? C11 C10 H10A 125.2 . . ? C9 C10 H10A 125.2 . . ? Fe1 C10 H10A 125.2 . . ? C10 C11 C12 107.5(6) . . ? C10 C11 Fe1 70.0(3) . . ? C12 C11 Fe1 69.4(3) . . ? C10 C11 H11A 126.3 . . ? C12 C11 H11A 126.3 . . ? Fe1 C11 H11A 126.0 . . ? C13 C12 C11 108.4(6) . . ? C13 C12 Fe1 70.2(3) . . ? C11 C12 Fe1 69.7(3) . . ? C13 C12 H12A 125.8 . . ? C11 C12 H12A 125.8 . . ? Fe1 C12 H12A 125.9 . . ? C12 C13 C9 109.2(5) . . ? C12 C13 Fe1 69.3(3) . . ? C9 C13 Fe1 71.8(3) . . ? C12 C13 H13A 125.4 . . ? C9 C13 H13A 125.4 . . ? Fe1 C13 H13A 125.1 . . ? N2 C14 C18 128.0(4) . . ? N2 C14 C15 126.2(4) . . ? C18 C14 C15 105.8(4) . . ? N2 C14 Fe1 131.7(3) . . ? C18 C14 Fe1 67.6(3) . . ? C15 C14 Fe1 67.2(3) . . ? N2 C14 Dy1 49.6(2) . . ? C18 C14 Dy1 119.3(3) . . ? C15 C14 Dy1 108.9(3) . . ? Fe1 C14 Dy1 82.25(15) . . ? C16 C15 C14 109.3(4) . . ? C16 C15 Fe1 69.0(3) . . ? C14 C15 Fe1 72.1(3) . . ? C16 C15 H15A 125.4 . . ? C14 C15 H15A 125.4 . . ? Fe1 C15 H15A 125.1 . . ? C15 C16 C17 108.0(4) . . ? C15 C16 Fe1 70.5(3) . . ? C17 C16 Fe1 69.8(3) . . ? C15 C16 H16A 126.0 . . ? C17 C16 H16A 126.0 . . ? Fe1 C16 H16A 125.3 . . ? C16 C17 C18 108.1(4) . . ? C16 C17 Fe1 69.2(3) . . ? C18 C17 Fe1 70.3(3) . . ? C16 C17 H17A 125.9 . . ? C18 C17 H17A 125.9 . . ? Fe1 C17 H17A 126.1 . . ? C17 C18 C14 108.7(4) . . ? C17 C18 Fe1 68.9(3) . . ? C14 C18 Fe1 72.0(3) . . ? C17 C18 H18A 125.6 . . ? C14 C18 H18A 125.6 . . ? Fe1 C18 H18A 125.0 . . ? C22 C21 C24 124.3(13) . . ? C22 C21 C23A 83.4(10) . . ? C24 C21 C23A 108.5(8) . . ? C22 C21 Si1A 94.0(9) . . ? C24 C21 Si1A 116.3(6) . . ? C23A C21 Si1A 126.5(8) . . ? C22 C21 C23 113.0(9) . . ? C24 C21 C23 105.6(7) . . ? C23A C21 C23 36.6(7) . . ? Si1A C21 C23 101.5(8) . . ? C22 C21 C22A 24.9(9) . . ? C24 C21 C22A 99.5(8) . . ? C23A C21 C22A 93.7(10) . . ? Si1A C21 C22A 105.8(6) . . ? C23 C21 C22A 129.2(8) . . ? C22 C21 Si1 109.3(9) . . ? C24 C21 Si1 107.6(6) . . ? C23A C21 Si1 123.6(9) . . ? Si1A C21 Si1 15.6(2) . . ? C23 C21 Si1 92.3(7) . . ? C22A C21 Si1 121.0(6) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 106.9(6) . . ? C29 C27 C30 109.3(5) . . ? C28 C27 C30 108.9(6) . . ? C29 C27 Si2 110.0(5) . . ? C28 C27 Si2 111.7(4) . . ? C30 C27 Si2 110.0(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 Si1 C20 113.8(5) . . ? N1 Si1 C19 111.8(5) . . ? C20 Si1 C19 107.0(9) . . ? N1 Si1 C21 101.6(4) . . ? C20 Si1 C21 116.0(6) . . ? C19 Si1 C21 106.5(7) . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 Si1A N1 121.1(4) . . ? C21 Si1A C20A 100.0(7) . . ? N1 Si1A C20A 101.0(7) . . ? C21 Si1A C19A 110.3(7) . . ? N1 Si1A C19A 113.7(6) . . ? C20A Si1A C19A 108.5(9) . . ? Si1A C19A H19D 109.5 . . ? Si1A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? Si1A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? Si1A C20A H20D 109.5 . . ? Si1A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? Si1A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C21 C22A H22D 109.5 . . ? C21 C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C21 C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C21 C23A H23D 109.5 . . ? C21 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C21 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.165 _refine_diff_density_min -5.222 _refine_diff_density_rms 0.155 #===END data_Dy2-biph _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H118 Dy2 Fe2 K2 N4 Si4' _chemical_formula_weight 1811.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Dy' 'Dy' -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.320(3) _cell_length_b 21.816(5) _cell_length_c 26.408(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.561(3) _cell_angle_gamma 90.00 _cell_volume 8211(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 2.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6382 _exptl_absorpt_correction_T_max 0.7990 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57552 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 30.85 _reflns_number_total 12199 _reflns_number_gt 10408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2, 2013' _computing_cell_refinement 'SAINT V8.32B (Bruker AXS Inc., 2013' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013' _computing_structure_solution 'SHELXS-2013 (Sheldrick 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+54.4145P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12199 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.084277(8) 0.842990(6) 0.819514(5) 0.01450(4) Uani 1 1 d . . . Fe1 Fe 0.07183(3) 0.858116(19) 0.939732(16) 0.01997(9) Uani 1 1 d . D . K1 K 0.13819(6) 1.03715(3) 0.83199(3) 0.03108(16) Uani 1 1 d . . . Si2 Si 0.16822(5) 0.68354(4) 0.85328(3) 0.01873(15) Uani 1 1 d . D . N1 N 0.1948(2) 0.91539(13) 0.85659(11) 0.0285(2) Uani 1 1 d . . . N2 N 0.12274(17) 0.75424(11) 0.86266(9) 0.0179(5) Uani 1 1 d . . . C1 C 0.0000 0.77597(19) 0.7500 0.0204(8) Uani 1 2 d S . . H1A H 0.0000 0.7324 0.7500 0.024 Uiso 1 2 calc SR D . C2 C -0.0739(2) 0.80820(13) 0.77080(11) 0.0188(5) Uani 1 1 d . . . H2A H -0.1260 0.7863 0.7813 0.023 Uiso 1 1 calc R . . C3 C -0.06953(19) 0.87531(13) 0.77611(10) 0.0163(5) Uani 1 1 d . . . H3A H -0.1112 0.8960 0.7962 0.020 Uiso 1 1 calc R D . C4 C 0.0000 0.91040(17) 0.7500 0.0146(7) Uani 1 2 d S . . C5 C 0.0000 0.97510(18) 0.7500 0.0170(7) Uani 1 2 d S . . C6 C -0.0621(2) 1.01066(14) 0.77825(12) 0.0237(6) Uani 1 1 d . . . H6A H -0.1050 0.9900 0.7976 0.028 Uiso 1 1 calc R . . C7 C -0.0609(3) 1.07417(16) 0.77790(14) 0.0359(9) Uani 1 1 d . . . H7A H -0.1027 1.0958 0.7972 0.043 Uiso 1 1 calc R D . C8 C 0.0000 1.1073(2) 0.7500 0.0432(15) Uani 1 2 d S . . H8A H 0.0000 1.1508 0.7500 0.052 Uiso 1 2 calc SR . . C9 C 0.1499(2) 0.92273(16) 0.90054(14) 0.0285(2) Uani 1 1 d . D . C10 C 0.0519(2) 0.93963(15) 0.90101(14) 0.0285(2) Uani 1 1 d . . . H10A H 0.0092 0.9460 0.8717 0.034 Uiso 1 1 calc R D . C11 C 0.0297(2) 0.94521(15) 0.95208(13) 0.0285(2) Uani 1 1 d . D . H11A H -0.0295 0.9563 0.9627 0.034 Uiso 1 1 calc R . . C12 C 0.1116(2) 0.93125(15) 0.98418(14) 0.0285(2) Uani 1 1 d . . . H12A H 0.1173 0.9320 1.0203 0.034 Uiso 1 1 calc R D . C13 C 0.1839(2) 0.91584(15) 0.95335(13) 0.0285(2) Uani 1 1 d . D . H13A H 0.2454 0.9030 0.9656 0.034 Uiso 1 1 calc R . . C14 C 0.0822(2) 0.76937(13) 0.90687(11) 0.0185(5) Uani 1 1 d . D . C15 C -0.0140(2) 0.78856(13) 0.90892(11) 0.0203(5) Uani 1 1 d . . . H15A H -0.0594 0.7926 0.8804 0.024 Uiso 1 1 calc R D . C16 C -0.0301(2) 0.80049(15) 0.96046(12) 0.0252(6) Uani 1 1 d . D . H16A H -0.0876 0.8131 0.9723 0.030 Uiso 1 1 calc R . . C17 C 0.0556(3) 0.79012(15) 0.99091(12) 0.0277(7) Uani 1 1 d . . . H17A H 0.0651 0.7939 1.0269 0.033 Uiso 1 1 calc R D . C18 C 0.1246(2) 0.77308(14) 0.95841(12) 0.0242(6) Uani 1 1 d . D . H18A H 0.1887 0.7653 0.9691 0.029 Uiso 1 1 calc R . . C19 C 0.3672(2) 0.97849(18) 0.90213(16) 0.0359(8) Uani 1 1 d . . . H19A H 0.4077 0.9676 0.9329 0.054 Uiso 1 1 calc R A 1 H19B H 0.3160 1.0048 0.9113 0.054 Uiso 1 1 calc R A 1 H19C H 0.4041 1.0004 0.8785 0.054 Uiso 1 1 calc R A 1 C20 C 0.3263(2) 0.96062(15) 0.77701(14) 0.0285(2) Uani 1 1 d . . . H20A H 0.2576 0.9598 0.7724 0.043 Uiso 1 1 calc R B 1 H20B H 0.3510 0.9621 0.7437 0.043 Uiso 1 1 calc R B 1 H20C H 0.3472 0.9970 0.7968 0.043 Uiso 1 1 calc R B 1 C22 C 0.3637(2) 0.83138(15) 0.90333(14) 0.0285(2) Uani 1 1 d . . . H22A H 0.3298 0.7959 0.8879 0.043 Uiso 1 1 calc R C 1 H22B H 0.3548 0.8333 0.9396 0.043 Uiso 1 1 calc R C 1 H22C H 0.4307 0.8273 0.8992 0.043 Uiso 1 1 calc R C 1 C25 C 0.2778(2) 0.66561(16) 0.89611(15) 0.0317(7) Uani 1 1 d . . . H25A H 0.3282 0.6934 0.8883 0.048 Uiso 1 1 calc R D . H25B H 0.2967 0.6231 0.8906 0.048 Uiso 1 1 calc R . . H25C H 0.2654 0.6710 0.9317 0.048 Uiso 1 1 calc R . . C26 C 0.2021(2) 0.67898(16) 0.78671(13) 0.0277(7) Uani 1 1 d . . . H26A H 0.2425 0.7138 0.7802 0.042 Uiso 1 1 calc R D . H26B H 0.1454 0.6801 0.7627 0.042 Uiso 1 1 calc R . . H26C H 0.2360 0.6406 0.7823 0.042 Uiso 1 1 calc R . . C27 C 0.0815(2) 0.61964(14) 0.86319(13) 0.0243(6) Uani 1 1 d . . . C28 C -0.0145(3) 0.63485(18) 0.83563(18) 0.0403(9) Uani 1 1 d . D . H28A H -0.0591 0.6023 0.8418 0.060 Uiso 1 1 calc R . . H28B H -0.0092 0.6382 0.7990 0.060 Uiso 1 1 calc R . . H28C H -0.0368 0.6739 0.8484 0.060 Uiso 1 1 calc R . . C29 C 0.0716(3) 0.61151(18) 0.91987(15) 0.0386(9) Uani 1 1 d . D . H29A H 0.0274 0.5782 0.9246 0.058 Uiso 1 1 calc R . . H29B H 0.0481 0.6496 0.9337 0.058 Uiso 1 1 calc R . . H29C H 0.1329 0.6016 0.9377 0.058 Uiso 1 1 calc R . . C30 C 0.1152(3) 0.55896(15) 0.84212(16) 0.0359(8) Uani 1 1 d . D . H30A H 0.0728 0.5259 0.8502 0.054 Uiso 1 1 calc R . . H30B H 0.1787 0.5500 0.8575 0.054 Uiso 1 1 calc R . . H30C H 0.1156 0.5622 0.8051 0.054 Uiso 1 1 calc R . . C31 C 0.1255(9) 1.2353(3) 0.8176(3) 0.143(5) Uani 1 1 d . D . H31A H 0.1768 1.2652 0.8218 0.214 Uiso 1 1 calc R . . H31B H 0.0655 1.2565 0.8193 0.214 Uiso 1 1 calc R . . H31C H 0.1258 1.2149 0.7846 0.214 Uiso 1 1 calc R . . C32 C 0.1382(4) 1.1887(2) 0.85911(17) 0.0506(12) Uani 1 1 d . . . C33 C 0.0638(3) 1.1656(2) 0.88091(19) 0.0478(11) Uani 1 1 d . D . H33A H -0.0011 1.1812 0.8710 0.057 Uiso 1 1 calc R . . C34 C 0.0820(6) 1.1212(3) 0.9230(3) 0.092(3) Uani 1 1 d . . . H34A H 0.0333 1.1090 0.9458 0.110 Uiso 1 1 calc R D . C35 C 0.1840(6) 1.1096(3) 0.93597(18) 0.082(2) Uani 1 1 d . D . H35A H 0.2069 1.0873 0.9679 0.099 Uiso 1 1 calc R . . C36 C 0.2447(5) 1.1372(4) 0.9077(3) 0.080(2) Uani 1 1 d . . . H36A H 0.3130 1.1302 0.9178 0.096 Uiso 1 1 calc R D . C37 C 0.2244(4) 1.1727(3) 0.8718(3) 0.0753(19) Uani 1 1 d . D . H37A H 0.2757 1.1919 0.8541 0.090 Uiso 1 1 calc R . . C1S C 0.2888(3) 0.4288(2) 0.88776(19) 0.0498(11) Uani 1 1 d . . . H1SA H 0.3447 0.4031 0.8869 0.075 Uiso 1 1 calc R . . H1SB H 0.3073 0.4693 0.9013 0.075 Uiso 1 1 calc R . . H1SC H 0.2577 0.4333 0.8532 0.075 Uiso 1 1 calc R . . C2S C 0.2223(2) 0.39933(19) 0.92134(15) 0.0352(8) Uani 1 1 d . . . C3S C 0.1616(3) 0.4347(2) 0.94717(15) 0.0383(8) Uani 1 1 d . . . H3SA H 0.1637 0.4781 0.9448 0.046 Uiso 1 1 calc R . . C4S C 0.0981(3) 0.4072(2) 0.97632(15) 0.0400(9) Uani 1 1 d . . . H4SA H 0.0564 0.4319 0.9934 0.048 Uiso 1 1 calc R . . C5S C 0.0950(3) 0.3440(2) 0.98070(16) 0.0408(9) Uani 1 1 d . . . H5SA H 0.0511 0.3252 1.0005 0.049 Uiso 1 1 calc R . . C6S C 0.1560(3) 0.3085(2) 0.95612(17) 0.0421(9) Uani 1 1 d . . . H6SA H 0.1553 0.2652 0.9596 0.051 Uiso 1 1 calc R . . C7S C 0.2187(3) 0.33604(19) 0.92619(16) 0.0388(9) Uani 1 1 d . . . H7SA H 0.2597 0.3112 0.9088 0.047 Uiso 1 1 calc R . . Si1 Si 0.31591(12) 0.90556(8) 0.87021(7) 0.0285(2) Uani 0.575(3) 1 d P D 1 C21 C 0.3639(4) 0.9006(3) 0.8065(2) 0.0285(2) Uani 0.575(3) 1 d P D 1 C23 C 0.4723(4) 0.9001(3) 0.8146(2) 0.0285(2) Uani 0.575(3) 1 d P D 1 H23A H 0.4978 0.8977 0.7816 0.043 Uiso 0.575(3) 1 calc PR D 1 H23B H 0.4934 0.8646 0.8354 0.043 Uiso 0.575(3) 1 calc PR D 1 H23C H 0.4944 0.9378 0.8321 0.043 Uiso 0.575(3) 1 calc PR D 1 C24 C 0.3335(4) 0.8411(3) 0.7793(3) 0.0285(2) Uani 0.575(3) 1 d P D 1 H24A H 0.3588 0.8397 0.7461 0.043 Uiso 0.575(3) 1 calc PR D 1 H24B H 0.2648 0.8393 0.7743 0.043 Uiso 0.575(3) 1 calc PR D 1 H24C H 0.3573 0.8060 0.7999 0.043 Uiso 0.575(3) 1 calc PR D 1 Si1A Si 0.31096(12) 0.93205(9) 0.84700(7) 0.0161(5) Uani 0.425(3) 1 d P D 2 C21A C 0.3860(6) 0.8605(4) 0.8475(3) 0.0285(2) Uani 0.425(3) 1 d P D 2 C23A C 0.4903(5) 0.8789(4) 0.8451(3) 0.0272(16) Uani 0.425(3) 1 d P D 2 H23D H 0.5291 0.8419 0.8454 0.041 Uiso 0.425(3) 1 calc PR D 2 H23E H 0.5110 0.9044 0.8747 0.041 Uiso 0.425(3) 1 calc PR D 2 H23F H 0.4965 0.9021 0.8138 0.041 Uiso 0.425(3) 1 calc PR D 2 C24A C 0.3545(6) 0.8198(4) 0.8019(4) 0.036(2) Uani 0.425(3) 1 d P D 2 H24D H 0.3940 0.7830 0.8027 0.053 Uiso 0.425(3) 1 calc PR D 2 H24E H 0.3605 0.8425 0.7703 0.053 Uiso 0.425(3) 1 calc PR D 2 H24F H 0.2889 0.8078 0.8034 0.053 Uiso 0.425(3) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01521(6) 0.01240(6) 0.01502(6) 0.00007(4) -0.00304(4) -0.00032(4) Fe1 0.0298(2) 0.01490(19) 0.01403(19) -0.00012(15) -0.00393(15) -0.00047(15) K1 0.0465(4) 0.0225(3) 0.0227(3) -0.0006(3) -0.0042(3) -0.0109(3) Si2 0.0169(3) 0.0145(4) 0.0244(4) 0.0025(3) -0.0001(3) 0.0012(3) N1 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) N2 0.0198(11) 0.0140(11) 0.0191(11) 0.0010(9) -0.0028(9) 0.0007(8) C1 0.0260(19) 0.0137(18) 0.0193(19) 0.000 -0.0093(15) 0.000 C2 0.0190(12) 0.0162(13) 0.0200(13) 0.0032(10) -0.0043(10) -0.0044(10) C3 0.0166(11) 0.0179(13) 0.0144(12) 0.0000(10) 0.0015(9) -0.0009(9) C4 0.0149(15) 0.0144(17) 0.0142(17) 0.000 -0.0008(12) 0.000 C5 0.0210(17) 0.0144(17) 0.0148(17) 0.000 -0.0027(13) 0.000 C6 0.0283(15) 0.0207(14) 0.0209(14) -0.0021(11) -0.0045(11) 0.0073(11) C7 0.054(2) 0.0230(17) 0.0279(17) -0.0084(14) -0.0118(15) 0.0151(15) C8 0.076(4) 0.015(2) 0.033(3) 0.000 -0.018(3) 0.000 C9 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C10 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C11 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C12 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C13 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C14 0.0241(13) 0.0121(12) 0.0183(13) 0.0003(10) -0.0035(10) -0.0011(10) C15 0.0248(13) 0.0177(13) 0.0176(13) 0.0009(10) -0.0026(10) -0.0018(10) C16 0.0339(16) 0.0226(15) 0.0190(14) 0.0003(12) 0.0025(12) -0.0021(12) C17 0.0463(19) 0.0194(15) 0.0159(14) 0.0040(11) -0.0044(13) -0.0032(13) C18 0.0329(16) 0.0158(13) 0.0216(14) 0.0029(11) -0.0094(12) -0.0006(11) C19 0.0251(15) 0.0354(19) 0.046(2) -0.0117(16) -0.0009(14) -0.0117(14) C20 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C22 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C25 0.0246(15) 0.0266(17) 0.042(2) 0.0043(14) -0.0065(13) 0.0051(12) C26 0.0262(15) 0.0236(15) 0.0345(18) 0.0055(13) 0.0080(13) 0.0050(12) C27 0.0303(15) 0.0139(13) 0.0290(16) -0.0005(12) 0.0040(12) -0.0032(11) C28 0.0276(17) 0.0283(18) 0.064(3) 0.0076(18) -0.0030(17) -0.0123(14) C29 0.058(2) 0.0272(18) 0.0329(19) -0.0025(15) 0.0171(17) -0.0156(16) C30 0.054(2) 0.0161(15) 0.039(2) -0.0028(14) 0.0111(17) -0.0041(14) C31 0.340(15) 0.038(3) 0.058(4) -0.008(3) 0.066(6) -0.049(6) C32 0.084(3) 0.033(2) 0.039(2) -0.0173(18) 0.025(2) -0.017(2) C33 0.040(2) 0.048(3) 0.056(3) -0.025(2) 0.0044(19) 0.0035(18) C34 0.142(6) 0.072(4) 0.076(4) -0.049(3) 0.086(5) -0.052(4) C35 0.166(7) 0.055(3) 0.020(2) -0.014(2) -0.023(3) 0.041(4) C36 0.064(4) 0.100(5) 0.074(4) -0.050(4) 0.000(3) -0.014(4) C37 0.057(3) 0.069(4) 0.100(5) -0.045(4) 0.009(3) -0.010(3) C1S 0.036(2) 0.060(3) 0.057(3) 0.010(2) 0.0213(19) 0.0053(19) C2S 0.0272(16) 0.044(2) 0.0348(19) 0.0040(16) 0.0053(14) 0.0041(14) C3S 0.0384(19) 0.040(2) 0.038(2) 0.0075(17) 0.0092(16) 0.0081(16) C4S 0.0358(19) 0.050(2) 0.035(2) 0.0043(18) 0.0109(15) 0.0100(17) C5S 0.0370(19) 0.050(2) 0.036(2) 0.0014(18) 0.0057(15) -0.0091(17) C6S 0.043(2) 0.039(2) 0.044(2) -0.0058(18) -0.0010(17) -0.0076(17) C7S 0.0321(18) 0.044(2) 0.041(2) -0.0075(17) 0.0043(15) 0.0038(15) Si1 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C21 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C23 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C24 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) Si1A 0.0117(7) 0.0184(9) 0.0180(9) 0.0047(8) 0.0004(6) -0.0048(6) C21A 0.0290(4) 0.0238(4) 0.0317(5) 0.0015(4) -0.0026(4) -0.0047(3) C23A 0.013(3) 0.034(4) 0.035(4) -0.004(3) 0.006(3) -0.005(3) C24A 0.024(4) 0.035(5) 0.048(6) -0.014(4) 0.008(4) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 N2 2.287(2) . ? Dy1 N1 2.379(3) . ? Dy1 C3 2.485(3) . ? Dy1 C2 2.494(3) 2_556 ? Dy1 C1 2.556(2) . ? Dy1 C4 2.561(2) . ? Dy1 C2 2.607(3) . ? Dy1 C3 2.611(3) 2_556 ? Dy1 C14 2.813(3) . ? Dy1 C9 2.846(3) . ? Dy1 Fe1 3.2139(9) . ? Fe1 C12 2.029(3) . ? Fe1 C11 2.029(4) . ? Fe1 C17 2.035(3) . ? Fe1 C16 2.040(3) . ? Fe1 C13 2.045(3) . ? Fe1 C18 2.045(3) . ? Fe1 C10 2.057(3) . ? Fe1 C15 2.069(3) . ? Fe1 C9 2.129(3) . ? Fe1 C14 2.133(3) . ? K1 N1 2.834(3) . ? K1 C6 3.063(3) 2_556 ? K1 C9 3.079(4) . ? K1 C5 3.0994(19) . ? K1 C7 3.111(4) 2_556 ? K1 C6 3.128(3) . ? K1 C10 3.132(4) . ? K1 C7 3.167(4) . ? K1 C8 3.180(3) . ? K1 C35 3.181(5) . ? K1 C34 3.187(5) . ? K1 C36 3.240(6) . ? Si2 N2 1.702(3) . ? Si2 C26 1.871(4) . ? Si2 C25 1.884(3) . ? Si2 C27 1.902(3) . ? N1 C9 1.389(5) . ? N1 Si1A 1.745(3) . ? N1 Si1 1.750(3) . ? N2 C14 1.393(4) . ? C1 C2 1.424(4) 2_556 ? C1 C2 1.424(4) . ? C1 Dy1 2.556(2) 2_556 ? C1 H1A 0.9500 . ? C2 C3 1.472(4) . ? C2 Dy1 2.494(3) 2_556 ? C2 H2A 0.9500 . ? C3 C4 1.478(3) . ? C3 Dy1 2.611(3) 2_556 ? C3 H3A 0.9500 . ? C4 C5 1.412(5) . ? C4 C3 1.478(3) 2_556 ? C4 Dy1 2.561(2) 2_556 ? C5 C6 1.441(4) 2_556 ? C5 C6 1.441(4) . ? C5 K1 3.0994(19) 2_556 ? C6 C7 1.386(5) . ? C6 K1 3.063(3) 2_556 ? C6 H6A 0.9500 . ? C7 C8 1.396(5) . ? C7 K1 3.111(4) 2_556 ? C7 H7A 0.9500 . ? C8 C7 1.396(5) 2_556 ? C8 K1 3.180(3) 2_556 ? C8 H8A 0.9500 . ? C9 C13 1.440(5) . ? C9 C10 1.452(5) . ? C10 C11 1.420(5) . ? C10 H10A 0.9500 . ? C11 C12 1.412(5) . ? C11 H11A 0.9500 . ? C12 C13 1.419(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C18 1.437(4) . ? C14 C15 1.446(4) . ? C15 C16 1.426(4) . ? C15 H15A 0.9500 . ? C16 C17 1.418(5) . ? C16 H16A 0.9500 . ? C17 C18 1.420(5) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 Si1A 1.889(4) . ? C19 Si1 1.913(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.591(7) . ? C20 Si1A 1.983(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C22 C21A 1.666(9) . ? C22 Si1 1.933(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.528(5) . ? C27 C28 1.528(5) . ? C27 C30 1.532(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.492(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.295(8) . ? C32 C33 1.356(7) . ? C33 C34 1.480(9) . ? C33 H33A 1.0000 . ? C34 C35 1.489(10) . ? C34 H34A 1.0000 . ? C35 C36 1.343(10) . ? C35 H35A 1.0000 . ? C36 C37 1.237(10) . ? C36 H36A 1.0000 . ? C37 H37A 1.0000 . ? C1S C2S 1.507(5) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S C7S 1.388(6) . ? C2S C3S 1.390(5) . ? C3S C4S 1.383(5) . ? C3S H3SA 0.9500 . ? C4S C5S 1.386(6) . ? C4S H4SA 0.9500 . ? C5S C6S 1.375(6) . ? C5S H5SA 0.9500 . ? C6S C7S 1.388(6) . ? C6S H6SA 0.9500 . ? C7S H7SA 0.9500 . ? Si1 C21 1.880(7) . ? C21 C24 1.527(8) . ? C21 C23 1.546(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Si1A C21A 1.894(9) . ? C21A C24A 1.528(12) . ? C21A C23A 1.554(10) . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Dy1 N1 103.81(9) . . ? N2 Dy1 C3 129.06(9) . . ? N1 Dy1 C3 121.74(10) . . ? N2 Dy1 C2 102.01(9) . 2_556 ? N1 Dy1 C2 124.86(10) . 2_556 ? C3 Dy1 C2 71.15(9) . 2_556 ? N2 Dy1 C1 87.00(10) . . ? N1 Dy1 C1 157.58(8) . . ? C3 Dy1 C1 59.69(9) . . ? C2 Dy1 C1 32.72(7) 2_556 . ? N2 Dy1 C4 156.54(9) . . ? N1 Dy1 C4 99.34(10) . . ? C3 Dy1 C4 34.03(7) . . ? C2 Dy1 C4 60.58(9) 2_556 . ? C1 Dy1 C4 69.93(10) . . ? N2 Dy1 C2 98.93(9) . . ? N1 Dy1 C2 155.23(9) . . ? C3 Dy1 C2 33.49(9) . . ? C2 Dy1 C2 58.04(12) 2_556 . ? C1 Dy1 C2 32.00(7) . . ? C4 Dy1 C2 59.13(9) . . ? N2 Dy1 C3 134.73(9) . 2_556 ? N1 Dy1 C3 101.95(10) . 2_556 ? C3 Dy1 C3 59.47(11) . 2_556 ? C2 Dy1 C3 33.41(9) 2_556 2_556 ? C1 Dy1 C3 58.10(9) . 2_556 ? C4 Dy1 C3 33.20(7) . 2_556 ? C2 Dy1 C3 67.43(9) . 2_556 ? N2 Dy1 C14 29.45(9) . . ? N1 Dy1 C14 95.79(9) . . ? C3 Dy1 C14 117.46(9) . . ? C2 Dy1 C14 127.31(9) 2_556 . ? C1 Dy1 C14 102.74(9) . . ? C4 Dy1 C14 150.91(6) . . ? C2 Dy1 C14 99.26(9) . . ? C3 Dy1 C14 160.23(8) 2_556 . ? N2 Dy1 C9 95.56(9) . . ? N1 Dy1 C9 29.13(10) . . ? C3 Dy1 C9 112.76(10) . . ? C2 Dy1 C9 152.88(10) 2_556 . ? C1 Dy1 C9 171.17(8) . . ? C4 Dy1 C9 106.64(10) . . ? C2 Dy1 C9 139.19(10) . . ? C3 Dy1 C9 123.51(9) 2_556 . ? C14 Dy1 C9 76.19(9) . . ? N2 Dy1 Fe1 68.19(6) . . ? N1 Dy1 Fe1 67.89(7) . . ? C3 Dy1 Fe1 107.16(7) . . ? C2 Dy1 Fe1 166.45(7) 2_556 . ? C1 Dy1 Fe1 134.47(4) . . ? C4 Dy1 Fe1 125.57(5) . . ? C2 Dy1 Fe1 112.88(7) . . ? C3 Dy1 Fe1 157.03(6) 2_556 . ? C14 Dy1 Fe1 40.77(6) . . ? C9 Dy1 Fe1 40.57(7) . . ? C12 Fe1 C11 40.71(13) . . ? C12 Fe1 C17 103.46(14) . . ? C11 Fe1 C17 121.39(15) . . ? C12 Fe1 C16 119.81(14) . . ? C11 Fe1 C16 107.61(14) . . ? C17 Fe1 C16 40.71(13) . . ? C12 Fe1 C13 40.75(14) . . ? C11 Fe1 C13 68.62(14) . . ? C17 Fe1 C13 118.07(14) . . ? C16 Fe1 C13 154.41(14) . . ? C12 Fe1 C18 119.83(13) . . ? C11 Fe1 C18 156.79(13) . . ? C17 Fe1 C18 40.72(14) . . ? C16 Fe1 C18 68.48(14) . . ? C13 Fe1 C18 104.54(14) . . ? C12 Fe1 C10 68.01(14) . . ? C11 Fe1 C10 40.67(14) . . ? C17 Fe1 C10 160.18(15) . . ? C16 Fe1 C10 126.71(14) . . ? C13 Fe1 C10 67.89(13) . . ? C18 Fe1 C10 159.07(14) . . ? C12 Fe1 C15 157.93(13) . . ? C11 Fe1 C15 125.12(13) . . ? C17 Fe1 C15 67.96(12) . . ? C16 Fe1 C15 40.60(12) . . ? C13 Fe1 C15 161.30(14) . . ? C18 Fe1 C15 67.73(12) . . ? C10 Fe1 C15 112.95(13) . . ? C12 Fe1 C9 68.25(14) . . ? C11 Fe1 C9 68.68(14) . . ? C17 Fe1 C9 154.78(14) . . ? C16 Fe1 C9 163.99(13) . . ? C13 Fe1 C9 40.30(13) . . ? C18 Fe1 C9 121.25(14) . . ? C10 Fe1 C9 40.54(13) . . ? C15 Fe1 C9 127.90(13) . . ? C12 Fe1 C14 157.27(13) . . ? C11 Fe1 C14 161.60(12) . . ? C17 Fe1 C14 68.01(12) . . ? C16 Fe1 C14 68.27(12) . . ? C13 Fe1 C14 123.10(13) . . ? C18 Fe1 C14 40.18(11) . . ? C10 Fe1 C14 126.45(13) . . ? C15 Fe1 C14 40.23(11) . . ? C9 Fe1 C14 110.03(13) . . ? C12 Fe1 Dy1 127.79(10) . . ? C11 Fe1 Dy1 107.49(10) . . ? C17 Fe1 Dy1 127.01(10) . . ? C16 Fe1 Dy1 108.14(9) . . ? C13 Fe1 Dy1 96.85(10) . . ? C18 Fe1 Dy1 95.19(9) . . ? C10 Fe1 Dy1 67.42(10) . . ? C15 Fe1 Dy1 67.91(8) . . ? C9 Fe1 Dy1 60.38(10) . . ? C14 Fe1 Dy1 59.48(8) . . ? N1 K1 C6 96.23(9) . 2_556 ? N1 K1 C9 26.77(9) . . ? C6 K1 C9 113.58(9) 2_556 . ? N1 K1 C5 84.25(9) . . ? C6 K1 C5 27.05(7) 2_556 . ? C9 K1 C5 92.94(9) . . ? N1 K1 C7 121.68(10) . 2_556 ? C6 K1 C7 25.92(9) 2_556 2_556 ? C9 K1 C7 138.87(9) . 2_556 ? C5 K1 C7 46.86(9) . 2_556 ? N1 K1 C6 99.21(8) . . ? C6 K1 C6 46.20(12) 2_556 . ? C9 K1 C6 96.45(9) . . ? C5 K1 C6 26.76(6) . . ? C7 K1 C6 52.91(10) 2_556 . ? N1 K1 C10 49.47(9) . . ? C6 K1 C10 107.51(9) 2_556 . ? C9 K1 C10 27.02(9) . . ? C5 K1 C10 81.30(8) . . ? C7 K1 C10 126.47(10) 2_556 . ? C6 K1 C10 75.08(9) . . ? N1 K1 C7 124.56(9) . . ? C6 K1 C7 52.96(9) 2_556 . ? C9 K1 C7 117.87(10) . . ? C5 K1 C7 46.41(8) . . ? C7 K1 C7 44.73(15) 2_556 . ? C6 K1 C7 25.43(9) . . ? C10 K1 C7 92.71(10) . . ? N1 K1 C8 138.77(10) . . ? C6 K1 C8 45.82(9) 2_556 . ? C9 K1 C8 141.74(9) . . ? C5 K1 C8 54.65(11) . . ? C7 K1 C8 25.61(9) 2_556 . ? C6 K1 C8 45.35(9) . . ? C10 K1 C8 117.93(8) . . ? C7 K1 C8 25.41(9) . . ? N1 K1 C35 103.72(12) . . ? C6 K1 C35 159.86(12) 2_556 . ? C9 K1 C35 84.27(13) . . ? C5 K1 C35 152.18(18) . . ? C7 K1 C35 134.54(12) 2_556 . ? C6 K1 C35 125.93(18) . . ? C10 K1 C35 83.98(16) . . ? C7 K1 C35 111.36(15) . . ? C8 K1 C35 114.31(13) . . ? N1 K1 C34 116.97(17) . . ? C6 K1 C34 137.13(19) 2_556 . ? C9 K1 C34 91.50(16) . . ? C5 K1 C34 125.98(16) . . ? C7 K1 C34 117.47(19) 2_556 . ? C6 K1 C34 99.28(17) . . ? C10 K1 C34 79.00(13) . . ? C7 K1 C34 84.94(19) . . ? C8 K1 C34 92.93(19) . . ? C35 K1 C34 27.04(19) . . ? N1 K1 C36 112.51(18) . . ? C6 K1 C36 144.73(19) 2_556 . ? C9 K1 C36 100.83(19) . . ? C5 K1 C36 162.92(17) . . ? C7 K1 C36 120.30(19) 2_556 . ? C6 K1 C36 139.52(15) . . ? C10 K1 C36 106.70(18) . . ? C7 K1 C36 117.13(16) . . ? C8 K1 C36 108.71(19) . . ? C35 K1 C36 24.12(19) . . ? C34 K1 C36 44.39(18) . . ? N2 Si2 C26 108.83(14) . . ? N2 Si2 C25 114.14(15) . . ? C26 Si2 C25 106.06(17) . . ? N2 Si2 C27 112.34(14) . . ? C26 Si2 C27 108.80(16) . . ? C25 Si2 C27 106.38(16) . . ? C9 N1 Si1A 128.5(2) . . ? C9 N1 Si1 111.8(2) . . ? Si1A N1 Si1 27.82(9) . . ? C9 N1 Dy1 94.43(19) . . ? Si1A N1 Dy1 133.16(17) . . ? Si1 N1 Dy1 127.57(16) . . ? C9 N1 K1 86.5(2) . . ? Si1A N1 K1 91.55(13) . . ? Si1 N1 K1 114.69(14) . . ? Dy1 N1 K1 111.34(11) . . ? C14 N2 Si2 122.2(2) . . ? C14 N2 Dy1 96.73(17) . . ? Si2 N2 Dy1 140.53(14) . . ? C2 C1 C2 120.8(4) 2_556 . ? C2 C1 Dy1 71.21(15) 2_556 . ? C2 C1 Dy1 75.94(16) . . ? C2 C1 Dy1 75.94(16) 2_556 2_556 ? C2 C1 Dy1 71.21(15) . 2_556 ? Dy1 C1 Dy1 110.22(15) . 2_556 ? C2 C1 H1A 119.6 2_556 . ? C2 C1 H1A 119.6 . . ? Dy1 C1 H1A 124.9 . . ? Dy1 C1 H1A 124.9 2_556 . ? C1 C2 C3 120.1(3) . . ? C1 C2 Dy1 76.07(14) . 2_556 ? C3 C2 Dy1 77.67(16) . 2_556 ? C1 C2 Dy1 72.06(13) . . ? C3 C2 Dy1 68.70(14) . . ? Dy1 C2 Dy1 110.61(11) 2_556 . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? Dy1 C2 H2A 117.1 2_556 . ? Dy1 C2 H2A 132.3 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 Dy1 77.81(15) . . ? C4 C3 Dy1 75.83(13) . . ? C2 C3 Dy1 68.92(15) . 2_556 ? C4 C3 Dy1 71.56(13) . 2_556 ? Dy1 C3 Dy1 110.77(10) . 2_556 ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? Dy1 C3 H3A 117.0 . . ? Dy1 C3 H3A 132.3 2_556 . ? C5 C4 C3 121.18(17) . 2_556 ? C5 C4 C3 121.18(17) . . ? C3 C4 C3 117.6(3) 2_556 . ? C5 C4 Dy1 125.04(7) . 2_556 ? C3 C4 Dy1 70.14(14) 2_556 2_556 ? C3 C4 Dy1 75.24(15) . 2_556 ? C5 C4 Dy1 125.04(7) . . ? C3 C4 Dy1 75.24(15) 2_556 . ? C3 C4 Dy1 70.14(14) . . ? Dy1 C4 Dy1 109.91(14) 2_556 . ? C4 C5 C6 122.56(19) . 2_556 ? C4 C5 C6 122.56(19) . . ? C6 C5 C6 114.9(4) 2_556 . ? C4 C5 K1 115.90(7) . . ? C6 C5 K1 75.07(15) 2_556 . ? C6 C5 K1 77.73(15) . . ? C4 C5 K1 115.90(7) . 2_556 ? C6 C5 K1 77.73(15) 2_556 2_556 ? C6 C5 K1 75.07(14) . 2_556 ? K1 C5 K1 128.20(13) . 2_556 ? C7 C6 C5 121.7(3) . . ? C7 C6 K1 79.0(2) . 2_556 ? C5 C6 K1 77.88(14) . 2_556 ? C7 C6 K1 78.8(2) . . ? C5 C6 K1 75.51(14) . . ? K1 C6 K1 128.49(12) 2_556 . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? K1 C6 H6A 114.3 2_556 . ? K1 C6 H6A 117.1 . . ? C6 C7 C8 122.0(4) . . ? C6 C7 K1 75.11(19) . 2_556 ? C8 C7 K1 79.96(17) . 2_556 ? C6 C7 K1 75.74(19) . . ? C8 C7 K1 77.84(18) . . ? K1 C7 K1 125.32(12) 2_556 . ? C6 C7 H7A 119.0 . . ? C8 C7 H7A 119.0 . . ? K1 C7 H7A 116.4 2_556 . ? K1 C7 H7A 118.1 . . ? C7 C8 C7 117.7(5) 2_556 . ? C7 C8 K1 76.75(19) 2_556 2_556 ? C7 C8 K1 74.43(18) . 2_556 ? C7 C8 K1 74.43(18) 2_556 . ? C7 C8 K1 76.75(19) . . ? K1 C8 K1 122.50(17) 2_556 . ? C7 C8 H8A 121.1 2_556 . ? C7 C8 H8A 121.1 . . ? K1 C8 H8A 118.7 2_556 . ? K1 C8 H8A 118.7 . . ? N1 C9 C13 131.0(3) . . ? N1 C9 C10 124.2(3) . . ? C13 C9 C10 104.8(3) . . ? N1 C9 Fe1 129.6(2) . . ? C13 C9 Fe1 66.70(19) . . ? C10 C9 Fe1 67.08(19) . . ? N1 C9 Dy1 56.45(17) . . ? C13 C9 Dy1 136.1(2) . . ? C10 C9 Dy1 85.0(2) . . ? Fe1 C9 Dy1 79.05(10) . . ? N1 C9 K1 66.76(18) . . ? C13 C9 K1 130.4(2) . . ? C10 C9 K1 78.55(19) . . ? Fe1 C9 K1 145.23(15) . . ? Dy1 C9 K1 93.35(10) . . ? C11 C10 C9 109.6(3) . . ? C11 C10 Fe1 68.6(2) . . ? C9 C10 Fe1 72.4(2) . . ? C11 C10 K1 129.2(2) . . ? C9 C10 K1 74.43(19) . . ? Fe1 C10 K1 146.40(16) . . ? C11 C10 H10A 125.2 . . ? C9 C10 H10A 125.2 . . ? Fe1 C10 H10A 125.4 . . ? K1 C10 H10A 71.6 . . ? C12 C11 C10 107.6(3) . . ? C12 C11 Fe1 69.6(2) . . ? C10 C11 Fe1 70.7(2) . . ? C12 C11 H11A 126.2 . . ? C10 C11 H11A 126.2 . . ? Fe1 C11 H11A 125.0 . . ? C11 C12 C13 108.5(3) . . ? C11 C12 Fe1 69.6(2) . . ? C13 C12 Fe1 70.2(2) . . ? C11 C12 H12A 125.8 . . ? C13 C12 H12A 125.8 . . ? Fe1 C12 H12A 126.0 . . ? C12 C13 C9 109.5(3) . . ? C12 C13 Fe1 69.04(19) . . ? C9 C13 Fe1 73.00(19) . . ? C12 C13 H13A 125.3 . . ? C9 C13 H13A 125.3 . . ? Fe1 C13 H13A 124.3 . . ? N2 C14 C18 129.4(3) . . ? N2 C14 C15 125.2(2) . . ? C18 C14 C15 105.3(3) . . ? N2 C14 Fe1 127.4(2) . . ? C18 C14 Fe1 66.63(16) . . ? C15 C14 Fe1 67.52(16) . . ? N2 C14 Dy1 53.82(14) . . ? C18 C14 Dy1 135.0(2) . . ? C15 C14 Dy1 87.20(17) . . ? Fe1 C14 Dy1 79.76(9) . . ? C16 C15 C14 109.3(3) . . ? C16 C15 Fe1 68.62(18) . . ? C14 C15 Fe1 72.24(16) . . ? C16 C15 H15A 125.3 . . ? C14 C15 H15A 125.3 . . ? Fe1 C15 H15A 125.4 . . ? C17 C16 C15 107.6(3) . . ? C17 C16 Fe1 69.45(19) . . ? C15 C16 Fe1 70.79(18) . . ? C17 C16 H16A 126.2 . . ? C15 C16 H16A 126.2 . . ? Fe1 C16 H16A 125.1 . . ? C16 C17 C18 108.2(3) . . ? C16 C17 Fe1 69.84(18) . . ? C18 C17 Fe1 70.02(18) . . ? C16 C17 H17A 125.9 . . ? C18 C17 H17A 125.9 . . ? Fe1 C17 H17A 125.8 . . ? C17 C18 C14 109.4(3) . . ? C17 C18 Fe1 69.26(18) . . ? C14 C18 Fe1 73.19(16) . . ? C17 C18 H18A 125.3 . . ? C14 C18 H18A 125.3 . . ? Fe1 C18 H18A 123.8 . . ? Si1A C19 Si1 25.53(8) . . ? Si1A C19 H19A 133.0 . . ? Si1 C19 H19A 109.5 . . ? Si1A C19 H19B 103.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1A C19 H19C 89.3 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 Si1A 49.3(3) . . ? C21 C20 H20A 109.5 . . ? Si1A C20 H20A 84.8 . . ? C21 C20 H20B 109.5 . . ? Si1A C20 H20B 158.4 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? Si1A C20 H20C 79.2 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21A C22 Si1 50.9(3) . . ? C21A C22 H22A 93.6 . . ? Si1 C22 H22A 109.5 . . ? C21A C22 H22B 154.8 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21A C22 H22C 70.3 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 109.1(3) . . ? C29 C27 C30 108.5(3) . . ? C28 C27 C30 108.4(3) . . ? C29 C27 Si2 110.1(2) . . ? C28 C27 Si2 110.2(2) . . ? C30 C27 Si2 110.5(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 123.9(6) . . ? C37 C32 C31 114.7(7) . . ? C33 C32 C31 121.3(7) . . ? C37 C32 K1 76.8(3) . . ? C33 C32 K1 75.1(3) . . ? C31 C32 K1 120.9(3) . . ? C32 C33 C34 118.3(5) . . ? C32 C33 K1 81.5(3) . . ? C34 C33 K1 72.4(2) . . ? C32 C33 H33A 120.7 . . ? C34 C33 H33A 120.7 . . ? K1 C33 H33A 120.7 . . ? C33 C34 C35 112.4(5) . . ? C33 C34 K1 81.3(3) . . ? C35 C34 K1 76.2(3) . . ? C33 C34 H34A 122.9 . . ? C35 C34 H34A 122.9 . . ? K1 C34 H34A 122.9 . . ? C36 C35 C34 118.0(6) . . ? C36 C35 K1 80.4(3) . . ? C34 C35 K1 76.7(3) . . ? C36 C35 H35A 120.7 . . ? C34 C35 H35A 120.7 . . ? K1 C35 H35A 120.7 . . ? C37 C36 C35 126.2(7) . . ? C37 C36 K1 83.5(4) . . ? C35 C36 K1 75.5(3) . . ? C37 C36 H36A 116.9 . . ? C35 C36 H36A 116.9 . . ? K1 C36 H36A 116.9 . . ? C36 C37 C32 121.0(7) . . ? C36 C37 K1 74.9(4) . . ? C32 C37 K1 81.0(3) . . ? C36 C37 H37A 119.4 . . ? C32 C37 H37A 119.4 . . ? K1 C37 H37A 119.4 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C7S C2S C3S 118.4(4) . . ? C7S C2S C1S 120.7(4) . . ? C3S C2S C1S 120.9(4) . . ? C4S C3S C2S 120.6(4) . . ? C4S C3S H3SA 119.7 . . ? C2S C3S H3SA 119.7 . . ? C3S C4S C5S 120.4(4) . . ? C3S C4S H4SA 119.8 . . ? C5S C4S H4SA 119.8 . . ? C6S C5S C4S 119.6(4) . . ? C6S C5S H5SA 120.2 . . ? C4S C5S H5SA 120.2 . . ? C5S C6S C7S 120.1(4) . . ? C5S C6S H6SA 120.0 . . ? C7S C6S H6SA 120.0 . . ? C2S C7S C6S 121.0(4) . . ? C2S C7S H7SA 119.5 . . ? C6S C7S H7SA 119.5 . . ? N1 Si1 C21 105.3(2) . . ? N1 Si1 C19 108.59(18) . . ? C21 Si1 C19 106.5(2) . . ? N1 Si1 C22 119.73(17) . . ? C21 Si1 C22 102.2(2) . . ? C19 Si1 C22 113.15(18) . . ? N1 Si1 K1 41.27(10) . . ? C21 Si1 K1 95.6(2) . . ? C19 Si1 K1 73.44(13) . . ? C22 Si1 K1 157.83(13) . . ? C24 C21 C23 107.3(5) . . ? C24 C21 C20 113.6(5) . . ? C23 C21 C20 111.1(4) . . ? C24 C21 Si1 111.0(4) . . ? C23 C21 Si1 109.0(4) . . ? C20 C21 Si1 104.8(4) . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 Si1A C19 109.94(18) . . ? N1 Si1A C21A 112.1(3) . . ? C19 Si1A C21A 103.8(3) . . ? N1 Si1A C20 113.22(17) . . ? C19 Si1A C20 118.18(18) . . ? C21A Si1A C20 98.7(3) . . ? N1 Si1A K1 57.26(11) . . ? C19 Si1A K1 88.79(14) . . ? C21A Si1A K1 166.3(2) . . ? C20 Si1A K1 79.80(12) . . ? C24A C21A C23A 109.3(7) . . ? C24A C21A C22 114.1(6) . . ? C23A C21A C22 113.7(6) . . ? C24A C21A Si1A 110.5(6) . . ? C23A C21A Si1A 109.5(5) . . ? C22 C21A Si1A 99.4(5) . . ? C21A C23A H23D 109.5 . . ? C21A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C21A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C21A C24A H24D 109.5 . . ? C21A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C21A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.047 _refine_diff_density_min -3.631 _refine_diff_density_rms 0.121 #===END data_Gd2-biph _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H118 Fe2 Gd2 K2 N4 Si4' _chemical_formula_weight 1800.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.349(4) _cell_length_b 21.880(6) _cell_length_c 26.449(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.136(3) _cell_angle_gamma 90.00 _cell_volume 8270(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 2.130 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4279 _exptl_absorpt_correction_T_max 0.5869 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57329 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 30.81 _reflns_number_total 12214 _reflns_number_gt 10867 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2, 2013' _computing_cell_refinement 'SAINT V8.32B (Bruker AXS Inc., 2013' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013' _computing_structure_solution 'SHELXS-2013 (Sheldrick 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+23.0634P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12214 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.585105(6) 0.655680(4) 0.820430(3) 0.01444(3) Uani 1 1 d . . . Fe1 Fe 0.57233(2) 0.641625(13) 0.940233(11) 0.01940(6) Uani 1 1 d . D . K1 K 0.63853(4) 0.46194(2) 0.831476(19) 0.03272(11) Uani 1 1 d . . . Si2 Si 0.66938(4) 0.81657(2) 0.85353(2) 0.01844(10) Uani 1 1 d . D . N1 N 0.69680(11) 0.58228(8) 0.85808(7) 0.0214(3) Uani 1 1 d . . . N2 N 0.62392(11) 0.74609(7) 0.86348(6) 0.0182(3) Uani 1 1 d . . . C1 C 0.5000 0.72260(12) 0.7500 0.0214(5) Uani 1 2 d S . . H1A H 0.5000 0.7660 0.7500 0.026 Uiso 1 2 calc SR D . C2 C 0.42640(14) 0.69041(9) 0.77113(8) 0.0206(4) Uani 1 1 d . . . H2A H 0.3748 0.7123 0.7823 0.025 Uiso 1 1 calc R . . C3 C 0.42993(13) 0.62349(9) 0.77579(7) 0.0165(3) Uani 1 1 d . . . H3A H 0.3873 0.6028 0.7953 0.020 Uiso 1 1 calc R D . C4 C 0.5000 0.58840(11) 0.7500 0.0141(4) Uani 1 2 d S . . C5 C 0.5000 0.52385(12) 0.7500 0.0179(5) Uani 1 2 d S . . C6 C 0.43769(16) 0.48832(10) 0.77833(8) 0.0252(4) Uani 1 1 d . . . H6A H 0.3945 0.5088 0.7976 0.030 Uiso 1 1 calc R . . C7 C 0.4394(2) 0.42484(11) 0.77803(10) 0.0396(6) Uani 1 1 d . . . H7A H 0.3978 0.4032 0.7976 0.048 Uiso 1 1 calc R D . C8 C 0.5000 0.39175(15) 0.7500 0.0472(11) Uani 1 2 d S . . H8A H 0.5000 0.3483 0.7500 0.057 Uiso 1 2 calc SR . . C9 C 0.65087(14) 0.57588(9) 0.90190(8) 0.0194(4) Uani 1 1 d . D . C10 C 0.68399(17) 0.58362(10) 0.95443(9) 0.0274(5) Uani 1 1 d . . . H10A H 0.7451 0.5965 0.9667 0.033 Uiso 1 1 calc R D . C11 C 0.6107(2) 0.56886(10) 0.98523(9) 0.0340(5) Uani 1 1 d . D . H11A H 0.6155 0.5686 1.0213 0.041 Uiso 1 1 calc R . . C12 C 0.52922(18) 0.55470(10) 0.95307(9) 0.0283(5) Uani 1 1 d . . . H12A H 0.4699 0.5438 0.9636 0.034 Uiso 1 1 calc R D . C13 C 0.55259(14) 0.55970(9) 0.90199(8) 0.0201(4) Uani 1 1 d . D . H13A H 0.5106 0.5534 0.8726 0.024 Uiso 1 1 calc R . . C14 C 0.58322(14) 0.73074(8) 0.90755(8) 0.0192(4) Uani 1 1 d . D . C15 C 0.62518(16) 0.72667(9) 0.95887(8) 0.0236(4) Uani 1 1 d . . . H15A H 0.6892 0.7342 0.9694 0.028 Uiso 1 1 calc R D . C16 C 0.55587(17) 0.70957(10) 0.99134(8) 0.0268(4) Uani 1 1 d . D . H16A H 0.5650 0.7058 1.0272 0.032 Uiso 1 1 calc R . . C17 C 0.47030(16) 0.69909(10) 0.96090(8) 0.0250(4) Uani 1 1 d . . . H17A H 0.4127 0.6864 0.9726 0.030 Uiso 1 1 calc R D . C18 C 0.48722(14) 0.71126(9) 0.90962(8) 0.0202(4) Uani 1 1 d . D . H18A H 0.4424 0.7072 0.8811 0.024 Uiso 1 1 calc R . . C19 C 0.6395(4) 0.31104(16) 0.85899(14) 0.0710(9) Uani 1 1 d . . . C20 C 0.5651(2) 0.33414(14) 0.88121(12) 0.0461(7) Uani 1 1 d . D . H20A H 0.5032 0.3220 0.8700 0.055 Uiso 1 1 calc R . . C21 C 0.5819(4) 0.37728(19) 0.92199(16) 0.0835(17) Uani 1 1 d . . . H21A H 0.5328 0.3955 0.9386 0.100 Uiso 1 1 calc R D . C22 C 0.6820(4) 0.39106(18) 0.93606(12) 0.0814(16) Uani 1 1 d . D . H22A H 0.7009 0.4177 0.9635 0.098 Uiso 1 1 calc R . . C23 C 0.7454(3) 0.3642(2) 0.90838(18) 0.0718(12) Uani 1 1 d . . . H23A H 0.8095 0.3737 0.9169 0.086 Uiso 1 1 calc R D . C24 C 0.7260(3) 0.3277(2) 0.8721(2) 0.0707(12) Uani 1 1 d . D . H24A H 0.7750 0.3118 0.8541 0.085 Uiso 1 1 calc R . . C25 C 0.6200(4) 0.26347(15) 0.81697(13) 0.0710(9) Uani 1 1 d . D . H25A H 0.6532 0.2255 0.8267 0.107 Uiso 1 1 calc R . . H25B H 0.6416 0.2790 0.7853 0.107 Uiso 1 1 calc R . . H25C H 0.5526 0.2554 0.8120 0.107 Uiso 1 1 calc R . . C26 C 0.77914(16) 0.83464(11) 0.89552(10) 0.0311(5) Uani 1 1 d . . . H26A H 0.8291 0.8066 0.8877 0.047 Uiso 1 1 calc R D . H26B H 0.7670 0.8300 0.9312 0.047 Uiso 1 1 calc R . . H26C H 0.7984 0.8768 0.8894 0.047 Uiso 1 1 calc R . . C27 C 0.70266(16) 0.82046(10) 0.78670(9) 0.0275(4) Uani 1 1 d . . . H27A H 0.7438 0.7860 0.7804 0.041 Uiso 1 1 calc R D . H27B H 0.7355 0.8590 0.7817 0.041 Uiso 1 1 calc R . . H27C H 0.6461 0.8184 0.7631 0.041 Uiso 1 1 calc R . . C28 C 0.58260(15) 0.88062(9) 0.86338(9) 0.0243(4) Uani 1 1 d . . . C29 C 0.5728(2) 0.88877(12) 0.92008(10) 0.0399(6) Uani 1 1 d . D . H29A H 0.5280 0.9216 0.9249 0.060 Uiso 1 1 calc R . . H29B H 0.6337 0.8993 0.9376 0.060 Uiso 1 1 calc R . . H29C H 0.5502 0.8506 0.9341 0.060 Uiso 1 1 calc R . . C30 C 0.6168(2) 0.94105(10) 0.84233(10) 0.0356(5) Uani 1 1 d . D . H30A H 0.5743 0.9741 0.8502 0.053 Uiso 1 1 calc R . . H30B H 0.6180 0.9378 0.8054 0.053 Uiso 1 1 calc R . . H30C H 0.6799 0.9500 0.8578 0.053 Uiso 1 1 calc R . . C31 C 0.48670(18) 0.86515(12) 0.83616(13) 0.0430(7) Uani 1 1 d . D . H31A H 0.4419 0.8973 0.8428 0.064 Uiso 1 1 calc R . . H31B H 0.4650 0.8260 0.8487 0.064 Uiso 1 1 calc R . . H31C H 0.4919 0.8623 0.7995 0.064 Uiso 1 1 calc R . . C32 C 0.87004(17) 0.52150(12) 0.90424(10) 0.0334(5) Uani 1 1 d . . . H32A H 0.8229 0.5020 0.9235 0.050 Uiso 1 1 calc R A 1 H32B H 0.9242 0.5331 0.9274 0.050 Uiso 1 1 calc R A 1 H32C H 0.8898 0.4928 0.8788 0.050 Uiso 1 1 calc R A 1 C33 C 0.8291(2) 0.53661(18) 0.77893(15) 0.0628(9) Uani 1 1 d . . . H33A H 0.8818 0.5084 0.7771 0.094 Uiso 1 1 calc R B 1 H33B H 0.8018 0.5460 0.7445 0.094 Uiso 1 1 calc R B 1 H33C H 0.7815 0.5176 0.7982 0.094 Uiso 1 1 calc R B 1 C35 C 0.8643(3) 0.66869(16) 0.90331(16) 0.0672(12) Uani 1 1 d . . . H35A H 0.9115 0.6588 0.9312 0.101 Uiso 1 1 calc R C 1 H35B H 0.8124 0.6908 0.9166 0.101 Uiso 1 1 calc R C 1 H35C H 0.8926 0.6943 0.8784 0.101 Uiso 1 1 calc R C 1 C1S C 0.77706(17) 0.39886(13) 0.07874(10) 0.0350(5) Uani 1 1 d . . . C2S C 0.78007(19) 0.33560(13) 0.07373(11) 0.0375(6) Uani 1 1 d . . . H2SA H 0.7384 0.3110 0.0909 0.045 Uiso 1 1 calc R . . C3S C 0.8429(2) 0.30782(13) 0.04403(11) 0.0398(6) Uani 1 1 d . . . H3SA H 0.8435 0.2646 0.0408 0.048 Uiso 1 1 calc R . . C4S C 0.9044(2) 0.34269(13) 0.01923(11) 0.0391(6) Uani 1 1 d . . . H4SA H 0.9482 0.3237 -0.0006 0.047 Uiso 1 1 calc R . . C5S C 0.90161(19) 0.40632(14) 0.02355(10) 0.0393(6) Uani 1 1 d . . . H5SA H 0.9436 0.4307 0.0064 0.047 Uiso 1 1 calc R . . C6S C 0.83823(19) 0.43396(13) 0.05264(10) 0.0374(6) Uani 1 1 d . . . H6SA H 0.8363 0.4773 0.0549 0.045 Uiso 1 1 calc R . . C7S C 0.7106(2) 0.42845(16) 0.11217(13) 0.0500(8) Uani 1 1 d . . . H7SA H 0.6540 0.4034 0.1125 0.075 Uiso 1 1 calc R . . H7SB H 0.6937 0.4692 0.0990 0.075 Uiso 1 1 calc R . . H7SC H 0.7408 0.4320 0.1468 0.075 Uiso 1 1 calc R . . Si1 Si 0.81751(7) 0.59330(6) 0.87076(5) 0.0229(4) Uani 0.567(3) 1 d P D 1 C34 C 0.8655(4) 0.5989(3) 0.8068(3) 0.0628(9) Uani 0.567(3) 1 d P D 1 C36 C 0.9741(3) 0.6005(3) 0.8148(3) 0.0458(14) Uani 0.567(3) 1 d P D 1 H36A H 0.9998 0.6033 0.7818 0.069 Uiso 0.567(3) 1 calc PR D 1 H36B H 0.9969 0.5630 0.8321 0.069 Uiso 0.567(3) 1 calc PR D 1 H36C H 0.9941 0.6360 0.8356 0.069 Uiso 0.567(3) 1 calc PR D 1 C37 C 0.8333(4) 0.6580(2) 0.7799(2) 0.0355(11) Uani 0.567(3) 1 d P D 1 H37A H 0.8588 0.6601 0.7468 0.053 Uiso 0.567(3) 1 calc PR D 1 H37B H 0.8557 0.6931 0.8006 0.053 Uiso 0.567(3) 1 calc PR D 1 H37C H 0.7648 0.6588 0.7751 0.053 Uiso 0.567(3) 1 calc PR D 1 Si1A Si 0.81298(9) 0.56561(7) 0.84951(6) 0.0178(4) Uani 0.433(3) 1 d P D 2 C34A C 0.8866(3) 0.6376(2) 0.8481(2) 0.0251(10) Uani 0.433(3) 1 d P D 2 C36A C 0.9912(4) 0.6210(3) 0.8461(2) 0.0315(12) Uani 0.433(3) 1 d P D 2 H36D H 1.0283 0.6586 0.8454 0.047 Uiso 0.433(3) 1 calc PR D 2 H36E H 0.9989 0.5969 0.8156 0.047 Uiso 0.433(3) 1 calc PR D 2 H36F H 1.0127 0.5971 0.8763 0.047 Uiso 0.433(3) 1 calc PR D 2 C37A C 0.8556(5) 0.6776(4) 0.8018(3) 0.0393(16) Uani 0.433(3) 1 d P D 2 H37D H 0.8949 0.7142 0.8021 0.059 Uiso 0.433(3) 1 calc PR D 2 H37E H 0.7901 0.6896 0.8032 0.059 Uiso 0.433(3) 1 calc PR D 2 H37F H 0.8620 0.6544 0.7706 0.059 Uiso 0.433(3) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01601(4) 0.01267(4) 0.01381(5) 0.00019(3) -0.00329(3) 0.00016(3) Fe1 0.02901(15) 0.01479(12) 0.01350(13) 0.00014(10) -0.00315(10) 0.00086(10) K1 0.0517(3) 0.0222(2) 0.0226(2) 0.00047(17) -0.0056(2) 0.0120(2) Si2 0.0178(2) 0.0141(2) 0.0230(3) -0.00188(19) -0.00068(19) -0.00106(18) N1 0.0167(7) 0.0221(8) 0.0251(9) 0.0062(7) -0.0003(6) 0.0032(6) N2 0.0204(7) 0.0140(7) 0.0194(8) -0.0007(6) -0.0030(6) -0.0009(6) C1 0.0307(14) 0.0126(11) 0.0185(13) 0.000 -0.0107(11) 0.000 C2 0.0220(9) 0.0188(9) 0.0196(9) -0.0040(7) -0.0054(7) 0.0066(7) C3 0.0162(8) 0.0177(8) 0.0154(8) 0.0004(6) 0.0011(6) 0.0020(6) C4 0.0148(11) 0.0141(11) 0.0130(11) 0.000 -0.0011(8) 0.000 C5 0.0235(12) 0.0152(11) 0.0139(12) 0.000 -0.0041(9) 0.000 C6 0.0325(11) 0.0213(10) 0.0204(10) 0.0033(8) -0.0052(8) -0.0091(8) C7 0.0641(17) 0.0232(11) 0.0281(12) 0.0089(9) -0.0151(12) -0.0189(11) C8 0.089(3) 0.0131(14) 0.035(2) 0.000 -0.021(2) 0.000 C9 0.0231(9) 0.0140(8) 0.0199(9) 0.0010(7) -0.0053(7) 0.0022(7) C10 0.0376(12) 0.0173(9) 0.0245(11) 0.0003(8) -0.0131(9) 0.0058(8) C11 0.0648(17) 0.0195(10) 0.0168(10) 0.0036(8) -0.0008(10) 0.0080(10) C12 0.0445(13) 0.0175(9) 0.0243(11) 0.0037(8) 0.0104(9) -0.0003(9) C13 0.0251(9) 0.0159(8) 0.0190(9) -0.0010(7) 0.0009(7) -0.0030(7) C14 0.0242(9) 0.0128(8) 0.0193(9) -0.0023(7) -0.0044(7) 0.0013(7) C15 0.0316(10) 0.0172(9) 0.0202(10) -0.0040(7) -0.0085(8) 0.0024(8) C16 0.0436(12) 0.0201(9) 0.0156(10) -0.0032(7) -0.0031(8) 0.0037(9) C17 0.0326(11) 0.0230(10) 0.0192(10) -0.0006(8) 0.0020(8) 0.0027(8) C18 0.0250(9) 0.0176(8) 0.0174(9) -0.0005(7) -0.0017(7) 0.0017(7) C19 0.135(3) 0.0375(12) 0.0451(14) 0.0145(10) 0.0312(16) 0.0263(15) C20 0.0426(15) 0.0451(16) 0.0502(18) 0.0217(13) 0.0019(13) 0.0006(12) C21 0.129(4) 0.067(2) 0.066(3) 0.039(2) 0.074(3) 0.049(3) C22 0.167(5) 0.055(2) 0.0174(14) 0.0119(13) -0.018(2) -0.037(3) C23 0.059(2) 0.090(3) 0.064(3) 0.044(2) -0.006(2) 0.009(2) C24 0.054(2) 0.059(2) 0.100(4) 0.042(2) 0.016(2) 0.0151(18) C25 0.135(3) 0.0375(12) 0.0451(14) 0.0145(10) 0.0312(16) 0.0263(15) C26 0.0250(10) 0.0279(11) 0.0388(13) -0.0053(9) -0.0062(9) -0.0056(8) C27 0.0301(11) 0.0243(10) 0.0288(11) -0.0038(8) 0.0058(9) -0.0035(8) C28 0.0292(10) 0.0159(9) 0.0280(11) 0.0004(8) 0.0040(8) 0.0029(7) C29 0.0583(17) 0.0279(12) 0.0363(14) 0.0038(10) 0.0199(12) 0.0154(11) C30 0.0534(15) 0.0177(10) 0.0370(14) 0.0042(9) 0.0110(11) 0.0039(10) C31 0.0298(12) 0.0274(12) 0.070(2) -0.0045(12) -0.0072(12) 0.0121(10) C32 0.0260(11) 0.0330(12) 0.0402(14) 0.0070(10) -0.0025(9) 0.0109(9) C33 0.0376(13) 0.082(2) 0.068(2) -0.0454(17) -0.0029(13) 0.0161(14) C35 0.063(2) 0.0474(18) 0.083(3) -0.0405(18) -0.0376(19) 0.0291(16) C1S 0.0284(11) 0.0428(14) 0.0347(13) -0.0038(11) 0.0071(10) -0.0034(10) C2S 0.0329(12) 0.0396(14) 0.0401(15) 0.0085(11) 0.0042(10) -0.0046(10) C3S 0.0434(14) 0.0344(13) 0.0411(15) 0.0057(11) 0.0001(11) 0.0057(11) C4S 0.0372(13) 0.0477(16) 0.0329(14) -0.0012(11) 0.0060(10) 0.0069(11) C5S 0.0381(13) 0.0487(16) 0.0326(13) -0.0049(11) 0.0115(11) -0.0106(12) C6S 0.0403(13) 0.0357(13) 0.0373(14) -0.0060(11) 0.0103(11) -0.0091(11) C7S 0.0387(15) 0.0594(19) 0.0548(19) -0.0110(15) 0.0207(13) -0.0061(13) Si1 0.0166(5) 0.0202(6) 0.0309(7) 0.0007(5) -0.0030(4) 0.0037(4) C34 0.0376(13) 0.082(2) 0.068(2) -0.0454(17) -0.0029(13) 0.0161(14) C36 0.021(2) 0.048(3) 0.069(4) 0.016(3) 0.010(2) 0.0081(19) C37 0.025(2) 0.035(3) 0.047(3) 0.012(2) 0.007(2) 0.0026(19) Si1A 0.0166(6) 0.0180(8) 0.0182(7) -0.0068(6) -0.0010(4) 0.0059(4) C34A 0.019(2) 0.026(2) 0.031(3) 0.005(2) 0.0054(18) 0.0054(17) C36A 0.017(2) 0.046(3) 0.031(3) 0.001(3) 0.003(2) 0.006(2) C37A 0.027(3) 0.040(4) 0.051(5) 0.020(3) 0.004(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N2 2.3252(17) . ? Gd1 N1 2.4194(17) . ? Gd1 C3 2.5253(19) . ? Gd1 C2 2.529(2) 2_656 ? Gd1 C1 2.5880(16) . ? Gd1 C4 2.5924(15) . ? Gd1 C3 2.631(2) 2_656 ? Gd1 C2 2.633(2) . ? Gd1 C14 2.832(2) . ? Gd1 C9 2.867(2) . ? Gd1 Fe1 3.2050(9) . ? Gd1 K1 4.3129(13) . ? Fe1 C11 2.034(2) . ? Fe1 C16 2.037(2) . ? Fe1 C12 2.038(2) . ? Fe1 C17 2.041(2) . ? Fe1 C10 2.052(2) . ? Fe1 C15 2.053(2) . ? Fe1 C13 2.065(2) . ? Fe1 C18 2.072(2) . ? Fe1 C9 2.138(2) . ? Fe1 C14 2.144(2) . ? K1 N1 2.832(2) . ? K1 C6 3.065(2) 2_656 ? K1 C9 3.107(2) . ? K1 C5 3.1084(14) . ? K1 C7 3.117(3) 2_656 ? K1 C6 3.145(2) . ? K1 C13 3.160(2) . ? K1 C7 3.178(3) . ? K1 C22 3.184(3) . ? K1 C21 3.189(3) . ? K1 C8 3.1916(18) . ? K1 C23 3.240(4) . ? Si2 N2 1.7039(18) . ? Si2 C27 1.874(2) . ? Si2 C26 1.886(2) . ? Si2 C28 1.908(2) . ? N1 C9 1.391(3) . ? N1 Si1A 1.741(2) . ? N1 Si1 1.751(2) . ? N2 C14 1.391(3) . ? C1 C2 1.425(3) . ? C1 C2 1.425(3) 2_656 ? C1 Gd1 2.5880(16) 2_656 ? C1 H1A 0.9500 . ? C2 C3 1.470(3) . ? C2 Gd1 2.529(2) 2_656 ? C2 H2A 0.9500 . ? C3 C4 1.479(2) . ? C3 Gd1 2.631(2) 2_656 ? C3 H3A 0.9500 . ? C4 C5 1.413(4) . ? C4 C3 1.479(2) 2_656 ? C4 Gd1 2.5924(15) 2_656 ? C5 C6 1.444(3) . ? C5 C6 1.444(3) 2_656 ? C5 K1 3.1084(14) 2_656 ? C6 C7 1.389(3) . ? C6 K1 3.065(2) 2_656 ? C6 H6A 0.9500 . ? C7 C8 1.395(4) . ? C7 K1 3.117(3) 2_656 ? C7 H7A 0.9500 . ? C8 C7 1.395(4) 2_656 ? C8 K1 3.1916(18) 2_656 ? C8 H8A 0.9500 . ? C9 C10 1.438(3) . ? C9 C13 1.454(3) . ? C10 C11 1.424(4) . ? C10 H10A 0.9500 . ? C11 C12 1.417(4) . ? C11 H11A 0.9500 . ? C12 C13 1.425(3) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.438(3) . ? C14 C18 1.448(3) . ? C15 C16 1.421(3) . ? C15 H15A 0.9500 . ? C16 C17 1.425(3) . ? C16 H16A 0.9500 . ? C17 C18 1.424(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.310(6) . ? C19 C20 1.361(5) . ? C19 C25 1.530(5) . ? C20 C21 1.437(6) . ? C20 H20A 0.9500 . ? C21 C22 1.482(7) . ? C21 H21A 0.9500 . ? C22 C23 1.351(7) . ? C22 H22A 0.9500 . ? C23 C24 1.261(7) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.529(3) . ? C28 C30 1.532(3) . ? C28 C31 1.533(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 Si1A 1.867(3) . ? C32 Si1 1.924(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.614(7) . ? C33 Si1A 2.004(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C35 C34A 1.668(6) . ? C35 Si1 1.952(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C1S C2S 1.392(4) . ? C1S C6S 1.395(4) . ? C1S C7S 1.504(4) . ? C2S C3S 1.388(4) . ? C2S H2SA 0.9500 . ? C3S C4S 1.376(4) . ? C3S H3SA 0.9500 . ? C4S C5S 1.398(4) . ? C4S H4SA 0.9500 . ? C5S C6S 1.382(4) . ? C5S H5SA 0.9500 . ? C6S H6SA 0.9500 . ? C7S H7SA 0.9800 . ? C7S H7SB 0.9800 . ? C7S H7SC 0.9800 . ? Si1 C34 1.886(7) . ? C34 C37 1.529(9) . ? C34 C36 1.554(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? Si1A C34A 1.899(6) . ? C34A C37A 1.537(9) . ? C34A C36A 1.550(7) . