# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2016 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mm469_5 _database_code_depnum_ccdc_archive 'CCDC 1454168' _audit_update_record ; 2016-02-18 deposited with the CCDC. 2016-08-08 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H79 Gd2 K N4 Si8' _chemical_formula_weight 1086.30 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' Gd Gd -0.1653 3.9035 '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 14.1700(7) _cell_length_b 14.2848(7) _cell_length_c 25.4039(12) _cell_angle_alpha 90 _cell_angle_beta 95.518(2) _cell_angle_gamma 90 _cell_volume 5118.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9831 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 30.42 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas n/a _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_F_000 2208 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.203 _exptl_crystal_size_min 0.139 _exptl_absorpt_coefficient_mu 2.861 _shelx_estimated_absorpt_T_min 0.491 _shelx_estimated_absorpt_T_max 0.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.531793 _exptl_absorpt_correction_T_max 0.746071 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25502 _diffrn_reflns_av_unetI/netI 0.0345 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.584 _diffrn_reflns_theta_max 30.595 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 15195 _reflns_number_gt 12026 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _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 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-03 (Sheldrick, 2003)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _refine_special_details ; Refined as a 2-component twin. ; _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^)+(0.0214P)^2^+6.7851P] 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 15195 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.009 _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 Gd1 Gd 0.16979(2) 0.23108(2) 1.06849(2) 0.02648(4) Uani 1 1 d . . . . . Gd2 Gd 0.30382(2) 0.22414(2) 0.93310(2) 0.02469(4) Uani 1 1 d . . . . . K1 K 0.43854(7) 0.21446(7) 0.80608(3) 0.0518(2) Uani 1 1 d . . . . . Si1 Si 0.31754(8) 0.20814(9) 1.19683(4) 0.0429(3) Uani 1 1 d . . . . . Si2 Si 0.17731(9) 0.06539(7) 1.15634(4) 0.0431(3) Uani 1 1 d . . . . . Si3 Si 0.04886(7) 0.38973(7) 1.13030(4) 0.0323(2) Uani 1 1 d . . . . . Si4 Si -0.08192(7) 0.28897(8) 1.05207(4) 0.0401(2) Uani 1 1 d . . . . . Si5 Si 0.54484(7) 0.25047(7) 0.93436(4) 0.0351(2) Uani 1 1 d . . . . . Si6 Si 0.44491(7) 0.42083(7) 0.89335(4) 0.0317(2) Uani 1 1 d . . . . . Si7 Si 0.29215(8) 0.01744(7) 0.84729(4) 0.0382(2) Uani 1 1 d . . . . . Si8 Si 0.18974(8) 0.19020(8) 0.81076(4) 0.0371(2) Uani 1 1 d . . . . . N1 N 0.2310(2) 0.1709(2) 1.14976(11) 0.0325(6) Uani 1 1 d . . . . . N2 N 0.0295(2) 0.3057(2) 1.08328(11) 0.0315(6) Uani 1 1 d . . . . . N3 N 0.44160(19) 0.30399(19) 0.91018(10) 0.0262(5) Uani 1 1 d . . . . . N4 N 0.2731(2) 0.13514(19) 0.85356(10) 0.0296(6) Uani 1 1 d . . . . . C1 C 0.3327(3) 0.2654(4) 1.03296(15) 0.0555(13) Uani 1 1 d . . . . . H1A H 0.3869 0.2879 1.0541 0.067 Uiso 1 1 calc R U . . . C2 C 0.3260(3) 0.1687(4) 1.02838(16) 0.0594(14) Uani 1 1 d . . . . . H2A H 0.3802 0.1345 1.0423 0.071 Uiso 1 1 calc R U . . . C3 C 0.2503(4) 0.1154(3) 1.00601(16) 0.0559(14) Uani 1 1 d . . . . . H3A H 0.2569 0.0496 1.0102 0.067 Uiso 1 1 calc R U . . . C4 C 0.1641(4) 0.1460(4) 0.97771(16) 0.0580(14) Uani 1 1 d . . . . . H4A H 0.1194 0.0986 0.9669 0.070 Uiso 1 1 calc R U . . . C5 C 0.1374(3) 0.2400(4) 0.96377(15) 0.0574(14) Uani 1 1 d . . . . . H5A H 0.0801 0.2472 0.9414 0.069 Uiso 1 1 calc R U . . . C6 C 0.1861(4) 0.3238(3) 0.97929(17) 0.0547(13) Uani 1 1 d . . . . . H6A H 0.1569 0.3802 0.9664 0.066 Uiso 1 1 calc R U . . . C7 C 0.2715(4) 0.3341(3) 1.01111(16) 0.0519(12) Uani 1 1 d . . . . . H7A H 0.2904 0.3968 1.0189 0.062 Uiso 1 1 calc R U . . . C8 C 0.4096(3) 0.2818(4) 1.16913(19) 0.0687(15) Uani 1 1 d . . . . . H8A H 0.4570 0.3010 1.1977 0.103 Uiso 1 1 calc R U . . . H8B H 0.4405 0.2455 1.1429 0.103 Uiso 1 1 calc R U . . . H8C H 0.3797 0.3374 1.1523 0.103 Uiso 1 1 calc R U . . . C9 C 0.3850(4) 0.1105(5) 1.2332(2) 0.089(2) Uani 1 1 d . . . . . H9A H 0.4330 0.1369 1.2593 0.133 Uiso 1 1 calc R U . . . H9B H 0.3410 0.0716 1.2512 0.133 Uiso 1 1 calc R U . . . H9C H 0.4160 0.0720 1.2080 0.133 Uiso 1 1 calc R U . . . C10 C 0.2700(4) 0.2779(4) 1.25084(18) 0.0679(14) Uani 1 1 d . . . . . H10A H 0.3225 0.2973 1.2765 0.102 Uiso 1 1 calc R U . . . H10B H 0.2373 0.3336 1.2357 0.102 Uiso 1 1 calc R U . . . H10C H 0.2254 0.2395 1.2686 0.102 Uiso 1 1 calc R U . . . C11 C 0.1287(4) 0.0487(3) 1.22136(16) 0.0567(12) Uani 1 1 d . . . . . H11A H 0.0990 -0.0132 1.2223 0.085 Uiso 1 1 calc R U . . . H11B H 0.1802 0.0533 1.2499 0.085 Uiso 1 1 calc R U . . . H11C H 0.0813 0.0972 1.2261 0.085 Uiso 1 1 calc R U . . . C12 C 0.2530(5) -0.0376(3) 1.1437(2) 0.088(2) Uani 1 1 d . . . . . H12A H 0.2174 -0.0954 1.1482 0.132 Uiso 1 1 calc R U . . . H12B H 0.2712 -0.0345 1.1075 0.132 Uiso 1 1 calc R U . . . H12C H 0.3101 -0.0370 1.1687 0.132 Uiso 1 1 calc R U . . . C13 C 0.0726(4) 0.0555(3) 1.10546(17) 0.0604(13) Uani 1 1 d . . . . . H13A H 0.0415 -0.0051 1.1091 0.091 Uiso 1 1 calc R U . . . H13B H 0.0276 0.1060 1.1107 0.091 Uiso 1 1 calc R U . . . H13C H 0.0940 0.0605 1.0700 0.091 Uiso 1 1 calc R U . . . C14 C 0.0233(3) 0.3471(3) 1.19770(14) 0.0448(9) Uani 1 1 d . . . . . H14A H 0.0354 0.3977 1.2235 0.067 Uiso 1 1 calc R U . . . H14B H -0.0432 0.3277 1.1966 0.067 Uiso 1 1 calc R U . . . H14C H 0.0644 0.2937 1.2080 0.067 Uiso 1 1 calc R U . . . C15 C -0.0207(3) 0.5010(3) 1.11967(19) 0.0550(11) Uani 1 1 d . . . . . H15A H -0.0037 0.5440 1.1492 0.082 Uiso 1 1 calc R U . . . H15B H -0.0060 0.5303 1.0865 0.082 Uiso 1 1 calc R U . . . H15C H -0.0886 0.4870 1.1178 0.082 Uiso 1 1 calc R U . . . C16 C 0.1755(3) 0.4279(3) 1.13360(16) 0.0422(9) Uani 1 1 d . . . . . H16A H 0.1872 0.4764 1.1607 0.063 Uiso 1 1 calc R U . . . H16B H 0.2170 0.3741 1.1426 0.063 Uiso 1 1 calc R U . . . H16C H 0.1889 0.4530 1.0992 0.063 Uiso 1 1 calc R U . . . C17 C -0.1172(4) 0.3820(4) 1.0020(2) 0.0799(18) Uani 1 1 d . . . . . H17A H -0.1812 0.3691 0.9854 0.120 Uiso 1 1 calc R U . . . H17B H -0.1163 0.4432 1.0195 0.120 Uiso 1 1 calc R U . . . H17C H -0.0724 0.3824 0.9749 0.120 Uiso 1 1 calc R U . . . C18 C -0.1737(3) 0.2857(3) 1.10030(17) 0.0491(10) Uani 1 1 d . . . . . H18A H -0.2364 0.2761 1.0812 0.074 Uiso 1 1 calc R U . . . H18B H -0.1597 0.2343 1.1253 0.074 Uiso 1 1 calc R U . . . H18C H -0.1731 0.3451 1.1196 0.074 Uiso 1 1 calc R U . . . C19 C -0.0963(3) 0.1758(4) 1.0149(2) 0.0725(16) Uani 1 1 d . . . . . H19A H -0.1614 0.1709 0.9982 0.109 Uiso 1 1 calc R U . . . H19B H -0.0519 0.1739 0.9877 0.109 Uiso 1 1 calc R U . . . H19C H -0.0833 0.1235 1.0395 0.109 Uiso 1 1 calc R U . . . C20 C 0.5237(3) 0.1210(3) 0.94016(18) 0.0492(10) Uani 1 1 d . . . . . H20A H 0.5827 0.0901 0.9540 0.074 Uiso 1 1 calc R U . . . H20B H 0.4748 0.1100 0.9643 0.074 Uiso 1 1 calc R U . . . H20C H 0.5025 0.0954 0.9052 0.074 Uiso 1 1 calc R U . . . C21 C 0.6421(3) 0.2627(3) 0.8893(2) 0.0602(13) Uani 1 1 d . . . . . H21A H 0.6993 0.2309 0.9050 0.090 Uiso 1 1 calc R U . . . H21B H 0.6217 0.2343 0.8549 0.090 Uiso 1 1 calc R U . . . H21C H 0.6559 0.3292 0.8844 0.090 Uiso 1 1 calc R U . . . C22 C 0.5943(3) 0.2876(3) 1.00175(19) 0.0572(12) Uani 1 1 d . . . . . H22A H 0.6530 0.2531 1.0119 0.086 Uiso 1 1 calc R U . . . H22B H 0.6077 0.3549 1.0017 0.086 Uiso 1 1 calc R U . . . H22C H 0.5481 0.2743 1.0271 0.086 Uiso 1 1 calc R U . . . C23 C 0.4579(4) 0.4354(3) 0.82062(15) 0.0556(12) Uani 1 1 d . . . . . H23A H 0.4596 0.5022 0.8120 0.083 Uiso 1 1 calc R U . . . H23B H 0.5169 0.4056 0.8121 0.083 Uiso 1 1 calc R U . . . H23C H 0.4040 0.4059 0.7999 0.083 Uiso 1 1 calc R U . . . C24 C 0.5464(3) 0.4891(3) 0.92675(17) 0.0482(10) Uani 1 1 d . . . . . H24A H 0.5422 0.5543 0.9147 0.072 Uiso 1 1 calc R U . . . H24B H 0.5438 0.4870 0.9651 0.072 Uiso 1 1 calc R U . . . H24C H 0.6063 0.4619 0.9179 0.072 Uiso 1 1 calc R U . . . C25 C 0.3373(3) 0.4880(3) 0.90712(17) 0.0456(9) Uani 1 1 d . . . . . H25A H 0.3443 0.5535 0.8966 0.068 Uiso 1 1 calc R U . . . H25B H 0.2814 0.4609 0.8870 0.068 Uiso 1 1 calc R U . . . H25C H 0.3295 0.4851 0.9450 0.068 Uiso 1 1 calc R U . . . C26 C 0.3253(3) -0.0447(3) 0.91103(17) 0.0511(10) Uani 1 1 d . . . . . H26A H 0.3349 -0.1114 0.9041 0.077 Uiso 1 1 calc R U . . . H26B H 0.3841 -0.0180 0.9282 0.077 Uiso 1 1 calc R U . . . H26C H 0.2744 -0.0375 0.9342 0.077 Uiso 1 1 calc R U . . . C27 C 0.1887(4) -0.0499(3) 0.81570(19) 0.0662(14) Uani 1 1 d . . . . . H27A H 0.2057 -0.1162 0.8137 0.099 Uiso 1 1 calc R U . . . H27B H 0.1348 -0.0430 0.8369 0.099 Uiso 1 1 calc R U . . . H27C H 0.1713 -0.0257 0.7800 0.099 Uiso 1 1 calc R U . . . C28 C 0.3918(4) -0.0068(3) 0.8053(2) 0.0737(17) Uani 1 1 d . . . . . H28A H 0.4009 -0.0745 0.8025 0.111 Uiso 1 1 calc R U . . . H28B H 0.3762 0.0197 0.7699 0.111 Uiso 1 1 calc R U . . . H28C H 0.4503 0.0220 0.8216 0.111 Uiso 1 1 calc R U . . . C29 C 0.2109(4) 0.1770(4) 0.73939(15) 0.0600(13) Uani 1 1 d . . . . . H29A H 0.1610 0.2099 0.7173 0.090 Uiso 1 1 calc R U . . . H29B H 0.2727 0.2038 0.7336 0.090 Uiso 1 1 calc R U . . . H29C H 0.2099 0.1105 0.7300 0.090 Uiso 1 1 calc R U . . . C30 C 0.0640(3) 0.1563(4) 0.81726(19) 0.0605(13) Uani 1 1 d . . . . . H30A H 0.0219 0.1912 0.7914 0.091 Uiso 1 1 calc R U . . . H30B H 0.0561 0.0890 0.8108 0.091 Uiso 1 1 calc R U . . . H30C H 0.0480 0.1710 0.8530 0.091 Uiso 1 1 calc R U . . . C31 C 0.1949(3) 0.3195(3) 0.82384(16) 0.0458(9) Uani 1 1 d . . . . . H31A H 0.1474 0.3514 0.7995 0.069 Uiso 1 1 calc R U . . . H31B H 0.1817 0.3316 0.8604 0.069 Uiso 1 1 calc R U . . . H31C H 0.2582 0.3431 0.8184 0.069 Uiso 1 1 calc R U . . . 