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 0.9800 . ? C37A H37D 0.9800 . ? C37A H37E 0.9800 . ? C37A H37F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Gd1 N1 104.03(6) . . ? N2 Gd1 C3 128.96(6) . . ? N1 Gd1 C3 122.08(6) . . ? N2 Gd1 C2 101.86(6) . 2_656 ? N1 Gd1 C2 125.28(7) . 2_656 ? C3 Gd1 C2 69.93(6) . 2_656 ? N2 Gd1 C1 87.02(7) . . ? N1 Gd1 C1 157.56(5) . . ? C3 Gd1 C1 58.79(6) . . ? C2 Gd1 C1 32.30(5) 2_656 . ? N2 Gd1 C4 155.74(6) . . ? N1 Gd1 C4 99.84(6) . . ? C3 Gd1 C4 33.57(5) . . ? C2 Gd1 C4 59.77(6) 2_656 . ? C1 Gd1 C4 69.06(7) . . ? N2 Gd1 C3 134.17(6) . 2_656 ? N1 Gd1 C3 102.37(6) . 2_656 ? C3 Gd1 C3 58.70(7) . 2_656 ? C2 Gd1 C3 33.03(6) 2_656 2_656 ? C1 Gd1 C3 57.50(6) . 2_656 ? C4 Gd1 C3 32.89(4) . 2_656 ? N2 Gd1 C2 98.95(6) . . ? N1 Gd1 C2 155.11(6) . . ? C3 Gd1 C2 33.03(6) . . ? C2 Gd1 C2 57.29(9) 2_656 . ? C1 Gd1 C2 31.65(5) . . ? C4 Gd1 C2 58.48(6) . . ? C3 Gd1 C2 66.79(6) 2_656 . ? N2 Gd1 C14 29.24(6) . . ? N1 Gd1 C14 95.99(6) . . ? C3 Gd1 C14 118.03(6) . . ? C2 Gd1 C14 126.89(6) 2_656 . ? C1 Gd1 C14 102.67(6) . . ? C4 Gd1 C14 151.14(4) . . ? C3 Gd1 C14 159.48(6) 2_656 . ? C2 Gd1 C14 99.48(6) . . ? N2 Gd1 C9 95.84(6) . . ? N1 Gd1 C9 28.96(6) . . ? C3 Gd1 C9 113.50(6) . . ? C2 Gd1 C9 153.07(6) 2_656 . ? C1 Gd1 C9 171.10(5) . . ? C4 Gd1 C9 107.24(6) . . ? C3 Gd1 C9 123.85(6) 2_656 . ? C2 Gd1 C9 139.46(6) . . ? C14 Gd1 C9 76.59(6) . . ? N2 Gd1 Fe1 68.28(4) . . ? N1 Gd1 Fe1 67.90(4) . . ? C3 Gd1 Fe1 108.02(4) . . ? C2 Gd1 Fe1 166.11(5) 2_656 . ? C1 Gd1 Fe1 134.49(3) . . ? C4 Gd1 Fe1 126.22(3) . . ? C3 Gd1 Fe1 157.47(4) 2_656 . ? C2 Gd1 Fe1 113.19(5) . . ? C14 Gd1 Fe1 41.03(4) . . ? C9 Gd1 Fe1 40.76(4) . . ? N2 Gd1 K1 140.33(4) . . ? N1 Gd1 K1 38.05(4) . . ? C3 Gd1 K1 84.35(4) . . ? C2 Gd1 K1 110.86(5) 2_656 . ? C1 Gd1 K1 132.41(5) . . ? C4 Gd1 K1 63.90(5) . . ? C3 Gd1 K1 78.53(4) 2_656 . ? C2 Gd1 K1 117.25(4) . . ? C14 Gd1 K1 121.97(4) . . ? C9 Gd1 K1 46.04(4) . . ? Fe1 Gd1 K1 82.199(9) . . ? C11 Fe1 C16 102.97(9) . . ? C11 Fe1 C12 40.73(10) . . ? C16 Fe1 C12 121.04(9) . . ? C11 Fe1 C17 119.23(10) . . ? C16 Fe1 C17 40.91(9) . . ? C12 Fe1 C17 107.13(10) . . ? C11 Fe1 C10 40.80(10) . . ? C16 Fe1 C10 117.71(9) . . ? C12 Fe1 C10 68.65(10) . . ? C17 Fe1 C10 154.02(9) . . ? C11 Fe1 C15 119.62(10) . . ? C16 Fe1 C15 40.66(9) . . ? C12 Fe1 C15 156.51(9) . . ? C17 Fe1 C15 68.64(9) . . ? C10 Fe1 C15 104.54(9) . . ? C11 Fe1 C13 67.99(9) . . ? C16 Fe1 C13 159.95(9) . . ? C12 Fe1 C13 40.63(8) . . ? C17 Fe1 C13 126.55(9) . . ? C10 Fe1 C13 67.88(9) . . ? C15 Fe1 C13 159.38(9) . . ? C11 Fe1 C18 157.45(10) . . ? C16 Fe1 C18 67.87(9) . . ? C12 Fe1 C18 125.06(10) . . ? C17 Fe1 C18 40.51(8) . . ? C10 Fe1 C18 161.75(9) . . ? C15 Fe1 C18 67.62(8) . . ? C13 Fe1 C18 113.38(8) . . ? C11 Fe1 C9 67.94(9) . . ? C16 Fe1 C9 154.55(9) . . ? C12 Fe1 C9 68.39(9) . . ? C17 Fe1 C9 164.26(8) . . ? C10 Fe1 C9 40.06(8) . . ? C15 Fe1 C9 121.65(9) . . ? C13 Fe1 C9 40.43(8) . . ? C18 Fe1 C9 128.82(8) . . ? C11 Fe1 C14 157.23(10) . . ? C16 Fe1 C14 67.72(9) . . ? C12 Fe1 C14 161.80(9) . . ? C17 Fe1 C14 68.14(8) . . ? C10 Fe1 C14 123.53(9) . . ? C15 Fe1 C14 39.99(8) . . ? C13 Fe1 C14 127.13(8) . . ? C18 Fe1 C14 40.12(8) . . ? C9 Fe1 C14 111.11(8) . . ? C11 Fe1 Gd1 128.11(7) . . ? C16 Fe1 Gd1 127.32(7) . . ? C12 Fe1 Gd1 107.41(7) . . ? C17 Fe1 Gd1 108.15(6) . . ? C10 Fe1 Gd1 97.32(7) . . ? C15 Fe1 Gd1 95.62(6) . . ? C13 Fe1 Gd1 67.45(6) . . ? C18 Fe1 Gd1 68.10(6) . . ? C9 Fe1 Gd1 61.09(5) . . ? C14 Fe1 Gd1 60.10(5) . . ? N1 K1 C6 97.63(6) . 2_656 ? N1 K1 C9 26.57(5) . . ? C6 K1 C9 114.41(6) 2_656 . ? N1 K1 C5 85.61(6) . . ? C6 K1 C5 27.04(4) 2_656 . ? C9 K1 C5 93.70(6) . . ? N1 K1 C7 123.11(6) . 2_656 ? C6 K1 C7 25.95(6) 2_656 2_656 ? C9 K1 C7 139.67(6) . 2_656 ? C5 K1 C7 46.81(6) . 2_656 ? N1 K1 C6 100.30(5) . . ? C6 K1 C6 46.13(8) 2_656 . ? C9 K1 C6 96.98(6) . . ? C5 K1 C6 26.69(4) . . ? C7 K1 C6 52.73(7) 2_656 . ? N1 K1 C13 49.18(5) . . ? C6 K1 C13 107.87(6) 2_656 . ? C9 K1 C13 26.82(5) . . ? C5 K1 C13 81.67(5) . . ? C7 K1 C13 126.75(6) 2_656 . ? C6 K1 C13 75.47(6) . . ? N1 K1 C7 125.57(6) . . ? C6 K1 C7 52.87(7) 2_656 . ? C9 K1 C7 118.18(7) . . ? C5 K1 C7 46.31(6) . . ? C7 K1 C7 44.51(11) 2_656 . ? C6 K1 C7 25.38(6) . . ? C13 K1 C7 93.01(7) . . ? N1 K1 C22 101.92(8) . . ? C6 K1 C22 160.13(8) 2_656 . ? C9 K1 C22 82.75(9) . . ? C5 K1 C22 151.40(12) . . ? C7 K1 C22 134.94(9) 2_656 . ? C6 K1 C22 125.33(12) . . ? C13 K1 C22 82.73(11) . . ? C7 K1 C22 111.13(11) . . ? N1 K1 C21 116.29(11) . . ? C6 K1 C21 136.66(13) 2_656 . ? C9 K1 C21 91.19(10) . . ? C5 K1 C21 125.69(11) . . ? C7 K1 C21 116.87(13) 2_656 . ? C6 K1 C21 99.05(11) . . ? C13 K1 C21 79.11(8) . . ? C7 K1 C21 84.61(12) . . ? C22 K1 C21 26.90(13) . . ? N1 K1 C8 140.11(6) . . ? C6 K1 C8 45.82(6) 2_656 . ? C9 K1 C8 142.13(6) . . ? C5 K1 C8 54.59(7) . . ? C7 K1 C8 25.51(6) 2_656 . ? C6 K1 C8 45.26(6) . . ? C13 K1 C8 118.15(5) . . ? C7 K1 C8 25.30(6) . . ? C22 K1 C8 114.45(9) . . ? C21 K1 C8 92.42(12) . . ? N1 K1 C23 110.17(11) . . ? C6 K1 C23 145.86(12) 2_656 . ? C9 K1 C23 98.90(12) . . ? C5 K1 C23 163.72(11) . . ? C7 K1 C23 121.43(12) 2_656 . ? C6 K1 C23 139.89(9) . . ? C13 K1 C23 105.29(11) . . ? C7 K1 C23 117.82(10) . . ? C22 K1 C23 24.26(12) . . ? C21 K1 C23 44.24(11) . . ? C8 K1 C23 109.72(12) . . ? N2 Si2 C27 108.68(9) . . ? N2 Si2 C26 114.19(10) . . ? C27 Si2 C26 106.02(12) . . ? N2 Si2 C28 112.34(9) . . ? C27 Si2 C28 108.66(10) . . ? C26 Si2 C28 106.64(11) . . ? C9 N1 Si1A 128.18(15) . . ? C9 N1 Si1 112.87(15) . . ? Si1A N1 Si1 27.33(6) . . ? C9 N1 Gd1 93.67(11) . . ? Si1A N1 Gd1 133.80(10) . . ? Si1 N1 Gd1 126.49(10) . . ? C9 N1 K1 87.83(11) . . ? Si1A N1 K1 92.17(9) . . ? Si1 N1 K1 116.14(9) . . ? Gd1 N1 K1 110.18(7) . . ? C14 N2 Si2 122.91(13) . . ? C14 N2 Gd1 96.01(11) . . ? Si2 N2 Gd1 140.58(10) . . ? C2 C1 C2 120.7(2) . 2_656 ? C2 C1 Gd1 71.58(10) . 2_656 ? C2 C1 Gd1 75.90(11) 2_656 2_656 ? C2 C1 Gd1 75.90(11) . . ? C2 C1 Gd1 71.58(10) 2_656 . ? Gd1 C1 Gd1 111.09(10) 2_656 . ? C2 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 2_656 . ? Gd1 C1 H1A 124.5 2_656 . ? Gd1 C1 H1A 124.5 . . ? C1 C2 C3 120.28(18) . . ? C1 C2 Gd1 76.12(10) . 2_656 ? C3 C2 Gd1 77.27(11) . 2_656 ? C1 C2 Gd1 72.44(9) . . ? C3 C2 Gd1 69.47(10) . . ? Gd1 C2 Gd1 111.52(7) 2_656 . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? Gd1 C2 H2A 117.5 2_656 . ? Gd1 C2 H2A 130.9 . . ? C2 C3 C4 119.87(17) . . ? C2 C3 Gd1 77.50(11) . . ? C4 C3 Gd1 75.70(9) . . ? C2 C3 Gd1 69.70(11) . 2_656 ? C4 C3 Gd1 72.13(9) . 2_656 ? Gd1 C3 Gd1 111.72(7) . 2_656 ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? Gd1 C3 H3A 117.5 . . ? Gd1 C3 H3A 130.7 2_656 . ? C5 C4 C3 121.26(11) . 2_656 ? C5 C4 C3 121.26(11) . . ? C3 C4 C3 117.5(2) 2_656 . ? C5 C4 Gd1 124.60(5) . . ? C3 C4 Gd1 74.97(10) 2_656 . ? C3 C4 Gd1 70.73(10) . . ? C5 C4 Gd1 124.60(5) . 2_656 ? C3 C4 Gd1 70.73(10) 2_656 2_656 ? C3 C4 Gd1 74.97(10) . 2_656 ? Gd1 C4 Gd1 110.80(9) . 2_656 ? C4 C5 C6 122.57(13) . . ? C4 C5 C6 122.57(13) . 2_656 ? C6 C5 C6 114.9(3) . 2_656 ? C4 C5 K1 115.83(5) . 2_656 ? C6 C5 K1 74.81(10) . 2_656 ? C6 C5 K1 78.05(11) 2_656 2_656 ? C4 C5 K1 115.83(5) . . ? C6 C5 K1 78.05(11) . . ? C6 C5 K1 74.81(10) 2_656 . ? K1 C5 K1 128.34(9) 2_656 . ? C7 C6 C5 121.6(2) . . ? C7 C6 K1 79.12(14) . 2_656 ? C5 C6 K1 78.15(10) . 2_656 ? C7 C6 K1 78.67(15) . . ? C5 C6 K1 75.26(10) . . ? K1 C6 K1 128.61(8) 2_656 . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? K1 C6 H6A 113.8 2_656 . ? K1 C6 H6A 117.5 . . ? C6 C7 C8 122.3(3) . . ? C6 C7 K1 74.93(13) . 2_656 ? C8 C7 K1 80.23(12) . 2_656 ? C6 C7 K1 75.95(14) . . ? C8 C7 K1 77.88(13) . . ? K1 C7 K1 125.45(9) 2_656 . ? C6 C7 H7A 118.9 . . ? C8 C7 H7A 118.9 . . ? K1 C7 H7A 116.4 2_656 . ? K1 C7 H7A 117.9 . . ? C7 C8 C7 117.5(3) 2_656 . ? C7 C8 K1 74.26(13) 2_656 . ? C7 C8 K1 76.82(13) . . ? C7 C8 K1 76.82(13) 2_656 2_656 ? C7 C8 K1 74.26(13) . 2_656 ? K1 C8 K1 122.47(11) . 2_656 ? C7 C8 H8A 121.3 2_656 . ? C7 C8 H8A 121.3 . . ? K1 C8 H8A 118.8 . . ? K1 C8 H8A 118.8 2_656 . ? N1 C9 C10 130.8(2) . . ? N1 C9 C13 123.91(18) . . ? C10 C9 C13 105.30(19) . . ? N1 C9 Fe1 129.54(14) . . ? C10 C9 Fe1 66.74(12) . . ? C13 C9 Fe1 67.09(11) . . ? N1 C9 Gd1 57.38(10) . . ? C10 C9 Gd1 135.46(13) . . ? C13 C9 Gd1 84.01(11) . . ? Fe1 C9 Gd1 78.15(6) . . ? N1 C9 K1 65.61(11) . . ? C10 C9 K1 132.07(13) . . ? C13 C9 K1 78.61(11) . . ? Fe1 C9 K1 145.07(9) . . ? Gd1 C9 K1 92.34(6) . . ? C11 C10 C9 109.2(2) . . ? C11 C10 Fe1 68.92(13) . . ? C9 C10 Fe1 73.20(12) . . ? C11 C10 H10A 125.4 . . ? C9 C10 H10A 125.4 . . ? Fe1 C10 H10A 124.1 . . ? C12 C11 C10 108.5(2) . . ? C12 C11 Fe1 69.79(13) . . ? C10 C11 Fe1 70.29(12) . . ? C12 C11 H11A 125.7 . . ? C10 C11 H11A 125.7 . . ? Fe1 C11 H11A 125.8 . . ? C11 C12 C13 107.5(2) . . ? C11 C12 Fe1 69.48(13) . . ? C13 C12 Fe1 70.72(12) . . ? C11 C12 H12A 126.2 . . ? C13 C12 H12A 126.2 . . ? Fe1 C12 H12A 125.2 . . ? C12 C13 C9 109.32(19) . . ? C12 C13 Fe1 68.65(12) . . ? C9 C13 Fe1 72.48(11) . . ? C12 C13 K1 130.16(14) . . ? C9 C13 K1 74.58(11) . . ? Fe1 C13 K1 146.39(9) . . ? C12 C13 H13A 125.3 . . ? C9 C13 H13A 125.3 . . ? Fe1 C13 H13A 125.1 . . ? K1 C13 H13A 70.9 . . ? N2 C14 C15 129.38(19) . . ? N2 C14 C18 125.11(17) . . ? C15 C14 C18 105.40(18) . . ? N2 C14 Fe1 127.50(13) . . ? C15 C14 Fe1 66.58(11) . . ? C18 C14 Fe1 67.24(11) . . ? N2 C14 Gd1 54.75(9) . . ? C15 C14 Gd1 134.32(13) . . ? C18 C14 Gd1 86.48(11) . . ? Fe1 C14 Gd1 78.87(6) . . ? C16 C15 C14 109.28(19) . . ? C16 C15 Fe1 69.08(12) . . ? C14 C15 Fe1 73.43(11) . . ? C16 C15 H15A 125.4 . . ? C14 C15 H15A 125.4 . . ? Fe1 C15 H15A 123.7 . . ? C15 C16 C17 108.38(19) . . ? C15 C16 Fe1 70.26(12) . . ? C17 C16 Fe1 69.70(12) . . ? C15 C16 H16A 125.8 . . ? C17 C16 H16A 125.8 . . ? Fe1 C16 H16A 125.8 . . ? C18 C17 C16 107.2(2) . . ? C18 C17 Fe1 70.89(12) . . ? C16 C17 Fe1 69.39(13) . . ? C18 C17 H17A 126.4 . . ? C16 C17 H17A 126.4 . . ? Fe1 C17 H17A 124.9 . . ? C17 C18 C14 109.58(18) . . ? C17 C18 Fe1 68.60(12) . . ? C14 C18 Fe1 72.64(11) . . ? C17 C18 H18A 125.2 . . ? C14 C18 H18A 125.2 . . ? Fe1 C18 H18A 125.1 . . ? C24 C19 C20 122.9(4) . . ? C24 C19 C25 119.3(4) . . ? C20 C19 C25 117.8(5) . . ? C24 C19 K1 76.8(2) . . ? C20 C19 K1 75.05(18) . . ? C25 C19 K1 120.7(2) . . ? C19 C20 C21 118.9(4) . . ? C19 C20 K1 81.49(19) . . ? C21 C20 K1 72.83(18) . . ? C19 C20 H20A 120.6 . . ? C21 C20 H20A 120.6 . . ? K1 C20 H20A 115.8 . . ? C20 C21 C22 114.5(3) . . ? C20 C21 K1 81.66(17) . . ? C22 C21 K1 76.35(18) . . ? C20 C21 H21A 122.7 . . ? C22 C21 H21A 122.7 . . ? K1 C21 H21A 110.6 . . ? C23 C22 C21 117.4(4) . . ? C23 C22 K1 80.2(2) . . ? C21 C22 K1 76.75(18) . . ? C23 C22 H22A 121.3 . . ? C21 C22 H22A 121.3 . . ? K1 C22 H22A 112.6 . . ? C24 C23 C22 125.1(4) . . ? C24 C23 K1 83.2(2) . . ? C22 C23 K1 75.5(2) . . ? C24 C23 H23A 117.5 . . ? C22 C23 H23A 117.5 . . ? K1 C23 H23A 113.5 . . ? C23 C24 C19 121.2(4) . . ? C23 C24 K1 74.7(2) . . ? C19 C24 K1 80.7(2) . . ? C23 C24 H24A 119.4 . . ? C19 C24 H24A 119.4 . . ? K1 C24 H24A 115.6 . . ? C19 C25 H25A 109.5 . . ? C19 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C19 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 108.4(2) . . ? C29 C28 C31 109.2(2) . . ? C30 C28 C31 108.8(2) . . ? C29 C28 Si2 109.77(16) . . ? C30 C28 Si2 110.50(16) . . ? C31 C28 Si2 110.06(15) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1A C32 Si1 25.08(6) . . ? Si1A C32 H32A 110.6 . . ? Si1 C32 H32A 109.5 . . ? Si1A C32 H32B 128.3 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1A C32 H32C 86.2 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 Si1A 50.7(3) . . ? C34 C33 H33A 109.5 . . ? Si1A C33 H33A 113.4 . . ? C34 C33 H33B 109.5 . . ? Si1A C33 H33B 136.8 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? Si1A C33 H33C 60.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34A C35 Si1 49.8(2) . . ? C34A C35 H35A 113.4 . . ? Si1 C35 H35A 109.5 . . ? C34A C35 H35B 136.7 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34A C35 H35C 61.4 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C2S C1S C6S 118.3(2) . . ? C2S C1S C7S 120.7(2) . . ? C6S C1S C7S 120.9(3) . . ? C3S C2S C1S 121.1(2) . . ? C3S C2S H2SA 119.4 . . ? C1S C2S H2SA 119.4 . . ? C4S C3S C2S 120.2(3) . . ? C4S C3S H3SA 119.9 . . ? C2S C3S H3SA 119.9 . . ? C3S C4S C5S 119.3(3) . . ? C3S C4S H4SA 120.4 . . ? C5S C4S H4SA 120.4 . . ? C6S C5S C4S 120.4(2) . . ? C6S C5S H5SA 119.8 . . ? C4S C5S H5SA 119.8 . . ? C5S C6S C1S 120.6(3) . . ? C5S C6S H6SA 119.7 . . ? C1S C6S H6SA 119.7 . . ? C1S C7S H7SA 109.5 . . ? C1S C7S H7SB 109.5 . . ? H7SA C7S H7SB 109.5 . . ? C1S C7S H7SC 109.5 . . ? H7SA C7S H7SC 109.5 . . ? H7SB C7S H7SC 109.5 . . ? N1 Si1 C34 105.8(2) . . ? N1 Si1 C32 108.41(11) . . ? C34 Si1 C32 107.8(2) . . ? N1 Si1 C35 119.75(14) . . ? C34 Si1 C35 101.7(3) . . ? C32 Si1 C35 112.45(15) . . ? N1 Si1 K1 40.29(7) . . ? C34 Si1 K1 95.3(2) . . ? C32 Si1 K1 75.19(9) . . ? C35 Si1 K1 157.70(13) . . ? C37 C34 C36 107.6(5) . . ? C37 C34 C33 115.5(5) . . ? C36 C34 C33 111.2(4) . . ? C37 C34 Si1 110.6(4) . . ? C36 C34 Si1 108.8(4) . . ? C33 C34 Si1 103.1(4) . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N1 Si1A C32 111.47(12) . . ? N1 Si1A C34A 111.69(17) . . ? C32 Si1A C34A 103.80(19) . . ? N1 Si1A C33 112.28(13) . . ? C32 Si1A C33 118.64(16) . . ? C34A Si1A C33 97.7(2) . . ? N1 Si1A K1 56.86(8) . . ? C32 Si1A K1 91.73(10) . . ? C34A Si1A K1 163.76(16) . . ? C33 Si1A K1 78.57(12) . . ? C37A C34A C36A 108.6(5) . . ? C37A C34A C35 113.6(5) . . ? C36A C34A C35 112.7(4) . . ? C37A C34A Si1A 111.5(4) . . ? C36A C34A Si1A 110.4(4) . . ? C35 C34A Si1A 99.8(3) . . ? C34A C36A H36D 109.5 . . ? C34A C36A H36E 109.5 . . ? H36D C36A H36E 109.5 . . ? C34A C36A H36F 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? C34A C37A H37D 109.5 . . ? C34A C37A H37E 109.5 . . ? H37D C37A H37E 109.5 . . ? C34A C37A H37F 109.5 . . ? H37D C37A H37F 109.5 . . ? H37E C37A H37F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.883 _refine_diff_density_min -1.544 _refine_diff_density_rms 0.084 #===END data_Dy2-biph-crown2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H158 Dy2 Fe2 K2 N4 O15 Si4' _chemical_formula_weight 2187.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Dy' 'Dy' -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C2 2 21' _space_group_name_Hall 'C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 17.237(6) _cell_length_b 22.611(8) _cell_length_c 34.538(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13461(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4544 _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6618 _exptl_absorpt_correction_T_max 0.7503 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79111 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 30.75 _reflns_number_total 20024 _reflns_number_gt 16819 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(6) _refine_ls_number_reflns 20024 _refine_ls_number_parameters 588 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.519638(9) 0.237687(6) 0.308656(4) 0.02871(4) Uani 1 1 d . . . Fe1 Fe 0.64347(3) 0.19979(2) 0.375399(15) 0.03285(11) Uani 1 1 d . . . K1 K 0.55584(5) 0.14144(4) 0.57838(2) 0.04370(19) Uani 1 1 d . . . Si1 Si 0.37967(7) 0.18505(4) 0.37978(3) 0.0406(2) Uani 1 1 d . A . Si2 Si 0.52547(7) 0.38291(4) 0.35984(3) 0.0349(2) Uani 1 1 d . . . N1 N 0.46502(16) 0.17842(13) 0.35680(8) 0.0343(6) Uani 1 1 d . . . N2 N 0.56068(18) 0.31650(12) 0.34680(8) 0.0332(6) Uani 1 1 d . . . O1 O 0.60238(18) 0.06678(12) 0.63722(9) 0.0489(7) Uani 1 1 d . . . O2 O 0.44618(16) 0.07540(13) 0.61652(8) 0.0457(6) Uani 1 1 d . . . O3 O 0.39911(17) 0.16585(14) 0.56843(8) 0.0491(7) Uani 1 1 d . . . O4 O 0.5101(2) 0.21722(13) 0.51749(8) 0.0569(8) Uani 1 1 d . . . O5 O 0.6686(2) 0.20391(15) 0.53575(8) 0.0563(8) Uani 1 1 d . . . O6 O 0.71080(16) 0.10588(13) 0.58170(9) 0.0493(7) Uani 1 1 d . . . O8 O 0.5357(2) 0.24000(19) 0.62057(13) 0.0929(14) Uani 1 1 d D . . C31 C 0.4772(3) 0.2402(3) 0.64990(17) 0.0824(16) Uani 1 1 d D . . H31A H 0.4813 0.2043 0.6662 0.099 Uiso 1 1 calc R . . H31B H 0.4249 0.2413 0.6381 0.099 Uiso 1 1 calc R . . C32 C 0.4906(4) 0.2937(3) 0.67344(18) 0.094(2) Uani 1 1 d D . . H32A H 0.4913 0.2840 0.7014 0.113 Uiso 1 1 calc R . . H32B H 0.4498 0.3237 0.6686 0.113 Uiso 1 1 calc R . . C33 C 0.5682(5) 0.3157(3) 0.6604(2) 0.108(3) Uani 1 1 d D . . H33A H 0.5676 0.3593 0.6578 0.130 Uiso 1 1 calc R . . H33B H 0.6089 0.3045 0.6792 0.130 Uiso 1 1 calc R . . C34 C 0.5824(4) 0.2890(4) 0.6243(2) 0.102(2) Uani 1 1 d D . . H34A H 0.5713 0.3174 0.6032 0.122 Uiso 1 1 calc R . . H34B H 0.6376 0.2772 0.6224 0.122 Uiso 1 1 calc R . . O7 O 0.5691(6) 0.0534(3) 0.5198(2) 0.060(2) Uani 0.50 1 d P . -1 C35 C 0.5180(8) 0.0488(4) 0.4908(3) 0.066(2) Uani 0.50 1 d PU . -1 H35A H 0.5245 0.0824 0.4727 0.079 Uiso 0.50 1 calc PR . -1 H35B H 0.4645 0.0501 0.5013 0.079 Uiso 0.50 1 calc PR . -1 C36 C 0.5304(10) -0.0064(7) 0.4705(4) 0.100(4) Uani 0.50 1 d PU . -1 H36A H 0.5575 0.0006 0.4456 0.120 Uiso 0.50 1 calc PR . -1 H36B H 0.4803 -0.0262 0.4651 0.120 Uiso 0.50 1 calc PR . -1 C37 C 0.5811(11) -0.0449(7) 0.4978(4) 0.077(4) Uani 0.50 1 d PU . -1 H37A H 0.5516 -0.0794 0.5076 0.092 Uiso 0.50 1 calc PR . -1 H37B H 0.6283 -0.0592 0.4844 0.092 Uiso 0.50 1 calc PR . -1 C38 C 0.6012(9) -0.0036(6) 0.5298(4) 0.084(3) Uani 0.50 1 d PU . -1 H38A H 0.5790 -0.0178 0.5545 0.101 Uiso 0.50 1 calc PR . -1 H38B H 0.6583 -0.0008 0.5327 0.101 Uiso 0.50 1 calc PR . -1 C1 C 0.5000 0.3029(2) 0.2500 0.0289(10) Uani 1 2 d S . . H1A H 0.5000 0.3449 0.2500 0.035 Uiso 1 2 calc SR . . C2 C 0.42935(19) 0.27211(14) 0.25860(9) 0.0305(7) Uani 1 1 d . . . H2A H 0.3849 0.2932 0.2672 0.037 Uiso 1 1 calc R . . C3 C 0.5734(2) 0.20727(15) 0.24602(10) 0.0337(8) Uani 1 1 d . . . H3A H 0.6219 0.1874 0.2464 0.040 Uiso 1 1 calc R . . C4 C 0.5000 0.1731(2) 0.2500 0.0328(11) Uani 1 2 d S . . C5 C 0.5000 0.1098(2) 0.2500 0.0519(18) Uani 1 2 d SU . . C6 C 0.5694(4) 0.07671(17) 0.24549(12) 0.0673(16) Uani 1 1 d U . . H6A H 0.6176 0.0965 0.2423 0.081 Uiso 1 1 calc R . . C7 C 0.5665(5) 0.01450(19) 0.24572(14) 0.0859(19) Uani 1 1 d U . . H7A H 0.6137 -0.0068 0.2427 0.103 Uiso 1 1 calc R . . C8 C 0.5000 -0.0164(3) 0.2500 0.0859(19) Uani 1 2 d SU . . H8A H 0.5000 -0.0584 0.2500 0.103 Uiso 1 2 calc SR . . C9 C 0.5341(2) 0.15518(14) 0.37025(10) 0.0336(8) Uani 1 1 d . . . C10 C 0.5663(2) 0.15412(16) 0.40922(11) 0.0395(8) Uani 1 1 d . . . H10A H 0.5420 0.1700 0.4316 0.047 Uiso 1 1 calc R . . C11 C 0.6392(3) 0.12578(15) 0.40860(11) 0.0438(9) Uani 1 1 d . . . H11A H 0.6705 0.1176 0.4306 0.053 Uiso 1 1 calc R . . C12 C 0.6583(3) 0.11138(16) 0.36923(13) 0.0465(10) Uani 1 1 d . . . H12A H 0.7046 0.0932 0.3603 0.056 Uiso 1 1 calc R . . C13 C 0.5932(2) 0.12995(14) 0.34605(10) 0.0336(7) Uani 1 1 d . . . H13A H 0.5898 0.1261 0.3187 0.040 Uiso 1 1 calc R . . C14 C 0.6286(2) 0.29050(14) 0.36089(11) 0.0341(7) Uani 1 1 d . . . C15 C 0.6533(2) 0.28151(15) 0.40050(11) 0.0411(9) Uani 1 1 d . . . H15A H 0.6262 0.2935 0.4231 0.049 Uiso 1 1 calc R . . C16 C 0.7261(3) 0.25125(16) 0.39927(14) 0.0536(12) Uani 1 1 d . . . H16A H 0.7565 0.2411 0.4212 0.064 Uiso 1 1 calc R . . C17 C 0.7453(2) 0.2390(2) 0.36127(14) 0.0499(9) Uani 1 1 d . . . H17A H 0.7905 0.2188 0.3527 0.060 Uiso 1 1 calc R . . C18 C 0.68545(19) 0.26201(17) 0.33728(11) 0.0391(7) Uani 1 1 d . . . H18A H 0.6836 0.2589 0.3099 0.047 Uiso 1 1 calc R . . C19 C 0.3853(4) 0.2224(2) 0.42793(13) 0.083(2) Uani 1 1 d . . . H19A H 0.4150 0.2592 0.4255 0.124 Uiso 1 1 calc R . . H19B H 0.4112 0.1962 0.4465 0.124 Uiso 1 1 calc R . . H19C H 0.3328 0.2314 0.4371 0.124 Uiso 1 1 calc R . . C20 C 0.3128(2) 0.22943(19) 0.34837(12) 0.0465(9) Uani 1 1 d . . . H20A H 0.3329 0.2698 0.3459 0.070 Uiso 1 1 calc R . . H20B H 0.2611 0.2305 0.3601 0.070 Uiso 1 1 calc R . . H20C H 0.3096 0.2111 0.3227 0.070 Uiso 1 1 calc R . . C21 C 0.3310(3) 0.1095(2) 0.38678(19) 0.0676(16) Uani 1 1 d . . . C22 C 0.3827(3) 0.0722(2) 0.41460(19) 0.0769(17) Uani 1 1 d . A . H22A H 0.3583 0.0337 0.4191 0.115 Uiso 1 1 calc R . . H22B H 0.3882 0.0931 0.4393 0.115 Uiso 1 1 calc R . . H22C H 0.4339 0.0665 0.4029 0.115 Uiso 1 1 calc R . . C23 C 0.2611(9) 0.1267(7) 0.4175(5) 0.097(5) Uani 0.50 1 d PU A 1 H23A H 0.2285 0.0919 0.4221 0.146 Uiso 0.50 1 calc PR A 1 H23B H 0.2295 0.1586 0.4067 0.146 Uiso 0.50 1 calc PR A 1 H23C H 0.2840 0.1397 0.4421 0.146 Uiso 0.50 1 calc PR A 1 C23A C 0.2463(5) 0.1120(4) 0.3968(3) 0.046(2) Uani 0.50 1 d PU A 2 H23D H 0.2303 0.0743 0.4084 0.069 Uiso 0.50 1 calc PR A 2 H23E H 0.2159 0.1193 0.3733 0.069 Uiso 0.50 1 calc PR A 2 H23F H 0.2373 0.1441 0.4154 0.069 Uiso 0.50 1 calc PR A 2 C24 C 0.3272(4) 0.0795(3) 0.3462(2) 0.101(2) Uani 1 1 d . A . H24A H 0.3030 0.0404 0.3486 0.151 Uiso 1 1 calc R . . H24B H 0.3798 0.0751 0.3358 0.151 Uiso 1 1 calc R . . H24C H 0.2964 0.1041 0.3286 0.151 Uiso 1 1 calc R . . C25 C 0.5131(4) 0.3925(2) 0.41355(13) 0.0737(15) Uani 1 1 d . . . H25A H 0.4863 0.3579 0.4243 0.111 Uiso 1 1 calc R . . H25B H 0.4823 0.4281 0.4186 0.111 Uiso 1 1 calc R . . H25C H 0.5641 0.3965 0.4258 0.111 Uiso 1 1 calc R . . C26 C 0.4292(2) 0.39342(18) 0.33689(13) 0.0475(10) Uani 1 1 d . . . H26A H 0.4345 0.3907 0.3087 0.071 Uiso 1 1 calc R . . H26B H 0.4087 0.4324 0.3439 0.071 Uiso 1 1 calc R . . H26C H 0.3935 0.3627 0.3460 0.071 Uiso 1 1 calc R . . C27 C 0.5927(2) 0.44433(16) 0.34233(15) 0.0515(11) Uani 1 1 d . . . C28 C 0.6724(3) 0.4352(2) 0.35927(19) 0.0681(15) Uani 1 1 d . . . H28A H 0.7090 0.4627 0.3472 0.102 Uiso 1 1 calc R . . H28B H 0.6893 0.3944 0.3544 0.102 Uiso 1 1 calc R . . H28C H 0.6708 0.4424 0.3872 0.102 Uiso 1 1 calc R . . C29 C 0.5637(4) 0.50541(19) 0.3543(2) 0.084(2) Uani 1 1 d . . . H29A H 0.5986 0.5358 0.3440 0.126 Uiso 1 1 calc R . . H29B H 0.5625 0.5081 0.3826 0.126 Uiso 1 1 calc R . . H29C H 0.5113 0.5116 0.3440 0.126 Uiso 1 1 calc R . . C30 C 0.5966(3) 0.4417(2) 0.29667(15) 0.0681(14) Uani 1 1 d . . . H30A H 0.6312 0.4729 0.2872 0.102 Uiso 1 1 calc R . . H30B H 0.5445 0.4475 0.2859 0.102 Uiso 1 1 calc R . . H30C H 0.6166 0.4031 0.2886 0.102 Uiso 1 1 calc R . . C39 C 0.6765(3) 0.04086(19) 0.63292(16) 0.0603(13) Uani 1 1 d . . . H39A H 0.6739 0.0077 0.6142 0.072 Uiso 1 1 calc R . . H39B H 0.6946 0.0251 0.6581 0.072 Uiso 1 1 calc R . . C40 C 0.7319(3) 0.0870(2) 0.61858(18) 0.0678(15) Uani 1 1 d . . . H40A H 0.7319 0.1211 0.6366 0.081 Uiso 1 1 calc R . . H40B H 0.7851 0.0704 0.6178 0.081 Uiso 1 1 calc R . . C41 C 0.7657(3) 0.1463(2) 0.56620(15) 0.0576(12) Uani 1 1 d . . . H41A H 0.8157 0.1258 0.5617 0.069 Uiso 1 1 calc R . . H41B H 0.7747 0.1789 0.5848 0.069 Uiso 1 1 calc R . . C42 C 0.7354(3) 0.1707(3) 0.52871(15) 0.0674(15) Uani 1 1 d . . . H42A H 0.7753 0.1960 0.5165 0.081 Uiso 1 1 calc R . . H42B H 0.7232 0.1379 0.5107 0.081 Uiso 1 1 calc R . . C43 C 0.6414(4) 0.2333(3) 0.50160(13) 0.0736(16) Uani 1 1 d . . . H43A H 0.6353 0.2044 0.4803 0.088 Uiso 1 1 calc R . . H43B H 0.6794 0.2636 0.4934 0.088 Uiso 1 1 calc R . . C44 C 0.5669(4) 0.2612(3) 0.51026(14) 0.0771(16) Uani 1 1 d . . . H44A H 0.5722 0.2870 0.5332 0.093 Uiso 1 1 calc R . . H44B H 0.5505 0.2860 0.4881 0.093 Uiso 1 1 calc R . . C45 C 0.4366(3) 0.2414(2) 0.52601(13) 0.0636(13) Uani 1 1 d . . . H45A H 0.4191 0.2666 0.5043 0.076 Uiso 1 1 calc R . . H45B H 0.4400 0.2662 0.5495 0.076 Uiso 1 1 calc R . . C46 C 0.3788(3) 0.1917(2) 0.53245(12) 0.0588(13) Uani 1 1 d . . . H46A H 0.3252 0.2074 0.5333 0.071 Uiso 1 1 calc R . . H46B H 0.3824 0.1621 0.5114 0.071 Uiso 1 1 calc R . . C47 C 0.3490(3) 0.1198(2) 0.57903(14) 0.0567(11) Uani 1 1 d . . . H47A H 0.3533 0.0870 0.5601 0.068 Uiso 1 1 calc R . . H47B H 0.2947 0.1341 0.5788 0.068 Uiso 1 1 calc R . . C48 C 0.3686(2) 0.0986(2) 0.61708(14) 0.0530(11) Uani 1 1 d . . . H48A H 0.3650 0.1313 0.6360 0.064 Uiso 1 1 calc R . . H48B H 0.3317 0.0672 0.6250 0.064 Uiso 1 1 calc R . . C49 C 0.4718(3) 0.05430(19) 0.65337(11) 0.0545(11) Uani 1 1 d . . . H49A H 0.4331 0.0264 0.6641 0.065 Uiso 1 1 calc R . . H49B H 0.4771 0.0878 0.6716 0.065 Uiso 1 1 calc R . . C50 C 0.5458(3) 0.02479(19) 0.64883(12) 0.0499(11) Uani 1 1 d . . . H50A H 0.5614 0.0064 0.6736 0.060 Uiso 1 1 calc R . . H50B H 0.5415 -0.0068 0.6291 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.03066(7) 0.02559(6) 0.02988(7) 0.00070(6) 0.00080(7) -0.00269(6) Fe1 0.0338(3) 0.0234(2) 0.0414(3) 0.00595(19) -0.0080(2) -0.00435(19) K1 0.0394(4) 0.0506(5) 0.0411(4) 0.0105(4) 0.0080(4) 0.0081(4) Si1 0.0467(6) 0.0306(5) 0.0446(6) 0.0092(4) 0.0156(5) 0.0025(4) Si2 0.0392(5) 0.0249(4) 0.0407(5) -0.0025(3) -0.0010(5) -0.0010(4) N1 0.0309(16) 0.0394(15) 0.0326(14) 0.0027(11) -0.0005(11) -0.0105(12) N2 0.0386(16) 0.0259(13) 0.0350(15) 0.0007(10) -0.0078(13) -0.0036(12) O1 0.0559(17) 0.0347(13) 0.0562(17) -0.0004(12) -0.0155(15) 0.0031(12) O2 0.0422(14) 0.0518(16) 0.0431(15) 0.0091(12) 0.0077(12) 0.0063(13) O3 0.0429(15) 0.0657(18) 0.0387(15) 0.0017(13) -0.0006(12) 0.0151(14) O4 0.074(2) 0.0529(16) 0.0437(15) 0.0146(12) 0.0085(15) 0.0094(16) O5 0.068(2) 0.0604(19) 0.0401(16) -0.0057(14) 0.0117(14) -0.0190(16) O6 0.0323(14) 0.0466(15) 0.069(2) -0.0145(14) -0.0144(13) -0.0051(12) O8 0.064(2) 0.084(2) 0.130(3) -0.045(3) 0.047(2) -0.027(2) C31 0.060(3) 0.099(4) 0.088(4) -0.020(3) 0.024(3) -0.019(4) C32 0.102(5) 0.105(5) 0.076(4) -0.021(3) 0.012(4) 0.023(4) C33 0.143(7) 0.078(4) 0.103(5) -0.014(4) -0.004(5) -0.044(5) C34 0.093(5) 0.121(6) 0.092(5) -0.019(4) 0.014(4) -0.035(4) O7 0.087(6) 0.042(4) 0.051(4) -0.007(3) -0.025(4) 0.010(4) C35 0.070(6) 0.057(5) 0.071(5) -0.003(4) -0.004(5) 0.007(5) C36 0.109(8) 0.095(7) 0.095(7) -0.020(6) -0.018(7) 0.010(7) C37 0.094(8) 0.064(6) 0.072(7) -0.016(6) -0.012(7) 0.024(6) C38 0.086(7) 0.078(6) 0.088(7) -0.011(6) -0.016(6) 0.014(6) C1 0.030(3) 0.029(2) 0.028(2) 0.000 -0.0038(17) 0.000 C2 0.0278(15) 0.0327(17) 0.0309(16) -0.0022(12) 0.0040(14) 0.0005(13) C3 0.037(2) 0.0328(16) 0.0317(17) 0.0004(13) 0.0019(14) 0.0068(16) C4 0.038(3) 0.025(2) 0.036(2) 0.000 0.0025(19) 0.000 C5 0.103(6) 0.025(2) 0.027(2) 0.000 0.002(3) 0.000 C6 0.133(5) 0.0357(18) 0.034(2) -0.0001(16) 0.003(3) 0.030(3) C7 0.177(6) 0.0384(19) 0.0420(19) -0.0005(19) -0.009(3) 0.036(3) C8 0.177(6) 0.0384(19) 0.0420(19) -0.0005(19) -0.009(3) 0.036(3) C9 0.039(2) 0.0271(14) 0.0353(17) 0.0026(12) -0.0036(15) -0.0120(13) C10 0.048(2) 0.0353(17) 0.0348(18) 0.0059(14) -0.0058(16) -0.0131(16) C11 0.062(3) 0.0288(16) 0.040(2) 0.0098(14) -0.0169(19) -0.0080(17) C12 0.054(2) 0.0265(16) 0.059(3) 0.0034(16) -0.011(2) -0.0011(16) C13 0.0392(19) 0.0251(14) 0.0366(18) 0.0024(12) -0.0028(15) -0.0021(13) C14 0.0334(17) 0.0237(15) 0.0452(19) 0.0048(13) -0.0093(15) -0.0079(13) C15 0.056(2) 0.0267(15) 0.041(2) 0.0014(13) -0.0144(17) -0.0088(16) C16 0.053(2) 0.032(2) 0.076(3) 0.0110(17) -0.034(2) -0.0140(16) C17 0.0339(18) 0.0436(19) 0.072(3) 0.014(2) -0.0064(18) -0.0077(18) C18 0.0302(16) 0.0342(15) 0.053(2) 0.0108(17) -0.0008(15) -0.0086(16) C19 0.139(5) 0.071(3) 0.038(2) 0.001(2) 0.012(3) 0.056(4) C20 0.043(2) 0.045(2) 0.051(2) 0.0075(17) 0.0130(17) -0.0008(18) C21 0.037(2) 0.048(2) 0.118(5) 0.038(3) 0.018(3) 0.0047(19) C22 0.073(3) 0.043(2) 0.115(5) 0.039(3) 0.031(3) 0.001(2) C23 0.089(8) 0.092(8) 0.111(9) 0.050(7) 0.015(7) 0.003(6) C23A 0.039(4) 0.037(4) 0.060(5) -0.004(4) 0.012(4) -0.007(3) C24 0.113(5) 0.053(3) 0.136(6) 0.003(3) -0.030(5) -0.043(3) C25 0.106(4) 0.063(3) 0.052(3) -0.017(2) -0.008(3) 0.016(3) C26 0.0330(19) 0.041(2) 0.068(3) -0.0146(19) 0.0074(19) 0.0048(16) C27 0.041(2) 0.0266(17) 0.087(3) 0.0033(18) -0.019(2) -0.0046(15) C28 0.044(2) 0.035(2) 0.126(5) 0.008(2) -0.026(3) -0.0137(18) C29 0.078(4) 0.028(2) 0.147(6) -0.008(3) -0.041(4) 0.003(2) C30 0.067(3) 0.057(3) 0.080(4) 0.021(2) 0.004(3) -0.020(2) C39 0.052(3) 0.040(2) 0.088(4) 0.000(2) -0.033(3) 0.0035(19) C40 0.050(3) 0.049(3) 0.105(4) 0.002(3) -0.025(3) 0.002(2) C41 0.035(2) 0.068(3) 0.070(3) -0.018(2) -0.003(2) -0.016(2) C42 0.056(3) 0.085(4) 0.061(3) -0.027(3) 0.019(2) -0.026(3) C43 0.087(4) 0.100(4) 0.034(2) 0.012(3) 0.002(2) -0.035(4) C44 0.117(5) 0.070(3) 0.045(2) 0.022(2) 0.004(3) -0.013(4) C45 0.093(4) 0.059(3) 0.039(2) 0.014(2) 0.010(2) 0.035(3) C46 0.064(3) 0.080(3) 0.033(2) 0.004(2) -0.0033(19) 0.036(3) C47 0.038(2) 0.072(3) 0.060(3) 0.003(2) 0.007(2) 0.012(2) C48 0.039(2) 0.055(2) 0.065(3) 0.009(2) 0.015(2) 0.0032(19) C49 0.075(3) 0.051(2) 0.037(2) 0.0082(16) 0.008(2) -0.002(2) C50 0.070(3) 0.042(2) 0.038(2) 0.0088(16) -0.0049(19) 0.0029(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 N2 2.326(3) . ? Dy1 N1 2.334(3) . ? Dy1 C3 2.452(4) . ? Dy1 C2 2.453(3) . ? Dy1 C4 2.521(3) . ? Dy1 C1 2.528(3) . ? Dy1 C3 2.571(4) 3_655 ? Dy1 C2 2.603(3) 3_655 ? Dy1 C9 2.840(3) . ? Dy1 C14 2.865(3) . ? Dy1 Fe1 3.2564(10) . ? Fe1 C16 2.015(4) . ? Fe1 C17 2.027(4) . ? Fe1 C12 2.027(4) . ? Fe1 C11 2.030(3) . ? Fe1 C15 2.048(4) . ? Fe1 C10 2.049(4) . ? Fe1 C18 2.058(4) . ? Fe1 C13 2.067(3) . ? Fe1 C14 2.127(3) . ? Fe1 C9 2.146(3) . ? K1 O8 2.685(4) . ? K1 O2 2.745(3) . ? K1 O1 2.761(3) . ? K1 O3 2.779(3) . ? K1 O6 2.792(3) . ? K1 O5 2.817(3) . ? K1 O4 2.825(3) . ? K1 O7 2.849(7) . ? K1 C37 3.447(13) 4_556 ? K1 C36 3.515(14) 4_556 ? Si1 N1 1.678(3) . ? Si1 C19 1.868(5) . ? Si1 C20 1.874(4) . ? Si1 C21 1.919(5) . ? Si2 N2 1.681(3) . ? Si2 C26 1.854(4) . ? Si2 C25 1.880(5) . ? Si2 C27 1.907(4) . ? N1 C9 1.382(5) . ? N2 C14 1.397(4) . ? O1 C39 1.414(5) . ? O1 C50 1.419(5) . ? O2 C49 1.429(5) . ? O2 C48 1.437(5) . ? O3 C47 1.402(6) . ? O3 C46 1.417(5) . ? O4 C45 1.410(6) . ? O4 C44 1.417(6) . ? O5 C42 1.396(6) . ? O5 C43 1.432(6) . ? O6 C40 1.392(6) . ? O6 C41 1.420(5) . ? O8 C34 1.375(7) . ? O8 C31 1.429(6) . ? C31 C32 1.476(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.496(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.406(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? O7 C35 1.336(14) . ? O7 C38 1.444(15) . ? C35 C36 1.449(16) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.55(2) . ? C36 K1 3.515(14) 4_556 ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.487(17) . ? C37 K1 3.447(13) 4_556 ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C1 C2 1.433(4) 3_655 ? C1 C2 1.433(4) . ? C1 Dy1 2.528(3) 3_655 ? C1 H1A 0.9500 . ? C2 C3 1.476(4) 3_655 ? C2 Dy1 2.603(3) 3_655 ? C2 H2A 0.9500 . ? C3 C2 1.476(4) 3_655 ? C3 C4 1.489(4) . ? C3 Dy1 2.571(4) 3_655 ? C3 H3A 0.9500 . ? C4 C5 1.431(7) . ? C4 C3 1.489(4) 3_655 ? C4 Dy1 2.521(3) 3_655 ? C5 C6 1.419(6) 3_655 ? C5 C6 1.419(6) . ? C6 C7 1.407(6) . ? C6 H6A 0.9500 . ? C7 C8 1.351(8) . ? C7 H7A 0.9500 . ? C8 C7 1.351(8) 3_655 ? C8 H8A 0.9500 . ? C9 C13 1.436(5) . ? C9 C10 1.456(5) . ? C10 C11 1.411(6) . ? C10 H10A 0.9500 . ? C11 C12 1.436(6) . ? C11 H11A 0.9500 . ? C12 C13 1.442(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C18 1.428(5) . ? C14 C15 1.447(5) . ? C15 C16 1.429(6) . ? C15 H15A 0.9500 . ? C16 C17 1.382(7) . ? C16 H16A 0.9500 . ? C17 C18 1.422(5) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23A 1.503(10) . ? C21 C22 1.557(7) . ? C21 C24 1.559(9) . ? C21 C23 1.653(17) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.508(6) . ? C27 C29 1.526(6) . ? C27 C30 1.580(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C39 C40 1.499(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.502(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.462(9) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.518(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.439(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.449(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Dy1 N1 99.15(10) . . ? N2 Dy1 C3 126.84(12) . . ? N1 Dy1 C3 128.32(11) . . ? N2 Dy1 C2 110.43(10) . . ? N1 Dy1 C2 115.37(10) . . ? C3 Dy1 C2 72.96(11) . . ? N2 Dy1 C4 160.05(10) . . ? N1 Dy1 C4 100.70(11) . . ? C3 Dy1 C4 34.82(10) . . ? C2 Dy1 C4 62.11(10) . . ? N2 Dy1 C1 92.75(11) . . ? N1 Dy1 C1 148.39(7) . . ? C3 Dy1 C1 60.47(11) . . ? C2 Dy1 C1 33.41(8) . . ? C4 Dy1 C1 71.08(11) . . ? N2 Dy1 C3 144.15(11) . 3_655 ? N1 Dy1 C3 96.78(11) . 3_655 ? C3 Dy1 C3 60.85(16) . 3_655 ? C2 Dy1 C3 34.06(10) . 3_655 ? C4 Dy1 C3 34.00(9) . 3_655 ? C1 Dy1 C3 58.93(10) . 3_655 ? N2 Dy1 C2 100.00(10) . 3_655 ? N1 Dy1 C2 160.70(10) . 3_655 ? C3 Dy1 C2 33.78(10) . 3_655 ? C2 Dy1 C2 59.37(13) . 3_655 ? C4 Dy1 C2 60.09(10) . 3_655 ? C1 Dy1 C2 32.40(8) . 3_655 ? C3 Dy1 C2 68.61(11) 3_655 3_655 ? N2 Dy1 C9 93.00(10) . . ? N1 Dy1 C9 28.91(10) . . ? C3 Dy1 C9 116.32(11) . . ? C2 Dy1 C9 142.36(10) . . ? C4 Dy1 C9 103.48(11) . . ? C1 Dy1 C9 174.17(10) . . ? C3 Dy1 C9 115.41(10) 3_655 . ? C2 Dy1 C9 146.64(10) 3_655 . ? N2 Dy1 C14 28.92(10) . . ? N1 Dy1 C14 93.16(10) . . ? C3 Dy1 C14 115.13(12) . . ? C2 Dy1 C14 136.68(10) . . ? C4 Dy1 C14 146.69(8) . . ? C1 Dy1 C14 110.46(10) . . ? C3 Dy1 C14 169.38(10) 3_655 . ? C2 Dy1 C14 102.47(11) 3_655 . ? C9 Dy1 C14 75.21(9) . . ? N2 Dy1 Fe1 66.50(7) . . ? N1 Dy1 Fe1 66.98(7) . . ? C3 Dy1 Fe1 107.64(9) . . ? C2 Dy1 Fe1 176.67(8) . . ? C4 Dy1 Fe1 120.30(7) . . ? C1 Dy1 Fe1 143.95(4) . . ? C3 Dy1 Fe1 149.13(8) 3_655 . ? C2 Dy1 Fe1 119.28(8) 3_655 . ? C9 Dy1 Fe1 40.49(7) . . ? C14 Dy1 Fe1 40.02(7) . . ? C16 Fe1 C17 39.99(19) . . ? C16 Fe1 C12 121.56(17) . . ? C17 Fe1 C12 107.25(19) . . ? C16 Fe1 C11 105.68(16) . . ? C17 Fe1 C11 121.85(18) . . ? C12 Fe1 C11 41.47(17) . . ? C16 Fe1 C15 41.18(17) . . ? C17 Fe1 C15 68.64(19) . . ? C12 Fe1 C15 157.52(16) . . ? C11 Fe1 C15 120.51(15) . . ? C16 Fe1 C10 121.08(18) . . ? C17 Fe1 C10 156.92(16) . . ? C12 Fe1 C10 69.19(18) . . ? C11 Fe1 C10 40.47(17) . . ? C15 Fe1 C10 105.49(16) . . ? C16 Fe1 C18 67.58(17) . . ? C17 Fe1 C18 40.75(15) . . ? C12 Fe1 C18 124.24(18) . . ? C11 Fe1 C18 159.63(17) . . ? C15 Fe1 C18 67.97(16) . . ? C10 Fe1 C18 159.59(15) . . ? C16 Fe1 C13 159.74(17) . . ? C17 Fe1 C13 125.40(18) . . ? C12 Fe1 C13 41.23(15) . . ? C11 Fe1 C13 68.42(15) . . ? C15 Fe1 C13 158.67(15) . . ? C10 Fe1 C13 67.82(14) . . ? C18 Fe1 C13 110.85(15) . . ? C16 Fe1 C14 67.96(14) . . ? C17 Fe1 C14 68.04(16) . . ? C12 Fe1 C14 160.34(16) . . ? C11 Fe1 C14 157.49(17) . . ? C15 Fe1 C14 40.50(14) . . ? C10 Fe1 C14 122.82(15) . . ? C18 Fe1 C14 39.87(15) . . ? C13 Fe1 C14 124.79(14) . . ? C16 Fe1 C9 157.84(18) . . ? C17 Fe1 C9 161.26(16) . . ? C12 Fe1 C9 68.81(16) . . ? C11 Fe1 C9 68.14(15) . . ? C15 Fe1 C9 122.13(16) . . ? C10 Fe1 C9 40.54(13) . . ? C18 Fe1 C9 125.26(14) . . ? C13 Fe1 C9 39.80(14) . . ? C14 Fe1 C9 109.14(13) . . ? C16 Fe1 Dy1 126.93(11) . . ? C17 Fe1 Dy1 106.40(12) . . ? C12 Fe1 Dy1 105.54(12) . . ? C11 Fe1 Dy1 126.39(12) . . ? C15 Fe1 Dy1 96.69(11) . . ? C10 Fe1 Dy1 96.35(11) . . ? C18 Fe1 Dy1 66.28(10) . . ? C13 Fe1 Dy1 65.10(10) . . ? C14 Fe1 Dy1 60.03(9) . . ? C9 Fe1 Dy1 59.27(9) . . ? O8 K1 O2 95.85(10) . . ? O8 K1 O1 98.37(13) . . ? O2 K1 O1 60.95(9) . . ? O8 K1 O3 77.08(11) . . ? O2 K1 O3 59.87(9) . . ? O1 K1 O3 119.67(9) . . ? O8 K1 O6 109.91(11) . . ? O2 K1 O6 118.84(9) . . ? O1 K1 O6 61.03(10) . . ? O3 K1 O6 172.97(9) . . ? O8 K1 O5 87.52(11) . . ? O2 K1 O5 176.54(9) . . ? O1 K1 O5 119.39(11) . . ? O3 K1 O5 120.41(10) . . ? O6 K1 O5 60.40(10) . . ? O8 K1 O4 82.21(13) . . ? O2 K1 O4 119.65(10) . . ? O1 K1 O4 179.15(10) . . ? O3 K1 O4 61.05(10) . . ? O6 K1 O4 118.19(10) . . ? O5 K1 O4 59.96(11) . . ? O8 K1 O7 167.46(19) . . ? O2 K1 O7 90.9(2) . . ? O1 K1 O7 94.15(16) . . ? O3 K1 O7 97.41(19) . . ? O6 K1 O7 75.59(19) . . ? O5 K1 O7 85.6(2) . . ? O4 K1 O7 85.26(17) . . ? O8 K1 C37 163.0(3) . 4_556 ? O2 K1 C37 96.3(3) . 4_556 ? O1 K1 C37 97.9(3) . 4_556 ? O3 K1 C37 98.9(3) . 4_556 ? O6 K1 C37 74.2(3) . 4_556 ? O5 K1 C37 80.3(3) . 4_556 ? O4 K1 C37 81.4(3) . 4_556 ? O7 K1 C37 5.5(4) . 4_556 ? O8 K1 C36 164.8(3) . 4_556 ? O2 K1 C36 70.8(3) . 4_556 ? O1 K1 C36 81.9(3) . 4_556 ? O3 K1 C36 89.5(3) . 4_556 ? O6 K1 C36 83.6(3) . 4_556 ? O5 K1 C36 105.7(3) . 4_556 ? O4 K1 C36 97.7(3) . 4_556 ? O7 K1 C36 20.3(3) . 4_556 ? C37 K1 C36 25.8(3) 4_556 4_556 ? N1 Si1 C19 114.6(3) . . ? N1 Si1 C20 108.24(16) . . ? C19 Si1 C20 107.8(2) . . ? N1 Si1 C21 111.28(19) . . ? C19 Si1 C21 108.3(3) . . ? C20 Si1 C21 106.3(2) . . ? N2 Si2 C26 108.85(16) . . ? N2 Si2 C25 114.1(2) . . ? C26 Si2 C25 107.8(3) . . ? N2 Si2 C27 110.24(18) . . ? C26 Si2 C27 108.37(19) . . ? C25 Si2 C27 107.3(3) . . ? C9 N1 Si1 129.1(2) . . ? C9 N1 Dy1 96.33(19) . . ? Si1 N1 Dy1 129.73(17) . . ? C14 N2 Si2 125.8(2) . . ? C14 N2 Dy1 97.5(2) . . ? Si2 N2 Dy1 136.56(17) . . ? C39 O1 C50 111.9(3) . . ? C39 O1 K1 116.0(3) . . ? C50 O1 K1 114.7(2) . . ? C49 O2 C48 113.4(3) . . ? C49 O2 K1 113.4(3) . . ? C48 O2 K1 116.7(2) . . ? C47 O3 C46 112.5(4) . . ? C47 O3 K1 114.8(2) . . ? C46 O3 K1 115.5(3) . . ? C45 O4 C44 112.7(4) . . ? C45 O4 K1 109.3(2) . . ? C44 O4 K1 111.3(3) . . ? C42 O5 C43 112.0(4) . . ? C42 O5 K1 113.0(3) . . ? C43 O5 K1 116.0(3) . . ? C40 O6 C41 111.6(3) . . ? C40 O6 K1 112.1(3) . . ? C41 O6 K1 115.9(3) . . ? C34 O8 C31 110.1(5) . . ? C34 O8 K1 130.0(3) . . ? C31 O8 K1 118.6(3) . . ? O8 C31 C32 106.5(4) . . ? O8 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? O8 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C31 C32 C33 104.2(4) . . ? C31 C32 H32A 110.9 . . ? C33 C32 H32A 110.9 . . ? C31 C32 H32B 110.9 . . ? C33 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? C34 C33 C32 106.3(5) . . ? C34 C33 H33A 110.5 . . ? C32 C33 H33A 110.5 . . ? C34 C33 H33B 110.5 . . ? C32 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? O8 C34 C33 109.0(5) . . ? O8 C34 H34A 109.9 . . ? C33 C34 H34A 109.9 . . ? O8 C34 H34B 109.9 . . ? C33 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? C35 O7 C38 111.3(8) . . ? C35 O7 K1 122.2(6) . . ? C38 O7 K1 118.9(7) . . ? O7 C35 C36 109.4(10) . . ? O7 C35 H35A 109.8 . . ? C36 C35 H35A 109.8 . . ? O7 C35 H35B 109.8 . . ? C36 C35 H35B 109.8 . . ? H35A C35 H35B 108.2 . . ? C35 C36 C37 105.7(11) . . ? C35 C36 K1 178.6(12) . 4_556 ? C37 C36 K1 74.6(7) . 4_556 ? C35 C36 H36A 110.6 . . ? C37 C36 H36A 110.6 . . ? K1 C36 H36A 70.4 4_556 . ? C35 C36 H36B 110.6 . . ? C37 C36 H36B 110.6 . . ? K1 C36 H36B 68.1 4_556 . ? H36A C36 H36B 108.7 . . ? C38 C37 C36 103.3(11) . . ? C38 C37 K1 173.7(12) . 4_556 ? C36 C37 K1 79.6(7) . 4_556 ? C38 C37 H37A 111.1 . . ? C36 C37 H37A 111.1 . . ? K1 C37 H37A 72.4 4_556 . ? C38 C37 H37B 111.1 . . ? C36 C37 H37B 111.1 . . ? K1 C37 H37B 62.7 4_556 . ? H37A C37 H37B 109.1 . . ? O7 C38 C37 107.0(10) . . ? O7 C38 H38A 110.3 . . ? C37 C38 H38A 110.3 . . ? O7 C38 H38B 110.3 . . ? C37 C38 H38B 110.3 . . ? H38A C38 H38B 108.6 . . ? C2 C1 C2 122.0(4) 3_655 . ? C2 C1 Dy1 70.42(17) 3_655 3_655 ? C2 C1 Dy1 76.68(18) . 3_655 ? C2 C1 Dy1 76.68(18) 3_655 . ? C2 C1 Dy1 70.42(17) . . ? Dy1 C1 Dy1 108.69(17) 3_655 . ? C2 C1 H1A 119.0 3_655 . ? C2 C1 H1A 119.0 . . ? Dy1 C1 H1A 125.7 3_655 . ? Dy1 C1 H1A 125.7 . . ? C1 C2 C3 119.1(3) . 3_655 ? C1 C2 Dy1 76.17(16) . . ? C3 C2 Dy1 77.4(2) 3_655 . ? C1 C2 Dy1 70.91(15) . 3_655 ? C3 C2 Dy1 67.50(19) 3_655 3_655 ? Dy1 C2 Dy1 108.65(12) . 3_655 ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 3_655 . ? Dy1 C2 H2A 116.9 . . ? Dy1 C2 H2A 134.5 3_655 . ? C2 C3 C4 119.9(4) 3_655 . ? C2 C3 Dy1 78.7(2) 3_655 . ? C4 C3 Dy1 75.10(16) . . ? C2 C3 Dy1 68.6(2) 3_655 3_655 ? C4 C3 Dy1 71.14(17) . 3_655 ? Dy1 C3 Dy1 109.70(15) . 3_655 ? C2 C3 H3A 120.1 3_655 . ? C4 C3 H3A 120.1 . . ? Dy1 C3 H3A 116.9 . . ? Dy1 C3 H3A 133.4 3_655 . ? C5 C4 C3 121.3(2) . . ? C5 C4 C3 121.3(2) . 3_655 ? C3 C4 C3 117.4(4) . 3_655 ? C5 C4 Dy1 125.42(9) . . ? C3 C4 Dy1 70.08(17) . . ? C3 C4 Dy1 74.87(18) 3_655 . ? C5 C4 Dy1 125.42(9) . 3_655 ? C3 C4 Dy1 74.87(18) . 3_655 ? C3 C4 Dy1 70.08(17) 3_655 3_655 ? Dy1 C4 Dy1 109.15(17) . 3_655 ? C6 C5 C6 116.4(6) 3_655 . ? C6 C5 C4 121.8(3) 3_655 . ? C6 C5 C4 121.8(3) . . ? C7 C6 C5 119.8(6) . . ? C7 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C8 C7 C6 123.2(7) . . ? C8 C7 H7A 118.4 . . ? C6 C7 H7A 118.4 . . ? C7 C8 C7 117.7(7) . 3_655 ? C7 C8 H8A 121.1 . . ? C7 C8 H8A 121.1 3_655 . ? N1 C9 C13 124.5(3) . . ? N1 C9 C10 130.2(3) . . ? C13 C9 C10 105.1(3) . . ? N1 C9 Fe1 127.3(2) . . ? C13 C9 Fe1 67.16(19) . . ? C10 C9 Fe1 66.17(19) . . ? N1 C9 Dy1 54.76(16) . . ? C13 C9 Dy1 83.52(19) . . ? C10 C9 Dy1 137.4(2) . . ? Fe1 C9 Dy1 80.23(10) . . ? C11 C10 C9 109.5(3) . . ? C11 C10 Fe1 69.0(2) . . ? C9 C10 Fe1 73.3(2) . . ? C11 C10 H10A 125.3 . . ? C9 C10 H10A 125.3 . . ? Fe1 C10 H10A 124.0 . . ? C10 C11 C12 108.7(3) . . ? C10 C11 Fe1 70.5(2) . . ? C12 C11 Fe1 69.1(2) . . ? C10 C11 H11A 125.6 . . ? C12 C11 H11A 125.6 . . ? Fe1 C11 H11A 126.3 . . ? C11 C12 C13 106.3(4) . . ? C11 C12 Fe1 69.4(2) . . ? C13 C12 Fe1 70.9(2) . . ? C11 C12 H12A 126.8 . . ? C13 C12 H12A 126.8 . . ? Fe1 C12 H12A 124.5 . . ? C9 C13 C12 110.2(3) . . ? C9 C13 Fe1 73.05(19) . . ? C12 C13 Fe1 67.9(2) . . ? C9 C13 H13A 124.9 . . ? C12 C13 H13A 124.9 . . ? Fe1 C13 H13A 125.7 . . ? N2 C14 C18 124.4(3) . . ? N2 C14 C15 129.4(4) . . ? C18 C14 C15 105.9(3) . . ? N2 C14 Fe1 126.1(2) . . ? C18 C14 Fe1 67.5(2) . . ? C15 C14 Fe1 66.82(18) . . ? N2 C14 Dy1 53.62(16) . . ? C18 C14 Dy1 84.4(2) . . ? C15 C14 Dy1 136.9(2) . . ? Fe1 C14 Dy1 79.95(10) . . ? C16 C15 C14 107.3(4) . . ? C16 C15 Fe1 68.2(2) . . ? C14 C15 Fe1 72.7(2) . . ? C16 C15 H15A 126.3 . . ? C14 C15 H15A 126.3 . . ? Fe1 C15 H15A 124.4 . . ? C17 C16 C15 109.6(4) . . ? C17 C16 Fe1 70.5(2) . . ? C15 C16 Fe1 70.6(2) . . ? C17 C16 H16A 125.2 . . ? C15 C16 H16A 125.2 . . ? Fe1 C16 H16A 125.3 . . ? C16 C17 C18 107.8(4) . . ? C16 C17 Fe1 69.6(2) . . ? C18 C17 Fe1 70.8(2) . . ? C16 C17 H17A 126.1 . . ? C18 C17 H17A 126.1 . . ? Fe1 C17 H17A 125.1 . . ? C17 C18 C14 109.3(4) . . ? C17 C18 Fe1 68.4(2) . . ? C14 C18 Fe1 72.7(2) . . ? C17 C18 H18A 125.4 . . ? C14 C18 H18A 125.4 . . ? Fe1 C18 H18A 125.1 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23A C21 C22 115.7(6) . . ? C23A C21 C24 100.6(6) . . ? C22 C21 C24 110.1(5) . . ? C23A C21 C23 30.0(6) . . ? C22 C21 C23 98.5(7) . . ? C24 C21 C23 130.5(8) . . ? C23A C21 Si1 114.8(4) . . ? C22 C21 Si1 108.0(4) . . ? C24 C21 Si1 107.0(3) . . ? C23 C21 Si1 100.9(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C23A H23D 109.5 . . ? C21 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C21 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 108.5(4) . . ? C28 C27 C30 110.1(5) . . ? C29 C27 C30 108.6(4) . . ? C28 C27 Si2 109.3(3) . . ? C29 C27 Si2 111.9(4) . . ? C30 C27 Si2 108.4(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C39 C40 108.8(4) . . ? O1 C39 H39A 109.9 . . ? C40 C39 H39A 109.9 . . ? O1 C39 H39B 109.9 . . ? C40 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? O6 C40 C39 110.4(4) . . ? O6 C40 H40A 109.6 . . ? C39 C40 H40A 109.6 . . ? O6 C40 H40B 109.6 . . ? C39 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? O6 C41 C42 109.3(4) . . ? O6 C41 H41A 109.8 . . ? C42 C41 H41A 109.8 . . ? O6 C41 H41B 109.8 . . ? C42 C41 H41B 109.8 . . ? H41A C41 H41B 108.3 . . ? O5 C42 C41 109.6(4) . . ? O5 C42 H42A 109.8 . . ? C41 C42 H42A 109.8 . . ? O5 C42 H42B 109.8 . . ? C41 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? O5 C43 C44 108.6(4) . . ? O5 C43 H43A 110.0 . . ? C44 C43 H43A 110.0 . . ? O5 C43 H43B 110.0 . . ? C44 C43 H43B 110.0 . . ? H43A C43 H43B 108.4 . . ? O4 C44 C43 110.0(5) . . ? O4 C44 H44A 109.7 . . ? C43 C44 H44A 109.7 . . ? O4 C44 H44B 109.7 . . ? C43 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? O4 C45 C46 109.5(4) . . ? O4 C45 H45A 109.8 . . ? C46 C45 H45A 109.8 . . ? O4 C45 H45B 109.8 . . ? C46 C45 H45B 109.8 . . ? H45A C45 H45B 108.2 . . ? O3 C46 C45 105.8(4) . . ? O3 C46 H46A 110.6 . . ? C45 C46 H46A 110.6 . . ? O3 C46 H46B 110.6 . . ? C45 C46 H46B 110.6 . . ? H46A C46 H46B 108.7 . . ? O3 C47 C48 110.0(4) . . ? O3 C47 H47A 109.7 . . ? C48 C47 H47A 109.7 . . ? O3 C47 H47B 109.7 . . ? C48 C47 H47B 109.7 . . ? H47A C47 H47B 108.2 . . ? O2 C48 C47 109.1(3) . . ? O2 C48 H48A 109.9 . . ? C47 C48 H48A 109.9 . . ? O2 C48 H48B 109.9 . . ? C47 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? O2 C49 C50 109.2(3) . . ? O2 C49 H49A 109.8 . . ? C50 C49 H49A 109.8 . . ? O2 C49 H49B 109.8 . . ? C50 C49 H49B 109.8 . . ? H49A C49 H49B 108.3 . . ? O1 C50 C49 109.1(3) . . ? O1 C50 H50A 109.9 . . ? C49 C50 H50A 109.9 . . ? O1 C50 H50B 109.9 . . ? C49 C50 H50B 109.9 . . ? H50A C50 H50B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 30.75 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.668 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.097 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.161 0.461 0.041 4392 581 ' ' _platon_squeeze_details ? #===END data_Gd2-biph-crown2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H157 Fe2 Gd2 K2 N4 O15 Si4' _chemical_formula_weight 2175.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _space_group_name_Hall 'P 2ac 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 17.518(4) _cell_length_b 22.148(5) _cell_length_c 34.963(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13565(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4524 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7259 _exptl_absorpt_correction_T_max 0.8270 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 117257 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 28.31 _reflns_number_total 33574 _reflns_number_gt 27814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2, 2013' _computing_cell_refinement 'SAINT V8.32B (Bruker AXS Inc., 2013' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013' _computing_structure_solution 'SHELXS-2013 (Sheldrick 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+17.2609P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.011(8) _refine_ls_number_reflns 33574 _refine_ls_number_parameters 1090 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1455 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.262022(15) 0.727355(12) 0.685211(7) 0.02516(6) Uani 1 1 d . . . Gd2 Gd 0.238713(14) 0.737680(11) 0.805115(6) 0.02341(6) Uani 1 1 d . . . Fe1 Fe 0.38631(4) 0.69341(3) 0.61892(2) 0.02437(16) Uani 1 1 d . . . Fe2 Fe 0.12560(4) 0.70513(3) 0.87525(2) 0.02652(17) Uani 1 1 d . . . K1 K 0.29540(7) 0.64970(6) 0.41709(4) 0.0334(3) Uani 1 1 d . . . K2 K 0.27088(7) 0.36401(5) 0.57487(3) 0.0312(2) Uani 1 1 d . . . Si1 Si 0.25936(9) 0.87765(6) 0.63273(4) 0.0270(3) Uani 1 1 d . . . Si2 Si 0.13501(9) 0.65792(8) 0.60731(5) 0.0322(3) Uani 1 1 d . . . Si3 Si 0.24938(9) 0.88785(6) 0.85740(4) 0.0279(3) Uani 1 1 d . . . Si4 Si 0.38819(8) 0.68451(7) 0.87325(4) 0.0256(3) Uani 1 1 d . . . N1 N 0.2965(3) 0.8102(2) 0.64504(13) 0.0285(10) Uani 1 1 d . . . N2 N 0.2108(3) 0.6584(2) 0.63793(13) 0.0314(11) Uani 1 1 d . . . N3 N 0.2047(3) 0.8237(2) 0.84282(14) 0.0294(10) Uani 1 1 d . . . N4 N 0.2997(3) 0.6795(2) 0.85310(14) 0.0316(11) Uani 1 1 d . . . O1 O 0.1445(3) 0.6781(2) 0.43476(12) 0.0437(11) Uani 1 1 d . . . O2 O 0.2634(3) 0.7257(2) 0.48096(11) 0.0455(10) Uani 1 1 d . . . O3 O 0.4147(3) 0.7025(2) 0.45950(13) 0.0476(12) Uani 1 1 d . . . O4 O 0.4450(2) 0.6029(2) 0.41163(15) 0.0420(11) Uani 1 1 d . . . O5 O 0.3294(3) 0.56942(19) 0.35936(13) 0.0395(10) Uani 1 1 d . . . O6 O 0.1780(2) 0.58286(19) 0.38425(12) 0.0382(10) Uani 1 1 d . . . O7 O 0.1629(2) 0.43281(19) 0.61308(12) 0.0355(9) Uani 1 1 d . . . O8 O 0.3167(2) 0.43089(19) 0.63876(12) 0.0357(9) Uani 1 1 d . . . O9 O 0.4268(2) 0.3880(2) 0.58637(13) 0.0418(11) Uani 1 1 d . . . O10 O 0.3814(3) 0.2932(2) 0.53630(13) 0.0452(11) Uani 1 1 d . . . O11 O 0.2233(3) 0.2897(2) 0.51307(11) 0.0431(11) Uani 1 1 d . . . O12 O 0.1132(2) 0.3455(2) 0.56266(12) 0.0390(10) Uani 1 1 d . . . O13 O 0.2794(4) 0.7387(3) 0.36599(18) 0.0779(18) Uani 1 1 d . . . O15 O 0.2485(3) 0.2532(2) 0.60889(13) 0.0547(12) Uani 1 1 d . . . O16 O 0.2991(3) 0.4423(2) 0.51609(14) 0.0533(13) Uani 1 1 d . . . C1 C 0.3231(4) 0.7014(3) 0.74744(16) 0.0300(13) Uani 1 1 d . . . H1A H 0.3709 0.6812 0.7462 0.036 Uiso 1 1 calc R . . C2 C 0.3199(3) 0.7682(3) 0.74954(15) 0.0307(12) Uani 1 1 d . . . H2A H 0.3650 0.7904 0.7550 0.037 Uiso 1 1 calc R . . C3 C 0.2492(3) 0.7996(2) 0.74345(13) 0.0267(12) Uani 1 1 d . . . H3A H 0.2484 0.8425 0.7426 0.032 Uiso 1 1 calc R . . C4 C 0.1788(3) 0.7655(3) 0.73862(15) 0.0256(11) Uani 1 1 d . . . H4A H 0.1331 0.7855 0.7313 0.031 Uiso 1 1 calc R . . C5 C 0.1789(3) 0.7006(3) 0.74504(16) 0.0282(13) Uani 1 1 d . . . H5A H 0.1317 0.6799 0.7478 0.034 Uiso 1 1 calc R . . C6 C 0.2513(2) 0.6664(2) 0.74726(11) 0.0193(10) Uani 1 1 d . . . C7 C 0.2513(3) 0.6004(3) 0.74798(11) 0.0269(12) Uani 1 1 d . . . C8 C 0.1847(4) 0.5650(3) 0.74623(16) 0.0314(13) Uani 1 1 d . . . H8A H 0.1366 0.5846 0.7448 0.038 Uiso 1 1 calc R . . C9 C 0.1867(4) 0.5029(3) 0.74654(18) 0.0394(15) Uani 1 1 d . . . H9A H 0.1400 0.4812 0.7457 0.047 Uiso 1 1 calc R . . C10 C 0.2552(4) 0.4707(3) 0.74808(16) 0.0489(19) Uani 1 1 d . . . H10A H 0.2558 0.4278 0.7479 0.059 Uiso 1 1 calc R . . C11 C 0.3234(5) 0.5044(3) 0.74989(18) 0.0453(17) Uani 1 1 d . . . H11A H 0.3709 0.4839 0.7512 0.054 Uiso 1 1 calc R . . C12 C 0.3222(4) 0.5675(3) 0.74981(15) 0.0310(13) Uani 1 1 d . . . H12A H 0.3690 0.5891 0.7510 0.037 Uiso 1 1 calc R . . C13 C 0.2438(4) 0.8888(3) 0.57961(16) 0.0406(14) Uani 1 1 d . . . H13A H 0.2115 0.8562 0.5697 0.061 Uiso 1 1 calc R . . H13B H 0.2932 0.8882 0.5664 0.061 Uiso 1 1 calc R . . H13C H 0.2187 0.9277 0.5752 0.061 Uiso 1 1 calc R . . C14 C 0.1641(3) 0.8854(3) 0.65722(19) 0.0377(14) Uani 1 1 d . . . H14A H 0.1309 0.8519 0.6496 0.057 Uiso 1 1 calc R . . H14B H 0.1404 0.9238 0.6498 0.057 Uiso 1 1 calc R . . H14C H 0.1714 0.8846 0.6850 0.057 Uiso 1 1 calc R . . C15 C 0.3239(4) 0.9430(3) 0.6482(2) 0.0384(14) Uani 1 1 d . . . C16 C 0.4030(4) 0.9356(3) 0.6300(3) 0.052(2) Uani 1 1 d . . . H16A H 0.4358 0.9692 0.6378 0.078 Uiso 1 1 calc R . . H16B H 0.3979 0.9354 0.6021 0.078 Uiso 1 1 calc R . . H16C H 0.4257 0.8974 0.6385 0.078 Uiso 1 1 calc R . . C17 C 0.2922(4) 1.0037(3) 0.6373(2) 0.0543(19) Uani 1 1 d . . . H17A H 0.3271 1.0355 0.6460 0.081 Uiso 1 1 calc R . . H17B H 0.2422 1.0093 0.6493 0.081 Uiso 1 1 calc R . . H17C H 0.2868 1.0060 0.6094 0.081 Uiso 1 1 calc R . . C18 C 0.3339(5) 0.9394(4) 0.6923(2) 0.059(2) Uani 1 1 d . . . H18A H 0.3662 0.9728 0.7009 0.089 Uiso 1 1 calc R . . H18B H 0.3579 0.9009 0.6991 0.089 Uiso 1 1 calc R . . H18C H 0.2838 0.9422 0.7046 0.089 Uiso 1 1 calc R . . C19 C 0.1335(4) 0.7266(3) 0.57524(15) 0.0355(13) Uani 1 1 d . . . H19A H 0.1809 0.7283 0.5604 0.053 Uiso 1 1 calc R . . H19B H 0.1290 0.7631 0.5909 0.053 Uiso 1 1 calc R . . H19C H 0.0899 0.7240 0.5578 0.053 Uiso 1 1 calc R . . C20 C 0.1323(4) 0.5890(3) 0.57458(19) 0.0400(14) Uani 1 1 d . . . H20A H 0.1795 0.5872 0.5596 0.060 Uiso 1 1 calc R . . H20B H 0.0884 0.5922 0.5573 0.060 Uiso 1 1 calc R . . H20C H 0.1275 0.5524 0.5901 0.060 Uiso 1 1 calc R . . C21 C 0.0422(3) 0.6571(3) 0.63557(18) 0.0376(14) Uani 1 1 d . . . C22 C -0.0264(4) 0.6548(4) 0.6089(2) 0.0525(19) Uani 1 1 d . . . H22A H -0.0735 0.6548 0.6240 0.079 Uiso 1 1 calc R . . H22B H -0.0240 0.6180 0.5934 0.079 Uiso 1 1 calc R . . H22C H -0.0258 0.6902 0.5921 0.079 Uiso 1 1 calc R . . C23 C 0.0405(4) 0.6009(3) 0.6616(2) 0.0437(16) Uani 1 1 d . . . H23A H -0.0073 0.6002 0.6761 0.066 Uiso 1 1 calc R . . H23B H 0.0838 0.6023 0.6793 0.066 Uiso 1 1 calc R . . H23C H 0.0441 0.5644 0.6458 0.066 Uiso 1 1 calc R . . C24 C 0.0381(3) 0.7149(3) 0.66103(18) 0.0377(14) Uani 1 1 d . . . H24A H -0.0099 0.7150 0.6754 0.057 Uiso 1 1 calc R . . H24B H 0.0405 0.7509 0.6447 0.057 Uiso 1 1 calc R . . H24C H 0.0812 0.7152 0.6789 0.057 Uiso 1 1 calc R . . C25 C 0.3409(4) 0.8948(3) 0.8298(2) 0.0519(19) Uani 1 1 d . . . H25A H 0.3298 0.8940 0.8023 0.078 Uiso 1 1 calc R . . H25B H 0.3747 0.8611 0.8363 0.078 Uiso 1 1 calc R . . H25C H 0.3660 0.9330 0.8363 0.078 Uiso 1 1 calc R . . C26 C 0.2766(5) 0.8891(3) 0.9098(2) 0.064(2) Uani 1 1 d . . . H26A H 0.3068 0.8531 0.9159 0.096 Uiso 1 1 calc R . . H26B H 0.2302 0.8895 0.9255 0.096 Uiso 1 1 calc R . . H26C H 0.3068 0.9254 0.9152 0.096 Uiso 1 1 calc R . . C27 C 0.1905(4) 0.9581(3) 0.8481(2) 0.0454(17) Uani 1 1 d . . . C28 C 0.1793(5) 0.9654(4) 0.8042(3) 0.077(3) Uani 1 1 d . . . H28A H 0.1493 1.0019 0.7991 0.116 Uiso 1 1 calc R . . H28B H 0.1523 0.9301 0.7941 0.116 Uiso 1 1 calc R . . H28C H 0.2293 0.9690 0.7918 0.116 Uiso 1 1 calc R . . C29 C 0.2290(5) 1.0154(3) 0.8639(3) 0.079(3) Uani 1 1 d . . . H29A H 0.1970 1.0506 0.8583 0.118 Uiso 1 1 calc R . . H29B H 0.2791 1.0205 0.8518 0.118 Uiso 1 1 calc R . . H29C H 0.2355 1.0115 0.8916 0.118 Uiso 1 1 calc R . . C30 C 0.1123(4) 0.9514(3) 0.8679(3) 0.071(3) Uani 1 1 d . . . H30A H 0.0817 0.9876 0.8631 0.106 Uiso 1 1 calc R . . H30B H 0.1198 0.9463 0.8954 0.106 Uiso 1 1 calc R . . H30C H 0.0858 0.9160 0.8576 0.106 Uiso 1 1 calc R . . C31 C 0.4490(3) 0.7323(3) 0.84129(17) 0.0364(13) Uani 1 1 d . . . H31A H 0.4263 0.7725 0.8389 0.055 Uiso 1 1 calc R . . H31B H 0.4523 0.7135 0.8160 0.055 Uiso 1 1 calc R . . H31C H 0.5003 0.7358 0.8523 0.055 Uiso 1 1 calc R . . C32 C 0.3894(4) 0.7188(3) 0.92260(16) 0.0412(15) Uani 1 1 d . . . H32A H 0.3640 0.7582 0.9220 0.062 Uiso 1 1 calc R . . H32B H 0.4423 0.7240 0.9311 0.062 Uiso 1 1 calc R . . H32C H 0.3625 0.6921 0.9404 0.062 Uiso 1 1 calc R . . C33 C 0.4376(3) 0.6077(3) 0.87710(18) 0.0317(12) Uani 1 1 d . . . C34 C 0.4396(4) 0.5791(3) 0.83747(19) 0.0467(16) Uani 1 1 d . . . H34A H 0.4653 0.5398 0.8389 0.070 Uiso 1 1 calc R . . H34B H 0.4674 0.6055 0.8199 0.070 Uiso 1 1 calc R . . H34C H 0.3873 0.5734 0.8282 0.070 Uiso 1 1 calc R . . C35 C 0.5187(4) 0.6140(3) 0.8917(2) 0.0489(17) Uani 1 1 d . . . H35A H 0.5430 0.5742 0.8926 0.073 Uiso 1 1 calc R . . H35B H 0.5180 0.6315 0.9175 0.073 Uiso 1 1 calc R . . H35C H 0.5477 0.6405 0.8746 0.073 Uiso 1 1 calc R . . C36 C 0.3915(4) 0.5676(3) 0.9051(2) 0.0463(17) Uani 1 1 d . . . H36A H 0.4157 0.5278 0.9071 0.069 Uiso 1 1 calc R . . H36B H 0.3392 0.5629 0.8957 0.069 Uiso 1 1 calc R . . H36C H 0.3905 0.5867 0.9304 0.069 Uiso 1 1 calc R . . C37 C 0.1316(4) 0.7041(4) 0.47088(19) 0.0500(19) Uani 1 1 d . . . H37A H 0.1359 0.6729 0.4911 0.060 Uiso 1 1 calc R . . H37B H 0.0795 0.7215 0.4719 0.060 Uiso 1 1 calc R . . C38 C 0.1900(5) 0.7529(4) 0.47735(19) 0.058(2) Uani 1 1 d . . . H38A H 0.1899 0.7814 0.4556 0.069 Uiso 1 1 calc R . . H38B H 0.1776 0.7757 0.5009 0.069 Uiso 1 1 calc R . . C39 C 0.3233(5) 0.7686(4) 0.4852(2) 0.061(2) Uani 1 1 d . . . H39A H 0.3120 0.7960 0.5069 0.074 Uiso 1 1 calc R . . H39B H 0.3281 0.7931 0.4617 0.074 Uiso 1 1 calc R . . C40 C 0.3959(5) 0.7350(4) 0.49259(19) 0.063(2) Uani 1 1 d . . . H40A H 0.4373 0.7636 0.4990 0.075 Uiso 1 1 calc R . . H40B H 0.3891 0.7070 0.5144 0.075 Uiso 1 1 calc R . . C41 C 0.4804(4) 0.6652(4) 0.4649(2) 0.053(2) Uani 1 1 d . . . H41A H 0.4683 0.6316 0.4825 0.064 Uiso 1 1 calc R . . H41B H 0.5226 0.6892 0.4760 0.064 Uiso 1 1 calc R . . C42 C 0.5034(4) 0.6409(3) 0.4266(2) 0.0500(18) Uani 1 1 d . . . H42A H 0.5128 0.6747 0.4087 0.060 Uiso 1 1 calc R . . H42B H 0.5514 0.6176 0.4292 0.060 Uiso 1 1 calc R . . C44 C 0.3998(4) 0.5409(3) 0.3605(2) 0.0507(19) Uani 1 1 d . . . H44A H 0.4124 0.5247 0.3349 0.061 Uiso 1 1 calc R . . H44B H 0.3978 0.5066 0.3787 0.061 Uiso 1 1 calc R . . C45 C 0.2713(4) 0.5284(3) 0.34911(17) 0.0398(14) Uani 1 1 d . . . H45A H 0.2681 0.4957 0.3684 0.048 Uiso 1 1 calc R . . H45B H 0.2833 0.5098 0.3240 0.048 Uiso 1 1 calc R . . C46 C 0.1972(4) 0.5608(3) 0.34687(19) 0.0435(16) Uani 1 1 d . . . H46A H 0.2012 0.5950 0.3287 0.052 Uiso 1 1 calc R . . H46B H 0.1568 0.5331 0.3376 0.052 Uiso 1 1 calc R . . C47 C 0.1049(4) 0.6110(3) 0.3858(2) 0.0497(18) Uani 1 1 d . . . H47A H 0.0648 0.5820 0.3780 0.060 Uiso 1 1 calc R . . H47B H 0.1033 0.6458 0.3680 0.060 Uiso 1 1 calc R . . C48 C 0.0909(4) 0.6320(4) 0.4258(2) 0.0529(19) Uani 1 1 d . . . H48A H 0.0383 0.6479 0.4282 0.063 Uiso 1 1 calc R . . H48B H 0.0967 0.5978 0.4438 0.063 Uiso 1 1 calc R . . C49 C 0.1853(4) 0.4544(3) 0.65035(19) 0.0396(15) Uani 1 1 d . . . H49A H 0.1838 0.4210 0.6691 0.047 Uiso 1 1 calc R . . H49B H 0.1498 0.4864 0.6590 0.047 Uiso 1 1 calc R . . C50 C 0.2650(4) 0.4791(3) 0.64721(17) 0.0384(13) Uani 1 1 d . . . H50A H 0.2672 0.5098 0.6267 0.046 Uiso 1 1 calc R . . H50B H 0.2798 0.4987 0.6716 0.046 Uiso 1 1 calc R . . C51 C 0.3922(4) 0.4512(3) 0.6383(2) 0.0456(16) Uani 1 1 d . . . H51A H 0.4070 0.4649 0.6642 0.055 Uiso 1 1 calc R . . H51B H 0.3968 0.4860 0.6206 0.055 Uiso 1 1 calc R . . C52 C 0.4444(4) 0.4016(3) 0.6256(2) 0.0467(17) Uani 1 1 d . . . H52A H 0.4983 0.4146 0.6279 0.056 Uiso 1 1 calc R . . H52B H 0.4368 0.3654 0.6417 0.056 Uiso 1 1 calc R . . C53 C 0.4784(4) 0.3442(4) 0.5709(2) 0.0496(18) Uani 1 1 d . . . H53A H 0.4806 0.3085 0.5879 0.060 Uiso 1 1 calc R . . H53B H 0.5303 0.3616 0.5691 0.060 Uiso 1 1 calc R . . C54 C 0.4512(4) 0.3261(4) 0.5323(2) 0.054(2) Uani 1 1 d . . . H54A H 0.4427 0.3624 0.5164 0.064 Uiso 1 1 calc R . . H54B H 0.4900 0.3006 0.5196 0.064 Uiso 1 1 calc R . . C55 C 0.3545(5) 0.2688(5) 0.50101(19) 0.067(3) Uani 1 1 d . . . H55A H 0.3896 0.2367 0.4921 0.080 Uiso 1 1 calc R . . H55B H 0.3528 0.3009 0.4813 0.080 Uiso 1 1 calc R . . C56 C 0.2756(5) 0.2428(4) 0.5068(2) 0.058(2) Uani 1 1 d . . . H56A H 0.2604 0.2195 0.4839 0.069 Uiso 1 1 calc R . . H56B H 0.2758 0.2152 0.5290 0.069 Uiso 1 1 calc R . . C57 C 0.1486(4) 0.2669(3) 0.52091(18) 0.0477(17) Uani 1 1 d . . . H57A H 0.1497 0.2412 0.5441 0.057 Uiso 1 1 calc R . . H57B H 0.1305 0.2421 0.4992 0.057 Uiso 1 1 calc R . . C58 C 0.0956(4) 0.3194(3) 0.52703(17) 0.0443(17) Uani 1 1 d . . . H58A H 0.1023 0.3495 0.5064 0.053 Uiso 1 1 calc R . . H58B H 0.0419 0.3055 0.5268 0.053 Uiso 1 1 calc R . . C59 C 0.0664(4) 0.3948(3) 0.5722(2) 0.0446(16) Uani 1 1 d . . . H59A H 0.0120 0.3829 0.5704 0.054 Uiso 1 1 calc R . . H59B H 0.0755 0.4284 0.5541 0.054 Uiso 1 1 calc R . . C60 C 0.0842(4) 0.4146(3) 0.61176(18) 0.0390(14) Uani 1 1 d . . . H60A H 0.0509 0.4487 0.6191 0.047 Uiso 1 1 calc R . . H60B H 0.0753 0.3810 0.6299 0.047 Uiso 1 1 calc R . . C61 C 0.3642(3) 0.7860(3) 0.63210(17) 0.0374(14) Uani 1 1 d . . . C62 C 0.3876(3) 0.7757(2) 0.59239(16) 0.0316(12) Uani 1 1 d . . . H62A H 0.3583 0.7854 0.5703 0.038 Uiso 1 1 calc R . . C63 C 0.4614(4) 0.7489(3) 0.59234(18) 0.0379(14) Uani 1 1 d . . . H63A H 0.4904 0.7392 0.5702 0.045 Uiso 1 1 calc R . . C64 C 0.4849(3) 0.7387(3) 0.63095(18) 0.0364(13) Uani 1 1 d . . . H64A H 0.5311 0.7207 0.6393 0.044 Uiso 1 1 calc R . . C65 C 0.4242(3) 0.7615(3) 0.65444(16) 0.0295(11) Uani 1 1 d . . . H65A H 0.4242 0.7603 0.6816 0.035 Uiso 1 1 calc R . . C66 C 0.2835(3) 0.6405(2) 0.62468(15) 0.0278(12) Uani 1 1 d . . . C67 C 0.3148(3) 0.6403(3) 0.58642(15) 0.0304(12) Uani 1 1 d . . . H67A H 0.2894 0.6542 0.5641 0.036 Uiso 1 1 calc R . . C68 C 0.3891(3) 0.6163(3) 0.58767(16) 0.0319(12) Uani 1 1 d . . . H68A H 0.4210 0.6088 0.5662 0.038 Uiso 1 1 calc R . . C69 C 0.4083(4) 0.6051(3) 0.62613(17) 0.0331(13) Uani 1 1 d . . . H69A H 0.4559 0.5904 0.6351 0.040 Uiso 1 1 calc R . . C70 C 0.3428(3) 0.6199(2) 0.64965(16) 0.0287(12) Uani 1 1 d . . . H70A H 0.3398 0.6165 0.6767 0.034 Uiso 1 1 calc R . . C71 C 0.1407(3) 0.7987(3) 0.85859(16) 0.0301(12) Uani 1 1 d . . . C72 C 0.0817(3) 0.7686(3) 0.83717(17) 0.0319(12) Uani 1 1 d . . . H72A H 0.0812 0.7646 0.8101 0.038 Uiso 1 1 calc R . . C73 C 0.0239(3) 0.7456(3) 0.8623(2) 0.0444(16) Uani 1 1 d . . . H73A H -0.0212 0.7247 0.8551 0.053 Uiso 1 1 calc R . . C74 C 0.0476(4) 0.7602(3) 0.9000(2) 0.0466(17) Uani 1 1 d . . . H74A H 0.0192 0.7513 0.9224 0.056 Uiso 1 1 calc R . . C75 C 0.1194(4) 0.7899(3) 0.89961(17) 0.0373(14) Uani 1 1 d . . . H75A H 0.1483 0.8020 0.9213 0.045 Uiso 1 1 calc R . . C76 C 0.2330(4) 0.6579(2) 0.86909(14) 0.0293(11) Uani 1 1 d . . . C77 C 0.1715(3) 0.6303(2) 0.84640(16) 0.0283(12) Uani 1 1 d . . . H77A H 0.1724 0.6232 0.8196 0.034 Uiso 1 1 calc R . . C78 C 0.1106(3) 0.6161(3) 0.87157(18) 0.0346(13) Uani 1 1 d . . . H78A H 0.0633 0.5986 0.8641 0.041 Uiso 1 1 calc R . . C79 C 0.1307(4) 0.6317(3) 0.90914(17) 0.0378(15) Uani 1 1 d . . . H79A H 0.1009 0.6251 0.9314 0.045 Uiso 1 1 calc R . . C80 C 0.2050(4) 0.6594(3) 0.90772(18) 0.0361(13) Uani 1 1 d . . . H80A H 0.2314 0.6761 0.9290 0.043 Uiso 1 1 calc R . . C81 C 0.3112(5) 0.7355(4) 0.3288(3) 0.075(3) Uani 1 1 d . . . H81A H 0.2897 0.7010 0.3143 0.090 Uiso 1 1 calc R . . H81B H 0.3674 0.7311 0.3300 0.090 Uiso 1 1 calc R . . C82 C 0.2894(5) 0.7945(4) 0.3104(3) 0.076(3) Uani 1 1 d . . . H82A H 0.3308 0.8246 0.3131 0.091 Uiso 1 1 calc R . . H82B H 0.2778 0.7890 0.2829 0.091 Uiso 1 1 calc R . . C83 C 0.2202(6) 0.8135(4) 0.3320(3) 0.082(3) Uani 1 1 d . . . H83A H 0.1812 0.8403 0.3237 0.098 Uiso 1 1 calc R . . C84 C 0.2247(8) 0.7842(6) 0.3663(4) 0.144(7) Uani 1 1 d . . . H84A H 0.1743 0.7665 0.3725 0.172 Uiso 1 1 calc R . . H84B H 0.2374 0.8137 0.3866 0.172 Uiso 1 1 calc R . . C85 C 0.2410(5) 0.4533(3) 0.4875(2) 0.0553(18) Uani 1 1 d . . . H85A H 0.1910 0.4614 0.4997 0.066 Uiso 1 1 calc R . . H85B H 0.2357 0.4181 0.4702 0.066 Uiso 1 1 calc R . . C86 C 0.2679(7) 0.5062(4) 0.4666(3) 0.099(4) Uani 1 1 d . . . H86A H 0.2953 0.4934 0.4432 0.118 Uiso 1 1 calc R . . H86B H 0.2240 0.5316 0.4588 0.118 Uiso 1 1 calc R . . C87 C 0.3187(5) 0.5405(4) 0.4910(2) 0.057(2) Uani 1 1 d . . . H87A H 0.2929 0.5770 0.5011 0.068 Uiso 1 1 calc R . . H87B H 0.3652 0.5529 0.4770 0.068 Uiso 1 1 calc R . . C88 C 0.3380(6) 0.4964(4) 0.5232(3) 0.076(3) Uani 1 1 d . . . H88A H 0.3937 0.4890 0.5239 0.092 Uiso 1 1 calc R . . H88B H 0.3221 0.5133 0.5481 0.092 Uiso 1 1 calc R . . C89 C 0.1959(4) 0.2562(5) 0.6404(2) 0.071(3) Uani 1 1 d . . . H89A H 0.1723 0.2967 0.6420 0.085 Uiso 1 1 calc R . . H89B H 0.1550 0.2257 0.6374 0.085 Uiso 1 1 calc R . . C90 C 0.2396(6) 0.2442(6) 0.6734(3) 0.104(4) Uani 1 1 d . . . H90A H 0.2083 0.2230 0.6928 0.125 Uiso 1 1 calc R . . H90B H 0.2584 0.2824 0.6847 0.125 Uiso 1 1 calc R . . C91 C 0.3048(6) 0.2059(5) 0.6615(2) 0.078(3) Uani 1 1 d . . . H91A H 0.3514 0.2157 0.6763 0.093 Uiso 1 1 calc R . . H91B H 0.2928 0.1625 0.6647 0.093 Uiso 1 1 calc R . . C92 C 0.3139(5) 0.2213(5) 0.6214(2) 0.080(3) Uani 1 1 d . . . H92A H 0.3600 0.2466 0.6180 0.096 Uiso 1 1 calc R . . H92B H 0.3202 0.1841 0.6061 0.096 Uiso 1 1 calc R . . C93 C 0.4607(4) 0.5849(4) 0.3729(2) 0.056(2) Uani 1 1 d . . . H93A H 0.5115 0.5656 0.3714 0.067 Uiso 1 1 calc R . . H93B H 0.4605 0.6207 0.3559 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02079(11) 0.03275(13) 0.02194(11) 0.00055(9) -0.00095(9) -0.00179(11) Gd2 0.01993(11) 0.02759(12) 0.02272(11) -0.00087(9) -0.00132(9) 0.00047(10) Fe1 0.0260(4) 0.0235(4) 0.0235(4) -0.0042(3) 0.0028(3) -0.0034(3) Fe2 0.0255(4) 0.0190(4) 0.0350(4) 0.0000(3) 0.0095(3) 0.0010(3) K1 0.0332(6) 0.0343(7) 0.0327(6) -0.0060(5) -0.0038(5) 0.0060(5) K2 0.0315(6) 0.0340(6) 0.0282(5) 0.0001(5) -0.0001(5) -0.0020(5) Si1 0.0230(7) 0.0292(7) 0.0289(7) 0.0023(5) 0.0002(6) -0.0012(6) Si2 0.0285(8) 0.0361(9) 0.0319(8) 0.0018(7) -0.0064(6) -0.0038(7) Si3 0.0272(9) 0.0232(6) 0.0334(7) -0.0024(5) -0.0044(6) -0.0021(6) Si4 0.0266(7) 0.0258(7) 0.0246(7) 0.0001(6) -0.0043(6) -0.0015(6) N1 0.025(2) 0.033(3) 0.028(2) -0.0023(19) 0.0011(18) 0.0003(19) N2 0.027(2) 0.039(3) 0.028(2) 0.002(2) -0.0051(19) -0.009(2) N3 0.027(2) 0.021(2) 0.040(3) -0.0072(19) 0.004(2) -0.0048(18) N4 0.023(2) 0.040(3) 0.031(2) 0.004(2) 0.0015(19) 0.006(2) O1 0.039(2) 0.057(3) 0.035(2) 0.003(2) -0.0012(19) 0.010(2) O2 0.057(3) 0.044(2) 0.036(2) -0.0042(18) -0.006(2) 0.013(3) O3 0.054(3) 0.045(3) 0.044(3) 0.000(2) -0.007(2) -0.010(2) O4 0.026(2) 0.033(2) 0.067(3) 0.006(2) 0.006(2) -0.0059(18) O5 0.043(3) 0.024(2) 0.050(3) -0.0048(19) 0.012(2) -0.0026(19) O6 0.036(2) 0.036(2) 0.042(2) 0.0018(19) -0.0101(19) 0.0041(19) O7 0.030(2) 0.039(2) 0.037(2) -0.0056(18) 0.0026(17) -0.0032(18) O8 0.038(2) 0.031(2) 0.038(2) 0.0004(18) -0.0072(18) -0.0034(18) O9 0.031(2) 0.052(3) 0.042(3) 0.005(2) -0.0088(19) 0.010(2) O10 0.047(3) 0.049(3) 0.040(2) 0.000(2) 0.001(2) 0.012(2) O11 0.057(3) 0.041(2) 0.031(2) -0.0031(18) 0.004(2) -0.005(2) O12 0.034(2) 0.052(3) 0.031(2) -0.0045(19) -0.0026(17) -0.010(2) O13 0.080(4) 0.078(4) 0.076(4) 0.029(3) 0.007(3) 0.027(3) O15 0.050(3) 0.063(3) 0.050(3) 0.018(2) 0.005(2) 0.016(3) O16 0.069(3) 0.039(3) 0.051(3) 0.011(2) -0.023(3) -0.012(2) C1 0.032(3) 0.034(3) 0.024(3) 0.000(2) -0.010(2) 0.000(2) C2 0.013(2) 0.044(3) 0.035(3) -0.011(3) -0.0036(19) -0.007(2) C3 0.032(4) 0.027(2) 0.021(2) 0.0000(18) 0.001(2) -0.002(2) C4 0.016(2) 0.030(3) 0.031(3) 0.002(2) 0.0013(19) 0.002(2) C5 0.029(3) 0.027(3) 0.028(3) -0.004(2) -0.015(2) -0.003(2) C6 0.016(3) 0.030(2) 0.0116(19) 0.0019(16) -0.0021(17) -0.0021(19) C7 0.032(3) 0.041(3) 0.0079(19) 0.0007(17) -0.0052(19) 0.006(2) C8 0.038(3) 0.031(3) 0.025(3) -0.002(2) -0.006(2) -0.009(2) C9 0.060(4) 0.026(3) 0.032(3) -0.005(3) -0.001(3) -0.011(3) C10 0.079(6) 0.031(3) 0.037(3) 0.000(2) 0.001(4) 0.002(3) C11 0.071(5) 0.039(4) 0.025(3) 0.005(3) -0.003(3) 0.024(3) C12 0.037(3) 0.035(3) 0.021(3) -0.002(2) -0.002(2) 0.007(3) C13 0.044(4) 0.042(3) 0.035(3) 0.009(2) -0.001(3) -0.003(3) C14 0.021(3) 0.039(3) 0.052(4) 0.000(3) -0.003(3) 0.006(2) C15 0.036(3) 0.025(3) 0.054(4) -0.008(3) 0.009(3) -0.003(2) C16 0.029(3) 0.030(3) 0.097(6) -0.013(4) 0.009(4) -0.008(3) C17 0.046(4) 0.033(4) 0.084(6) -0.005(4) 0.011(4) 0.001(3) C18 0.063(5) 0.056(5) 0.059(5) -0.014(4) -0.006(4) -0.015(4) C19 0.047(3) 0.035(3) 0.025(3) 0.007(2) 0.002(2) 0.008(3) C20 0.035(3) 0.042(3) 0.043(3) -0.012(3) -0.009(3) 0.001(3) C21 0.028(3) 0.045(4) 0.039(3) -0.005(3) 0.000(2) -0.002(3) C22 0.025(3) 0.080(5) 0.053(4) -0.001(4) -0.010(3) -0.008(3) C23 0.036(3) 0.046(4) 0.049(4) 0.009(3) 0.007(3) -0.010(3) C24 0.029(3) 0.044(4) 0.039(3) -0.011(3) -0.002(2) 0.005(3) C25 0.032(3) 0.039(4) 0.085(6) -0.012(4) 0.009(3) -0.011(3) C26 0.102(7) 0.040(4) 0.049(4) 0.004(3) -0.030(4) -0.022(4) C27 0.030(3) 0.029(3) 0.077(5) 0.010(3) 0.000(3) 0.001(3) C28 0.063(5) 0.084(6) 0.085(6) 0.049(5) -0.023(5) 0.000(5) C29 0.050(5) 0.027(3) 0.159(9) 0.000(4) -0.002(6) 0.007(3) C30 0.045(4) 0.021(3) 0.147(9) -0.005(4) 0.026(5) 0.008(3) C31 0.032(3) 0.040(3) 0.037(3) 0.010(3) -0.001(2) -0.005(3) C32 0.059(4) 0.035(3) 0.030(3) -0.007(2) 0.004(3) -0.011(3) C33 0.026(3) 0.027(3) 0.043(3) 0.000(2) -0.005(2) -0.001(2) C34 0.054(4) 0.042(4) 0.044(4) -0.008(3) -0.002(3) 0.011(3) C35 0.027(3) 0.057(4) 0.063(5) 0.004(4) -0.014(3) 0.004(3) C36 0.055(4) 0.026(3) 0.057(4) 0.014(3) -0.013(3) -0.005(3) C37 0.048(4) 0.067(5) 0.036(3) 0.000(3) 0.010(3) 0.032(4) C38 0.091(6) 0.055(5) 0.028(3) 0.002(3) 0.009(3) 0.036(4) C39 0.089(6) 0.049(4) 0.047(4) -0.012(4) -0.006(4) -0.015(4) C40 0.070(5) 0.087(6) 0.031(3) -0.011(4) -0.011(3) -0.022(5) C41 0.044(4) 0.064(5) 0.051(4) 0.021(4) -0.016(3) -0.024(4) C42 0.025(3) 0.050(4) 0.074(5) 0.010(4) 0.003(3) -0.012(3) C44 0.040(4) 0.034(3) 0.078(5) -0.009(3) 0.030(4) 0.001(3) C45 0.054(4) 0.031(3) 0.035(3) -0.009(2) 0.002(3) 0.000(3) C46 0.055(4) 0.039(4) 0.037(3) -0.006(3) -0.011(3) -0.006(3) C47 0.036(4) 0.047(4) 0.067(5) 0.003(3) -0.014(3) 0.012(3) C48 0.033(3) 0.062(5) 0.064(5) 0.017(4) 0.013(3) 0.019(3) C49 0.044(4) 0.033(3) 0.041(4) -0.009(3) 0.002(3) 0.002(3) C50 0.047(3) 0.033(3) 0.035(3) -0.008(2) -0.005(3) -0.004(3) C51 0.040(4) 0.047(4) 0.050(4) 0.001(3) -0.018(3) -0.006(3) C52 0.036(3) 0.045(4) 0.059(4) 0.003(3) -0.015(3) 0.002(3) C53 0.032(3) 0.064(5) 0.053(4) 0.003(4) -0.006(3) 0.019(3) C54 0.048(4) 0.065(5) 0.048(4) 0.011(4) 0.006(3) 0.028(4) C55 0.065(5) 0.109(7) 0.026(3) -0.033(4) 0.000(3) 0.025(5) C56 0.078(6) 0.058(4) 0.036(3) -0.013(3) 0.006(3) 0.003(4) C57 0.063(4) 0.050(4) 0.030(3) 0.006(3) -0.007(3) -0.028(4) C58 0.049(4) 0.057(4) 0.027(3) 0.003(3) -0.004(3) -0.030(3) C59 0.028(3) 0.055(4) 0.051(4) 0.003(3) -0.001(3) -0.008(3) C60 0.032(3) 0.043(4) 0.042(4) 0.000(3) 0.003(3) 0.002(3) C61 0.029(3) 0.051(4) 0.032(3) 0.002(3) 0.004(2) -0.004(3) C62 0.037(3) 0.023(3) 0.035(3) 0.000(2) 0.006(2) -0.008(2) C63 0.038(3) 0.031(3) 0.045(3) -0.003(3) 0.019(3) -0.009(2) C64 0.021(2) 0.038(3) 0.050(3) -0.009(3) 0.008(2) -0.002(2) C65 0.025(3) 0.029(3) 0.035(3) 0.000(2) 0.001(2) -0.008(2) C66 0.031(3) 0.031(3) 0.022(2) -0.002(2) 0.000(2) -0.011(2) C67 0.038(3) 0.030(3) 0.023(3) -0.009(2) -0.007(2) -0.010(2) C68 0.036(3) 0.034(3) 0.026(3) -0.007(2) 0.004(2) -0.003(2) C69 0.038(3) 0.028(3) 0.034(3) -0.002(2) 0.006(2) -0.001(2) C70 0.031(3) 0.028(3) 0.027(3) 0.002(2) -0.002(2) -0.004(2) C71 0.028(3) 0.026(3) 0.036(3) 0.005(2) 0.008(2) 0.000(2) C72 0.025(3) 0.025(3) 0.046(3) 0.001(3) 0.004(2) 0.004(2) C73 0.018(3) 0.034(3) 0.081(5) -0.007(3) 0.009(3) 0.001(2) C74 0.049(4) 0.023(3) 0.067(5) 0.003(3) 0.034(3) 0.007(3) C75 0.048(4) 0.029(3) 0.035(3) -0.005(2) 0.013(3) 0.008(3) C76 0.042(3) 0.027(2) 0.018(2) 0.0017(19) 0.002(2) 0.012(3) C77 0.038(3) 0.020(3) 0.027(3) -0.004(2) 0.007(2) 0.005(2) C78 0.030(3) 0.023(3) 0.050(4) -0.001(3) 0.012(3) -0.003(2) C79 0.056(4) 0.023(3) 0.034(3) 0.008(2) 0.024(3) 0.003(3) C80 0.040(3) 0.033(3) 0.035(3) 0.008(3) 0.006(3) 0.010(3) C81 0.068(6) 0.076(6) 0.082(6) 0.009(5) 0.033(5) 0.008(5) C82 0.075(6) 0.081(6) 0.072(6) 0.034(5) 0.013(5) 0.000(5) C83 0.110(8) 0.062(5) 0.072(6) 0.005(5) -0.010(6) 0.031(6) C84 0.158(13) 0.153(12) 0.120(10) 0.074(9) 0.067(9) 0.114(11) C85 0.062(5) 0.047(4) 0.057(4) 0.000(3) -0.016(4) -0.009(4) C86 0.136(10) 0.065(6) 0.095(7) 0.047(5) -0.050(7) -0.033(6) C87 0.066(5) 0.053(5) 0.050(4) -0.002(4) 0.000(4) -0.022(4) C88 0.088(7) 0.052(5) 0.089(6) 0.019(4) -0.044(5) -0.037(5) C89 0.040(4) 0.104(8) 0.068(5) 0.024(5) 0.019(4) 0.018(4) C90 0.070(6) 0.184(12) 0.058(5) -0.004(6) 0.009(5) 0.054(8) C91 0.076(6) 0.100(7) 0.058(5) 0.011(5) 0.005(4) 0.041(6) C92 0.060(5) 0.111(8) 0.068(5) 0.036(5) 0.006(4) 0.049(5) C93 0.038(4) 0.055(4) 0.074(5) -0.013(4) 0.026(4) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N1 2.388(5) . ? Gd1 N2 2.423(5) . ? Gd1 C1 2.492(5) . ? Gd1 C4 2.515(5) . ? Gd1 C6 2.562(4) . ? Gd1 C3 2.599(5) . ? Gd1 C5 2.617(6) . ? Gd1 C2 2.627(5) . ? Gd1 C66 2.884(5) . ? Gd1 C61 2.888(6) . ? Gd1 C70 3.035(6) . ? Gd1 Fe1 3.2677(9) . ? Gd2 N4 2.369(5) . ? Gd2 N3 2.391(4) . ? Gd2 C5 2.487(5) . ? Gd2 C2 2.500(6) . ? Gd2 C3 2.562(5) . ? Gd2 C6 2.575(4) . ? Gd2 C4 2.624(5) . ? Gd2 C1 2.627(6) . ? Gd2 C76 2.852(5) . ? Gd2 C71 2.876(6) . ? Gd2 C77 3.021(5) . ? Gd2 C72 3.047(5) . ? Fe1 C69 2.009(6) . ? Fe1 C63 2.026(6) . ? Fe1 C68 2.029(6) . ? Fe1 C64 2.042(6) . ? Fe1 C62 2.046(6) . ? Fe1 C67 2.060(5) . ? Fe1 C65 2.064(6) . ? Fe1 C70 2.094(6) . ? Fe1 C61 2.138(7) . ? Fe1 C66 2.158(5) . ? Fe2 C78 1.994(6) . ? Fe2 C79 2.015(6) . ? Fe2 C74 2.026(6) . ? Fe2 C73 2.045(6) . ? Fe2 C80 2.061(6) . ? Fe2 C75 2.065(6) . ? Fe2 C72 2.083(6) . ? Fe2 C77 2.101(5) . ? Fe2 C76 2.164(6) . ? Fe2 C71 2.169(6) . ? K1 O13 2.675(6) . ? K1 O5 2.755(4) . ? K1 O6 2.782(4) . ? K1 O1 2.786(5) . ? K1 O3 2.817(5) . ? K1 O4 2.825(5) . ? K1 O2 2.852(4) . ? K2 O16 2.734(5) . ? K2 O15 2.755(5) . ? K2 O7 2.772(4) . ? K2 O8 2.798(4) . ? K2 O9 2.811(5) . ? K2 O12 2.825(4) . ? K2 O10 2.833(5) . ? K2 O11 2.841(4) . ? Si1 N1 1.686(5) . ? Si1 C14 1.884(6) . ? Si1 C13 1.893(6) . ? Si1 C15 1.914(6) . ? Si2 N2 1.706(5) . ? Si2 C19 1.890(6) . ? Si2 C21 1.903(6) . ? Si2 C20 1.908(6) . ? Si3 N3 1.701(5) . ? Si3 C25 1.878(7) . ? Si3 C27 1.894(6) . ? Si3 C26 1.895(7) . ? Si4 N4 1.707(5) . ? Si4 C31 1.872(6) . ? Si4 C32 1.885(6) . ? Si4 C33 1.912(6) . ? N1 C61 1.378(7) . ? N2 C66 1.411(7) . ? N3 C71 1.367(7) . ? N4 C76 1.380(8) . ? O1 C37 1.406(8) . ? O1 C48 1.422(9) . ? O2 C39 1.423(9) . ? O2 C38 1.426(9) . ? O3 C40 1.401(9) . ? O3 C41 1.428(9) . ? O4 C42 1.424(8) . ? O4 C93 1.438(9) . ? O5 C44 1.387(8) . ? O5 C45 1.411(8) . ? O6 C47 1.426(7) . ? O6 C46 1.435(8) . ? O7 C60 1.438(7) . ? O7 C49 1.442(7) . ? O8 C51 1.397(8) . ? O8 C50 1.431(7) . ? O9 C53 1.432(8) . ? O9 C52 1.437(8) . ? O10 C55 1.427(8) . ? O10 C54 1.430(9) . ? O11 C56 1.402(9) . ? O11 C57 1.428(8) . ? O12 C59 1.405(8) . ? O12 C58 1.407(7) . ? O13 C84 1.391(11) . ? O13 C81 1.418(10) . ? O15 C92 1.415(8) . ? O15 C89 1.439(8) . ? O16 C88 1.400(9) . ? O16 C85 1.447(8) . ? C1 C6 1.478(7) . ? C1 C2 1.483(8) . ? C1 H1A 0.9500 . ? C2 C3 1.437(8) . ? C2 H2A 0.9500 . ? C3 C4 1.455(7) . ? C3 H3A 0.9500 . ? C4 C5 1.455(8) . ? C4 H4A 0.9500 . ? C5 C6 1.479(7) . ? C5 H5A 0.9500 . ? C6 C7 1.461(8) . ? C7 C8 1.408(8) . ? C7 C12 1.442(8) . ? C8 C9 1.376(8) . ? C8 H8A 0.9500 . ? C9 C10 1.395(10) . ? C9 H9A 0.9500 . ? C10 C11 1.410(11) . ? C10 H10A 0.9500 . ? C11 C12 1.397(9) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.506(9) . ? C15 C16 1.534(9) . ? C15 C18 1.552(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.522(8) . ? C21 C23 1.542(9) . ? C21 C24 1.561(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.541(10) . ? C27 C30 1.540(10) . ? C27 C28 1.555(11) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.517(8) . ? C33 C34 1.524(9) . ? C33 C36 1.551(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.506(12) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.496(12) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.498(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C44 C93 1.508(10) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.486(10) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.494(11) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.504(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.497(10) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.486(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.510(12) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.503(11) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.485(9) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C65 1.417(8) . ? C61 C62 1.465(8) . ? C62 C63 1.424(9) . ? C62 H62A 0.9500 . ? C63 C64 1.429(9) . ? C63 H63A 0.9500 . ? C64 C65 1.435(8) . ? C64 H64A 0.9500 . ? C65 H65A 0.9500 . ? C66 C70 1.432(8) . ? C66 C67 1.446(7) . ? C67 C68 1.407(8) . ? C67 H67A 0.9500 . ? C68 C69 1.407(8) . ? C68 H68A 0.9500 . ? C69 C70 1.448(8) . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? C71 C72 1.439(8) . ? C71 C75 1.495(8) . ? C72 C73 1.434(8) . ? C72 H72A 0.9500 . ? C73 C74 1.419(10) . ? C73 H73A 0.9500 . ? C74 C75 1.420(9) . ? C74 H74A 0.9500 . ? C75 H75A 0.9500 . ? C76 C80 1.438(7) . ? C76 C77 1.471(8) . ? C77 C78 1.419(8) . ? C77 H77A 0.9500 . ? C78 C79 1.404(9) . ? C78 H78A 0.9500 . ? C79 C80 1.440(9) . ? C79 H79A 0.9500 . ? C80 H80A 0.9500 . ? C81 C82 1.505(12) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.490(13) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.366(13) . ? C83 H83A 0.9500 . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.461(10) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C87 1.447(12) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.529(11) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.410(12) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 C91 1.482(12) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.452(11) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Gd1 N2 100.15(16) . . ? N1 Gd1 C1 125.63(18) . . ? N2 Gd1 C1 127.52(18) . . ? N1 Gd1 C4 108.97(17) . . ? N2 Gd1 C4 120.27(17) . . ? C1 Gd1 C4 71.23(19) . . ? N1 Gd1 C6 157.14(15) . . ? N2 Gd1 C6 102.62(16) . . ? C1 Gd1 C6 33.97(16) . . ? C4 Gd1 C6 60.38(17) . . ? N1 Gd1 C3 90.57(16) . . ? N2 Gd1 C3 152.94(16) . . ? C1 Gd1 C3 59.70(18) . . ? C4 Gd1 C3 33.00(16) . . ? C6 Gd1 C3 69.79(15) . . ? N1 Gd1 C5 141.69(17) . . ? N2 Gd1 C5 101.36(16) . . ? C1 Gd1 C5 59.3(2) . . ? C4 Gd1 C5 32.86(17) . . ? C6 Gd1 C5 33.17(16) . . ? C3 Gd1 C5 57.64(16) . . ? N1 Gd1 C2 98.16(18) . . ? N2 Gd1 C2 160.70(18) . . ? C1 Gd1 C2 33.54(19) . . ? C4 Gd1 C2 58.15(17) . . ? C6 Gd1 C2 58.99(17) . . ? C3 Gd1 C2 31.90(17) . . ? C5 Gd1 C2 66.93(16) . . ? N1 Gd1 C66 92.73(15) . . ? N2 Gd1 C66 29.21(16) . . ? C1 Gd1 C66 115.51(18) . . ? C4 Gd1 C66 147.61(16) . . ? C6 Gd1 C66 106.23(15) . . ? C3 Gd1 C66 175.21(16) . . ? C5 Gd1 C66 120.54(16) . . ? C2 Gd1 C66 143.84(17) . . ? N1 Gd1 C61 28.31(17) . . ? N2 Gd1 C61 94.27(17) . . ? C1 Gd1 C61 113.51(19) . . ? C4 Gd1 C61 133.26(19) . . ? C6 Gd1 C61 145.79(16) . . ? C3 Gd1 C61 106.28(17) . . ? C5 Gd1 C61 163.89(17) . . ? C2 Gd1 C61 99.00(17) . . ? C66 Gd1 C61 75.38(17) . . ? N1 Gd1 C70 104.09(15) . . ? N2 Gd1 C70 53.04(16) . . ? C1 Gd1 C70 88.64(18) . . ? C4 Gd1 C70 146.92(17) . . ? C6 Gd1 C70 88.18(15) . . ? C3 Gd1 C70 147.55(16) . . ? C5 Gd1 C70 114.19(16) . . ? C2 Gd1 C70 116.14(17) . . ? C66 Gd1 C70 27.86(15) . . ? C61 Gd1 C70 78.48(17) . . ? N1 Gd1 Fe1 65.86(11) . . ? N2 Gd1 Fe1 67.51(12) . . ? C1 Gd1 Fe1 106.26(15) . . ? C4 Gd1 Fe1 171.91(12) . . ? C6 Gd1 Fe1 121.90(11) . . ? C3 Gd1 Fe1 139.02(11) . . ? C5 Gd1 Fe1 152.35(13) . . ? C2 Gd1 Fe1 115.43(12) . . ? C66 Gd1 Fe1 40.48(10) . . ? C61 Gd1 Fe1 40.04(13) . . ? C70 Gd1 Fe1 38.58(10) . . ? N4 Gd2 N3 98.90(17) . . ? N4 Gd2 C5 127.49(18) . . ? N3 Gd2 C5 128.58(18) . . ? N4 Gd2 C2 116.16(17) . . ? N3 Gd2 C2 110.78(18) . . ? C5 Gd2 C2 70.88(18) . . ? N4 Gd2 C3 148.73(16) . . ? N3 Gd2 C3 93.18(17) . . ? C5 Gd2 C3 59.73(17) . . ? C2 Gd2 C3 32.95(17) . . ? N4 Gd2 C6 100.63(16) . . ? N3 Gd2 C6 160.46(16) . . ? C5 Gd2 C6 33.92(17) . . ? C2 Gd2 C6 60.44(16) . . ? C3 Gd2 C6 70.18(15) . . ? N4 Gd2 C4 159.27(17) . . ? N3 Gd2 C4 101.64(17) . . ? C5 Gd2 C4 32.93(17) . . ? C2 Gd2 C4 58.36(17) . . ? C3 Gd2 C4 32.56(15) . . ? C6 Gd2 C4 58.82(16) . . ? N4 Gd2 C1 97.09(17) . . ? N3 Gd2 C1 143.82(17) . . ? C5 Gd2 C1 59.2(2) . . ? C2 Gd2 C1 33.50(19) . . ? C3 Gd2 C1 58.50(17) . . ? C6 Gd2 C1 32.99(15) . . ? C4 Gd2 C1 67.47(16) . . ? N4 Gd2 C76 28.80(17) . . ? N3 Gd2 C76 93.00(15) . . ? C5 Gd2 C76 116.31(18) . . ? C2 Gd2 C76 142.80(18) . . ? C3 Gd2 C76 173.80(15) . . ? C6 Gd2 C76 103.84(15) . . ? C4 Gd2 C76 145.73(17) . . ? C1 Gd2 C76 115.60(17) . . ? N4 Gd2 C71 93.68(16) . . ? N3 Gd2 C71 28.21(15) . . ? C5 Gd2 C71 116.90(19) . . ? C2 Gd2 C71 135.87(18) . . ? C3 Gd2 C71 109.77(16) . . ? C6 Gd2 C71 148.17(15) . . ? C4 Gd2 C71 103.11(16) . . ? C1 Gd2 C71 168.26(17) . . ? C76 Gd2 C71 76.14(16) . . ? N4 Gd2 C77 53.79(17) . . ? N3 Gd2 C77 105.46(15) . . ? C5 Gd2 C77 88.83(17) . . ? C2 Gd2 C77 143.65(17) . . ? C3 Gd2 C77 148.37(16) . . ? C6 Gd2 C77 85.75(14) . . ? C4 Gd2 C77 116.91(16) . . ? C1 Gd2 C77 110.18(16) . . ? C76 Gd2 C77 28.82(17) . . ? C71 Gd2 C77 80.02(15) . . ? N4 Gd2 C72 105.57(16) . . ? N3 Gd2 C72 52.68(16) . . ? C5 Gd2 C72 90.25(19) . . ? C2 Gd2 C72 137.57(17) . . ? C3 Gd2 C72 104.70(16) . . ? C6 Gd2 C72 120.24(15) . . ? C4 Gd2 C72 84.96(16) . . ? C1 Gd2 C72 149.21(17) . . ? C76 Gd2 C72 79.59(17) . . ? C71 Gd2 C72 27.93(16) . . ? C77 Gd2 C72 69.49(15) . . ? C69 Fe1 C63 121.6(2) . . ? C69 Fe1 C68 40.8(2) . . ? C63 Fe1 C68 104.3(2) . . ? C69 Fe1 C64 106.9(3) . . ? C63 Fe1 C64 41.1(3) . . ? C68 Fe1 C64 120.3(2) . . ? C69 Fe1 C62 157.3(2) . . ? C63 Fe1 C62 40.9(2) . . ? C68 Fe1 C62 120.4(2) . . ? C64 Fe1 C62 69.3(3) . . ? C69 Fe1 C67 68.3(2) . . ? C63 Fe1 C67 119.2(2) . . ? C68 Fe1 C67 40.3(2) . . ? C64 Fe1 C67 155.3(2) . . ? C62 Fe1 C67 105.4(2) . . ? C69 Fe1 C65 125.1(2) . . ? C63 Fe1 C65 67.9(2) . . ? C68 Fe1 C65 158.8(2) . . ? C64 Fe1 C65 40.9(2) . . ? C62 Fe1 C65 67.5(2) . . ? C67 Fe1 C65 160.9(2) . . ? C69 Fe1 C70 41.3(2) . . ? C63 Fe1 C70 160.6(2) . . ? C68 Fe1 C70 68.3(2) . . ? C64 Fe1 C70 125.8(2) . . ? C62 Fe1 C70 158.3(2) . . ? C67 Fe1 C70 67.5(2) . . ? C65 Fe1 C70 112.1(2) . . ? C69 Fe1 C61 160.3(2) . . ? C63 Fe1 C61 68.6(2) . . ? C68 Fe1 C61 158.2(2) . . ? C64 Fe1 C61 68.7(2) . . ? C62 Fe1 C61 40.9(2) . . ? C67 Fe1 C61 123.8(2) . . ? C65 Fe1 C61 39.4(2) . . ? C70 Fe1 C61 124.7(2) . . ? C69 Fe1 C66 67.7(2) . . ? C63 Fe1 C66 156.1(2) . . ? C68 Fe1 C66 67.3(2) . . ? C64 Fe1 C66 162.5(2) . . ? C62 Fe1 C66 122.3(2) . . ? C67 Fe1 C66 40.0(2) . . ? C65 Fe1 C66 127.5(2) . . ? C70 Fe1 C66 39.3(2) . . ? C61 Fe1 C66 110.5(2) . . ? C69 Fe1 Gd1 105.22(17) . . ? C63 Fe1 Gd1 128.22(17) . . ? C68 Fe1 Gd1 126.30(17) . . ? C64 Fe1 Gd1 107.72(16) . . ? C62 Fe1 Gd1 97.10(16) . . ? C67 Fe1 Gd1 96.75(16) . . ? C65 Fe1 Gd1 67.61(15) . . ? C70 Fe1 Gd1 64.70(16) . . ? C61 Fe1 Gd1 60.38(16) . . ? C66 Fe1 Gd1 60.17(14) . . ? C78 Fe2 C79 41.0(3) . . ? C78 Fe2 C74 122.3(2) . . ? C79 Fe2 C74 105.4(2) . . ? C78 Fe2 C73 107.7(3) . . ? C79 Fe2 C73 121.5(3) . . ? C74 Fe2 C73 40.8(3) . . ? C78 Fe2 C80 68.8(3) . . ? C79 Fe2 C80 41.4(3) . . ? C74 Fe2 C80 121.1(3) . . ? C73 Fe2 C80 157.7(3) . . ? C78 Fe2 C75 156.8(2) . . ? C79 Fe2 C75 119.6(2) . . ? C74 Fe2 C75 40.6(3) . . ? C73 Fe2 C75 69.3(3) . . ? C80 Fe2 C75 104.8(3) . . ? C78 Fe2 C72 125.3(3) . . ? C79 Fe2 C72 159.6(3) . . ? C74 Fe2 C72 67.5(3) . . ? C73 Fe2 C72 40.7(2) . . ? C80 Fe2 C72 158.8(2) . . ? C75 Fe2 C72 68.3(2) . . ? C78 Fe2 C77 40.4(2) . . ? C79 Fe2 C77 68.2(2) . . ? C74 Fe2 C77 159.8(3) . . ? C73 Fe2 C77 124.9(3) . . ? C80 Fe2 C77 67.6(2) . . ? C75 Fe2 C77 159.4(2) . . ? C72 Fe2 C77 111.5(2) . . ? C78 Fe2 C76 68.3(2) . . ? C79 Fe2 C76 68.2(2) . . ? C74 Fe2 C76 157.0(3) . . ? C73 Fe2 C76 161.3(3) . . ? C80 Fe2 C76 39.7(2) . . ? C75 Fe2 C76 121.8(3) . . ? C72 Fe2 C76 125.7(2) . . ? C77 Fe2 C76 40.3(2) . . ? C78 Fe2 C71 160.7(2) . . ? C79 Fe2 C71 157.5(3) . . ? C74 Fe2 C71 67.8(2) . . ? C73 Fe2 C71 68.2(2) . . ? C80 Fe2 C71 122.3(2) . . ? C75 Fe2 C71 41.3(2) . . ? C72 Fe2 C71 39.5(2) . . ? C77 Fe2 C71 125.3(2) . . ? C76 Fe2 C71 109.2(2) . . ? C78 Fe2 Gd2 104.63(17) . . ? C79 Fe2 Gd2 126.77(17) . . ? C74 Fe2 Gd2 127.08(18) . . ? C73 Fe2 Gd2 105.5(2) . . ? C80 Fe2 Gd2 96.52(17) . . ? C75 Fe2 Gd2 98.19(17) . . ? C72 Fe2 Gd2 65.85(15) . . ? C77 Fe2 Gd2 64.99(15) . . ? C76 Fe2 Gd2 59.96(13) . . ? C71 Fe2 Gd2 60.58(15) . . ? O13 K1 O5 90.51(18) . . ? O13 K1 O6 92.23(18) . . ? O5 K1 O6 60.92(14) . . ? O13 K1 O1 83.25(17) . . ? O5 K1 O1 120.87(14) . . ? O6 K1 O1 60.68(14) . . ? O13 K1 O3 97.09(19) . . ? O5 K1 O3 119.56(15) . . ? O6 K1 O3 170.65(14) . . ? O1 K1 O3 119.57(15) . . ? O13 K1 O4 108.82(17) . . ? O5 K1 O4 60.87(15) . . ? O6 K1 O4 117.57(14) . . ? O1 K1 O4 167.93(14) . . ? O3 K1 O4 59.97(15) . . ? O13 K1 O2 93.89(17) . . ? O5 K1 O2 175.55(14) . . ? O6 K1 O2 119.47(15) . . ? O1 K1 O2 60.45(14) . . ? O3 K1 O2 59.24(15) . . ? O4 K1 O2 116.85(15) . . ? O16 K2 O15 156.24(16) . . ? O16 K2 O7 97.88(16) . . ? O15 K2 O7 100.63(14) . . ? O16 K2 O8 102.26(14) . . ? O15 K2 O8 99.65(14) . . ? O7 K2 O8 61.30(13) . . ? O16 K2 O9 79.14(15) . . ? O15 K2 O9 104.19(14) . . ? O7 K2 O9 119.32(14) . . ? O8 K2 O9 60.45(14) . . ? O16 K2 O12 98.95(15) . . ? O15 K2 O12 78.27(14) . . ? O7 K2 O12 59.05(13) . . ? O8 K2 O12 118.56(13) . . ? O9 K2 O12 177.41(14) . . ? O16 K2 O10 82.51(16) . . ? O15 K2 O10 79.03(14) . . ? O7 K2 O10 179.58(14) . . ? O8 K2 O10 118.49(14) . . ? O9 K2 O10 60.60(14) . . ? O12 K2 O10 121.05(14) . . ? O16 K2 O11 81.31(14) . . ? O15 K2 O11 76.74(14) . . ? O7 K2 O11 119.01(14) . . ? O8 K2 O11 176.39(13) . . ? O9 K2 O11 120.23(14) . . ? O12 K2 O11 60.92(13) . . ? O10 K2 O11 61.17(14) . . ? N1 Si1 C14 107.8(3) . . ? N1 Si1 C13 114.9(3) . . ? C14 Si1 C13 107.9(3) . . ? N1 Si1 C15 111.7(3) . . ? C14 Si1 C15 109.0(3) . . ? C13 Si1 C15 105.3(3) . . ? N2 Si2 C19 112.2(3) . . ? N2 Si2 C21 109.9(3) . . ? C19 Si2 C21 107.7(3) . . ? N2 Si2 C20 113.6(3) . . ? C19 Si2 C20 106.7(3) . . ? C21 Si2 C20 106.4(3) . . ? N3 Si3 C25 107.9(3) . . ? N3 Si3 C27 112.6(3) . . ? C25 Si3 C27 108.0(3) . . ? N3 Si3 C26 114.7(3) . . ? C25 Si3 C26 106.4(4) . . ? C27 Si3 C26 106.9(4) . . ? N4 Si4 C31 107.9(3) . . ? N4 Si4 C32 114.4(3) . . ? C31 Si4 C32 108.2(3) . . ? N4 Si4 C33 112.5(3) . . ? C31 Si4 C33 106.7(3) . . ? C32 Si4 C33 106.8(3) . . ? C61 N1 Si1 126.3(4) . . ? C61 N1 Gd1 96.5(4) . . ? Si1 N1 Gd1 137.2(3) . . ? C66 N2 Si2 119.6(4) . . ? C66 N2 Gd1 93.9(3) . . ? Si2 N2 Gd1 136.1(3) . . ? C71 N3 Si3 126.5(4) . . ? C71 N3 Gd2 96.0(3) . . ? Si3 N3 Gd2 135.8(3) . . ? C76 N4 Si4 128.6(4) . . ? C76 N4 Gd2 95.4(3) . . ? Si4 N4 Gd2 131.8(3) . . ? C37 O1 