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 0.02760(9) 0.03209(8) 0.02119(7) -0.00093(6) 0.00983(6) -0.00042(7) Gd2 0.02611(8) 0.03095(7) 0.01799(7) -0.00193(6) 0.00713(5) -0.00313(6) K1 0.0593(6) 0.0631(6) 0.0369(5) -0.0209(4) 0.0244(4) -0.0209(5) Si1 0.0361(6) 0.0629(7) 0.0302(5) 0.0114(5) 0.0049(4) 0.0069(5) Si2 0.0627(8) 0.0324(5) 0.0383(6) 0.0061(4) 0.0265(5) 0.0033(5) Si3 0.0343(5) 0.0344(5) 0.0297(5) 0.0004(4) 0.0106(4) 0.0060(4) Si4 0.0278(5) 0.0599(7) 0.0330(5) 0.0050(5) 0.0046(4) -0.0023(5) Si5 0.0257(5) 0.0367(5) 0.0435(6) -0.0035(4) 0.0062(4) 0.0011(4) Si6 0.0361(6) 0.0329(5) 0.0270(5) 0.0012(4) 0.0079(4) -0.0059(4) Si7 0.0500(7) 0.0330(5) 0.0329(5) -0.0090(4) 0.0106(5) -0.0083(4) Si8 0.0407(6) 0.0464(6) 0.0236(5) 0.0002(4) -0.0002(4) -0.0098(5) N1 0.0358(17) 0.0363(15) 0.0273(14) 0.0064(12) 0.0118(12) 0.0058(12) N2 0.0266(15) 0.0401(15) 0.0288(14) -0.0010(12) 0.0072(11) 0.0014(12) N3 0.0246(14) 0.0295(13) 0.0254(13) -0.0014(11) 0.0069(11) -0.0038(11) N4 0.0364(16) 0.0299(14) 0.0228(13) -0.0058(11) 0.0044(11) -0.0080(12) C1 0.038(2) 0.108(4) 0.0215(18) -0.010(2) 0.0103(16) -0.025(3) C2 0.048(3) 0.104(4) 0.029(2) 0.020(2) 0.0175(19) 0.040(3) C3 0.105(4) 0.0273(17) 0.043(2) 0.0071(16) 0.048(3) 0.014(2) C4 0.071(3) 0.072(3) 0.036(2) -0.030(2) 0.032(2) -0.052(3) C5 0.023(2) 0.127(5) 0.0220(18) -0.002(2) 0.0040(14) 0.010(2) C6 0.079(3) 0.051(2) 0.040(2) 0.017(2) 0.035(2) 0.031(2) C7 0.083(3) 0.039(2) 0.040(2) -0.0144(17) 0.038(2) -0.027(2) C8 0.046(3) 0.114(4) 0.044(3) 0.012(3) -0.002(2) -0.030(3) C9 0.058(4) 0.117(5) 0.090(4) 0.050(4) 0.001(3) 0.028(3) C10 0.068(4) 0.101(4) 0.034(2) -0.009(2) 0.000(2) 0.003(3) C11 0.071(3) 0.061(3) 0.042(2) 0.011(2) 0.028(2) -0.004(2) C12 0.130(6) 0.047(3) 0.099(4) 0.014(3) 0.068(4) 0.025(3) C13 0.086(4) 0.052(3) 0.045(2) -0.004(2) 0.017(2) -0.029(2) C14 0.053(3) 0.052(2) 0.0304(19) 0.0005(17) 0.0123(17) 0.0043(19) C15 0.057(3) 0.040(2) 0.070(3) 0.003(2) 0.015(2) 0.015(2) C16 0.042(2) 0.041(2) 0.045(2) -0.0046(17) 0.0088(18) -0.0024(17) C17 0.062(3) 0.114(5) 0.060(3) 0.048(3) -0.015(3) -0.016(3) C18 0.028(2) 0.068(3) 0.053(3) 0.007(2) 0.0087(18) -0.0013(19) C19 0.043(3) 0.106(4) 0.069(3) -0.034(3) 0.005(2) -0.015(3) C20 0.044(2) 0.041(2) 0.063(3) -0.001(2) 0.005(2) 0.0046(18) C21 0.037(2) 0.058(3) 0.090(4) -0.008(3) 0.028(2) 0.003(2) C22 0.046(3) 0.065(3) 0.057(3) -0.005(2) -0.014(2) 0.003(2) C23 0.076(3) 0.058(3) 0.035(2) 0.0104(19) 0.016(2) -0.012(2) C24 0.051(3) 0.041(2) 0.054(3) -0.0017(19) 0.008(2) -0.0114(18) C25 0.051(3) 0.0337(18) 0.053(3) 0.0051(17) 0.0074(19) 0.0012(18) C26 0.062(3) 0.0351(19) 0.055(3) -0.0017(18) 0.003(2) 0.0020(19) C27 0.094(4) 0.046(2) 0.055(3) -0.003(2) -0.015(3) -0.023(2) C28 0.093(4) 0.052(3) 0.085(4) -0.024(3) 0.051(3) -0.002(3) C29 0.086(4) 0.068(3) 0.026(2) 0.001(2) 0.002(2) -0.013(3) C30 0.044(3) 0.082(3) 0.053(3) 0.010(3) -0.009(2) -0.015(2) C31 0.047(2) 0.048(2) 0.042(2) 0.0005(19) 0.0000(18) 0.0061(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 Gd1 N2 2.318(3) . ? Gd1 N1 2.326(3) . ? Gd1 C4 2.601(4) . ? Gd1 C7 2.602(4) . ? Gd1 C1 2.605(4) . ? Gd1 C3 2.626(4) . ? Gd1 C6 2.654(4) . ? Gd1 C5 2.659(4) . ? Gd1 C2 2.677(4) . ? Gd1 C13 3.052(4) . ? Gd1 Si2 3.2477(10) . ? Gd1 Si3 3.3251(10) . ? Gd2 N3 2.381(3) . ? Gd2 N4 2.391(3) . ? Gd2 C2 2.537(4) . ? Gd2 C6 2.561(4) . ? Gd2 C5 2.564(4) . ? Gd2 C3 2.586(4) . ? Gd2 C1 2.598(4) . ? Gd2 C7 2.603(4) . ? Gd2 C4 2.623(4) . ? Gd2 Si8 3.3971(10) . ? Gd2 Si5 3.4330(11) . ? Gd2 K1 3.9064(8) . ? K1 N3 2.934(3) . ? K1 N4 2.962(3) . ? K1 C23 3.186(5) . ? K1 C28 3.228(5) . ? K1 C14 3.230(4) 4_665 ? K1 C21 3.477(6) . ? K1 Si5 3.4942(15) . ? K1 C29 3.538(5) . ? K1 Si8 3.5558(15) . ? K1 Si6 3.6844(13) . ? K1 Si7 3.7065(14) . ? Si1 N1 1.713(3) . ? Si1 C8 1.865(5) . ? Si1 C10 1.873(5) . ? Si1 C9 1.883(5) . ? Si2 N1 1.703(3) . ? Si2 C11 1.865(4) . ? Si2 C12 1.866(5) . ? Si2 C13 1.877(5) . ? Si3 N2 1.697(3) . ? Si3 C16 1.870(4) . ? Si3 C15 1.876(4) . ? Si3 C14 1.885(4) . ? Si4 N2 1.715(3) . ? Si4 C18 1.871(4) . ? Si4 C19 1.873(5) . ? Si4 C17 1.874(5) . ? Si5 N3 1.711(3) . ? Si5 C22 1.863(5) . ? Si5 C20 1.882(4) . ? Si5 C21 1.883(5) . ? Si6 N3 1.725(3) . ? Si6 C25 1.864(4) . ? Si6 C24 1.872(4) . ? Si6 C23 1.886(4) . ? Si7 N4 1.713(3) . ? Si7 C26 1.867(4) . ? Si7 C27 1.869(4) . ? Si7 C28 1.883(5) . ? Si8 N4 1.718(3) . ? Si8 C30 1.869(4) . ? Si8 C29 1.875(4) . ? Si8 C31 1.877(4) . ? C1 C2 1.389(7) . ? C1 C7 1.389(7) . ? C2 C3 1.392(7) . ? C3 C4 1.424(7) . ? C4 C5 1.430(7) . ? C5 C6 1.418(7) . ? C6 C7 1.397(7) . ? C14 K1 3.230(4) 4_566 ? 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 106.19(10) . . ? N2 Gd1 C4 113.88(15) . . ? N1 Gd1 C4 126.24(15) . . ? N2 Gd1 C7 111.12(14) . . ? N1 Gd1 C7 121.80(14) . . ? C4 Gd1 C7 74.87(12) . . ? N2 Gd1 C1 140.51(15) . . ? N1 Gd1 C1 96.32(13) . . ? C4 Gd1 C1 74.54(13) . . ? C7 Gd1 C1 30.93(15) . . ? N2 Gd1 C3 144.72(15) . . ? N1 Gd1 C3 99.05(12) . . ? C4 Gd1 C3 31.61(16) . . ? C7 Gd1 C3 73.79(12) . . ? C1 Gd1 C3 57.20(15) . . ? N2 Gd1 C6 93.17(11) . . ? N1 Gd1 C6 152.46(14) . . ? C4 Gd1 C6 58.25(15) . . ? C7 Gd1 C6 30.80(15) . . ? C1 Gd1 C6 57.12(15) . . ? C3 Gd1 C6 73.68(12) . . ? N2 Gd1 C5 94.12(11) . . ? N1 Gd1 C5 156.87(13) . . ? C4 Gd1 C5 31.54(15) . . ? C7 Gd1 C5 57.59(15) . . ? C1 Gd1 C5 73.60(12) . . ? C3 Gd1 C5 57.90(14) . . ? C6 Gd1 C5 30.97(15) . . ? N2 Gd1 C2 165.50(11) . . ? N1 Gd1 C2 87.90(11) . . ? C4 Gd1 C2 57.53(16) . . ? C7 Gd1 C2 56.77(16) . . ? C1 Gd1 C2 30.45(16) . . ? C3 Gd1 C2 30.42(16) . . ? C6 Gd1 C2 72.40(13) . . ? C5 Gd1 C2 72.82(12) . . ? N2 Gd1 C13 84.78(12) . . ? N1 Gd1 C13 64.14(12) . . ? C4 Gd1 C13 84.98(12) . . ? C7 Gd1 C13 158.05(12) . . ? C1 Gd1 C13 134.63(16) . . ? C3 Gd1 C13 84.50(13) . . ? C6 Gd1 C13 138.73(15) . . ? C5 Gd1 C13 107.92(15) . . ? C2 Gd1 C13 104.94(16) . . ? N2 Gd1 Si2 101.30(7) . . ? N1 Gd1 Si2 30.21(8) . . ? C4 Gd1 Si2 105.36(12) . . ? C7 Gd1 Si2 144.45(13) . . ? C1 Gd1 Si2 113.82(12) . . ? C3 Gd1 Si2 88.25(8) . . ? C6 Gd1 Si2 161.91(9) . . ? C5 Gd1 Si2 135.53(13) . . ? C2 Gd1 Si2 92.61(10) . . ? C13 Gd1 Si2 34.49(9) . . ? N2 Gd1 Si3 28.47(7) . . ? N1 Gd1 Si3 89.89(7) . . ? C4 Gd1 Si3 139.80(14) . . ? C7 Gd1 Si3 102.57(10) . . ? C1 Gd1 Si3 123.32(12) . . ? C3 Gd1 Si3 170.97(11) . . ? C6 Gd1 Si3 98.88(9) . . ? C5 Gd1 Si3 113.12(11) . . ? C2 Gd1 Si3 152.76(14) . . ? C13 Gd1 Si3 98.43(10) . . ? Si2 Gd1 Si3 99.01(3) . . ? N3 Gd2 N4 97.75(9) . . ? N3 Gd2 C2 110.69(14) . . ? N4 Gd2 C2 129.49(16) . . ? N3 Gd2 C6 115.54(14) . . ? N4 Gd2 C6 127.52(15) . . ? C2 Gd2 C6 76.27(13) . . ? N3 Gd2 C5 146.27(15) . . ? N4 Gd2 C5 101.89(13) . . ? C2 Gd2 C5 76.75(13) . . ? C6 Gd2 C5 32.13(16) . . ? N3 Gd2 C3 140.06(15) . . ? N4 Gd2 C3 104.12(12) . . ? C2 Gd2 C3 31.51(16) . . ? C6 Gd2 C3 75.91(12) . . ? C5 Gd2 C3 59.57(16) . . ? N3 Gd2 C1 94.26(11) . . ? N4 Gd2 C1 160.79(14) . . ? C2 Gd2 C1 31.34(16) . . ? C6 Gd2 C1 58.32(16) . . ? C5 Gd2 C1 75.30(13) . . ? C3 Gd2 C1 57.75(15) . . ? N3 Gd2 C7 96.05(11) . . ? N4 Gd2 C7 158.89(14) . . ? C2 Gd2 C7 58.44(16) . . ? C6 Gd2 C7 31.37(15) . . ? C5 Gd2 C7 58.75(15) . . ? C3 Gd2 C7 74.44(12) . . ? C1 Gd2 C7 30.96(15) . . ? N3 Gd2 C4 168.53(11) . . ? N4 Gd2 C4 93.17(10) . . ? C2 Gd2 C4 58.97(17) . . ? C6 Gd2 C4 59.13(16) . . ? C5 Gd2 C4 31.99(16) . . ? C3 Gd2 C4 31.72(16) . . ? C1 Gd2 C4 74.29(13) . . ? C7 Gd2 C4 74.49(12) . . ? N3 Gd2 Si8 100.02(7) . . ? N4 Gd2 Si8 28.28(7) . . ? C2 Gd2 Si8 146.37(15) . . ? C6 Gd2 Si8 103.00(12) . . ? C5 Gd2 Si8 85.41(9) . . ? C3 Gd2 Si8 115.02(13) . . ? C1 Gd2 Si8 160.38(11) . . ? C7 Gd2 Si8 132.81(13) . . ? C4 Gd2 Si8 91.26(10) . . ? N3 Gd2 Si5 27.31(7) . . ? N4 Gd2 Si5 99.56(7) . . ? C2 Gd2 Si5 89.62(11) . . ? C6 Gd2 Si5 128.74(13) . . ? C5 Gd2 Si5 158.56(11) . . ? C3 Gd2 Si5 114.79(13) . . ? C1 Gd2 Si5 84.43(9) . . ? C7 Gd2 Si5 100.04(11) . . ? C4 Gd2 Si5 146.51(13) . . ? Si8 Gd2 Si5 114.18(3) . . ? N3 Gd2 K1 48.53(6) . . ? N4 Gd2 K1 49.22(7) . . ? C2 Gd2 K1 138.71(9) . . ? C6 Gd2 K1 142.15(9) . . ? C5 Gd2 K1 142.28(9) . . ? C3 Gd2 K1 140.42(8) . . ? C1 Gd2 K1 140.44(9) . . ? C7 Gd2 K1 141.79(8) . . ? C4 Gd2 K1 142.27(8) . . ? Si8 Gd2 K1 57.77(2) . . ? Si5 Gd2 K1 56.42(2) . . ? N3 K1 N4 75.13(7) . . ? N3 K1 C23 58.00(9) . . ? N4 K1 C23 113.22(10) . . ? N3 K1 C28 114.69(11) . . ? N4 K1 C28 57.21(10) . . ? C23 K1 C28 170.27(11) . . ? N3 K1 C14 155.85(10) . 4_665 ? N4 K1 C14 128.07(9) . 4_665 ? C23 K1 C14 109.48(10) . 4_665 ? C28 K1 C14 79.68(11) . 4_665 ? N3 K1 C21 55.00(9) . . ? N4 K1 C21 118.10(10) . . ? C23 K1 C21 71.11(12) . . ? C28 K1 C21 110.82(14) . . ? C14 K1 C21 102.55(11) 4_665 . ? N3 K1 Si5 29.26(6) . . ? N4 K1 Si5 87.91(6) . . ? C23 K1 Si5 73.83(8) . . ? C28 K1 Si5 102.70(11) . . ? C14 K1 Si5 132.29(9) 4_665 . ? C21 K1 Si5 31.35(8) . . ? N3 K1 C29 115.55(9) . . ? N4 K1 C29 54.29(9) . . ? C23 K1 C29 105.64(13) . . ? C28 K1 C29 70.86(14) . . ? C14 K1 C29 86.98(11) 4_665 . ? C21 K1 C29 170.47(11) . . ? Si5 K1 C29 139.50(7) . . ? N3 K1 Si8 86.62(6) . . ? N4 K1 Si8 28.76(6) . . ? C23 K1 Si8 99.63(10) . . ? C28 K1 Si8 72.63(10) . . ? C14 K1 Si8 116.94(8) 4_665 . ? C21 K1 Si8 140.02(8) . . ? Si5 K1 Si8 108.84(3) . . ? C29 K1 Si8 30.66(7) . . ? N3 K1 Si6 27.32(5) . . ? N4 K1 Si6 92.04(6) . . ? C23 K1 Si6 30.78(7) . . ? C28 K1 Si6 141.28(9) . . ? C14 K1 Si6 137.83(8) 4_665 . ? C21 K1 Si6 60.33(8) . . ? Si5 K1 Si6 48.52(3) . . ? C29 K1 Si6 112.18(9) . . ? Si8 K1 Si6 91.42(3) . . ? N3 K1 Si7 92.09(6) . . ? N4 K1 Si7 26.92(6) . . ? C23 K1 Si7 139.79(8) . . ? C28 K1 Si7 30.52(8) . . ? C14 K1 Si7 107.35(8) 4_665 . ? C21 K1 Si7 115.65(9) . . ? Si5 K1 Si7 92.93(3) . . ? C29 K1 Si7 60.73(8) . . ? Si8 K1 Si7 48.16(3) . . ? Si6 K1 Si7 114.81(3) . . ? N3 K1 Gd2 37.45(5) . . ? N4 K1 Gd2 37.68(5) . . ? C23 K1 Gd2 84.99(7) . . ? C28 K1 Gd2 85.63(8) . . ? C14 K1 Gd2 164.82(8) 4_665 . ? C21 K1 Gd2 86.20(8) . . ? Si5 K1 Gd2 54.93(2) . . ? C29 K1 Gd2 84.57(7) . . ? Si8 K1 Gd2 53.91(2) . . ? Si6 K1 Gd2 57.336(19) . . ? Si7 K1 Gd2 57.48(2) . . ? N1 Si1 C8 113.05(18) . . ? N1 Si1 C10 113.2(2) . . ? C8 Si1 C10 106.9(3) . . ? N1 Si1 C9 114.1(2) . . ? C8 Si1 C9 105.2(3) . . ? C10 Si1 C9 103.7(3) . . ? N1 Si2 C11 113.99(19) . . ? N1 Si2 C12 114.2(2) . . ? C11 Si2 C12 108.6(2) . . ? N1 Si2 C13 109.27(17) . . ? C11 Si2 C13 105.4(2) . . ? C12 Si2 C13 104.6(3) . . ? N1 Si2 Gd1 43.40(10) . . ? C11 Si2 Gd1 135.33(15) . . ? C12 Si2 Gd1 115.94(16) . . ? C13 Si2 Gd1 67.05(13) . . ? N2 Si3 C16 109.07(16) . . ? N2 Si3 C15 116.80(19) . . ? C16 Si3 C15 104.4(2) . . ? N2 Si3 C14 112.27(17) . . ? C16 Si3 C14 108.72(19) . . ? C15 Si3 C14 105.1(2) . . ? N2 Si3 Gd1 40.63(10) . . ? C16 Si3 Gd1 71.56(12) . . ? C15 Si3 Gd1 142.84(15) . . ? C14 Si3 Gd1 111.19(13) . . ? N2 Si4 C18 111.60(17) . . ? N2 Si4 C19 113.9(2) . . ? C18 Si4 C19 105.0(2) . . ? N2 Si4 C17 112.8(2) . . ? C18 Si4 C17 107.8(2) . . ? C19 Si4 C17 105.1(3) . . ? N3 Si5 C22 115.82(18) . . ? N3 Si5 C20 109.27(17) . . ? C22 Si5 C20 104.9(2) . . ? N3 Si5 C21 113.0(2) . . ? C22 Si5 C21 107.5(2) . . ? C20 Si5 C21 105.7(2) . . ? N3 Si5 Gd2 39.67(9) . . ? C22 Si5 Gd2 109.00(16) . . ? C20 Si5 Gd2 74.17(13) . . ? C21 Si5 Gd2 142.19(18) . . ? N3 Si5 K1 56.91(9) . . ? C22 Si5 K1 171.50(16) . . ? C20 Si5 K1 82.57(14) . . ? C21 Si5 K1 73.82(18) . . ? Gd2 Si5 K1 68.65(2) . . ? N3 Si6 C25 114.19(16) . . ? N3 Si6 C24 115.47(17) . . ? C25 Si6 C24 104.66(19) . . ? N3 Si6 C23 110.92(17) . . ? C25 Si6 C23 106.6(2) . . ? C24 Si6 C23 104.1(2) . . ? N3 Si6 K1 51.33(9) . . ? C25 Si6 K1 123.51(14) . . ? C24 Si6 K1 131.53(14) . . ? C23 Si6 K1 59.85(14) . . ? N4 Si7 C26 114.53(16) . . ? N4 Si7 C27 114.9(2) . . ? C26 Si7 C27 104.4(2) . . ? N4 Si7 C28 111.49(19) . . ? C26 Si7 C28 105.3(2) . . ? C27 Si7 C28 105.2(2) . . ? N4 Si7 K1 51.55(10) . . ? C26 Si7 K1 120.34(15) . . ? C27 Si7 K1 134.97(16) . . ? C28 Si7 K1 60.56(15) . . ? N4 Si8 C30 115.42(18) . . ? N4 Si8 C29 113.7(2) . . ? C30 Si8 C29 107.5(2) . . ? N4 Si8 C31 109.03(16) . . ? C30 Si8 C31 105.1(2) . . ? C29 Si8 C31 105.2(2) . . ? N4 Si8 Gd2 41.26(9) . . ? C30 Si8 Gd2 109.27(15) . . ? C29 Si8 Gd2 142.44(17) . . ? C31 Si8 Gd2 71.99(13) . . ? N4 Si8 K1 56.07(10) . . ? C30 Si8 K1 170.04(17) . . ? C29 Si8 K1 74.13(16) . . ? C31 Si8 K1 83.59(13) . . ? Gd2 Si8 K1 68.32(2) . . ? Si2 N1 Si1 120.20(17) . . ? Si2 N1 Gd1 106.39(15) . . ? Si1 N1 Gd1 133.26(16) . . ? Si3 N2 Si4 120.23(17) . . ? Si3 N2 Gd1 110.90(14) . . ? Si4 N2 Gd1 128.82(15) . . ? Si5 N3 Si6 118.59(16) . . ? Si5 N3 Gd2 113.01(13) . . ? Si6 N3 Gd2 124.52(14) . . ? Si5 N3 K1 93.83(11) . . ? Si6 N3 K1 101.35(11) . . ? Gd2 N3 K1 94.02(9) . . ? Si7 N4 Si8 119.70(16) . . ? Si7 N4 Gd2 125.67(15) . . ? Si8 N4 Gd2 110.46(13) . . ? Si7 N4 K1 101.53(12) . . ? Si8 N4 K1 95.18(11) . . ? Gd2 N4 K1 93.10(9) . . ? C2 C1 C7 129.4(4) . . ? C2 C1 Gd2 71.9(2) . . ? C7 C1 Gd2 74.7(2) . . ? C2 C1 Gd1 77.7(2) . . ? C7 C1 Gd1 74.4(2) . . ? Gd2 C1 Gd1 103.54(14) . . ? C1 C2 C3 128.4(4) . . ? C1 C2 Gd2 76.8(2) . . ? C3 C2 Gd2 76.2(2) . . ? C1 C2 Gd1 71.9(2) . . ? C3 C2 Gd1 72.8(2) . . ? Gd2 C2 Gd1 103.19(14) . . ? C2 C3 C4 128.9(4) . . ? C2 C3 Gd2 72.3(2) . . ? C4 C3 Gd2 75.6(2) . . ? C2 C3 Gd1 76.8(2) . . ? C4 C3 Gd1 73.2(2) . . ? Gd2 C3 Gd1 103.28(13) . . ? C3 C4 C5 127.3(4) . . ? C3 C4 Gd1 75.1(2) . . ? C5 C4 Gd1 76.4(2) . . ? C3 C4 Gd2 72.7(2) . . ? C5 C4 Gd2 71.7(2) . . ? Gd1 C4 Gd2 102.95(13) . . ? C6 C5 C4 127.8(4) . . ? C6 C5 Gd2 73.8(2) . . ? C4 C5 Gd2 76.3(2) . . ? C6 C5 Gd1 74.3(2) . . ? C4 C5 Gd1 72.0(2) . . ? Gd2 C5 Gd1 102.98(14) . . ? C7 C6 C5 128.4(4) . . ? C7 C6 Gd2 76.0(2) . . ? C5 C6 Gd2 74.0(2) . . ? C7 C6 Gd1 72.6(2) . . ? C5 C6 Gd1 74.7(2) . . ? Gd2 C6 Gd1 103.19(14) . . ? C1 C7 C6 129.0(4) . . ? C1 C7 Gd1 74.6(2) . . ? C6 C7 Gd1 76.6(2) . . ? C1 C7 Gd2 74.3(2) . . ? C6 C7 Gd2 72.6(2) . . ? Gd1 C7 Gd2 103.46(13) . . ? Si2 C13 Gd1 78.46(14) . . ? Si3 C14 K1 169.1(2) . 4_566 ? Si5 C21 K1 74.84(16) . . ? Si6 C23 K1 89.37(15) . . ? Si7 C28 K1 88.92(16) . . ? Si8 C29 K1 75.21(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Si2 N1 Si1 52.4(3) . . . . ? C12 Si2 N1 Si1 -73.3(3) . . . . ? C13 Si2 N1 Si1 170.0(2) . . . . ? Gd1 Si2 N1 Si1 -176.2(3) . . . . ? C11 Si2 N1 Gd1 -131.48(19) . . . . ? C12 Si2 N1 Gd1 102.8(2) . . . . ? C13 Si2 N1 Gd1 -13.9(2) . . . . ? C8 Si1 N1 Si2 147.9(3) . . . . ? C10 Si1 N1 Si2 -90.4(3) . . . . ? C9 Si1 N1 Si2 27.8(3) . . . . ? C8 Si1 N1 Gd1 -27.0(3) . . . . ? C10 Si1 N1 Gd1 94.6(3) . . . . ? C9 Si1 N1 Gd1 -147.2(2) . . . . ? C16 Si3 N2 Si4 -154.1(2) . . . . ? C15 Si3 N2 Si4 -36.1(3) . . . . ? C14 Si3 N2 Si4 85.3(2) . . . . ? Gd1 Si3 N2 Si4 -177.6(3) . . . . ? C16 Si3 N2 Gd1 23.5(2) . . . . ? C15 Si3 N2 Gd1 141.48(18) . . . . ? C14 Si3 N2 Gd1 -97.04(19) . . . . ? C18 Si4 N2 Si3 -46.4(3) . . . . ? C19 Si4 N2 Si3 -165.1(2) . . . . ? C17 Si4 N2 Si3 75.1(3) . . . . ? C18 Si4 N2 Gd1 136.4(2) . . . . ? C19 Si4 N2 Gd1 17.7(3) . . . . ? C17 Si4 N2 Gd1 -102.0(3) . . . . ? C22 Si5 N3 Si6 69.8(3) . . . . ? C20 Si5 N3 Si6 -172.10(19) . . . . ? C21 Si5 N3 Si6 -54.8(2) . . . . ? Gd2 Si5 N3 Si6 158.8(2) . . . . ? K1 Si5 N3 Si6 -105.13(17) . . . . ? C22 Si5 N3 Gd2 -89.0(2) . . . . ? C20 Si5 N3 Gd2 29.1(2) . . . . ? C21 Si5 N3 Gd2 146.38(18) . . . . ? K1 Si5 N3 Gd2 96.02(13) . . . . ? C22 Si5 N3 K1 174.93(19) . . . . ? C20 Si5 N3 K1 -66.96(17) . . . . ? C21 Si5 N3 K1 50.36(19) . . . . ? Gd2 Si5 N3 K1 -96.02(13) . . . . ? C25 Si6 N3 Si5 -144.7(2) . . . . ? C24 Si6 N3 Si5 -23.2(2) . . . . ? C23 Si6 N3 Si5 94.8(2) . . . . ? K1 Si6 N3 Si5 100.78(18) . . . . ? C25 Si6 N3 Gd2 11.6(2) . . . . ? C24 Si6 N3 Gd2 132.99(19) . . . . ? C23 Si6 N3 Gd2 -108.9(2) . . . . ? K1 Si6 N3 Gd2 -102.99(17) . . . . ? C25 Si6 N3 K1 114.56(17) . . . . ? C24 Si6 N3 K1 -124.02(17) . . . . ? C23 Si6 N3 K1 -5.9(2) . . . . ? C26 Si7 N4 Si8 -146.9(2) . . . . ? C27 Si7 N4 Si8 -25.9(3) . . . . ? C28 Si7 N4 Si8 93.7(3) . . . . ? K1 Si7 N4 Si8 102.85(19) . . . . ? C26 Si7 N4 Gd2 7.9(3) . . . . ? C27 Si7 N4 Gd2 128.9(2) . . . . ? C28 Si7 N4 Gd2 -111.6(2) . . . . ? K1 Si7 N4 Gd2 -102.38(19) . . . . ? C26 Si7 N4 K1 110.28(18) . . . . ? C27 Si7 N4 K1 -128.8(2) . . . . ? C28 Si7 N4 K1 -9.2(2) . . . . ? C30 Si8 N4 Si7 67.6(3) . . . . ? C29 Si8 N4 Si7 -57.4(3) . . . . ? C31 Si8 N4 Si7 -174.45(19) . . . . ? Gd2 Si8 N4 Si7 158.3(3) . . . . ? K1 Si8 N4 Si7 -106.43(19) . . . . ? C30 Si8 N4 Gd2 -90.7(2) . . . . ? C29 Si8 N4 Gd2 144.31(18) . . . . ? C31 Si8 N4 Gd2 27.2(2) . . . . ? K1 Si8 N4 Gd2 95.26(12) . . . . ? C30 Si8 N4 K1 174.03(19) . . . . ? C29 Si8 N4 K1 49.05(19) . . . . ? C31 Si8 N4 K1 -68.02(16) . . . . ? Gd2 Si8 N4 K1 -95.26(12) . . . . ? C7 C1 C2 C3 -8.8(7) . . . . ? Gd2 C1 C2 C3 -60.0(4) . . . . ? Gd1 C1 C2 C3 48.9(4) . . . . ? C7 C1 C2 Gd2 51.2(4) . . . . ? Gd1 C1 C2 Gd2 108.88(12) . . . . ? C7 C1 C2 Gd1 -57.7(4) . . . . ? Gd2 C1 C2 Gd1 -108.88(12) . . . . ? C1 C2 C3 C4 6.7(7) . . . . ? Gd2 C2 C3 C4 -53.6(4) . . . . ? Gd1 C2 C3 C4 55.2(4) . . . . ? C1 C2 C3 Gd2 60.2(4) . . . . ? Gd1 C2 C3 Gd2 108.80(11) . . . . ? C1 C2 C3 Gd1 -48.6(4) . . . . ? Gd2 C2 C3 Gd1 -108.80(11) . . . . ? C2 C3 C4 C5 2.9(7) . . . . ? Gd2 C3 C4 C5 -49.5(4) . . . . ? Gd1 C3 C4 C5 59.5(4) . . . . ? C2 C3 C4 Gd1 -56.7(4) . . . . ? Gd2 C3 C4 Gd1 -108.98(11) . . . . ? C2 C3 C4 Gd2 52.3(4) . . . . ? Gd1 C3 C4 Gd2 108.98(11) . . . . ? C3 C4 C5 C6 -6.7(7) . . . . ? Gd1 C4 C5 C6 52.3(4) . . . . ? Gd2 C4 C5 C6 -56.5(4) . . . . ? C3 C4 C5 Gd2 49.8(4) . . . . ? Gd1 C4 C5 Gd2 108.80(11) . . . . ? C3 C4 C5 Gd1 -59.0(4) . . . . ? Gd2 C4 C5 Gd1 -108.80(11) . . . . ? C4 C5 C6 C7 0.7(7) . . . . ? Gd2 C5 C6 C7 -56.7(4) . . . . ? Gd1 C5 C6 C7 52.2(4) . . . . ? C4 C5 C6 Gd2 57.5(4) . . . . ? Gd1 C5 C6 Gd2 108.92(11) . . . . ? C4 C5 C6 Gd1 -51.4(4) . . . . ? Gd2 C5 C6 Gd1 -108.92(11) . . . . ? C2 C1 C7 C6 1.1(7) . . . . ? Gd2 C1 C7 C6 51.2(4) . . . . ? Gd1 C1 C7 C6 -57.9(4) . . . . ? C2 C1 C7 Gd1 59.0(4) . . . . ? Gd2 C1 C7 Gd1 109.14(11) . . . . ? C2 C1 C7 Gd2 -50.2(4) . . . . ? Gd1 C1 C7 Gd2 -109.14(11) . . . . ? C5 C6 C7 C1 4.1(7) . . . . ? Gd2 C6 C7 C1 -51.9(4) . . . . ? Gd1 C6 C7 C1 57.1(4) . . . . ? C5 C6 C7 Gd1 -53.0(4) . . . . ? Gd2 C6 C7 Gd1 -108.96(11) . . . . ? C5 C6 C7 Gd2 56.0(4) . . . . ? Gd1 C6 C7 Gd2 108.96(11) . . . . ? N1 Si2 C13 Gd1 10.31(16) . . . . ? C11 Si2 C13 Gd1 133.20(16) . . . . ? C12 Si2 C13 Gd1 -112.38(18) . . . . ? N2 Si3 C14 K1 -86.0(11) . . . 4_566 ? C16 Si3 C14 K1 153.3(10) . . . 4_566 ? C15 Si3 C14 K1 42.0(11) . . . 4_566 ? Gd1 Si3 C14 K1 -129.8(10) . . . 4_566 ? N3 Si5 C21 K1 -42.21(14) . . . . ? C22 Si5 C21 K1 -171.22(16) . . . . ? C20 Si5 C21 K1 77.22(17) . . . . ? Gd2 Si5 C21 K1 -7.0(2) . . . . ? N3 Si6 C23 K1 5.35(18) . . . . ? C25 Si6 C23 K1 -119.53(16) . . . . ? C24 Si6 C23 K1 130.15(16) . . . . ? N4 Si7 C28 K1 8.2(2) . . . . ? C26 Si7 C28 K1 -116.53(17) . . . . ? C27 Si7 C28 K1 133.43(17) . . . . ? N4 Si8 C29 K1 -40.65(15) . . . . ? C30 Si8 C29 K1 -169.75(18) . . . . ? C31 Si8 C29 K1 78.60(16) . . . . ? Gd2 Si8 C29 K1 -1.5(3) . . . . ? _refine_diff_density_max 2.022 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.107 _shelx_res_file ; mm469_5.res created by SHELXL-2014/7 TITL mm469_4 in P2(1)/n CELL 0.71073 14.17000 14.28480 25.40390 90.0000 95.5181 90.0000 ZERR 4.00 0.00070 0.00070 0.00120 0.0000 0.0023 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N SI K GD UNIT 124 316 16 32 4 8 TEMP -73.150 SIZE 0.139 0.203 0.29 L.S. 80 ACTA CONF LIST 0 BOND FMAP 2 PLAN 5 OMIT -7 3 32 OMIT -7 3 32 OMIT 3 1 20 OMIT 1 1 0 OMIT -11 5 11 OMIT -1 1 22 OMIT -1 1 24 OMIT 1 1 32 OMIT 1 12 14 OMIT 1 1 16 OMIT 3 1 26 OMIT -1 0 13 OMIT 1 1 24 OMIT 3 1 24 OMIT 5 1 28 OMIT 3 7 16 OMIT 2 3 5 OMIT 7 1 22 OMIT -6 8 13 OMIT -1 1 2 OMIT 15 4 4 OMIT -14 10 2 OMIT -1 2 10 OMIT 5 15 1 OMIT 11 12 7 OMIT 9 1 24 OMIT 5 1 26 OMIT 1 4 4 OMIT -7 9 12 OMIT -2 19 7 OMIT -15 8 12 OMIT -2 1 7 OMIT 7 1 30 OMIT -2 15 6 OMIT 3 4 0 OMIT -14 0 24 OMIT 2 2 23 OMIT -11 3 7 OMIT -3 9 16 OMIT 3 1 32 OMIT -15 13 3 OMIT 1 7 20 OMIT 1 1 30 OMIT 12 9 7 OMIT 0 14 4 OMIT 10 3 25 OMIT 4 14 1 OMIT 6 2 29 OMIT 0 2 23 OMIT -8 8 10 WGHT 0.021400 6.785100 BASF 0.17980 FVAR 0.14706 GD1 6 0.169794 0.231076 1.068493 11.00000 0.02760 0.03209 = 0.02119 -0.00093 0.00983 -0.00042 GD2 6 0.303820 0.224143 0.933095 11.00000 0.02611 0.03095 = 0.01799 -0.00193 0.00713 -0.00313 K1 5 0.438541 0.214460 0.806078 11.00000 0.05932 0.06305 = 0.03691 -0.02092 0.02444 -0.02094 SI1 4 0.317543 0.208139 1.196828 11.00000 0.03606 0.06290 = 0.03018 0.01140 0.00492 0.00695 SI2 4 0.177306 0.065391 1.156341 11.00000 0.06271 0.03243 = 0.03825 0.00609 0.02649 0.00327 SI3 4 0.048863 0.389735 1.130304 11.00000 0.03430 0.03442 = 0.02974 0.00039 0.01062 0.00602 SI4 4 -0.081922 0.288975 1.052068 11.00000 0.02776 0.05990 = 0.03299 0.00504 0.00456 -0.00227 SI5 4 0.544838 0.250473 0.934359 11.00000 0.02565 0.03671 = 0.04348 -0.00346 0.00624 0.00106 SI6 4 0.444908 0.420830 0.893347 11.00000 0.03613 0.03285 = 0.02702 0.00121 0.00791 -0.00585 SI7 4 0.292148 0.017438 0.847291 11.00000 0.05002 0.03305 = 0.03293 -0.00896 0.01057 -0.00826 SI8 4 0.189741 0.190200 0.810762 11.00000 0.04073 0.04640 = 0.02355 0.00019 -0.00022 -0.00979 N1 3 0.231004 0.170856 1.149761 11.00000 0.03580 0.03629 = 0.02725 0.00644 0.01176 0.00577 N2 3 0.029548 0.305745 1.083277 11.00000 0.02658 0.04011 = 0.02884 -0.00099 0.00724 0.00143 N3 3 0.441597 0.303991 0.910179 11.00000 0.02459 0.02950 = 0.02536 -0.00142 0.00691 -0.00383 N4 3 0.273140 0.135144 0.853562 11.00000 0.03642 0.02986 = 0.02276 -0.00578 0.00439 -0.00799 C1 1 0.332680 0.265428 1.032959 11.00000 0.03811 0.10847 = 0.02148 -0.00964 0.01033 -0.02535 AFIX 43 H1A 2 0.386925 0.287858 1.054098 11.00000 -1.20000 AFIX 0 C2 1 0.326014 0.168738 1.028383 11.00000 0.04785 0.10429 = 0.02872 0.01956 0.01746 0.04026 AFIX 43 H2A 2 0.380217 0.134496 1.042341 11.00000 -1.20000 AFIX 0 C3 1 0.250263 0.115448 1.006010 11.00000 0.10515 0.02728 = 0.04324 0.00708 0.04754 0.01420 AFIX 43 H3A 2 0.256934 0.049622 1.010198 11.00000 -1.20000 AFIX 0 C4 1 0.164138 0.146000 0.977706 11.00000 0.07125 0.07151 = 0.03638 -0.02951 0.03150 -0.05170 AFIX 43 H4A 2 0.119402 0.098609 0.966855 11.00000 -1.20000 AFIX 0 C5 1 0.137398 0.240004 0.963773 11.00000 0.02316 0.12749 = 0.02204 -0.00247 0.00402 0.01043 AFIX 43 H5A 2 0.080118 0.247191 0.941446 11.00000 -1.20000 AFIX 0 C6 1 0.186133 0.323765 0.979290 11.00000 0.07913 0.05064 = 0.04007 0.01734 0.03539 0.03102 AFIX 43 H6A 2 0.156906 0.380176 0.966366 11.00000 -1.20000 AFIX 0 C7 1 0.271531 0.334080 1.011109 11.00000 0.08315 0.03933 = 0.03961 -0.01440 0.03825 -0.02689 AFIX 43 H7A 2 0.290397 0.396780 1.018880 11.00000 -1.20000 AFIX 0 C8 1 0.409605 0.281757 1.169131 11.00000 0.04629 0.11445 = 0.04429 0.01225 -0.00162 -0.02951 AFIX 33 H8A 2 0.457042 0.300982 1.197707 11.00000 -1.50000 H8B 2 0.440458 0.245545 1.142855 11.00000 -1.50000 H8C 2 0.379683 0.337421 1.152280 11.00000 -1.50000 AFIX 0 C9 1 0.384996 0.110461 1.233192 11.00000 0.05802 0.11748 = 0.09026 0.04972 0.00100 0.02832 AFIX 33 H9A 2 0.433033 0.136932 1.259333 11.00000 -1.50000 H9B 2 0.341031 0.071611 1.251208 11.00000 -1.50000 H9C 2 0.416038 0.071992 1.207964 11.00000 -1.50000 AFIX 0 C10 1 0.270023 0.277949 1.250841 11.00000 0.06818 0.10058 = 0.03399 -0.00909 -0.00033 0.00289 AFIX 33 H10A 2 0.322518 0.297267 1.276475 11.00000 -1.50000 H10B 2 0.237295 0.333563 1.235668 11.00000 -1.50000 H10C 2 0.225392 0.239541 1.268639 11.00000 -1.50000 AFIX 0 C11 1 0.128684 0.048698 1.221356 11.00000 0.07109 0.06121 = 0.04213 0.01068 0.02753 -0.00360 AFIX 33 H11A 2 0.099003 -0.013165 1.222317 11.00000 -1.50000 H11B 2 0.180221 0.053313 1.249863 11.00000 -1.50000 H11C 2 0.081278 0.097176 1.226050 11.00000 -1.50000 AFIX 0 C12 1 0.253004 -0.037581 1.143689 11.00000 0.13003 0.04663 = 0.09901 0.01365 0.06755 0.02500 AFIX 33 H12A 2 0.217431 -0.095393 1.148209 11.00000 -1.50000 H12B 2 0.271227 -0.034452 1.107481 11.00000 -1.50000 H12C 2 0.310099 -0.036963 1.168733 11.00000 -1.50000 AFIX 0 C13 1 0.072613 0.055503 1.105463 11.00000 0.08610 0.05212 = 0.04500 -0.00403 0.01670 -0.02897 AFIX 33 H13A 2 0.041549 -0.005122 1.109143 11.00000 -1.50000 H13B 2 0.027607 0.105986 1.110661 11.00000 -1.50000 H13C 2 0.094018 0.060481 1.070017 11.00000 -1.50000 AFIX 0 C14 1 0.023288 0.347079 1.197704 11.00000 0.05324 0.05242 = 0.03036 0.00046 0.01230 0.00429 AFIX 33 H14A 2 0.035354 0.397670 1.223531 11.00000 -1.50000 H14B 2 -0.043212 