C48 112.7(6) . . ? C37 O1 K1 116.4(4) . . ? C48 O1 K1 114.6(4) . . ? C39 O2 C38 113.0(6) . . ? C39 O2 K1 109.4(4) . . ? C38 O2 K1 110.9(4) . . ? C40 O3 C41 112.2(6) . . ? C40 O3 K1 118.2(4) . . ? C41 O3 K1 115.2(4) . . ? C42 O4 C93 111.9(5) . . ? C42 O4 K1 115.2(4) . . ? C93 O4 K1 110.0(4) . . ? C44 O5 C45 110.8(5) . . ? C44 O5 K1 117.7(4) . . ? C45 O5 K1 116.5(3) . . ? C47 O6 C46 113.2(5) . . ? C47 O6 K1 114.6(4) . . ? C46 O6 K1 112.6(4) . . ? C60 O7 C49 112.5(5) . . ? C60 O7 K2 119.0(3) . . ? C49 O7 K2 115.7(3) . . ? C51 O8 C50 111.1(5) . . ? C51 O8 K2 115.6(4) . . ? C50 O8 K2 112.2(3) . . ? C53 O9 C52 111.5(5) . . ? C53 O9 K2 115.5(4) . . ? C52 O9 K2 112.6(4) . . ? C55 O10 C54 113.1(6) . . ? C55 O10 K2 113.3(4) . . ? C54 O10 K2 110.4(4) . . ? C56 O11 C57 111.6(6) . . ? C56 O11 K2 110.9(4) . . ? C57 O11 K2 109.1(3) . . ? C59 O12 C58 113.6(5) . . ? C59 O12 K2 115.0(3) . . ? C58 O12 K2 114.1(4) . . ? C84 O13 C81 108.3(7) . . ? C84 O13 K1 127.0(6) . . ? C81 O13 K1 122.4(5) . . ? C92 O15 C89 107.7(5) . . ? C92 O15 K2 117.6(5) . . ? C89 O15 K2 112.4(5) . . ? C88 O16 C85 108.7(5) . . ? C88 O16 K2 119.9(5) . . ? C85 O16 K2 119.9(4) . . ? C6 C1 C2 119.4(5) . . ? C6 C1 Gd1 75.6(3) . . ? C2 C1 Gd1 78.3(3) . . ? C6 C1 Gd2 71.6(3) . . ? C2 C1 Gd2 68.6(3) . . ? Gd1 C1 Gd2 111.0(2) . . ? C6 C1 H1A 120.3 . . ? C2 C1 H1A 120.3 . . ? Gd1 C1 H1A 116.6 . . ? Gd2 C1 H1A 132.4 . . ? C3 C2 C1 120.6(5) . . ? C3 C2 Gd2 75.9(3) . . ? C1 C2 Gd2 77.9(4) . . ? C3 C2 Gd1 73.0(3) . . ? C1 C2 Gd1 68.2(3) . . ? Gd2 C2 Gd1 110.67(19) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? Gd2 C2 H2A 117.2 . . ? Gd1 C2 H2A 132.1 . . ? C2 C3 C4 119.7(5) . . ? C2 C3 Gd2 71.2(3) . . ? C4 C3 Gd2 76.1(3) . . ? C2 C3 Gd1 75.1(3) . . ? C4 C3 Gd1 70.3(3) . . ? Gd2 C3 Gd1 109.6(2) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? Gd2 C3 H3A 124.1 . . ? Gd1 C3 H3A 126.3 . . ? C5 C4 C3 119.6(5) . . ? C5 C4 Gd1 77.4(3) . . ? C3 C4 Gd1 76.7(3) . . ? C5 C4 Gd2 68.3(3) . . ? C3 C4 Gd2 71.4(3) . . ? Gd1 C4 Gd2 110.31(19) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? Gd1 C4 H4A 116.5 . . ? Gd2 C4 H4A 133.2 . . ? C4 C5 C6 121.0(5) . . ? C4 C5 Gd2 78.7(3) . . ? C6 C5 Gd2 76.3(3) . . ? C4 C5 Gd1 69.7(3) . . ? C6 C5 Gd1 71.4(3) . . ? Gd2 C5 Gd1 111.5(2) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? Gd2 C5 H5A 116.0 . . ? Gd1 C5 H5A 132.5 . . ? C7 C6 C1 121.5(4) . . ? C7 C6 C5 120.9(4) . . ? C1 C6 C5 117.5(5) . . ? C7 C6 Gd1 122.8(3) . . ? C1 C6 Gd1 70.4(3) . . ? C5 C6 Gd1 75.4(3) . . ? C7 C6 Gd2 126.8(3) . . ? C1 C6 Gd2 75.4(3) . . ? C5 C6 Gd2 69.8(3) . . ? Gd1 C6 Gd2 110.40(19) . . ? C8 C7 C12 115.7(5) . . ? C8 C7 C6 123.8(5) . . ? C12 C7 C6 120.5(5) . . ? C9 C8 C7 122.4(6) . . ? C9 C8 H8A 118.8 . . ? C7 C8 H8A 118.8 . . ? C8 C9 C10 122.2(6) . . ? C8 C9 H9A 118.9 . . ? C10 C9 H9A 118.9 . . ? C9 C10 C11 117.4(6) . . ? C9 C10 H10A 121.3 . . ? C11 C10 H10A 121.3 . . ? C12 C11 C10 121.2(7) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C11 C12 C7 121.2(6) . . ? C11 C12 H12A 119.4 . . ? C7 C12 H12A 119.4 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 108.8(6) . . ? C17 C15 C18 109.8(6) . . ? C16 C15 C18 107.8(6) . . ? C17 C15 Si1 112.7(5) . . ? C16 C15 Si1 109.6(4) . . ? C18 C15 Si1 108.0(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 108.7(6) . . ? C22 C21 C24 109.9(5) . . ? C23 C21 C24 109.0(5) . . ? C22 C21 Si2 110.9(4) . . ? C23 C21 Si2 109.2(4) . . ? C24 C21 Si2 109.1(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C30 107.9(7) . . ? C29 C27 C28 108.8(7) . . ? C30 C27 C28 109.9(7) . . ? C29 C27 Si3 112.1(5) . . ? C30 C27 Si3 109.2(5) . . ? C28 C27 Si3 108.9(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si4 C31 H31A 109.5 . . ? Si4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si4 C32 H32A 109.5 . . ? Si4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C34 108.9(6) . . ? C35 C33 C36 109.1(5) . . ? C34 C33 C36 110.4(5) . . ? C35 C33 Si4 111.5(4) . . ? C34 C33 Si4 108.5(4) . . ? C36 C33 Si4 108.6(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1 C37 C38 108.6(6) . . ? O1 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? O1 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.3 . . ? O2 C38 C37 108.8(6) . . ? O2 C38 H38A 109.9 . . ? C37 C38 H38A 109.9 . . ? O2 C38 H38B 109.9 . . ? C37 C38 H38B 109.9 . . ? H38A C38 H38B 108.3 . . ? O2 C39 C40 108.2(7) . . ? O2 C39 H39A 110.1 . . ? C40 C39 H39A 110.1 . . ? O2 C39 H39B 110.1 . . ? C40 C39 H39B 110.1 . . ? H39A C39 H39B 108.4 . . ? O3 C40 C39 108.3(6) . . ? O3 C40 H40A 110.0 . . ? C39 C40 H40A 110.0 . . ? O3 C40 H40B 110.0 . . ? C39 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? O3 C41 C42 107.9(6) . . ? O3 C41 H41A 110.1 . . ? C42 C41 H41A 110.1 . . ? O3 C41 H41B 110.1 . . ? C42 C41 H41B 110.1 . . ? H41A C41 H41B 108.4 . . ? O4 C42 C41 110.3(5) . . ? O4 C42 H42A 109.6 . . ? C41 C42 H42A 109.6 . . ? O4 C42 H42B 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? O5 C44 C93 110.0(5) . . ? O5 C44 H44A 109.7 . . ? C93 C44 H44A 109.7 . . ? O5 C44 H44B 109.7 . . ? C93 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? O5 C45 C46 109.4(5) . . ? O5 C45 H45A 109.8 . . ? C46 C45 H45A 109.8 . . ? O5 C45 H45B 109.8 . . ? C46 C45 H45B 109.8 . . ? H45A C45 H45B 108.3 . . ? O6 C46 C45 108.7(5) . . ? O6 C46 H46A 109.9 . . ? C45 C46 H46A 109.9 . . ? O6 C46 H46B 109.9 . . ? C45 C46 H46B 109.9 . . ? H46A C46 H46B 108.3 . . ? O6 C47 C48 108.5(5) . . ? O6 C47 H47A 110.0 . . ? C48 C47 H47A 110.0 . . ? O6 C47 H47B 110.0 . . ? C48 C47 H47B 110.0 . . ? H47A C47 H47B 108.4 . . ? O1 C48 C47 108.7(6) . . ? O1 C48 H48A 109.9 . . ? C47 C48 H48A 109.9 . . ? O1 C48 H48B 109.9 . . ? C47 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? O7 C49 C50 107.9(5) . . ? O7 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? O7 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? O8 C50 C49 109.3(5) . . ? O8 C50 H50A 109.8 . . ? C49 C50 H50A 109.8 . . ? O8 C50 H50B 109.8 . . ? C49 C50 H50B 109.8 . . ? H50A C50 H50B 108.3 . . ? O8 C51 C52 110.2(5) . . ? O8 C51 H51A 109.6 . . ? C52 C51 H51A 109.6 . . ? O8 C51 H51B 109.6 . . ? C52 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? O9 C52 C51 107.8(5) . . ? O9 C52 H52A 110.1 . . ? C51 C52 H52A 110.1 . . ? O9 C52 H52B 110.1 . . ? C51 C52 H52B 110.1 . . ? H52A C52 H52B 108.5 . . ? O9 C53 C54 108.8(5) . . ? O9 C53 H53A 109.9 . . ? C54 C53 H53A 109.9 . . ? O9 C53 H53B 109.9 . . ? C54 C53 H53B 109.9 . . ? H53A C53 H53B 108.3 . . ? O10 C54 C53 108.9(6) . . ? O10 C54 H54A 109.9 . . ? C53 C54 H54A 109.9 . . ? O10 C54 H54B 109.9 . . ? C53 C54 H54B 109.9 . . ? H54A C54 H54B 108.3 . . ? O10 C55 C56 109.3(6) . . ? O10 C55 H55A 109.8 . . ? C56 C55 H55A 109.8 . . ? O10 C55 H55B 109.8 . . ? C56 C55 H55B 109.8 . . ? H55A C55 H55B 108.3 . . ? O11 C56 C55 109.7(7) . . ? O11 C56 H56A 109.7 . . ? C55 C56 H56A 109.7 . . ? O11 C56 H56B 109.7 . . ? C55 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? O11 C57 C58 108.7(5) . . ? O11 C57 H57A 110.0 . . ? C58 C57 H57A 110.0 . . ? O11 C57 H57B 110.0 . . ? C58 C57 H57B 110.0 . . ? H57A C57 H57B 108.3 . . ? O12 C58 C57 107.9(5) . . ? O12 C58 H58A 110.1 . . ? C57 C58 H58A 110.1 . . ? O12 C58 H58B 110.1 . . ? C57 C58 H58B 110.1 . . ? H58A C58 H58B 108.4 . . ? O12 C59 C60 109.1(5) . . ? O12 C59 H59A 109.9 . . ? C60 C59 H59A 109.9 . . ? O12 C59 H59B 109.9 . . ? C60 C59 H59B 109.9 . . ? H59A C59 H59B 108.3 . . ? O7 C60 C59 108.3(5) . . ? O7 C60 H60A 110.0 . . ? C59 C60 H60A 110.0 . . ? O7 C60 H60B 110.0 . . ? C59 C60 H60B 110.0 . . ? H60A C60 H60B 108.4 . . ? N1 C61 C65 127.3(5) . . ? N1 C61 C62 127.7(6) . . ? C65 C61 C62 104.9(5) . . ? N1 C61 Fe1 126.8(4) . . ? C65 C61 Fe1 67.5(4) . . ? C62 C61 Fe1 66.2(3) . . ? N1 C61 Gd1 55.2(3) . . ? C65 C61 Gd1 86.2(3) . . ? C62 C61 Gd1 135.4(4) . . ? Fe1 C61 Gd1 79.57(19) . . ? C63 C62 C61 108.6(5) . . ? C63 C62 Fe1 68.8(3) . . ? C61 C62 Fe1 72.9(3) . . ? C63 C62 H62A 125.7 . . ? C61 C62 H62A 125.7 . . ? Fe1 C62 H62A 124.2 . . ? C62 C63 C64 109.0(5) . . ? C62 C63 Fe1 70.3(3) . . ? C64 C63 Fe1 70.0(3) . . ? C62 C63 H63A 125.5 . . ? C64 C63 H63A 125.5 . . ? Fe1 C63 H63A 125.8 . . ? C63 C64 C65 105.8(5) . . ? C63 C64 Fe1 68.8(3) . . ? C65 C64 Fe1 70.4(3) . . ? C63 C64 H64A 127.1 . . ? C65 C64 H64A 127.1 . . ? Fe1 C64 H64A 125.3 . . ? C61 C65 C64 111.6(5) . . ? C61 C65 Fe1 73.1(4) . . ? C64 C65 Fe1 68.7(3) . . ? C61 C65 H65A 124.2 . . ? C64 C65 H65A 124.2 . . ? Fe1 C65 H65A 125.5 . . ? N2 C66 C70 123.0(5) . . ? N2 C66 C67 130.3(5) . . ? C70 C66 C67 106.7(5) . . ? N2 C66 Fe1 129.1(4) . . ? C70 C66 Fe1 67.9(3) . . ? C67 C66 Fe1 66.3(3) . . ? N2 C66 Gd1 56.9(2) . . ? C70 C66 Gd1 81.9(3) . . ? C67 C66 Gd1 136.9(4) . . ? Fe1 C66 Gd1 79.35(16) . . ? C68 C67 C66 108.9(5) . . ? C68 C67 Fe1 68.7(3) . . ? C66 C67 Fe1 73.7(3) . . ? C68 C67 H67A 125.6 . . ? C66 C67 H67A 125.6 . . ? Fe1 C67 H67A 123.7 . . ? C67 C68 C69 108.4(5) . . ? C67 C68 Fe1 71.1(3) . . ? C69 C68 Fe1 68.8(3) . . ? C67 C68 H68A 125.8 . . ? C69 C68 H68A 125.8 . . ? Fe1 C68 H68A 125.9 . . ? C68 C69 C70 108.3(5) . . ? C68 C69 Fe1 70.4(3) . . ? C70 C69 Fe1 72.5(3) . . ? C68 C69 H69A 125.8 . . ? C70 C69 H69A 125.8 . . ? Fe1 C69 H69A 122.9 . . ? C66 C70 C69 107.5(5) . . ? C66 C70 Fe1 72.8(3) . . ? C69 C70 Fe1 66.2(3) . . ? C66 C70 Gd1 70.2(3) . . ? C69 C70 Gd1 141.2(4) . . ? Fe1 C70 Gd1 76.72(17) . . ? C66 C70 H70A 126.3 . . ? C69 C70 H70A 126.3 . . ? Fe1 C70 H70A 126.3 . . ? Gd1 C70 H70A 68.1 . . ? N3 C71 C72 124.5(5) . . ? N3 C71 C75 130.1(6) . . ? C72 C71 C75 105.1(5) . . ? N3 C71 Fe2 126.5(4) . . ? C72 C71 Fe2 67.0(3) . . ? C75 C71 Fe2 65.7(3) . . ? N3 C71 Gd2 55.8(3) . . ? C72 C71 Gd2 82.7(3) . . ? C75 C71 Gd2 135.4(4) . . ? Fe2 C71 Gd2 78.36(17) . . ? C73 C72 C71 110.7(6) . . ? C73 C72 Fe2 68.2(4) . . ? C71 C72 Fe2 73.5(3) . . ? C73 C72 Gd2 141.5(4) . . ? C71 C72 Gd2 69.4(3) . . ? Fe2 C72 Gd2 75.55(15) . . ? C73 C72 H72A 124.7 . . ? C71 C72 H72A 124.7 . . ? Fe2 C72 H72A 125.2 . . ? Gd2 C72 H72A 67.8 . . ? C74 C73 C72 106.3(5) . . ? C74 C73 Fe2 68.9(4) . . ? C72 C73 Fe2 71.1(3) . . ? C74 C73 H73A 126.8 . . ? C72 C73 H73A 126.8 . . ? Fe2 C73 H73A 124.8 . . ? C75 C74 C73 110.9(5) . . ? C75 C74 Fe2 71.2(3) . . ? C73 C74 Fe2 70.3(3) . . ? C75 C74 H74A 124.6 . . ? C73 C74 H74A 124.6 . . ? Fe2 C74 H74A 125.5 . . ? C74 C75 C71 106.9(6) . . ? C74 C75 Fe2 68.2(3) . . ? C71 C75 Fe2 73.1(3) . . ? C74 C75 H75A 126.6 . . ? C71 C75 H75A 126.6 . . ? Fe2 C75 H75A 123.8 . . ? N4 C76 C80 131.4(6) . . ? N4 C76 C77 123.1(5) . . ? C80 C76 C77 105.5(5) . . ? N4 C76 Fe2 127.5(4) . . ? C80 C76 Fe2 66.3(3) . . ? C77 C76 Fe2 67.5(3) . . ? N4 C76 Gd2 55.8(3) . . ? C80 C76 Gd2 137.2(4) . . ? C77 C76 Gd2 82.0(3) . . ? Fe2 C76 Gd2 78.99(15) . . ? C78 C77 C76 108.0(5) . . ? C78 C77 Fe2 65.8(3) . . ? C76 C77 Fe2 72.1(3) . . ? C78 C77 Gd2 139.8(4) . . ? C76 C77 Gd2 69.2(3) . . ? Fe2 C77 Gd2 75.95(16) . . ? C78 C77 H77A 126.0 . . ? C76 C77 H77A 126.0 . . ? Fe2 C77 H77A 127.6 . . ? Gd2 C77 H77A 69.6 . . ? C79 C78 C77 109.6(5) . . ? C79 C78 Fe2 70.3(3) . . ? C77 C78 Fe2 73.8(3) . . ? C79 C78 H78A 125.2 . . ? C77 C78 H78A 125.2 . . ? Fe2 C78 H78A 122.3 . . ? C78 C79 C80 107.5(5) . . ? C78 C79 Fe2 68.7(3) . . ? C80 C79 Fe2 71.1(3) . . ? C78 C79 H79A 126.3 . . ? C80 C79 H79A 126.3 . . ? Fe2 C79 H79A 125.5 . . ? C76 C80 C79 109.3(6) . . ? C76 C80 Fe2 74.0(3) . . ? C79 C80 Fe2 67.6(3) . . ? C76 C80 H80A 125.3 . . ? C79 C80 H80A 125.3 . . ? Fe2 C80 H80A 124.6 . . ? O13 C81 C82 104.4(7) . . ? O13 C81 H81A 110.9 . . ? C82 C81 H81A 110.9 . . ? O13 C81 H81B 110.9 . . ? C82 C81 H81B 110.9 . . ? H81A C81 H81B 108.9 . . ? C83 C82 C81 103.7(7) . . ? C83 C82 H82A 111.0 . . ? C81 C82 H82A 111.0 . . ? C83 C82 H82B 111.0 . . ? C81 C82 H82B 111.0 . . ? H82A C82 H82B 109.0 . . ? C84 C83 C82 105.2(8) . . ? C84 C83 H83A 127.4 . . ? C82 C83 H83A 127.4 . . ? C83 C84 O13 112.2(9) . . ? C83 C84 H84A 109.2 . . ? O13 C84 H84A 109.2 . . ? C83 C84 H84B 109.2 . . ? O13 C84 H84B 109.2 . . ? H84A C84 H84B 107.9 . . ? O16 C85 C86 104.7(7) . . ? O16 C85 H85A 110.8 . . ? C86 C85 H85A 110.8 . . ? O16 C85 H85B 110.8 . . ? C86 C85 H85B 110.8 . . ? H85A C85 H85B 108.9 . . ? C87 C86 C85 108.9(7) . . ? C87 C86 H86A 109.9 . . ? C85 C86 H86A 109.9 . . ? C87 C86 H86B 109.9 . . ? C85 C86 H86B 109.9 . . ? H86A C86 H86B 108.3 . . ? C86 C87 C88 103.6(6) . . ? C86 C87 H87A 111.1 . . ? C88 C87 H87A 111.0 . . ? C86 C87 H87B 111.0 . . ? C88 C87 H87B 111.0 . . ? H87A C87 H87B 109.0 . . ? O16 C88 C87 108.1(6) . . ? O16 C88 H88A 110.1 . . ? C87 C88 H88A 110.1 . . ? O16 C88 H88B 110.1 . . ? C87 C88 H88B 110.1 . . ? H88A C88 H88B 108.4 . . ? C90 C89 O15 105.7(6) . . ? C90 C89 H89A 110.6 . . ? O15 C89 H89A 110.6 . . ? C90 C89 H89B 110.6 . . ? O15 C89 H89B 110.6 . . ? H89A C89 H89B 108.7 . . ? C89 C90 C91 107.1(8) . . ? C89 C90 H90A 110.3 . . ? C91 C90 H90A 110.3 . . ? C89 C90 H90B 110.3 . . ? C91 C90 H90B 110.3 . . ? H90A C90 H90B 108.5 . . ? C92 C91 C90 102.8(7) . . ? C92 C91 H91A 111.2 . . ? C90 C91 H91A 111.2 . . ? C92 C91 H91B 111.2 . . ? C90 C91 H91B 111.2 . . ? H91A C91 H91B 109.1 . . ? O15 C92 C91 109.1(7) . . ? O15 C92 H92A 109.9 . . ? C91 C92 H92A 109.9 . . ? O15 C92 H92B 109.9 . . ? C91 C92 H92B 109.9 . . ? H92A C92 H92B 108.3 . . ? O4 C93 C44 108.4(5) . . ? O4 C93 H93A 110.0 . . ? C44 C93 H93A 110.0 . . ? O4 C93 H93B 110.0 . . ? C44 C93 H93B 110.0 . . ? H93A C93 H93B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 5.215 _refine_diff_density_min -1.886 _refine_diff_density_rms 0.142 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.327 -0.095 0.028 4232 621 ' ' _platon_squeeze_details ? #===END data_Er2-biph-crown2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Er2 Fe2 N4 Si4, 2(K C12 H24 O6), 10(C4 H8 O)' _chemical_formula_sum 'C120 H214 Er2 Fe2 K2 N4 O22 Si4' _chemical_formula_weight 2701.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 20 _space_group_name_H-M_alt 'C 2 2 21' _space_group_name_Hall 'C 2c 2' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 17.2570(19) _cell_length_b 22.701(3) _cell_length_c 34.573(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13544(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9175 _cell_measurement_theta_min 3.70 _cell_measurement_theta_max 28.09 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_F_000 5680 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.310 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.210 _exptl_absorpt_coefficient_mu 1.596 _shelx_estimated_absorpt_T_min 0.638 _shelx_estimated_absorpt_T_max 0.731 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.617 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed X-Ray Tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 76816 _diffrn_reflns_av_unetI/netI 0.0426 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 3.638 _diffrn_reflns_theta_max 28.295 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 16722 _reflns_number_gt 15396 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.863 _reflns_Friedel_fraction_max 0.993 _reflns_Friedel_fraction_full 0.995 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+6.5827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 6707 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.003(3) _chemical_absolute_configuration unk _refine_ls_number_reflns 16722 _refine_ls_number_parameters 785 _refine_ls_number_restraints 1143 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.52134(2) 0.23682(2) 0.30785(2) 0.02002(5) Uani 1 1 d . U . . . Fe1 Fe 0.64667(4) 0.19841(3) 0.37389(2) 0.02384(14) Uani 1 1 d . U . . . K1 K 0.56002(6) 0.14255(5) 0.57778(3) 0.0324(2) Uani 1 1 d . U . . . Si1 Si 0.38243(8) 0.18413(6) 0.37935(4) 0.0291(3) Uani 1 1 d . U . . . Si2 Si 0.53015(8) 0.38105(5) 0.35829(4) 0.0267(3) Uani 1 1 d . U . . . N1 N 0.4675(2) 0.17926(17) 0.35586(11) 0.0241(8) Uani 1 1 d . U . . . N2 N 0.5651(2) 0.31475(16) 0.34480(11) 0.0248(8) Uani 1 1 d . U . . . O1 O 0.6070(2) 0.06865(16) 0.63718(12) 0.0387(9) Uani 1 1 d . U . . . O2 O 0.4492(2) 0.07788(16) 0.61660(10) 0.0353(8) Uani 1 1 d . U . . . O3 O 0.4031(2) 0.16745(17) 0.56815(10) 0.0361(8) Uani 1 1 d . U . . . O4 O 0.5137(2) 0.21707(16) 0.51647(10) 0.0421(9) Uani 1 1 d . U . . . O5 O 0.6727(2) 0.20385(19) 0.53472(11) 0.0429(9) Uani 1 1 d . U . . . O6 O 0.7154(2) 0.10654(17) 0.58123(13) 0.0415(9) Uani 1 1 d . U . . . O8 O 0.5392(3) 0.2421(2) 0.61918(16) 0.0730(15) Uani 1 1 d D U . . . C31 C 0.4813(4) 0.2421(3) 0.6484(2) 0.0657(18) Uani 1 1 d D U . . . H31A H 0.4851 0.2060 0.6644 0.079 Uiso 1 1 calc R U . . . H31B H 0.4290 0.2437 0.6366 0.079 Uiso 1 1 calc R U . . . C32 C 0.4953(4) 0.2951(3) 0.6723(2) 0.070(2) Uani 1 1 d D U . . . H32A H 0.4543 0.3249 0.6680 0.084 Uiso 1 1 calc R U . . . H32B H 0.4968 0.2848 0.7001 0.084 Uiso 1 1 calc R U . . . C33 C 0.5710(6) 0.3170(4) 0.6591(3) 0.088(3) Uani 1 1 d D U . . . H33A H 0.5708 0.3606 0.6577 0.106 Uiso 1 1 calc R U . . . H33B H 0.6125 0.3045 0.6771 0.106 Uiso 1 1 calc R U . . . C34 C 0.5829(5) 0.2923(4) 0.6220(2) 0.076(2) Uani 1 1 d D U . . . H34A H 0.5671 0.3207 0.6017 0.091 Uiso 1 1 calc R U . . . H34B H 0.6384 0.2828 0.6183 0.091 Uiso 1 1 calc R U . . . O7 O 0.5729(6) 0.0537(4) 0.5204(3) 0.047(2) Uani 0.5 1 d D U P A -1 C35 C 0.5157(9) 0.0468(5) 0.4917(3) 0.050(3) Uani 0.5 1 d D U P A -1 H35A H 0.5173 0.0798 0.4730 0.060 Uiso 0.5 1 calc R U P A -1 H35B H 0.4634 0.0452 0.5035 0.060 Uiso 0.5 1 calc R U P A -1 C36 C 0.5340(13) -0.0079(7) 0.4729(5) 0.085(5) Uani 0.5 1 d D U P A -1 H36A H 0.4858 -0.0294 0.4665 0.102 Uiso 0.5 1 calc R U P A -1 H36B H 0.5627 -0.0003 0.4487 0.102 Uiso 0.5 1 calc R U P A -1 C37 C 0.5802(11) -0.0420(6) 0.4987(5) 0.063(4) Uani 0.5 1 d D U P A -1 H37A H 0.6275 -0.0564 0.4855 0.076 Uiso 0.5 1 calc R U P A -1 H37B H 0.5507 -0.0763 0.5084 0.076 Uiso 0.5 1 calc R U P A -1 C38 C 0.6003(10) -0.0026(5) 0.5302(4) 0.059(3) Uani 0.5 1 d D U P A -1 H38A H 0.5760 -0.0161 0.5545 0.071 Uiso 0.5 1 calc R U P A -1 H38B H 0.6572 -0.0017 0.5339 0.071 Uiso 0.5 1 calc R U P A -1 C1 C 0.5000 0.3013(3) 0.2500 0.0211(13) Uani 1 2 d S TU P . . H1A H 0.5000 0.3432 0.2500 0.025 Uiso 1 2 calc R U P . . C2 C 0.4299(2) 0.2704(2) 0.25926(12) 0.0226(9) Uani 1 1 d . U . . . H2A H 0.3861 0.2913 0.2686 0.027 Uiso 1 1 calc R U . . . C3 C 0.5735(3) 0.2059(2) 0.24588(13) 0.0252(10) Uani 1 1 d . U . . . H3A H 0.6221 0.1863 0.2466 0.030 Uiso 1 1 calc R U . . . C4 C 0.5000 0.1717(3) 0.2500 0.0227(14) Uani 1 2 d S TU P . . C5 C 0.5000 0.1084(3) 0.2500 0.0349(18) Uani 1 2 d S TU P . . C6 C 0.5691(5) 0.0751(2) 0.24539(16) 0.0506(17) Uani 1 1 d . U . . . H6A H 0.6172 0.0948 0.2424 0.061 Uiso 1 1 calc R U . . . C7 C 0.5670(6) 0.0136(3) 0.24520(17) 0.071(2) Uani 1 1 d . U . . . H7A H 0.6141 -0.0074 0.2416 0.085 Uiso 1 1 calc R U . . . C8 C 0.5000 -0.0176(4) 0.2500 0.074(3) Uani 1 2 d S TU P . . H8A H 0.5000 -0.0594 0.2500 0.089 Uiso 1 2 calc R U P . . C9 C 0.5370(3) 0.15528(19) 0.36977(13) 0.0230(9) Uani 1 1 d . U . . . C10 C 0.5688(3) 0.1545(2) 0.40819(14) 0.0302(10) Uani 1 1 d . U . . . H10A H 0.5450 0.1709 0.4305 0.036 Uiso 1 1 calc R U . . . C11 C 0.6415(3) 0.1253(2) 0.40749(16) 0.0346(11) Uani 1 1 d . U . . . H11A H 0.6732 0.1176 0.4294 0.042 Uiso 1 1 calc R U . . . C12 C 0.6592(3) 0.1095(2) 0.36836(16) 0.0340(11) Uani 1 1 d . U . . . H12A H 0.7048 0.0905 0.3594 0.041 Uiso 1 1 calc R U . . . C13 C 0.5945(3) 0.12815(19) 0.34549(15) 0.0267(10) Uani 1 1 d . U . . . H13A H 0.5902 0.1233 0.3183 0.032 Uiso 1 1 calc R U . . . C14 C 0.6326(3) 0.2890(2) 0.35875(14) 0.0258(9) Uani 1 1 d . U . . . C15 C 0.6574(3) 0.2805(2) 0.39836(15) 0.0325(11) Uani 1 1 d . U . . . H15A H 0.6307 0.2930 0.4209 0.039 Uiso 1 1 calc R U . . . C16 C 0.7305(3) 0.2493(2) 0.39726(17) 0.0378(12) Uani 1 1 d . U . . . H16A H 0.7610 0.2392 0.4191 0.045 Uiso 1 1 calc R U . . . C17 C 0.7491(3) 0.2363(3) 0.35844(17) 0.0373(11) Uani 1 1 d . U . . . H17A H 0.7939 0.2159 0.3497 0.045 Uiso 1 1 calc R U . . . C18 C 0.6888(3) 0.2593(2) 0.33469(15) 0.0293(9) Uani 1 1 d . U . . . H18A H 0.6860 0.2557 0.3073 0.035 Uiso 1 1 calc R U . . . C19 C 0.3871(4) 0.2209(3) 0.42741(17) 0.0565(18) Uani 1 1 d . U . . . H19A H 0.4166 0.2576 0.4252 0.085 Uiso 1 1 calc R U . . . H19B H 0.4125 0.1947 0.4460 0.085 Uiso 1 1 calc R U . . . H19C H 0.3344 0.2298 0.4363 0.085 Uiso 1 1 calc R U . . . C20 C 0.3142(3) 0.2282(2) 0.34844(15) 0.0358(12) Uani 1 1 d . U . . . H20A H 0.3354 0.2678 0.3445 0.054 Uiso 1 1 calc R U . . . H20B H 0.2637 0.2311 0.3613 0.054 Uiso 1 1 calc R U . . . H20C H 0.3079 0.2088 0.3233 0.054 Uiso 1 1 calc R U . . . C21 C 0.3367(3) 0.1079(3) 0.3866(2) 0.0522(16) Uani 1 1 d . U . . . C22 C 0.3877(4) 0.0724(3) 0.4152(2) 0.0576(18) Uani 1 1 d . U . . . H22A H 0.3672 0.0323 0.4176 0.086 Uiso 1 1 calc R U . . . H22B H 0.3871 0.0916 0.4406 0.086 Uiso 1 1 calc R U . . . H22C H 0.4410 0.0708 0.4055 0.086 Uiso 1 1 calc R U . . . C23 C 0.2652(10) 0.1210(9) 0.4165(7) 0.080(5) Uani 0.5 1 d . U P B 1 H23A H 0.2345 0.0851 0.4199 0.120 Uiso 0.5 1 calc R U P B 1 H23B H 0.2323 0.1522 0.4059 0.120 Uiso 0.5 1 calc R U P B 1 H23C H 0.2861 0.1335 0.4415 0.120 Uiso 0.5 1 calc R U P B 1 C23A C 0.2495(8) 0.1087(6) 0.3961(4) 0.041(3) Uani 0.5 1 d . U P B 2 H23D H 0.2344 0.0709 0.4075 0.062 Uiso 0.5 1 calc R U P B 2 H23E H 0.2198 0.1152 0.3723 0.062 Uiso 0.5 1 calc R U P B 2 H23F H 0.2386 0.1406 0.4144 0.062 Uiso 0.5 1 calc R U P B 2 C24 C 0.3342(5) 0.0767(3) 0.3470(3) 0.075(2) Uani 1 1 d . U . . . H24A H 0.3122 0.0372 0.3501 0.112 Uiso 1 1 calc R U . . . H24B H 0.3869 0.0735 0.3366 0.112 Uiso 1 1 calc R U . . . H24C H 0.3020 0.0995 0.3291 0.112 Uiso 1 1 calc R U . . . C25 C 0.5168(5) 0.3900(3) 0.41221(17) 0.0585(17) Uani 1 1 d . U . . . H25A H 0.4851 0.3575 0.4222 0.088 Uiso 1 1 calc R U . . . H25B H 0.4907 0.4275 0.4175 0.088 Uiso 1 1 calc R U . . . H25C H 0.5675 0.3896 0.4250 0.088 Uiso 1 1 calc R U . . . C26 C 0.4329(3) 0.3916(2) 0.33565(17) 0.0372(12) Uani 1 1 d . U . . . H26A H 0.4372 0.3868 0.3076 0.056 Uiso 1 1 calc R U . . . H26B H 0.4139 0.4313 0.3415 0.056 Uiso 1 1 calc R U . . . H26C H 0.3967 0.3624 0.3460 0.056 Uiso 1 1 calc R U . . . C27 C 0.5960(3) 0.4429(2) 0.34080(19) 0.0398(13) Uani 1 1 d . U . . . C28 C 0.6777(3) 0.4332(3) 0.3569(2) 0.0559(18) Uani 1 1 d . U . . . H28A H 0.7121 0.4645 0.3475 0.084 Uiso 1 1 calc R U . . . H28B H 0.6973 0.3949 0.3482 0.084 Uiso 1 1 calc R U . . . H28C H 0.6761 0.4340 0.3852 0.084 Uiso 1 1 calc R U . . . C29 C 0.5685(4) 0.5038(3) 0.3535(3) 0.064(2) Uani 1 1 d . U . . . H29A H 0.6035 0.5339 0.3430 0.096 Uiso 1 1 calc R U . . . H29B H 0.5683 0.5060 0.3818 0.096 Uiso 1 1 calc R U . . . H29C H 0.5159 0.5107 0.3437 0.096 Uiso 1 1 calc R U . . . C30 C 0.6007(4) 0.4409(3) 0.2964(2) 0.0577(18) Uani 1 1 d . U . . . H30A H 0.6420 0.4673 0.2875 0.087 Uiso 1 1 calc R U . . . H30B H 0.5511 0.4534 0.2854 0.087 Uiso 1 1 calc R U . . . H30C H 0.6122 0.4005 0.2880 0.087 Uiso 1 1 calc R U . . . C39 C 0.6815(3) 0.0429(3) 0.6324(2) 0.0501(16) Uani 1 1 d . U . . . H39A H 0.6785 0.0103 0.6134 0.060 Uiso 1 1 calc R U . . . H39B H 0.6995 0.0264 0.6574 0.060 Uiso 1 1 calc R U . . . C40 C 0.7372(4) 0.0880(3) 0.6187(2) 0.0522(16) Uani 1 1 d . U . . . H40A H 0.7372 0.1221 0.6366 0.063 Uiso 1 1 calc R U . . . H40B H 0.7902 0.0713 0.6180 0.063 Uiso 1 1 calc R U . . . C41 C 0.7699(3) 0.1474(3) 0.5655(2) 0.0493(15) Uani 1 1 d . U . . . H41A H 0.8206 0.1278 0.5616 0.059 Uiso 1 1 calc R U . . . H41B H 0.7774 0.1807 0.5836 0.059 Uiso 1 1 calc R U . . . C42 C 0.7402(3) 0.1694(3) 0.52811(19) 0.0497(15) Uani 1 1 d . U . . . H42A H 0.7803 0.1937 0.5152 0.060 Uiso 1 1 calc R U . . . H42B H 0.7276 0.1358 0.5110 0.060 Uiso 1 1 calc R U . . . C43 C 0.6458(4) 0.2318(4) 0.49991(17) 0.0583(16) Uani 1 1 d . U . . . H43A H 0.6394 0.2021 0.4792 0.070 Uiso 1 1 calc R U . . . H43B H 0.6841 0.2614 0.4911 0.070 Uiso 1 1 calc R U . . . C44 C 0.5708(4) 0.2607(3) 0.50795(17) 0.0567(15) Uani 1 1 d . U . . . H44A H 0.5763 0.2879 0.5302 0.068 Uiso 1 1 calc R U . . . H44B H 0.5544 0.2840 0.4852 0.068 Uiso 1 1 calc R U . . . C45 C 0.4404(4) 0.2425(3) 0.52502(16) 0.0463(13) Uani 1 1 d . U . . . H45A H 0.4228 0.2672 0.5031 0.056 Uiso 1 1 calc R U . . . H45B H 0.4444 0.2678 0.5483 0.056 Uiso 1 1 calc R U . . . C46 C 0.3834(3) 0.1936(3) 0.53210(15) 0.0413(13) Uani 1 1 d . U . . . H46A H 0.3300 0.2095 0.5330 0.050 Uiso 1 1 calc R U . . . H46B H 0.3864 0.1641 0.5111 0.050 Uiso 1 1 calc R U . . . C47 C 0.3513(3) 0.1213(3) 0.57863(18) 0.0410(13) Uani 1 1 d . U . . . H47A H 0.3552 0.0885 0.5599 0.049 Uiso 1 1 calc R U . . . H47B H 0.2973 0.1360 0.5786 0.049 Uiso 1 1 calc R U . . . C48 C 0.3730(3) 0.1008(3) 0.61781(18) 0.0424(13) Uani 1 1 d . U . . . H48A H 0.3704 0.1341 0.6363 0.051 Uiso 1 1 calc R U . . . H48B H 0.3364 0.0700 0.6265 0.051 Uiso 1 1 calc R U . . . C49 C 0.4740(4) 0.0561(2) 0.65355(15) 0.0421(12) Uani 1 1 d . U . . . H49A H 0.4351 0.0283 0.6640 0.050 Uiso 1 1 calc R U . . . H49B H 0.4794 0.0892 0.6720 0.050 Uiso 1 1 calc R U . . . C50 C 0.5504(4) 0.0255(2) 0.64871(16) 0.0394(13) Uani 1 1 d . U . . . H50A H 0.5661 0.0069 0.6734 0.047 Uiso 1 1 calc R U . . . H50B H 0.5461 -0.0056 0.6288 0.047 Uiso 1 1 calc R U . . . O1S O 0.6185(6) 0.1630(5) 0.7780(3) 0.104(4) Uani 0.721(19) 1 d D U P C 1 O1SA O 0.672(2) 0.2047(11) 0.7732(7) 0.153(12) Uani 0.279(19) 1 d D U P C 2 C1S C 0.6106(8) 0.2025(6) 0.7417(4) 0.135(4) Uani 1 1 d D U . . . H1S1 H 0.5564 0.2033 0.7323 0.161 Uiso 0.721(19) 1 calc R U P C 1 H1S2 H 0.6276 0.2433 0.7472 0.161 Uiso 0.721(19) 1 calc R U P C 1 H1S3 H 0.5656 0.1777 0.7487 0.161 Uiso 0.279(19) 1 calc R U P C 2 H1S4 H 0.5931 0.2421 0.7334 0.161 Uiso 0.279(19) 1 calc R U P C 2 C2S C 0.6611(10) 0.1748(7) 0.7139(4) 0.165(5) Uani 1 1 d D U . . . H2S1 H 0.6296 0.1576 0.6927 0.198 Uiso 1 1 calc R U . . . H2S2 H 0.6959 0.2047 0.7025 0.198 Uiso 1 1 calc R U . . . C3S C 0.7062(6) 0.1296(5) 0.7314(3) 0.098(3) Uani 1 1 d D U . . . H3S1 H 0.7619 0.1350 0.7256 0.117 Uiso 1 1 calc R U . . . H3S2 H 0.6898 0.0903 0.7222 0.117 Uiso 1 1 calc R U . . . C4S C 0.6915(6) 0.1359(5) 0.7727(3) 0.099(3) Uani 1 1 d D U . . . H4S1 H 0.6920 0.0968 0.7852 0.119 Uiso 0.721(19) 1 calc R U P C 1 H4S2 H 0.7326 0.1604 0.7846 0.119 Uiso 0.721(19) 1 calc R U P C 1 H4S3 H 0.7378 0.1265 0.7884 0.119 Uiso 0.279(19) 1 calc R U P C 2 H4S4 H 0.6471 0.1117 0.7813 0.119 Uiso 0.279(19) 1 calc R U P C 2 O2S O 0.8515(4) 0.1293(3) 0.45276(18) 0.096(2) Uani 1 1 d D U . . . C5S C 0.906(2) 0.0907(12) 0.4713(7) 0.084(8) Uani 0.42(4) 1 d D U P D 1 H5S1 H 0.9574 0.1094 0.4738 0.100 Uiso 0.42(4) 1 calc R U P D 1 H5S2 H 0.8873 0.0786 0.4972 0.100 Uiso 0.42(4) 1 calc R U P D 1 C6S C 0.908(4) 0.0421(16) 0.4452(8) 0.141(18) Uani 0.42(4) 1 d D U P D 1 H6S1 H 0.8830 0.0075 0.4576 0.169 Uiso 0.42(4) 1 calc R U P D 1 H6S2 H 0.9622 0.0318 0.4395 0.169 Uiso 0.42(4) 1 calc R U P D 1 C5SA C 0.8588(19) 0.0722(8) 0.4729(5) 0.091(7) Uani 0.58(4) 1 d D U P D 2 H5S3 H 0.9084 0.0703 0.4872 0.109 Uiso 0.58(4) 1 calc R U P D 2 H5S4 H 0.8158 0.0672 0.4917 0.109 Uiso 0.58(4) 1 calc R U P D 2 C6SA C 0.8558(18) 0.0257(8) 0.4434(5) 0.102(6) Uani 0.58(4) 1 d D U P D 2 H6S3 H 0.8972 -0.0038 0.4477 0.122 Uiso 0.58(4) 1 calc R U P D 2 H6S4 H 0.8050 0.0054 0.4438 0.122 Uiso 0.58(4) 1 calc R U P D 2 C7S C 0.8670(8) 0.0552(4) 0.4085(3) 0.108(4) Uani 1 1 d D U . . . H7S1 H 0.8979 0.0439 0.3856 0.130 Uiso 0.42(4) 1 calc R U P D 1 H7S2 H 0.8153 0.0364 0.4073 0.130 Uiso 0.42(4) 1 calc R U P D 1 H7S3 H 0.8274 0.0420 0.3897 0.130 Uiso 0.58(4) 1 calc R U P D 2 H7S4 H 0.9186 0.0450 0.3980 0.130 Uiso 0.58(4) 1 calc R U P D 2 C8S C 0.8617(5) 0.1188(4) 0.4131(2) 0.075(2) Uani 1 1 d D U . . . H8S1 H 0.9097 0.1380 0.4037 0.090 Uiso 1 1 calc R U . . . H8S2 H 0.8173 0.1345 0.3982 0.090 Uiso 1 1 calc R U . . . O3S O 0.3317(4) 0.4028(4) 0.6883(2) 0.071(3) Uani 0.691(14) 1 d D U P E 1 C12S C 0.2702(7) 0.3894(7) 0.7142(4) 0.085(4) Uani 0.691(14) 1 d D U P E 1 H14S H 0.2440 0.3527 0.7059 0.102 Uiso 0.691(14) 1 calc R U P E 1 H15S H 0.2317 0.4217 0.7140 0.102 Uiso 0.691(14) 1 calc R U P E 1 O3SA O 0.3169(11) 0.4570(13) 0.7016(8) 0.116(11) Uani 0.309(14) 1 d D U P E 2 C13S C 0.2656(14) 0.4379(11) 0.7313(7) 0.079(6) Uani 0.309(14) 1 d D U P E 2 H16S H 0.2147 0.4275 0.7199 0.095 Uiso 0.309(14) 1 calc R U P E 2 H17S H 0.2575 0.4700 0.7502 0.095 Uiso 0.309(14) 1 calc R U P E 2 C9S C 0.3890(6) 0.4307(4) 0.7107(3) 0.085(2) Uani 1 1 d D U . . . H20S H 0.3763 0.4727 0.7149 0.102 Uiso 0.691(14) 1 calc R U P E 1 H21S H 0.4404 0.4278 0.6981 0.102 Uiso 0.691(14) 1 calc R U P E 1 H22S H 0.4291 0.4618 0.7123 0.102 Uiso 0.309(14) 1 calc R U P E 2 H23S H 0.4038 0.4036 0.6895 0.102 Uiso 0.309(14) 1 calc R U P E 2 C10S C 0.3876(6) 0.3972(4) 0.7479(3) 0.090(3) Uani 1 1 d D U . . . H24S H 0.4061 0.4218 0.7697 0.108 Uiso 1 1 calc R U . . . H25S H 0.4197 0.3612 0.7463 0.108 Uiso 1 1 calc R U . . . C11S C 0.3016(7) 0.3823(6) 0.7521(4) 0.127(4) Uani 1 1 d D U . . . H26S H 0.2947 0.3413 0.7613 0.153 Uiso 0.691(14) 1 calc R U P E 1 H27S H 0.2761 0.4094 0.7706 0.153 Uiso 0.691(14) 1 calc R U P E 1 H28S H 0.2856 0.3799 0.7796 0.153 Uiso 0.309(14) 1 calc R U P E 2 H29S H 0.2880 0.3451 0.7388 0.153 Uiso 0.309(14) 1 calc R U P E 2 O4S O 0.1155(13) 0.0000 0.5000 0.200(6) Uiso 1 2 d DS U P . . C15S C 0.098(2) 0.0565(11) 0.4821(11) 0.200(6) Uiso 0.5 1 d D U P . . H36S H 0.1035 0.0527 0.4537 0.240 Uiso 0.5 1 calc R U P . . H37S H 0.0431 0.0667 0.4876 0.240 Uiso 0.5 1 calc R U P . . C16S C 0.144(2) 0.1005(12) 0.4946(12) 0.200(6) Uiso 0.5 1 d D U P . . H30S H 0.1583 0.1264 0.4727 0.240 Uiso 0.5 1 calc R U P . . H31S H 0.1161 0.1245 0.5141 0.240 Uiso 0.5 1 calc R U P . . C17S C 0.206(2) 0.0763(15) 0.5099(12) 0.200(6) Uiso 0.5 1 d D U P . . H32S H 0.2165 0.0936 0.5357 0.240 Uiso 0.5 1 calc R U P . . H33S H 0.2515 0.0833 0.4931 0.240 Uiso 0.5 1 calc R U P . . C18S C 0.1918(16) 0.0159(14) 0.5133(11) 0.200(6) Uiso 0.5 1 d D U P . . H34S H 0.1974 0.0041 0.5408 0.240 Uiso 0.5 1 calc R U P . . H35S H 0.2309 -0.0060 0.4981 0.240 Uiso 0.5 1 calc R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.02365(8) 0.01624(8) 0.02017(8) 0.00084(8) 0.00053(8) -0.00232(8) Fe1 0.0259(3) 0.0149(3) 0.0307(4) 0.0040(3) -0.0073(3) -0.0034(2) K1 0.0296(5) 0.0364(6) 0.0311(6) 0.0064(5) 0.0047(4) 0.0051(4) Si1 0.0348(7) 0.0213(6) 0.0312(7) 0.0056(5) 0.0104(6) 0.0018(5) Si2 0.0320(7) 0.0166(5) 0.0316(6) -0.0032(5) -0.0028(6) -0.0009(5) N1 0.0222(19) 0.0276(19) 0.0225(18) 0.0020(15) -0.0013(14) -0.0052(15) N2 0.032(2) 0.0156(17) 0.0265(19) 0.0003(14) -0.0060(16) -0.0015(15) O1 0.043(2) 0.0242(17) 0.048(2) 0.0038(16) -0.0128(18) -0.0020(15) O2 0.0345(18) 0.0370(19) 0.0345(19) 0.0070(16) 0.0056(15) 0.0027(15) O3 0.0327(18) 0.046(2) 0.0295(18) 0.0066(16) -0.0010(14) 0.0071(16) O4 0.052(2) 0.039(2) 0.0350(19) 0.0081(15) 0.0095(18) 0.0054(18) O5 0.049(2) 0.047(2) 0.033(2) -0.0048(17) 0.0085(16) -0.0138(18) O6 0.0276(18) 0.033(2) 0.064(3) -0.0110(18) -0.0096(17) -0.0030(15) O8 0.059(3) 0.063(3) 0.097(4) -0.034(3) 0.035(2) -0.021(2) C31 0.063(4) 0.064(4) 0.070(4) -0.018(3) 0.022(4) -0.007(4) C32 0.079(5) 0.065(4) 0.066(4) -0.019(4) 0.009(4) 0.005(4) C33 0.117(7) 0.056(5) 0.091(6) -0.021(4) 0.009(5) -0.029(5) C34 0.065(5) 0.080(5) 0.082(5) -0.019(4) 0.011(4) -0.019(4) O7 0.071(6) 0.029(4) 0.039(4) -0.005(3) -0.017(4) 0.010(4) C35 0.063(6) 0.043(5) 0.043(5) -0.005(4) -0.012(5) 0.010(5) C36 0.116(10) 0.063(7) 0.076(7) -0.021(6) -0.041(7) 0.024(7) C37 0.089(9) 0.043(6) 0.058(7) -0.015(5) -0.023(7) 0.021(6) C38 0.080(8) 0.042(5) 0.055(6) -0.003(5) -0.018(6) 0.013(5) C1 0.024(3) 0.018(3) 0.021(3) 0.000 -0.001(2) 0.000 C2 0.0213(19) 0.026(2) 0.021(2) -0.0032(18) 0.0009(17) 0.0003(18) C3 0.027(2) 0.024(2) 0.025(2) 0.0011(18) 0.0007(17) 0.003(2) C4 0.030(4) 0.016(3) 0.022(3) 0.000 0.001(2) 0.000 C5 0.074(5) 0.018(3) 0.012(3) 0.000 0.002(3) 0.000 C6 0.100(5) 0.026(2) 0.026(3) 0.000(2) -0.003(3) 0.028(3) C7 0.159(8) 0.031(3) 0.022(3) -0.003(2) -0.008(4) 0.033(4) C8 0.166(9) 0.025(4) 0.032(4) 0.000 -0.006(5) 0.000 C9 0.029(2) 0.0163(19) 0.024(2) 0.0016(16) -0.0048(16) -0.0104(15) C10 0.044(3) 0.020(2) 0.027(2) 0.0078(18) -0.0070(19) -0.0097(19) C11 0.044(3) 0.021(2) 0.038(3) 0.0105(19) -0.016(2) -0.008(2) C12 0.039(3) 0.016(2) 0.047(3) 0.002(2) -0.011(2) 0.0019(18) C13 0.031(2) 0.015(2) 0.034(2) 0.0012(17) -0.0043(18) -0.0047(17) C14 0.028(2) 0.0155(19) 0.034(2) 0.0039(18) -0.0066(18) -0.0077(16) C15 0.042(3) 0.020(2) 0.035(3) 0.0023(18) -0.014(2) -0.0056(18) C16 0.037(3) 0.023(3) 0.054(3) 0.005(2) -0.022(2) -0.0081(18) C17 0.025(2) 0.030(2) 0.057(3) 0.009(3) -0.006(2) -0.002(2) C18 0.025(2) 0.024(2) 0.039(2) 0.005(2) -0.0020(17) -0.0071(19) C19 0.087(5) 0.049(4) 0.034(3) 0.001(3) 0.006(3) 0.035(3) C20 0.034(3) 0.033(3) 0.041(3) 0.007(2) 0.010(2) 0.003(2) C21 0.036(3) 0.027(3) 0.094(5) 0.024(3) 0.019(3) 0.002(2) C22 0.058(4) 0.033(3) 0.082(5) 0.021(3) 0.017(3) -0.003(3) C23 0.052(8) 0.068(10) 0.121(12) 0.053(9) 0.032(8) 0.013(7) C23A 0.040(5) 0.027(5) 0.057(8) -0.010(6) 0.014(5) -0.014(4) C24 0.080(5) 0.041(4) 0.104(6) -0.003(4) -0.009(4) -0.024(4) C25 0.092(5) 0.045(3) 0.039(3) -0.014(3) 0.002(3) 0.013(4) C26 0.029(3) 0.031(3) 0.052(3) -0.011(2) 0.006(2) 0.002(2) C27 0.033(3) 0.020(2) 0.067(4) 0.005(2) -0.014(2) -0.0043(19) C28 0.035(3) 0.024(3) 0.108(6) 0.006(3) -0.023(3) -0.009(2) C29 0.062(4) 0.019(3) 0.111(6) -0.003(3) -0.028(4) -0.001(3) C30 0.052(4) 0.050(4) 0.072(4) 0.024(3) -0.004(3) -0.022(3) C39 0.044(3) 0.029(3) 0.077(4) 0.005(3) -0.026(3) 0.004(2) C40 0.037(3) 0.037(3) 0.083(4) -0.001(3) -0.019(3) 0.002(2) C41 0.031(3) 0.050(3) 0.067(4) -0.016(3) -0.002(3) -0.010(2) C42 0.042(3) 0.056(4) 0.051(3) -0.022(3) 0.010(3) -0.014(3) C43 0.066(4) 0.078(4) 0.031(3) 0.013(3) 0.005(3) -0.018(4) C44 0.079(4) 0.055(3) 0.036(3) 0.019(3) 0.000(3) -0.014(3) C45 0.066(3) 0.046(3) 0.027(2) 0.006(2) 0.007(2) 0.022(3) C46 0.042(3) 0.059(4) 0.024(3) 0.002(2) 0.000(2) 0.021(2) C47 0.029(3) 0.044(3) 0.049(3) -0.001(3) 0.003(2) 0.009(2) C48 0.031(3) 0.043(3) 0.053(3) 0.007(3) 0.013(2) 0.000(2) C49 0.058(3) 0.036(3) 0.031(3) 0.007(2) 0.007(3) 0.003(3) C50 0.056(3) 0.032(3) 0.030(3) 0.005(2) -0.006(2) -0.002(2) O1S 0.091(7) 0.132(10) 0.089(6) -0.023(5) 0.004(5) 0.009(6) O1SA 0.16(2) 0.138(14) 0.159(15) -0.036(11) -0.019(15) 0.046(14) C1S 0.111(8) 0.171(10) 0.122(8) -0.012(7) 0.009(6) 0.068(8) C2S 0.205(11) 0.162(9) 0.128(7) 0.007(7) 0.028(7) 0.066(8) C3S 0.088(7) 0.092(7) 0.112(7) -0.009(5) 0.015(5) 0.001(5) C4S 0.095(7) 0.102(7) 0.099(6) -0.040(5) -0.018(5) 0.000(5) O2S 0.119(5) 0.084(4) 0.085(4) -0.014(3) -0.002(4) 0.020(4) C5S 0.116(17) 0.068(11) 0.067(8) -0.005(7) -0.004(10) 0.008(11) C6S 0.23(4) 0.103(12) 0.091(11) -0.026(9) -0.059(18) 0.074(19) C5SA 0.120(18) 0.085(8) 0.067(6) -0.005(5) -0.010(8) 0.045(9) C6SA 0.131(13) 0.082(6) 0.093(7) -0.006(5) 0.009(8) 0.017(7) C7S 0.159(10) 0.093(6) 0.073(5) -0.017(4) -0.019(5) 0.053(6) C8S 0.055(4) 0.092(5) 0.079(5) 0.005(4) 0.004(4) 0.005(4) O3S 0.070(5) 0.104(7) 0.038(4) -0.004(4) 0.014(3) -0.023(4) C12S 0.073(7) 0.108(11) 0.074(7) -0.011(7) 0.019(5) -0.018(6) O3SA 0.092(10) 0.14(2) 0.116(15) 0.043(16) 0.041(9) -0.005(10) C13S 0.087(10) 0.104(15) 0.045(11) -0.019(9) 0.013(8) -0.038(8) C9S 0.086(5) 0.083(6) 0.086(5) -0.002(4) 0.014(4) -0.027(4) C10S 0.095(6) 0.102(6) 0.073(5) -0.016(5) 0.014(4) 0.001(5) C11S 0.105(8) 0.174(11) 0.104(7) 0.038(7) 0.031(5) -0.022(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N1 2.308(4) . ? Er1 N2 2.309(4) . ? Er1 C3 2.427(5) . ? Er1 C2 2.428(4) . ? Er1 C1 2.506(4) . ? Er1 C4 2.514(4) . ? Er1 C3 2.573(5) 3_655 ? Er1 C2 2.583(4) 3_655 ? Er1 C9 2.843(4) . ? Er1 C14 2.861(4) . ? Er1 Fe1 3.2636(7) . ? Fe1 C16 2.020(5) . ? Fe1 C11 2.027(5) . ? Fe1 C12 2.038(5) . ? Fe1 C17 2.038(5) . ? Fe1 C10 2.051(5) . ? Fe1 C15 2.054(5) . ? Fe1 C18 2.068(5) . ? Fe1 C13 2.078(4) . ? Fe1 C14 2.135(5) . ? Fe1 C9 2.135(4) . ? K1 O8 2.699(5) . ? K1 O2 2.760(4) . ? K1 O1 2.773(4) . ? K1 O3 2.786(4) . ? K1 O6 2.806(4) . ? K1 O5 2.817(4) . ? K1 O4 2.827(4) . ? K1 O7 2.839(9) . ? Si1 N1 1.681(4) . ? Si1 C19 1.861(6) . ? Si1 C20 1.879(5) . ? Si1 C21 1.919(6) . ? Si2 N2 1.687(4) . ? Si2 C26 1.867(5) . ? Si2 C25 1.889(6) . ? Si2 C27 1.904(5) . ? N1 C9 1.403(6) . ? N2 C14 1.390(6) . ? O1 C39 1.422(7) . ? O1 C50 1.439(7) . ? O2 C48 1.415(6) . ? O2 C49 1.435(6) . ? O3 C46 1.422(6) . ? O3 C47 1.423(7) . ? O4 C45 1.422(7) . ? O4 C44 1.427(7) . ? O5 C42 1.422(7) . ? O5 C43 1.437(7) . ? O6 C40 1.412(8) . ? O6 C41 1.429(7) . ? O8 C34 1.369(8) . ? O8 C31 1.421(7) . ? C31 C32 1.479(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.471(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.416(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? O7 C38 1.403(13) . ? O7 C35 1.408(13) . ? C35 C36 1.436(14) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.425(15) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.451(15) . ? C37 K1 3.510(13) 4_556 ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C1 C2 1.434(5) 3_655 ? C1 C2 1.434(5) . ? C1 Er1 2.506(4) 3_655 ? C1 H1A 0.9500 . ? C2 C3 1.476(6) 3_655 ? C2 Er1 2.583(4) 3_655 ? C2 H2A 0.9500 . ? C3 C2 1.476(6) 3_655 ? C3 C4 1.494(6) . ? C3 Er1 2.573(5) 3_655 ? C3 H3A 0.9500 . ? C4 C5 1.437(9) . ? C4 C3 1.494(6) 3_655 ? C4 Er1 2.514(4) 3_655 ? C5 C6 1.421(8) 3_655 ? C5 C6 1.421(8) . ? C6 C7 1.395(8) . ? C6 H6A 0.9500 . ? C7 C8 1.366(10) . ? C7 H7A 0.9500 . ? C8 C7 1.366(10) 3_655 ? C8 H8A 0.9500 . ? C9 C10 1.438(6) . ? C9 C13 1.438(7) . ? C10 C11 1.418(8) . ? C10 H10A 0.9500 . ? C11 C12 1.432(8) . ? C11 H11A 0.9500 . ? C12 C13 1.432(7) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C18 1.444(7) . ? C14 C15 1.448(7) . ? C15 C16 1.446(7) . ? C15 H15A 0.9500 . ? C16 C17 1.411(8) . ? C16 H16A 0.9500 . ? C17 C18 1.425(7) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23A 1.540(14) . ? C21 C24 1.542(11) . ? C21 C22 1.549(9) . ? C21 C23 1.635(19) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.527(8) . ? C27 C28 1.532(8) . ? C27 C30 1.537(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C39 C40 1.483(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.477(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.479(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.503(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.480(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.499(8) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? O1S C4S 1.414(12) . ? O1S C1S 1.551(13) . ? O1SA C1S 1.52(2) . ? O1SA C4S 1.60(2) . ? C1S C2S 1.442(13) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C1S H1S3 0.9900 . ? C1S H1S4 0.9900 . ? C2S C3S 1.423(14) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.455(11) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C4S H4S3 0.9900 . ? C4S H4S4 0.9900 . ? O2S C8S 1.404(9) . ? O2S C5S 1.434(18) . ? O2S C5SA 1.479(15) . ? C5S C6S 1.428(19) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C6S C7S 1.478(18) . ? C6S H6S1 0.9900 . ? C6S H6S2 0.9900 . ? C5SA C6SA 1.469(17) . ? C5SA H5S3 0.9900 . ? C5SA H5S4 0.9900 . ? C6SA C7S 1.395(16) . ? C6SA H6S3 0.9900 . ? C6SA H6S4 0.9900 . ? C7S C8S 1.455(11) . ? C7S H7S1 0.9900 . ? C7S H7S2 0.9900 . ? C7S H7S3 0.9900 . ? C7S H7S4 0.9900 . ? C8S H8S1 0.9900 . ? C8S H8S2 0.9900 . ? O3S C9S 1.406(10) . ? O3S C12S 1.419(12) . ? C12S C11S 1.429(14) . ? C12S H14S 0.9900 . ? C12S H15S 0.9900 . ? O3SA C9S 1.415(18) . ? O3SA C13S 1.422(19) . ? C13S C11S 1.58(2) . ? C13S H16S 0.9900 . ? C13S H17S 0.9900 . ? C9S C10S 1.494(12) . ? C9S H20S 0.9900 . ? C9S H21S 0.9900 . ? C9S H22S 0.9900 . ? C9S H23S 0.9900 . ? C10S C11S 1.531(12) . ? C10S H24S 0.9900 . ? C10S H25S 0.9900 . ? C11S H26S 0.9900 . ? C11S H27S 0.9900 . ? C11S H28S 0.9900 . ? C11S H29S 0.9900 . ? O4S C18S 1.440(19) . ? O4S C18S 1.440(19) 4_556 ? O4S C15S 1.457(19) 4_556 ? O4S C15S 1.457(19) . ? C15S C16S 1.346(19) . ? C15S H36S 0.9900 . ? C15S H37S 0.9900 . ? C16S C17S 1.318(19) . ? C16S H30S 0.9900 . ? C16S H31S 0.9900 . ? C17S C18S 1.399(19) . ? C17S H32S 0.9900 . ? C17S H33S 0.9900 . ? C18S H34S 0.9900 . ? C18S H35S 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Er1 N2 99.65(13) . . ? N1 Er1 C3 128.35(14) . . ? N2 Er1 C3 126.05(15) . . ? N1 Er1 C2 114.45(13) . . ? N2 Er1 C2 110.77(14) . . ? C3 Er1 C2 73.79(15) . . ? N1 Er1 C1 147.74(10) . . ? N2 Er1 C1 92.40(14) . . ? C3 Er1 C1 61.24(14) . . ? C2 Er1 C1 33.75(11) . . ? N1 Er1 C4 100.38(13) . . ? N2 Er1 C4 159.80(13) . . ? C3 Er1 C4 35.14(12) . . ? C2 Er1 C4 62.54(14) . . ? C1 Er1 C4 71.76(15) . . ? N1 Er1 C3 96.24(14) . 3_655 ? N2 Er1 C3 144.70(14) . 3_655 ? C3 Er1 C3 61.3(2) . 3_655 ? C2 Er1 C3 34.17(14) . 3_655 ? C1 Er1 C3 59.31(14) . 3_655 ? C4 Er1 C3 34.13(12) . 3_655 ? N1 Er1 C2 160.78(13) . 3_655 ? N2 Er1 C2 99.46(14) . 3_655 ? C3 Er1 C2 34.08(13) . 3_655 ? C2 Er1 C2 59.81(17) . 3_655 ? C1 Er1 C2 32.69(11) . 3_655 ? C4 Er1 C2 60.44(14) . 3_655 ? C3 Er1 C2 68.84(13) 3_655 3_655 ? N1 Er1 C9 29.32(13) . . ? N2 Er1 C9 92.94(12) . . ? C3 Er1 C9 116.18(14) . . ? C2 Er1 C9 141.95(13) . . ? C1 Er1 C9 174.50(13) . . ? C4 Er1 C9 103.30(14) . . ? C3 Er1 C9 115.25(13) 3_655 . ? C2 Er1 C9 146.89(14) 3_655 . ? N1 Er1 C14 93.57(13) . . ? N2 Er1 C14 28.76(13) . . ? C3 Er1 C14 114.43(15) . . ? C2 Er1 C14 137.05(14) . . ? C1 Er1 C14 110.35(13) . . ? C4 Er1 C14 146.19(10) . . ? C3 Er1 C14 169.64(14) 3_655 . ? C2 Er1 C14 102.23(14) 3_655 . ? C9 Er1 C14 75.07(12) . . ? N1 Er1 Fe1 67.20(9) . . ? N2 Er1 Fe1 66.49(9) . . ? C3 Er1 Fe1 107.13(12) . . ? C2 Er1 Fe1 177.18(11) . . ? C1 Er1 Fe1 144.28(5) . . ? C4 Er1 Fe1 119.77(9) . . ? C3 Er1 Fe1 148.62(11) 3_655 . ? C2 Er1 Fe1 119.44(9) 3_655 . ? C9 Er1 Fe1 40.20(8) . . ? C14 Er1 Fe1 40.13(9) . . ? C16 Fe1 C11 105.7(2) . . ? C16 Fe1 C12 121.9(2) . . ? C11 Fe1 C12 41.3(2) . . ? C16 Fe1 C17 40.7(2) . . ? C11 Fe1 C17 122.3(2) . . ? C12 Fe1 C17 107.6(2) . . ? C16 Fe1 C10 121.1(2) . . ? C11 Fe1 C10 40.7(2) . . ? C12 Fe1 C10 69.0(2) . . ? C17 Fe1 C10 157.7(2) . . ? C16 Fe1 C15 41.6(2) . . ? C11 Fe1 C15 120.7(2) . . ? C12 Fe1 C15 157.9(2) . . ? C17 Fe1 C15 69.3(2) . . ? C10 Fe1 C15 105.2(2) . . ? C16 Fe1 C18 68.2(2) . . ? C11 Fe1 C18 159.7(2) . . ? C12 Fe1 C18 124.3(2) . . ? C17 Fe1 C18 40.60(19) . . ? C10 Fe1 C18 159.1(2) . . ? C15 Fe1 C18 68.4(2) . . ? C16 Fe1 C13 159.8(2) . . ? C11 Fe1 C13 67.9(2) . . ? C12 Fe1 C13 40.70(19) . . ? C17 Fe1 C13 125.2(2) . . ? C10 Fe1 C13 67.43(19) . . ? C15 Fe1 C13 158.4(2) . . ? C18 Fe1 C13 110.8(2) . . ? C16 Fe1 C14 68.22(18) . . ? C11 Fe1 C14 157.4(2) . . ? C12 Fe1 C14 160.4(2) . . ? C17 Fe1 C14 68.1(2) . . ? C10 Fe1 C14 122.4(2) . . ? C15 Fe1 C14 40.38(18) . . ? C18 Fe1 C14 40.15(19) . . ? C13 Fe1 C14 125.01(18) . . ? C16 Fe1 C9 157.5(2) . . ? C11 Fe1 C9 67.91(19) . . ? C12 Fe1 C9 68.51(19) . . ? C17 Fe1 C9 160.9(2) . . ? C10 Fe1 C9 40.11(18) . . ? C15 Fe1 C9 121.6(2) . . ? C18 Fe1 C9 125.06(18) . . ? C13 Fe1 C9 39.87(18) . . ? C14 Fe1 C9 108.92(17) . . ? C16 Fe1 Er1 126.99(14) . . ? C11 Fe1 Er1 126.18(15) . . ? C12 Fe1 Er1 105.61(15) . . ? C17 Fe1 Er1 106.18(15) . . ? C10 Fe1 Er1 95.76(14) . . ? C15 Fe1 Er1 96.06(14) . . ? C18 Fe1 Er1 66.17(13) . . ? C13 Fe1 Er1 65.63(13) . . ? C14 Fe1 Er1 59.72(12) . . ? C9 Fe1 Er1 59.24(12) . . ? O8 K1 O2 95.47(13) . . ? O8 K1 O1 98.78(16) . . ? O2 K1 O1 61.37(11) . . ? O8 K1 O3 76.37(14) . . ? O2 K1 O3 59.50(11) . . ? O1 K1 O3 119.71(12) . . ? O8 K1 O6 110.39(14) . . ? O2 K1 O6 119.13(12) . . ? O1 K1 O6 60.83(13) . . ? O3 K1 O6 173.21(12) . . ? O8 K1 O5 87.62(13) . . ? O2 K1 O5 176.74(12) . . ? O1 K1 O5 119.23(13) . . ? O3 K1 O5 120.50(12) . . ? O6 K1 O5 60.44(13) . . ? O8 K1 O4 81.90(15) . . ? O2 K1 O4 119.15(12) . . ? O1 K1 O4 179.14(13) . . ? O3 K1 O4 60.94(11) . . ? O6 K1 O4 118.45(13) . . ? O5 K1 O4 60.21(12) . . ? O8 K1 O7 167.5(2) . . ? O2 K1 O7 90.9(2) . . ? O1 K1 O7 93.72(18) . . ? O3 K1 O7 97.9(2) . . ? O6 K1 O7 75.4(2) . . ? O5 K1 O7 85.8(2) . . ? O4 K1 O7 85.60(18) . . ? N1 Si1 C19 115.0(3) . . ? N1 Si1 C20 107.9(2) . . ? C19 Si1 C20 107.2(3) . . ? N1 Si1 C21 111.3(2) . . ? C19 Si1 C21 107.8(3) . . ? C20 Si1 C21 107.3(3) . . ? N2 Si2 C26 108.7(2) . . ? N2 Si2 C25 114.4(2) . . ? C26 Si2 C25 106.8(3) . . ? N2 Si2 C27 110.9(2) . . ? C26 Si2 C27 107.9(2) . . ? C25 Si2 C27 107.9(3) . . ? C9 N1 Si1 127.3(3) . . ? C9 N1 Er1 97.0(3) . . ? Si1 N1 Er1 131.4(2) . . ? C14 N2 Si2 125.4(3) . . ? C14 N2 Er1 98.2(3) . . ? Si2 N2 Er1 136.0(2) . . ? C39 O1 C50 111.5(4) . . ? C39 O1 K1 115.3(4) . . ? C50 O1 K1 114.7(3) . . ? C48 O2 C49 112.2(4) . . ? C48 O2 K1 117.6(3) . . ? C49 O2 K1 114.1(3) . . ? C46 O3 C47 112.3(4) . . ? C46 O3 K1 115.0(3) . . ? C47 O3 K1 115.5(3) . . ? C45 O4 C44 112.0(5) . . ? C45 O4 K1 109.8(3) . . ? C44 O4 K1 112.0(3) . . ? C42 O5 C43 111.9(5) . . ? C42 O5 K1 112.3(4) . . ? C43 O5 K1 115.9(3) . . ? C40 O6 C41 111.5(4) . . ? C40 O6 K1 112.4(4) . . ? C41 O6 K1 115.1(3) . . ? C34 O8 C31 109.7(5) . . ? C34 O8 K1 131.4(4) . . ? C31 O8 K1 118.1(4) . . ? O8 C31 C32 106.4(6) . . ? O8 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? O8 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.6 . . ? C33 C32 C31 104.3(6) . . ? C33 C32 H32A 110.9 . . ? C31 C32 H32A 110.9 . . ? C33 C32 H32B 110.9 . . ? C31 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? C34 C33 C32 106.0(6) . . ? C34 C33 H33A 110.5 . . ? C32 C33 H33A 110.5 . . ? C34 C33 H33B 110.5 . . ? C32 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? O8 C34 C33 108.3(6) . . ? O8 C34 H34A 110.0 . . ? C33 C34 H34A 110.0 . . ? O8 C34 H34B 110.0 . . ? C33 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? C38 O7 C35 107.8(9) . . ? C38 O7 K1 120.3(7) . . ? C35 O7 K1 121.1(7) . . ? O7 C35 C36 105.1(10) . . ? O7 C35 H35A 110.7 . . ? C36 C35 H35A 110.7 . . ? O7 C35 H35B 110.7 . . ? C36 C35 H35B 110.7 . . ? H35A C35 H35B 108.8 . . ? C37 C36 C35 108.1(11) . . ? C37 C36 H36A 110.1 . . ? C35 C36 H36A 110.1 . . ? C37 C36 H36B 110.1 . . ? C35 C36 H36B 110.1 . . ? H36A C36 H36B 108.4 . . ? C36 C37 C38 105.5(11) . . ? C36 C37 K1 80.1(7) . 4_556 ? C38 C37 K1 171.8(12) . 4_556 ? C36 C37 H37A 110.6 . . ? C38 C37 H37A 110.6 . . ? K1 C37 H37A 61.4 4_556 . ? C36 C37 H37B 110.6 . . ? C38 C37 H37B 110.6 . . ? K1 C37 H37B 72.1 4_556 . ? H37A C37 H37B 108.8 . . ? O7 C38 C37 107.4(10) . . ? O7 C38 H38A 110.2 . . ? C37 C38 H38A 110.2 . . ? O7 C38 H38B 110.2 . . ? C37 C38 H38B 110.2 . . ? H38A C38 H38B 108.5 . . ? C2 C1 C2 121.4(6) 3_655 . ? C2 C1 Er1 76.6(2) 3_655 . ? C2 C1 Er1 70.1(2) . . ? C2 C1 Er1 70.1(2) 3_655 3_655 ? C2 C1 Er1 76.6(2) . 3_655 ? Er1 C1 Er1 108.5(2) . 3_655 ? C2 C1 H1A 119.3 3_655 . ? C2 C1 H1A 119.3 . . ? Er1 C1 H1A 125.8 . . ? Er1 C1 H1A 125.8 3_655 . ? C1 C2 C3 119.5(4) . 3_655 ? C1 C2 Er1 76.1(2) . . ? C3 C2 Er1 78.3(3) 3_655 . ? C1 C2 Er1 70.7(2) . 3_655 ? C3 C2 Er1 67.2(3) 3_655 3_655 ? Er1 C2 Er1 108.50(16) . 3_655 ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 3_655 . ? Er1 C2 H2A 116.0 . . ? Er1 C2 H2A 135.5 3_655 . ? C2 C3 C4 119.5(5) 3_655 . ? C2 C3 Er1 78.7(3) 3_655 . ? C4 C3 Er1 75.6(2) . . ? C2 C3 Er1 67.5(3) 3_655 3_655 ? C4 C3 Er1 70.8(2) . 3_655 ? Er1 C3 Er1 108.82(19) . 3_655 ? C2 C3 H3A 120.2 3_655 . ? C4 C3 H3A 120.2 . . ? Er1 C3 H3A 116.2 . . ? Er1 C3 H3A 135.0 3_655 . ? C5 C4 C3 121.3(3) . . ? C5 C4 C3 121.3(3) . 3_655 ? C3 C4 C3 117.3(5) . 3_655 ? C5 C4 Er1 126.01(11) . . ? C3 C4 Er1 69.3(2) . . ? C3 C4 Er1 75.1(2) 3_655 . ? C5 C4 Er1 126.01(11) . 3_655 ? C3 C4 Er1 75.1(2) . 3_655 ? C3 C4 Er1 69.3(2) 3_655 3_655 ? Er1 C4 Er1 108.0(2) . 3_655 ? C6 C5 C6 115.6(7) 3_655 . ? C6 C5 C4 122.2(4) 3_655 . ? C6 C5 C4 122.2(4) . . ? C7 C6 C5 120.8(8) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C8 C7 C6 122.6(9) . . ? C8 C7 H7A 118.7 . . ? C6 C7 H7A 118.7 . . ? C7 C8 C7 117.6(9) . 3_655 ? C7 C8 H8A 121.2 . . ? C7 C8 H8A 121.2 3_655 . ? N1 C9 C10 130.4(4) . . ? N1 C9 C13 123.8(4) . . ? C10 C9 C13 105.7(4) . . ? N1 C9 Fe1 127.1(3) . . ? C10 C9 Fe1 66.8(3) . . ? C13 C9 Fe1 67.9(2) . . ? N1 C9 Er1 53.7(2) . . ? C10 C9 Er1 137.8(3) . . ? C13 C9 Er1 84.6(3) . . ? Fe1 C9 Er1 80.56(13) . . ? C11 C10 C9 109.1(5) . . ? C11 C10 Fe1 68.8(3) . . ? C9 C10 Fe1 73.1(3) . . ? C11 C10 H10A 125.4 . . ? C9 C10 H10A 125.4 . . ? Fe1 C10 H10A 124.2 . . ? C10 C11 C12 108.8(4) . . ? C10 C11 Fe1 70.5(3) . . ? C12 C11 Fe1 69.8(3) . . ? C10 C11 H11A 125.6 . . ? C12 C11 H11A 125.6 . . ? Fe1 C11 H11A 125.6 . . ? C13 C12 C11 106.4(5) . . ? C13 C12 Fe1 71.2(3) . . ? C11 C12 Fe1 69.0(3) . . ? C13 C12 H12A 126.8 . . ? C11 C12 H12A 126.8 . . ? Fe1 C12 H12A 124.7 . . ? C12 C13 C9 110.0(4) . . ? C12 C13 Fe1 68.1(3) . . ? C9 C13 Fe1 72.2(2) . . ? C12 C13 H13A 125.0 . . ? C9 C13 H13A 125.0 . . ? Fe1 C13 H13A 126.2 . . ? N2 C14 C18 124.0(4) . . ? N2 C14 C15 129.2(5) . . ? C18 C14 C15 106.5(4) . . ? N2 C14 Fe1 125.9(3) . . ? C18 C14 Fe1 67.4(3) . . ? C15 C14 Fe1 66.8(3) . . ? N2 C14 Er1 53.0(2) . . ? C18 C14 Er1 84.5(3) . . ? C15 C14 Er1 136.5(3) . . ? Fe1 C14 Er1 80.15(13) . . ? C16 C15 C14 107.4(5) . . ? C16 C15 Fe1 67.9(3) . . ? C14 C15 Fe1 72.8(3) . . ? C16 C15 H15A 126.3 . . ? C14 C15 H15A 126.3 . . ? Fe1 C15 H15A 124.5 . . ? C17 C16 C15 109.0(4) . . ? C17 C16 Fe1 70.3(3) . . ? C15 C16 Fe1 70.5(3) . . ? C17 C16 H16A 125.5 . . ? C15 C16 H16A 125.5 . . ? Fe1 C16 H16A 125.3 . . ? C16 C17 C18 107.8(5) . . ? C16 C17 Fe1 69.0(3) . . ? C18 C17 Fe1 70.9(3) . . ? C16 C17 H17A 126.1 . . ? C18 C17 H17A 126.1 . . ? Fe1 C17 H17A 125.6 . . ? C17 C18 C14 109.2(5) . . ? C17 C18 Fe1 68.5(3) . . ? C14 C18 Fe1 72.4(3) . . ? C17 C18 H18A 125.4 . . ? C14 C18 H18A 125.4 . . ? Fe1 C18 H18A 125.2 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23A C21 C24 99.6(7) . . ? C23A C21 C22 115.2(8) . . ? C24 C21 C22 110.1(6) . . ? C24 C21 C23 128.5(10) . . ? C22 C21 C23 97.0(8) . . ? C23A C21 Si1 114.7(6) . . ? C24 C21 Si1 108.0(4) . . ? C22 C21 Si1 108.6(4) . . ? C23 C21 Si1 103.2(8) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C23A H23D 109.5 . . ? C21 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C21 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 108.2(5) . . ? C29 C27 C30 109.2(5) . . ? C28 C27 C30 107.9(6) . . ? C29 C27 Si2 113.1(5) . . ? C28 C27 Si2 109.2(4) . . ? C30 C27 Si2 109.1(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C39 C40 109.8(5) . . ? O1 C39 H39A 109.7 . . ? C40 C39 H39A 109.7 . . ? O1 C39 H39B 109.7 . . ? C40 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? O6 C40 C39 109.1(5) . . ? O6 C40 H40A 109.9 . . ? C39 C40 H40A 109.9 . . ? O6 C40 H40B 109.9 . . ? C39 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? O6 C41 C42 108.9(5) . . ? O6 C41 H41A 109.9 . . ? C42 C41 H41A 109.9 . . ? O6 C41 H41B 109.9 . . ? C42 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? O5 C42 C41 109.2(5) . . ? O5 C42 H42A 109.8 . . ? C41 C42 H42A 109.8 . . ? O5 C42 H42B 109.8 . . ? C41 C42 H42B 109.8 . . ? H42A C42 H42B 108.3 . . ? O5 C43 C44 108.7(5) . . ? O5 C43 H43A 109.9 . . ? C44 C43 H43A 109.9 . . ? O5 C43 H43B 109.9 . . ? C44 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? O4 C44 C43 109.5(6) . . ? O4 C44 H44A 109.8 . . ? C43 C44 H44A 109.8 . . ? O4 C44 H44B 109.8 . . ? C43 C44 H44B 109.8 . . ? H44A C44 H44B 108.2 . . ? O4 C45 C46 108.5(5) . . ? O4 C45 H45A 110.0 . . ? C46 C45 H45A 110.0 . . ? O4 C45 H45B 110.0 . . ? C46 C45 H45B 110.0 . . ? H45A C45 H45B 108.4 . . ? O3 C46 C45 107.1(5) . . ? O3 C46 H46A 110.3 . . ? C45 C46 H46A 110.3 . . ? O3 C46 H46B 110.3 . . ? C45 C46 H46B 110.3 . . ? H46A C46 H46B 108.5 . . ? O3 C47 C48 107.8(5) . . ? O3 C47 H47A 110.1 . . ? C48 C47 H47A 110.1 . . ? O3 C47 H47B 110.1 . . ? C48 C47 H47B 110.1 . . ? H47A C47 H47B 108.5 . . ? O2 C48 C47 108.9(5) . . ? O2 C48 H48A 109.9 . . ? C47 C48 H48A 109.9 . . ? O2 C48 H48B 109.9 . . ? C47 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? O2 C49 C50 108.8(4) . . ? O2 C49 H49A 109.9 . . ? C50 C49 H49A 109.9 . . ? O2 C49 H49B 109.9 . . ? C50 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? O1 C50 C49 108.2(4) . . ? O1 C50 H50A 110.1 . . ? C49 C50 H50A 110.1 . . ? O1 C50 H50B 110.1 . . ? C49 C50 H50B 110.1 . . ? H50A C50 H50B 108.4 . . ? C4S O1S C1S 102.9(9) . . ? C1S O1SA C4S 96.1(14) . . ? C2S C1S O1SA 94.1(12) . . ? C2S C1S O1S 103.6(9) . . ? C2S C1S H1S1 111.0 . . ? O1S C1S H1S1 111.0 . . ? C2S C1S H1S2 111.0 . . ? O1S C1S H1S2 111.0 . . ? H1S1 C1S H1S2 109.0 . . ? C2S C1S H1S3 112.9 . . ? O1SA C1S H1S3 112.9 . . ? C2S C1S H1S4 112.9 . . ? O1SA C1S H1S4 112.9 . . ? H1S3 C1S H1S4 110.3 . . ? C3S C2S C1S 111.1(10) . . ? C3S C2S H2S1 109.4 . . ? C1S C2S H2S1 109.4 . . ? C3S C2S H2S2 109.4 . . ? C1S C2S H2S2 109.4 . . ? H2S1 C2S H2S2 108.0 . . ? C2S C3S C4S 104.6(8) . . ? C2S C3S H3S1 110.8 . . ? C4S C3S H3S1 110.8 . . ? C2S C3S H3S2 110.8 . . ? C4S C3S H3S2 110.8 . . ? H3S1 C3S H3S2 108.9 . . ? O1S C4S C3S 109.1(9) . . ? C3S C4S O1SA 98.3(12) . . ? O1S C4S H4S1 109.9 . . ? C3S C4S H4S1 109.9 . . ? O1S C4S H4S2 109.9 . . ? C3S C4S H4S2 109.9 . . ? H4S1 C4S H4S2 108.3 . . ? C3S C4S H4S3 112.1 . . ? O1SA C4S H4S3 112.1 . . ? C3S C4S H4S4 112.1 . . ? O1SA C4S H4S4 112.1 . . ? H4S3 C4S H4S4 109.7 . . ? C8S O2S C5S 104.6(11) . . ? C8S O2S C5SA 107.6(8) . . ? C6S C5S O2S 101.8(16) . . ? C6S C5S H5S1 111.4 . . ? O2S C5S H5S1 111.4 . . ? C6S C5S H5S2 111.4 . . ? O2S C5S H5S2 111.4 . . ? H5S1 C5S H5S2 109.3 . . ? C5S C6S C7S 112.0(18) . . ? C5S C6S H6S1 109.2 . . ? C7S C6S H6S1 109.2 . . ? C5S C6S H6S2 109.2 . . ? C7S C6S H6S2 109.2 . . ? H6S1 C6S H6S2 107.9 . . ? C6SA C5SA O2S 107.5(12) . . ? C6SA C5SA H5S3 110.2 . . ? O2S C5SA H5S3 110.2 . . ? C6SA C5SA H5S4 110.2 . . ? O2S C5SA H5S4 110.2 . . ? H5S3 C5SA H5S4 108.5 . . ? C7S C6SA C5SA 104.5(14) . . ? C7S C6SA H6S3 110.9 . . ? C5SA C6SA H6S3 110.9 . . ? C7S C6SA H6S4 110.9 . . ? C5SA C6SA H6S4 110.9 . . ? H6S3 C6SA H6S4 108.9 . . ? C6SA C7S C8S 112.1(10) . . ? C8S C7S C6S 97.9(14) . . ? C8S C7S H7S1 112.2 . . ? C6S C7S H7S1 112.2 . . ? C8S C7S H7S2 112.2 . . ? C6S C7S H7S2 112.2 . . ? H7S1 C7S H7S2 109.8 . . ? C6SA C7S H7S3 109.2 . . ? C8S C7S H7S3 109.2 . . ? C6SA C7S H7S4 109.2 . . ? C8S C7S H7S4 109.2 . . ? H7S3 C7S H7S4 107.9 . . ? O2S C8S C7S 106.4(7) . . ? O2S C8S H8S1 110.5 . . ? C7S C8S H8S1 110.5 . . ? O2S C8S H8S2 110.5 . . ? C7S C8S H8S2 110.5 . . ? H8S1 C8S H8S2 108.6 . . ? C9S O3S C12S 106.0(8) . . ? O3S C12S C11S 108.7(10) . . ? O3S C12S H14S 110.0 . . ? C11S C12S H14S 110.0 . . ? O3S C12S H15S 110.0 . . ? C11S C12S H15S 110.0 . . ? H14S C12S H15S 108.3 . . ? C9S O3SA C13S 105.1(17) . . ? O3SA C13S C11S 109.1(17) . . ? O3SA C13S H16S 109.9 . . ? C11S C13S H16S 109.9 . . ? O3SA C13S H17S 109.9 . . ? C11S C13S H17S 109.9 . . ? H16S C13S H17S 108.3 . . ? O3S C9S C10S 103.5(7) . . ? O3SA C9S C10S 113.0(11) . . ? O3S C9S H20S 111.1 . . ? C10S C9S H20S 111.1 . . ? O3S C9S H21S 111.1 . . ? C10S C9S H21S 111.1 . . ? H20S C9S H21S 109.0 . . ? O3SA C9S H22S 109.0 . . ? C10S C9S H22S 109.0 . . ? O3SA C9S H23S 109.0 . . ? C10S C9S H23S 109.0 . . ? H22S C9S H23S 107.8 . . ? C9S C10S C11S 102.1(9) . . ? C9S C10S H24S 111.3 . . ? C11S C10S H24S 111.3 . . ? C9S C10S H25S 111.3 . . ? C11S C10S H25S 111.3 . . ? H24S C10S H25S 109.2 . . ? C12S C11S C10S 104.7(9) . . ? C10S C11S C13S 99.2(12) . . ? C12S C11S H26S 110.8 . . ? C10S C11S H26S 110.8 . . ? C12S C11S H27S 110.8 . . ? C10S C11S H27S 110.8 . . ? H26S C11S H27S 108.9 . . ? C10S C11S H28S 111.9 . . ? C13S C11S H28S 111.9 . . ? C10S C11S H29S 111.9 . . ? C13S C11S H29S 111.9 . . ? H28S C11S H29S 109.6 . . ? C18S O4S C18S 48(3) . 4_556 ? C18S O4S C15S 106(3) . 4_556 ? C18S O4S C15S 96.2(17) 4_556 4_556 ? C18S O4S C15S 96.2(17) . . ? C18S O4S C15S 106(3) 4_556 . ? C15S O4S C15S 156(3) 4_556 . ? C16S C15S O4S 113(2) . . ? C16S C15S H36S 109.0 . . ? O4S C15S H36S 109.0 . . ? C16S C15S H37S 108.9 . . ? O4S C15S H37S 109.0 . . ? H36S C15S H37S 107.8 . . ? C17S C16S C15S 107(2) . . ? C17S C16S H30S 110.2 . . ? C15S C16S H30S 110.2 . . ? C17S C16S H31S 110.2 . . ? C15S C16S H31S 110.2 . . ? H30S C16S H31S 108.5 . . ? C16S C17S C18S 107(2) . . ? C16S C17S H32S 110.2 . . ? C18S C17S H32S 110.2 . . ? C16S C17S H33S 110.2 . . ? C18S C17S H33S 110.2 . . ? H32S C17S H33S 108.5 . . ? C17S C18S O4S 112.2(19) . . ? C17S C18S H34S 109.2 . . ? O4S C18S H34S 109.2 . . ? C17S C18S H35S 109.2 . . ? O4S C18S H35S 109.2 . . ? H34S C18S H35S 107.9 . . ? _refine_diff_density_max 0.791 _refine_diff_density_min -0.872 # start Validation Reply Form _vrf_PLAT910_pld1367sm ; PROBLEM: Missing # of FCF Reflections Below Th(Min) ..... 29 Why ? RESPONSE: Few reflections could not be collected due to beam stop and high theta-min settings for data collection. ; # end Validation Reply Form _refine_diff_density_rms 0.081 _shelxl_version_number 2013-4 _shelx_res_file ; TITL pld1367sm in C222(1) CELL 0.71073 17.25700 22.70150 34.57330 90.0000 90.0000 90.0000 ZERR 4.00 0.00190 0.00250 0.00380 0.0000 0.0000 0.0000 LATT -7 SYMM -X, -Y, 0.5+Z SYMM -X, Y, 0.5-Z SYMM X, -Y, -Z SFAC C H N O Si K Fe Er UNIT 480 856 16 88 16 8 8 8 L.S. 15 BOND $H FMAP 2 PLAN 10 acta rigu isor .01 c35 c36 c37 c38 c8 c23 c23a c2s c6sa sadi o8 c31 o8 c34 sadi c31 c32 c32 c33 c33 c34 sadi c31 c33 c34 c32 rem sadi o1s c1s o1s c4s o1sa c1s o1sa c4s sadi c1s c2s c2s c3s c3s c4s sadi o1s c3s o1s c2s o1sa c3s o1sa c2s rem sadi o2s c5s o2s c8s o2s c5sa sadi c5s c6s c6s c7s c7s c8s c5sa c6sa c6sa c7s delu c5s c6s c5sa c6sa c7s c8s o2s c23 c23a c5 c6 c7 c8 rem sadi o3s c9s o3s c12s o3sa c9s o3sa c13s sadi c9s c10s c10s c11s c11s c12s c11s c13s rem free C18S C18S_$1 eqiv $1 x, -y, -z+1 SIZE 0.21 0.27 0.31 TEMP -173.000 WGHT 0.039000 6.582700 FVAR 0.03065 0.72112 0.41739 0.69106 0.20031 ER1 8 0.521340 0.236824 0.307852 11.00000 0.02365 0.01624 = 0.02017 0.00084 0.00053 -0.00232 FE1 7 0.646669 0.198408 0.373890 11.00000 0.02594 0.01487 = 0.03072 0.00404 -0.00732 -0.00341 K1 6 0.560024 0.142553 0.577781 11.00000 0.02960 0.03636 = 0.03115 0.00636 0.00467 0.00510 SI1 5 0.382434 0.184126 0.379352 11.00000 0.03478 0.02133 = 0.03116 0.00559 0.01044 0.00181 SI2 5 0.530150 0.381048 0.358292 11.00000 0.03198 0.01657 = 0.03161 -0.00321 -0.00282 -0.00086 N1 3 0.467483 0.179262 0.355857 11.00000 0.02224 0.02763 = 0.02249 0.00197 -0.00131 -0.00522 N2 3 0.565064 0.314755 0.344804 11.00000 0.03218 0.01558 = 0.02653 0.00025 -0.00601 -0.00147 O1 4 0.607037 0.068649 0.637183 11.00000 0.04347 0.02417 = 0.04838 0.00377 -0.01282 -0.00196 O2 4 0.449167 0.077879 0.616604 11.00000 0.03445 0.03703 = 0.03454 0.00697 0.00559 0.00272 O3 4 0.403112 0.167454 0.568148 11.00000 0.03268 0.04613 = 0.02952 0.00655 -0.00100 0.00714 O4 4 0.513721 0.217074 0.516466 11.00000 0.05219 0.03909 = 0.03498 0.00809 0.00946 0.00542 O5 4 0.672710 0.203854 0.534718 11.00000 0.04903 0.04654 = 0.03311 -0.00475 0.00852 -0.01376 O6 4 0.715401 0.106538 0.581232 11.00000 0.02756 0.03341 = 0.06359 -0.01096 -0.00963 -0.00302 O8 4 0.539241 0.242086 0.619179 11.00000 0.05915 0.06303 = 0.09694 -0.03420 0.03475 -0.02124 C31 1 0.481254 0.242092 0.648371 11.00000 0.06275 0.06412 = 0.07029 -0.01770 0.02179 -0.00718 AFIX 23 H31A 2 0.485067 0.206024 0.664353 11.00000 -1.20000 H31B 2 0.428997 0.243661 0.636600 11.00000 -1.20000 AFIX 0 C32 1 0.495270 0.295060 0.672287 11.00000 0.07877 0.06507 = 0.06580 -0.01869 0.00889 0.00457 AFIX 23 H32A 2 0.454312 0.324902 0.668040 11.00000 -1.20000 H32B 2 0.496831 0.284815 0.700110 11.00000 -1.20000 AFIX 0 C33 1 0.570979 0.316996 0.659101 11.00000 0.11664 0.05580 = 0.09147 -0.02111 0.00911 -0.02949 AFIX 23 H33A 2 0.570793 0.360551 0.657674 11.00000 -1.20000 H33B 2 0.612479 0.304469 0.677079 11.00000 -1.20000 AFIX 0 C34 1 0.582866 0.292294 0.621960 11.00000 0.06508 0.08042 = 0.08192 -0.01853 0.01086 -0.01948 AFIX 23 H34A 2 0.567142 0.320743 0.601726 11.00000 -1.20000 H34B 2 0.638383 0.282849 0.618272 11.00000 -1.20000 AFIX 0 same o8 > c34 part -1 O7 4 0.572925 0.053666 0.520372 10.50000 0.07144 0.02948 = 0.03892 -0.00497 -0.01674 0.00964 C35 1 0.515668 0.046782 0.491703 10.50000 0.06323 0.04349 = 0.04302 -0.00515 -0.01233 0.00952 AFIX 23 H35A 2 0.517343 0.079837 0.473044 10.50000 -1.20000 H35B 2 0.463412 0.045154 0.503470 10.50000 -1.20000 AFIX 0 C36 1 0.533973 -0.007874 0.472926 10.50000 0.11586 0.06299 = 0.07605 -0.02079 -0.04097 0.02399 AFIX 23 H36A 2 0.485774 -0.029385 0.466473 10.50000 -1.20000 H36B 2 0.562732 -0.000292 0.448654 10.50000 -1.20000 AFIX 0 C37 1 0.580232 -0.041997 0.498680 10.50000 0.08946 0.04264 = 0.05805 -0.01475 -0.02274 0.02075 AFIX 23 H37A 2 0.627507 -0.056350 0.485477 10.50000 -1.20000 H37B 2 0.550727 -0.076325 0.508425 10.50000 -1.20000 AFIX 0 C38 1 0.600278 -0.002591 0.530178 10.50000 0.08050 0.04154 = 0.05522 -0.00250 -0.01824 0.01320 AFIX 23 H38A 2 0.575951 -0.016143 0.554537 10.50000 -1.20000 H38B 2 0.657156 -0.001686 0.533864 10.50000 -1.20000 AFIX 0 part 0 C1 1 0.500000 0.301324 0.250000 10.50000 0.02424 0.01781 = 0.02136 0.00000 -0.00081 0.00000 AFIX 43 H1A 2 0.500001 0.343171 0.249999 10.50000 -1.20000 AFIX 0 C2 1 0.429923 0.270417 0.259257 11.00000 0.02130 0.02561 = 0.02077 -0.00322 0.00092 0.00029 AFIX 43 H2A 2 0.386054 0.291291 0.268621 11.00000 -1.20000 AFIX 0 C3 1 0.573501 0.205928 0.245883 11.00000 0.02698 0.02399 = 0.02454 0.00106 0.00069 0.00259 AFIX 43 H3A 2 0.622107 0.186309 0.246568 11.00000 -1.20000 AFIX 0 C4 1 0.500000 0.171711 0.250000 10.50000 0.03015 0.01602 = 0.02185 0.00000 0.00065 0.00000 C5 1 0.500000 0.108430 0.250000 10.50000 0.07434 0.01832 = 0.01197 0.00000 0.00191 0.00000 C6 1 0.569075 0.075067 0.245391 11.00000 0.09976 0.02583 = 0.02631 0.00034 -0.00340 0.02799 AFIX 43 H6A 2 0.617220 0.094842 0.242402 11.00000 -1.20000 AFIX 0 C7 1 0.567039 0.013620 0.245203 11.00000 0.15869 0.03104 = 0.02224 -0.00276 -0.00770 0.03304 AFIX 43 H7A 2 0.614120 -0.007360 0.241597 11.00000 -1.20000 AFIX 0 C8 1 0.500000 -0.017565 0.250000 10.50000 0.16585 0.02456 = 0.03193 0.00000 -0.00640 0.00000 AFIX 43 H8A 2 0.500000 -0.059413 0.249998 10.50000 -1.20000 AFIX 0 C9 1 0.537011 0.155278 0.369765 11.00000 0.02910 0.01627 = 0.02371 0.00159 -0.00481 -0.01037 C10 1 0.568826 0.154491 0.408195 11.00000 0.04391 0.02005 = 0.02667 0.00784 -0.00697 -0.00972 AFIX 43 H10A 2 0.544979 0.170885 0.430499 11.00000 -1.20000 AFIX 0 C11 1 0.641482 0.125337 0.407490 11.00000 0.04427 0.02104 = 0.03845 0.01050 -0.01570 -0.00794 AFIX 43 H11A 2 0.673196 0.117560 0.429362 11.00000 -1.20000 AFIX 0 C12 1 0.659172 0.109550 0.368362 11.00000 0.03936 0.01575 = 0.04688 0.00169 -0.01107 0.00187 AFIX 43 H12A 2 0.704771 0.090516 0.359372 11.00000 -1.20000 AFIX 0 C13 1 0.594485 0.128151 0.345493 11.00000 0.03135 0.01498 = 0.03390 0.00116 -0.00427 -0.00467 AFIX 43 H13A 2 0.590171 0.123288 0.318286 11.00000 -1.20000 AFIX 0 C14 1 0.632593 0.288959 0.358746 11.00000 0.02828 0.01546 = 0.03364 0.00388 -0.00657 -0.00772 C15 1 0.657424 0.280469 0.398359 11.00000 0.04247 0.01973 = 0.03534 0.00228 -0.01364 -0.00560 AFIX 43 H15A 2 0.630669 0.293049 0.420908 11.00000 -1.20000 AFIX 0 C16 1 0.730492 0.249294 0.397259 11.00000 0.03685 0.02251 = 0.05398 0.00504 -0.02179 -0.00812 AFIX 43 H16A 2 0.761015 0.239175 0.419140 11.00000 -1.20000 AFIX 0 C17 1 0.749112 0.236343 0.358443 11.00000 0.02545 0.02984 = 0.05673 0.00879 -0.00642 -0.00237 AFIX 43 H17A 2 0.793875 0.215939 0.349706 11.00000 -1.20000 AFIX 0 C18 1 0.688806 0.259324 0.334689 11.00000 0.02462 0.02449 = 0.03880 0.00473 -0.00203 -0.00708 AFIX 43 H18A 2 0.686014 0.255723 0.307349 11.00000 -1.20000 AFIX 0 C19 1 0.387057 0.220917 0.427406 11.00000 0.08703 0.04891 = 0.03356 0.00074 0.00577 0.03487 AFIX 137 H19A 2 0.416643 0.257607 0.425171 11.00000 -1.50000 H19B 2 0.412533 0.194745 0.446020 11.00000 -1.50000 H19C 2 0.334430 0.229770 0.436330 11.00000 -1.50000 AFIX 0 C20 1 0.314192 0.228227 0.348438 11.00000 0.03389 0.03275 = 0.04065 0.00735 0.00964 0.00270 AFIX 137 H20A 2 0.335370 0.267840 0.344543 11.00000 -1.50000 H20B 2 0.263743 0.231068 0.361319 11.00000 -1.50000 H20C 2 0.307876 0.208770 0.323332 11.00000 -1.50000 AFIX 0 C21 1 0.336677 0.107892 0.386626 11.00000 0.03571 0.02738 = 0.09358 0.02357 0.01927 0.00155 C22 1 0.387691 0.072401 0.415201 11.00000 0.05793 0.03259 = 0.08233 0.02137 0.01650 -0.00252 AFIX 137 H22A 2 0.367244 0.032299 0.417637 11.00000 -1.50000 H22B 2 0.387113 0.091637 0.440575 11.00000 -1.50000 H22C 2 0.440984 0.070817 0.405466 11.00000 -1.50000 AFIX 0 part 1 C23 1 0.265208 0.121006 0.416456 10.50000 0.05151 0.06797 = 0.12075 0.05324 0.03150 0.01303 AFIX 33 H23A 2 0.234466 0.085089 0.419893 10.50000 -1.50000 H23B 2 0.232265 0.152241 0.405851 10.50000 -1.50000 H23C 2 0.286056 0.133549 0.441503 10.50000 -1.50000 AFIX 0 part 2 C23A 1 0.249469 0.108744 0.396081 10.50000 0.04027 0.02673 = 0.05721 -0.01041 0.01401 -0.01413 AFIX 33 H23D 2 0.234443 0.070947 0.407539 10.50000 -1.50000 H23E 2 0.219847 0.115246 0.372277 10.50000 -1.50000 H23F 2 0.238625 0.140581 0.414443 10.50000 -1.50000 AFIX 0 part 0 C24 1 0.334202 0.076690 0.347019 11.00000 0.07962 0.04070 = 0.10371 -0.00300 -0.00873 -0.02375 AFIX 137 H24A 2 0.312161 0.037190 0.350137 11.00000 -1.50000 H24B 2 0.386876 0.073530 0.336631 11.00000 -1.50000 H24C 2 0.301997 0.099524 0.329123 11.00000 -1.50000 AFIX 0 C25 1 0.516759 0.390017 0.412208 11.00000 0.09192 0.04453 = 0.03897 -0.01403 0.00199 0.01294 AFIX 137 H25A 2 0.485120 0.357529 0.422157 11.00000 -1.50000 H25B 2 0.490728 0.427533 0.417483 11.00000 -1.50000 H25C 2 0.567484 0.389642 0.424950 11.00000 -1.50000 AFIX 0 C26 1 0.432926 0.391648 0.335651 11.00000 0.02872 0.03111 = 0.05186 -0.01135 0.00581 0.00191 AFIX 137 H26A 2 0.437202 0.386815 0.307565 11.00000 -1.50000 H26B 2 0.413860 0.431316 0.341520 11.00000 -1.50000 H26C 2 0.396682 0.362376 0.345984 11.00000 -1.50000 AFIX 0 C27 1 0.595958 0.442858 0.340796 11.00000 0.03293 0.01968 = 0.06678 0.00458 -0.01386 -0.00429 C28 1 0.677727 0.433185 0.356854 11.00000 0.03469 0.02450 = 0.10847 0.00566 -0.02314 -0.00949 AFIX 137 H28A 2 0.712076 0.464454 0.347475 11.00000 -1.50000 H28B 2 0.697278 0.394871 0.348176 11.00000 -1.50000 H28C 2 0.676127 0.434043 0.385183 11.00000 -1.50000 AFIX 0 C29 1 0.568470 0.503830 0.353456 11.00000 0.06173 0.01942 = 0.11120 -0.00348 -0.02783 -0.00081 AFIX 137 H29A 2 0.603515 0.533858 0.343030 11.00000 -1.50000 H29B 2 0.568326 0.506036 0.381764 11.00000 -1.50000 H29C 2 0.515928 0.510718 0.343697 11.00000 -1.50000 AFIX 0 C30 1 0.600742 0.440857 0.296421 11.00000 0.05196 0.04951 = 0.07155 0.02397 -0.00397 -0.02152 AFIX 137 H30A 2 0.641956 0.467303 0.287547 11.00000 -1.50000 H30B 2 0.551133 0.453449 0.285377 11.00000 -1.50000 H30C 2 0.612186 0.400543 0.288046 11.00000 -1.50000 AFIX 0 C39 1 0.681508 0.042863 0.632414 11.00000 0.04357 0.02947 = 0.07722 0.00500 -0.02572 0.00372 AFIX 23 H39A 2 0.678522 0.010301 0.613425 11.00000 -1.20000 H39B 2 0.699460 0.026396 0.657369 11.00000 -1.20000 AFIX 0 C40 1 0.737199 0.088010 0.618674 11.00000 0.03655 0.03722 = 0.08283 -0.00136 -0.01948 0.00161 AFIX 23 H40A 2 0.737209 0.122071 0.636556 11.00000 -1.20000 H40B 2 0.790151 0.071259 0.618035 11.00000 -1.20000 AFIX 0 C41 1 0.769935 0.147419 0.565498 11.00000 0.03102 0.05013 = 0.06661 -0.01591 -0.00160 -0.01041 AFIX 23 H41A 2 0.820583 0.127799 0.561641 11.00000 -1.20000 H41B 2 0.777379 0.180716 0.583612 11.00000 -1.20000 AFIX 0 C42 1 0.740238 0.169413 0.528110 11.00000 0.04155 0.05599 = 0.05146 -0.02179 0.01013 -0.01430 AFIX 23 H42A 2 0.780325 0.193663 0.515225 11.00000 -1.20000 H42B 2 0.727595 0.135808 0.510986 11.00000 -1.20000 AFIX 0 C43 1 0.645820 0.231776 0.499913 11.00000 0.06626 0.07788 = 0.03075 0.01296 0.00539 -0.01833 AFIX 23 H43A 2 0.639418 0.202054 0.479204 11.00000 -1.20000 H43B 2 0.684108 0.261356 0.491113 11.00000 -1.20000 AFIX 0 C44 1 0.570760 0.260717 0.507954 11.00000 0.07924 0.05542 = 0.03550 0.01915 -0.00028 -0.01372 AFIX 23 H44A 2 0.576285 0.287852 0.530200 11.00000 -1.20000 H44B 2 0.554377 0.284030 0.485178 11.00000 -1.20000 AFIX 0 C45 1 0.440381 0.242505 0.525023 11.00000 0.06588 0.04580 = 0.02728 0.00636 0.00666 0.02211 AFIX 23 H45A 2 0.422850 0.267157 0.503083 11.00000 -1.20000 H45B 2 0.444395 0.267808 0.548259 11.00000 -1.20000 AFIX 0 C46 1 0.383379 0.193632 0.532100 11.00000 0.04156 0.05875 = 0.02369 0.00202 -0.00007 0.02079 AFIX 23 H46A 2 0.329953 0.209459 0.533009 11.00000 -1.20000 H46B 2 0.386382 0.164070 0.511102 11.00000 -1.20000 AFIX 0 C47 1 0.351309 0.121349 0.578635 11.00000 0.02938 0.04421 = 0.04946 -0.00063 0.00274 0.00858 AFIX 23 H47A 2 0.355224 0.088501 0.559902 11.00000 -1.20000 H47B 2 0.297273 0.135994 0.578606 11.00000 -1.20000 AFIX 0 C48 1 0.372962 0.100833 0.617809 11.00000 0.03126 0.04285 = 0.05313 0.00706 0.01343 -0.00036 AFIX 23 H48A 2 0.370429 0.134054 0.636316 11.00000 -1.20000 H48B 2 0.336401 0.069964 0.626531 11.00000 -1.20000 AFIX 0 C49 1 0.474022 0.056140 0.653550 11.00000 0.05845 0.03648 = 0.03129 0.00691 0.00709 0.00339 AFIX 23 H49A 2 0.435127 0.028280 0.663961 11.00000 -1.20000 H49B 2 0.479418 0.089235 0.672001 11.00000 -1.20000 AFIX 0 C50 1 0.550417 0.025543 0.648713 11.00000 0.05614 0.03173 = 0.03029 0.00545 -0.00566 -0.00236 AFIX 23 H50A 2 0.566149 0.006917 0.673385 11.00000 -1.20000 H50B 2 0.546149 -0.005582 0.628770 11.00000 -1.20000 AFIX 0 mole 3 part 1 O1S 4 0.618489 0.162962 0.778036 21.00000 0.09129 0.13243 = 0.08930 -0.02272 0.00391 0.00886 part 2 O1SA 4 0.672057 0.204695 0.773185 -21.00000 0.16168 0.13754 = 0.15912 -0.03609 -0.01900 0.04626 part 0 C1S 1 0.610611 0.202500 0.741668 11.00000 0.11072 0.17145 = 0.12152 -0.01209 0.00892 0.06823 part 1 AFIX 23 H1S1 2 0.556431 0.203268 0.732270 21.00000 -1.20000 H1S2 2 0.627563 0.243302 0.747196 21.00000 -1.20000 AFIX 23 part 2 H1S3 2 0.565596 0.177688 0.748716 -21.00000 -1.20000 H1S4 2 0.593083 0.242084 0.733432 -21.00000 -1.20000 AFIX 0 part 0 C2S 1 0.661052 0.174753 0.713866 11.00000 0.20526 0.16195 = 0.12834 0.00733 0.02834 0.06616 AFIX 23 H2S1 2 0.629571 0.157624 0.692735 11.00000 -1.20000 H2S2 2 0.695912 0.204715 0.702459 11.00000 -1.20000 AFIX 0 C3S 1 0.706164 0.129615 0.731433 11.00000 0.08843 0.09206 = 0.11203 -0.00875 0.01540 0.00134 AFIX 23 H3S1 2 0.761886 0.135007 0.725616 11.00000 -1.20000 H3S2 2 0.689763 0.090266 0.722194 11.00000 -1.20000 AFIX 0 C4S 1 0.691514 0.135949 0.772656 11.00000 0.09537 0.10236 = 0.09911 -0.04023 -0.01772 -0.00019 part 1 AFIX 23 H4S1 2 0.692025 0.096771 0.785229 21.00000 -1.20000 H4S2 2 0.732562 0.160384 0.784604 21.00000 -1.20000 AFIX 23 part 2 H4S3 2 0.737799 0.126450 0.788382 -21.00000 -1.20000 H4S4 2 0.647072 0.111738 0.781323 -21.00000 -1.20000 AFIX 0 part 0 mole 4 O2S 4 0.851479 0.129315 0.452758 11.00000 0.11894 0.08441 = 0.08478 -0.01357 -0.00213 0.01975 part 1 C5S 1 0.905768 0.090715 0.471310 31.00000 0.11578 0.06796 = 0.06732 -0.00536 -0.00420 0.00764 AFIX 23 H5S1 2 0.957394 0.109359 0.473773 31.00000 -1.20000 H5S2 2 0.887349 0.078581 0.497232 31.00000 -1.20000 AFIX 0 C6S 1 0.907614 0.042060 0.445161 31.00000 0.22954 0.10258 = 0.09056 -0.02570 -0.05900 0.07387 AFIX 23 H6S1 2 0.883044 0.007493 0.457586 31.00000 -1.20000 H6S2 2 0.962197 0.031807 0.439473 31.00000 -1.20000 AFIX 0 part 2 C5SA 1 0.858755 0.072159 0.472936 -31.00000 0.12039 0.08500 = 0.06707 -0.00461 -0.01026 0.04509 AFIX 23 H5S3 2 0.908442 0.070318 0.487198 -31.00000 -1.20000 H5S4 2 0.815848 0.067158 0.491657 -31.00000 -1.20000 AFIX 0 C6SA 1 0.855798 0.025664 0.443438 -31.00000 0.13107 0.08188 = 0.09308 -0.00555 0.00868 0.01724 AFIX 23 H6S3 2 0.897197 -0.003802 0.447750 -31.00000 -1.20000 H6S4 2 0.804983 0.005431 0.443778 -31.00000 -1.20000 AFIX 0 part 0 C7S 1 0.866958 0.055241 0.408527 11.00000 0.15867 0.09294 = 0.07257 -0.01691 -0.01949 0.05322 part 1 AFIX 23 H7S1 2 0.897918 0.043929 0.385593 31.00000 -1.20000 H7S2 2 0.815290 0.036388 0.407269 31.00000 -1.20000 AFIX 23 part 2 H7S3 2 0.827435 0.042026 0.389674 -31.00000 -1.20000 H7S4 2 0.918595 0.044997 0.398019 -31.00000 -1.20000 AFIX 0 part 0 C8S 1 0.861702 0.118835 0.413074 11.00000 0.05514 0.09153 = 0.07909 0.00492 0.00353 0.00538 AFIX 23 H8S1 2 0.909683 0.138039 0.403727 11.00000 -1.20000 H8S2 2 0.817255 0.134541 0.398194 11.00000 -1.20000 AFIX 0 mole 5 part 1 O3S 4 0.331679 0.402787 0.688328 41.00000 0.07020 0.10435 = 0.03811 -0.00406 0.01363 -0.02282 C12S 1 0.270244 0.389426 0.714157 41.00000 0.07268 0.10815 = 0.07421 -0.01130 0.01866 -0.01823 AFIX 23 H14S 2 0.243986 0.352727 0.705941 41.00000 -1.20000 H15S 2 0.231700 0.421726 0.714049 41.00000 -1.20000 AFIX 0 part 2 O3SA 4 0.316895 0.456963 0.701634 -41.00000 0.09196 0.13958 = 0.11593 0.04259 0.04085 -0.00519 C13S 1 0.265557 0.437856 0.731253 -41.00000 0.08695 0.10438 = 0.04505 -0.01881 0.01260 -0.03830 AFIX 23 H16S 2 0.214688 0.427477 0.719904 -41.00000 -1.20000 H17S 2 0.257534 0.469954 0.750219 -41.00000 -1.20000 AFIX 0 part 0 C9S 1 0.389008 0.430670 0.710692 11.00000 0.08631 0.08252 = 0.08579 -0.00248 0.01383 -0.02678 part 1 AFIX 23 H20S 2 0.376318 0.472711 0.714908 41.00000 -1.20000 H21S 2 0.440406 0.427810 0.698113 41.00000 -1.20000 AFIX 23 part 2 H22S 2 0.429059 0.461796 0.712298 -41.00000 -1.20000 H23S 2 0.403797 0.403554 0.689516 -41.00000 -1.20000 AFIX 0 part 0 C10S 1 0.387633 0.397249 0.747909 11.00000 0.09540 0.10238 = 0.07312 -0.01593 0.01396 0.00094 AFIX 23 H24S 2 0.406057 0.421837 0.769697 11.00000 -1.20000 H25S 2 0.419683 0.361160 0.746329 11.00000 -1.20000 AFIX 0 C11S 1 0.301551 0.382294 0.752145 11.00000 0.10512 0.17352 = 0.10355 0.03808 0.03110 -0.02241 part 1 AFIX 23 H26S 2 0.294679 0.341310 0.761310 41.00000 -1.20000 H27S 2 0.276062 0.409366 0.770642 41.00000 -1.20000 AFIX 23 part 2 H28S 2 0.285629 0.379882 0.779610 -41.00000 -1.20000 H29S 2 0.288003 0.345144 0.738759 -41.00000 -1.20000 part 0 AFIX 0 same o8 > c34 O4S 4 0.115532 0.000000 0.500000 10.50000 51.00000 C15S 1 0.097779 0.056468 0.482063 10.50000 51.00000 AFIX 23 H36S 2 0.103460 0.052681 0.453678 10.50000 -1.20000 H37S 2 0.043103 0.066678 0.487561 10.50000 -1.20000 AFIX 0 C16S 1 0.143646 0.100501 0.494577 10.50000 51.00000 AFIX 23 H30S 2 0.158298 0.126395 0.472728 10.50000 -1.20000 H31S 2 0.116110 0.124489 0.514146 10.50000 -1.20000 AFIX 0 C17S 1 0.205935 0.076316 0.509904 10.50000 51.00000 AFIX 23 H32S 2 0.216461 0.093642 0.535652 10.50000 -1.20000 H33S 2 0.251511 0.083302 0.493130 10.50000 -1.20000 AFIX 0 C18S 1 0.191774 0.015882 0.513332 10.50000 51.00000 AFIX 23 H34S 2 0.197357 0.004144 0.540769 10.50000 -1.20000 H35S 2 0.230944 -0.006013 0.498133 10.50000 -1.20000 part 0 AFIX 0 HKLF 4 REM pld1367sm in C222(1) REM R1 = 0.0316 for 15396 Fo > 4sig(Fo) and 0.0373 for all 16722 data REM 785 parameters refined using 1143 restraints END WGHT 0.0389 6.5687 REM Highest difference peak 0.791, deepest hole -0.872, 1-sigma level 0.081 Q1 1 0.4971 0.2663 0.3091 11.00000 0.05 0.79 Q2 1 0.1815 0.0935 0.5043 11.00000 0.05 0.71 Q3 1 0.5410 0.2306 0.2852 11.00000 0.05 0.69 Q4 1 0.4749 0.2392 0.3269 11.00000 0.05 0.64 Q5 1 0.5367 0.2340 0.3312 11.00000 0.05 0.61 Q6 1 0.1269 0.0703 0.4889 11.00000 0.05 0.60 Q7 1 0.5202 0.1874 0.3064 11.00000 0.05 0.60 Q8 1 0.5379 0.2692 0.3160 11.00000 0.05 0.56 Q9 1 0.4661 0.2411 0.2960 11.00000 0.05 0.55 Q10 1 0.5608 0.2390 0.4250 11.00000 0.05 0.54 ; _shelx_res_checksum 13699 _shelx_hkl_file ; -4 0 0 19.09 0.99 -4 0 0 18.88 1.03 -6 0 0 50.64 2.41 -6 0 0 51.41 2.53 -6 0 0 52.12 2.45 -8 0 0 30.73 1.54 -8 0 0 30.98 1.60 -8 0 0 30.63 1.68 -10 0 0 12.06 0.79 -10 0 0 12.58 0.89 -10 0 0 14.20 0.99 -12 0 0 0.58 0.30 12 0 0 0.20 0.41 -12 0 0 -0.04 0.39 -14 0 0 3.41 0.62 14 0 0 2.34 0.29 14 0 0 2.78 0.70 -14 0 0 2.75 0.50 16 0 0 8.19 1.11 -16 0 0 10.14 1.03 -18 0 0 17.07 1.45 18 0 0 18.22 1.63 -20 0 0 12.96 1.37 -22 0 0 21.48 1.95 -3 -1 0 1.94 0.23 -5 1 0 1.31 0.24 -5 -1 0 0.72 0.24 -5 1 0 1.05 0.26 -5 1 0 1.50 0.22 5 1 0 1.65 0.29 -5 -1 0 1.45 0.21 -7 1 0 0.17 0.20 -7 1 0 -0.31 0.23 7 1 0 0.11 0.25 -7 -1 0 0.31 0.19 -7 1 0 0.01 0.26 -7 -1 0 -0.23 0.25 -9 -1 0 2.31 0.44 -9 1 0 2.54 0.46 9 1 0 2.27 0.21 9 1 0 2.40 0.44 -9 1 0 1.74 0.38 -9 -1 0 2.68 0.33 -9 1 0 2.20 0.34 -11 -1 0 5.53 0.63 -11 1 0 6.31 0.63 11 1 0 5.62 0.40 -11 1 0 5.47 0.53 11 1 0 5.65 0.70 -11 -1 0 5.43 0.52 -11 1 0 5.42 0.67 -13 -1 0 0.08 0.42 -13 1 0 -0.15 0.32 -13 1 0 -0.33 0.38 13 1 0 0.00 0.46 13 1 0 -0.17 0.17 -13 1 0 -0.41 0.45 -13 -1 0 0.19 0.32 15 -1 0 0.29 0.59 -15 -1 0 0.55 0.54 -15 1 0 0.68 0.52 -15 1 0 0.11 0.41 15 1 0 0.29 0.61 17 1 0 0.39 0.71 -17 -1 0 0.45 0.64 17 -1 0 1.21 0.73 -17 1 0 0.92 0.60 -19 1 0 1.50 0.76 -19 -1 0 1.70 0.78 -21 1 0 0.89 0.80 -21 -1 0 0.50 0.85 -4 -2 0 159.91 7.16 -4 2 0 160.37 7.16 -4 2 0 162.07 7.13 -4 2 0 157.83 7.34 4 2 0 150.18 7.35 -6 -2 0 162.96 7.41 -6 2 0 165.14 7.43 -6 -2 0 162.94 7.44 -6 2 0 163.65 7.64 -6 2 0 165.11 7.41 6 2 0 158.10 7.65 6 2 0 165.30 8.20 8 2 0 76.42 3.83 -8 2 0 75.54 3.79 8 2 0 80.34 3.96 -8 -2 0 75.78 3.62 -8 2 0 79.32 3.65 -8 2 0 79.80 3.67 -8 -2 0 76.98 3.70 -10 -2 0 2.15 0.33 -10 -2 0 1.72 0.43 -10 2 0 1.74 0.34 10 2 0 1.61 0.24 10 2 0 2.14 0.48 -10 2 0 2.05 0.39 -10 2 0 1.78 0.45 12 2 0 -0.20 0.18 -12 2 0 0.35 0.44 -12 2 0 -0.09 0.36 -12 2 0 0.20 0.31 -12 -2 0 -0.02 0.38 12 2 0 0.73 0.45 -12 -2 0 0.00 0.26 -14 2 0 0.34 0.54 -14 2 0 -0.02 0.39 -14 -2 0 -0.16 0.37 14 2 0 0.61 0.56 -14 -2 0 -0.15 0.45 -14 2 0 0.07 0.43 -16 2 0 7.59 0.90 -16 -2 0 8.21 0.99 16 2 0 7.51 1.04 -18 -2 0 27.19 1.90 -18 2 0 25.52 1.81 18 -2 0 26.46 1.99 -20 -2 0 14.08 1.47 -20 2 0 15.05 1.47 -22 -2 0 16.44 1.72 -22 2 0 17.42 1.66 -3 3 0 169.00 7.45 3 -3 0 166.64 8.22 -3 -3 0 164.64 7.43 -3 3 0 159.53 7.62 3 3 0 162.34 7.63 5 3 0 7.14 0.58 -5 3 0 7.45 0.51 -5 3 0 8.05 0.58 -5 3 0 7.69 0.50 -5 -3 0 8.19 0.52 -7 -3 0 30.38 1.50 -7 3 0 29.38 1.51 -7 -3 0 29.87 1.57 -7 3 0 29.12 1.60 -7 3 0 30.06 1.52 7 3 0 31.87 1.64 -9 -3 0 1.69 0.40 -9 -3 0 1.79 0.31 -9 3 0 1.80 0.43 -9 3 0 1.88 0.36 9 3 0 1.71 0.27 9 3 0 1.73 0.43 -9 3 0 2.00 0.35 11 3 0 3.56 0.59 -11 -3 0 3.15 0.52 -11 3 0 4.10 0.53 -11 3 0 3.02 0.56 -11 3 0 2.98 0.45 -11 -3 0 3.46 0.42 11 3 0 3.65 0.39 13 3 0 -0.62 0.42 -13 3 0 0.24 0.35 -13 3 0 0.12 0.40 -13 -3 0 0.26 0.46 -13 3 0 0.31 0.48 -13 -3 0 0.48 0.31 -15 3 0 0.41 0.60 15 3 0 -0.16 0.55 -15 3 0 0.68 0.49 -15 -3 0 0.22 0.54 -15 3 0 0.21 0.43 -17 3 0 0.19 0.59 -17 -3 0 1.49 0.70 17 3 0 0.62 0.69 -19 3 0 0.19 0.66 19 -3 0 -1.41 0.78 -19 -3 0 -0.31 0.71 -21 -3 0 2.11 0.93 -21 3 0 0.95 0.82 2 -4 0 413.99 18.87 2 4 0 412.22 19.29 -2 4 0 425.95 19.30 2 -4 0 426.28 20.99 -4 -4 0 134.72 6.05 4 4 0 133.32 6.21 4 -4 0 132.38 6.66 -4 -4 0 133.92 6.06 -4 4 0 134.89 6.07 -4 4 0 128.57 6.21 -6 -4 0 103.80 4.71 -6 -4 0 96.69 4.72 -6 4 0 105.87 4.73 -6 4 0 102.32 4.67 -6 4 0 101.62 4.86 6 4 0 102.57 4.87 -8 4 0 18.68 1.08 -8 -4 0 19.62 1.16 8 4 0 19.94 1.21 -8 4 0 19.28 1.07 -8 -4 0 19.58 1.07 -8 4 0 19.69 1.18 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9.35 0.85 -10 6 0 10.87 0.81 10 6 0 10.84 0.89 -10 6 0 10.12 0.88 -10 6 0 9.37 0.73 -10 -6 0 10.11 0.73 -12 6 0 1.97 0.53 -12 6 0 1.10 0.43 12 6 0 1.37 0.48 -12 -6 0 1.09 0.48 -12 6 0 1.42 0.41 -12 -6 0 1.45 0.36 -14 -6 0 14.04 1.21 -14 6 0 14.95 1.08 -14 6 0 13.87 1.09 -14 6 0 12.80 1.26 14 6 0 15.67 1.25 16 6 0 11.79 1.25 -16 -6 0 13.26 1.26 -16 6 0 10.66 1.07 -16 6 0 12.61 1.32 -18 -6 0 14.96 1.48 -18 6 0 14.84 1.52 -20 6 0 9.84 1.53 -20 -6 0 12.01 1.40 -22 -6 0 8.53 1.40 1 -7 0 66.22 3.10 1 7 0 66.62 3.18 -1 -7 0 63.65 3.43 -1 7 0 65.61 3.18 1 -7 0 65.53 3.42 -1 -7 0 67.07 3.09 -3 -7 0 16.31 0.89 -3 -7 0 16.14 0.89 3 -7 0 16.76 0.95 3 7 0 17.10 0.95 3 -7 0 15.28 0.96 -3 7 0 16.34 0.97 -5 -7 0 70.15 3.26 5 7 0 67.96 3.34 -5 7 0 66.98 3.35 5 -7 0 69.79 3.29 -5 -7 0 70.63 3.23 5 -7 0 66.87 3.53 7 7 0 98.33 4.77 -7 7 0 102.34 4.54 7 -7 0 97.45 4.67 7 -7 0 101.38 5.03 -7 7 0 99.47 4.80 -7 -7 0 98.79 4.64 7 -7 0 96.87 5.03 -7 -7 0 98.33 4.65 -9 -7 0 7.17 0.66 9 -7 0 8.22 0.51 -9 -7 0 7.02 0.72 9 7 0 7.33 0.72 -9 7 0 6.94 0.60 -9 7 0 8.42 0.81 9 -7 0 9.59 0.53 -11 -7 0 4.15 0.50 -11 7 0 4.06 0.65 11 7 0 4.24 0.63 -11 7 0 3.75 0.50 -11 -7 0 3.52 0.62 -13 7 0 0.32 0.41 13 7 0 0.73 0.50 -13 -7 0 1.36 0.56 -13 7 0 0.65 0.56 -15 -7 0 11.02 1.12 15 7 0 9.69 1.10 -15 7 0 10.62 1.04 -15 7 0 10.38 1.17 -17 -7 0 12.21 1.30 -17 7 0 13.84 1.41 -19 -7 0 7.90 1.20 -19 7 0 9.85 1.35 -21 -7 0 4.34 1.12 0 -8 0 107.74 5.42 0 8 0 105.75 5.00 0 -8 0 101.68 4.86 -2 -8 0 67.46 3.63 2 -8 0 69.03 3.61 2 -8 0 68.99 3.29 -2 -8 0 71.56 3.26 2 8 0 69.07 3.36 -2 -8 0 69.70 3.20 -2 8 0 69.25 3.37 4 -8 0 420.95 21.05 4 -8 0 411.19 18.96 -4 -8 0 428.48 18.86 4 8 0 421.11 19.38 -4 -8 0 421.41 18.91 -4 8 0 416.65 19.39 6 -8 0 36.36 1.99 6 -8 0 38.71 2.09 6 8 0 39.80 2.04 -6 8 0 40.55 1.87 -6 8 0 39.23 2.08 -6 -8 0 40.25 2.00 -6 -8 0 39.27 1.95 -8 8 0 0.75 0.25 8 -8 0 0.13 0.19 8 -8 0 1.51 0.39 -8 -8 0 0.57 0.37 -8 8 0 1.01 0.41 8 8 0 0.56 0.32 8 -8 0 0.42 0.20 -8 -8 0 0.58 0.33 -10 -8 0 1.31 0.43 10 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5.95 0.70 9 9 0 7.04 0.69 9 -9 0 6.53 0.53 9 -9 0 7.23 0.72 -11 -9 0 1.10 0.38 -11 -9 0 0.56 0.46 11 -9 0 0.76 0.25 11 -9 0 0.75 0.44 11 9 0 0.92 0.43 -11 9 0 1.10 0.54 -13 9 0 1.03 0.62 13 -9 0 1.14 0.27 -13 -9 0 1.15 0.60 13 9 0 1.55 0.57 13 -9 0 0.77 0.52 -15 -9 0 2.77 0.77 15 9 0 3.34 0.76 15 -9 0 4.92 0.77 -15 9 0 4.45 0.86 15 -9 0 3.81 0.40 17 -9 0 9.13 0.68 -17 9 0 8.22 1.18 17 -9 0 11.86 1.17 -17 -9 0 10.19 1.23 -19 -9 0 4.11 1.06 -19 9 0 2.57 1.02 19 -9 0 2.88 0.39 -21 -9 0 1.32 1.02 0 -10 0 3.96 0.45 0 -10 0 4.39 0.54 0 10 0 4.25 0.51 2 -10 0 94.39 4.92 -2 -10 0 95.29 4.35 2 -10 0 91.70 4.46 -2 -10 0 93.02 4.43 -2 10 0 94.77 4.58 2 10 0 94.14 4.57 -2 -10 0 99.10 4.96 -4 -10 0 176.51 8.00 4 -10 0 171.58 8.89 -4 10 0 177.93 8.25 4 10 0 176.60 8.23 4 -10 0 172.55 8.06 -4 -10 0 173.06 7.95 -6 10 0 3.04 0.52 6 -10 0 2.80 0.49 6 10 0 2.67 0.44 -6 -10 0 3.18 0.42 6 -10 0 2.38 0.37 -6 -10 0 2.26 0.41 -8 10 0 2.55 0.49 8 10 0 2.16 0.44 -8 -10 0 3.02 0.51 8 -10 0 2.27 0.45 8 -10 0 3.01 0.39 -8 -10 0 1.97 0.41 -10 -10 0 10.04 0.92 10 -10 0 9.85 0.73 10 10 0 9.47 0.88 -10 10 0 10.03 0.98 10 -10 0 10.43 0.90 -10 -10 0 10.78 0.86 12 10 0 1.00 0.50 -12 -10 0 0.25 0.54 12 -10 0 -0.60 0.42 12 -10 0 -0.15 0.25 -12 10 0 0.02 0.47 14 -10 0 14.26 0.93 -14 -10 0 12.89 1.27 14 -10 0 15.04 1.25 -14 10 0 14.57 1.38 14 10 0 14.16 1.22 -16 10 0 -0.12 0.69 16 -10 0 1.03 0.65 -16 -10 0 0.59 0.72 16 -10 0 0.54 0.30 -18 10 0 4.01 1.07 -18 -10 0 4.77 1.02 18 -10 0 3.29 0.44 -20 -10 0 8.28 1.32 -20 10 0 6.62 1.29 20 -10 0 7.10 0.66 -1 -11 0 80.20 3.58 -1 11 0 78.34 3.83 1 -11 0 77.40 3.73 -1 -11 0 78.19 4.13 1 11 0 76.72 3.81 1 -11 0 75.49 4.11 -1 -11 0 77.67 3.71 3 -11 0 209.88 9.83 -3 -11 0 214.31 9.70 -3 11 0 208.40 10.06 -3 -11 0 211.37 9.78 3 11 0 210.68 10.05 -3 -11 0 224.82 10.94 3 -11 0 220.57 10.90 -5 -11 0 66.97 3.20 -5 11 0 66.43 3.35 5 11 0 68.47 3.34 5 -11 0 67.79 3.29 5 -11 0 63.92 3.53 -5 -11 0 66.14 3.20 -7 -11 0 -0.34 0.28 7 11 0 0.46 0.33 7 -11 0 0.05 0.36 -7 -11 0 0.07 0.33 7 -11 0 0.20 0.26 -7 11 0 -0.20 0.36 9 11 0 1.45 0.45 -9 -11 0 1.02 0.47 9 -11 0 1.41 0.49 -9 -11 0 1.49 0.42 -9 11 0 0.12 0.45 9 -11 0 0.72 0.30 11 11 0 4.30 0.69 11 -11 0 6.03 0.80 -11 -11 0 4.91 0.75 11 -11 0 4.45 0.52 -11 11 0 5.83 0.83 -13 11 0 1.13 0.65 13 -11 0 0.46 0.31 13 11 0 0.74 0.53 -13 -11 0 0.31 0.60 13 -11 0 0.60 0.54 15 11 0 0.23 0.58 -15 11 0 0.12 0.70 -15 -11 0 -0.20 0.68 15 -11 0 0.25 0.30 15 -11 0 -0.26 0.54 -17 -11 0 3.09 0.91 -17 11 0 2.08 0.86 17 -11 0 3.69 0.83 17 -11 0 2.76 0.45 -19 -11 0 8.36 1.26 19 -11 0 7.03 0.71 -19 11 0 6.57 1.27 -21 -11 0 8.71 1.43 21 -11 0 8.07 0.78 0 -12 0 2.88 0.51 0 -12 0 2.72 0.44 0 -12 0 3.05 0.29 0 12 0 2.40 0.43 -2 -12 0 60.63 2.77 -2 -12 0 61.20 3.23 -2 -12 0 56.56 2.87 -2 12 0 58.24 2.99 2 12 0 57.74 2.97 2 -12 0 59.33 3.19 2 -12 0 55.87 2.89 -4 12 0 88.89 4.32 -4 -12 0 87.37 4.10 -4 -12 0 90.26 4.65 -4 -12 0 87.52 4.14 4 -12 0 89.24 4.61 4 12 0 86.42 4.29 4 -12 0 81.71 4.19 -6 -12 0 12.17 0.88 -6 12 0 13.47 1.01 6 12 0 12.19 0.92 6 -12 0 12.95 0.97 -6 -12 0 12.66 0.86 6 -12 0 10.86 0.89 -8 -12 0 0.24 0.39 8 12 0 0.50 0.37 -8 -12 0 1.09 0.38 8 -12 0 1.11 0.35 8 -12 0 0.81 0.40 -8 12 0 0.79 0.48 -10 -12 0 8.19 0.85 10 -12 0 9.85 0.90 -10 -12 0 9.35 0.95 10 -12 0 9.56 0.79 -10 12 0 10.74 1.07 10 12 0 9.30 0.94 12 -12 0 0.72 0.34 12 12 0 0.85 0.53 -12 12 0 0.66 0.60 12 -12 0 0.08 0.47 -12 -12 0 0.56 0.55 -14 12 0 14.63 1.41 14 12 0 14.09 1.28 -14 -12 0 13.76 1.34 14 -12 0 14.74 1.28 14 -12 0 13.23 0.99 16 -12 0 0.29 0.64 -16 -12 0 -0.41 0.72 -16 12 0 0.37 0.74 16 -12 0 -0.03 0.34 18 -12 0 1.44 0.78 -18 -12 0 2.10 0.92 -18 12 0 0.92 0.90 18 -12 0 0.12 0.38 -20 -12 0 6.29 1.26 20 -12 0 6.06 0.67 -20 12 0 8.32 1.40 -1 -13 0 165.03 8.66 -1 -13 0 170.72 7.60 -1 13 0 170.87 8.00 -1 -13 0 166.38 7.77 1 -13 0 168.24 7.80 1 -13 0 170.68 8.66 1 13 0 163.78 7.98 -3 -13 0 348.75 15.46 3 -13 0 346.69 17.37 3 13 0 334.46 15.98 -3 -13 0 346.60 17.39 -3 -13 0 341.57 15.59 -3 13 0 338.29 16.00 3 -13 0 346.09 15.64 -5 13 0 52.09 2.78 5 13 0 53.27 2.75 5 -13 0 54.45 2.91 -5 -13 0 54.32 2.62 -5 -13 0 50.77 2.61 5 -13 0 50.99 2.69 -7 -13 0 0.26 0.35 -7 -13 0 0.24 0.36 -7 13 0 -0.02 0.43 7 13 0 0.21 0.37 7 -13 0 0.11 0.30 7 -13 0 0.38 0.41 -9 -13 0 5.26 0.70 9 13 0 3.78 0.63 9 -13 0 4.26 0.55 -9 -13 0 4.07 0.59 9 -13 0 2.62 0.58 -9 13 0 4.40 0.75 -11 -13 0 0.31 0.51 11 -13 0 0.86 0.55 11 -13 0 0.94 0.38 11 13 0 0.47 0.48 -11 13 0 0.75 0.64 13 -13 0 10.30 1.10 -13 13 0 8.88 1.10 -13 -13 0 9.76 1.09 13 -13 0 8.16 0.81 13 13 0 10.15 1.06 15 -13 0 7.57 0.79 -15 -13 0 6.64 1.04 15 -13 0 7.40 1.02 -15 13 0 6.12 1.06 17 -13 0 4.66 0.97 17 -13 0 3.89 0.60 -17 -13 0 2.66 0.96 -17 13 0 5.29 1.12 -19 13 0 11.29 1.54 -19 -13 0 13.89 1.59 19 -13 0 12.55 1.04 0 -14 0 13.64 1.08 0 -14 0 12.62 0.96 0 14 0 13.57 0.99 0 -14 0 13.67 0.77 -2 -14 0 5.55 0.61 2 14 0 5.78 0.65 -2 -14 0 6.55 0.76 -2 -14 0 6.07 0.54 2 -14 0 4.97 0.61 -2 14 0 5.78 0.68 2 -14 0 8.05 0.80 -4 -14 0 46.15 2.42 4 14 0 48.91 2.56 4 -14 0 46.61 2.51 -4 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2.54 0.90 -21 -5 -4 1.15 0.96 21 -5 4 1.08 1.08 -21 -5 4 0.81 0.92 0 -6 -4 7.11 0.48 0 6 -4 5.83 0.48 0 6 4 6.59 0.50 0 -6 4 6.42 0.47 0 -6 -4 6.94 0.56 0 -6 4 6.15 0.54 -2 6 4 94.66 4.35 -2 -6 -4 93.86 4.19 2 -6 4 94.14 4.24 2 -6 4 92.23 4.69 -2 -6 -4 93.53 4.19 2 6 -4 93.75 4.30 -2 -6 4 90.40 4.23 2 6 4 87.05 4.35 -2 6 -4 88.89 4.34 2 -6 -4 89.59 4.68 -2 -6 4 88.02 4.18 4 -6 4 14.10 0.89 -4 -6 -4 14.12 0.80 -4 -6 -4 15.23 0.89 -4 6 4 13.82 0.90 4 -6 4 14.44 0.92 4 6 -4 14.90 0.87 -4 6 4 13.85 0.88 -4 -6 4 18.42 0.91 -4 -6 4 18.29 0.92 4 -6 -4 17.64 0.92 4 6 4 18.20 0.99 -4 6 -4 17.92 0.97 -6 6 4 5.86 0.54 -6 6 4 4.86 0.51 -6 -6 -4 5.38 0.43 6 -6 4 5.36 0.51 6 6 -4 5.41 0.46 -6 -6 -4 5.20 0.51 6 -6 4 4.90 0.43 6 -6 4 4.15 0.43 -6 -6 4 8.12 0.59 -8 6 4 61.85 2.95 -8 -6 -4 59.65 2.82 8 6 -4 59.53 2.96 -8 -6 -4 57.89 2.95 8 -6 4 56.79 3.09 -8 6 4 60.98 3.02 8 -6 4 59.23 2.92 8 -6 4 53.93 3.10 -8 6 -4 65.96 2.86 -8 6 -4 61.68 3.07 8 6 4 66.19 3.12 8 -6 -4 60.57 3.06 -8 -6 4 61.87 2.98 -8 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10.14 1.51 15 1 -28 9.72 1.31 -15 -1 -28 9.83 1.35 15 -1 -28 11.98 1.40 -15 1 -28 9.10 1.28 -15 -1 28 9.45 1.47 15 1 28 11.11 1.62 15 -1 -28 10.54 1.33 -17 -1 -28 5.93 1.23 17 -1 28 7.70 1.63 17 1 -28 8.63 1.32 17 1 -28 8.35 