0.327678 1.196584 11.00000 -1.50000 H14C 2 0.064427 0.293713 1.208035 11.00000 -1.50000 AFIX 0 C15 1 -0.020675 0.501022 1.119672 11.00000 0.05732 0.03966 = 0.06976 0.00294 0.01525 0.01461 AFIX 33 H15A 2 -0.003700 0.543956 1.149157 11.00000 -1.50000 H15B 2 -0.006038 0.530270 1.086521 11.00000 -1.50000 H15C 2 -0.088611 0.486970 1.117784 11.00000 -1.50000 AFIX 0 C16 1 0.175531 0.427870 1.133603 11.00000 0.04162 0.04126 = 0.04451 -0.00461 0.00877 -0.00244 AFIX 33 H16A 2 0.187152 0.476412 1.160712 11.00000 -1.50000 H16B 2 0.216971 0.374147 1.142623 11.00000 -1.50000 H16C 2 0.188855 0.453039 1.099201 11.00000 -1.50000 AFIX 0 C17 1 -0.117167 0.382032 1.001976 11.00000 0.06161 0.11442 = 0.05984 0.04821 -0.01450 -0.01634 AFIX 33 H17A 2 -0.181170 0.369117 0.985401 11.00000 -1.50000 H17B 2 -0.116317 0.443199 1.019484 11.00000 -1.50000 H17C 2 -0.072442 0.382432 0.974854 11.00000 -1.50000 AFIX 0 C18 1 -0.173696 0.285724 1.100297 11.00000 0.02786 0.06759 = 0.05271 0.00677 0.00874 -0.00131 AFIX 33 H18A 2 -0.236381 0.276073 1.081203 11.00000 -1.50000 H18B 2 -0.159670 0.234256 1.125338 11.00000 -1.50000 H18C 2 -0.173106 0.345141 1.119610 11.00000 -1.50000 AFIX 0 C19 1 -0.096346 0.175838 1.014932 11.00000 0.04279 0.10621 = 0.06852 -0.03428 0.00483 -0.01544 AFIX 33 H19A 2 -0.161396 0.170917 0.998171 11.00000 -1.50000 H19B 2 -0.051857 0.173913 0.987706 11.00000 -1.50000 H19C 2 -0.083332 0.123476 1.039485 11.00000 -1.50000 AFIX 0 C20 1 0.523675 0.120976 0.940159 11.00000 0.04388 0.04084 = 0.06298 -0.00102 0.00531 0.00463 AFIX 33 H20A 2 0.582678 0.090118 0.953999 11.00000 -1.50000 H20B 2 0.474831 0.110021 0.964275 11.00000 -1.50000 H20C 2 0.502497 0.095360 0.905223 11.00000 -1.50000 AFIX 0 C21 1 0.642109 0.262668 0.889256 11.00000 0.03655 0.05841 = 0.09006 -0.00826 0.02840 0.00269 AFIX 33 H21A 2 0.699276 0.230858 0.905005 11.00000 -1.50000 H21B 2 0.621725 0.234337 0.854902 11.00000 -1.50000 H21C 2 0.655942 0.329156 0.884392 11.00000 -1.50000 AFIX 0 C22 1 0.594287 0.287609 1.001746 11.00000 0.04565 0.06510 = 0.05720 -0.00500 -0.01393 0.00285 AFIX 33 H22A 2 0.653010 0.253115 1.011895 11.00000 -1.50000 H22B 2 0.607738 0.354900 1.001665 11.00000 -1.50000 H22C 2 0.548120 0.274341 1.027117 11.00000 -1.50000 AFIX 0 C23 1 0.457903 0.435376 0.820621 11.00000 0.07621 0.05821 = 0.03462 0.01039 0.01640 -0.01231 AFIX 33 H23A 2 0.459619 0.502183 0.811992 11.00000 -1.50000 H23B 2 0.516883 0.405607 0.812138 11.00000 -1.50000 H23C 2 0.403960 0.405899 0.799938 11.00000 -1.50000 AFIX 0 C24 1 0.546384 0.489148 0.926748 11.00000 0.05093 0.04076 = 0.05352 -0.00171 0.00764 -0.01142 AFIX 33 H24A 2 0.542197 0.554339 0.914735 11.00000 -1.50000 H24B 2 0.543758 0.486953 0.965136 11.00000 -1.50000 H24C 2 0.606311 0.461911 0.917856 11.00000 -1.50000 AFIX 0 C25 1 0.337271 0.488037 0.907120 11.00000 0.05095 0.03369 = 0.05265 0.00506 0.00744 0.00117 AFIX 33 H25A 2 0.344316 0.553469 0.896582 11.00000 -1.50000 H25B 2 0.281384 0.460901 0.887017 11.00000 -1.50000 H25C 2 0.329510 0.485082 0.945003 11.00000 -1.50000 AFIX 0 C26 1 0.325338 -0.044745 0.911035 11.00000 0.06236 0.03514 = 0.05519 -0.00175 0.00323 0.00204 AFIX 33 H26A 2 0.334921 -0.111381 0.904074 11.00000 -1.50000 H26B 2 0.384079 -0.017952 0.928241 11.00000 -1.50000 H26C 2 0.274434 -0.037542 0.934247 11.00000 -1.50000 AFIX 0 C27 1 0.188679 -0.049873 0.815699 11.00000 0.09378 0.04593 = 0.05459 -0.00253 -0.01486 -0.02275 AFIX 33 H27A 2 0.205656 -0.116196 0.813700 11.00000 -1.50000 H27B 2 0.134800 -0.043000 0.836859 11.00000 -1.50000 H27C 2 0.171319 -0.025722 0.779971 11.00000 -1.50000 AFIX 0 C28 1 0.391833 -0.006766 0.805268 11.00000 0.09251 0.05182 = 0.08512 -0.02417 0.05090 -0.00220 AFIX 33 H28A 2 0.400890 -0.074533 0.802460 11.00000 -1.50000 H28B 2 0.376202 0.019656 0.769903 11.00000 -1.50000 H28C 2 0.450298 0.021978 0.821567 11.00000 -1.50000 AFIX 0 C29 1 0.210856 0.177038 0.739387 11.00000 0.08557 0.06751 = 0.02631 0.00147 0.00178 -0.01257 AFIX 33 H29A 2 0.160966 0.209940 0.717252 11.00000 -1.50000 H29B 2 0.272706 0.203808 0.733628 11.00000 -1.50000 H29C 2 0.209929 0.110488 0.729982 11.00000 -1.50000 AFIX 0 C30 1 0.063995 0.156323 0.817255 11.00000 0.04384 0.08155 = 0.05342 0.00983 -0.00902 -0.01479 AFIX 33 H30A 2 0.021894 0.191155 0.791372 11.00000 -1.50000 H30B 2 0.056122 0.089016 0.810778 11.00000 -1.50000 H30C 2 0.048032 0.171033 0.853022 11.00000 -1.50000 AFIX 0 C31 1 0.194862 0.319541 0.823838 11.00000 0.04652 0.04776 = 0.04231 0.00054 0.00005 0.00607 AFIX 33 H31A 2 0.147427 0.351418 0.799539 11.00000 -1.50000 H31B 2 0.181676 0.331622 0.860392 11.00000 -1.50000 H31C 2 0.258155 0.343097 0.818409 11.00000 -1.50000 AFIX 0 HKLF 5 REM mm469_4 in P2(1)/n REM R1 = 0.0330 for 12026 Fo > 4sig(Fo) and 0.0544 for all 15195 data REM 416 parameters refined using 0 restraints END WGHT 0.0214 6.7851 REM Highest difference peak 2.022, deepest hole -0.913, 1-sigma level 0.107 Q1 1 0.0359 0.2369 1.2040 11.00000 0.05 2.02 Q2 1 0.1666 0.3132 1.0665 11.00000 0.05 0.96 Q3 1 0.3602 0.2214 0.9307 11.00000 0.05 0.84 Q4 1 0.2997 0.3114 0.9314 11.00000 0.05 0.81 Q5 1 0.4190 0.2782 0.8145 11.00000 0.05 0.73 ; _shelx_res_checksum 20499 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mm462 _database_code_depnum_ccdc_archive 'CCDC 1454169' _audit_update_record ; 2016-02-18 deposited with the CCDC. 2016-08-08 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H79 Dy2 K N4 Si8' _chemical_formula_weight 1096.80 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' Dy Dy -0.1892 4.4098 '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 14.1259(4) _cell_length_b 14.2954(4) _cell_length_c 25.2343(6) _cell_angle_alpha 90 _cell_angle_beta 95.2741(13) _cell_angle_gamma 90 _cell_volume 5074.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9537 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.38 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas n/a _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_F_000 2224 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 3.217 _shelx_estimated_absorpt_T_min 0.551 _shelx_estimated_absorpt_T_max 0.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5770 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 58488 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.723 _diffrn_reflns_theta_max 28.424 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 0.993 _reflns_number_total 12645 _reflns_number_gt 10273 _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 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-03 (Sheldrick, 2003)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0248P)^2^+8.8760P] 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 12645 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.009 _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 Dy1 Dy 0.17122(2) 0.23147(2) 1.06792(2) 0.02502(4) Uani 1 1 d . . . . . Dy2 Dy 0.30311(2) 0.22487(2) 0.93352(2) 0.02336(4) Uani 1 1 d . . . . . K1 K 0.43712(7) 0.21521(7) 0.80635(3) 0.0517(2) Uani 1 1 d . . . . . Si1 Si 0.31778(8) 0.20789(9) 1.19576(4) 0.0408(3) Uani 1 1 d . . . . . Si2 Si 0.17732(9) 0.06564(7) 1.15527(4) 0.0408(3) Uani 1 1 d . . . . . Si3 Si 0.05042(7) 0.38801(7) 1.12996(4) 0.0311(2) Uani 1 1 d . . . . . Si4 Si -0.08004(7) 0.28752(8) 1.05108(4) 0.0383(2) Uani 1 1 d . . . . . Si5 Si 0.54326(7) 0.25022(7) 0.93452(4) 0.0330(2) Uani 1 1 d . . . . . Si6 Si 0.44355(7) 0.42079(7) 0.89389(4) 0.0293(2) Uani 1 1 d . . . . . Si7 Si 0.29052(8) 0.01964(7) 0.84804(4) 0.0361(2) Uani 1 1 d . . . . . Si8 Si 0.18819(8) 0.19249(8) 0.81184(4) 0.0347(2) Uani 1 1 d . . . . . N1 N 0.2307(2) 0.1713(2) 1.14826(11) 0.0305(6) Uani 1 1 d . . . . . N2 N 0.0321(2) 0.3043(2) 1.08244(11) 0.0301(6) Uani 1 1 d . . . . . N3 N 0.43899(19) 0.30421(19) 0.91073(10) 0.0263(6) Uani 1 1 d . . . . . N4 N 0.2718(2) 0.13755(19) 0.85486(10) 0.0267(6) Uani 1 1 d . . . . . C1 C 0.3335(3) 0.2648(4) 1.03276(15) 0.0553(13) Uani 1 1 d . . . . . H1A H 0.3886 0.2867 1.0536 0.066 Uiso 1 1 calc R U . . . C2 C 0.3260(3) 0.1686(4) 1.02820(16) 0.0561(13) Uani 1 1 d . . . . . H2A H 0.3798 0.1339 1.0424 0.067 Uiso 1 1 calc R U . . . C3 C 0.2498(4) 0.1160(3) 1.00552(17) 0.0588(15) Uani 1 1 d . . . . . H3A H 0.2562 0.0501 1.0093 0.071 Uiso 1 1 calc R U . . . C4 C 0.1634(4) 0.1474(4) 0.97731(16) 0.0576(14) Uani 1 1 d . . . . . H4A H 0.1182 0.1004 0.9666 0.069 Uiso 1 1 calc R U . . . C5 C 0.1373(3) 0.2404(4) 0.96341(15) 0.0551(14) Uani 1 1 d . . . . . H5A H 0.0799 0.2478 0.9410 0.066 Uiso 1 1 calc R U . . . C6 C 0.1866(4) 0.3239(3) 0.97896(16) 0.0536(13) Uani 1 1 d . . . . . H6A H 0.1578 0.3803 0.9657 0.064 Uiso 1 1 calc R U . . . C7 C 0.2722(4) 0.3345(3) 1.01131(15) 0.0498(12) Uani 1 1 d . . . . . H7A H 0.2908 0.3970 1.0197 0.060 Uiso 1 1 calc R U . . . C8 C 0.4103(3) 0.2812(4) 1.16847(18) 0.0644(14) Uani 1 1 d . . . . . H8A H 0.4577 0.2997 1.1974 0.097 Uiso 1 1 calc R U . . . H8B H 0.4413 0.2453 1.1419 0.097 Uiso 1 1 calc R U . . . H8C H 0.3807 0.3372 1.1518 0.097 Uiso 1 1 calc R U . . . C9 C 0.3853(4) 0.1104(4) 1.2315(2) 0.0832(18) Uani 1 1 d . . . . . H9A H 0.4334 0.1365 1.2579 0.125 Uiso 1 1 calc R U . . . H9B H 0.3413 0.0712 1.2496 0.125 Uiso 1 1 calc R U . . . H9C H 0.4164 0.0724 1.2059 0.125 Uiso 1 1 calc R U . . . C10 C 0.2703(4) 0.2769(4) 1.25041(17) 0.0640(14) Uani 1 1 d . . . . . H10A H 0.3230 0.2958 1.2762 0.096 Uiso 1 1 calc R U . . . H10B H 0.2377 0.3327 1.2354 0.096 Uiso 1 1 calc R U . . . H10C H 0.2255 0.2384 1.2683 0.096 Uiso 1 1 calc R U . . . C11 C 0.1285(3) 0.0495(3) 1.22131(16) 0.0550(12) Uani 1 1 d . . . . . H11A H 0.0990 -0.0124 1.2226 0.082 Uiso 1 1 calc R U . . . H11B H 0.1802 0.0546 1.2498 0.082 Uiso 1 1 calc R U . . . H11C H 0.0808 0.0979 1.2260 0.082 Uiso 1 1 calc R U . . . C12 C 0.2529(5) -0.0382(3) 1.1420(2) 0.0834(19) Uani 1 1 d . . . . . H12A H 0.2171 -0.0958 1.1469 0.125 Uiso 1 1 calc R U . . . H12B H 0.2706 -0.0353 1.1053 0.125 Uiso 1 1 calc R U . . . H12C H 0.3105 -0.0378 1.1668 0.125 Uiso 1 1 calc R U . . . C13 C 0.0712(4) 0.0574(3) 1.10494(16) 0.0565(12) Uani 1 1 d . . . . . H13A H 0.0398 -0.0031 1.1085 0.085 Uiso 1 1 calc R U . . . H13B H 0.0266 0.1080 1.1110 0.085 Uiso 1 1 calc R U . . . H13C H 0.0918 0.0630 1.0690 0.085 Uiso 1 1 calc R U . . . C14 C 0.0248(3) 0.3443(3) 1.19739(14) 0.0399(9) Uani 1 1 d . . . . . H14A H 0.0363 0.3946 1.2236 0.060 Uiso 1 1 calc R U . . . H14B H -0.0417 0.3243 1.1962 0.060 Uiso 1 1 calc R U . . . H14C H 0.0666 0.2913 1.2076 0.060 Uiso 1 1 calc R U . . . C15 C -0.0205(3) 0.4987(3) 1.11988(19) 0.0550(11) Uani 1 1 d . . . . . H15A H -0.0039 0.5414 1.1497 0.083 Uiso 1 1 calc R U . . . H15B H -0.0061 0.5286 1.0866 0.083 Uiso 1 1 calc R U . . . H15C H -0.0885 0.4840 1.1181 0.083 Uiso 1 1 calc R U . . . C16 C 0.1774(3) 0.4272(3) 1.13354(15) 0.0395(8) Uani 1 1 d . . . . . H16A H 0.1883 0.4756 1.1609 0.059 Uiso 1 1 calc R U . . . H16B H 0.2193 0.3738 1.1426 0.059 Uiso 1 1 calc R U . . . H16C H 0.1910 0.4528 1.0990 0.059 Uiso 1 1 calc R U . . . C17 C -0.1151(4) 0.3807(4) 1.00089(19) 0.0741(16) Uani 1 1 d . . . . . H17A H -0.1792 0.3679 0.9843 0.111 Uiso 1 1 calc R U . . . H17B H -0.1142 0.4417 1.0186 0.111 Uiso 1 1 calc R U . . . H17C H -0.0701 0.3812 0.9735 0.111 Uiso 1 1 calc R U . . . C18 C -0.1721(3) 0.2843(3) 1.09992(17) 0.0459(10) Uani 1 1 d . . . . . H18A H -0.2350 0.2747 1.0809 0.069 Uiso 1 1 calc R U . . . H18B H -0.1580 0.2329 1.1251 0.069 Uiso 1 