1.31 -17 1 28 3.81 1.18 17 -1 -28 8.15 1.27 17 -1 -28 5.80 1.17 -17 1 -28 7.94 1.29 -17 -1 28 8.61 1.48 17 1 28 7.22 1.55 0 2 -28 43.06 2.44 0 -2 28 41.59 2.32 0 -2 -28 43.72 2.45 0 -2 -28 42.15 2.71 0 2 28 44.73 2.32 2 -2 28 41.79 2.25 -2 -2 -28 40.65 2.32 2 2 -28 38.58 2.30 2 2 -28 41.98 2.61 2 -2 28 41.38 2.16 -2 2 28 41.38 2.21 2 -2 -28 37.11 2.54 -2 2 -28 37.81 2.28 2 2 28 39.12 2.24 -2 -2 28 38.66 2.23 2 -2 -28 37.22 2.28 -4 2 28 14.10 1.19 -4 -2 -28 15.42 1.30 4 2 -28 17.66 1.51 4 2 -28 13.76 1.20 4 -2 28 13.84 1.21 -4 -2 28 15.28 1.23 -4 2 -28 13.77 1.26 4 2 28 15.79 1.25 4 -2 -28 15.27 1.29 4 -2 -28 15.09 1.44 -6 2 28 19.78 1.50 -6 -2 -28 19.79 1.56 6 2 -28 22.20 1.59 6 2 -28 23.95 1.75 6 -2 28 21.63 1.58 6 -2 -28 21.45 1.75 -6 -2 28 18.47 1.50 6 -2 -28 19.02 1.53 -6 2 -28 19.86 1.53 6 2 28 18.57 1.58 8 -2 28 5.83 0.99 8 2 -28 5.10 0.88 -8 2 28 4.56 0.90 -8 -2 -28 5.57 0.90 8 2 -28 5.97 0.99 8 -2 -28 4.79 0.90 8 -2 -28 4.95 0.91 -8 -2 28 4.13 0.85 8 2 28 5.21 0.95 -8 2 -28 3.30 0.79 10 2 -28 3.43 0.87 10 2 -28 2.60 0.74 -10 2 28 2.77 0.83 -10 -2 -28 2.78 0.81 10 -2 28 3.81 0.92 10 2 28 2.28 0.86 -10 2 -28 3.77 0.83 10 -2 -28 3.43 0.83 -10 -2 28 3.17 0.78 10 -2 -28 4.63 0.89 -12 -2 -28 4.77 0.98 12 2 -28 3.80 0.92 12 2 -28 4.95 0.94 -12 2 28 4.21 0.95 12 -2 28 4.39 1.10 -12 -2 28 4.41 0.92 12 -2 -28 5.12 0.98 -12 2 -28 4.31 0.91 12 2 28 3.86 1.04 12 -2 -28 5.52 0.99 14 -2 28 1.10 0.93 14 2 -28 0.79 0.80 -14 -2 -28 -0.29 0.75 14 2 -28 2.07 0.86 -14 2 28 1.17 0.92 14 -2 -28 0.85 0.76 -14 2 -28 1.43 0.81 14 -2 -28 1.94 0.88 14 2 28 0.71 0.83 -14 -2 28 -0.32 0.81 16 -2 28 4.34 1.34 16 2 -28 2.07 0.95 -16 -2 -28 4.43 1.13 16 2 -28 4.56 1.08 -16 2 28 3.31 1.16 -16 2 -28 4.95 1.11 16 -2 -28 2.17 0.90 16 -2 -28 5.74 1.13 16 2 28 4.67 1.30 -16 -2 28 4.62 1.17 18 2 -28 4.94 1.17 18 -2 28 3.51 1.47 -18 2 28 4.29 1.24 -18 -2 -28 4.23 1.18 18 2 -28 4.81 1.19 -18 -2 28 5.47 1.31 18 -2 -28 4.45 1.10 -18 2 -28 4.49 1.21 18 2 28 4.50 1.43 18 -2 -28 4.37 1.08 1 3 -28 9.81 1.20 -1 3 28 9.73 0.89 1 3 -28 8.56 1.00 -1 -3 -28 7.82 0.96 1 -3 28 7.76 0.86 1 -3 -28 11.58 1.21 1 -3 -28 9.89 1.03 1 3 28 10.79 0.96 -1 3 -28 9.06 1.01 -1 -3 28 10.96 1.03 1 3 28 10.19 0.86 3 3 -28 3.73 0.85 -3 3 28 2.91 0.61 -3 -3 -28 3.58 0.73 3 3 -28 2.92 0.71 3 -3 28 2.79 0.56 3 -3 28 2.74 0.62 -3 3 -28 2.28 0.68 -3 -3 28 1.66 0.57 3 -3 -28 2.28 0.66 3 3 28 2.67 0.64 3 -3 -28 2.70 0.73 -5 3 28 16.04 1.28 5 -3 28 13.58 1.27 5 3 -28 15.06 1.47 -5 -3 -28 14.00 1.30 5 3 -28 14.18 1.31 5 3 28 13.58 1.27 -5 -3 28 14.85 1.26 5 -3 -28 16.44 1.46 5 -3 -28 15.18 1.30 -5 3 -28 15.75 1.30 7 -3 28 18.41 1.61 -7 -3 -28 17.95 1.55 7 3 -28 18.45 1.54 7 3 -28 19.77 1.74 -7 3 28 19.10 1.54 -7 3 -28 21.26 1.56 7 3 28 23.01 1.68 -7 -3 28 21.09 1.59 7 -3 -28 24.93 1.82 7 -3 -28 23.98 1.63 9 3 -28 16.20 1.45 9 3 -28 17.91 1.64 -9 3 28 15.69 1.50 -9 -3 -28 18.87 1.52 9 -3 28 17.09 1.58 9 -3 -28 19.57 1.67 -9 3 -28 18.75 1.48 9 3 28 16.20 1.58 9 -3 -28 16.87 1.48 -9 -3 28 18.19 1.52 11 -3 28 14.89 1.60 11 3 -28 16.45 1.47 11 3 -28 15.44 1.52 -11 -3 -28 15.73 1.46 -11 3 28 13.30 1.40 11 -3 -28 13.44 1.41 11 3 28 11.88 1.42 -11 -3 28 12.13 1.38 -11 3 -28 12.87 1.34 11 -3 -28 13.65 1.45 13 3 -28 9.99 1.27 13 -3 28 9.10 1.44 -13 3 28 8.46 1.28 13 3 -28 10.00 1.23 -13 -3 -28 9.35 1.22 -13 3 -28 9.59 1.26 -13 -3 28 8.83 1.30 13 -3 -28 9.92 1.25 13 -3 -28 10.33 1.28 13 3 28 9.79 1.43 15 3 -28 10.68 1.37 15 -3 28 8.37 1.55 -15 3 28 9.76 1.45 -15 -3 -28 9.06 1.32 15 3 -28 9.37 1.34 -15 3 -28 10.10 1.32 -15 -3 28 10.66 1.44 15 -3 -28 11.30 1.38 15 -3 -28 9.46 1.30 15 3 28 10.00 1.57 -17 3 28 5.11 1.32 17 -3 28 6.42 1.57 -17 -3 -28 6.18 1.28 17 3 -28 6.75 1.24 17 3 -28 6.64 1.26 -17 3 -28 5.71 1.22 17 -3 -28 5.02 1.10 -17 -3 28 3.60 1.22 17 -3 -28 5.00 1.15 17 3 28 6.44 1.49 0 4 -28 35.46 2.13 0 -4 -28 37.01 2.15 0 -4 -28 34.73 2.37 0 -4 28 34.85 2.05 0 4 28 36.31 1.99 0 4 28 36.75 2.06 -2 -4 -28 48.79 2.59 -2 4 28 49.08 2.48 2 -4 28 50.83 2.54 2 -4 28 45.06 2.44 2 4 -28 46.56 2.56 2 4 -28 46.70 2.88 2 4 28 43.44 2.50 -2 -4 28 39.14 2.44 -2 4 -28 43.02 2.52 2 -4 -28 39.63 2.77 2 -4 -28 44.28 2.53 -4 4 28 36.31 2.06 4 -4 28 38.49 2.14 4 4 -28 39.07 2.39 -4 -4 -28 36.21 2.15 4 4 -28 37.16 2.16 4 -4 -28 32.03 2.07 4 -4 -28 31.49 2.33 -4 -4 28 31.37 2.06 4 4 28 32.55 2.12 -4 4 -28 32.21 2.07 6 4 -28 18.85 1.50 6 -4 28 18.78 1.56 6 4 -28 19.97 1.69 -6 4 28 18.54 1.47 -6 -4 -28 18.63 1.51 6 -4 -28 19.46 1.69 -6 4 -28 20.77 1.50 -6 -4 28 19.52 1.50 6 4 28 20.62 1.55 6 -4 -28 18.72 1.49 8 4 -28 6.83 1.01 8 4 -28 5.72 0.94 -8 4 28 4.83 0.91 -8 -4 -28 5.24 0.93 8 -4 28 4.88 0.93 8 -4 -28 7.20 1.01 -8 -4 28 5.25 0.95 -8 4 -28 6.76 0.92 8 -4 -28 6.45 1.01 8 4 28 5.75 1.02 -10 4 28 1.58 0.79 10 4 -28 1.71 0.72 -10 -4 -28 1.40 0.76 10 4 -28 2.07 0.78 10 -4 28 1.44 0.81 -10 -4 28 1.64 0.69 10 -4 -28 1.06 0.75 10 4 28 1.20 0.78 10 -4 -28 1.25 0.73 -10 4 -28 1.39 0.68 -12 -4 -28 1.39 0.83 12 4 -28 1.62 0.78 12 -4 28 0.75 0.89 -12 4 28 0.97 0.81 12 4 -28 1.97 0.77 12 -4 -28 2.65 0.82 12 4 28 1.97 0.98 -12 -4 28 1.06 0.80 -12 4 -28 2.96 0.82 12 -4 -28 1.31 0.77 14 4 -28 8.70 1.25 -14 -4 -28 5.63 1.11 14 -4 28 5.78 1.27 14 4 -28 6.28 1.12 -14 4 28 5.61 1.17 14 4 28 5.45 1.25 14 -4 -28 5.29 1.08 -14 -4 28 5.72 1.18 14 -4 -28 6.18 1.11 -14 4 -28 5.97 1.05 -16 -4 -28 5.88 1.24 16 -4 28 6.05 1.52 -16 4 28 4.52 1.25 16 4 -28 4.70 1.11 16 4 -28 4.83 1.11 16 -4 -28 6.03 1.17 -16 4 -28 5.99 1.16 16 -4 -28 5.60 1.08 -16 -4 28 4.20 1.21 16 4 28 5.08 1.39 18 4 -28 3.26 1.11 -18 -4 -28 5.03 1.27 18 -4 -28 4.04 1.06 -18 4 -28 5.18 1.17 1 -5 28 5.58 0.79 -1 -5 -28 5.35 0.83 1 5 -28 7.08 0.92 -1 5 28 5.70 0.73 -1 -5 28 6.80 0.86 1 -5 -28 7.78 1.08 1 -5 -28 7.06 0.92 1 5 28 7.98 0.88 -1 5 -28 5.80 0.84 -3 5 28 16.20 1.26 3 5 -28 17.03 1.35 3 5 -28 18.32 1.53 -3 -5 -28 15.74 1.34 3 -5 28 16.40 1.26 3 -5 28 16.59 1.19 -3 5 -28 14.19 1.27 -3 -5 28 13.09 1.25 3 5 28 14.98 1.27 3 -5 -28 15.94 1.31 3 -5 -28 15.09 1.50 5 5 -28 24.06 1.66 -5 -5 -28 24.01 1.63 5 5 -28 24.33 1.86 5 -5 28 24.50 1.68 -5 5 28 25.01 1.62 5 5 28 20.72 1.64 5 -5 -28 21.48 1.61 -5 -5 28 22.01 1.63 -5 5 -28 21.83 1.59 5 -5 -28 21.79 1.84 -7 -5 -28 36.17 2.30 -7 5 28 37.73 2.30 7 5 -28 34.50 2.51 7 -5 28 38.39 2.38 7 5 -28 36.38 2.28 -7 5 -28 37.15 2.26 7 -5 -28 39.64 2.32 7 -5 -28 39.61 2.57 -7 -5 28 40.95 2.35 7 5 28 38.85 2.42 -9 5 28 10.06 1.18 9 5 -28 13.52 1.40 9 -5 28 10.57 1.28 9 5 -28 12.95 1.30 -9 -5 -28 12.66 1.31 -9 -5 28 11.03 1.25 -9 5 -28 13.65 1.30 9 5 28 13.03 1.42 9 -5 -28 15.25 1.47 9 -5 -28 13.15 1.30 -11 -5 -28 14.55 1.47 11 -5 28 17.58 1.74 11 5 -28 15.20 1.55 -11 5 28 12.36 1.40 11 5 -28 14.80 1.44 11 -5 -28 15.01 1.45 11 5 28 12.48 1.44 -11 -5 28 11.00 1.33 -11 5 -28 12.11 1.29 11 -5 -28 15.17 1.51 -13 5 28 7.86 1.25 -13 -5 -28 8.89 1.27 13 -5 28 7.82 1.41 13 5 -28 7.79 1.20 13 5 -28 7.17 1.18 -13 -5 28 11.85 1.41 13 -5 -28 9.73 1.26 13 -5 -28 9.21 1.19 -13 5 -28 10.65 1.26 13 5 28 9.30 1.45 -15 5 28 3.58 1.11 15 5 -28 4.66 1.11 15 -5 28 6.51 1.49 15 5 -28 5.08 1.08 -15 -5 -28 6.25 1.17 15 5 28 9.25 1.53 15 -5 -28 7.34 1.15 -15 -5 28 6.15 1.24 15 -5 -28 8.15 1.22 -15 5 -28 7.16 1.16 17 5 -28 2.81 1.03 17 -5 28 4.91 1.44 -17 -5 -28 3.09 1.17 -17 5 28 4.04 1.29 17 5 -28 2.90 1.06 17 5 28 7.93 1.57 17 -5 -28 3.78 1.07 -17 -5 28 3.84 1.22 17 -5 -28 3.99 1.01 0 -6 28 18.78 1.39 0 6 28 19.13 1.27 0 -6 -28 21.06 1.65 0 6 -28 19.09 1.43 0 6 28 18.10 1.36 0 -6 -28 19.58 1.45 2 6 -28 36.40 2.19 -2 -6 -28 35.52 2.20 -2 6 28 36.95 2.08 2 -6 28 36.01 2.14 -2 -6 28 38.70 2.21 2 -6 -28 35.69 2.44 2 -6 -28 36.61 2.18 -2 6 -28 37.18 2.18 2 6 28 38.73 2.21 -4 6 28 31.12 1.95 -4 -6 -28 33.95 2.08 4 -6 28 33.61 2.05 4 -6 28 32.22 1.91 4 6 -28 33.64 2.07 4 6 -28 32.56 2.29 4 -6 -28 34.14 2.04 -4 -6 28 33.30 2.06 -4 6 -28 32.87 2.01 4 -6 -28 30.39 2.27 4 6 28 32.18 2.06 6 6 -28 19.24 1.48 6 6 -28 17.67 1.59 -6 -6 -28 17.16 1.47 6 -6 28 17.24 1.47 -6 6 28 15.75 1.39 -6 -6 28 17.93 1.48 6 6 28 16.99 1.50 6 -6 -28 18.43 1.65 -6 6 -28 18.65 1.41 6 -6 -28 17.74 1.44 8 6 -28 6.53 1.03 -8 -6 -28 6.08 0.96 -8 6 28 5.59 0.91 8 6 -28 5.68 0.92 8 -6 28 6.24 1.01 8 6 28 5.98 1.02 8 -6 -28 7.25 0.97 -8 6 -28 7.46 0.95 -8 -6 28 8.37 1.07 8 -6 -28 9.00 1.11 10 -6 28 4.36 1.00 10 6 -28 6.39 1.03 10 6 -28 4.93 0.94 -10 -6 -28 4.90 0.99 -10 6 28 4.67 0.90 10 -6 -28 5.68 1.00 -10 -6 28 4.42 0.94 -10 6 -28 3.69 0.81 10 -6 -28 3.96 0.88 10 6 28 2.53 0.89 -12 -6 -28 0.75 0.80 -12 6 28 0.12 0.77 12 6 -28 0.63 0.74 12 6 -28 0.88 0.77 12 -6 28 0.24 0.89 -12 -6 28 0.46 0.73 12 6 28 0.50 0.83 12 -6 -28 0.57 0.74 12 -6 -28 0.50 0.70 -12 6 -28 0.31 0.64 -14 6 28 2.88 0.92 14 6 -28 1.65 0.90 14 -6 28 4.91 1.28 14 6 -28 3.18 1.00 -14 -6 -28 3.02 1.03 14 -6 -28 3.90 0.94 14 -6 -28 3.47 0.97 14 6 28 3.43 1.14 -14 6 -28 3.19 0.94 -14 -6 28 2.37 0.98 -16 6 28 1.33 1.05 16 6 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7 -28 11.64 1.26 -9 7 28 12.12 1.30 9 7 -28 12.34 1.36 -9 7 -28 12.28 1.22 9 7 28 12.24 1.40 -9 -7 28 12.66 1.36 9 -7 -28 13.16 1.40 9 -7 -28 13.47 1.29 -11 -7 -28 16.42 1.54 11 7 -28 16.45 1.51 11 -7 28 13.97 1.58 -11 7 28 13.84 1.49 11 7 -28 13.31 1.48 11 7 28 14.15 1.62 11 -7 -28 15.75 1.58 11 -7 -28 16.43 1.53 -11 -7 28 11.96 1.38 -11 7 -28 14.61 1.40 -13 -7 -28 8.10 1.26 13 -7 28 6.17 1.28 -13 7 28 6.33 1.23 13 7 -28 8.28 1.25 13 7 -28 7.06 1.15 -13 -7 28 7.44 1.26 13 -7 -28 9.72 1.25 -13 7 -28 7.02 1.10 13 7 28 7.92 1.39 13 -7 -28 9.77 1.23 -15 -7 -28 5.86 1.24 15 7 -28 4.42 1.10 15 -7 28 4.57 1.40 15 7 -28 5.61 1.14 -15 7 28 3.31 1.15 15 -7 -28 5.71 1.07 -15 -7 28 4.42 1.13 15 7 28 5.48 1.30 -17 -7 -28 2.82 1.16 17 7 -28 2.73 1.05 -17 7 28 3.11 1.17 17 7 -28 2.97 1.06 17 -7 28 4.42 1.56 17 -7 -28 3.25 0.97 -17 -7 28 3.62 1.20 17 7 28 3.07 1.31 0 -8 -28 -0.24 0.57 0 -8 28 0.42 0.57 0 8 28 0.15 0.51 0 8 -28 0.98 0.57 2 -8 28 14.28 1.29 -2 8 28 15.42 1.21 -2 -8 -28 16.31 1.35 2 8 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7 9 -28 6.86 1.10 -7 -9 -28 3.53 0.87 7 9 -28 6.16 0.95 -7 9 28 5.06 0.93 -7 9 -28 8.62 1.12 -7 -9 28 9.39 1.16 7 -9 -28 6.58 1.06 7 -9 -28 8.27 1.02 7 9 28 7.60 1.14 -7 9 -28 8.13 0.99 -9 -9 -28 13.45 1.44 -9 9 28 17.47 1.53 9 9 -28 14.96 1.47 9 -9 28 14.97 1.66 9 9 -28 14.54 1.62 9 9 28 16.07 1.64 9 -9 -28 16.86 1.46 -9 9 -28 17.44 1.63 9 -9 -28 15.80 1.63 -9 -9 28 15.93 1.55 -9 9 -28 14.25 1.35 -11 -9 -28 16.88 1.61 11 9 -28 15.95 1.58 -11 9 28 16.17 1.64 11 9 -28 18.25 1.77 11 -9 -28 15.17 1.52 11 -9 -28 16.79 1.70 -11 -9 28 14.99 1.50 11 9 28 18.03 1.78 13 9 -28 16.39 1.79 -13 9 28 17.11 1.75 -13 -9 -28 15.23 1.58 13 9 -28 14.80 1.61 13 -9 28 12.42 1.67 13 9 28 16.86 1.86 13 -9 -28 18.60 1.77 -13 -9 28 14.15 1.61 15 9 -28 10.91 1.48 15 9 -28 11.91 1.55 15 -9 28 10.02 1.64 -15 -9 -28 10.78 1.52 -15 9 28 7.80 1.37 15 9 28 8.35 1.57 15 -9 -28 10.49 1.36 -15 -9 28 11.26 1.53 0 10 -28 7.45 0.96 0 10 28 5.96 0.90 0 -10 28 7.86 1.01 0 -10 -28 8.03 0.97 -2 10 28 20.31 1.48 2 -10 28 20.81 1.47 -2 10 28 18.31 1.36 -2 -10 -28 19.66 1.51 2 10 -28 20.21 1.50 2 -10 -28 18.96 1.69 -2 10 -28 19.27 1.44 2 -10 -28 17.77 1.44 -2 -10 28 20.13 1.58 2 10 28 17.34 1.51 4 10 -28 22.15 1.59 4 -10 28 21.48 1.46 -4 10 28 20.30 1.44 4 -10 28 20.45 1.79 -4 -10 -28 19.73 1.55 -4 10 -28 17.51 1.49 4 -10 -28 18.95 1.76 -4 -10 28 19.32 1.63 -4 10 -28 18.31 1.55 4 10 28 22.59 1.69 4 -10 -28 19.09 1.51 6 10 -28 4.40 0.83 6 -10 28 4.65 0.83 -6 -10 -28 5.18 0.94 6 -10 28 5.41 1.03 -6 10 28 3.93 0.82 6 10 -28 6.01 1.03 -6 -10 28 2.66 0.82 -6 10 -28 3.46 0.85 6 -10 -28 4.17 0.80 6 -10 -28 4.05 0.92 6 10 28 4.45 0.96 -6 10 -28 4.13 0.80 8 10 -28 7.50 1.04 8 10 -28 5.72 1.05 -8 -10 -28 6.31 1.06 8 -10 28 7.64 1.18 -8 10 28 6.37 1.04 8 -10 -28 8.48 1.05 8 -10 -28 6.51 1.10 8 10 28 8.40 1.26 -8 -10 28 7.93 1.16 -8 10 -28 7.67 1.11 -8 10 -28 7.11 0.94 10 10 -28 16.14 1.69 -10 -10 -28 14.84 1.53 10 10 -28 14.41 1.48 10 -10 28 17.12 1.77 -10 10 28 16.10 1.57 10 -10 -28 15.47 1.68 10 10 28 16.44 1.74 -10 10 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19.19 1.44 -5 -11 -28 19.24 1.56 -5 11 28 18.70 1.50 -5 11 -28 23.61 1.66 5 -11 -28 20.12 1.51 5 -11 -28 19.67 1.78 -5 -11 28 19.29 1.65 -5 11 -28 17.92 1.47 5 11 28 18.24 1.68 7 11 -28 7.15 0.99 7 11 -28 6.54 1.11 -7 11 28 7.88 1.01 -7 -11 -28 7.53 1.09 7 -11 28 5.53 1.05 7 -11 -28 7.42 0.98 7 -11 -28 6.74 1.11 7 11 28 7.82 1.21 -7 11 -28 6.39 1.05 -7 -11 28 6.08 1.04 9 11 -28 15.03 1.41 9 -11 28 11.02 1.41 -9 11 28 10.56 1.29 -9 -11 -28 11.28 1.32 9 11 -28 14.06 1.51 -9 11 -28 12.19 1.42 9 11 28 11.52 1.49 -9 -11 28 8.87 1.27 9 -11 -28 10.64 1.37 -11 11 28 9.39 1.34 -11 -11 -28 8.83 1.29 11 11 -28 9.15 1.34 11 11 -28 7.99 1.19 11 -11 28 7.80 1.30 -11 -11 28 8.79 1.28 11 11 28 10.02 1.48 -11 11 -28 8.13 1.30 11 -11 -28 10.42 1.34 13 -11 28 5.77 1.23 13 11 -28 5.48 1.11 13 11 -28 6.46 1.22 -13 -11 -28 4.99 1.16 -13 11 28 4.93 1.19 -13 11 -28 6.26 1.30 13 -11 -28 5.58 1.14 13 11 28 7.11 1.38 -13 -11 28 7.19 1.23 -15 11 28 7.02 1.40 15 11 -28 7.12 1.31 -15 -11 -28 6.36 1.30 15 11 -28 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-1 -3 -42 3.10 1.10 -1 3 -42 1.52 1.01 1 -3 -42 2.64 1.02 -3 -3 -42 1.09 1.00 3 3 -42 3.07 1.10 -3 -3 42 2.71 0.91 -3 3 -42 3.16 1.09 3 -3 -42 3.23 1.07 5 3 -42 1.00 0.97 -5 3 42 0.27 0.79 -5 -3 -42 0.83 1.00 5 -3 -42 1.21 1.01 -5 -3 42 1.56 0.88 -5 3 -42 0.70 0.95 -7 -3 -42 3.02 1.17 -7 3 42 1.98 0.96 7 3 -42 2.59 1.17 7 -3 -42 3.48 1.21 -7 3 -42 4.24 1.20 -7 -3 42 3.78 1.09 9 3 -42 6.87 1.41 -9 -3 -42 5.88 1.31 -9 3 42 4.77 1.16 9 -3 -42 5.16 1.46 9 -3 -42 5.38 1.32 -9 3 -42 4.57 1.28 -9 -3 42 4.88 1.20 0 -4 -42 15.19 1.73 0 4 -42 13.54 1.61 2 4 -42 11.04 1.48 -2 -4 -42 14.22 1.68 -2 4 -42 12.98 1.58 2 -4 -42 12.74 1.58 -4 -4 -42 6.79 1.34 4 4 -42 7.81 1.35 4 -4 -42 7.11 1.29 -4 4 -42 9.32 1.39 -4 -4 42 8.52 1.25 -6 4 42 5.37 1.11 6 4 -42 7.61 1.43 -6 -4 -42 5.36 1.29 -6 -4 42 5.47 1.17 -6 4 -42 3.80 1.18 6 -4 -42 4.21 1.22 -8 -4 -42 5.13 1.31 -8 4 42 4.13 1.08 8 4 -42 3.27 1.24 -8 -4 42 3.52 1.08 -8 4 -42 3.41 1.17 8 -4 -42 3.22 1.23 1 5 -42 4.72 1.13 -1 -5 -42 6.11 1.29 -1 5 -42 5.05 1.17 1 -5 -42 5.71 1.18 -3 -5 -42 6.08 1.28 3 5 -42 5.03 1.21 3 -5 -42 4.94 1.21 -3 5 -42 6.75 1.28 -3 -5 42 5.16 1.12 5 5 -42 3.02 1.18 -5 -5 -42 3.64 1.14 5 -5 -42 3.08 1.11 -5 5 -42 4.02 1.11 -5 -5 42 3.96 1.04 7 5 -42 2.51 1.19 -7 5 42 2.06 0.96 -7 -5 -42 4.12 1.25 7 -5 -42 2.29 1.18 -7 -5 42 2.71 0.99 -7 5 -42 2.72 1.10 0 6 -42 19.79 1.93 0 -6 -42 18.23 1.89 -2 -6 -42 15.91 1.76 2 6 -42 17.54 1.81 -2 6 -42 13.94 1.66 2 -6 -42 18.37 1.89 -2 -6 42 16.07 1.66 4 6 -42 9.86 1.53 -4 -6 -42 9.66 1.52 4 -6 -42 9.49 1.43 -4 6 -42 9.70 1.43 -4 -6 42 11.28 1.47 -6 -6 -42 5.08 1.25 6 6 -42 6.09 1.35 6 -6 -42 5.99 1.30 -6 -6 42 4.86 1.12 -6 6 -42 5.97 1.27 -8 6 42 0.36 0.92 8 6 -42 2.19 1.16 -8 -6 -42 2.39 1.19 -8 6 -42 2.25 1.08 -8 -6 42 0.81 0.95 8 -6 -42 1.55 1.10 -1 -7 -42 5.35 1.21 1 7 -42 6.45 1.28 1 -7 -42 6.04 1.30 -1 7 -42 5.61 1.18 -3 -7 -42 8.27 1.45 3 7 -42 7.62 1.36 -3 -7 42 9.50 1.34 -3 7 -42 6.85 1.28 3 -7 -42 8.05 1.37 -5 -7 -42 3.87 1.17 5 7 -42 4.45 1.24 -5 -7 42 4.38 1.12 -5 7 -42 6.02 1.19 5 -7 -42 4.08 1.17 -7 -7 -42 0.76 1.07 -7 7 42 1.43 0.93 7 7 -42 0.79 1.00 7 -7 -42 0.62 1.02 -7 7 -42 0.69 1.02 -7 -7 42 1.22 1.00 0 8 -42 15.38 1.68 0 -8 -42 15.54 1.77 -2 -8 -42 15.63 1.77 2 8 -42 12.47 1.63 2 -8 -42 14.17 1.68 -2 -8 42 12.17 1.54 -2 8 -42 11.83 1.55 -4 -8 -42 10.58 1.57 4 8 -42 10.98 1.59 -4 -8 42 9.82 1.43 4 -8 -42 9.76 1.50 -4 8 -42 9.70 1.47 -6 -8 -42 9.21 1.46 6 8 -42 8.65 1.48 -6 8 -42 9.03 1.45 6 -8 -42 8.10 1.43 -6 -8 42 9.63 1.47 1 9 -42 5.49 1.26 -1 -9 -42 4.02 1.15 -1 -9 42 1.68 0.98 1 -9 -42 2.78 1.12 -1 9 -42 2.80 1.07 -3 -9 -42 7.08 1.38 3 9 -42 7.38 1.36 -3 -9 42 4.26 1.16 -3 9 -42 5.13 1.15 3 -9 -42 3.56 1.14 5 9 -42 5.43 1.28 -5 -9 -42 6.47 1.41 5 -9 -42 3.83 1.22 -5 -9 42 4.96 1.20 -5 9 -42 4.07 1.18 0 10 -42 8.88 1.40 0 -10 -42 7.19 1.33 2 10 -42 3.90 1.14 -2 -10 -42 4.59 1.24 -2 10 -42 4.93 1.21 -2 -10 42 6.15 1.20 2 -10 -42 5.62 1.23 -4 -10 -42 4.92 1.24 4 10 -42 4.15 1.22 -4 -10 42 5.56 1.27 -4 10 -42 4.23 1.16 4 -10 -42 5.90 1.32 -1 -11 -42 6.34 1.31 1 11 -42 7.25 1.34 -1 11 -42 4.98 1.22 1 -11 -42 5.83 1.24 -1 -11 42 5.17 1.24 3 11 -42 5.41 1.21 -3 -11 -42 4.85 1.28 -3 -11 42 6.33 1.30 3 -11 -42 5.00 1.26 -3 11 -42 4.63 1.18 0 -12 -42 5.50 1.27 0 12 -42 7.41 1.32 -2 -12 -42 3.29 1.13 2 -12 -42 0.81 1.03 -2 -12 42 0.91 1.04 0 0 -43 1.27 1.00 2 0 -43 2.55 1.03 -2 0 -43 2.04 1.06 -4 0 -43 0.49 0.99 4 0 -43 -0.15 0.89 -6 0 43 -1.35 0.78 6 0 -43 0.25 0.94 -6 0 -43 0.68 1.05 -8 0 -43 0.29 1.05 -8 0 43 1.22 0.96 8 0 -43 1.45 1.16 -1 -1 -43 19.94 1.96 1 1 -43 19.86 1.97 1 -1 -43 22.69 2.02 -1 1 -43 20.47 1.98 3 1 -43 8.64 1.45 -3 -1 -43 11.75 1.57 3 -1 -43 8.02 1.35 -3 1 -43 11.38 1.52 -5 -1 -43 8.67 1.43 -5 1 43 9.62 1.32 5 1 -43 11.53 1.60 -5 -1 43 7.82 1.27 5 -1 -43 8.98 1.49 -5 1 -43 10.23 1.53 7 1 -43 12.92 1.71 -7 -1 -43 10.17 1.55 -7 1 43 11.13 1.42 7 -1 -43 9.98 1.58 -7 -1 43 12.07 1.51 -7 1 -43 12.04 1.62 0 -2 -43 2.55 1.03 0 2 -43 -0.21 0.92 -2 -2 -43 1.41 1.02 2 2 -43 1.92 0.99 2 -2 -43 0.85 1.00 -2 2 -43 1.41 1.00 4 2 -43 -0.80 0.91 -4 -2 -43 -0.73 0.94 -4 2 -43 1.18 0.99 4 -2 -43 0.63 0.99 -4 -2 43 -1.05 0.72 -6 -2 -43 0.83 1.04 6 2 -43 0.07 0.96 -6 2 43 0.00 0.80 6 -2 -43 0.24 1.04 -6 2 -43 0.63 1.03 -6 -2 43 -0.24 0.84 -8 2 43 0.48 0.92 -8 -2 -43 2.50 1.17 -8 -2 43 1.29 0.97 -8 2 -43 0.10 1.03 -1 -3 -43 27.64 2.24 1 3 -43 25.45 2.19 1 -3 -43 26.70 2.31 -1 3 -43 24.77 2.17 3 3 -43 11.55 1.55 -3 -3 -43 12.92 1.63 3 -3 -43 10.21 1.50 -3 3 -43 9.92 1.52 -5 -3 -43 7.79 1.41 5 3 -43 8.37 1.45 -5 3 -43 5.91 1.32 5 -3 -43 9.75 1.52 -5 -3 43 7.08 1.24 7 3 -43 7.06 1.38 -7 3 43 5.68 1.18 -7 -3 -43 5.45 1.32 7 -3 -43 7.98 1.47 -7 -3 43 4.89 1.16 -7 3 -43 5.69 1.30 0 -4 -43 5.00 1.25 0 4 -43 6.18 1.31 -2 -4 -43 2.55 1.15 2 4 -43 1.64 1.05 -2 4 -43 2.47 1.06 2 -4 -43 1.94 1.05 4 4 -43 -0.27 0.96 -4 -4 -43 0.13 1.02 4 -4 -43 1.56 1.02 -4 4 -43 -0.34 0.86 -4 -4 43 0.01 0.78 -6 -4 -43 0.62 1.01 6 4 -43 0.69 1.10 -6 4 43 1.60 0.90 -6 -4 43 2.23 0.98 6 -4 -43 2.12 1.12 -6 4 -43 2.44 1.13 1 5 -43 22.81 2.09 -1 -5 -43 24.16 2.12 1 -5 -43 22.74 2.09 -1 5 -43 22.25 2.15 -3 -5 -43 15.42 1.85 3 5 -43 15.89 1.78 -3 -5 43 16.16 1.66 3 -5 -43 17.00 1.82 -3 5 -43 15.85 1.78 5 5 -43 13.35 1.77 -5 -5 -43 13.85 1.75 -5 -5 43 11.41 1.49 5 -5 -43 14.09 1.71 -5 5 -43 12.02 1.58 7 5 -43 4.07 1.26 -7 -5 -43 2.83 1.18 -7 5 43 4.01 1.11 -7 5 -43 4.93 1.24 7 -5 -43 2.12 1.14 -7 -5 43 4.73 1.19 0 6 -43 15.10 1.74 0 -6 -43 14.83 1.74 -2 -6 -43 11.37 1.59 2 6 -43 9.93 1.50 -2 6 -43 9.10 1.47 2 -6 -43 9.46 1.46 -4 -6 -43 1.23 1.10 4 6 -43 2.13 1.05 -4 6 -43 2.04 1.06 4 -6 -43 1.81 1.07 -4 -6 43 2.99 1.05 -6 -6 -43 4.88 1.29 6 6 -43 0.89 1.09 -6 -6 43 1.37 0.96 6 -6 -43 3.79 1.21 -6 6 -43 1.29 1.05 -1 -7 -43 10.51 1.49 1 7 -43 7.80 1.35 1 -7 -43 8.49 1.48 -1 7 -43 9.75 1.46 3 7 -43 12.11 1.70 -3 -7 -43 16.31 1.84 3 -7 -43 12.53 1.66 -3 -7 43 14.79 1.63 -3 7 -43 14.03 1.69 5 7 -43 7.70 1.50 -5 -7 -43 8.50 1.51 -5 7 -43 8.45 1.43 -5 -7 43 12.60 1.54 5 -7 -43 10.48 1.53 0 8 -43 9.58 1.47 0 -8 -43 8.07 1.40 2 8 -43 7.60 1.41 -2 -8 -43 5.78 1.34 -2 -8 43 8.80 1.33 2 -8 -43 8.66 1.48 -2 8 -43 10.39 1.47 4 8 -43 6.97 1.42 -4 -8 -43 5.46 1.36 4 -8 -43 7.16 1.36 -4 -8 43 5.15 1.19 -4 8 -43 7.86 1.33 -1 -9 -43 4.48 1.26 1 9 -43 4.49 1.19 -1 9 -43 5.01 1.22 1 -9 -43 5.94 1.33 -3 -9 -43 7.74 1.49 3 9 -43 8.41 1.43 -3 -9 43 7.71 1.40 -3 9 -43 8.22 1.40 3 -9 -43 10.42 1.51 0 10 -43 3.42 1.14 0 -10 -43 0.78 1.00 2 10 -43 6.52 1.35 -2 -10 -43 6.75 1.36 -2 -10 43 5.07 1.26 2 -10 -43 4.68 1.25 -2 10 -43 4.17 1.19 0 0 -44 27.45 2.39 2 0 -44 7.87 1.46 -2 0 -44 10.59 1.51 -4 0 -44 8.23 1.43 4 0 -44 6.80 1.35 6 0 -44 10.85 1.60 -6 0 -44 9.36 1.55 -6 0 44 8.88 1.38 -1 -1 -44 0.54 1.02 1 1 -44 1.64 1.05 1 -1 -44 0.25 0.98 -1 1 -44 -0.75 0.93 -3 -1 -44 -0.73 0.93 3 1 -44 -1.00 0.89 -3 1 -44 0.18 0.98 3 -1 -44 -0.15 0.91 5 1 -44 -0.83 0.98 -5 -1 -44 1.01 1.03 -5 -1 44 0.07 0.83 5 -1 -44 0.47 1.06 -5 1 -44 1.98 1.12 0 2 -44 30.73 2.38 0 -2 -44 27.86 2.31 2 2 -44 14.33 1.73 -2 -2 -44 12.65 1.67 2 -2 -44 12.94 1.67 -2 2 -44 13.41 1.73 -4 -2 -44 6.61 1.33 4 2 -44 5.15 1.29 4 -2 -44 7.84 1.41 -4 2 -44 5.92 1.31 6 2 -44 11.40 1.66 -6 2 44 10.28 1.43 -6 -2 -44 11.54 1.67 -6 2 -44 9.06 1.51 6 -2 -44 10.08 1.66 -6 -2 44 8.44 1.39 -1 -3 -44 3.28 1.21 1 3 -44 4.30 1.21 1 -3 -44 5.49 1.27 -1 3 -44 5.17 1.22 3 3 -44 0.60 1.01 -3 -3 -44 -0.76 0.96 -3 3 -44 -0.42 0.97 3 -3 -44 -0.15 0.97 -5 -3 -44 1.74 1.07 5 3 -44 1.17 1.10 -5 -3 44 1.07 0.89 -5 3 -44 0.98 1.10 5 -3 -44 2.42 1.12 0 4 -44 18.89 1.95 0 -4 -44 19.47 1.98 2 4 -44 15.06 1.80 -2 -4 -44 15.16 1.73 -2 4 -44 11.09 1.59 2 -4 -44 11.96 1.64 4 4 -44 10.00 1.56 -4 -4 -44 9.80 1.55 -4 4 -44 7.35 1.39 4 -4 -44 9.01 1.46 -4 -4 44 6.80 1.25 -6 -4 -44 10.73 1.61 -6 -4 44 9.44 1.44 -6 4 -44 9.80 1.52 1 5 -44 5.93 1.28 -1 -5 -44 7.02 1.39 1 -5 -44 4.13 1.25 -1 5 -44 5.12 1.25 3 5 -44 0.91 1.08 -3 -5 -44 2.93 1.19 -3 5 -44 1.79 1.09 3 -5 -44 1.52 1.10 5 5 -44 2.17 1.21 -5 -5 -44 1.01 1.07 -5 5 -44 2.80 1.14 -5 -5 44 1.81 1.07 5 -5 -44 1.89 1.15 0 6 -44 5.99 1.37 0 -6 -44 8.21 1.40 2 6 -44 6.47 1.38 -2 -6 -44 9.16 1.54 2 -6 -44 8.77 1.44 -2 6 -44 9.49 1.46 4 6 -44 14.64 1.81 -4 -6 -44 12.16 1.71 -4 6 -44 15.22 1.72 4 -6 -44 14.82 1.76 -4 -6 44 13.58 1.59 -1 -7 -44 4.42 1.26 1 7 -44 3.67 1.19 1 -7 -44 3.92 1.26 -1 7 -44 6.04 1.30 -3 -7 -44 3.40 1.21 3 7 -44 3.41 1.21 -3 -7 44 2.28 1.00 3 -7 -44 2.45 1.13 -3 7 -44 1.66 1.08 0 8 -44 5.84 1.31 0 -8 -44 8.64 1.44 2 8 -44 11.38 1.66 -2 -8 -44 10.58 1.61 -2 8 -44 10.52 1.56 2 -8 -44 10.71 1.59 0 0 -45 0.37 0.99 -2 0 -45 1.95 1.11 2 0 -45 1.63 1.03 4 0 -45 3.75 1.26 -4 0 -45 3.15 1.17 -1 -1 -45 10.11 1.61 1 1 -45 9.62 1.50 -1 1 -45 8.96 1.51 1 -1 -45 11.51 1.57 3 1 -45 3.48 1.18 -3 -1 -45 5.02 1.27 3 -1 -45 6.07 1.32 -3 1 -45 4.28 1.21 0 -2 -45 2.02 1.12 0 2 -45 0.80 1.06 2 2 -45 0.92 1.03 -2 -2 -45 0.95 1.05 -2 2 -45 -0.36 1.00 2 -2 -45 1.55 1.06 4 2 -45 0.86 1.03 -4 -2 -45 1.25 1.09 -4 2 -45 0.19 1.00 4 -2 -45 0.01 1.03 -1 -3 -45 12.35 1.67 1 3 -45 10.25 1.59 1 -3 -45 13.80 1.74 -1 3 -45 12.98 1.67 3 3 -45 5.46 1.33 -3 -3 -45 7.98 1.47 -3 3 -45 7.36 1.37 3 -3 -45 4.95 1.31 0 4 -45 2.85 1.20 0 -4 -45 2.08 1.11 -2 -4 -45 0.94 1.04 2 4 -45 1.13 1.02 2 -4 -45 0.53 1.01 -2 4 -45 1.95 1.10 1 5 -45 10.59 1.55 -1 -5 -45 10.79 1.60 1 -5 -45 9.40 1.57 -1 5 -45 10.15 1.59 0 6 -45 2.51 1.15 0 -6 -45 2.73 1.17 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 80755 #===END data_Er2-biph _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C56 H86 Er2 Fe2 N4 Si4), 4(C4 H10 O), C4 H8 O, 4(K)' _chemical_formula_sum 'C132 H220 Er4 Fe4 K4 N8 O5 Si8' _chemical_formula_weight 3272.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0037(19) _cell_length_b 22.794(3) _cell_length_c 23.376(3) _cell_angle_alpha 90 _cell_angle_beta 97.0190(15) _cell_angle_gamma 90 _cell_volume 7934.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9829 _cell_measurement_theta_min 3.55 _cell_measurement_theta_max 28.17 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_F_000 3344 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.110 _exptl_absorpt_coefficient_mu 2.657 _shelx_estimated_absorpt_T_min 0.534 _shelx_estimated_absorpt_T_max 0.759 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.74 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed X-Ray Tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 79126 _diffrn_reflns_av_unetI/netI 0.0424 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.542 _diffrn_reflns_theta_max 28.271 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 19525 _reflns_number_gt 16010 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+131.4472P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 19525 _refine_ls_number_parameters 874 _refine_ls_number_restraints 2084 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1753 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.44704(2) 0.79717(2) 0.63120(2) 0.02668(10) Uani 1 1 d . U . . . Er2 Er 0.71898(2) 0.77727(2) 0.62162(2) 0.02240(9) Uani 1 1 d . U . . . Fe1 Fe 0.28132(9) 0.88396(7) 0.59050(7) 0.0428(4) Uani 1 1 d . U . . . Fe2 Fe 0.90356(9) 0.73185(6) 0.69392(7) 0.0411(4) Uani 1 1 d . U . . . Si1 Si 0.3024(2) 0.68324(14) 0.54624(15) 0.0506(8) Uani 1 1 d . U . . . Si2 Si 0.3152(3) 0.7850(2) 0.7542(2) 0.0875(14) Uani 1 1 d . U . . . N1 N 0.3365(5) 0.7511(4) 0.5714(4) 0.0384(17) Uani 1 1 d . U . . . N2 N 0.3732(6) 0.8280(5) 0.7087(4) 0.050(2) Uani 1 1 d . U . . . C1 C 0.5797(5) 0.8460(3) 0.6030(3) 0.0227(14) Uani 1 1 d . U . . . H1A H 0.5702 0.8844 0.5877 0.027 Uiso 1 1 calc R U . . . C2 C 0.5727(5) 0.7955(4) 0.5646(4) 0.0223(14) Uani 1 1 d . U . . . H2A H 0.5744 0.8009 0.5245 0.027 Uiso 1 1 calc R U . . . C3 C 0.5633(6) 0.7380(4) 0.5869(4) 0.0272(15) Uani 1 1 d . U . . . H3A H 0.5502 0.7060 0.5612 0.033 Uiso 1 1 calc R U . . . C4 C 0.5735(5) 0.7281(4) 0.6474(4) 0.0260(15) Uani 1 1 d . U . . . H4A H 0.5597 0.6906 0.6618 0.031 Uiso 1 1 calc R U . . . C5 C 0.6055(5) 0.7759(4) 0.6883(4) 0.0252(14) Uani 1 1 d . U . . . H5A H 0.6276 0.7674 0.7273 0.030 Uiso 1 1 calc R U . . . C6 C 0.6018(5) 0.8374(3) 0.6665(3) 0.0215(14) Uani 1 1 d . U . . . C7 C 0.6212(6) 0.8857(4) 0.7046(4) 0.0324(17) Uani 1 1 d . U . . . C8 C 0.6518(7) 0.8791(5) 0.7645(4) 0.044(2) Uani 1 1 d . U . . . H8A H 0.6617 0.8408 0.7799 0.052 Uiso 1 1 calc R U . A 1 C9 C 0.6675(9) 0.9269(6) 0.8010(6) 0.061(3) Uani 1 1 d . U . . . H9A H 0.6875 0.9202 0.8406 0.073 Uiso 1 1 calc R U . B 1 C10 C 0.6549(9) 0.9842(6) 0.7817(6) 0.063(3) Uani 1 1 d . U . . . H10A H 0.6659 1.0165 0.8071 0.075 Uiso 1 1 calc R U . C 1 C11 C 0.6254(8) 0.9924(5) 0.7231(6) 0.056(3) Uani 1 1 d . U . . . H11A H 0.6158 1.0312 0.7088 0.067 Uiso 1 1 calc R U . D 1 C12 C 0.6097(6) 0.9458(4) 0.6854(5) 0.040(2) Uani 1 1 d . U . . . H12A H 0.5910 0.9534 0.6458 0.048 Uiso 1 1 calc R U . E 1 C13 C 0.2945(6) 0.8027(5) 0.5484(4) 0.0368(17) Uani 1 1 d . U . . . C14 C 0.2022(7) 0.8215(6) 0.5473(5) 0.053(2) Uani 1 1 d . U . . . H14A H 0.1562 0.8005 0.5629 0.064 Uiso 1 1 calc R U . . . C15 C 0.1918(8) 0.8761(6) 0.5193(6) 0.057(2) Uani 1 1 d . U . . . H15A H 0.1372 0.8974 0.5115 0.068 Uiso 1 1 calc R U . . . C16 C 0.2760(7) 0.8938(5) 0.5049(5) 0.051(2) Uani 1 1 d . U . . . H16A H 0.2884 0.9296 0.4867 0.061 Uiso 1 1 calc R U . . . C17 C 0.3395(7) 0.8491(4) 0.5223(5) 0.0399(19) Uani 1 1 d . U . . . H17A H 0.4015 0.8498 0.5175 0.048 Uiso 1 1 calc R U . . . C18 C 0.3287(7) 0.8746(5) 0.6793(5) 0.046(2) Uani 1 1 d . U . . . C19 C 0.2352(7) 0.8896(6) 0.6695(5) 0.052(2) Uani 1 1 d . U . . . H19A H 0.1873 0.8672 0.6814 0.062 Uiso 1 1 calc R U . . . C20 C 0.2266(7) 0.9446(5) 0.6385(5) 0.050(2) Uani 1 1 d . U . . . H20A H 0.1720 0.9650 0.6276 0.060 Uiso 1 1 calc R U . . . C21 C 0.3115(7) 0.9627(6) 0.6272(5) 0.050(2) Uani 1 1 d . U . . . H21A H 0.3243 0.9972 0.6070 0.060 Uiso 1 1 calc R U . . . C22 C 0.3752(7) 0.9210(5) 0.6510(5) 0.045(2) Uani 1 1 d . U . . . H22A H 0.4380 0.9228 0.6491 0.054 Uiso 1 1 calc R U . . . C23 C 0.1809(8) 0.6667(6) 0.5518(7) 0.072(4) Uani 1 1 d . U . . . H23A H 0.1706 0.6672 0.5924 0.108 Uiso 1 1 calc R U . . . H23B H 0.1658 0.6279 0.5354 0.108 Uiso 1 1 calc R U . . . H23C H 0.1430 0.6964 0.5305 0.108 Uiso 1 1 calc R U . . . C24 C 0.3719(8) 0.6278(5) 0.5904(5) 0.055(3) Uani 1 1 d . U . . . H24A H 0.3679 0.6348 0.6314 0.082 Uiso 1 1 calc R U . . . H24B H 0.4346 0.6311 0.5830 0.082 Uiso 1 1 calc R U . . . H24C H 0.3496 0.5883 0.5800 0.082 Uiso 1 1 calc R U . . . C25 C 0.3186(9) 0.6735(6) 0.4667(6) 0.063(3) Uani 1 1 d . U . . . C26 C 0.2511(11) 0.7088(7) 0.4276(7) 0.083(4) Uani 1 1 d . U . . . H26A H 0.2513 0.6956 0.3877 0.124 Uiso 1 1 calc R U . . . H26B H 0.2671 0.7505 0.4305 0.124 Uiso 1 1 calc R U . . . H26C H 0.1911 0.7031 0.4392 0.124 Uiso 1 1 calc R U . . . C27 C 0.3075(12) 0.6091(7) 0.4499(7) 0.085(4) Uani 1 1 d . U . . . H27A H 0.3033 0.6053 0.4079 0.128 Uiso 1 1 calc R U . . . H27B H 0.2526 0.5937 0.4632 0.128 Uiso 1 1 calc R U . . . H27C H 0.3594 0.5868 0.4679 0.128 Uiso 1 1 calc R U . . . C28 C 0.4123(10) 0.6928(7) 0.4566(6) 0.077(4) Uani 1 1 d . U . . . H28A H 0.4192 0.6885 0.4157 0.115 Uiso 1 1 calc R U . . . H28B H 0.4569 0.6684 0.4797 0.115 Uiso 1 1 calc R U . . . H28C H 0.4212 0.7340 0.4680 0.115 Uiso 1 1 calc R U . . . C29 C 0.2283(11) 0.7321(8) 0.7109(7) 0.086(4) Uani 1 1 d . U . . . H29A H 0.1882 0.7157 0.7369 0.129 Uiso 1 1 calc R U . . . H29B H 0.2604 0.7002 0.6942 0.129 Uiso 1 1 calc R U . . . H29C H 0.1929 0.7540 0.6800 0.129 Uiso 1 1 calc R U . . . C30 C 0.2544(11) 0.8343(9) 0.8019(7) 0.092(4) Uani 1 1 d . U . . . H30A H 0.2282 0.8104 0.8305 0.138 Uiso 1 1 calc R U . . . H30B H 0.2066 0.8556 0.7782 0.138 Uiso 1 1 calc R U . . . H30C H 0.2969 0.8624 0.8218 0.138 Uiso 1 1 calc R U . . . C31 C 0.3965(12) 0.7357(8) 0.8002(8) 0.088(4) Uani 1 1 d . U . . . C32 C 0.4695(12) 0.7800(8) 0.8298(7) 0.090(4) Uani 1 1 d . U . . . H32A H 0.4397 0.8157 0.8412 0.136 Uiso 1 1 calc R U . . . H32B H 0.5118 0.7901 0.8026 0.136 Uiso 1 1 calc R U . . . H32C H 0.5020 0.7616 0.8641 0.136 Uiso 1 1 calc R U . . . C33 C 0.4306(13) 0.6874(8) 0.7628(8) 0.097(5) Uani 1 1 d . U . . . H33A H 0.4645 0.6584 0.7876 0.146 Uiso 1 1 calc R U . . . H33B H 0.4697 0.7047 0.7367 0.146 Uiso 1 1 calc R U . . . H33C H 0.3794 0.6683 0.7402 0.146 Uiso 1 1 calc R U . . . C34 C 0.3458(15) 0.7071(10) 0.8471(9) 0.115(6) Uani 1 1 d . U . . . H34A H 0.3839 0.6771 0.8677 0.172 Uiso 1 1 calc R U . . . H34B H 0.2903 0.6890 0.8288 0.172 Uiso 1 1 calc R U . . . H34C H 0.3311 0.7372 0.8743 0.172 Uiso 1 1 calc R U . . . C35 C 0.8396(7) 0.6815(5) 0.6250(5) 0.044(2) Uani 1 1 d . U . . . C36 C 0.8129(8) 0.6640(5) 0.6792(5) 0.050(2) Uani 1 1 d . U . . . H36A H 0.7536 0.6637 0.6895 0.060 Uiso 1 1 calc R U . . . C37 C 0.8931(9) 0.6469(5) 0.7146(6) 0.063(3) Uani 1 1 d . U . . . H37A H 0.8957 0.6327 0.7530 0.075 Uiso 1 1 calc R U . . . C38 C 0.9647(10) 0.6541(6) 0.6854(7) 0.067(3) Uani 1 1 d . U . . . H38A H 1.0251 0.6455 0.7000 0.080 Uiso 1 1 calc R U . . . C39 C 0.9360(8) 0.6764(6) 0.6300(6) 0.061(3) Uani 1 1 d . U . . . H39A H 0.9733 0.6862 0.6014 0.073 Uiso 1 1 calc R U . . . C40 C 0.8845(6) 0.8213(4) 0.6747(5) 0.0373(17) Uani 1 1 d . U . . . C41 C 0.8503(7) 0.8047(4) 0.7266(5) 0.0386(18) Uani 1 1 d . U . . . H41A H 0.7897 0.8094 0.7336 0.046 Uiso 1 1 calc R U . F 1 C42 C 0.9203(8) 0.7799(5) 0.7669(5) 0.051(2) Uani 1 1 d . U . . . H42A H 0.9146 0.7656 0.8044 0.061 Uiso 1 1 calc R U . . . C43 C 0.9990(7) 0.7808(5) 0.7397(5) 0.050(2) Uani 1 1 d . U . . . H43A H 1.0565 0.7676 0.7563 0.060 Uiso 1 1 calc R U . . . C44 C 0.9785(7) 0.8048(5) 0.6830(5) 0.047(2) Uani 1 1 d . U . . . H44A H 1.0197 0.8092 0.6555 0.056 Uiso 1 1 calc R U . . . K2 K 0.8181(3) 0.9428(2) 0.6972(2) 0.0336(10) Uani 0.5 1 d . U P G 1 O2 O 0.8510(11) 1.0565(7) 0.6662(7) 0.055(4) Uani 0.5 1 d D U P G 1 C62 C 0.813(4) 1.0954(15) 0.7019(18) 0.146(19) Uiso 0.5 1 d D . P G 1 H62A H 0.8498 1.0956 0.7402 0.175 Uiso 0.5 1 calc R U P G 1 H62B H 0.7523 1.0816 0.7073 0.175 Uiso 0.5 1 calc R U P G 1 C63 C 0.911(2) 1.0847(14) 0.6343(15) 0.090(10) Uiso 0.5 1 d D . P G 1 H63A H 0.9070 1.0689 0.5947 0.108 Uiso 0.5 1 calc R U P G 1 H63B H 0.9733 1.0817 0.6532 0.108 Uiso 0.5 1 calc R U P G 1 C64 C 0.807(3) 1.1578(17) 0.6783(18) 0.111(13) Uiso 0.5 1 d D . P G 1 H64A H 0.8269 1.1875 0.7080 0.133 Uiso 0.5 1 calc R U P G 1 H64B H 0.7462 1.1675 0.6593 0.133 Uiso 0.5 1 calc R U P G 1 C65 C 0.875(3) 1.1489(18) 0.635(2) 0.17(2) Uiso 0.5 1 d D . P G 1 H65A H 0.9266 1.1758 0.6446 0.198 Uiso 0.5 1 calc R U P G 1 H65B H 0.8464 1.1592 0.5957 0.198 Uiso 0.5 1 calc R U P G 1 K2A K 0.8092(4) 0.9333(3) 0.7328(4) 0.074(2) Uani 0.5 1 d . U P H 2 O2A O 0.9410(11) 0.9904(7) 0.7913(8) 0.076(5) Uani 0.5 1 d D U P I 2 C61A C 1.021(2) 0.9089(10) 0.8267(15) 0.094(9) Uani 0.5 1 d D U P I 2 H61A H 1.0634 0.8930 0.8583 0.141 Uiso 0.5 1 calc R U P I 2 H61B H 1.0477 0.9056 0.7905 0.141 Uiso 0.5 1 calc R U P I 2 H61C H 0.9650 0.8866 0.8237 0.141 Uiso 0.5 1 calc R U P I 2 C62A C 1.002(2) 0.9741(10) 0.8387(12) 0.095(7) Uani 0.5 1 d D U P I 2 H62C H 0.9758 0.9787 0.8752 0.113 Uiso 0.5 1 calc R U P I 2 H62D H 1.0579 0.9978 0.8407 0.113 Uiso 0.5 1 calc R U P I 2 C63A C 0.934(2) 1.0513(9) 0.8015(12) 0.088(7) Uani 0.5 1 d D U P I 2 H63C H 0.9930 1.0707 0.8017 0.106 Uiso 0.5 1 calc R U P I 2 H63D H 0.9118 1.0585 0.8391 0.106 Uiso 0.5 1 calc R U P I 2 C64A C 0.867(2) 1.0747(12) 0.7519(14) 0.096(9) Uani 0.5 1 d D U P I 2 H64C H 0.8593 1.1171 0.7565 0.144 Uiso 0.5 1 calc R U P I 2 H64D H 0.8086 1.0552 0.7526 0.144 Uiso 0.5 1 calc R U P I 2 H64E H 0.8893 1.0668 0.7151 0.144 Uiso 0.5 1 calc R U P I 2 Si3 Si 0.7682(2) 0.66460(16) 0.51372(15) 0.0551(9) Uani 1 1 d D U . . . N3 N 0.7791(6) 0.7007(4) 0.5786(4) 0.0429(18) Uani 1 1 d . U . . . C45 C 0.6870(8) 0.7054(5) 0.4614(4) 0.052(3) Uani 1 1 d D U . . . H45A H 0.7082 0.7458 0.4577 0.078 Uiso 1 1 calc R U . . . H45B H 0.6280 0.7059 0.4753 0.078 Uiso 1 1 calc R U . . . H45C H 0.6823 0.6860 0.4237 0.078 Uiso 1 1 calc R U . . . C47 C 0.7263(8) 0.5868(5) 0.5198(5) 0.067(3) Uani 1 1 d D U . . . C46 C 0.8787(14) 0.6454(15) 0.4879(15) 0.067(7) Uani 0.51(2) 1 d D U P J 1 H46A H 0.9162 0.6240 0.5182 0.101 Uiso 0.51(2) 1 calc R U P J 1 H46B H 0.9095 0.6815 0.4787 0.101 Uiso 0.51(2) 1 calc R U P J 1 H46C H 0.8679 0.6209 0.4533 0.101 Uiso 0.51(2) 1 calc R U P J 1 C48 C 0.6229(11) 0.5877(11) 0.5281(9) 0.058(5) Uani 0.51(2) 1 d D U P J 1 H48A H 0.6152 0.6070 0.5646 0.088 Uiso 0.51(2) 1 calc R U P J 1 H48B H 0.6003 0.5474 0.5285 0.088 Uiso 0.51(2) 1 calc R U P J 1 H48C H 0.5893 0.6094 0.4962 0.088 Uiso 0.51(2) 1 calc R U P J 1 C49 C 0.7138(11) 0.5541(8) 0.4609(6) 0.092(4) Uani 1 1 d D U . . . H49A H 0.6883 0.5811 0.4306 0.137 Uiso 1 1 calc R U . . . H49B H 0.6731 0.5208 0.4631 0.137 Uiso 1 1 calc R U . . . H49C H 0.7722 0.5398 0.4519 0.137 Uiso 1 1 calc R U . . . C50 C 0.7593(19) 0.5493(11) 0.5743(9) 0.069(4) Uani 0.51(2) 1 d D U P J 1 H50A H 0.7626 0.5741 0.6087 0.104 Uiso 0.51(2) 1 calc R U P J 1 H50B H 0.8189 0.5333 0.5705 0.104 Uiso 0.51(2) 1 calc R U P J 1 H50C H 0.7171 0.5171 0.5777 0.104 Uiso 0.51(2) 1 calc R U P J 1 C46A C 0.8736(15) 0.6715(15) 0.4762(14) 0.064(6) Uani 0.49(2) 1 d D U P J 2 H46D H 0.9237 0.6517 0.4993 0.096 Uiso 0.49(2) 1 calc R U P J 2 H46E H 0.8882 0.7131 0.4721 0.096 Uiso 0.49(2) 1 calc R U P J 2 H46F H 0.8630 0.6533 0.4380 0.096 Uiso 0.49(2) 1 calc R U P J 2 C48A C 0.6479(19) 0.5852(14) 0.5561(14) 0.072(6) Uani 0.49(2) 1 d D U P J 2 H48D H 0.5962 0.6057 0.5357 0.108 Uiso 0.49(2) 1 calc R U P J 2 H48E H 0.6658 0.6044 0.5932 0.108 Uiso 0.49(2) 1 calc R U P J 2 H48F H 0.6316 0.5443 0.5627 0.108 Uiso 0.49(2) 1 calc R U P J 2 C50A C 0.8149(16) 0.5565(12) 0.5499(11) 0.069(4) Uani 0.49(2) 1 d D U P J 2 H50D H 0.8611 0.5575 0.5237 0.104 Uiso 0.49(2) 1 calc R U P J 2 H50E H 0.8019 0.5157 0.5591 0.104 Uiso 0.49(2) 1 calc R U P J 2 H50F H 0.8363 0.5777 0.5854 0.104 Uiso 0.49(2) 1 calc R U P J 2 Si4 Si 0.8936(3) 0.8694(2) 0.5677(2) 0.0358(14) Uani 0.586(8) 1 d D U P G 1 N4 N 0.8350(10) 0.8437(7) 0.6212(6) 0.028(3) Uani 0.586(8) 1 d . U P G 1 C51 C 0.9481(16) 0.8104(9) 0.5268(11) 0.051(5) Uani 0.586(8) 1 d D U P G 1 H51A H 0.9907 0.7882 0.5535 0.076 Uiso 0.586(8) 1 calc R U P G 1 H51B H 0.9799 0.8287 0.4972 0.076 Uiso 0.586(8) 1 calc R U P G 1 H51C H 0.9018 0.7839 0.5083 0.076 Uiso 0.586(8) 1 calc R U P G 1 C52 C 0.9837(11) 0.9228(8) 0.5980(9) 0.047(4) Uani 0.586(8) 1 d D U P G 1 H52A H 1.0273 0.9026 0.6258 0.071 Uiso 0.586(8) 1 calc R U P G 1 H52B H 0.9562 0.9551 0.6173 0.071 Uiso 0.586(8) 1 calc R U P G 1 H52C H 1.0143 0.9385 0.5666 0.071 Uiso 0.586(8) 1 calc R U P G 1 C53 C 0.8127(9) 0.9110(6) 0.5147(6) 0.039(3) Uani 0.586(8) 1 d D U P G 1 C54 C 0.7459(11) 0.8685(7) 0.4805(7) 0.035(3) Uani 0.586(8) 1 d D U P G 1 H54A H 0.7790 0.8402 0.4597 0.053 Uiso 0.586(8) 1 calc R U P G 1 H54B H 0.7046 0.8908 0.4530 0.053 Uiso 0.586(8) 1 calc R U P G 1 H54C H 0.7117 0.8475 0.5073 0.053 Uiso 0.586(8) 1 calc R U P G 1 C55 C 0.7582(11) 0.9557(7) 0.5466(8) 0.043(4) Uani 0.586(8) 1 d D U P G 1 H55A H 0.7996 0.9831 0.5686 0.065 Uiso 0.586(8) 1 calc R U P G 1 H55B H 0.7235 0.9347 0.5730 0.065 Uiso 0.586(8) 1 calc R U P G 1 H55C H 0.7173 0.9775 0.5184 0.065 Uiso 0.586(8) 1 calc R U P G 1 C56 C 0.8650(14) 0.9428(11) 0.4701(9) 0.062(5) Uani 0.586(8) 1 d D U P G 1 H56A H 0.9084 0.9702 0.4903 0.093 Uiso 0.586(8) 1 calc R U P G 1 H56B H 0.8227 0.9645 0.4427 0.093 Uiso 0.586(8) 1 calc R U P G 1 H56C H 0.8969 0.9138 0.4493 0.093 Uiso 0.586(8) 1 calc R U P G 1 Si4A Si 0.8640(4) 0.9090(3) 0.5959(4) 0.045(2) Uani 0.414(8) 1 d D U P G 2 N4A N 0.8284(15) 0.8555(10) 0.6389(10) 0.032(3) Uani 0.414(8) 1 d . U P G 2 C51A C 0.7758(16) 0.9681(10) 0.5899(14) 0.049(6) Uani 0.414(8) 1 d D U P G 2 H51D H 0.7672 0.9820 0.6285 0.074 Uiso 0.414(8) 1 calc R U P G 2 H51E H 0.7191 0.9523 0.5708 0.074 Uiso 0.414(8) 1 calc R U P G 2 H51F H 0.7951 1.0009 0.5672 0.074 Uiso 0.414(8) 1 calc R U P G 2 C52A C 0.9712(16) 0.9447(13) 0.6287(16) 0.060(6) Uani 0.414(8) 1 d D U P G 2 H52D H 0.9645 0.9579 0.6678 0.091 Uiso 0.414(8) 1 calc R U P G 2 H52E H 0.9845 0.9784 0.6052 0.091 Uiso 0.414(8) 1 calc R U P G 2 H52F H 1.0205 0.9163 0.6302 0.091 Uiso 0.414(8) 1 calc R U P G 2 C53A C 0.8795(17) 0.8846(10) 0.5211(10) 0.061(5) Uani 0.414(8) 1 d D U P G 2 C54A C 0.920(2) 0.9321(15) 0.4843(17) 0.071(7) Uani 0.414(8) 1 d D U P G 2 H54D H 0.8810 0.9669 0.4817 0.107 Uiso 0.414(8) 1 calc R U P G 2 H54E H 0.9232 0.9167 0.4455 0.107 Uiso 0.414(8) 1 calc R U P G 2 H54F H 0.9798 0.9427 0.5023 0.107 Uiso 0.414(8) 1 calc R U P G 2 C55A C 0.946(3) 0.8324(15) 0.526(2) 0.067(8) Uani 0.414(8) 1 d D U P G 2 H55D H 1.0032 0.8447 0.5465 0.101 Uiso 0.414(8) 1 calc R U P G 2 H55E H 0.9548 0.8193 0.4868 0.101 Uiso 0.414(8) 1 calc R U P G 2 H55F H 0.9208 0.8001 0.5463 0.101 Uiso 0.414(8) 1 calc R U P G 2 C56A C 0.787(2) 0.8667(18) 0.4900(18) 0.071(7) Uani 0.414(8) 1 d D U P G 2 H56D H 0.7455 0.8999 0.4898 0.107 Uiso 0.414(8) 1 calc R U P G 2 H56E H 0.7636 0.8335 0.5103 0.107 Uiso 0.414(8) 1 calc R U P G 2 H56F H 0.7932 0.8553 0.4503 0.107 Uiso 0.414(8) 1 calc R U P G 2 K1 K 0.4629(2) 0.92292(17) 0.77309(13) 0.0769(10) Uani 1 1 d . U . . . O1 O 0.4018(7) 0.9982(5) 0.8481(4) 0.090(3) Uani 1 1 d D U . . . C57 C 0.5128(10) 0.9616(7) 0.9172(7) 0.086(4) Uani 1 1 d D U . . . H57A H 0.5440 0.9683 0.9560 0.129 Uiso 1 1 calc R U . . . H57B H 0.5564 0.9623 0.8892 0.129 Uiso 1 1 calc R U . . . H57C H 0.4828 0.9234 0.9159 0.129 Uiso 1 1 calc R U . . . C58 C 0.4457(10) 1.0080(7) 0.9031(6) 0.077(3) Uani 1 1 d D U . . . H58A H 0.4018 1.0078 0.9315 0.093 Uiso 1 1 calc R U . . . H58B H 0.4756 1.0468 0.9047 0.093 Uiso 1 1 calc R U . . . C59 C 0.3328(11) 1.0379(8) 0.8342(7) 0.095(4) Uani 1 1 d D U . . . H59A H 0.3565 1.0784 0.8378 0.114 Uiso 1 1 calc R U . . . H59B H 0.2871 1.0333 0.8611 0.114 Uiso 1 1 calc R U . . . C60 C 0.2916(15) 1.0274(11) 0.7749(8) 0.142(7) Uani 1 1 d D U . . . H60A H 0.2427 1.0555 0.7650 0.212 Uiso 1 1 calc R U . . . H60B H 0.2677 0.9874 0.7716 0.212 Uiso 1 1 calc R U . . . H60C H 0.3369 1.0324 0.7484 0.212 Uiso 1 1 calc R U . . . O1S O 0.5399(15) 0.9285(10) 0.4050(10) 0.100 Uiso 0.5 1 d D U P K -1 C1S C 0.498(3) 0.9914(15) 0.4766(14) 0.100 Uiso 0.5 1 d D U P K -1 H1S1 H 0.4809 0.9916 0.5158 0.150 Uiso 0.5 1 calc R U P K -1 H1S2 H 0.4515 1.0108 0.4503 0.150 Uiso 0.5 1 calc R U P K -1 H1S3 H 0.5551 1.0124 0.4764 0.150 Uiso 0.5 1 calc R U P K -1 C2S C 0.509(3) 0.9282(13) 0.4572(13) 0.100 Uiso 0.5 1 d D U P K -1 H2S1 H 0.5520 0.9072 0.4856 0.120 Uiso 0.5 1 calc R U P K -1 H2S2 H 0.4506 0.9076 0.4543 0.120 Uiso 0.5 1 calc R U P K -1 C3S C 0.5359(18) 0.8747(13) 0.3755(16) 0.100 Uiso 0.5 1 d D U P K -1 H3S1 H 0.5685 0.8436 0.3991 0.120 Uiso 0.5 1 calc R U P K -1 H3S2 H 0.5612 0.8781 0.3385 0.120 Uiso 0.5 1 calc R U P K -1 C4S C 0.4346(19) 0.8621(15) 0.3656(10) 0.100 Uiso 0.5 1 d D U P K -1 H4S1 H 0.4245 0.8224 0.3502 0.150 Uiso 0.5 1 calc R U P K -1 H4S2 H 0.4052 0.8906 0.3382 0.150 Uiso 0.5 1 calc R U P K -1 H4S3 H 0.4096 0.8653 0.4023 0.150 Uiso 0.5 1 calc R U P K -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01579(16) 0.0334(2) 0.0312(2) 0.00373(16) 0.00430(13) -0.00380(14) Er2 0.01732(16) 0.01931(17) 0.03095(19) 0.00272(14) 0.00450(13) 0.00169(13) Fe1 0.0187(6) 0.0525(9) 0.0570(9) 0.0117(7) 0.0043(6) 0.0037(6) Fe2 0.0334(7) 0.0290(7) 0.0569(9) 0.0004(6) -0.0102(6) 0.0131(5) Si1 0.0421(15) 0.0416(16) 0.0621(19) 0.0130(14) -0.0186(14) -0.0225(13) Si2 0.083(3) 0.113(3) 0.077(3) 0.027(2) 0.055(2) 0.028(2) N1 0.024(3) 0.042(3) 0.048(4) 0.010(3) -0.005(3) -0.009(2) N2 0.040(4) 0.069(4) 0.044(4) 0.003(3) 0.015(3) 0.014(3) C1 0.017(3) 0.020(3) 0.030(3) -0.002(2) -0.002(2) -0.005(2) C2 0.016(3) 0.025(3) 0.025(3) 0.001(2) 0.005(2) -0.002(2) C3 0.027(3) 0.025(3) 0.029(3) 0.000(2) 0.002(2) -0.005(2) C4 0.026(3) 0.021(3) 0.030(3) 0.004(2) 0.000(2) -0.004(2) C5 0.023(3) 0.025(3) 0.027(3) 0.001(2) 0.001(2) -0.001(2) C6 0.018(3) 0.021(3) 0.025(3) -0.003(2) 0.002(2) -0.001(2) C7 0.026(4) 0.030(3) 0.039(3) -0.011(3) -0.003(3) 0.003(3) C8 0.045(5) 0.044(4) 0.039(4) -0.013(3) -0.006(3) 0.008(3) C9 0.065(6) 0.056(4) 0.056(5) -0.022(4) -0.011(4) 0.009(4) C10 0.067(6) 0.052(5) 0.065(5) -0.025(4) -0.008(4) 0.007(4) C11 0.057(5) 0.041(4) 0.067(5) -0.021(4) -0.005(4) 0.010(4) C12 0.034(4) 0.032(3) 0.053(4) -0.009(3) -0.003(3) 0.007(3) C13 0.026(3) 0.044(3) 0.039(4) 0.011(3) -0.003(3) -0.006(3) C14 0.033(4) 0.061(4) 0.063(5) 0.006(4) -0.003(3) 0.001(3) C15 0.040(4) 0.063(5) 0.063(5) 0.006(4) -0.005(3) 0.008(3) C16 0.042(4) 0.051(4) 0.059(4) 0.010(3) -0.002(3) 0.009(3) C17 0.033(4) 0.037(4) 0.048(4) 0.012(3) 0.000(3) 0.001(3) C18 0.031(3) 0.059(4) 0.052(4) 0.001(3) 0.012(3) 0.006(3) C19 0.035(4) 0.060(5) 0.063(5) 0.004(4) 0.013(3) 0.005(3) C20 0.029(4) 0.054(4) 0.067(5) 0.002(4) 0.006(3) 0.003(3) C21 0.032(4) 0.056(4) 0.061(5) -0.001(3) 0.006(3) 0.002(3) C22 0.029(3) 0.056(4) 0.051(4) -0.002(3) 0.006(3) 0.000(3) C23 0.048(5) 0.072(8) 0.092(9) 0.017(7) -0.015(5) -0.032(5) C24 0.056(6) 0.042(5) 0.060(6) 0.010(4) -0.015(5) -0.022(4) C25 0.067(5) 0.056(5) 0.060(5) 0.002(4) -0.016(4) -0.018(4) C26 0.090(8) 0.075(8) 0.073(7) 0.006(6) -0.027(6) -0.011(6) C27 0.098(9) 0.065(6) 0.084(9) -0.006(5) -0.021(7) -0.018(6) C28 0.085(6) 0.085(9) 0.056(7) -0.011(6) -0.009(5) -0.028(6) C29 0.075(7) 0.103(9) 0.088(8) 0.013(7) 0.047(6) -0.008(6) C30 0.083(8) 0.126(9) 0.074(8) 0.009(7) 0.043(7) 0.029(7) C31 0.090(6) 0.098(6) 0.081(6) 0.014(5) 0.033(5) 0.009(5) C32 0.090(7) 0.105(7) 0.081(7) 0.006(6) 0.033(5) 0.009(5) C33 0.110(10) 0.094(8) 0.098(9) 0.016(6) 0.053(8) 0.007(7) C34 0.127(11) 0.127(11) 0.101(9) 0.027(8) 0.057(8) 0.002(8) C35 0.038(4) 0.036(4) 0.055(4) -0.010(3) -0.003(3) 0.012(3) C36 0.053(4) 0.035(4) 0.058(4) -0.001(3) -0.008(3) 0.005(3) C37 0.068(5) 0.038(4) 0.076(5) 0.002(4) -0.016(4) 0.006(4) C38 0.061(5) 0.048(5) 0.086(5) -0.006(4) -0.015(4) 0.017(4) C39 0.047(4) 0.057(5) 0.077(5) -0.011(4) -0.005(3) 0.019(4) C40 0.028(3) 0.030(3) 0.051(4) 0.002(3) -0.004(3) 0.000(2) C41 0.032(4) 0.033(4) 0.050(4) -0.004(3) -0.002(3) 0.000(3) C42 0.045(4) 0.050(5) 0.055(4) -0.001(3) -0.006(3) 0.002(3) C43 0.037(4) 0.051(5) 0.059(4) -0.001(4) -0.010(3) 0.006(3) C44 0.030(3) 0.049(4) 0.058(4) 0.003(3) -0.005(3) 0.003(3) K2 0.040(2) 0.025(2) 0.035(2) -0.0015(18) 0.0060(19) -0.0050(15) O2 0.065(7) 0.037(6) 0.061(7) -0.003(5) 0.003(6) -0.009(5) K2A 0.043(3) 0.040(3) 