1 calc R U . . . H18C H -0.1714 0.3437 1.1194 0.069 Uiso 1 1 calc R U . . . C19 C -0.0954(3) 0.1750(4) 1.0135(2) 0.0687(15) Uani 1 1 d . . . . . H19A H -0.1607 0.1706 0.9968 0.103 Uiso 1 1 calc R U . . . H19B H -0.0510 0.1730 0.9859 0.103 Uiso 1 1 calc R U . . . H19C H -0.0826 0.1224 1.0380 0.103 Uiso 1 1 calc R U . . . C20 C 0.5230(3) 0.1213(3) 0.93987(18) 0.0471(10) Uani 1 1 d . . . . . H20A H 0.5824 0.0906 0.9534 0.071 Uiso 1 1 calc R U . . . H20B H 0.4743 0.1096 0.9643 0.071 Uiso 1 1 calc R U . . . H20C H 0.5017 0.0960 0.9047 0.071 Uiso 1 1 calc R U . . . C21 C 0.6402(3) 0.2628(3) 0.8890(2) 0.0568(12) Uani 1 1 d . . . . . H21A H 0.6975 0.2309 0.9045 0.085 Uiso 1 1 calc R U . . . H21B H 0.6196 0.2349 0.8543 0.085 Uiso 1 1 calc R U . . . H21C H 0.6541 0.3293 0.8842 0.085 Uiso 1 1 calc R U . . . C22 C 0.5940(3) 0.2871(3) 1.00210(18) 0.0555(12) Uani 1 1 d . . . . . H22A H 0.6529 0.2524 1.0119 0.083 Uiso 1 1 calc R U . . . H22B H 0.6077 0.3543 1.0020 0.083 Uiso 1 1 calc R U . . . H22C H 0.5481 0.2739 1.0280 0.083 Uiso 1 1 calc R U . . . C23 C 0.4566(4) 0.4360(3) 0.82081(15) 0.0541(11) Uani 1 1 d . . . . . H23A H 0.4590 0.5029 0.8124 0.081 Uiso 1 1 calc R U . . . H23B H 0.5154 0.4059 0.8120 0.081 Uiso 1 1 calc R U . . . H23C H 0.4022 0.4073 0.8000 0.081 Uiso 1 1 calc R U . . . C24 C 0.5459(3) 0.4883(3) 0.92696(16) 0.0440(9) Uani 1 1 d . . . . . H24A H 0.5421 0.5535 0.9148 0.066 Uiso 1 1 calc R U . . . H24B H 0.5436 0.4863 0.9656 0.066 Uiso 1 1 calc R U . . . H24C H 0.6057 0.4606 0.9177 0.066 Uiso 1 1 calc R U . . . C25 C 0.3360(3) 0.4893(3) 0.90782(16) 0.0418(9) Uani 1 1 d . . . . . H25A H 0.3439 0.5546 0.8972 0.063 Uiso 1 1 calc R U . . . H25B H 0.2798 0.4628 0.8876 0.063 Uiso 1 1 calc R U . . . H25C H 0.3279 0.4864 0.9459 0.063 Uiso 1 1 calc R U . . . C26 C 0.3246(3) -0.0438(3) 0.91136(16) 0.0478(10) Uani 1 1 d . . . . . H26A H 0.3339 -0.1103 0.9038 0.072 Uiso 1 1 calc R U . . . H26B H 0.3839 -0.0176 0.9284 0.072 Uiso 1 1 calc R U . . . H26C H 0.2741 -0.0370 0.9352 0.072 Uiso 1 1 calc R U . . . C27 C 0.1856(4) -0.0467(3) 0.81664(18) 0.0633(14) Uani 1 1 d . . . . . H27A H 0.2021 -0.1131 0.8142 0.095 Uiso 1 1 calc R U . . . H27B H 0.1321 -0.0397 0.8384 0.095 Uiso 1 1 calc R U . . . H27C H 0.1678 -0.0220 0.7809 0.095 Uiso 1 1 calc R U . . . C28 C 0.3896(4) -0.0035(3) 0.8048(2) 0.0683(15) Uani 1 1 d . . . . . H28A H 0.3988 -0.0711 0.8015 0.103 Uiso 1 1 calc R U . . . H28B H 0.3732 0.0234 0.7694 0.103 Uiso 1 1 calc R U . . . H28C H 0.4484 0.0252 0.8208 0.103 Uiso 1 1 calc R U . . . C29 C 0.2096(4) 0.1776(4) 0.73962(14) 0.0580(12) Uani 1 1 d . . . . . H29A H 0.1599 0.2103 0.7172 0.087 Uiso 1 1 calc R U . . . H29B H 0.2719 0.2038 0.7336 0.087 Uiso 1 1 calc R U . . . H29C H 0.2084 0.1109 0.7306 0.087 Uiso 1 1 calc R U . . . C30 C 0.0621(3) 0.1585(4) 0.81868(18) 0.0567(12) Uani 1 1 d . . . . . H30A H 0.0198 0.1932 0.7927 0.085 Uiso 1 1 calc R U . . . H30B H 0.0542 0.0913 0.8122 0.085 Uiso 1 1 calc R U . . . H30C H 0.0460 0.1733 0.8547 0.085 Uiso 1 1 calc R U . . . C31 C 0.1936(3) 0.3211(3) 0.82445(16) 0.0450(9) Uani 1 1 d . . . . . H31A H 0.1460 0.3528 0.8000 0.067 Uiso 1 1 calc R U . . . H31B H 0.1804 0.3336 0.8612 0.067 Uiso 1 1 calc R U . . . H31C H 0.2570 0.3444 0.8187 0.067 Uiso 1 1 calc R U . . . 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 0.02628(8) 0.02874(8) 0.02133(7) -0.00082(6) 0.00907(6) -0.00011(6) Dy2 0.02530(8) 0.02723(8) 0.01846(7) -0.00184(5) 0.00692(5) -0.00298(6) K1 0.0600(6) 0.0621(6) 0.0366(4) -0.0184(4) 0.0240(4) -0.0189(5) Si1 0.0349(6) 0.0584(7) 0.0294(5) 0.0098(5) 0.0039(4) 0.0055(5) Si2 0.0597(7) 0.0281(5) 0.0383(5) 0.0055(4) 0.0248(5) 0.0035(5) Si3 0.0354(5) 0.0300(5) 0.0293(5) 0.0003(4) 0.0111(4) 0.0057(4) Si4 0.0280(5) 0.0543(7) 0.0329(5) 0.0060(4) 0.0036(4) -0.0009(5) Si5 0.0256(5) 0.0316(5) 0.0422(5) -0.0036(4) 0.0052(4) 0.0009(4) Si6 0.0335(5) 0.0288(5) 0.0265(4) 0.0009(4) 0.0069(4) -0.0056(4) Si7 0.0481(6) 0.0294(5) 0.0321(5) -0.0086(4) 0.0106(4) -0.0078(4) Si8 0.0384(6) 0.0411(5) 0.0240(4) 0.0013(4) -0.0005(4) -0.0086(4) N1 0.0352(16) 0.0313(15) 0.0270(14) 0.0049(11) 0.0138(12) 0.0063(12) N2 0.0259(14) 0.0390(16) 0.0263(13) -0.0006(12) 0.0075(11) 0.0006(12) N3 0.0250(14) 0.0284(14) 0.0265(13) -0.0023(11) 0.0074(11) -0.0025(11) N4 0.0321(15) 0.0280(14) 0.0205(12) -0.0041(10) 0.0050(11) -0.0061(12) C1 0.035(2) 0.109(4) 0.0235(18) -0.008(2) 0.0104(16) -0.028(3) C2 0.047(3) 0.092(4) 0.032(2) 0.020(2) 0.0190(19) 0.033(3) C3 0.110(4) 0.028(2) 0.047(2) 0.0055(17) 0.050(3) 0.014(2) C4 0.068(3) 0.072(3) 0.038(2) -0.027(2) 0.033(2) -0.050(3) C5 0.0233(19) 0.120(5) 0.0220(17) -0.001(2) 0.0044(14) 0.010(2) C6 0.079(3) 0.046(2) 0.041(2) 0.0173(19) 0.036(2) 0.031(2) C7 0.080(3) 0.038(2) 0.037(2) -0.0138(17) 0.035(2) -0.025(2) C8 0.048(3) 0.104(4) 0.039(2) 0.007(2) -0.005(2) -0.023(3) C9 0.064(3) 0.102(5) 0.082(4) 0.042(3) -0.005(3) 0.025(3) C10 0.063(3) 0.094(4) 0.034(2) -0.014(2) -0.002(2) 0.000(3) C11 0.069(3) 0.058(3) 0.042(2) 0.010(2) 0.025(2) -0.006(2) C12 0.123(5) 0.041(3) 0.096(4) 0.011(3) 0.060(4) 0.026(3) C13 0.082(3) 0.048(2) 0.042(2) -0.0002(19) 0.018(2) -0.024(2) C14 0.046(2) 0.046(2) 0.0297(18) -0.0001(15) 0.0104(16) 0.0017(18) C15 0.059(3) 0.042(2) 0.065(3) 0.003(2) 0.013(2) 0.016(2) C16 0.044(2) 0.0347(19) 0.040(2) -0.0065(15) 0.0066(17) -0.0019(17) C17 0.060(3) 0.102(4) 0.057(3) 0.035(3) -0.013(2) -0.010(3) C18 0.0273(19) 0.060(3) 0.051(2) 0.007(2) 0.0095(17) 0.0000(18) C19 0.043(3) 0.098(4) 0.066(3) -0.027(3) 0.004(2) -0.016(3) C20 0.044(2) 0.036(2) 0.062(3) -0.0003(18) 0.008(2) 0.0069(18) C21 0.038(2) 0.050(3) 0.086(4) -0.004(2) 0.026(2) 0.004(2) C22 0.046(3) 0.057(3) 0.060(3) -0.003(2) -0.017(2) 0.000(2) C23 0.073(3) 0.056(3) 0.035(2) 0.0120(19) 0.014(2) -0.012(2) C24 0.045(2) 0.033(2) 0.054(2) -0.0044(17) 0.0085(19) -0.0127(17) C25 0.044(2) 0.0310(19) 0.051(2) 0.0031(16) 0.0079(18) 0.0057(17) C26 0.061(3) 0.0295(19) 0.052(2) -0.0004(17) 0.001(2) 0.0019(18) C27 0.085(4) 0.045(3) 0.056(3) -0.001(2) -0.016(3) -0.022(2) C28 0.092(4) 0.044(3) 0.077(3) -0.021(2) 0.048(3) -0.005(3) C29 0.080(3) 0.070(3) 0.0239(18) -0.0017(19) 0.002(2) -0.012(3) C30 0.041(2) 0.072(3) 0.055(3) 0.008(2) -0.007(2) -0.014(2) C31 0.049(2) 0.044(2) 0.041(2) 0.0062(17) 0.0026(18) 0.0038(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 2.283(3) . ? Dy1 N1 2.290(3) . ? Dy1 C7 2.573(4) . ? Dy1 C4 2.576(4) . ? Dy1 C1 2.578(4) . ? Dy1 C3 2.600(4) . ? Dy1 C6 2.631(4) . ? Dy1 C5 2.640(4) . ? Dy1 C2 2.645(4) . ? Dy1 Si2 3.2328(10) . ? Dy1 Si3 3.2957(9) . ? Dy2 N3 2.346(3) . ? Dy2 N4 2.352(2) . ? Dy2 C2 2.514(4) . ? Dy2 C6 2.525(4) . ? Dy2 C5 2.536(4) . ? Dy2 C3 2.558(4) . ? Dy2 C1 2.566(4) . ? Dy2 C7 2.580(4) . ? Dy2 C4 2.596(4) . ? Dy2 Si8 3.3707(9) . ? Dy2 Si5 3.4095(10) . ? Dy2 K1 3.8752(8) . ? K1 N3 2.923(3) . ? K1 N4 2.952(3) . ? K1 C23 3.187(5) . ? K1 C28 3.197(5) . ? K1 C14 3.232(4) 4_665 ? K1 C21 3.455(5) . ? K1 Si5 3.4737(14) . ? K1 C29 3.529(5) . ? K1 Si8 3.5467(15) . ? K1 Si6 3.6727(13) . ? K1 Si7 3.6894(14) . ? Si1 N1 1.719(3) . ? Si1 C8 1.856(5) . ? Si1 C10 1.869(5) . ? Si1 C9 1.873(5) . ? Si2 N1 1.704(3) . ? Si2 C11 1.875(4) . ? Si2 C12 1.877(5) . ? Si2 C13 1.877(5) . ? Si3 N2 1.697(3) . ? Si3 C16 1.874(4) . ? Si3 C15 1.878(4) . ? Si3 C14 1.879(4) . ? Si4 N2 1.721(3) . ? Si4 C19 1.870(5) . ? Si4 C18 1.872(4) . ? Si4 C17 1.873(5) . ? Si5 N3 1.721(3) . ? Si5 C22 1.864(4) . ? Si5 C20 1.872(4) . ? Si5 C21 1.875(4) . ? Si6 N3 1.723(3) . ? Si6 C25 1.868(4) . ? Si6 C24 1.870(4) . ? Si6 C23 1.883(4) . ? Si7 N4 1.717(3) . ? Si7 C26 1.862(4) . ? Si7 C27 1.873(4) . ? Si7 C28 1.882(4) . ? Si8 N4 1.719(3) . ? Si8 C31 1.866(4) . ? Si8 C30 1.870(4) . ? Si8 C29 1.887(4) . ? C1 C2 1.383(7) . ? C1 C7 1.396(7) . ? C2 C3 1.392(7) . ? C3 C4 1.427(7) . ? C4 C5 1.415(7) . ? C5 C6 1.419(7) . ? C6 C7 1.404(7) . ? C14 K1 3.232(4) 4_566 ? 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 106.28(10) . . ? N2 Dy1 C7 110.97(14) . . ? N1 Dy1 C7 121.98(14) . . ? N2 Dy1 C4 112.81(15) . . ? N1 Dy1 C4 126.36(16) . . ? C7 Dy1 C4 75.79(12) . . ? N2 Dy1 C1 140.98(15) . . ? N1 Dy1 C1 96.24(13) . . ? C7 Dy1 C1 31.44(15) . . ? C4 Dy1 C1 75.38(13) . . ? N2 Dy1 C3 143.94(16) . . ? N1 Dy1 C3 98.94(13) . . ? C7 Dy1 C3 74.78(13) . . ? C4 Dy1 C3 32.02(16) . . ? C1 Dy1 C3 57.73(16) . . ? N2 Dy1 C6 92.74(12) . . ? N1 Dy1 C6 153.10(14) . . ? C7 Dy1 C6 31.27(15) . . ? C4 Dy1 C6 58.46(16) . . ? C1 Dy1 C6 57.83(15) . . ? C3 Dy1 C6 74.25(12) . . ? N2 Dy1 C5 93.34(11) . . ? N1 Dy1 C5 157.05(13) . . ? C7 Dy1 C5 58.45(15) . . ? C4 Dy1 C5 31.44(16) . . ? C1 Dy1 C5 74.51(12) . . ? C3 Dy1 C5 58.26(15) . . ? C6 Dy1 C5 31.24(16) . . ? N2 Dy1 C2 165.80(11) . . ? N1 Dy1 C2 87.66(11) . . ? C7 Dy1 C2 57.58(16) . . ? C4 Dy1 C2 58.31(16) . . ? C1 Dy1 C2 30.68(16) . . ? C3 Dy1 C2 30.78(16) . . ? C6 Dy1 C2 73.21(13) . . ? C5 Dy1 C2 73.64(12) . . ? N2 Dy1 Si2 101.20(7) . . ? N1 Dy1 Si2 30.24(8) . . ? C7 Dy1 Si2 144.77(12) . . ? C4 Dy1 Si2 105.04(12) . . ? C1 Dy1 Si2 113.67(12) . . ? C3 Dy1 Si2 87.78(9) . . ? C6 Dy1 Si2 161.97(9) . . ? C5 Dy1 Si2 135.04(13) . . ? C2 Dy1 Si2 92.19(10) . . ? N2 Dy1 Si3 28.75(7) . . ? N1 Dy1 Si3 89.91(7) . . ? C7 Dy1 Si3 102.30(10) . . ? C4 Dy1 Si3 139.15(14) . . ? C1 Dy1 Si3 123.62(13) . . ? C3 Dy1 Si3 170.91(12) . . ? C6 Dy1 Si3 98.71(9) . . ? C5 Dy1 Si3 112.79(11) . . ? C2 Dy1 Si3 153.23(14) . . ? Si2 Dy1 Si3 99.01(3) . . ? N3 Dy2 N4 98.31(9) . . ? N3 Dy2 C2 110.55(14) . . ? N4 Dy2 C2 129.06(15) . . ? N3 Dy2 C6 114.99(14) . . ? N4 Dy2 C6 126.93(14) . . ? C2 Dy2 C6 77.28(13) . . ? N3 Dy2 C5 146.06(15) . . ? N4 Dy2 C5 100.95(12) . . ? C2 Dy2 C5 77.69(13) . . ? C6 Dy2 C5 32.58(16) . . ? N3 Dy2 C3 140.28(15) . . ? N4 Dy2 C3 103.39(13) . . ? C2 Dy2 C3 31.86(16) . . ? C6 Dy2 C3 76.80(13) . . ? C5 Dy2 C3 60.10(16) . . ? N3 Dy2 C1 93.68(11) . . ? N4 Dy2 C1 160.61(14) . . ? C2 Dy2 C1 31.58(17) . . ? C6 Dy2 C1 59.32(16) . . ? C5 Dy2 C1 76.51(13) . . ? C3 Dy2 C1 58.40(16) . . ? N3 Dy2 C7 95.30(11) . . ? N4 Dy2 C7 158.83(14) . . ? C2 Dy2 C7 59.13(16) . . ? C6 Dy2 C7 31.90(16) . . ? C5 Dy2 C7 59.68(15) . . ? C3 Dy2 C7 75.38(13) . . ? C1 Dy2 C7 31.47(15) . . ? N3 Dy2 C4 168.92(11) . . ? N4 Dy2 C4 92.37(11) . . ? C2 Dy2 C4 59.70(17) . . ? C6 Dy2 C4 59.54(16) . . ? C5 Dy2 C4 31.97(16) . . ? C3 Dy2 C4 32.15(16) . . ? C1 Dy2 C4 75.24(13) . . ? C7 Dy2 C4 75.33(12) . . ? N3 Dy2 Si8 100.34(7) . . ? N4 Dy2 Si8 28.46(7) . . ? C2 Dy2 Si8 146.21(14) . . ? C6 Dy2 Si8 102.20(12) . . ? C5 Dy2 Si8 84.39(9) . . ? C3 Dy2 Si8 114.52(13) . . ? C1 Dy2 Si8 160.58(10) . . ? C7 Dy2 Si8 132.51(12) . . ? C4 Dy2 Si8 90.46(10) . . ? N3 Dy2 Si5 27.69(7) . . ? N4 Dy2 Si5 99.94(7) . . ? C2 Dy2 Si5 89.20(11) . . ? C6 Dy2 Si5 128.81(13) . . ? C5 Dy2 Si5 159.11(10) . . ? C3 Dy2 Si5 114.65(14) . . ? C1 Dy2 Si5 83.79(9) . . ? C7 Dy2 Si5 99.64(11) . . ? C4 Dy2 Si5 146.80(14) . . ? Si8 Dy2 Si5 114.64(3) . . ? N3 Dy2 K1 48.80(6) . . ? N4 Dy2 K1 49.51(7) . . ? C2 Dy2 K1 138.23(9) . . ? C6 Dy2 K1 141.68(9) . . ? C5 Dy2 K1 141.66(9) . . ? C3 Dy2 K1 139.88(9) . . ? C1 Dy2 K1 139.93(9) . . ? C7 Dy2 K1 141.39(9) . . ? C4 Dy2 K1 141.77(8) . . ? Si8 Dy2 K1 58.11(2) . . ? Si5 Dy2 K1 56.53(2) . . ? N3 K1 N4 74.45(7) . . ? N3 K1 C23 58.14(9) . . ? N4 K1 C23 112.85(10) . . ? N3 K1 C28 114.92(11) . . ? N4 K1 C28 57.59(10) . . ? C23 K1 C28 170.37(12) . . ? N3 K1 C14 155.34(10) . 4_665 ? N4 K1 C14 129.32(9) . 4_665 ? C23 K1 C14 108.81(10) . 4_665 ? C28 K1 C14 80.12(11) . 4_665 ? N3 K1 C21 55.41(9) . . ? N4 K1 C21 117.94(10) . . ? C23 K1 C21 71.19(12) . . ? C28 K1 C21 111.22(14) . . ? C14 K1 C21 101.73(11) 4_665 . ? N3 K1 Si5 29.65(6) . . ? N4 K1 Si5 87.61(6) . . ? C23 K1 Si5 74.06(8) . . ? C28 K1 Si5 102.99(11) . . ? C14 K1 Si5 131.57(8) 4_665 . ? C21 K1 Si5 31.41(8) . . ? N3 K1 C29 115.39(9) . . ? N4 K1 C29 54.55(8) . . ? C23 K1 C29 105.72(13) . . ? C28 K1 C29 70.36(14) . . ? C14 K1 C29 87.56(10) 4_665 . ? C21 K1 C29 170.71(10) . . ? Si5 K1 C29 139.67(7) . . ? N3 K1 Si8 86.07(6) . . ? N4 K1 Si8 28.85(6) . . ? C23 K1 Si8 99.31(10) . . ? C28 K1 Si8 72.73(10) . . ? C14 K1 Si8 117.91(8) 4_665 . ? C21 K1 Si8 139.96(8) . . ? Si5 K1 Si8 108.75(3) . . ? C29 K1 Si8 30.93(7) . . ? N3 K1 Si6 27.38(6) . . ? N4 K1 Si6 91.62(6) . . ? C23 K1 Si6 30.84(7) . . ? C28 K1 Si6 141.59(9) . . ? C14 K1 Si6 137.07(8) 4_665 . ? C21 K1 Si6 60.41(8) . . ? Si5 K1 Si6 48.70(2) . . ? C29 K1 Si6 112.34(9) . . ? Si8 K1 Si6 91.12(3) . . ? N3 K1 Si7 91.82(6) . . ? N4 K1 Si7 27.18(6) . . ? C23 K1 Si7 139.71(9) . . ? C28 K1 Si7 30.66(8) . . ? C14 K1 Si7 108.19(8) 4_665 . ? C21 K1 Si7 115.71(9) . . ? Si5 K1 Si7 92.82(3) . . ? C29 K1 Si7 60.67(8) . . ? Si8 K1 Si7 48.32(3) . . ? Si6 K1 Si7 114.73(3) . . ? N3 K1 Dy2 37.15(5) . . ? N4 K1 Dy2 37.30(5) . . ? C23 K1 Dy2 85.04(7) . . ? C28 K1 Dy2 85.82(8) . . ? C14 K1 Dy2 165.59(8) 4_665 . ? C21 K1 Dy2 86.27(8) . . ? Si5 K1 Dy2 54.96(2) . . ? C29 K1 Dy2 84.71(7) . . ? Si8 K1 Dy2 53.80(2) . . ? Si6 K1 Dy2 57.339(19) . . ? Si7 K1 Dy2 57.40(2) . . ? N1 Si1 C8 113.35(17) . . ? N1 Si1 C10 113.14(19) . . ? C8 Si1 C10 106.8(3) . . ? N1 Si1 C9 114.2(2) . . ? C8 Si1 C9 104.7(3) . . ? C10 Si1 C9 103.8(3) . . ? N1 Si2 C11 113.79(18) . . ? N1 Si2 C12 114.7(2) . . ? C11 Si2 C12 108.9(2) . . ? N1 Si2 C13 108.58(17) . . ? C11 Si2 C13 104.9(2) . . ? C12 Si2 C13 105.1(3) . . ? N1 Si2 Dy1 42.58(10) . . ? C11 Si2 Dy1 135.00(15) . . ? C12 Si2 Dy1 115.98(17) . . ? C13 Si2 Dy1 67.37(13) . . ? N2 Si3 C16 109.17(15) . . ? N2 Si3 C15 117.00(18) . . ? C16 Si3 C15 104.5(2) . . ? N2 Si3 C14 112.08(17) . . ? C16 Si3 C14 108.59(18) . . ? C15 Si3 C14 104.97(19) . . ? N2 Si3 Dy1 40.31(10) . . ? C16 Si3 Dy1 72.00(12) . . ? C15 Si3 Dy1 143.22(15) . . ? C14 Si3 Dy1 110.83(13) . . ? N2 Si4 C19 114.33(19) . . ? N2 Si4 C18 111.49(16) . . ? C19 Si4 C18 104.9(2) . . ? N2 Si4 C17 112.8(2) . . ? C19 Si4 C17 104.9(3) . . ? C18 Si4 C17 107.8(2) . . ? N3 Si5 C22 115.92(18) . . ? N3 Si5 C20 109.58(17) . . ? C22 Si5 C20 105.1(2) . . ? N3 Si5 C21 113.11(19) . . ? C22 Si5 C21 107.0(2) . . ? C20 Si5 C21 105.3(2) . . ? N3 Si5 Dy2 39.30(9) . . ? C22 Si5 Dy2 109.60(16) . . ? C20 Si5 Dy2 74.77(13) . . ? C21 Si5 Dy2 141.95(17) . . ? N3 Si5 K1 57.16(9) . . ? C22 Si5 K1 171.59(15) . . ? C20 Si5 K1 82.51(14) . . ? C21 Si5 K1 73.74(17) . . ? Dy2 Si5 K1 68.52(2) . . ? N3 Si6 C25 114.28(16) . . ? N3 Si6 C24 115.74(16) . . ? C25 Si6 C24 104.74(19) . . ? N3 Si6 C23 111.28(17) . . ? C25 Si6 C23 106.1(2) . . ? C24 Si6 C23 103.6(2) . . ? N3 Si6 K1 51.30(9) . . ? C25 Si6 K1 123.85(13) . . ? C24 Si6 K1 131.05(14) . . ? C23 Si6 K1 60.18(14) . . ? N4 Si7 C26 114.98(16) . . ? N4 Si7 C27 114.59(19) . . ? C26 Si7 C27 104.4(2) . . ? N4 Si7 C28 111.14(18) . . ? C26 Si7 C28 105.4(2) . . ? C27 Si7 C28 105.5(2) . . ? N4 Si7 K1 51.74(10) . . ? C26 Si7 K1 120.41(14) . . ? C27 Si7 K1 134.92(15) . . ? C28 Si7 K1 60.06(15) . . ? N4 Si8 C31 109.13(16) . . ? N4 Si8 C30 115.34(18) . . ? C31 Si8 C30 105.3(2) . . ? N4 Si8 C29 113.37(19) . . ? C31 Si8 C29 105.6(2) . . ? C30 Si8 C29 107.4(2) . . ? N4 Si8 Dy2 40.70(9) . . ? C31 Si8 Dy2 72.59(12) . . ? C30 Si8 Dy2 109.55(14) . . ? C29 Si8 Dy2 142.07(16) . . ? N4 Si8 K1 55.99(10) . . ? C31 Si8 K1 83.78(14) . . ? C30 Si8 K1 169.71(16) . . ? C29 Si8 K1 74.03(16) . . ? Dy2 Si8 K1 68.09(2) . . ? Si2 N1 Si1 119.50(16) . . ? Si2 N1 Dy1 107.17(15) . . ? Si1 N1 Dy1 133.15(16) . . ? Si3 N2 Si4 119.80(17) . . ? Si3 N2 Dy1 110.93(14) . . ? Si4 N2 Dy1 129.22(15) . . ? Si5 N3 Si6 118.01(16) . . ? Si5 N3 Dy2 113.01(13) . . ? Si6 N3 Dy2 125.32(14) . . ? Si5 N3 K1 93.19(11) . . ? Si6 N3 K1 101.32(11) . . ? Dy2 N3 K1 94.05(9) . . ? Si7 N4 Si8 119.24(15) . . ? Si7 N4 Dy2 125.93(14) . . ? Si8 N4 Dy2 110.84(13) . . ? Si7 N4 K1 101.08(12) . . ? Si8 N4 K1 95.16(11) . . ? Dy2 N4 K1 93.19(9) . . ? C2 C1 C7 129.5(4) . . ? C2 C1 Dy2 72.1(2) . . ? C7 C1 Dy2 74.8(2) . . ? C2 C1 Dy1 77.3(2) . . ? C7 C1 Dy1 74.1(2) . . ? Dy2 C1 Dy1 102.72(14) . . ? C1 C2 C3 128.5(4) . . ? C1 C2 Dy2 76.3(2) . . ? C3 C2 Dy2 75.8(2) . . ? C1 C2 Dy1 72.0(2) . . ? C3 C2 Dy1 72.8(2) . . ? Dy2 C2 Dy1 102.30(14) . . ? C2 C3 C4 128.9(4) . . ? C2 C3 Dy2 72.3(2) . . ? C4 C3 Dy2 75.4(2) . . ? C2 C3 Dy1 76.4(2) . . ? C4 C3 Dy1 73.1(2) . . ? Dy2 C3 Dy1 102.36(14) . . ? C5 C4 C3 127.7(4) . . ? C5 C4 Dy1 76.8(2) . . ? C3 C4 Dy1 74.9(2) . . ? C5 C4 Dy2 71.7(2) . . ? C3 C4 Dy2 72.4(2) . . ? Dy1 C4 Dy2 101.94(13) . . ? C4 C5 C6 127.7(4) . . ? C4 C5 Dy2 76.4(2) . . ? C6 C5 Dy2 73.3(2) . . ? C4 C5 Dy1 71.8(2) . . ? C6 C5 Dy1 74.0(2) . . ? Dy2 C5 Dy1 101.83(13) . . ? C7 C6 C5 128.8(4) . . ? C7 C6 Dy2 76.2(2) . . ? C5 C6 Dy2 74.2(2) . . ? C7 C6 Dy1 72.1(2) . . ? C5 C6 Dy1 74.7(2) . . ? Dy2 C6 Dy1 102.39(14) . . ? C1 C7 C6 128.3(4) . . ? C1 C7 Dy1 74.5(2) . . ? C6 C7 Dy1 76.6(2) . . ? C1 C7 Dy2 73.7(2) . . ? C6 C7 Dy2 71.9(2) . . ? Dy1 C7 Dy2 102.49(13) . . ? Si3 C14 K1 168.2(2) . 4_566 ? Si5 C21 K1 74.85(15) . . ? Si6 C23 K1 88.98(15) . . ? Si7 C28 K1 89.28(16) . . ? Si8 C29 K1 75.05(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Si2 N1 Si1 52.7(3) . . . . ? C12 Si2 N1 Si1 -73.6(3) . . . . ? C13 Si2 N1 Si1 169.1(2) . . . . ? Dy1 Si2 N1 Si1 -175.9(3) . . . . ? C11 Si2 N1 Dy1 -131.47(19) . . . . ? C12 Si2 N1 Dy1 102.2(2) . . . . ? C13 Si2 N1 Dy1 -15.0(2) . . . . ? C8 Si1 N1 Si2 147.9(2) . . . . ? C10 Si1 N1 Si2 -90.4(3) . . . . ? C9 Si1 N1 Si2 28.0(3) . . . . ? C8 Si1 N1 Dy1 -26.7(3) . . . . ? C10 Si1 N1 Dy1 95.0(3) . . . . ? C9 Si1 N1 Dy1 -146.6(3) . . . . ? C16 Si3 N2 Si4 -154.09(19) . . . . ? C15 Si3 N2 Si4 -35.7(3) . . . . ? C14 Si3 N2 Si4 85.6(2) . . . . ? Dy1 Si3 N2 Si4 -177.8(3) . . . . ? C16 Si3 N2 Dy1 23.7(2) . . . . ? C15 Si3 N2 Dy1 142.09(19) . . . . ? C14 Si3 N2 Dy1 -96.60(18) . . . . ? C19 Si4 N2 Si3 -164.9(2) . . . . ? C18 Si4 N2 Si3 -46.1(3) . . . . ? C17 Si4 N2 Si3 75.4(3) . . . . ? C19 Si4 N2 Dy1 17.7(3) . . . . ? C18 Si4 N2 Dy1 136.5(2) . . . . ? C17 Si4 N2 Dy1 -102.0(3) . . . . ? C22 Si5 N3 Si6 69.9(2) . . . . ? C20 Si5 N3 Si6 -171.39(19) . . . . ? C21 Si5 N3 Si6 -54.3(2) . . . . ? Dy2 Si5 N3 Si6 159.6(2) . . . . ? K1 Si5 N3 Si6 -104.62(17) . . . . ? C22 Si5 N3 Dy2 -89.7(2) . . . . ? C20 Si5 N3 Dy2 29.0(2) . . . . ? C21 Si5 N3 Dy2 146.14(18) . . . . ? K1 Si5 N3 Dy2 95.77(13) . . . . ? C22 Si5 N3 K1 174.51(18) . . . . ? C20 Si5 N3 K1 -66.78(17) . . . . ? C21 Si5 N3 K1 50.37(19) . . . . ? Dy2 Si5 N3 K1 -95.77(13) . . . . ? C25 Si6 N3 Si5 -145.23(18) . . . . ? C24 Si6 N3 Si5 -23.4(2) . . . . ? C23 Si6 N3 Si5 94.6(2) . . . . ? K1 Si6 N3 Si5 99.83(18) . . . . ? C25 Si6 N3 Dy2 11.6(2) . . . . ? C24 Si6 N3 Dy2 133.46(19) . . . . ? C23 Si6 N3 Dy2 -108.6(2) . . . . ? K1 Si6 N3 Dy2 -103.31(17) . . . . ? C25 Si6 N3 K1 114.94(16) . . . . ? C24 Si6 N3 K1 -123.23(16) . . . . ? C23 Si6 N3 K1 -5.3(2) . . . . ? C26 Si7 N4 Si8 -147.5(2) . . . . ? C27 Si7 N4 Si8 -26.5(3) . . . . ? C28 Si7 N4 Si8 92.9(3) . . . . ? K1 Si7 N4 Si8 102.40(18) . . . . ? C26 Si7 N4 Dy2 7.9(3) . . . . ? C27 Si7 N4 Dy2 128.9(2) . . . . ? C28 Si7 N4 Dy2 -111.7(2) . . . . ? K1 Si7 N4 Dy2 -102.23(18) . . . . ? C26 Si7 N4 K1 110.11(18) . . . . ? C27 Si7 N4 K1 -128.91(19) . . . . ? C28 Si7 N4 K1 -9.4(2) . . . . ? C31 Si8 N4 Si7 -173.90(19) . . . . ? C30 Si8 N4 Si7 67.8(3) . . . . ? C29 Si8 N4 Si7 -56.6(2) . . . . ? Dy2 Si8 N4 Si7 158.8(3) . . . . ? K1 Si8 N4 Si7 -105.77(18) . . . . ? C31 Si8 N4 Dy2 27.3(2) . . . . ? C30 Si8 N4 Dy2 -91.0(2) . . . . ? C29 Si8 N4 Dy2 144.61(18) . . . . ? K1 Si8 N4 Dy2 95.40(12) . . . . ? C31 Si8 N4 K1 -68.13(16) . . . . ? C30 Si8 N4 K1 173.61(18) . . . . ? C29 Si8 N4 K1 49.21(19) . . . . ? Dy2 Si8 N4 K1 -95.40(13) . . . . ? C7 C1 C2 C3 -7.5(7) . . . . ? Dy2 C1 C2 C3 -59.0(4) . . . . ? Dy1 C1 C2 C3 49.1(4) . . . . ? C7 C1 C2 Dy2 51.4(4) . . . . ? Dy1 C1 C2 Dy2 108.04(12) . . . . ? C7 C1 C2 Dy1 -56.6(4) . . . . ? Dy2 C1 C2 Dy1 -108.04(12) . . . . ? C1 C2 C3 C4 5.8(7) . . . . ? Dy2 C2 C3 C4 -53.4(4) . . . . ? Dy1 C2 C3 C4 54.6(4) . . . . ? C1 C2 C3 Dy2 59.2(4) . . . . ? Dy1 C2 C3 Dy2 107.95(12) . . . . ? C1 C2 C3 Dy1 -48.8(4) . . . . ? Dy2 C2 C3 Dy1 -107.95(12) . . . . ? C2 C3 C4 C5 3.6(7) . . . . ? Dy2 C3 C4 C5 -48.6(4) . . . . ? Dy1 C3 C4 C5 59.5(4) . . . . ? C2 C3 C4 Dy1 -55.9(4) . . . . ? Dy2 C3 C4 Dy1 -108.07(12) . . . . ? C2 C3 C4 Dy2 52.2(4) . . . . ? Dy1 C3 C4 Dy2 108.07(12) . . . . ? C3 C4 C5 C6 -7.0(7) . . . . ? Dy1 C4 C5 C6 51.7(4) . . . . ? Dy2 C4 C5 C6 -55.9(4) . . . . ? C3 C4 C5 Dy2 48.9(4) . . . . ? Dy1 C4 C5 Dy2 107.57(11) . . . . ? C3 C4 C5 Dy1 -58.7(4) . . . . ? Dy2 C4 C5 Dy1 -107.57(11) . . . . ? C4 C5 C6 C7 0.2(7) . . . . ? Dy2 C5 C6 C7 -56.9(4) . . . . ? Dy1 C5 C6 C7 51.1(4) . . . . ? C4 C5 C6 Dy2 57.1(4) . . . . ? Dy1 C5 C6 Dy2 107.98(11) . . . . ? C4 C5 C6 Dy1 -50.9(4) . . . . ? Dy2 C5 C6 Dy1 -107.98(11) . . . . ? C2 C1 C7 C6 -0.5(7) . . . . ? Dy2 C1 C7 C6 50.0(4) . . . . ? Dy1 C1 C7 C6 -58.4(4) . . . . ? C2 C1 C7 Dy1 57.9(4) . . . . ? Dy2 C1 C7 Dy1 108.35(11) . . . . ? C2 C1 C7 Dy2 -50.4(4) . . . . ? Dy1 C1 C7 Dy2 -108.35(11) . . . . ? C5 C6 C7 C1 5.4(7) . . . . ? Dy2 C6 C7 C1 -50.7(4) . . . . ? Dy1 C6 C7 C1 57.5(4) . . . . ? C5 C6 C7 Dy1 -52.1(4) . . . . ? Dy2 C6 C7 Dy1 -108.15(11) . . . . ? C5 C6 C7 Dy2 56.1(4) . . . . ? Dy1 C6 C7 Dy2 108.15(11) . . . . ? N2 Si3 C14 K1 -90.6(9) . . . 4_566 ? C16 Si3 C14 K1 148.8(9) . . . 4_566 ? C15 Si3 C14 K1 37.4(10) . . . 4_566 ? Dy1 Si3 C14 K1 -134.0(9) . . . 