0.133(7) -0.036(4) -0.016(4) -0.001(2) O2A 0.053(7) 0.089(7) 0.084(8) 0.014(6) 0.005(6) -0.020(6) C61A 0.074(14) 0.087(10) 0.114(16) -0.012(9) -0.010(13) -0.009(9) C62A 0.093(11) 0.090(9) 0.097(10) -0.002(7) -0.005(7) -0.006(7) C63A 0.082(10) 0.090(8) 0.091(10) 0.001(6) 0.005(8) -0.013(6) C64A 0.095(14) 0.092(13) 0.099(13) -0.003(10) 0.002(11) -0.006(11) Si3 0.0512(18) 0.064(2) 0.0506(18) -0.0230(15) 0.0091(14) 0.0212(15) N3 0.038(3) 0.041(4) 0.049(3) -0.012(3) 0.003(3) 0.014(3) C45 0.057(5) 0.059(6) 0.042(5) -0.010(4) 0.015(4) 0.007(5) C47 0.081(5) 0.055(5) 0.064(5) -0.015(4) -0.001(4) 0.013(4) C46 0.064(8) 0.064(12) 0.077(13) -0.023(10) 0.019(8) 0.023(7) C48 0.083(7) 0.034(9) 0.055(10) -0.012(8) -0.003(6) 0.005(6) C49 0.110(9) 0.087(9) 0.075(6) -0.032(6) 0.000(6) 0.011(7) C50 0.083(7) 0.053(7) 0.069(7) -0.013(5) 0.000(5) 0.012(6) C46A 0.062(8) 0.063(13) 0.071(12) -0.007(10) 0.021(8) 0.027(7) C48A 0.092(9) 0.049(11) 0.075(12) -0.019(9) 0.008(9) 0.000(8) C50A 0.083(7) 0.053(7) 0.069(7) -0.013(5) 0.000(5) 0.012(6) Si4 0.022(2) 0.046(3) 0.040(2) 0.0093(19) 0.0027(16) -0.0073(17) N4 0.017(4) 0.031(5) 0.035(4) 0.003(4) 0.000(3) 0.001(3) C51 0.040(8) 0.055(9) 0.060(9) 0.001(7) 0.016(7) -0.002(7) C52 0.029(6) 0.059(8) 0.056(9) -0.003(7) 0.012(6) -0.012(6) C53 0.033(5) 0.039(5) 0.044(5) 0.014(4) -0.001(4) -0.008(4) C54 0.028(6) 0.041(7) 0.035(7) 0.016(5) 0.002(5) -0.005(5) C55 0.040(7) 0.037(7) 0.051(8) 0.012(6) -0.004(6) -0.005(5) C56 0.050(8) 0.074(10) 0.061(8) 0.032(7) 0.003(7) -0.016(7) Si4A 0.029(3) 0.019(3) 0.089(5) 0.015(3) 0.015(3) 0.000(2) N4A 0.023(5) 0.023(5) 0.048(6) -0.001(4) 0.000(4) -0.001(3) C51A 0.043(9) 0.031(8) 0.074(13) 0.015(8) 0.011(8) 0.004(7) C52A 0.043(8) 0.042(11) 0.096(13) 0.010(9) 0.006(8) -0.006(7) C53A 0.058(8) 0.051(7) 0.077(7) 0.011(5) 0.018(5) -0.004(6) C54A 0.061(12) 0.060(10) 0.096(12) 0.023(9) 0.022(9) -0.001(9) C55A 0.062(11) 0.052(10) 0.091(14) 0.014(8) 0.023(9) -0.001(8) C56A 0.064(9) 0.070(13) 0.083(12) 0.011(9) 0.019(8) -0.010(8) K1 0.0680(18) 0.107(2) 0.0553(17) -0.0363(16) 0.0060(14) 0.0282(17) O1 0.097(5) 0.096(6) 0.081(5) -0.026(4) 0.031(4) 0.005(4) C57 0.092(7) 0.091(7) 0.080(7) -0.014(6) 0.027(6) -0.014(6) C58 0.088(6) 0.079(7) 0.071(5) -0.021(5) 0.032(5) -0.017(5) C59 0.095(7) 0.098(8) 0.099(7) -0.014(6) 0.034(5) 0.004(6) C60 0.150(10) 0.147(11) 0.126(8) -0.022(7) 0.012(7) 0.019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N1 2.289(8) . ? Er1 N2 2.344(9) . ? Er1 C1 2.440(8) . ? Er1 C4 2.459(8) . ? Er1 C3 2.525(9) . ? Er1 C6 2.538(8) . ? Er1 C2 2.588(8) . ? Er1 C5 2.626(8) . ? Er1 C13 2.813(9) . ? Er1 C18 2.832(11) . ? Er1 Fe1 3.2284(15) . ? Er1 K1 4.368(3) . ? Er2 N3 2.257(8) . ? Er2 N4 2.309(15) . ? Er2 N4A 2.42(2) . ? Er2 C5 2.446(8) . ? Er2 C2 2.460(8) . ? Er2 C3 2.540(8) . ? Er2 C6 2.554(8) . ? Er2 C4 2.590(8) . ? Er2 C1 2.605(8) . ? Er2 C40 2.821(9) . ? Er2 C35 2.830(10) . ? Er2 Fe2 3.2333(14) . ? Fe1 C16 2.005(12) . ? Fe1 C15 2.014(12) . ? Fe1 C21 2.017(12) . ? Fe1 C20 2.017(12) . ? Fe1 C14 2.039(12) . ? Fe1 C22 2.053(11) . ? Fe1 C19 2.054(12) . ? Fe1 C17 2.067(11) . ? Fe1 C13 2.118(11) . ? Fe1 C18 2.120(12) . ? Fe2 C37 2.006(12) . ? Fe2 C38 2.016(12) . ? Fe2 C43 2.017(11) . ? Fe2 C42 2.016(12) . ? Fe2 C41 2.032(10) . ? Fe2 C44 2.042(12) . ? Fe2 C39 2.060(13) . ? Fe2 C36 2.061(12) . ? Fe2 C40 2.101(10) . ? Fe2 C35 2.111(11) . ? Si1 N1 1.711(9) . ? Si1 C24 1.868(12) . ? Si1 C23 1.882(13) . ? Si1 C25 1.917(15) . ? Si2 N2 1.754(11) . ? Si2 C31 1.893(19) . ? Si2 C30 1.894(15) . ? Si2 C29 1.966(18) . ? Si2 K1 3.840(7) . ? N1 C13 1.409(12) . ? N2 C18 1.391(14) . ? N2 K1 2.875(11) . ? C1 C2 1.456(11) . ? C1 C6 1.492(11) . ? C1 H1A 0.9500 . ? C2 C3 1.423(11) . ? C2 H2A 0.9500 . ? C3 C4 1.421(12) . ? C3 H3A 0.9500 . ? C4 C5 1.490(11) . ? C4 H4A 0.9500 . ? C5 C6 1.491(11) . ? C5 H5A 0.9500 . ? C6 C7 1.424(11) . ? C7 C8 1.427(14) . ? C7 C12 1.446(13) . ? C7 K1 3.139(10) . ? C7 K2 3.253(10) . ? C8 C9 1.386(15) . ? C8 K1 3.034(11) . ? C8 K2 3.431(13) . ? C8 H8A 0.9500 . ? C9 C10 1.387(18) . ? C9 K1 3.061(13) . ? C9 K2 3.531(15) . ? C9 H9A 0.9500 . ? C10 C11 1.399(18) . ? C10 K1 3.186(14) . ? C10 K2 3.458(15) . ? C10 H10A 0.9500 . ? C11 C12 1.383(14) . ? C11 K2 3.230(13) . ? C11 K1 3.243(14) . ? C11 H11A 0.9500 . ? C12 K2 3.105(11) . ? C12 K1 3.230(12) . ? C12 H12A 0.9500 . ? C13 C17 1.431(13) . ? C13 C14 1.447(14) . ? C14 C15 1.405(17) . ? C14 H14A 0.9500 . ? C15 C16 1.407(17) . ? C15 H15A 0.9500 . ? C16 C17 1.421(14) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.433(14) . ? C18 C22 1.469(16) . ? C18 K1 3.000(12) . ? C19 C20 1.447(17) . ? C19 H19A 0.9500 . ? C20 C21 1.394(15) . ? C20 H20A 0.9500 . ? C21 C22 1.412(15) . ? C21 H21A 0.9500 . ? C22 K1 2.992(11) . ? C22 H22A 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.510(19) . ? C25 C28 1.52(2) . ? C25 C27 1.525(19) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.53(2) . ? C31 C34 1.55(2) . ? C31 C32 1.58(2) . ? C32 K1 3.515(19) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N3 1.397(13) . ? C35 C36 1.431(17) . ? C35 C39 1.442(15) . ? C36 C37 1.429(16) . ? C36 H36A 0.9500 . ? C37 C38 1.35(2) . ? C37 H37A 0.9500 . ? C38 C39 1.408(19) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 N4A 1.36(2) . ? C40 C41 1.425(15) . ? C40 C44 1.450(13) . ? C40 N4 1.466(17) . ? C40 K2 3.010(11) . ? C41 C42 1.439(14) . ? C41 K2 3.244(11) . ? C41 H41A 0.9500 . ? C42 C43 1.408(17) . ? C42 H42A 0.9500 . ? C43 C44 1.431(16) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? K2 O2 2.753(16) . ? O2 C62 1.386(17) . ? O2 C63 1.390(17) . ? C62 C64 1.524(19) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C65 1.556(19) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.542(19) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? O2A C62A 1.400(16) . ? O2A C63A 1.415(16) . ? C61A C62A 1.547(18) . ? C61A H61A 0.9800 . ? C61A H61B 0.9800 . ? C61A H61C 0.9800 . ? C62A H62C 0.9900 . ? C62A H62D 0.9900 . ? C63A C64A 1.537(18) . ? C63A H63C 0.9900 . ? C63A H63D 0.9900 . ? C64A H64C 0.9800 . ? C64A H64D 0.9800 . ? C64A H64E 0.9800 . ? Si3 N3 1.715(9) . ? Si3 C45 1.866(10) . ? Si3 C46 1.883(14) . ? Si3 C47 1.893(11) . ? Si3 C46A 1.905(14) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 C48A 1.533(15) . ? C47 C49 1.557(12) . ? C47 C50 1.562(14) . ? C47 C50A 1.583(14) . ? C47 C48 1.587(14) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C46A H46D 0.9800 . ? C46A H46E 0.9800 . ? C46A H46F 0.9800 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? C50A H50D 0.9800 . ? C50A H50E 0.9800 . ? C50A H50F 0.9800 . ? Si4 N4 1.715(16) . ? Si4 C53 1.881(12) . ? Si4 C52 1.892(13) . ? Si4 C51 1.893(14) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.544(14) . ? C53 C55 1.554(14) . ? C53 C56 1.560(14) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? Si4A N4A 1.71(2) . ? Si4A C53A 1.88(2) . ? Si4A C52A 1.88(2) . ? Si4A C51A 1.882(19) . ? C51A H51D 0.9800 . ? C51A H51E 0.9800 . ? C51A H51F 0.9800 . ? C52A H52D 0.9800 . ? C52A H52E 0.9800 . ? C52A H52F 0.9800 . ? C53A C56A 1.54(3) . ? C53A C55A 1.55(2) . ? C53A C54A 1.55(2) . ? C54A H54D 0.9800 . ? C54A H54E 0.9800 . ? C54A H54F 0.9800 . ? C55A H55D 0.9800 . ? C55A H55E 0.9800 . ? C55A H55F 0.9800 . ? C56A H56D 0.9800 . ? C56A H56E 0.9800 . ? C56A H56F 0.9800 . ? K1 O1 2.694(10) . ? O1 C59 1.383(14) . ? O1 C58 1.389(13) . ? C57 C58 1.470(17) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.467(19) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O1S C2S 1.355(17) . ? O1S C3S 1.406(17) . ? C1S C2S 1.527(19) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.535(19) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Er1 N2 103.5(3) . . ? N1 Er1 C1 126.8(3) . . ? N2 Er1 C1 123.4(3) . . ? N1 Er1 C4 106.7(3) . . ? N2 Er1 C4 120.1(3) . . ? C1 Er1 C4 72.2(3) . . ? N1 Er1 C3 89.4(3) . . ? N2 Er1 C3 153.2(3) . . ? C1 Er1 C3 60.4(3) . . ? C4 Er1 C3 33.1(3) . . ? N1 Er1 C6 158.4(3) . . ? N2 Er1 C6 98.1(3) . . ? C1 Er1 C6 34.8(3) . . ? C4 Er1 C6 61.6(3) . . ? C3 Er1 C6 71.1(3) . . ? N1 Er1 C2 98.8(3) . . ? N2 Er1 C2 156.5(3) . . ? C1 Er1 C2 33.5(2) . . ? C4 Er1 C2 58.5(3) . . ? C3 Er1 C2 32.3(3) . . ? C6 Er1 C2 59.7(3) . . ? N1 Er1 C5 140.3(3) . . ? N2 Er1 C5 98.4(3) . . ? C1 Er1 C5 60.3(3) . . ? C4 Er1 C5 33.9(3) . . ? C3 Er1 C5 58.8(3) . . ? C6 Er1 C5 33.5(2) . . ? C2 Er1 C5 67.8(3) . . ? N1 Er1 C13 29.9(3) . . ? N2 Er1 C13 95.5(3) . . ? C1 Er1 C13 114.6(3) . . ? C4 Er1 C13 133.0(3) . . ? C3 Er1 C13 106.7(3) . . ? C6 Er1 C13 147.4(3) . . ? C2 Er1 C13 100.3(3) . . ? C5 Er1 C13 165.5(3) . . ? N1 Er1 C18 94.9(3) . . ? N2 Er1 C18 29.3(3) . . ? C1 Er1 C18 113.2(3) . . ? C4 Er1 C18 147.9(3) . . ? C3 Er1 C18 173.6(3) . . ? C6 Er1 C18 103.8(3) . . ? C2 Er1 C18 141.8(3) . . ? C5 Er1 C18 119.1(3) . . ? C13 Er1 C18 75.4(3) . . ? N1 Er1 Fe1 68.1(2) . . ? N2 Er1 Fe1 67.9(2) . . ? C1 Er1 Fe1 105.39(19) . . ? C4 Er1 Fe1 171.8(2) . . ? C3 Er1 Fe1 138.8(2) . . ? C6 Er1 Fe1 121.02(18) . . ? C2 Er1 Fe1 115.05(18) . . ? C5 Er1 Fe1 151.64(19) . . ? C13 Er1 Fe1 40.3(2) . . ? C18 Er1 Fe1 40.3(2) . . ? N1 Er1 K1 137.1(2) . . ? N2 Er1 K1 37.2(3) . . ? C1 Er1 K1 86.28(19) . . ? C4 Er1 K1 109.5(2) . . ? C3 Er1 K1 133.28(19) . . ? C6 Er1 K1 63.49(18) . . ? C2 Er1 K1 119.37(18) . . ? C5 Er1 K1 76.89(19) . . ? C13 Er1 K1 117.2(2) . . ? C18 Er1 K1 43.0(2) . . ? Fe1 Er1 K1 77.88(5) . . ? N3 Er2 N4 99.4(4) . . ? N3 Er2 N4A 110.1(6) . . ? N3 Er2 C5 128.4(3) . . ? N4 Er2 C5 126.6(4) . . ? N4A Er2 C5 114.4(6) . . ? N3 Er2 C2 105.5(3) . . ? N4 Er2 C2 120.7(4) . . ? N4A Er2 C2 120.5(6) . . ? C5 Er2 C2 72.7(3) . . ? N3 Er2 C3 89.2(3) . . ? N4 Er2 C3 153.4(4) . . ? N4A Er2 C3 152.9(6) . . ? C5 Er2 C3 60.9(3) . . ? C2 Er2 C3 33.0(3) . . ? N3 Er2 C6 158.6(3) . . ? N4 Er2 C6 102.0(4) . . ? N4A Er2 C6 91.3(6) . . ? C5 Er2 C6 34.6(3) . . ? C2 Er2 C6 61.2(3) . . ? C3 Er2 C6 70.6(3) . . ? N3 Er2 C4 99.4(3) . . ? N4 Er2 C4 160.5(4) . . ? N4A Er2 C4 148.5(6) . . ? C5 Er2 C4 34.3(3) . . ? C2 Er2 C4 58.5(3) . . ? C3 Er2 C4 32.1(3) . . ? C6 Er2 C4 59.6(3) . . ? N3 Er2 C1 138.3(3) . . ? N4 Er2 C1 101.2(4) . . ? N4A Er2 C1 95.7(6) . . ? C5 Er2 C1 60.5(3) . . ? C2 Er2 C1 33.3(2) . . ? C3 Er2 C1 58.1(3) . . ? C6 Er2 C1 33.6(2) . . ? C4 Er2 C1 67.5(2) . . ? N3 Er2 C40 95.4(3) . . ? N4 Er2 C40 31.2(4) . . ? N4A Er2 C40 28.7(6) . . ? C5 Er2 C40 111.6(3) . . ? C2 Er2 C40 149.0(3) . . ? C3 Er2 C40 172.5(3) . . ? C6 Er2 C40 104.0(3) . . ? C4 Er2 C40 140.7(3) . . ? C1 Er2 C40 120.3(3) . . ? N3 Er2 C35 29.2(3) . . ? N4 Er2 C35 91.5(4) . . ? N4A Er2 C35 98.3(6) . . ? C5 Er2 C35 117.7(3) . . ? C2 Er2 C35 132.1(3) . . ? C3 Er2 C35 107.3(3) . . ? C6 Er2 C35 150.8(3) . . ? C4 Er2 C35 102.4(3) . . ? C1 Er2 C35 164.9(3) . . ? C40 Er2 C35 74.7(3) . . ? N3 Er2 Fe2 67.8(2) . . ? N4 Er2 Fe2 67.3(4) . . ? N4A Er2 Fe2 68.2(5) . . ? C5 Er2 Fe2 106.33(19) . . ? C2 Er2 Fe2 171.04(19) . . ? C3 Er2 Fe2 138.56(19) . . ? C6 Er2 Fe2 123.10(18) . . ? C4 Er2 Fe2 115.62(18) . . ? C1 Er2 Fe2 153.90(17) . . ? C40 Er2 Fe2 39.9(2) . . ? C35 Er2 Fe2 40.0(2) . . ? C16 Fe1 C15 41.0(5) . . ? C16 Fe1 C21 107.7(5) . . ? C15 Fe1 C21 121.5(5) . . ? C16 Fe1 C20 120.6(5) . . ? C15 Fe1 C20 104.1(5) . . ? C21 Fe1 C20 40.4(4) . . ? C16 Fe1 C14 68.6(5) . . ? C15 Fe1 C14 40.5(5) . . ? C21 Fe1 C14 156.7(5) . . ? C20 Fe1 C14 120.1(5) . . ? C16 Fe1 C22 125.6(5) . . ? C15 Fe1 C22 159.7(5) . . ? C21 Fe1 C22 40.6(4) . . ? C20 Fe1 C22 68.1(4) . . ? C14 Fe1 C22 159.6(5) . . ? C16 Fe1 C19 156.0(5) . . ? C15 Fe1 C19 119.0(5) . . ? C21 Fe1 C19 69.2(5) . . ? C20 Fe1 C19 41.6(5) . . ? C14 Fe1 C19 104.4(5) . . ? C22 Fe1 C19 68.4(5) . . ? C16 Fe1 C17 40.8(4) . . ? C15 Fe1 C17 68.4(5) . . ? C21 Fe1 C17 125.2(4) . . ? C20 Fe1 C17 158.6(5) . . ? C14 Fe1 C17 68.0(5) . . ? C22 Fe1 C17 111.7(4) . . ? C19 Fe1 C17 159.6(4) . . ? C16 Fe1 C13 68.3(4) . . ? C15 Fe1 C13 68.3(4) . . ? C21 Fe1 C13 161.3(4) . . ? C20 Fe1 C13 157.7(4) . . ? C14 Fe1 C13 40.7(4) . . ? C22 Fe1 C13 125.8(4) . . ? C19 Fe1 C13 122.2(4) . . ? C17 Fe1 C13 40.0(4) . . ? C16 Fe1 C18 162.8(4) . . ? C15 Fe1 C18 155.4(5) . . ? C21 Fe1 C18 69.0(5) . . ? C20 Fe1 C18 68.6(5) . . ? C14 Fe1 C18 121.3(5) . . ? C22 Fe1 C18 41.2(4) . . ? C19 Fe1 C18 40.1(4) . . ? C17 Fe1 C18 126.4(4) . . ? C13 Fe1 C18 109.1(4) . . ? C16 Fe1 Er1 107.3(3) . . ? C15 Fe1 Er1 126.9(4) . . ? C21 Fe1 Er1 107.2(3) . . ? C20 Fe1 Er1 127.4(3) . . ? C14 Fe1 Er1 95.7(3) . . ? C22 Fe1 Er1 67.1(3) . . ? C19 Fe1 Er1 96.0(3) . . ? C17 Fe1 Er1 67.0(3) . . ? C13 Fe1 Er1 59.2(2) . . ? C18 Fe1 Er1 59.8(3) . . ? C37 Fe2 C38 39.3(6) . . ? C37 Fe2 C43 118.5(5) . . ? C38 Fe2 C43 103.7(5) . . ? C37 Fe2 C42 109.0(5) . . ? C38 Fe2 C42 123.3(5) . . ? C43 Fe2 C42 40.9(5) . . ? C37 Fe2 C41 130.7(5) . . ? C38 Fe2 C41 163.7(5) . . ? C43 Fe2 C41 68.6(4) . . ? C42 Fe2 C41 41.6(4) . . ? C37 Fe2 C44 151.3(5) . . ? C38 Fe2 C44 116.1(5) . . ? C43 Fe2 C44 41.3(5) . . ? C42 Fe2 C44 69.5(5) . . ? C41 Fe2 C44 68.2(4) . . ? C37 Fe2 C39 67.4(6) . . ? C38 Fe2 C39 40.4(5) . . ? C43 Fe2 C39 120.6(5) . . ? C42 Fe2 C39 158.5(5) . . ? C41 Fe2 C39 155.9(5) . . ? C44 Fe2 C39 103.1(6) . . ? C37 Fe2 C36 41.1(5) . . ? C38 Fe2 C36 67.8(5) . . ? C43 Fe2 C36 156.3(5) . . ? C42 Fe2 C36 124.1(5) . . ? C41 Fe2 C36 113.3(4) . . ? C44 Fe2 C36 162.4(5) . . ? C39 Fe2 C36 68.1(5) . . ? C37 Fe2 C40 167.4(5) . . ? C38 Fe2 C40 152.1(6) . . ? C43 Fe2 C40 69.2(4) . . ? C42 Fe2 C40 69.7(5) . . ? C41 Fe2 C40 40.3(4) . . ? C44 Fe2 C40 41.0(4) . . ? C39 Fe2 C40 118.6(5) . . ? C36 Fe2 C40 128.6(4) . . ? C37 Fe2 C35 67.6(5) . . ? C38 Fe2 C35 67.5(5) . . ? C43 Fe2 C35 158.9(5) . . ? C42 Fe2 C35 159.9(5) . . ? C41 Fe2 C35 124.6(4) . . ? C44 Fe2 C35 123.6(5) . . ? C39 Fe2 C35 40.4(4) . . ? C36 Fe2 C35 40.1(5) . . ? C40 Fe2 C35 109.1(4) . . ? C37 Fe2 Er2 110.4(4) . . ? C38 Fe2 Er2 126.9(4) . . ? C43 Fe2 Er2 127.4(3) . . ? C42 Fe2 Er2 106.2(3) . . ? C41 Fe2 Er2 65.4(3) . . ? C44 Fe2 Er2 97.1(3) . . ? C39 Fe2 Er2 94.6(3) . . ? C36 Fe2 Er2 69.4(3) . . ? C40 Fe2 Er2 59.4(3) . . ? C35 Fe2 Er2 59.6(3) . . ? N1 Si1 C24 107.4(5) . . ? N1 Si1 C23 114.2(6) . . ? C24 Si1 C23 107.8(6) . . ? N1 Si1 C25 111.7(5) . . ? C24 Si1 C25 109.2(6) . . ? C23 Si1 C25 106.4(6) . . ? N2 Si2 C31 110.1(6) . . ? N2 Si2 C30 109.7(7) . . ? C31 Si2 C30 110.0(8) . . ? N2 Si2 C29 112.1(6) . . ? C31 Si2 C29 105.6(9) . . ? C30 Si2 C29 109.3(8) . . ? N2 Si2 K1 44.8(4) . . ? C31 Si2 K1 95.6(6) . . ? C30 Si2 K1 76.1(6) . . ? C29 Si2 K1 154.1(5) . . ? C13 N1 Si1 121.4(6) . . ? C13 N1 Er1 96.2(6) . . ? Si1 N1 Er1 142.1(5) . . ? C18 N2 Si2 118.9(7) . . ? C18 N2 Er1 95.2(6) . . ? Si2 N2 Er1 128.2(6) . . ? C18 N2 K1 81.4(7) . . ? Si2 N2 K1 109.7(5) . . ? Er1 N2 K1 113.3(4) . . ? C2 C1 C6 120.0(7) . . ? C2 C1 Er1 78.8(4) . . ? C6 C1 Er1 76.2(4) . . ? C2 C1 Er2 67.9(4) . . ? C6 C1 Er2 71.3(4) . . ? Er1 C1 Er2 110.2(3) . . ? C2 C1 H1A 120.0 . . ? C6 C1 H1A 120.0 . . ? Er1 C1 H1A 115.6 . . ? Er2 C1 H1A 134.2 . . ? C3 C2 C1 120.3(7) . . ? C3 C2 Er2 76.6(5) . . ? C1 C2 Er2 78.9(4) . . ? C3 C2 Er1 71.4(5) . . ? C1 C2 Er1 67.7(4) . . ? Er2 C2 Er1 110.1(3) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? Er2 C2 H2A 115.3 . . ? Er1 C2 H2A 134.6 . . ? C4 C3 C2 120.5(8) . . ? C4 C3 Er1 70.9(5) . . ? C2 C3 Er1 76.3(5) . . ? C4 C3 Er2 75.9(5) . . ? C2 C3 Er2 70.4(4) . . ? Er1 C3 Er2 109.6(3) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? Er1 C3 H3A 124.7 . . ? Er2 C3 H3A 125.7 . . ? C3 C4 C5 120.6(7) . . ? C3 C4 Er1 76.0(5) . . ? C5 C4 Er1 79.2(5) . . ? C3 C4 Er2 72.0(5) . . ? C5 C4 Er2 67.6(4) . . ? Er1 C4 Er2 110.1(3) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? Er1 C4 H4A 115.7 . . ? Er2 C4 H4A 134.2 . . ? C4 C5 C6 118.1(7) . . ? C4 C5 Er2 78.2(5) . . ? C6 C5 Er2 76.6(4) . . ? C4 C5 Er1 66.9(4) . . ? C6 C5 Er1 70.0(4) . . ? Er2 C5 Er1 109.3(3) . . ? C4 C5 H5A 120.9 . . ? C6 C5 H5A 120.9 . . ? Er2 C5 H5A 115.1 . . ? Er1 C5 H5A 135.5 . . ? C7 C6 C1 121.7(7) . . ? C7 C6 C5 121.0(7) . . ? C1 C6 C5 117.3(7) . . ? C7 C6 Er1 126.3(6) . . ? C1 C6 Er1 69.0(4) . . ? C5 C6 Er1 76.5(4) . . ? C7 C6 Er2 125.0(6) . . ? C1 C6 Er2 75.1(4) . . ? C5 C6 Er2 68.7(4) . . ? Er1 C6 Er2 108.7(3) . . ? C6 C7 C8 123.5(9) . . ? C6 C7 C12 122.0(8) . . ? C8 C7 C12 114.6(8) . . ? C6 C7 K1 114.8(6) . . ? C8 C7 K1 72.6(6) . . ? C12 C7 K1 80.4(6) . . ? C6 C7 K2 113.2(6) . . ? C8 C7 K2 84.8(6) . . ? C12 C7 K2 71.2(5) . . ? K1 C7 K2 131.9(3) . . ? C9 C8 C7 122.2(11) . . ? C9 C8 K1 77.9(7) . . ? C7 C8 K1 80.8(6) . . ? C9 C8 K2 82.6(8) . . ? C7 C8 K2 70.8(6) . . ? K1 C8 K2 129.0(4) . . ? C9 C8 H8A 118.9 . . ? C7 C8 H8A 118.9 . . ? K1 C8 H8A 112.5 . . ? K2 C8 H8A 118.3 . . ? C8 C9 C10 122.1(12) . . ? C8 C9 K1 75.8(7) . . ? C10 C9 K1 82.3(8) . . ? C8 C9 K2 74.5(8) . . ? C10 C9 K2 75.6(9) . . ? K1 C9 K2 124.4(4) . . ? C8 C9 H9A 118.9 . . ? C10 C9 H9A 118.9 . . ? K1 C9 H9A 113.1 . . ? K2 C9 H9A 122.2 . . ? C9 C10 C11 117.4(11) . . ? C9 C10 K1 72.2(8) . . ? C11 C10 K1 79.7(8) . . ? C9 C10 K2 81.5(8) . . ? C11 C10 K2 68.9(7) . . ? K1 C10 K2 122.8(4) . . ? C9 C10 H10A 121.3 . . ? C11 C10 H10A 121.3 . . ? K1 C10 H10A 117.8 . . ? K2 C10 H10A 119.2 . . ? C12 C11 C10 122.0(12) . . ? C12 C11 K2 72.4(6) . . ? C10 C11 K2 87.3(8) . . ? C12 C11 K1 77.2(7) . . ? C10 C11 K1 75.2(8) . . ? K2 C11 K1 128.8(4) . . ? C12 C11 H11A 119.0 . . ? C10 C11 H11A 119.0 . . ? K2 C11 H11A 111.2 . . ? K1 C11 H11A 119.5 . . ? C11 C12 C7 121.7(10) . . ? C11 C12 K2 82.5(7) . . ? C7 C12 K2 82.6(5) . . ? C11 C12 K1 78.2(8) . . ? C7 C12 K1 73.4(6) . . ? K2 C12 K1 134.2(4) . . ? C11 C12 H12A 119.1 . . ? C7 C12 H12A 119.1 . . ? K2 C12 H12A 105.4 . . ? K1 C12 H12A 120.3 . . ? N1 C13 C17 124.5(8) . . ? N1 C13 C14 129.7(9) . . ? C17 C13 C14 105.8(9) . . ? N1 C13 Fe1 128.0(7) . . ? C17 C13 Fe1 68.1(6) . . ? C14 C13 Fe1 66.7(7) . . ? N1 C13 Er1 54.0(4) . . ? C17 C13 Er1 86.5(6) . . ? C14 C13 Er1 136.3(8) . . ? Fe1 C13 Er1 80.4(3) . . ? C15 C14 C13 108.9(10) . . ? C15 C14 Fe1 68.8(7) . . ? C13 C14 Fe1 72.6(6) . . ? C15 C14 H14A 125.5 . . ? C13 C14 H14A 125.5 . . ? Fe1 C14 H14A 124.7 . . ? C16 C15 C14 108.2(10) . . ? C16 C15 Fe1 69.1(7) . . ? C14 C15 Fe1 70.7(7) . . ? C16 C15 H15A 125.9 . . ? C14 C15 H15A 125.9 . . ? Fe1 C15 H15A 125.9 . . ? C15 C16 C17 108.4(11) . . ? C15 C16 Fe1 69.9(7) . . ? C17 C16 Fe1 72.0(7) . . ? C15 C16 H16A 125.8 . . ? C17 C16 H16A 125.8 . . ? Fe1 C16 H16A 124.0 . . ? C16 C17 C13 108.5(9) . . ? C16 C17 Fe1 67.2(7) . . ? C13 C17 Fe1 71.9(6) . . ? C16 C17 H17A 125.7 . . ? C13 C17 H17A 125.7 . . ? Fe1 C17 H17A 126.7 . . ? N2 C18 C19 131.4(11) . . ? N2 C18 C22 123.1(9) . . ? C19 C18 C22 105.5(10) . . ? N2 C18 Fe1 130.0(8) . . ? C19 C18 Fe1 67.4(7) . . ? C22 C18 Fe1 67.0(6) . . ? N2 C18 Er1 55.5(5) . . ? C19 C18 Er1 137.2(8) . . ? C22 C18 Er1 85.1(6) . . ? Fe1 C18 Er1 80.0(3) . . ? N2 C18 K1 71.3(6) . . ? C19 C18 K1 125.8(8) . . ? C22 C18 K1 75.5(6) . . ? Fe1 C18 K1 142.5(5) . . ? Er1 C18 K1 97.0(3) . . ? C18 C19 C20 108.2(10) . . ? C18 C19 Fe1 72.4(7) . . ? C20 C19 Fe1 67.8(7) . . ? C18 C19 H19A 125.9 . . ? C20 C19 H19A 125.9 . . ? Fe1 C19 H19A 125.4 . . ? C21 C20 C19 108.9(10) . . ? C21 C20 Fe1 69.8(7) . . ? C19 C20 Fe1 70.6(7) . . ? C21 C20 H20A 125.6 . . ? C19 C20 H20A 125.6 . . ? Fe1 C20 H20A 125.7 . . ? C20 C21 C22 108.5(11) . . ? C20 C21 Fe1 69.8(7) . . ? C22 C21 Fe1 71.1(7) . . ? C20 C21 H21A 125.8 . . ? C22 C21 H21A 125.8 . . ? Fe1 C21 H21A 125.0 . . ? C21 C22 C18 109.0(9) . . ? C21 C22 Fe1 68.3(6) . . ? C18 C22 Fe1 71.9(6) . . ? C21 C22 K1 124.3(8) . . ? C18 C22 K1 76.1(6) . . ? Fe1 C22 K1 148.0(5) . . ? C21 C22 H22A 125.5 . . ? C18 C22 H22A 125.5 . . ? Fe1 C22 H22A 125.8 . . ? K1 C22 H22A 73.9 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C28 108.5(13) . . ? C26 C25 C27 108.2(11) . . ? C28 C25 C27 108.3(14) . . ? C26 C25 Si1 111.7(11) . . ? C28 C25 Si1 110.3(9) . . ? C27 C25 Si1 109.7(10) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C34 109.1(16) . . ? C33 C31 C32 116.5(15) . . ? C34 C31 C32 109.3(15) . . ? C33 C31 Si2 109.9(13) . . ? C34 C31 Si2 108.2(13) . . ? C32 C31 Si2 103.5(12) . . ? C31 C32 K1 116.0(11) . . ? C31 C32 H32A 109.5 . . ? K1 C32 H32A 48.7 . . ? C31 C32 H32B 109.5 . . ? K1 C32 H32B 61.8 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? K1 C32 H32C 133.9 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 C36 123.3(10) . . ? N3 C35 C39 129.7(12) . . ? C36 C35 C39 106.9(10) . . ? N3 C35 Fe2 128.0(7) . . ? C36 C35 Fe2 68.1(6) . . ? C39 C35 Fe2 67.9(7) . . ? N3 C35 Er2 52.0(5) . . ? C36 C35 Er2 89.6(6) . . ? C39 C35 Er2 134.2(8) . . ? Fe2 C35 Er2 80.3(3) . . ? C37 C36 C35 106.4(11) . . ? C37 C36 Fe2 67.4(7) . . ? C35 C36 Fe2 71.8(7) . . ? C37 C36 H36A 126.8 . . ? C35 C36 H36A 126.8 . . ? Fe2 C36 H36A 125.6 . . ? C38 C37 C36 109.8(12) . . ? C38 C37 Fe2 70.7(8) . . ? C36 C37 Fe2 71.5(7) . . ? C38 C37 H37A 125.1 . . ? C36 C37 H37A 125.1 . . ? Fe2 C37 H37A 124.2 . . ? C37 C38 C39 109.7(12) . . ? C37 C38 Fe2 70.0(8) . . ? C39 C38 Fe2 71.5(7) . . ? C37 C38 H38A 125.2 . . ? C39 C38 H38A 125.2 . . ? Fe2 C38 H38A 124.9 . . ? C38 C39 C35 107.1(13) . . ? C38 C39 Fe2 68.1(8) . . ? C35 C39 Fe2 71.7(7) . . ? C38 C39 H39A 126.4 . . ? C35 C39 H39A 126.4 . . ? Fe2 C39 H39A 125.3 . . ? N4A C40 C41 114.6(13) . . ? N4A C40 C44 138.7(14) . . ? C41 C40 C44 105.2(9) . . ? C41 C40 N4 128.4(10) . . ? C44 C40 N4 126.0(11) . . ? N4A C40 Fe2 138.4(11) . . ? C41 C40 Fe2 67.3(6) . . ? C44 C40 Fe2 67.3(6) . . ? N4 C40 Fe2 124.2(8) . . ? N4A C40 Er2 59.2(10) . . ? C41 C40 Er2 83.7(6) . . ? C44 C40 Er2 139.2(7) . . ? N4 C40 Er2 54.7(7) . . ? Fe2 C40 Er2 80.7(3) . . ? C41 C40 K2 86.2(6) . . ? C44 C40 K2 123.5(7) . . ? N4 C40 K2 71.6(7) . . ? Fe2 C40 K2 153.5(5) . . ? Er2 C40 K2 96.4(3) . . ? C40 C41 C42 110.6(9) . . ? C40 C41 Fe2 72.4(6) . . ? C42 C41 Fe2 68.6(6) . . ? C40 C41 K2 67.8(5) . . ? C42 C41 K2 126.8(7) . . ? Fe2 C41 K2 140.2(5) . . ? C40 C41 H41A 124.7 . . ? C42 C41 H41A 124.7 . . ? Fe2 C41 H41A 125.9 . . ? K2 C41 H41A 78.8 . . ? C43 C42 C41 106.5(11) . . ? C43 C42 Fe2 69.6(7) . . ? C41 C42 Fe2 69.8(6) . . ? C43 C42 H42A 126.8 . . ? C41 C42 H42A 126.8 . . ? Fe2 C42 H42A 125.5 . . ? C42 C43 C44 109.0(10) . . ? C42 C43 Fe2 69.5(7) . . ? C44 C43 Fe2 70.3(6) . . ? C42 C43 H43A 125.5 . . ? C44 C43 H43A 125.5 . . ? Fe2 C43 H43A 126.3 . . ? C43 C44 C40 108.6(10) . . ? C43 C44 Fe2 68.4(7) . . ? C40 C44 Fe2 71.7(6) . . ? C43 C44 H44A 125.7 . . ? C40 C44 H44A 125.7 . . ? Fe2 C44 H44A 125.7 . . ? C62 O2 C63 111(3) . . ? C62 O2 K2 110(2) . . ? C63 O2 K2 136.5(17) . . ? O2 C62 C64 113(3) . . ? O2 C62 K2 47.9(15) . . ? C64 C62 K2 157(3) . . ? O2 C62 H62A 109.0 . . ? C64 C62 H62A 109.0 . . ? K2 C62 H62A 91.3 . . ? O2 C62 H62B 109.0 . . ? C64 C62 H62B 109.0 . . ? K2 C62 H62B 73.1 . . ? H62A C62 H62B 107.8 . . ? O2 C63 C65 101(3) . . ? O2 C63 H63A 111.6 . . ? C65 C63 H63A 111.6 . . ? O2 C63 H63B 111.6 . . ? C65 C63 H63B 111.6 . . ? H63A C63 H63B 109.4 . . ? C62 C64 C65 96(3) . . ? C62 C64 H64A 112.6 . . ? C65 C64 H64A 112.6 . . ? C62 C64 H64B 112.6 . . ? C65 C64 H64B 112.6 . . ? H64A C64 H64B 110.1 . . ? C64 C65 C63 112(3) . . ? C64 C65 H65A 109.1 . . ? C63 C65 H65A 109.1 . . ? C64 C65 H65B 109.1 . . ? C63 C65 H65B 109.1 . . ? H65A C65 H65B 107.8 . . ? C62A O2A C63A 100.5(14) . . ? C62A C61A H61A 109.5 . . ? C62A C61A H61B 109.5 . . ? H61A C61A H61B 109.5 . . ? C62A C61A H61C 109.5 . . ? H61A C61A H61C 109.5 . . ? H61B C61A H61C 109.5 . . ? O2A C62A C61A 103.3(15) . . ? O2A C62A H62C 111.1 . . ? C61A C62A H62C 111.1 . . ? O2A C62A H62D 111.1 . . ? C61A C62A H62D 111.1 . . ? H62C C62A H62D 109.1 . . ? O2A C63A C64A 105.6(16) . . ? O2A C63A H63C 110.6 . . ? C64A C63A H63C 110.6 . . ? O2A C63A H63D 110.6 . . ? C64A C63A H63D 110.6 . . ? H63C C63A H63D 108.7 . . ? C63A C64A H64C 109.5 . . ? C63A C64A H64D 109.5 . . ? H64C C64A H64D 109.5 . . ? C63A C64A H64E 109.5 . . ? H64C C64A H64E 109.5 . . ? H64D C64A H64E 109.5 . . ? N3 Si3 C45 108.9(5) . . ? N3 Si3 C46 113.7(11) . . ? C45 Si3 C46 115.8(12) . . ? N3 Si3 C47 112.3(5) . . ? C45 Si3 C47 108.7(6) . . ? C46 Si3 C47 96.9(11) . . ? N3 Si3 C46A 111.9(12) . . ? C45 Si3 C46A 99.7(11) . . ? C47 Si3 C46A 114.5(11) . . ? C35 N3 Si3 121.3(7) . . ? C35 N3 Er2 98.8(6) . . ? Si3 N3 Er2 139.9(5) . . ? Si3 C45 H45A 109.5 . . ? Si3 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si3 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C48A C47 C49 117.4(15) . . ? C49 C47 C50 116.8(14) . . ? C48A C47 C50A 113.7(19) . . ? C49 C47 C50A 100.8(10) . . ? C49 C47 C48 95.8(10) . . ? C50 C47 C48 97.2(12) . . ? C48A C47 Si3 110.4(13) . . ? C49 C47 Si3 112.8(10) . . ? C50 C47 Si3 119.9(12) . . ? C50A C47 Si3 100.0(13) . . ? C48 C47 Si3 109.6(11) . . ? Si3 C46 H46A 109.5 . . ? Si3 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si3 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si3 C46A H46D 109.5 . . ? Si3 C46A H46E 109.5 . . ? H46D C46A H46E 109.5 . . ? Si3 C46A H46F 109.5 . . ? H46D C46A H46F 109.5 . . ? H46E C46A H46F 109.5 . . ? C47 C48A H48D 109.5 . . ? C47 C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? C47 C48A H48F 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? C47 C50A H50D 109.5 . . ? C47 C50A H50E 109.5 . . ? H50D C50A H50E 109.5 . . ? C47 C50A H50F 109.5 . . ? H50D C50A H50F 109.5 . . ? H50E C50A H50F 109.5 . . ? N4 Si4 C53 107.7(7) . . ? N4 Si4 C52 110.7(8) . . ? C53 Si4 C52 107.2(8) . . ? N4 Si4 C51 114.7(10) . . ? C53 Si4 C51 107.9(10) . . ? C52 Si4 C51 108.3(10) . . ? N4 Si4 K2 48.1(5) . . ? C53 Si4 K2 94.2(5) . . ? C52 Si4 K2 71.5(6) . . ? C51 Si4 K2 156.4(8) . . ? C40 N4 Si4 119.2(10) . . ? C40 N4 Er2 94.1(8) . . ? Si4 N4 Er2 132.9(8) . . ? C40 N4 K2 79.7(7) . . ? Si4 N4 K2 105.8(7) . . ? Er2 N4 K2 112.7(6) . . ? Si4 C51 H51A 109.5 . . ? Si4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si4 C52 H52A 109.5 . . ? Si4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C55 108.3(12) . . ? C54 C53 C56 107.1(13) . . ? C55 C53 C56 110.7(15) . . ? C54 C53 Si4 110.5(10) . . ? C55 C53 Si4 110.4(10) . . ? C56 C53 Si4 109.8(11) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N4A Si4A C53A 114.9(11) . . ? N4A Si4A C52A 112.5(14) . . ? C53A Si4A C52A 108.1(15) . . ? N4A Si4A C51A 106.7(12) . . ? C53A Si4A C51A 108.0(13) . . ? C52A Si4A C51A 106.2(14) . . ? C40 N4A Si4A 123.9(16) . . ? C40 N4A Er2 92.1(12) . . ? Si4A N4A Er2 133.0(13) . . ? Si4A C51A H51D 109.5 . . ? Si4A C51A H51E 109.5 . . ? H51D C51A H51E 109.5 . . ? Si4A C51A H51F 109.5 . . ? H51D C51A H51F 109.5 . . ? H51E C51A H51F 109.5 . . ? Si4A C52A H52D 109.5 . . ? Si4A C52A H52E 109.5 . . ? H52D C52A H52E 109.5 . . ? Si4A C52A H52F 109.5 . . ? H52D C52A H52F 109.5 . . ? H52E C52A H52F 109.5 . . ? C56A C53A C55A 111(3) . . ? C56A C53A C54A 108(3) . . ? C55A C53A C54A 107(2) . . ? C56A C53A Si4A 108(2) . . ? C55A C53A Si4A 108(2) . . ? C54A C53A Si4A 114(2) . . ? C53A C54A H54D 109.5 . . ? C53A C54A H54E 109.5 . . ? H54D C54A H54E 109.5 . . ? C53A C54A H54F 109.5 . . ? H54D C54A H54F 109.5 . . ? H54E C54A H54F 109.5 . . ? C53A C55A H55D 109.5 . . ? C53A C55A H55E 109.5 . . ? H55D C55A H55E 109.5 . . ? C53A C55A H55F 109.5 . . ? H55D C55A H55F 109.5 . . ? H55E C55A H55F 109.5 . . ? C53A C56A H56D 109.5 . . ? C53A C56A H56E 109.5 . . ? H56D C56A H56E 109.5 . . ? C53A C56A H56F 109.5 . . ? H56D C56A H56F 109.5 . . ? H56E C56A H56F 109.5 . . ? C59 O1 C58 111.7(13) . . ? C59 O1 K1 124.6(9) . . ? C58 O1 K1 123.0(8) . . ? C58 C57 K1 84.5(8) . . ? C58 C57 H57A 109.5 . . ? K1 C57 H57A 163.4 . . ? C58 C57 H57B 109.5 . . ? K1 C57 H57B 55.8 . . ? H57A C57 H57B 109.5 . . ? C58 C57 H57C 109.5 . . ? K1 C57 H57C 72.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O1 C58 C57 109.1(11) . . ? O1 C58 H58A 109.9 . . ? C57 C58 H58A 109.9 . . ? O1 C58 H58B 109.9 . . ? C57 C58 H58B 109.9 . . ? H58A C58 H58B 108.3 . . ? O1 C59 C60 109.4(13) . . ? O1 C59 H59A 109.8 . . ? C60 C59 H59A 109.8 . . ? O1 C59 H59B 109.8 . . ? C60 C59 H59B 109.8 . . ? H59A C59 H59B 108.2 . . ? C59 C60 K1 84.1(9) . . ? C59 C60 H60A 109.5 . . ? K1 C60 H60A 165.8 . . ? C59 C60 H60B 109.5 . . ? K1 C60 H60B 68.2 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? K1 C60 H60C 60.4 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C2S O1S C3S 116(3) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O1S C2S C1S 108.8(17) . . ? O1S C2S H2S1 109.9 . . ? C1S C2S H2S1 109.9 . . ? O1S C2S H2S2 109.9 . . ? C1S C2S H2S2 109.9 . . ? H2S1 C2S H2S2 108.3 . . ? O1S C3S C4S 102.7(16) . . ? O1S C3S H3S1 111.2 . . ? C4S C3S H3S1 111.2 . . ? O1S C3S H3S2 111.3 . . ? C4S C3S H3S2 111.2 . . ? H3S1 C3S H3S2 109.2 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? _refine_diff_density_max 4.419 _refine_diff_density_min -2.427 _refine_diff_density_rms 0.195 _shelxl_version_number 2013-4 _shelx_res_file ; TITL pld1366sm in P2(1)/n CELL 0.71073 15.0037 22.7939 23.3759 90.000 97.019 90.000 ZERR 2.00 0.00190 0.00290 0.00300 0.0000 0.0015 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O Si K Fe Er UNIT 264 440 16 10 16 8 8 8 L.S. 15 BOND $H ACTA FMAP 2 PLAN 5 SIZE 0.11 0.18 0.27 TEMP -173.000 conn k1 1 conn k2 1 conn k2a 1 bump rigu sadi si4 c51 si4 c52 si4 c53 si3 c45 si3 c46 si3 c47 si3 c46a sadi c53 c54 c53 c55 c53 c56 c47 c48 c47 c49 c47 c50 c47 c48a c47 c50a sadi si4A c51a si4a c52a si4a c53a sadi c53a c54a c53a c55a c53a c56a sadi c57 c58 c59 c60 sadi o1 c58 o1 c59 o2 c62 o2 c63 o2a c62a o2a c63a o1s c2s o1s c3s sadi o1 c57 o1 c60 o2a c61a o2a c64a o1s c1s o1s c4s dfix 1.55 c61a c62a c63a c64a c1s c2s c3s c4s isor .01 eadp c50a c50 dfix 1.55 c63 c65 c65 c64 c64 c62 WGHT 0.035800 131.447189 FVAR 0.15476 0.58627 0.50914 ER1 8 0.447038 0.797170 0.631195 11.00000 0.01579 0.03344 = 0.03118 0.00373 0.00430 -0.00380 ER2 8 0.718982 0.777266 0.621616 11.00000 0.01732 0.01931 = 0.03095 0.00272 0.00450 0.00169 FE1 7 0.281317 0.883960 0.590501 11.00000 0.01867 0.05251 = 0.05703 0.01171 0.00430 0.00369 FE2 7 0.903563 0.731849 0.693921 11.00000 0.03342 0.02899 = 0.05688 0.00042 -0.01023 0.01308 SI1 5 0.302408 0.683240 0.546242 11.00000 0.04206 0.04162 = 0.06207 0.01301 -0.01856 -0.02248 SI2 5 0.315235 0.785029 0.754235 11.00000 0.08298 0.11338 = 0.07717 0.02717 0.05476 0.02842 N1 3 0.336548 0.751095 0.571423 11.00000 0.02382 0.04165 = 0.04752 0.00996 -0.00468 -0.00881 N2 3 0.373174 0.828020 0.708665 11.00000 0.04020 0.06892 = 0.04410 0.00350 0.01486 0.01384 C1 1 0.579683 0.845977 0.603040 11.00000 0.01666 0.02013 = 0.03005 -0.00155 -0.00195 -0.00451 AFIX 43 H1A 2 0.570169 0.884387 0.587730 11.00000 -1.20000 AFIX 0 C2 1 0.572703 0.795472 0.564612 11.00000 0.01649 0.02536 = 0.02546 0.00066 0.00451 -0.00239 AFIX 43 H2A 2 0.574420 0.800904 0.524468 11.00000 -1.20000 AFIX 0 C3 1 0.563320 0.738010 0.586920 11.00000 0.02723 0.02509 = 0.02902 0.00006 0.00193 -0.00461 AFIX 43 H3A 2 0.550179 0.706043 0.561194 11.00000 -1.20000 AFIX 0 C4 1 0.573455 0.728083 0.647384 11.00000 0.02644 0.02067 = 0.03008 0.00449 -0.00015 -0.00360 AFIX 43 H4A 2 0.559696 0.690633 0.661838 11.00000 -1.20000 AFIX 0 C5 1 0.605466 0.775871 0.688332 11.00000 0.02335 0.02509 = 0.02664 0.00142 0.00094 -0.00110 AFIX 43 H5A 2 0.627601 0.767380 0.727273 11.00000 -1.20000 AFIX 0 C6 1 0.601777 0.837399 0.666461 11.00000 0.01814 0.02118 = 0.02514 -0.00293 0.00224 -0.00115 C7 1 0.621177 0.885651 0.704647 11.00000 0.02634 0.02981 = 0.03920 -0.01070 -0.00313 0.00331 C8 1 0.651750 0.879136 0.764539 11.00000 0.04470 0.04431 = 0.03938 -0.01319 -0.00570 0.00826 AFIX 43 H8A 2 0.661664 0.840778 0.779902 11.00000 -1.20000 AFIX 0 C9 1 0.667465 0.926919 0.801048 11.00000 0.06537 0.05618 = 0.05554 -0.02242 -0.01128 0.00872 AFIX 43 H9A 2 0.687489 0.920232 0.840650 11.00000 -1.20000 AFIX 0 C10 1 0.654911 0.984177 0.781651 11.00000 0.06722 0.05169 = 0.06543 -0.02500 -0.00819 0.00686 AFIX 43 H10A 2 0.665937 1.016544 0.807136 11.00000 -1.20000 AFIX 0 C11 1 0.625380 0.992408 0.723101 11.00000 0.05664 0.04127 = 0.06714 -0.02111 -0.00459 0.01001 AFIX 43 H11A 2 0.615779 1.031203 0.708815 11.00000 -1.20000 AFIX 0 C12 1 0.609744 0.945751 0.685392 11.00000 0.03382 0.03191 = 0.05255 -0.00893 -0.00326 0.00656 AFIX 43 H12A 2 0.590999 0.953396 0.645797 11.00000 -1.20000 AFIX 0 C13 1 0.294476 0.802670 0.548449 11.00000 0.02596 0.04376 = 0.03883 0.01120 -0.00316 -0.00610 C14 1 0.202227 0.821550 0.547288 11.00000 0.03337 0.06065 = 0.06268 0.00613 -0.00280 0.00119 AFIX 43 H14A 2 0.156194 0.800465 0.562886 11.00000 -1.20000 AFIX 0 C15 1 0.191752 0.876128 0.519347 11.00000 0.04049 0.06327 = 0.06331 0.00618 -0.00452 0.00774 AFIX 43 H15A 2 0.137179 0.897407 0.511534 11.00000 -1.20000 AFIX 0 C16 1 0.276045 0.893833 0.504934 11.00000 0.04212 0.05063 = 0.05851 0.01013 -0.00169 0.00897 AFIX 43 H16A 2 0.288416 0.929643 0.486663 11.00000 -1.20000 AFIX 0 C17 1 0.339542 0.849057 0.522346 11.00000 0.03301 0.03748 = 0.04799 0.01156 0.00032 0.00115 AFIX 43 H17A 2 0.401474 0.849796 0.517476 11.00000 -1.20000 AFIX 0 C18 1 0.328652 0.874617 0.679276 11.00000 0.03065 0.05888 = 0.05152 0.00091 0.01199 0.00592 C19 1 0.235235 0.889560 0.669529 11.00000 0.03450 0.05960 = 0.06345 0.00366 0.01326 0.00531 AFIX 43 H19A 2 0.187300 0.867205 0.681389 11.00000 -1.20000 AFIX 0 C20 1 0.226589 0.944593 0.638495 11.00000 0.02903 0.05422 = 0.06686 0.00176 0.00556 0.00266 AFIX 43 H20A 2 0.171989 0.965046 0.627573 11.00000 -1.20000 AFIX 0 C21 1 0.311493 0.962700 0.627240 11.00000 0.03221 0.05648 = 0.06141 -0.00092 0.00590 0.00151 AFIX 43 H21A 2 0.324313 0.997222 0.606991 11.00000 -1.20000 AFIX 0 C22 1 0.375221 0.921044 0.651030 11.00000 0.02916 0.05581 = 0.05063 -0.00241 0.00629 0.00024 AFIX 43 H22A 2 0.438039 0.922778 0.649075 11.00000 -1.20000 AFIX 0 C23 1 0.180856 0.666701 0.551791 11.00000 0.04772 0.07184 = 0.09153 0.01723 -0.01467 -0.03193 AFIX 137 H23A 2 0.170556 0.667171 0.592388 11.00000 -1.50000 H23B 2 0.165753 0.627890 0.535350 11.00000 -1.50000 H23C 2 0.142973 0.696433 0.530525 11.00000 -1.50000 AFIX 0 C24 1 0.371905 0.627764 0.590404 11.00000 0.05642 0.04239 = 0.06043 0.01005 -0.01547 -0.02180 AFIX 137 H24A 2 0.367923 0.634765 0.631377 11.00000 -1.50000 H24B 2 0.434621 0.631118 0.583047 11.00000 -1.50000 H24C 2 0.349634 0.588303 0.579957 11.00000 -1.50000 AFIX 0 C25 1 0.318596 0.673543 0.466709 11.00000 0.06714 0.05550 = 0.06025 0.00213 -0.01594 -0.01775 C26 1 0.251084 0.708795 0.427614 11.00000 0.09046 0.07518 = 0.07307 0.00555 -0.02683 -0.01073 AFIX 137 H26A 2 0.251293 0.695650 0.387715 11.00000 -1.50000 H26B 2 0.267064 0.750467 0.430530 11.00000 -1.50000 H26C 2 0.191085 0.703144 0.439228 11.00000 -1.50000 AFIX 0 C27 1 0.307462 0.609066 0.449940 11.00000 0.09836 0.06533 = 0.08438 -0.00593 -0.02071 -0.01751 AFIX 137 H27A 2 0.303309 0.605309 0.407935 11.00000 -1.50000 H27B 2 0.252567 0.593679 0.463229 11.00000 -1.50000 H27C 2 0.359354 0.586775 0.467879 11.00000 -1.50000 AFIX 0 C28 1 0.412268 0.692813 0.456644 11.00000 0.08481 0.08516 = 0.05566 -0.01053 -0.00942 -0.02793 AFIX 137 H28A 2 0.419234 0.688476 0.415717 11.00000 -1.50000 H28B 2 0.456877 0.668413 0.479736 11.00000 -1.50000 H28C 2 0.421165 0.733992 0.467979 11.00000 -1.50000 AFIX 0 C29 1 0.228271 0.732073 0.710879 11.00000 0.07539 0.10323 = 0.08754 0.01257 0.04677 -0.00783 AFIX 137 H29A 2 0.188180 0.715683 0.736887 11.00000 -1.50000 H29B 2 0.260416 0.700153 0.694179 11.00000 -1.50000 H29C 2 0.192858 0.753982 0.679953 11.00000 -1.50000 AFIX 0 C30 1 0.254390 0.834319 0.801937 11.00000 0.08340 0.12650 = 0.07422 0.00923 0.04334 0.02869 AFIX 137 H30A 2 0.228203 0.810423 0.830483 11.00000 -1.50000 H30B 2 0.206555 0.855613 0.778238 11.00000 -1.50000 H30C 2 0.296932 0.862423 0.821770 11.00000 -1.50000 AFIX 0 C31 1 0.396526 0.735749 0.800169 11.00000 0.09002 0.09850 = 0.08114 0.01380 0.03294 0.00861 C32 1 0.469457 0.779985 0.829816 11.00000 0.09015 0.10547 = 0.08108 0.00555 0.03317 0.00897 AFIX 33 H32A 2 0.439684 0.815672 0.841151 11.00000 -1.50000 H32B 2 0.511780 0.790098 0.802584 11.00000 -1.50000 H32C 2 0.502030 0.761553 0.864057 11.00000 -1.50000 AFIX 0 C33 1 0.430592 0.687425 0.762777 11.00000 0.11012 0.09443 = 0.09754 0.01611 0.05283 0.00722 AFIX 137 H33A 2 0.464465 0.658381 0.787568 11.00000 -1.50000 H33B 2 0.469713 0.704714 0.736652 11.00000 -1.50000 H33C 2 0.379385 0.668270 0.740196 11.00000 -1.50000 AFIX 0 C34 1 0.345765 0.707124 0.847081 11.00000 0.12659 0.12729 = 0.10127 0.02732 0.05665 0.00178 AFIX 137 H34A 2 0.383899 0.677106 0.867698 11.00000 -1.50000 H34B 2 0.290271 0.688960 0.828798 11.00000 -1.50000 H34C 2 0.331099 0.737247 0.874348 11.00000 -1.50000 AFIX 0 C35 1 0.839613 0.681527 0.624997 11.00000 0.03807 0.03565 = 0.05529 -0.00954 -0.00334 0.01176 C36 1 0.812909 0.663953 0.679168 11.00000 0.05258 0.03483 = 0.05778 -0.00095 -0.00821 0.00514 AFIX 43 H36A 2 0.753605 0.663666 0.689494 11.00000 -1.20000 AFIX 0 C37 1 0.893085 0.646926 0.714648 11.00000 0.06788 0.03820 = 0.07599 0.00207 -0.01595 0.00574 AFIX 43 H37A 2 0.895686 0.632682 0.753009 11.00000 -1.20000 AFIX 0 C38 1 0.964666 0.654137 0.685415 11.00000 0.06098 0.04775 = 0.08639 -0.00624 -0.01486 0.01722 AFIX 43 H38A 2 1.025122 0.645487 0.700019 11.00000 -1.20000 AFIX 0 C39 1 0.936044 0.676407 0.630046 11.00000 0.04668 0.05674 = 0.07696 -0.01111 -0.00529 0.01914 AFIX 43 H39A 2 0.973275 0.686222 0.601383 11.00000 -1.20000 AFIX 0 C40 1 0.884490 0.821322 0.674667 11.00000 0.02815 0.03035 = 0.05118 0.00205 -0.00407 0.00022 C41 1 0.850316 0.804739 0.726574 11.00000 0.03176 0.03255 = 0.04955 -0.00364 -0.00240 0.00015 AFIX 43 H41A 2 0.789690 0.809446 0.733608 11.00000 -1.20000 AFIX 0 C42 1 0.920347 0.779877 0.766864 11.00000 0.04496 0.04992 = 0.05458 -0.00079 -0.00568 0.00247 AFIX 43 H42A 2 0.914611 0.765623 0.804429 11.00000 -1.20000 AFIX 0 C43 1 0.999036 0.780827 0.739670 11.00000 0.03683 0.05126 = 0.05910 -0.00106 -0.00958 0.00577 AFIX 43 H43A 2 1.056512 0.767650 0.756258 11.00000 -1.20000 AFIX 0 C44 1 0.978530 0.804836 0.683019 11.00000 0.03028 0.04902 = 0.05831 0.00286 -0.00514 0.00344 AFIX 43 H44A 2 1.019665 0.809238 0.655479 11.00000 -1.20000 AFIX 0 part 1 K2 6 0.818092 0.942777 0.697220 10.50000 0.04028 0.02547 = 0.03535 -0.00152 0.00599 -0.00497 O2 4 0.851032 1.056503 0.666212 10.50000 0.06531 0.03698 = 0.06061 -0.00340 0.00312 -0.00910 C62 1 0.813259 1.095397 0.701944 10.50000 0.14590 AFIX 23 H62A 2 0.849795 1.095619 0.740192 10.50000 -1.20000 H62B 2 0.752274 1.081592 0.707316 10.50000 -1.20000 AFIX 0 C63 1 0.910660 1.084725 0.634348 10.50000 0.09029 AFIX 23 H63A 2 0.907012 1.068929 0.594679 10.50000 -1.20000 H63B 2 0.973288 1.081733 0.653169 10.50000 -1.20000 AFIX 0 C64 1 0.806996 1.157769 0.678304 10.50000 0.11062 AFIX 23 H64A 2 0.826949 1.187498 0.708006 10.50000 -1.20000 H64B 2 0.746160 1.167513 0.659341 10.50000 -1.20000 AFIX 0 C65 1 0.875238 1.148875 0.634792 10.50000 0.16540 AFIX 23 H65A 2 0.926614 1.175804 0.644569 10.50000 -1.20000 H65B 2 0.846412 1.159152 0.595707 10.50000 -1.20000 AFIX 0 part 2 K2A 6 0.809230 0.933269 0.732755 10.50000 0.04339 0.04007 = 0.13269 -0.03631 -0.01603 -0.00119 O2A 4 0.940993 0.990380 0.791307 10.50000 0.05255 0.08922 = 0.08418 0.01360 0.00490 -0.01962 C61A 1 1.021333 0.908854 0.826693 10.50000 0.07443 0.08737 = 0.11419 -0.01195 -0.01046 -0.00919 AFIX 33 H61A 2 1.063360 0.893028 0.858321 10.50000 -1.50000 H61B 2 1.047671 0.905557 0.790474 10.50000 -1.50000 H61C 2 0.965039 0.886631 0.823684 10.50000 -1.50000 AFIX 0 C62A 1 1.002281 0.974116 0.838691 10.50000 0.09259 0.09035 = 0.09666 -0.00233 -0.00463 -0.00593 AFIX 23 H62C 2 0.975807 0.978695 0.875206 10.50000 -1.20000 H62D 2 1.057855 0.997828 0.840662 10.50000 -1.20000 AFIX 0 C63A 1 0.933911 1.051296 0.801538 10.50000 0.08213 0.09045 = 0.09080 0.00133 0.00529 -0.01299 AFIX 23 H63C 2 0.993003 1.070652 0.801660 10.50000 -1.20000 H63D 2 0.911774 1.058459 0.839121 10.50000 -1.20000 AFIX 0 C64A 1 0.866705 1.074733 0.751923 10.50000 0.09480 0.09206 = 0.09916 -0.00284 0.00239 -0.00639 AFIX 33 H64C 2 0.859318 1.117129 0.756476 10.50000 -1.50000 H64D 2 0.808632 1.055220 0.752562 10.50000 -1.50000 H64E 2 0.889305 1.066795 0.715090 10.50000 -1.50000 AFIX 0 part 0 SI3 5 0.768246 0.664597 0.513715 11.00000 0.05116 0.06408 = 0.05064 -0.02304 0.00911 0.02119 N3 3 0.779071 0.700661 0.578568 11.00000 0.03772 0.04137 = 0.04908 -0.01231 0.00341 0.01363 C45 1 0.687031 0.705430 0.461382 11.00000 0.05696 0.05948 = 0.04166 -0.01017 0.01538 0.00734 AFIX 33 H45A 2 0.708167 0.745775 0.457689 11.00000 -1.50000 H45B 2 0.627980 0.705941 0.475250 11.00000 -1.50000 H45C 2 0.682302 0.686014 0.423727 11.00000 -1.50000 AFIX 0 C47 1 0.726316 0.586798 0.519804 11.00000 0.08071 0.05489 = 0.06352 -0.01525 -0.00101 0.01274 part 1 C46 1 0.878689 0.645449 0.487884 31.00000 0.06377 0.06403 = 0.07688 -0.02349 0.01909 0.02326 AFIX 33 H46A 2 0.916167 0.623996 0.518209 31.00000 -1.50000 H46B 2 0.909499 0.681517 0.478662 31.00000 -1.50000 H46C 2 0.867883 0.620868 0.453336 31.00000 -1.50000 AFIX 0 C48 1 0.622909 0.587742 0.528070 31.00000 0.08349 0.03397 = 0.05474 -0.01218 -0.00331 0.00462 AFIX 33 H48A 2 0.615213 0.607024 0.564615 31.00000 -1.50000 H48B 2 0.600309 0.547427 0.528523 31.00000 -1.50000 H48C 2 0.589346 0.609357 0.496177 31.00000 -1.50000 AFIX 0 part 0 C49 1 0.713807 0.554081 0.460896 11.00000 0.10989 0.08707 = 0.07510 -0.03190 -0.00024 0.01064 AFIX 33 H49A 2 0.688325 0.581057 0.430575 11.00000 -1.50000 H49B 2 0.673073 0.520769 0.463091 11.00000 -1.50000 H49C 2 0.772151 0.539827 0.451945 11.00000 -1.50000 AFIX 0 part 1 C50 1 0.759292 0.549335 0.574268 31.00000 0.08301 0.05333 = 0.06934 -0.01343 -0.00006 0.01227 AFIX 33 H50A 2 0.762614 0.574138 0.608706 31.00000 -1.50000 H50B 2 0.818891 0.533265 0.570538 31.00000 -1.50000 H50C 2 0.717057 0.517101 0.577721 31.00000 -1.50000 AFIX 0 part 2 C46A 1 0.873558 0.671518 0.476232 -31.00000 0.06153 0.06348 = 0.07098 -0.00676 0.02056 0.02692 AFIX 33 H46D 2 0.923693 0.651719 0.499264 -31.00000 -1.50000 H46E 2 0.888168 0.713091 0.472118 -31.00000 -1.50000 H46F 2 0.862999 0.653307 0.438027 -31.00000 -1.50000 AFIX 0 C48A 1 0.647916 0.585154 0.556133 -31.00000 0.09191 0.04936 = 0.07506 -0.01897 0.00813 0.00039 AFIX 33 H48D 2 0.596186 0.605723 0.535664 -31.00000 -1.50000 H48E 2 0.665838 0.604399 0.593247 -31.00000 -1.50000 H48F 2 0.631608 0.544287 0.562711 -31.00000 -1.50000 AFIX 0 C50A 1 0.814868 0.556544 0.549873 -31.00000 0.08301 0.05333 = 0.06934 -0.01343 -0.00006 0.01227 AFIX 33 H50D 2 0.861143 0.557499 0.523708 -31.00000 -1.50000 H50E 2 0.801926 0.515724 0.559121 -31.00000 -1.50000 H50F 2 0.836347 0.577681 0.585404 -31.00000 -1.50000 AFIX 0 part 0 part 1 SI4 5 0.893589 0.869363 0.567747 21.00000 0.02156 0.04604 = 0.03966 0.00925 0.00269 -0.00732 N4 3 0.835001 0.843724 0.621173 21.00000 0.01652 0.03100 = 0.03512 0.00289 0.00013 0.00076 C51 1 0.948070 0.810436 0.526758 21.00000 0.04014 0.05496 = 0.06034 0.00051 0.01624 -0.00206 AFIX 33 H51A 2 0.990716 0.788163 0.553509 21.00000 -1.50000 H51B 2 0.979942 0.828716 0.497201 21.00000 -1.50000 H51C 2 0.901763 0.783915 0.508340 21.00000 -1.50000 AFIX 0 C52 1 0.983701 0.922848 0.598008 21.00000 0.02854 0.05870 = 0.05620 -0.00297 0.01171 -0.01249 AFIX 33 H52A 2 1.027312 0.902599 0.625840 21.00000 -1.50000 H52B 2 0.956159 0.955126 0.617274 21.00000 -1.50000 H52C 2 1.014300 0.938517 0.566583 21.00000 -1.50000 AFIX 0 C53 1 0.812725 0.910959 0.514720 21.00000 0.03347 0.03870 = 0.04372 0.01384 -0.00060 -0.00784 C54 1 0.745893 0.868492 0.480543 21.00000 0.02806 0.04130 = 0.03548 0.01590 0.00206 -0.00493 AFIX 33 H54A 2 0.779023 0.840192 0.459675 21.00000 -1.50000 H54B 2 0.704558 0.890808 0.452997 21.00000 -1.50000 H54C 2 0.711689 0.847527 0.507269 21.00000 -1.50000 AFIX 0 C55 1 0.758230 0.955715 0.546633 21.00000 