4_566 ? N3 Si5 C21 K1 -42.38(14) . . . . ? C22 Si5 C21 K1 -171.25(16) . . . . ? C20 Si5 C21 K1 77.26(16) . . . . ? Dy2 Si5 C21 K1 -7.4(2) . . . . ? N3 Si6 C23 K1 4.74(18) . . . . ? C25 Si6 C23 K1 -120.16(15) . . . . ? C24 Si6 C23 K1 129.78(15) . . . . ? N4 Si7 C28 K1 8.6(2) . . . . ? C26 Si7 C28 K1 -116.59(16) . . . . ? C27 Si7 C28 K1 133.31(17) . . . . ? N4 Si8 C29 K1 -40.75(15) . . . . ? C31 Si8 C29 K1 78.65(16) . . . . ? C30 Si8 C29 K1 -169.36(17) . . . . ? Dy2 Si8 C29 K1 -2.9(3) . . . . ? _refine_diff_density_max 1.430 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.098 _shelx_res_file ; mm462.res created by SHELXL-2014/7 TITL mm462 in P2(1)/n CELL 0.71073 14.12590 14.29540 25.23430 90.0000 95.2741 90.0000 ZERR 4.00 0.00040 0.00040 0.00060 0.0000 0.0013 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N SI K DY UNIT 124 316 16 32 4 8 TEMP -73.150 SIZE 0.12 0.14 0.21 L.S. 80 ACTA CONF BOND FMAP 2 PLAN 5 LIST 0 OMIT 4 3 2 OMIT -1 8 1 OMIT 3 6 5 OMIT 2 5 4 OMIT 2 1 4 OMIT 3 4 5 OMIT 6 3 8 OMIT 0 11 4 OMIT 6 1 8 OMIT 3 4 1 OMIT 4 5 8 OMIT 1 6 3 OMIT 0 5 2 OMIT 5 0 1 OMIT -1 1 30 OMIT 1 0 3 OMIT 1 1 24 OMIT 4 4 8 OMIT 9 6 5 OMIT 2 5 0 OMIT 1 4 4 OMIT 3 2 1 OMIT 7 6 1 OMIT 6 7 8 OMIT 2 7 0 OMIT 2 10 4 OMIT 1 2 3 OMIT 1 0 5 OMIT 3 8 5 OMIT 3 10 5 OMIT 5 2 1 OMIT 7 2 9 OMIT 1 1 0 OMIT 6 3 2 OMIT 2 11 6 OMIT -3 1 7 OMIT 6 5 8 OMIT -1 1 24 OMIT 6 1 4 OMIT 2 7 8 OMIT 9 0 7 OMIT 0 2 31 OMIT 6 9 0 OMIT 1 1 26 OMIT -3 8 3 OMIT 0 2 23 OMIT 0 3 2 OMIT -1 1 2 OMIT 4 5 7 OMIT -1 3 30 WGHT 0.024800 8.875999 FVAR 0.04111 DY1 6 0.171218 0.231470 1.067924 11.00000 0.02628 0.02874 = 0.02133 -0.00082 0.00907 -0.00011 DY2 6 0.303107 0.224875 0.933517 11.00000 0.02530 0.02723 = 0.01846 -0.00184 0.00692 -0.00298 K1 5 0.437124 0.215208 0.806352 11.00000 0.06002 0.06208 = 0.03659 -0.01842 0.02403 -0.01887 SI1 4 0.317779 0.207894 1.195764 11.00000 0.03488 0.05840 = 0.02942 0.00977 0.00389 0.00554 SI2 4 0.177319 0.065641 1.155274 11.00000 0.05968 0.02814 = 0.03828 0.00553 0.02484 0.00345 SI3 4 0.050417 0.388014 1.129961 11.00000 0.03536 0.03001 = 0.02933 0.00030 0.01108 0.00571 SI4 4 -0.080037 0.287520 1.051084 11.00000 0.02795 0.05430 = 0.03292 0.00604 0.00365 -0.00091 SI5 4 0.543262 0.250218 0.934518 11.00000 0.02562 0.03163 = 0.04221 -0.00358 0.00522 0.00090 SI6 4 0.443551 0.420791 0.893894 11.00000 0.03348 0.02878 = 0.02654 0.00089 0.00690 -0.00560 SI7 4 0.290520 0.019636 0.848036 11.00000 0.04810 0.02943 = 0.03210 -0.00856 0.01065 -0.00784 SI8 4 0.188190 0.192485 0.811836 11.00000 0.03838 0.04111 = 0.02400 0.00128 -0.00046 -0.00857 N1 3 0.230670 0.171279 1.148257 11.00000 0.03520 0.03128 = 0.02699 0.00491 0.01379 0.00629 N2 3 0.032099 0.304268 1.082436 11.00000 0.02588 0.03903 = 0.02632 -0.00061 0.00750 0.00059 N3 3 0.438989 0.304207 0.910729 11.00000 0.02502 0.02842 = 0.02651 -0.00230 0.00745 -0.00250 N4 3 0.271757 0.137552 0.854864 11.00000 0.03215 0.02804 = 0.02048 -0.00406 0.00495 -0.00608 C1 1 0.333549 0.264815 1.032763 11.00000 0.03532 0.10862 = 0.02349 -0.00845 0.01036 -0.02780 AFIX 43 H1A 2 0.388571 0.286705 1.053563 11.00000 -1.20000 AFIX 0 C2 1 0.326002 0.168632 1.028204 11.00000 0.04714 0.09208 = 0.03198 0.01965 0.01898 0.03332 AFIX 43 H2A 2 0.379832 0.133937 1.042403 11.00000 -1.20000 AFIX 0 C3 1 0.249800 0.116015 1.005519 11.00000 0.10976 0.02772 = 0.04682 0.00552 0.05003 0.01369 AFIX 43 H3A 2 0.256174 0.050144 1.009339 11.00000 -1.20000 AFIX 0 C4 1 0.163422 0.147444 0.977312 11.00000 0.06788 0.07217 = 0.03774 -0.02718 0.03254 -0.04953 AFIX 43 H4A 2 0.118156 0.100388 0.966615 11.00000 -1.20000 AFIX 0 C5 1 0.137269 0.240382 0.963408 11.00000 0.02330 0.12050 = 0.02200 -0.00063 0.00435 0.01037 AFIX 43 H5A 2 0.079917 0.247780 0.941022 11.00000 -1.20000 AFIX 0 C6 1 0.186614 0.323887 0.978962 11.00000 0.07926 0.04598 = 0.04125 0.01735 0.03623 0.03094 AFIX 43 H6A 2 0.157789 0.380263 0.965683 11.00000 -1.20000 AFIX 0 C7 1 0.272240 0.334453 1.011308 11.00000 0.07994 0.03819 = 0.03682 -0.01383 0.03459 -0.02505 AFIX 43 H7A 2 0.290832 0.396992 1.019662 11.00000 -1.20000 AFIX 0 C8 1 0.410297 0.281164 1.168471 11.00000 0.04803 0.10402 = 0.03937 0.00665 -0.00530 -0.02257 AFIX 33 H8A 2 0.457701 0.299750 1.197352 11.00000 -1.50000 H8B 2 0.441333 0.245269 1.141864 11.00000 -1.50000 H8C 2 0.380709 0.337160 1.151785 11.00000 -1.50000 AFIX 0 C9 1 0.385256 0.110377 1.231545 11.00000 0.06406 0.10179 = 0.08174 0.04155 -0.00458 0.02495 AFIX 33 H9A 2 0.433413 0.136537 1.257856 11.00000 -1.50000 H9B 2 0.341251 0.071187 1.249619 11.00000 -1.50000 H9C 2 0.416406 0.072389 1.205878 11.00000 -1.50000 AFIX 0 C10 1 0.270334 0.276898 1.250406 11.00000 0.06264 0.09426 = 0.03393 -0.01360 -0.00205 -0.00038 AFIX 33 H10A 2 0.322993 0.295785 1.276185 11.00000 -1.50000 H10B 2 0.237672 0.332719 1.235431 11.00000 -1.50000 H10C 2 0.225462 0.238371 1.268252 11.00000 -1.50000 AFIX 0 C11 1 0.128518 0.049515 1.221307 11.00000 0.06896 0.05771 = 0.04185 0.01025 0.02478 -0.00557 AFIX 33 H11A 2 0.099008 -0.012384 1.222621 11.00000 -1.50000 H11B 2 0.180233 0.054640 1.249830 11.00000 -1.50000 H11C 2 0.080808 0.097862 1.225982 11.00000 -1.50000 AFIX 0 C12 1 0.252904 -0.038230 1.141969 11.00000 0.12270 0.04101 = 0.09562 0.01089 0.05954 0.02642 AFIX 33 H12A 2 0.217090 -0.095820 1.146856 11.00000 -1.50000 H12B 2 0.270555 -0.035322 1.105345 11.00000 -1.50000 H12C 2 0.310529 -0.037776 1.166761 11.00000 -1.50000 AFIX 0 C13 1 0.071209 0.057390 1.104939 11.00000 0.08207 0.04755 = 0.04212 -0.00016 0.01778 -0.02432 AFIX 33 H13A 2 0.039783 -0.003102 1.108521 11.00000 -1.50000 H13B 2 0.026600 0.107953 1.110975 11.00000 -1.50000 H13C 2 0.091847 0.063010 1.069045 11.00000 -1.50000 AFIX 0 C14 1 0.024840 0.344325 1.197392 11.00000 0.04565 0.04576 = 0.02969 -0.00009 0.01036 0.00172 AFIX 33 H14A 2 0.036256 0.394638 1.223578 11.00000 -1.50000 H14B 2 -0.041657 0.324251 1.196207 11.00000 -1.50000 H14C 2 0.066576 0.291294 1.207566 11.00000 -1.50000 AFIX 0 C15 1 -0.020485 0.498730 1.119879 11.00000 0.05875 0.04236 = 0.06541 0.00336 0.01331 0.01580 AFIX 33 H15A 2 -0.003855 0.541394 1.149685 11.00000 -1.50000 H15B 2 -0.006144 0.528569 1.086578 11.00000 -1.50000 H15C 2 -0.088460 0.484008 1.118110 11.00000 -1.50000 AFIX 0 C16 1 0.177402 0.427249 1.133543 11.00000 0.04442 0.03474 = 0.03985 -0.00654 0.00664 -0.00186 AFIX 33 H16A 2 0.188334 0.475623 1.160940 11.00000 -1.50000 H16B 2 0.219319 0.373844 1.142555 11.00000 -1.50000 H16C 2 0.190972 0.452799 1.099006 11.00000 -1.50000 AFIX 0 C17 1 -0.115070 0.380699 1.000890 11.00000 0.06009 0.10190 = 0.05703 0.03525 -0.01262 -0.00973 AFIX 33 H17A 2 -0.179214 0.367925 0.984268 11.00000 -1.50000 H17B 2 -0.114213 0.441739 1.018605 11.00000 -1.50000 H17C 2 -0.070115 0.381186 0.973535 11.00000 -1.50000 AFIX 0 C18 1 -0.172092 0.284342 1.099919 11.00000 0.02729 0.05995 = 0.05142 0.00734 0.00953 0.00001 AFIX 33 H18A 2 -0.234967 0.274742 1.080862 11.00000 -1.50000 H18B 2 -0.158048 0.232904 1.125092 11.00000 -1.50000 H18C 2 -0.171441 0.343717 1.119362 11.00000 -1.50000 AFIX 0 C19 1 -0.095418 0.175010 1.013466 11.00000 0.04270 0.09757 = 0.06579 -0.02728 0.00406 -0.01648 AFIX 33 H19A 2 -0.160740 0.170628 0.996827 11.00000 -1.50000 H19B 2 -0.050963 0.173034 0.985871 11.00000 -1.50000 H19C 2 -0.082612 0.122410 1.037985 11.00000 -1.50000 AFIX 0 C20 1 0.523006 0.121259 0.939873 11.00000 0.04403 0.03566 = 0.06218 -0.00035 0.00817 0.00692 AFIX 33 H20A 2 0.582430 0.090635 0.953420 11.00000 -1.50000 H20B 2 0.474271 0.109629 0.964325 11.00000 -1.50000 H20C 2 0.501714 0.096017 0.904676 11.00000 -1.50000 AFIX 0 C21 1 0.640167 0.262821 0.888959 11.00000 0.03809 0.05003 = 0.08623 -0.00385 0.02636 0.00366 AFIX 33 H21A 2 0.697524 0.230858 0.904487 11.00000 -1.50000 H21B 2 0.619552 0.234882 0.854347 11.00000 -1.50000 H21C 2 0.654062 0.329308 0.884238 11.00000 -1.50000 AFIX 0 C22 1 0.594001 0.287065 1.002105 11.00000 0.04562 0.05731 = 0.05956 -0.00337 -0.01730 0.00039 AFIX 33 H22A 2 0.652899 0.252427 1.011867 11.00000 -1.50000 H22B 2 0.607657 0.354273 1.001981 11.00000 -1.50000 H22C 2 0.548120 0.273865 1.027997 11.00000 -1.50000 AFIX 0 C23 1 0.456598 0.436048 0.820813 11.00000 0.07287 0.05634 = 0.03479 0.01204 0.01413 -0.01173 AFIX 33 H23A 2 0.458995 0.502887 0.812409 11.00000 -1.50000 H23B 2 0.515411 0.405851 0.811971 11.00000 -1.50000 H23C 2 0.402180 0.407348 0.800020 11.00000 -1.50000 AFIX 0 C24 1 0.545926 0.488322 0.926962 11.00000 0.04537 0.03314 = 0.05432 -0.00445 0.00852 -0.01268 AFIX 33 H24A 2 0.542138 0.553454 0.914836 11.00000 -1.50000 H24B 2 0.543571 0.486282 0.965637 11.00000 -1.50000 H24C 2 0.605712 0.460617 0.917740 11.00000 -1.50000 AFIX 0 C25 1 0.335985 0.489281 0.907819 11.00000 0.04434 0.03103 = 0.05074 0.00308 0.00787 0.00569 AFIX 33 H25A 2 0.343861 0.554577 0.897241 11.00000 -1.50000 H25B 2 0.279775 0.462763 0.887582 11.00000 -1.50000 H25C 2 0.327882 0.486436 0.945941 11.00000 -1.50000 AFIX 0 C26 1 0.324621 -0.043823 0.911359 11.00000 0.06060 0.02952 = 0.05245 -0.00039 0.00129 0.00192 AFIX 33 H26A 2 0.333857 -0.110267 0.903780 11.00000 -1.50000 H26B 2 0.383872 -0.017562 0.928412 11.00000 -1.50000 H26C 2 0.274084 -0.037040 0.935214 11.00000 -1.50000 AFIX 0 C27 1 0.185630 -0.046694 0.816639 11.00000 0.08511 0.04491 = 0.05573 -0.00065 -0.01613 -0.02199 AFIX 33 H27A 2 0.202111 -0.113050 0.814210 11.00000 -1.50000 H27B 2 0.132057 -0.039741 0.838397 11.00000 -1.50000 H27C 2 0.167827 -0.022006 0.780878 11.00000 -1.50000 AFIX 0 C28 1 0.389576 -0.003503 0.804770 11.00000 0.09214 0.04361 = 0.07666 -0.02115 0.04768 -0.00530 AFIX 33 H28A 2 0.398789 -0.071139 0.801535 11.00000 -1.50000 H28B 2 0.373168 0.023395 0.769395 11.00000 -1.50000 H28C 2 0.448365 0.025181 0.820845 11.00000 -1.50000 AFIX 0 C29 1 0.209646 0.177569 0.739618 11.00000 0.07971 0.06968 = 0.02393 -0.00174 0.00169 -0.01180 AFIX 33 H29A 2 0.159880 0.210314 0.717193 11.00000 -1.50000 H29B 2 0.271852 0.203766 0.733563 11.00000 -1.50000 H29C 2 0.208351 0.110879 0.730586 11.00000 -1.50000 AFIX 0 C30 1 0.062054 0.158542 0.818682 11.00000 0.04079 0.07216 = 0.05486 0.00819 -0.00741 -0.01438 AFIX 33 H30A 2 0.019826 0.193236 0.792679 11.00000 -1.50000 H30B 2 0.054227 0.091259 0.812249 11.00000 -1.50000 H30C 2 0.046003 0.173342 0.854706 11.00000 -1.50000 AFIX 0 C31 1 0.193551 0.321101 0.824446 11.00000 0.04898 0.04439 = 0.04126 0.00623 0.00261 0.00382 AFIX 33 H31A 2 0.146014 0.352787 0.800003 11.00000 -1.50000 H31B 2 0.180406 0.333629 0.861242 11.00000 -1.50000 H31C 2 0.257046 0.344423 0.818715 11.00000 -1.50000 AFIX 0 HKLF 4 REM mm462 in P2(1)/n REM R1 = 0.0299 for 10273 Fo > 4sig(Fo) and 0.0424 for all 12645 data REM 415 parameters refined using 0 restraints END WGHT 0.0248 8.8691 REM Highest difference peak 1.430, deepest hole -1.064, 1-sigma level 0.098 Q1 1 0.3248 0.2216 0.9017 11.00000 0.05 1.43 Q2 1 0.1907 0.2323 1.0371 11.00000 0.05 1.36 Q3 1 0.2792 0.2204 0.9642 11.00000 0.05 1.29 Q4 1 0.1420 0.2282 1.0991 11.00000 0.05 1.13 Q5 1 0.3196 0.2754 0.9200 11.00000 0.05 0.98 ; _shelx_res_checksum 87934 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mm466_5 _database_code_depnum_ccdc_archive 'CCDC 1454170' _audit_update_record ; 2016-02-18 deposited with the CCDC. 2016-08-08 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H79 Er2 K N4 Si8' _chemical_formula_weight 1106.32 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' 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 14.0946(7) _cell_length_b 14.2965(8) _cell_length_c 25.1055(13) _cell_angle_alpha 90 _cell_angle_beta 95.170(3) _cell_angle_gamma 90 _cell_volume 5038.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 30.63 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_density_meas n/a _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_F_000 2240 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.543 _exptl_crystal_size_min 0.430 _exptl_absorpt_coefficient_mu 3.606 _shelx_estimated_absorpt_T_min 0.161 _shelx_estimated_absorpt_T_max 0.