0.03992 0.03717 = 0.05068 0.01234 -0.00367 -0.00535 AFIX 33 H55A 2 0.799567 0.983136 0.568562 21.00000 -1.50000 H55B 2 0.723488 0.934718 0.573039 21.00000 -1.50000 H55C 2 0.717269 0.977514 0.518424 21.00000 -1.50000 AFIX 0 C56 1 0.865041 0.942822 0.470085 21.00000 0.04991 0.07421 = 0.06076 0.03188 0.00299 -0.01635 AFIX 33 H56A 2 0.908443 0.970178 0.490270 21.00000 -1.50000 H56B 2 0.822663 0.964537 0.442669 21.00000 -1.50000 H56C 2 0.896891 0.913772 0.449270 21.00000 -1.50000 AFIX 0 part 2 SI4A 5 0.864019 0.908989 0.595888 -21.00000 0.02909 0.01924 = 0.08937 0.01507 0.01512 -0.00016 N4A 3 0.828379 0.855513 0.638908 -21.00000 0.02347 0.02321 = 0.04797 -0.00094 -0.00049 -0.00089 C51A 1 0.775773 0.968117 0.589888 -21.00000 0.04283 0.03145 = 0.07414 0.01464 0.01103 0.00361 AFIX 33 H51D 2 0.767189 0.982022 0.628506 -21.00000 -1.50000 H51E 2 0.719064 0.952250 0.570840 -21.00000 -1.50000 H51F 2 0.795127 1.000859 0.567193 -21.00000 -1.50000 AFIX 0 C52A 1 0.971197 0.944662 0.628692 -21.00000 0.04296 0.04208 = 0.09590 0.00978 0.00635 -0.00604 AFIX 33 H52D 2 0.964460 0.957910 0.667816 -21.00000 -1.50000 H52E 2 0.984514 0.978393 0.605164 -21.00000 -1.50000 H52F 2 1.020492 0.916281 0.630198 -21.00000 -1.50000 AFIX 0 C53A 1 0.879490 0.884635 0.521080 -21.00000 0.05842 0.05094 = 0.07685 0.01085 0.01833 -0.00366 C54A 1 0.919561 0.932111 0.484252 -21.00000 0.06072 0.06024 = 0.09564 0.02291 0.02206 -0.00104 AFIX 33 H54D 2 0.880992 0.966944 0.481703 -21.00000 -1.50000 H54E 2 0.923219 0.916713 0.445465 -21.00000 -1.50000 H54F 2 0.979821 0.942708 0.502290 -21.00000 -1.50000 AFIX 0 C55A 1 0.945629 0.832381 0.525592 -21.00000 0.06211 0.05168 = 0.09150 0.01447 0.02331 -0.00145 AFIX 33 H55D 2 1.003220 0.844673 0.546478 -21.00000 -1.50000 H55E 2 0.954784 0.819266 0.486813 -21.00000 -1.50000 H55F 2 0.920819 0.800072 0.546345 -21.00000 -1.50000 AFIX 0 C56A 1 0.787038 0.866667 0.490038 -21.00000 0.06367 0.06956 = 0.08328 0.01076 0.01855 -0.01027 AFIX 33 H56D 2 0.745465 0.899851 0.489803 -21.00000 -1.50000 H56E 2 0.763624 0.833463 0.510266 -21.00000 -1.50000 H56F 2 0.793202 0.855254 0.450293 -21.00000 -1.50000 AFIX 0 part 0 K1 6 0.462873 0.922924 0.773085 11.00000 0.06801 0.10702 = 0.05528 -0.03626 0.00602 0.02819 O1 4 0.401823 0.998243 0.848127 11.00000 0.09745 0.09570 = 0.08134 -0.02569 0.03058 0.00527 C57 1 0.512827 0.961613 0.917233 11.00000 0.09189 0.09084 = 0.07997 -0.01396 0.02722 -0.01390 AFIX 33 H57A 2 0.544038 0.968253 0.956018 11.00000 -1.50000 H57B 2 0.556385 0.962272 0.889229 11.00000 -1.50000 H57C 2 0.482797 0.923370 0.915866 11.00000 -1.50000 AFIX 0 C58 1 0.445737 1.008019 0.903115 11.00000 0.08751 0.07852 = 0.07110 -0.02128 0.03160 -0.01716 AFIX 23 H58A 2 0.401838 1.007821 0.931477 11.00000 -1.20000 H58B 2 0.475611 1.046812 0.904724 11.00000 -1.20000 AFIX 0 C59 1 0.332794 1.037899 0.834203 11.00000 0.09469 0.09764 = 0.09911 -0.01440 0.03360 0.00378 AFIX 23 H59A 2 0.356526 1.078429 0.837848 11.00000 -1.20000 H59B 2 0.287121 1.033337 0.861072 11.00000 -1.20000 AFIX 0 C60 1 0.291631 1.027441 0.774891 11.00000 0.14997 0.14726 = 0.12640 -0.02153 0.01178 0.01859 AFIX 33 H60A 2 0.242699 1.055516 0.765016 11.00000 -1.50000 H60B 2 0.267745 0.987405 0.771597 11.00000 -1.50000 H60C 2 0.336945 1.032413 0.748432 11.00000 -1.50000 AFIX 0 rem part -1 O1S 4 0.539929 0.928543 0.405013 10.50000 10.10000 C1S 1 0.498185 0.991403 0.476644 10.50000 10.10000 AFIX 33 H1S1 2 0.480945 0.991621 0.515750 10.50000 -1.50000 H1S2 2 0.451457 1.010808 0.450319 10.50000 -1.50000 H1S3 2 0.555149 1.012378 0.476374 10.50000 -1.50000 AFIX 0 C2S 1 0.509095 0.928156 0.457151 10.50000 10.10000 AFIX 23 H2S1 2 0.552030 0.907175 0.485558 10.50000 -1.20000 H2S2 2 0.450616 0.907577 0.454347 10.50000 -1.20000 AFIX 0 C3S 1 0.535874 0.874701 0.375488 10.50000 10.10000 AFIX 23 H3S1 2 0.568456 0.843614 0.399114 10.50000 -1.20000 H3S2 2 0.561203 0.878125 0.338460 10.50000 -1.20000 AFIX 0 C4S 1 0.434636 0.862143 0.365649 10.50000 10.10000 AFIX 33 H4S1 2 0.424521 0.822423 0.350162 10.50000 -1.50000 H4S2 2 0.405178 0.890646 0.338179 10.50000 -1.50000 H4S3 2 0.409582 0.865346 0.402324 10.50000 -1.50000 part 0 AFIX 0 HKLF 4 REM pld1366sm in P2(1)/n REM R1 = 0.0817 for 16010 Fo > 4sig(Fo) and 0.1001 for all 19525 data REM 874 parameters refined using 2084 restraints END WGHT 0.0328 131.4948 REM Highest difference peak 4.419, deepest hole -2.427, 1-sigma level 0.195 Q1 1 0.4400 0.7967 0.5971 11.00000 0.05 4.42 Q2 1 0.3578 0.8126 0.7733 11.00000 0.05 3.16 Q3 1 0.9559 0.9591 0.7788 11.00000 0.05 3.01 Q4 1 0.2680 0.8763 0.5532 11.00000 0.05 2.84 Q5 1 0.4434 0.8242 0.6417 11.00000 0.05 2.16 ; _shelx_res_checksum 74817 _shelx_hkl_file ; 3 0 0 -1.20 1.50 -3 0 0 -1.30 2.10 -4 0 0 841.62 18.80 4 0 0 827.82 17.30 4 0 0 827.52 17.30 5 0 0 7.20 2.50 5 0 0 -1.10 1.80 5 0 0 6.90 2.40 -5 0 0 3.50 2.80 6 0 0 1065.79 22.40 6 0 0 1031.70 22.30 -6 0 0 1032.00 24.20 6 0 0 1065.39 21.40 7 0 0 11.20 2.60 -7 0 0 13.00 4.20 7 0 0 8.90 3.10 7 0 0 7.70 3.30 8 0 0 1274.87 27.60 -8 0 0 1247.28 29.80 8 0 0 1256.97 27.50 8 0 0 1290.77 26.10 9 0 0 -0.70 3.30 9 0 0 3.50 2.50 -9 0 0 1.40 4.40 9 0 0 1.30 3.60 10 0 0 0.60 3.90 -10 0 0 -0.40 4.80 10 0 0 5.60 3.10 10 0 0 3.70 3.60 11 0 0 -17.50 4.70 -11 0 0 -3.60 5.30 11 0 0 3.10 4.30 -12 0 0 992.00 28.00 12 0 0 999.40 25.20 -13 0 0 15.70 7.40 13 0 0 11.90 5.70 14 0 0 177.08 11.90 -14 0 0 194.48 14.80 -15 0 0 71.99 11.30 15 0 0 63.19 8.80 16 0 0 100.09 11.20 -16 0 0 121.49 14.00 -17 0 0 6.10 10.50 17 0 0 -8.20 7.70 -18 0 0 739.63 29.30 18 0 0 702.73 26.00 -19 0 0 35.50 13.70 3 -1 0 11.60 2.10 -3 -1 0 12.20 2.60 -3 1 0 9.00 2.40 4 -1 0 2139.19 41.90 -4 -1 0 2162.28 44.10 4 -1 0 2198.58 41.30 -4 1 0 2200.68 43.90 4 1 0 2145.39 41.50 5 -1 0 10.60 2.60 5 -1 0 7.20 2.40 -5 -1 0 10.20 3.20 5 1 0 10.00 2.30 5 1 0 7.60 2.60 5 1 0 4.40 2.10 -5 1 0 8.40 3.00 6 -1 0 124.89 5.70 6 -1 0 118.89 4.40 6 -1 0 126.89 5.90 -6 -1 0 113.79 6.60 -6 1 0 115.99 6.40 6 1 0 131.49 6.00 6 1 0 128.19 5.40 6 1 0 117.39 4.90 -7 -1 0 210.38 9.20 7 -1 0 209.88 6.50 7 -1 0 212.78 7.90 7 -1 0 217.98 8.40 -7 1 0 190.18 8.70 7 1 0 212.68 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3.90 9.80 -13 -13 -4 90.29 13.10 13 -13 4 82.19 11.30 13 -13 4 96.89 12.30 -13 13 -4 80.09 13.10 -14 -13 -4 127.79 15.20 14 -13 4 114.29 13.50 14 -13 4 108.69 13.50 -14 13 -4 114.09 14.70 -15 -13 -4 3.80 10.90 15 -13 4 -8.50 10.40 15 -13 4 -3.00 11.30 -15 13 -4 27.30 13.00 16 -13 4 107.59 16.20 -16 -13 -4 123.79 16.90 -16 13 -4 93.39 16.30 -17 -13 -4 104.29 17.50 17 -13 4 124.59 16.90 -17 13 -4 88.79 17.90 -17 -14 4 153.18 20.10 17 -14 -4 161.88 17.60 16 -14 -4 48.10 13.60 -16 -14 4 62.99 14.50 15 -14 -4 59.59 12.60 -15 -14 4 21.30 12.40 15 14 -4 31.80 10.50 -14 -14 4 94.19 14.50 14 -14 -4 90.79 12.70 14 14 -4 88.59 12.30 -14 14 4 102.49 13.20 13 -14 -4 514.15 21.80 -13 -14 4 557.94 24.70 -13 14 4 557.54 22.30 13 14 -4 531.15 21.80 12 -14 -4 120.89 12.20 -12 -14 4 125.49 13.90 12 14 -4 110.49 11.80 -12 14 4 124.29 12.40 11 -14 -4 38.10 9.00 -11 -14 4 45.70 10.00 -11 14 4 48.10 9.20 11 14 -4 71.29 10.10 10 -14 -4 74.69 9.40 10 -14 -4 60.89 8.90 -10 -14 4 61.09 10.30 -10 14 4 78.49 9.80 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9.10 8.70 -10 16 4 11.70 8.40 10 16 -4 12.60 8.10 9 -16 -4 -2.40 7.40 9 -16 -4 12.50 7.60 -9 -16 4 9.10 8.10 -9 16 4 1.50 7.80 9 16 -4 3.20 7.30 8 -16 -4 55.49 8.80 -8 -16 4 57.39 9.90 8 -16 -4 45.70 8.40 -8 16 4 57.49 9.60 8 16 -4 63.59 9.00 7 -16 -4 29.10 7.40 7 -16 -4 22.60 6.70 -7 -16 4 32.40 8.20 7 16 -4 36.10 7.60 -7 16 4 15.30 5.70 -7 16 4 31.00 8.10 6 -16 -4 62.79 7.60 -6 -16 4 58.69 9.20 6 -16 -4 54.59 7.90 -6 16 4 61.19 7.10 -6 16 4 70.49 8.60 6 16 -4 65.99 8.40 -5 -16 4 876.11 26.50 5 -16 -4 911.41 24.60 5 -16 -4 918.21 23.80 5 16 -4 890.31 24.80 -5 16 4 911.51 23.30 -5 16 4 912.61 24.70 -4 -16 4 148.49 11.80 4 -16 -4 154.28 10.90 4 -16 -4 143.69 9.60 4 16 -4 137.09 10.70 -4 16 4 150.38 9.50 -4 16 4 154.78 10.60 3 -16 -4 105.49 8.20 -3 -16 4 134.59 11.10 3 -16 -4 132.79 9.90 -3 16 4 110.29 8.60 3 16 -4 121.09 9.50 -3 16 4 124.99 9.70 -2 -16 4 490.65 18.10 2 -16 -4 478.15 14.60 2 16 -4 494.95 16.20 -2 16 4 511.75 15.90 -1 -16 4 45.20 7.80 1 -16 -4 55.29 6.90 1 -16 -4 40.20 5.40 -1 16 4 48.00 6.80 1 16 -4 54.19 6.80 0 -16 4 454.85 14.50 0 -16 -4 448.86 13.30 0 -16 -4 466.35 15.40 0 16 -4 446.66 17.70 0 16 -4 459.85 14.90 0 16 4 458.95 15.80 -1 -16 -4 275.77 12.10 1 -16 4 265.77 11.30 1 -16 4 277.17 9.60 -1 -16 -4 262.07 10.00 -1 16 -4 271.37 14.20 1 16 4 266.57 12.40 -1 16 -4 293.97 11.80 -2 -16 -4 191.88 11.00 2 -16 4 175.18 8.70 2 -16 4 184.18 10.00 2 16 4 198.08 11.20 -2 16 -4 204.08 12.80 -2 16 -4 174.48 9.70 -3 -16 -4 59.99 7.60 3 -16 4 65.59 6.50 3 -16 4 82.19 6.90 3 16 4 70.99 7.80 -3 16 -4 66.79 6.60 -3 16 -4 65.09 9.10 4 -16 4 69.29 7.00 -4 -16 -4 68.29 8.20 4 -16 4 66.59 6.70 -4 16 -4 72.69 6.80 4 16 4 82.19 8.70 -4 16 -4 66.69 9.30 5 -16 4 155.48 10.30 5 -16 4 168.28 10.10 -5 -16 -4 156.28 11.50 -5 16 -4 173.08 13.30 5 16 4 161.88 11.20 6 -16 4 7.40 5.40 -6 -16 -4 11.80 6.60 6 -16 4 -1.40 5.90 -6 16 -4 7.00 8.30 6 16 4 9.60 6.30 -7 -16 -4 88.89 10.30 7 -16 4 64.99 7.80 7 -16 4 68.59 8.60 7 16 4 76.79 9.30 -7 16 -4 91.19 11.30 -8 -16 -4 70.69 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15.70 -4 -23 4 10.90 11.60 -4 23 4 15.10 8.90 4 23 -4 8.70 10.10 3 -23 -4 20.40 9.80 -3 -23 4 16.80 11.10 -3 23 4 14.10 9.20 3 23 -4 33.80 10.40 2 -23 -4 158.38 13.70 -2 -23 4 162.48 16.00 2 23 -4 137.79 13.80 -2 23 4 130.09 13.30 1 -23 -4 46.80 10.10 -1 -23 4 48.80 12.30 -1 23 4 60.99 10.80 1 23 -4 42.10 10.90 0 -23 -4 25.30 9.90 0 -23 4 18.70 11.30 0 23 4 25.60 10.20 0 23 -4 20.00 9.50 -1 -23 -4 -5.10 8.80 1 -23 4 -0.30 10.70 -1 23 -4 10.40 9.00 1 23 4 22.80 9.40 -2 -23 -4 160.78 14.70 2 23 4 177.98 14.60 -2 23 -4 193.68 14.40 -3 -23 -4 147.39 14.60 3 -23 4 145.39 13.00 -3 23 -4 171.78 16.70 3 23 4 165.58 14.80 4 -23 4 28.00 9.70 -4 -23 -4 4.40 9.80 -4 23 -4 27.40 12.10 4 23 4 24.60 10.40 5 -23 4 58.29 11.10 -5 -23 -4 50.79 11.60 -5 23 -4 66.79 14.00 5 23 4 36.80 10.90 6 -23 4 240.98 17.80 -6 -23 -4 237.48 18.50 -6 23 -4 240.08 19.70 6 23 4 228.68 17.90 -7 -23 -4 10.10 11.40 7 -23 4 16.10 10.70 7 23 4 16.10 10.40 -7 23 -4 24.00 13.50 8 -23 4 28.60 11.00 -8 -23 -4 42.10 13.40 8 23 4 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13.30 -14 -16 14 35.20 15.10 14 16 -14 59.09 14.90 13 -16 -14 26.70 13.00 -13 -16 14 31.40 14.60 13 16 -14 44.40 13.80 12 -16 -14 118.99 15.20 -12 -16 14 109.59 17.30 12 16 -14 100.09 15.00 -11 -16 14 77.39 15.60 11 -16 -14 70.19 13.30 11 16 -14 70.99 13.50 -11 16 14 61.19 11.90 -10 -16 14 127.99 16.80 10 -16 -14 151.28 15.10 10 16 -14 130.49 15.00 -10 16 14 151.48 13.80 -9 -16 14 352.76 22.20 9 -16 -14 377.16 20.10 -9 16 14 391.06 18.50 9 16 -14 369.86 20.00 -8 -16 14 133.39 16.00 8 -16 -14 127.59 13.80 -8 16 14 125.09 12.80 8 16 -14 140.39 14.40 7 -16 -14 108.39 12.80 -7 -16 14 121.19 15.00 -7 16 14 110.79 12.30 7 16 -14 117.19 12.70 6 -16 -14 178.28 14.40 -6 -16 14 169.68 16.40 6 16 -14 127.69 13.30 -6 16 14 163.38 13.60 5 -16 -14 46.80 9.70 -5 -16 14 31.20 11.50 -5 16 14 39.10 9.60 5 16 -14 57.59 10.60 -4 -16 14 142.59 15.00 4 -16 -14 127.39 12.20 4 16 -14 128.29 12.10 -4 16 14 97.99 11.00 3 -16 -14 8.40 8.00 -3 -16 14 3.70 9.40 3 16 -14 11.40 8.40 -3 16 14 3.60 7.70 2 -16 -14 7.90 7.70 -2 -16 14 21.50 9.70 -2 16 14 1.80 7.20 2 16 -14 7.80 8.00 1 -16 -14 128.29 11.60 -1 -16 14 136.19 8.40 -1 16 14 114.49 11.40 1 16 -14 140.79 14.20 1 16 -14 134.09 11.80 0 -16 14 65.49 6.00 0 -16 -14 56.39 9.50 0 16 -14 64.29 11.50 0 16 14 63.29 9.60 0 16 -14 79.99 9.90 -1 -16 -14 32.40 8.80 1 -16 14 36.40 5.20 -1 16 -14 31.20 10.60 1 16 14 34.90 8.40 -1 16 -14 28.40 8.10 2 -16 14 68.99 6.00 -2 -16 -14 69.29 10.10 2 16 14 67.49 9.80 -2 16 -14 62.19 11.90 3 -16 14 292.67 15.20 3 -16 14 287.07 11.10 -3 -16 -14 278.67 15.90 3 16 14 316.07 16.80 -3 16 -14 295.07 18.40 -4 -16 -14 159.38 12.80 4 -16 14 162.28 12.20 4 -16 14 164.88 9.60 -4 16 -14 157.88 15.00 4 16 14 158.48 13.20 5 -16 14 92.69 10.80 5 -16 14 80.19 7.70 5 16 14 93.79 11.30 -5 16 -14 68.99 13.40 6 -16 14 218.28 12.30 6 -16 14 281.27 16.30 6 16 14 275.07 16.80 -6 16 -14 233.38 18.90 7 -16 14 7.70 9.70 7 -16 14 13.70 7.20 -7 16 -14 17.30 12.20 7 16 14 13.50 9.10 8 -16 14 121.89 10.40 8 -16 14 94.69 12.40 -8 16 -14 92.29 15.20 8 16 14 94.49 12.30 9 -16 14 156.28 14.90 9 -16 14 160.48 12.20 -9 16 -14 120.59 16.40 9 16 14 147.69 14.30 10 -16 14 31.50 12.20 10 -16 14 52.79 10.40 10 16 14 50.39 10.70 -10 16 -14 90.39 16.10 11 -16 14 91.59 14.90 11 -16 14 102.69 12.80 -11 16 -14 88.49 16.70 12 -16 14 20.50 11.50 12 -16 14 5.40 12.90 -12 16 -14 47.60 16.10 13 -16 14 68.29 15.10 13 -16 14 59.29 13.70 -13 16 -14 48.30 17.30 -14 -17 14 11.00 15.40 14 -17 -14 12.70 13.50 14 17 -14 13.80 14.30 13 -17 -14 196.98 19.00 -13 -17 14 199.28 21.30 13 17 -14 200.28 18.90 -12 -17 14 31.70 15.40 12 -17 -14 37.80 12.90 12 17 -14 70.69 14.90 11 -17 -14 60.09 14.10 -11 -17 14 69.09 16.40 11 17 -14 57.79 14.00 -10 -17 14 15.50 13.20 10 -17 -14 36.00 12.10 -10 17 14 57.79 11.90 10 17 -14 42.40 12.70 9 -17 -14 19.80 11.40 -9 -17 14 -2.50 12.60 -9 17 14 21.00 10.40 9 17 -14 11.10 11.40 -8 -17 14 54.29 13.90 8 -17 -14 78.99 12.50 8 17 -14 90.39 12.80 -8 17 14 88.79 11.80 -7 -17 14 76.79 14.00 7 -17 -14 63.79 11.50 -7 17 14 65.29 11.20 7 17 -14 62.99 12.10 -6 -17 14 16.40 11.50 6 -17 -14 23.60 9.70 6 17 -14 28.50 10.50 -6 17 14 25.50 9.50 -5 -17 14 158.28 16.60 5 -17 -14 130.39 13.40 -5 17 14 165.28 13.80 5 17 -14 149.19 13.80 4 -17 -14 104.89 11.60 -4 -17 14 133.89 15.10 4 17 -14 96.49 11.90 -4 17 14 128.99 12.40 3 -17 -14 34.70 8.90 -3 -17 14 32.40 11.70 -3 17 14 32.20 8.70 3 17 -14 27.50 9.10 2 -17 -14 174.88 13.20 -2 -17 14 203.28 16.60 -2 17 14 191.28 14.30 2 17 -14 176.88 13.70 1 -17 -14 326.97 16.90 1 17 -14 328.27 16.60 -1 17 14 357.86 17.10 0 -17 14 101.59 7.30 0 -17 -14 135.09 12.10 0 17 -14 124.49 11.40 0 17 -14 122.29 13.60 0 17 14 97.29 11.10 -1 -17 -14 28.40 8.90 1 -17 14 11.70 5.30 1 17 14 16.40 8.10 -1 17 -14 0.30 10.00 -2 -17 -14 204.78 15.10 2 -17 14 212.28 10.20 2 17 14 234.88 15.10 -2 17 -14 214.88 16.50 -3 -17 -14 27.90 8.70 3 -17 14 17.80 5.60 3 17 14 33.20 9.30 -3 17 -14 16.50 11.20 4 -17 14 36.00 6.20 4 17 14 20.10 8.90 -4 17 -14 11.00 10.90 5 -17 14 179.58 11.10 5 -17 14 165.98 13.20 5 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144.39 11.80 3 13 -15 167.88 12.20 2 -13 -15 570.74 20.20 -2 13 15 530.75 19.50 2 13 -15 577.64 19.60 1 -13 -15 96.39 10.30 -1 13 15 121.69 10.50 1 13 -15 139.49 12.70 1 13 -15 95.49 10.00 0 -13 15 43.20 7.50 0 -13 -15 40.90 8.60 0 13 15 54.39 8.40 0 13 -15 51.29 8.40 0 13 -15 50.29 10.30 -1 -13 -15 46.00 8.70 1 -13 15 34.40 6.90 -1 13 -15 27.00 7.30 1 13 15 35.00 8.00 -1 13 -15 28.30 9.50 -2 -13 -15 40.70 8.90 2 -13 15 39.80 7.70 2 -13 15 46.20 4.00 -2 13 -15 52.59 10.50 2 13 15 40.50 8.20 3 -13 15 16.60 4.10 3 -13 15 10.40 7.30 -3 -13 -15 27.40 8.20 -3 13 -15 20.00 9.80 3 13 15 20.50 7.30 -4 -13 -15 65.09 9.80 4 -13 15 73.19 5.80 4 -13 15 76.79 9.80 -4 13 -15 73.89 11.60 4 13 15 73.49 9.40 5 -13 15 278.27 15.30 5 -13 15 254.47 10.50 -5 -13 -15 255.27 15.40 -5 13 -15 261.07 17.60 5 13 15 251.37 14.60 -6 -13 -15 181.38 14.20 6 -13 15 156.28 12.80 6 -13 15 171.78 10.10 6 13 15 181.98 13.40 -6 13 -15 154.88 14.70 -7 -13 -15 19.40 8.40 7 -13 15 -0.50 6.10 7 -13 15 11.50 9.40 -7 13 -15 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2 -14 15 724.13 16.40 -2 14 -15 698.63 24.80 2 14 15 703.83 23.00 3 -14 15 39.10 4.70 3 -14 15 39.40 8.30 -3 -14 -15 37.40 8.60 3 14 15 24.10 8.10 -3 14 -15 34.20 10.60 4 -14 15 5.90 4.60 4 -14 15 22.20 8.20 -4 -14 -15 4.70 7.90 4 14 15 7.00 7.40 -4 14 -15 0.00 10.00 -5 -14 -15 164.98 13.30 5 -14 15 118.39 9.00 5 -14 15 152.78 12.40 5 14 15 135.69 12.20 -5 14 -15 142.59 14.60 -6 -14 -15 190.08 14.90 6 -14 15 226.48 15.90 6 -14 15 213.48 11.20 -6 14 -15 227.98 18.10 6 14 15 217.48 15.00 7 -14 15 228.48 16.50 7 -14 15 210.38 12.20 7 14 15 191.88 14.90 -7 14 -15 214.88 17.30 8 -14 15 -6.90 10.00 8 -14 15 20.50 7.70 -8 14 -15 32.50 12.70 8 14 15 2.80 8.10 9 -14 15 3.00 8.00 9 -14 15 -4.40 10.30 9 14 15 2.00 8.20 -9 14 -15 28.20 13.00 10 -14 15 1.00 8.90 10 -14 15 1.50 11.10 -10 14 -15 29.80 13.50 11 -14 15 11.60 10.00 11 -14 15 9.60 11.90 -11 14 -15 -3.10 13.50 12 -14 15 -22.60 11.30 12 -14 15 -1.00 10.30 -12 14 -15 19.50 15.20 13 -14 15 5.70 11.30 13 -14 15 -0.40 13.30 -13 14 -15 -2.60 15.50 15 -15 -15 25.80 14.60 -15 -15 15 18.70 15.30 15 15 -15 8.40 13.60 -14 -15 15 45.30 15.50 14 -15 -15 22.30 13.40 14 15 -15 33.50 14.50 -13 -15 15 70.19 16.00 13 -15 -15 29.90 12.80 13 15 -15 29.40 13.60 12 -15 -15 83.79 14.10 -12 -15 15 86.29 15.40 12 15 -15 73.89 14.00 11 -15 -15 33.60 12.10 -11 -15 15 46.60 14.00 -11 15 15 42.80 11.30 11 15 -15 35.40 12.60 -10 -15 15 48.60 13.70 10 -15 -15 42.90 11.90 -10 15 15 42.30 10.90 10 15 -15 47.20 11.70 -9 -15 15 82.79 14.70 9 -15 -15 76.39 12.50 -9 15 15 87.19 11.60 9 15 -15 54.79 11.80 -8 -15 15 326.87 20.60 8 -15 -15 324.07 18.80 -8 15 15 314.57 17.90 8 15 -15 291.57 18.30 -7 -15 15 351.16 20.60 7 -15 -15 356.36 18.90 7 15 -15 366.26 18.90 -7 15 15 367.16 18.50 -6 -15 15 -0.60 10.40 6 -15 -15 11.10 9.20 6 15 -15 -1.00 9.30 -6 15 15 19.60 8.70 -5 -15 15 111.89 14.00 5 -15 -15 116.69 12.20 -5 15 15 106.59 11.80 5 15 -15 108.29 12.10 4 -15 -15 45.40 9.60 -4 -15 15 36.80 11.10 4 15 -15 45.60 9.90 -4 15 15 48.50 9.40 3 -15 -15 211.38 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13.70 9 16 -15 106.79 14.30 -8 -16 15 59.29 13.80 8 -16 -15 51.59 11.40 8 16 -15 54.79 11.80 -8 16 15 56.99 11.00 -7 -16 15 24.20 12.50 7 -16 -15 22.50 10.30 7 16 -15 9.30 10.10 -7 16 15 18.60 9.60 6 -16 -15 157.58 13.70 -6 -16 15 159.58 16.20 6 16 -15 188.08 15.20 -6 16 15 194.78 14.90 5 -16 -15 40.30 10.50 -5 -16 15 28.40 11.90 5 16 -15 34.70 10.30 -5 16 15 26.70 9.40 -4 -16 15 268.17 19.10 4 -16 -15 272.77 16.40 4 16 -15 288.07 17.20 -4 16 15 274.37 16.00 -3 -16 15 7.60 10.80 3 -16 -15 13.20 8.30 3 16 -15 23.50 9.10 -3 16 15 35.80 9.20 -2 -16 15 32.00 10.90 2 -16 -15 32.70 9.40 -2 16 15 35.40 9.20 2 16 -15 27.80 9.10 -1 -16 15 133.59 8.40 1 -16 -15 155.28 12.70 1 16 -15 142.09 12.30 -1 16 15 153.68 12.60 1 16 -15 151.88 15.00 0 -16 -15 22.50 9.00 0 -16 15 21.10 5.20 0 16 -15 24.70 10.50 0 16 -15 8.60 8.20 0 16 15 20.50 8.50 -1 -16 -15 91.59 11.00 1 -16 15 97.39 7.70 1 16 15 112.59 11.50 -1 16 -15 91.49 12.80 2 -16 15 240.98 9.80 -2 -16 -15 235.08 15.90 2 16 15 266.97 15.60 -2 16 -15 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159.28 9.30 0 -17 -15 179.78 14.10 0 17 15 180.08 14.10 0 17 -15 177.48 13.10 0 17 -15 171.98 15.80 1 -17 15 59.99 6.50 -1 -17 -15 51.19 10.10 1 17 15 64.59 10.50 -1 17 -15 60.59 12.20 -2 -17 -15 6.10 8.70 2 -17 15 15.30 5.60 2 17 15 -1.00 8.10 -2 17 -15 8.00 10.70 3 -17 15 15.30 5.50 -3 -17 -15 23.90 8.70 -3 17 -15 -8.10 11.00 3 17 15 26.50 9.40 4 -17 15 15.10 6.00 -4 17 -15 13.50 11.70 4 17 15 8.20 9.20 5 -17 15 2.80 6.30 5 -17 15 2.00 8.80 5 17 15 7.80 9.20 -5 17 -15 15.30 11.90 6 -17 15 227.58 12.80 6 -17 15 234.98 16.60 -6 17 -15 249.08 20.10 6 17 15 200.28 16.20 7 -17 15 118.79 10.50 7 -17 15 116.59 13.50 -7 17 -15 140.49 16.70 7 17 15 127.49 13.40 8 -17 15 -2.30 10.40 8 -17 15 20.30 8.70 -8 17 -15 -2.20 12.80 8 17 15 6.20 9.10 9 -17 15 96.69 11.30 9 -17 15 85.39 13.80 9 17 15 77.59 12.30 -9 17 -15 76.39 16.00 10 -17 15 57.49 11.20 10 -17 15 84.39 14.70 -10 17 -15 52.09 16.10 11 -17 15 92.19 13.10 11 -17 15 77.79 15.30 -11 17 -15 84.79 17.80 12 -17 15 11.90 12.10 12 -17 15 2.30 13.40 -12 17 -15 -10.10 15.40 13 -18 -15 107.89 17.00 -13 -18 15 124.39 19.50 13 18 -15 177.28 19.40 -12 -18 15 45.00 16.80 12 -18 -15 61.29 14.70 12 18 -15 82.99 15.50 -11 -18 15 52.19 16.00 11 -18 -15 49.99 13.60 11 18 -15 47.30 14.50 10 -18 -15 16.50 12.20 -10 -18 15 -8.40 13.40 10 18 -15 8.10 12.70 -10 18 15 15.50 11.20 9 -18 -15 248.38 19.90 -9 -18 15 246.88 22.10 -9 18 15 251.27 18.20 9 18 -15 281.87 19.80 -8 -18 15 25.40 14.30 8 -18 -15 41.30 12.20 8 18 -15 49.10 12.70 -8 18 15 22.70 11.10 -7 -18 15 41.40 14.20 7 -18 -15 32.50 11.60 -7 18 15 41.70 11.40 7 18 -15 55.29 12.10 6 -18 -15 81.79 12.50 -6 -18 15 83.79 15.30 6 18 -15 84.99 13.10 -6 18 15 87.59 12.50 -5 -18 15 18.30 12.70 5 -18 -15 15.70 10.20 5 18 -15 11.30 10.80 -5 18 15 22.80 10.30 4 -18 -15 135.59 13.00 -4 -18 15 153.38 17.50 4 18 -15 125.09 13.90 -4 18 15 144.29 13.70 3 -18 -15 17.70 9.50 -3 -18 15 15.70 12.30 -3 18 15 33.30 9.90 3 18 -15 14.20 9.60 -2 -18 15 43.90 12.70 2 -18 -15 40.70 9.80 2 18 -15 26.10 10.00 -2 18 15 32.50 9.80 1 -18 -15 493.45 20.90 1 18 -15 502.35 20.20 -1 18 15 520.85 21.60 0 -18 15 39.40 6.10 0 -18 -15 46.00 10.00 0 18 -15 53.89 12.80 0 18 -15 43.20 9.70 0 18 15 49.60 10.60 -1 -18 -15 56.29 10.50 1 -18 15 80.79 7.50 1 18 15 86.09 11.50 -1 18 -15 61.29 13.10 -2 -18 -15 44.10 10.70 2 -18 15 57.49 7.10 2 18 15 70.79 11.30 -2 18 -15 60.69 13.20 3 -18 15 213.78 11.40 3 18 15 230.18 16.40 -3 18 -15 227.88 18.30 4 -18 15 83.29 8.10 4 18 15 89.49 12.40 -4 18 -15 103.49 14.80 5 -18 15 121.09 9.40 5 18 15 121.19 13.60 -5 18 -15 119.69 16.10 6 -18 15 36.80 8.20 6 -18 15 35.00 10.70 6 18 15 46.90 11.20 -6 18 -15 41.20 14.00 7 -18 15 -3.70 10.20 7 -18 15 13.00 8.10 7 18 15 6.50 9.90 -7 18 -15 17.10 13.70 8 -18 15 -7.20 8.20 8 -18 15 -19.90 10.30 -8 18 -15 22.70 14.20 8 18 15 -2.40 9.50 9 -18 15 50.89 10.50 9 -18 15 27.10 13.00 -9 18 -15 28.50 15.20 9 18 15 26.20 11.20 10 -18 15 13.70 10.40 10 -18 15 1.00 12.40 10 18 15 -2.60 10.40 -10 18 -15 4.90 15.00 11 -18 15 66.59 12.90 11 -18 15 55.29 14.70 -11 18 -15 64.49 17.60 -13 -19 15 25.50 16.60 13 -19 -15 22.00 14.20 13 19 -15 21.70 15.50 -12 -19 15 5.80 16.20 12 -19 -15 17.30 13.70 12 19 -15 27.40 14.80 11 -19 -15 62.39 14.50 -11 -19 15 73.99 17.90 11 19 -15 70.59 15.30 -10 -19 15 34.80 15.80 10 -19 -15 43.70 13.80 -10 19 15 57.19 13.00 10 19 -15 73.49 15.00 -9 -19 15 55.99 16.50 9 -19 -15 90.09 15.00 9 19 -15 69.39 14.70 -9 19 15 90.19 13.90 -8 -19 15 29.50 15.30 8 -19 -15 13.10 11.70 8 19 -15 22.70 12.40 -8 19 15 38.30 12.20 -7 -19 15 31.70 14.70 7 -19 -15 31.20 12.00 -7 19 15 32.20 11.50 7 19 -15 45.60 12.60 6 -19 -15 30.50 11.60 -6 -19 15 23.70 14.20 -6 19 15 4.30 10.20 6 19 -15 21.30 11.80 -5 -19 15 431.56 25.50 5 -19 -15 429.96 21.40 5 19 -15 458.35 21.30 -5 19 15 449.66 21.00 -4 -19 15 30.90 13.00 4 -19 -15 7.50 9.60 -4 19 15 32.00 10.50 4 19 -15 22.50 10.70 3 -19 -15 9.10 9.80 -3 -19 15 17.30 12.50 -3 19 15 5.10 9.70 3 19 -15 1.00 9.90 2 -19 -15 62.89 11.20 -2 -19 15 54.59 14.10 2 19 -15 54.69 11.20 -2 19 15 69.99 11.70 1 -19 -15 174.38 14.40 -1 19 15 203.38 15.90 1 19 -15 180.98 14.00 0 -19 15 76.79 7.50 0 -19 -15 82.99 11.70 0 19 -15 112.29 15.30 0 19 15 67.99 11.70 -1 -19 -15 193.98 14.90 1 -19 15 167.78 10.90 -1 19 -15 194.28 17.40 1 19 15 187.28 15.20 2 -19 15 -2.20 6.10 2 19 15 4.70 9.50 -2 19 -15 -16.10 11.20 3 -19 15 74.49 8.10 3 19 15 66.29 11.80 -3 19 -15 44.20 13.30 4 -19 15 7.10 7.00 4 19 15 -8.80 9.80 -4 19 -15 1.20 12.40 5 -19 15 16.30 7.70 -5 19 -15 8.40 12.90 5 19 15 -2.90 10.00 6 -19 15 18.10 8.10 6 19 15 17.20 10.60 -6 19 -15 37.90 14.30 7 -19 15 76.49 13.60 7 -19 15 93.99 10.60 7 19 15 107.89 14.20 -7 19 -15 80.39 16.00 8 -19 15 27.40 9.50 8 -19 15 29.60 12.20 -8 19 -15 25.80 15.10 8 19 15 35.70 11.20 9 -19 15 87.99 11.60 9 -19 15 58.69 13.90 -9 19 -15 67.69 17.10 9 19 15 84.19 13.70 10 -19 15 9.20 12.70 10 -19 15 10.00 11.00 10 19 15 2.20 10.60 -10 19 -15 15.40 15.90 12 -20 -15 27.00 13.90 -12 -20 15 -36.20 15.20 12 20 -15 -6.00 14.20 11 -20 -15 -8.30 12.50 -11 -20 15 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10.00 2 -20 15 8.00 7.20 -2 20 -15 3.40 12.30 2 20 15 9.50 10.50 3 -20 15 162.68 12.60 -3 20 -15 157.58 17.40 3 20 15 193.58 16.20 4 -20 15 74.49 9.20 4 20 15 84.49 13.10 -4 20 -15 64.69 15.20 5 -20 15 215.08 14.30 -5 20 -15 213.98 19.50 5 20 15 214.08 17.80 6 -20 15 11.10 8.50 6 20 15 5.40 10.70 -6 20 -15 31.30 14.20 7 -20 15 0.30 8.70 7 20 15 -5.50 10.50 -7 20 -15 -3.20 14.10 8 -20 15 -1.20 9.30 -8 20 -15 22.40 15.10 8 20 15 4.50 10.90 9 -20 15 95.99 15.10 9 -20 15 96.89 12.40 -9 20 -15 62.89 17.20 9 20 15 84.29 14.50 10 -20 15 11.40 11.20 10 -20 15 4.10 13.10 10 20 15 20.00 12.10 -10 20 -15 40.70 17.00 -11 -21 15 -3.70 15.80 11 -21 -15 11.20 14.10 11 21 -15 34.80 15.30 -10 -21 15 30.10 16.90 10 -21 -15 60.59 15.30 10 21 -15 33.00 15.20 9 -21 -15 57.59 14.90 -9 -21 15 59.29 17.80 9 21 -15 81.19 16.40 -9 21 15 90.89 14.20 8 -21 -15 21.00 13.00 -8 -21 15 27.60 16.30 8 21 -15 19.10 13.50 -8 21 15 29.90 12.20 -7 -21 15 -0.20 14.40 7 -21 -15 31.70 12.90 7 21 -15 27.40 12.60 -7 21 15 25.40 12.60 6 -21 -15 35.90 12.20 -6 -21 15 -19.10 14.40 6 21 -15 29.40 12.90 -6 21 15 31.30 12.40 -5 -21 15 476.75 27.20 5 -21 -15 463.65 23.30 5 21 -15 473.75 22.80 -5 21 15 521.45 23.30 4 -21 -15 19.90 11.20 -4 -21 15 27.50 15.20 -4 21 15 41.10 12.40 4 21 -15 33.60 12.30 3 -21 -15 12.00 10.50 -3 -21 15 -11.90 13.70 3 21 -15 4.70 10.40 -3 21 15 23.40 11.50 -2 -21 15 -4.20 13.20 2 -21 -15 5.60 10.00 -2 21 15 34.50 11.10 2 21 -15 6.60 10.30 -1 -21 15 69.39 15.50 -1 21 15 61.59 12.70 1 21 -15 60.79 11.90 0 21 15 23.90 11.20 1 -21 15 86.09 9.20 -1 21 -15 107.99 16.60 1 21 15 116.09 14.60 2 -21 15 2.50 7.60 2 21 15 11.30 10.90 -2 21 -15 2.10 13.60 3 -21 15 235.38 14.30 -3 21 -15 219.58 19.80 3 21 15 236.18 18.80 4 -21 15 6.40 8.40 4 21 15 26.70 11.60 -4 21 -15 13.80 14.10 5 -21 15 -8.10 8.20 5 21 15 -7.90 11.00 -5 21 -15 -0.80 14.00 6 -21 15 -0.40 9.30 -6 21 -15 16.80 14.90 6 21 15 7.70 11.40 7 -21 15 67.79 11.00 -7 21 -15 87.39 17.50 7 21 15 60.69 13.40 8 -21 15 26.80 10.60 -8 21 -15 7.30 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-6 -1 -22 229.48 17.60 -6 1 -22 221.88 17.30 -7 -1 -22 27.10 11.60 -7 1 -22 38.00 11.70 -8 -1 -22 64.29 13.60 9 -1 22 4.80 11.30 10 -1 22 -10.80 11.60 10 1 22 3.10 11.60 11 -1 22 3.50 12.70 11 -1 22 -13.40 10.20 11 1 22 -6.80 10.80 11 1 22 -1.60 11.60 12 -1 22 240.48 20.60 12 -1 22 271.17 20.10 12 1 22 240.48 20.00 12 1 22 246.48 19.50 -15 -2 22 18.40 13.80 -15 2 22 31.40 13.60 14 -2 -22 184.38 17.60 -14 -2 22 159.08 17.80 -14 2 22 182.08 17.70 -13 -2 22 66.99 13.80 13 -2 -22 55.89 13.80 -13 2 22 47.10 13.80 12 -2 -22 -18.80 10.70 -12 -2 22 -0.60 11.10 -12 2 22 15.40 11.50 11 -2 -22 22.00 11.70 -11 -2 22 18.10 11.60 -11 2 22 45.20 12.20 -10 -2 22 515.75 23.20 10 -2 -22 472.95 22.10 -10 2 22 526.35 23.60 10 2 -22 464.75 21.50 9 -2 -22 9.10 10.40 -9 -2 22 13.30 10.20 9 2 -22 7.40 9.80 -9 2 22 20.60 10.90 8 -2 -22 85.39 12.30 -8 -2 22 66.89 11.40 8 2 -22 82.09 11.70 -8 2 22 72.59 11.40 7 -2 -22 113.49 13.30 -7 -2 22 75.59 11.40 -7 2 22 99.89 12.10 7 2 -22 102.49 12.20 6 -2 -22 43.20 10.90 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9.80 10 -2 22 -0.70 11.80 10 2 22 0.10 11.70 11 -2 22 30.60 13.60 11 -2 22 12.10 11.30 11 2 22 22.00 12.80 12 -2 22 21.20 13.80 12 -2 22 10.20 11.80 12 2 22 -3.30 11.70 12 2 22 7.70 12.50 -15 -3 22 55.09 14.80 15 -3 -22 50.39 15.50 -15 3 22 57.19 15.20 14 -3 -22 126.39 16.80 -14 -3 22 96.09 15.80 -14 3 22 135.69 16.90 13 -3 -22 10.70 12.40 -13 3 22 16.30 12.40 12 -3 -22 0.60 11.80 -12 3 22 7.70 11.90 11 -3 -22 123.79 15.30 -11 3 22 148.79 15.80 10 -3 -22 53.89 12.10 -10 3 22 13.00 11.50 9 -3 -22 59.99 12.00 -9 3 22 33.80 11.60 9 3 -22 48.10 11.00 8 -3 -22 34.30 11.10 -8 -3 22 22.70 10.00 8 3 -22 9.80 9.60 -8 3 22 5.30 9.90 -7 -3 22 15.90 9.70 7 -3 -22 34.90 10.50 7 3 -22 38.50 10.00 -7 3 22 17.30 9.60 -6 -3 22 129.19 12.90 6 -3 -22 152.78 14.20 -6 3 22 99.79 12.70 6 3 -22 129.59 12.90 5 -3 -22 28.20 10.30 -5 -3 22 2.60 8.60 5 3 -22 15.30 9.30 -5 3 22 12.20 8.90 4 -3 -22 23.90 10.10 -4 -3 22 41.60 9.90 4 3 -22 49.80 9.80 -4 3 22 39.10 9.40 3 -3 -22 344.07 18.40 -3 -3 22 299.17 16.80 -3 3 22 348.07 17.50 3 3 -22 338.87 17.60 -2 -3 22 185.08 13.80 2 -3 -22 168.78 14.40 2 3 -22 169.08 13.20 -2 3 22 192.58 15.10 -1 -3 22 9.90 7.80 1 -3 -22 6.80 8.60 -1 3 22 1.50 8.10 1 3 -22 -3.70 8.30 0 -3 -22 273.87 17.20 0 -3 22 276.67 15.40 0 3 22 334.17 16.30 0 3 -22 289.97 16.60 1 -3 22 151.18 11.90 -1 -3 -22 120.39 12.80 1 3 22 170.48 13.10 -1 3 -22 176.28 14.10 -2 -3 -22 12.40 9.10 2 -3 22 9.70 7.60 -2 3 -22 14.40 9.30 2 3 22 8.60 8.20 -3 -3 -22 13.40 9.60 -3 3 -22 15.20 9.40 3 3 22 17.80 8.00 -4 -3 -22 203.48 15.70 -4 3 -22 202.18 15.60 -5 -3 -22 16.30 10.20 -5 3 -22 18.40 10.00 -6 -3 -22 5.10 10.00 -6 3 -22 6.00 10.30 -7 -3 -22 89.49 14.10 8 -3 22 53.99 12.50 -8 -3 -22 39.60 12.80 9 -3 22 70.89 13.70 10 -3 22 1.60 12.00 10 -3 22 -6.00 9.90 10 3 22 3.20 11.80 11 -3 22 2.20 10.60 11 -3 22 26.30 13.60 11 3 22 -6.60 12.00 12 -3 22 180.98 15.90 12 -3 22 172.78 18.60 12 3 22 204.38 17.50 -12 3 -22 190.58 20.40 12 3 22 140.29 17.60 15 -4 -22 33.60 14.70 -15 4 22 51.59 15.20 14 -4 -22 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126.79 16.70 -11 9 22 93.09 15.40 10 -9 -22 19.60 12.80 10 9 -22 7.40 12.70 -10 9 22 45.60 13.40 9 -9 -22 -0.10 11.60 9 9 -22 -14.60 11.70 -9 9 22 20.90 11.90 8 -9 -22 87.59 13.90 -8 9 22 104.69 14.50 8 9 -22 62.49 13.00 7 -9 -22 31.60 11.70 7 9 -22 16.90 11.30 -7 9 22 31.10 11.40 6 -9 -22 191.88 15.90 6 9 -22 167.98 15.80 -6 9 22 199.08 16.20 5 -9 -22 33.50 11.50 -5 9 22 40.40 11.30 5 9 -22 59.99 12.30 4 -9 -22 87.09 13.20 -4 9 22 119.59 13.40 4 9 -22 113.89 13.20 3 -9 -22 188.68 15.90 3 9 -22 199.38 15.10 -3 9 22 198.18 15.40 3 9 -22 201.98 14.80 2 -9 -22 -6.70 9.40 2 9 -22 4.60 8.30 -2 9 22 -3.90 9.00 2 9 -22 -3.10 8.80 1 -9 -22 101.59 13.50 1 9 -22 108.99 11.70 1 9 -22 98.49 11.60 -1 9 22 97.99 12.70 0 -9 -22 48.60 10.80 0 9 22 30.70 10.20 0 9 -22 33.60 9.50 -1 -9 -22 191.08 15.80 1 9 22 231.08 16.40 -1 9 -22 216.38 15.80 -2 -9 -22 246.38 17.90 2 9 22 256.07 17.00 -2 9 -22 231.18 16.60 -3 -9 -22 26.70 11.10 3 9 22 31.70 9.80 -3 9 -22 16.50 9.80 -3 9 -22 26.90 11.30 -4 -9 -22 109.19 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12.00 -7 11 -22 14.20 13.70 8 -11 22 28.30 9.20 8 -11 22 0.90 12.50 -8 -11 -22 9.50 13.10 -8 11 -22 32.40 14.80 -9 -11 -22 -8.00 12.80 9 -11 22 25.90 9.90 9 -11 22 34.30 13.90 -9 11 -22 28.00 15.30 10 -11 22 -9.20 10.00 10 -11 22 1.70 14.20 -10 -11 -22 -20.50 12.90 -10 11 -22 13.20 16.20 13 -12 -22 23.80 15.20 -13 12 22 -7.60 14.50 13 12 -22 15.90 15.10 12 -12 -22 32.10 15.30 -12 12 22 17.80 14.20 12 12 -22 25.60 14.80 11 -12 -22 98.79 16.80 11 12 -22 137.29 17.60 -11 12 22 150.98 18.60 10 -12 -22 91.69 15.90 -10 12 22 113.89 16.40 10 12 -22 120.79 16.80 9 -12 -22 95.89 15.50 9 12 -22 103.29 15.90 -9 12 22 97.89 15.70 8 -12 -22 17.70 12.50 8 12 -22 -12.90 12.10 -8 12 22 14.00 12.20 7 -12 -22 29.70 12.50 7 12 -22 31.10 12.40 -7 12 22 17.50 12.20 6 -12 -22 5.80 11.30 6 12 -22 -7.40 11.00 -6 12 22 10.90 11.40 5 -12 -22 152.78 16.20 5 12 -22 164.78 15.80 -5 12 22 165.38 16.10 4 -12 -22 120.39 14.80 -4 12 22 132.59 14.40 4 12 -22 100.29 13.60 3 -12 -22 -3.60 10.00 3 12 -22 -19.10 10.00 -3 12 22 3.90 10.20 2 -12 -22 81.59 13.20 -2 12 22 72.39 12.20 2 12 -22 62.39 12.20 1 -12 -22 6.70 10.60 1 12 -22 -2.70 9.50 -1 12 22 25.80 10.90 0 -12 -22 43.90 12.30 0 12 22 67.49 12.60 0 12 -22 43.70 12.30 -1 -12 -22 7.60 10.60 -1 12 -22 -8.20 11.10 1 12 22 7.50 10.20 -2 -12 -22 3.40 10.50 2 12 22 6.50 10.50 -2 12 -22 2.60 11.30 -3 -12 -22 161.48 16.10 3 -12 22 143.59 14.00 3 12 22 167.38 15.50 -3 12 -22 144.89 15.80 4 -12 22 93.19 12.90 4 -12 22 64.39 6.60 -4 -12 -22 69.89 13.50 -4 12 -22 71.49 14.00 4 12 22 75.19 12.40 -5 -12 -22 72.99 13.90 5 -12 22 85.29 7.90 5 -12 22 71.09 13.40 5 12 22 79.69 12.40 -5 12 -22 92.79 15.20 6 -12 22 15.60 7.50 -6 -12 -22 24.00 12.80 6 -12 22 25.20 12.10 -6 12 -22 44.60 14.40 6 12 22 29.70 10.90 -7 -12 -22 20.50 13.50 7 -12 22 44.30 8.80 7 -12 22 31.30 13.20 -7 12 -22 41.60 15.00 -8 -12 -22 46.00 14.60 8 -12 22 89.29 10.80 8 -12 22 76.69 14.50 -8 12 -22 101.39 17.40 9 -12 22 41.70 15.00 9 -12 22 55.29 10.80 -9 -12 -22 -8.10 13.40 -9 12 -22 32.40 15.90 12 -13 -22 2.70 14.00 12 13 -22 24.60 14.60 -12 13 22 32.30 15.10 11 -13 -22 50.69 15.50 -11 13 22 36.90 14.50 11 13 -22 30.20 14.80 10 -13 -22 22.50 13.40 -10 13 22 47.20 14.70 10 13 -22 55.69 14.80 9 -13 -22 2.40 13.00 -9 13 22 11.90 13.20 9 13 -22 -19.90 12.00 8 -13 -22 49.00 14.00 -8 13 22 46.20 13.90 8 13 -22 12.90 12.70 7 -13 -22 82.99 14.80 7 13 -22 131.09 15.80 -7 13 22 116.79 15.90 6 -13 -22 151.88 16.70 -6 13 22 174.38 16.70 6 13 -22 113.59 15.10 5 -13 -22 219.08 18.20 5 13 -22 192.38 17.10 -5 13 22 222.18 17.80 4 -13 -22 9.40 11.60 4 13 -22 6.00 10.70 -4 13 22 18.20 11.50 3 -13 -22 15.70 11.30 -3 13 22 17.70 10.60 3 13 -22 8.90 11.20 2 -13 -22 42.30 12.30 -2 13 22 38.10 11.40 2 13 -22 26.20 11.60 1 -13 -22 277.57 20.00 1 13 -22 245.28 17.30 -1 13 22 264.17 18.80 0 -13 -22 154.18 15.60 0 13 -22 153.18 15.70 0 13 22 164.18 15.90 -1 -13 -22 7.30 10.90 1 13 22 45.30 11.80 -1 13 -22 10.20 12.20 -2 -13 -22 -12.40 10.50 2 -13 22 22.20 10.70 -2 13 -22 -5.10 11.30 2 13 22 -1.50 10.60 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10.20 11.50 7 -14 22 34.80 13.80 7 -14 22 12.30 8.60 -7 -14 -22 -4.30 12.70 -7 14 -22 39.70 16.20 8 -14 22 36.20 9.80 8 -14 22 33.00 14.70 -8 14 -22 39.20 16.10 11 -15 -22 39.70 15.80 11 15 -22 78.29 17.40 -11 15 22 51.49 15.70 10 -15 -22 13.40 14.10 10 15 -22 17.60 13.80 -10 15 22 1.20 13.70 9 -15 -22 38.50 14.90 -9 15 22 59.49 15.30 9 15 -22 38.00 14.90 8 -15 -22 6.90 13.40 -8 15 22 -1.30 12.80 8 15 -22 12.40 13.10 7 -15 -22 34.60 14.20 -7 15 22 29.80 13.40 7 15 -22 30.40 13.70 6 -15 -22 37.10 13.50 6 15 -22 33.20 13.50 -6 15 22 16.80 12.70 5 -15 -22 123.79 15.60 -5 15 22 167.08 16.90 5 15 -22 142.89 15.90 4 -15 -22 13.90 12.50 4 15 -22 29.10 12.50 -4 15 22 17.80 12.00 -3 -15 22 -8.00 12.60 3 -15 -22 18.50 12.30 3 15 -22 -4.60 10.90 -3 15 22 8.00 12.00 -2 -15 22 82.79 15.30 2 -15 -22 84.39 14.60 2 15 -22 88.59 13.50 -2 15 22 98.89 14.70 1 -15 -22 355.36 22.20 -1 15 22 404.56 22.00 0 -15 -22 44.40 13.20 0 15 22 72.49 14.30 0 15 -22 64.49 14.50 -1 -15 -22 -8.90 10.90 1 15 22 27.90 12.20 -1 15 -22 -2.20 12.50 -2 -15 -22 46.30 12.90 2 15 22 71.79 13.60 -2 15 -22 34.80 14.10 -3 -15 -22 5.90 11.40 3 -15 22 11.00 5.30 3 15 22 -0.70 10.80 -3 15 -22 2.00 13.60 -4 -15 -22 101.99 15.30 4 -15 22 87.89 7.70 4 15 22 105.59 14.50 -4 15 -22 104.39 16.90 -5 -15 -22 69.19 14.30 5 -15 22 43.50 13.00 5 -15 22 68.39 8.10 -5 15 -22 58.19 15.90 5 15 22 92.09 14.40 6 -15 22 2.10 7.40 -6 -15 -22 -17.30 11.90 6 -15 22 -3.80 12.60 -6 15 -22 4.20 15.20 6 15 22 -23.80 10.40 7 -15 22 53.09 14.60 7 -15 22 52.89 9.30 -7 15 -22 62.89 16.80 8 -15 22 -9.40 9.00 8 -15 22 3.60 14.00 -8 15 -22 20.50 16.40 11 -16 -22 25.80 15.60 -11 16 22 11.30 14.00 11 16 -22 11.50 16.00 10 -16 -22 90.29 16.90 10 16 -22 67.49 16.30 -10 16 22 76.29 16.40 9 -16 -22 70.29 16.50 9 16 -22 60.19 15.60 -9 16 22 52.29 14.70 8 -16 -22 107.89 17.00 8 16 -22 70.99 15.40 -8 16 22 120.89 17.10 7 -16 -22 65.49 15.40 7 16 -22 78.99 15.50 -7 16 22 79.79 15.20 6 -16 -22 27.30 13.70 6 16 -22 23.20 13.10 -6 16 22 45.80 13.80 5 -16 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10 17 -22 9.70 15.40 9 -17 -22 39.90 15.90 -9 17 22 26.70 15.10 9 17 -22 32.80 15.40 8 -17 -22 33.70 15.30 8 17 -22 48.10 15.30 -8 17 22 47.60 14.90 7 -17 -22 -3.80 13.70 7 17 -22 33.10 14.70 -7 17 22 38.10 14.80 6 -17 -22 14.40 13.40 6 17 -22 -15.90 12.60 -6 17 22 -4.70 13.40 5 -17 -22 62.79 14.80 -5 -17 22 53.09 17.50 -5 17 22 32.10 14.20 5 17 -22 38.50 13.40 4 -17 -22 110.49 16.20 -4 -17 22 119.29 18.10 4 17 -22 110.99 15.10 -4 17 22 69.49 15.20 -3 -17 22 39.20 15.60 3 -17 -22 44.50 13.30 3 17 -22 60.29 13.30 -3 17 22 57.59 14.40 -2 -17 22 53.49 16.10 2 -17 -22 59.09 13.90 -2 17 22 64.19 14.20 -1 -17 22 120.79 17.20 1 -17 -22 98.29 15.40 -1 17 22 146.69 16.80 0 -17 -22 33.10 12.80 0 17 22 40.20 13.50 0 17 -22 12.90 14.40 -1 -17 -22 21.70 12.60 1 17 22 -2.40 12.30 -1 17 -22 -25.90 13.10 -2 -17 -22 71.79 14.20 -2 17 -22 81.39 16.40 2 17 22 65.89 14.30 3 -17 22 4.00 6.00 -3 -17 -22 13.60 11.90 -3 17 -22 11.70 15.20 3 17 22 23.50 12.90 4 -17 22 -1.00 6.60 -4 -17 -22 6.20 12.40 4 17 22 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12 23 103.19 17.90 11 -12 -23 83.69 16.40 11 12 -23 99.39 17.50 -11 12 23 116.99 17.30 10 -12 -23 2.90 14.10 10 12 -23 31.50 14.70 -10 12 23 11.40 14.60 9 -12 -23 29.80 13.80 -9 12 23 77.59 15.70 9 12 -23 89.79 15.80 8 -12 -23 14.10 13.10 8 12 -23 -11.90 12.80 -8 12 23 25.40 13.30 7 -12 -23 4.30 12.20 7 12 -23 8.00 12.50 -7 12 23 31.30 13.20 6 -12 -23 16.80 12.10 -6 12 23 10.80 12.20 6 12 -23 17.60 12.50 5 -12 -23 4.80 11.60 -5 12 23 -2.20 11.00 5 12 -23 0.90 12.10 4 -12 -23 24.80 12.50 -4 12 23 62.99 12.80 4 12 -23 47.10 12.80 3 -12 -23 60.09 13.40 -3 12 23 62.09 12.90 3 12 -23 75.69 13.50 2 -12 -23 63.29 13.20 -2 12 23 43.30 12.00 2 12 -23 39.80 11.80 1 -12 -23 45.60 12.90 1 12 -23 25.70 11.30 -1 12 23 24.20 11.60 0 -12 -23 152.98 15.60 0 12 23 193.18 17.20 -1 -12 -23 288.67 20.10 1 12 23 274.67 20.10 -2 -12 -23 144.29 16.10 2 12 23 207.48 17.40 -2 12 -23 141.99 17.50 3 -12 23 11.50 10.90 -3 -12 -23 5.90 11.70 -3 12 -23 5.80 12.00 3 12 23 3.40 10.50 -4 -12 -23 50.99 13.40 4 -12 23 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21.30 12.50 0 -15 -23 19.00 12.70 0 15 -23 18.00 14.00 0 15 23 -11.40 12.00 -1 -15 -23 2.40 11.80 1 15 23 -8.40 11.90 -1 15 -23 2.50 13.40 -2 -15 -23 67.69 14.10 -2 15 -23 67.19 15.70 2 15 23 58.39 13.60 -3 -15 -23 0.70 11.80 -3 15 -23 1.30 14.00 3 15 23 -7.90 11.60 -4 -15 -23 58.89 13.70 4 -15 23 60.59 7.40 -4 15 -23 69.39 16.90 4 15 23 95.49 14.70 5 -15 23 33.50 13.70 -5 -15 -23 29.80 13.70 5 -15 23 44.50 7.80 -5 15 -23 27.30 15.30 5 15 23 37.90 13.00 -6 -15 -23 4.50 13.60 6 -15 23 -6.80 7.60 6 -15 23 -8.10 12.90 -6 15 -23 7.40 16.00 6 15 23 -3.00 12.20 7 -15 23 48.80 15.10 7 -15 23 32.90 9.00 -7 15 -23 54.69 17.40 10 -16 -23 18.90 15.40 -10 16 23 16.80 14.70 10 16 -23 9.40 15.40 9 -16 -23 18.70 15.30 -9 16 23 28.10 14.90 9 16 -23 27.20 15.20 8 -16 -23 27.00 15.10 -8 16 23 29.70 14.40 8 16 -23 20.20 14.80 7 -16 -23 -0.50 13.80 -7 16 23 9.80 13.10 7 16 -23 17.10 14.10 6 -16 -23 42.00 14.70 -6 16 23 76.39 15.40 6 16 -23 32.80 14.70 5 -16 -23 4.00 13.30 5 16 -23 -7.30 12.40 -5 16 23 12.20 13.60 4 -16 -23 101.49 15.90 -4 16 23 98.69 16.20 4 16 -23 107.49 14.90 3 -16 -23 41.20 13.80 3 16 -23 38.50 13.10 -3 16 23 54.09 14.10 2 -16 -23 25.20 13.30 -2 16 23 0.00 12.80 1 -16 -23 53.19 14.00 -1 -16 23 53.39 15.50 -1 16 23 28.20 13.70 0 -16 -23 66.59 14.50 0 16 23 81.59 14.90 0 16 -23 58.89 16.00 -1 -16 -23 15.00 12.00 -1 16 -23 6.40 13.90 1 16 23 9.80 13.00 -2 -16 -23 28.80 12.70 2 16 23 32.60 13.10 -2 16 -23 14.60 14.50 -3 -16 -23 67.59 13.70 3 16 23 74.29 14.30 -3 16 -23 49.60 16.00 -4 -16 -23 17.00 13.10 4 -16 23 4.50 6.50 4 16 23 11.90 12.20 -4 16 -23 15.90 15.60 -5 -16 -23 11.30 13.30 5 -16 23 32.70 7.70 5 16 23 7.20 12.90 -5 16 -23 20.40 15.80 6 -16 23 99.29 9.70 6 16 23 74.69 15.00 -6 16 -23 87.59 18.40 9 -17 -23 49.00 16.80 9 17 -23 14.70 15.90 -9 17 23 34.20 15.40 8 -17 -23 81.99 16.80 8 17 -23 85.19 17.30 -8 17 23 120.09 17.50 7 -17 -23 38.00 15.50 7 17 -23 47.50 15.10 -7 17 23 57.19 15.70 6 -17 -23 6.70 13.50 -6 17 23 -7.50 13.80 6 17 -23 -36.30 12.70 5 -17 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0 28 1.00 13.40 -7 0 28 21.70 13.50 7 0 -28 8.20 13.20 6 0 -28 288.07 21.00 -6 0 28 248.78 20.60 5 0 -28 -6.50 12.10 -5 0 28 -3.00 12.30 -4 0 28 14.20 12.00 4 0 -28 -5.40 11.90 3 0 -28 -8.10 11.70 -3 0 28 -9.30 11.30 2 0 -28 240.68 19.00 -2 0 28 244.38 19.50 -1 0 28 -0.70 11.30 1 0 -28 -1.50 12.20 0 0 28 230.58 17.90 0 0 -28 215.48 18.80 -1 0 -28 -1.00 12.80 -2 0 -28 -3.40 13.30 -3 0 -28 -31.60 12.20 -4 0 -28 153.88 18.00 -5 0 -28 -11.00 13.50 -6 0 -28 15.80 14.60 10 -1 -28 286.67 22.90 -10 -1 28 251.07 21.70 -10 1 28 232.08 21.80 -9 -1 28 10.40 13.60 9 -1 -28 23.10 14.80 9 1 -28 4.30 13.40 -9 1 28 -2.90 13.90 8 -1 -28 1.60 13.90 -8 -1 28 -16.40 12.00 -8 1 28 -0.10 13.40 8 1 -28 -0.70 12.70 -7 -1 28 28.40 13.70 7 -1 -28 30.20 14.10 7 1 -28 46.80 14.20 -7 1 28 29.70 13.70 -6 -1 28 54.99 14.60 6 -1 -28 38.40 13.90 -6 1 28 40.40 14.10 6 1 -28 74.69 14.50 -5 -1 28 2.00 12.90 5 -1 -28 18.20 13.10 -5 1 28 -5.30 12.40 5 1 -28 4.10 12.60 -4 -1 28 49.90 13.20 4 -1 -28 22.60 13.60 -4 1 28 41.10 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12.70 13.10 5 -2 -28 5.10 13.10 -5 2 28 -13.60 12.40 5 2 -28 0.20 12.30 -4 -2 28 18.40 12.80 4 -2 -28 7.10 12.60 -4 2 28 -21.80 11.50 4 2 -28 -22.60 11.30 3 -2 -28 53.09 14.10 -3 -2 28 33.20 12.90 -3 2 28 50.49 13.30 3 2 -28 37.30 12.90 2 -2 -28 82.79 15.30 -2 -2 28 71.89 14.00 2 2 -28 88.49 14.90 -2 2 28 87.49 15.00 -1 -2 28 25.50 11.80 1 -2 -28 29.40 13.40 -1 2 28 55.69 13.20 1 2 -28 26.50 13.10 0 -2 -28 103.09 15.80 0 2 28 100.89 15.00 0 2 -28 94.89 15.30 -1 -2 -28 38.20 14.40 1 2 28 32.90 13.00 -1 2 -28 33.30 13.70 -2 -2 -28 3.30 13.10 -2 2 -28 -11.70 13.20 -3 -2 -28 -4.70 13.60 -3 2 -28 -12.40 12.90 -4 -2 -28 63.09 15.80 -4 2 -28 84.59 16.20 -5 -2 -28 9.10 13.90 -5 2 -28 -3.90 13.50 -6 -2 -28 -10.50 13.90 -6 2 -28 -9.00 14.40 10 -3 -28 190.48 20.30 -10 -3 28 170.78 19.40 -10 3 28 164.48 19.80 -9 -3 28 14.40 14.30 9 -3 -28 31.40 15.20 -9 3 28 2.40 14.30 -8 -3 28 21.90 14.20 8 -3 -28 12.90 14.40 -8 3 28 -8.80 13.20 -7 -3 28 132.79 17.30 7 -3 -28 131.79 17.70 7 3 -28 132.59 15.90 -7 3 28 148.29 17.90 6 -3 -28 81.79 15.60 -6 -3 28 64.29 15.10 -6 3 28 76.39 15.30 6 3 -28 71.39 14.70 -5 -3 28 20.90 12.70 5 -3 -28 31.30 14.00 5 3 -28 17.60 12.80 -5 3 28 73.69 15.00 4 -3 -28 30.00 13.80 -4 -3 28 26.40 12.80 4 3 -28 50.29 13.60 -4 3 28 25.00 13.10 3 -3 -28 19.40 13.40 -3 -3 28 -1.00 12.10 -3 3 28 6.50 12.30 3 3 -28 6.50 12.30 2 -3 -28 60.09 14.50 -2 -3 28 53.69 13.20 2 3 -28 73.39 14.70 -2 3 28 70.89 14.20 -1 -3 28 2.90 11.20 1 -3 -28 -8.50 12.30 -1 3 28 -15.30 11.80 1 3 -28 20.00 12.50 0 -3 -28 1.80 13.10 0 3 28 -2.50 11.90 0 3 -28 24.70 13.20 -1 -3 -28 67.29 15.10 -1 3 -28 36.50 13.70 1 3 28 41.40 13.30 -2 -3 -28 66.39 15.40 -2 3 -28 58.49 14.90 -3 -3 -28 -22.70 13.20 -3 3 -28 -7.50 12.70 -4 -3 -28 83.49 16.20 -4 3 -28 80.69 15.70 -5 -3 -28 59.49 15.80 -5 3 -28 101.19 17.00 -6 -3 -28 9.10 14.50 -6 3 -28 7.20 14.60 -10 -4 28 15.80 14.40 10 -4 -28 25.10 15.30 -10 4 28 16.10 15.20 9 -4 -28 78.39 16.60 -9 -4 28 78.19 16.80 -9 4 28 68.09 16.60 8 -4 -28 1.80 14.10 -8 -4 28 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109.19 17.50 -6 -7 28 -1.80 12.60 6 -7 -28 -17.50 13.50 -6 7 28 -4.10 13.80 -5 -7 28 31.70 13.80 5 -7 -28 28.10 14.30 -5 7 28 39.20 14.90 4 -7 -28 17.90 14.40 -4 -7 28 -1.60 12.10 -4 7 28 -0.20 12.70 -3 -7 28 13.00 12.50 3 -7 -28 33.60 13.90 3 7 -28 22.50 12.50 -3 7 28 41.90 14.30 2 -7 -28 33.90 14.10 -2 -7 28 33.60 12.70 -2 7 28 54.59 14.50 2 7 -28 23.00 13.00 1 -7 -28 5.10 13.30 1 7 -28 -8.10 12.60 -1 7 28 -19.20 12.00 0 -7 -28 15.60 13.40 0 7 28 11.60 12.90 0 7 -28 42.90 13.90 -1 -7 -28 85.89 16.20 1 7 28 125.29 16.10 -1 7 -28 122.29 16.00 -2 -7 -28 -15.60 13.20 2 7 28 15.80 12.50 -2 7 -28 1.20 12.80 -3 -7 -28 -2.30 13.80 -3 7 -28 9.70 13.50 -4 -7 -28 -3.30 14.10 -4 7 -28 -12.00 13.00 -5 -7 -28 144.89 19.60 -9 -8 28 43.30 15.40 9 -8 -28 73.09 17.40 -9 8 28 74.69 17.20 8 -8 -28 67.59 16.40 -8 -8 28 46.00 15.20 -8 8 28 44.10 16.60 7 -8 -28 12.30 14.90 -7 -8 28 -1.80 13.40 -7 8 28 4.70 14.10 -6 -8 28 20.90 13.50 6 -8 -28 -4.60 13.70 -6 8 28 -16.90 13.50 -5 -8 28 15.90 13.30 5 -8 -28 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