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.304526 _exptl_absorpt_correction_T_max 0.746065 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26202 _diffrn_reflns_av_unetI/netI 0.0493 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.598 _diffrn_reflns_theta_max 30.659 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.979 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 15164 _reflns_number_gt 12527 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _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 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-03 (Sheldrick, 2003)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _refine_special_details ; Refined as a 2-component twin. ; _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^)+(0.0571P)^2^+21.3484P] 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 15164 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_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 0.17213(2) 0.23105(2) 1.06695(2) 0.02263(6) Uani 1 1 d . . . . . Er2 Er 0.30279(2) 0.22558(2) 0.93389(2) 0.02065(6) Uani 1 1 d . . . . . K1 K 0.43466(13) 0.21707(12) 0.80531(6) 0.0416(4) Uani 1 1 d . . . . . Si1 Si 0.31766(14) 0.20724(17) 1.19452(8) 0.0411(5) Uani 1 1 d . . . . . Si2 Si 0.17648(16) 0.06606(14) 1.15422(8) 0.0390(4) Uani 1 1 d . . . . . Si3 Si 0.05170(13) 0.38678(13) 1.12981(7) 0.0300(3) Uani 1 1 d . . . . . Si4 Si -0.07829(13) 0.28720(15) 1.05050(8) 0.0370(4) Uani 1 1 d . . . . . Si5 Si 0.54219(12) 0.25042(13) 0.93443(7) 0.0308(3) Uani 1 1 d . . . . . Si6 Si 0.44222(12) 0.42101(12) 0.89416(7) 0.0285(3) Uani 1 1 d . . . . . Si7 Si 0.28996(14) 0.02123(14) 0.84845(7) 0.0346(4) Uani 1 1 d . . . . . Si8 Si 0.18786(13) 0.19325(15) 0.81248(7) 0.0337(4) Uani 1 1 d . . . . . N1 N 0.2301(4) 0.1714(4) 1.1468(2) 0.0313(11) Uani 1 1 d . . . . . N2 N 0.0345(3) 0.3040(4) 1.08219(19) 0.0278(10) Uani 1 1 d . . . . . N3 N 0.4372(3) 0.3046(3) 0.91099(19) 0.0242(9) Uani 1 1 d . . . . . N4 N 0.2713(4) 0.1387(4) 0.85588(19) 0.0283(10) Uani 1 1 d . . . . . C1 C 0.3347(5) 0.2662(8) 1.0331(3) 0.055(3) Uani 1 1 d . . . . . H1A H 0.3894 0.2888 1.0541 0.067 Uiso 1 1 calc R U . . . C2 C 0.3277(6) 0.1703(9) 1.0279(3) 0.063(3) Uani 1 1 d . . . . . H2A H 0.3822 0.1358 1.0415 0.075 Uiso 1 1 calc R U . . . C3 C 0.2495(7) 0.1157(5) 1.0046(3) 0.056(3) Uani 1 1 d . . . . . H3A H 0.2560 0.0498 1.0078 0.067 Uiso 1 1 calc R U . . . C4 C 0.1616(6) 0.1495(6) 0.9769(3) 0.055(3) Uani 1 1 d . . . . . H4A H 0.1147 0.1034 0.9668 0.066 Uiso 1 1 calc R U . . . C5 C 0.1374(5) 0.2425(7) 0.9630(3) 0.050(2) Uani 1 1 d . . . . . H5A H 0.0805 0.2508 0.9403 0.060 Uiso 1 1 calc R U . . . C6 C 0.1872(7) 0.3247(6) 0.9787(3) 0.055(2) Uani 1 1 d . . . . . H6A H 0.1592 0.3811 0.9649 0.066 Uiso 1 1 calc R U . . . C7 C 0.2707(7) 0.3351(6) 1.0112(3) 0.051(2) Uani 1 1 d . . . . . H7A H 0.2877 0.3979 1.0202 0.061 Uiso 1 1 calc R U . . . C8 C 0.4113(6) 0.2816(8) 1.1675(3) 0.064(3) Uani 1 1 d . . . . . H8A H 0.4587 0.2995 1.1967 0.096 Uiso 1 1 calc R U . . . H8B H 0.4425 0.2464 1.1405 0.096 Uiso 1 1 calc R U . . . H8C H 0.3818 0.3380 1.1512 0.096 Uiso 1 1 calc R U . . . C9 C 0.3853(8) 0.1088(9) 1.2300(5) 0.086(4) Uani 1 1 d . . . . . H9A H 0.4338 0.1345 1.2564 0.129 Uiso 1 1 calc R U . . . H9B H 0.3412 0.0695 1.2481 0.129 Uiso 1 1 calc R U . . . H9C H 0.4163 0.0712 1.2039 0.129 Uiso 1 1 calc R U . . . C10 C 0.2709(7) 0.2767(8) 1.2504(3) 0.066(3) Uani 1 1 d . . . . . H10A H 0.3240 0.2950 1.2761 0.099 Uiso 1 1 calc R U . . . H10B H 0.2385 0.3329 1.2357 0.099 Uiso 1 1 calc R U . . . H10C H 0.2258 0.2384 1.2684 0.099 Uiso 1 1 calc R U . . . C11 C 0.1283(6) 0.0489(6) 1.2205(3) 0.052(2) Uani 1 1 d . . . . . H11A H 0.0987 -0.0130 1.2216 0.078 Uiso 1 1 calc R U . . . H11B H 0.1803 0.0536 1.2490 0.078 Uiso 1 1 calc R U . . . H11C H 0.0806 0.0972 1.2256 0.078 Uiso 1 1 calc R U . . . C12 C 0.2512(9) -0.0368(7) 1.1406(5) 0.081(4) Uani 1 1 d . . . . . H12A H 0.2154 -0.0944 1.1457 0.121 Uiso 1 1 calc R U . . . H12B H 0.2684 -0.0339 1.1037 0.121 Uiso 1 1 calc R U . . . H12C H 0.3093 -0.0364 1.1652 0.121 Uiso 1 1 calc R U . . . C13 C 0.0699(7) 0.0563(6) 1.1045(3) 0.056(2) Uani 1 1 d . . . . . H13A H 0.0389 -0.0043 1.1087 0.084 Uiso 1 1 calc R U . . . H13B H 0.0249 0.1067 1.1106 0.084 Uiso 1 1 calc R U . . . H13C H 0.0898 0.0614 1.0683 0.084 Uiso 1 1 calc R U . . . C14 C 0.0235(5) 0.3439(5) 1.1974(3) 0.0409(16) Uani 1 1 d . . . . . H14A H 0.0346 0.3943 1.2237 0.061 Uiso 1 1 calc R U . . . H14B H -0.0433 0.3243 1.1957 0.061 Uiso 1 1 calc R U . . . H14C H 0.0646 0.2906 1.2081 0.061 Uiso 1 1 calc R U . . . C15 C -0.0201(7) 0.4975(6) 1.1204(4) 0.056(2) Uani 1 1 d . . . . . H15A H -0.0036 0.5397 1.1506 0.084 Uiso 1 1 calc R U . . . H15B H -0.0059 0.5280 1.0871 0.084 Uiso 1 1 calc R U . . . H15C H -0.0881 0.4824 1.1186 0.084 Uiso 1 1 calc R U . . . C16 C 0.1786(5) 0.4280(5) 1.1334(3) 0.0384(15) Uani 1 1 d . . . . . H16A H 0.1888 0.4762 1.1611 0.058 Uiso 1 1 calc R U . . . H16B H 0.2214 0.3752 1.1423 0.058 Uiso 1 1 calc R U . . . H16C H 0.1918 0.4542 1.0988 0.058 Uiso 1 1 calc R U . . . C17 C -0.1133(7) 0.3821(9) 1.0007(4) 0.078(3) Uani 1 1 d . . . . . H17A H -0.1775 0.3697 0.9838 0.117 Uiso 1 1 calc R U . . . H17B H -0.1127 0.4426 1.0191 0.117 Uiso 1 1 calc R U . . . H17C H -0.0681 0.3835 0.9733 0.117 Uiso 1 1 calc R U . . . C18 C -0.1703(5) 0.2834(6) 1.0999(3) 0.0447(18) Uani 1 1 d . . . . . H18A H -0.2334 0.2738 1.0809 0.067 Uiso 1 1 calc R U . . . H18B H -0.1560 0.2318 1.1250 0.067 Uiso 1 1 calc R U . . . H18C H -0.1697 0.3426 1.1196 0.067 Uiso 1 1 calc R U . . . C19 C -0.0943(6) 0.1757(8) 1.0122(4) 0.065(3) Uani 1 1 d . . . . . H19A H -0.1598 0.1718 0.9956 0.097 Uiso 1 1 calc R U . . . H19B H -0.0499 0.1740 0.9843 0.097 Uiso 1 1 calc R U . . . H19C H -0.0816 0.1226 1.0365 0.097 Uiso 1 1 calc R U . . . C20 C 0.5222(6) 0.1210(5) 0.9390(4) 0.0489(19) Uani 1 1 d . . . . . H20A H 0.5819 0.0903 0.9523 0.073 Uiso 1 1 calc R U . . . H20B H 0.4735 0.1086 0.9635 0.073 Uiso 1 1 calc R U . . . H20C H 0.5009 0.0964 0.9034 0.073 Uiso 1 1 calc R U . . . C21 C 0.6397(6) 0.2639(6) 0.8882(4) 0.054(2) Uani 1 1 d . . . . . H21A H 0.6973 0.2319 0.9035 0.082 Uiso 1 1 calc R U . . . H21B H 0.6190 0.2364 0.8533 0.082 Uiso 1 1 calc R U . . . H21C H 0.6536 0.3305 0.8837 0.082 Uiso 1 1 calc R U . . . C22 C 0.5929(6) 0.2862(6) 1.0021(4) 0.053(2) Uani 1 1 d . . . . . H22A H 0.6521 0.2516 1.0116 0.079 Uiso 1 1 calc R U . . . H22B H 0.6064 0.3534 1.0022 0.079 Uiso 1 1 calc R U . . . H22C H 0.5471 0.2724 1.0281 0.079 Uiso 1 1 calc R U . . . C23 C 0.4560(6) 0.4352(6) 0.8209(3) 0.051(2) Uani 1 1 d . . . . . H23A H 0.4587 0.5019 0.8122 0.077 Uiso 1 1 calc R U . . . H23B H 0.5149 0.4046 0.8123 0.077 Uiso 1 1 calc R U . . . H23C H 0.4015 0.4064 0.8000 0.077 Uiso 1 1 calc R U . . . C24 C 0.5458(5) 0.4882(5) 0.9273(3) 0.0454(17) Uani 1 1 d . . . . . H24A H 0.5423 0.5534 0.9152 0.068 Uiso 1 1 calc R U . . . H24B H 0.5438 0.4861 0.9662 0.068 Uiso 1 1 calc R U . . . H24C H 0.6055 0.4602 0.9178 0.068 Uiso 1 1 calc R U . . . C25 C 0.3347(5) 0.4899(5) 0.9082(3) 0.0393(14) Uani 1 1 d . . . . . H25A H 0.3429 0.5551 0.8976 0.059 Uiso 1 1 calc R U . . . H25B H 0.2783 0.4636 0.8879 0.059 Uiso 1 1 calc R U . . . H25C H 0.3265 0.4870 0.9466 0.059 Uiso 1 1 calc R U . . . C26 C 0.3238(6) -0.0442(5) 0.9112(3) 0.0480(17) Uani 1 1 d . . . . . H26A H 0.3328 -0.1104 0.9028 0.072 Uiso 1 1 calc R U . . . H26B H 0.3832 -0.0186 0.9286 0.072 Uiso 1 1 calc R U . . . H26C H 0.2731 -0.0382 0.9353 0.072 Uiso 1 1 calc R U . . . C27 C 0.1847(7) -0.0449(6) 0.8170(3) 0.058(2) Uani 1 1 d . . . . . H27A H 0.2013 -0.1111 0.8142 0.086 Uiso 1 1 calc R U . . . H27B H 0.1312 -0.0383 0.8390 0.086 Uiso 1 1 calc R U . . . H27C H 0.1666 -0.0197 0.7812 0.086 Uiso 1 1 calc R U . . . C28 C 0.3874(7) -0.0019(6) 0.8036(4) 0.064(3) Uani 1 1 d . . . . . H28A H 0.3964 -0.0695 0.8001 0.096 Uiso 1 1 calc R U . . . H28B H 0.3697 0.0252 0.7682 0.096 Uiso 1 1 calc R U . . . H28C H 0.4469 0.0267 0.8190 0.096 Uiso 1 1 calc R U . . . C29 C 0.2094(7) 0.1769(7) 0.7403(3) 0.056(2) Uani 1 1 d . . . . . H29A H 0.1598 0.2095 0.7176 0.084 Uiso 1 1 calc R U . . . H29B H 0.2719 0.2027 0.7341 0.084 Uiso 1 1 calc R U . . . H29C H 0.2079 0.1101 0.7316 0.084 Uiso 1 1 calc R U . . . C30 C 0.0607(5) 0.1589(7) 0.8193(3) 0.054(2) Uani 1 1 d . . . . . H30A H 0.0184 0.1934 0.7931 0.080 Uiso 1 1 calc R U . . . H30B H 0.0530 0.0916 0.8130 0.080 Uiso 1 1 calc R U . . . H30C H 0.0443 0.1739 0.8555 0.080 Uiso 1 1 calc R U . . . C31 C 0.1923(6) 0.3221(5) 0.8242(3) 0.0453(17) Uani 1 1 d . . . . . H31A H 0.1446 0.3530 0.7993 0.068 Uiso 1 1 calc R U . . . H31B H 0.1789 0.3354 0.8610 0.068 Uiso 1 1 calc R U . . . H31C H 0.2559 0.3456 0.8183 0.068 Uiso 1 1 calc R U . . . 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 0.02367(12) 0.02770(13) 0.01755(11) -0.00068(9) 0.00762(8) 0.00015(10) Er2 0.02287(12) 0.02523(12) 0.01457(10) -0.00170(8) 0.00566(7) -0.00227(9) K1 0.0494(8) 0.0508(9) 0.0271(6) -0.0181(6) 0.0175(6) -0.0205(7) Si1 0.0339(9) 0.0640(13) 0.0258(8) 0.0111(9) 0.0050(7) 0.0071(9) Si2 0.0551(12) 0.0291(9) 0.0364(9) 0.0075(8) 0.0233(8) 0.0043(8) Si3 0.0349(9) 0.0280(8) 0.0287(8) 0.0009(7) 0.0116(6) 0.0062(7) Si4 0.0255(8) 0.0534(12) 0.0325(9) 0.0063(8) 0.0050(6) -0.0018(7) Si5 0.0229(7) 0.0301(9) 0.0401(9) -0.0022(7) 0.0054(6) 0.0009(6) Si6 0.0327(8) 0.0292(8) 0.0244(7) 0.0008(6) 0.0071(6) -0.0056(6) Si7 0.0435(10) 0.0300(9) 0.0316(9) -0.0085(7) 0.0100(7) -0.0065(7) Si8 0.0357(9) 0.0427(11) 0.0223(7) 0.0005(7) 0.0005(6) -0.0050(8) N1 0.033(3) 0.037(3) 0.025(2) 0.012(2) 0.0102(19) 0.010(2) N2 0.020(2) 0.038(3) 0.026(2) -0.001(2) 0.0092(17) 0.005(2) N3 0.024(2) 0.024(2) 0.026(2) -0.004(2) 0.0105(17) -0.0057(18) N4 0.033(3) 0.027(3) 0.025(2) -0.011(2) 0.0058(18) -0.009(2) C1 0.035(4) 0.107(8) 0.027(3) -0.016(4) 0.013(3) -0.034(4) C2 0.050(4) 0.111(8) 0.030(4) 0.023(4) 0.019(3) 0.042(5) C3 0.106(8) 0.023(3) 0.044(4) 0.011(3) 0.044(5) 0.017(4) C4 0.067(5) 0.071(6) 0.031(3) -0.036(4) 0.030(3) -0.056(5) C5 0.027(3) 0.103(7) 0.020(3) -0.003(4) 0.005(2) 0.006(4) C6 0.075(6) 0.051(5) 0.043(4) 0.015(4) 0.037(4) 0.030(4) C7 0.083(6) 0.037(4) 0.040(4) -0.016(3) 0.039(4) -0.023(4) C8 0.046(5) 0.112(8) 0.034(4) 0.008(4) -0.004(3) -0.028(5) C9 0.056(6) 0.108(9) 0.091(8) 0.036(7) -0.004(5) 0.023(6) C10 0.063(6) 0.106(9) 0.030(4) -0.019(4) 0.004(4) 0.004(5) C11 0.062(5) 0.056(5) 0.043(4) 0.013(4) 0.024(4) -0.003(4) C12 0.117(9) 0.040(5) 0.093(8) 0.017(5) 0.058(7) 0.030(6) C13 0.080(6) 0.048(5) 0.042(4) -0.002(4) 0.011(4) -0.026(4) C14 0.051(4) 0.041(4) 0.033(3) -0.001(3) 0.012(3) 0.010(3) C15 0.066(5) 0.035(4) 0.069(6) 0.008(4) 0.013(4) 0.016(4) C16 0.043(4) 0.032(3) 0.040(4) -0.004(3) 0.002(3) -0.010(3) C17 0.056(5) 0.105(9) 0.068(6) 0.050(6) -0.016(4) -0.016(6) C18 0.030(3) 0.056(5) 0.049(4) 0.007(4) 0.011(3) 0.003(3) C19 0.041(4) 0.095(8) 0.058(5) -0.032(5) 0.000(4) -0.010(5) C20 0.051(4) 0.029(4) 0.068(5) 0.001(4) 0.015(4) 0.004(3) C21 0.038(4) 0.047(5) 0.082(6) -0.007(4) 0.029(4) 0.000(3) C22 0.047(5) 0.051(5) 0.056(5) 0.000(4) -0.015(4) 0.002(4) C23 0.069(5) 0.066(5) 0.021(3) 0.008(3) 0.009(3) -0.018(4) C24 0.043(4) 0.035(4) 0.059(5) -0.002(4) 0.008(3) -0.011(3) C25 0.043(4) 0.029(3) 0.046(4) 0.003(3) 0.005(3) 0.001(3) C26 0.062(5) 0.033(4) 0.049(4) -0.004(3) 0.003(3) 0.002(4) C27 0.081(6) 0.040(4) 0.049(5) -0.004(4) -0.009(4) -0.019(4) C28 0.089(7) 0.038(4) 0.073(6) -0.022(4) 0.047(5) -0.006(4) C29 0.078(6) 0.069(6) 0.020(3) 0.000(3) 0.000(3) -0.012(5) C30 0.036(4) 0.068(6) 0.055(5) 0.006(4) -0.005(3) -0.011(4) C31 0.043(4) 0.044(4) 0.048(4) 0.005(4) -0.001(3) 0.007(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 Er1 N1 2.263(5) . ? Er1 N2 2.265(5) . ? Er1 C4 2.537(6) . ? Er1 C7 2.540(7) . ? Er1 C1 2.564(7) . ? Er1 C3 2.581(7) . ? Er1 C6 2.613(7) . ? Er1 C5 2.616(6) . ? Er1 C2 2.630(7) . ? Er1 Si2 3.2163(19) . ? Er1 Si3 3.2880(17) . ? Er1 Er2 3.9580(3) . ? Er2 N3 2.322(4) . ? Er2 N4 2.328(5) . ? Er2 C2 2.483(7) . ? Er2 C6 2.502(7) . ? Er2 C5 2.517(7) . ? Er2 C3 2.535(7) . ? Er2 C1 2.559(7) . ? Er2 C7 2.566(7) . ? Er2 C4 2.588(6) . ? Er2 Si8 3.3524(17) . ? Er2 Si5 3.3917(17) . ? Er2 K1 3.8692(12) . ? K1 N3 2.931(5) . ? K1 N4 2.948(5) . ? K1 C23 3.154(9) . ? K1 C28 3.199(9) . ? K1 C14 3.205(7) 4_665 ? K1 C21 3.471(11) . ? K1 C29 3.484(9) . ? K1 Si5 3.485(3) . ? K1 Si8 3.516(2) . ? K1 Si6 3.667(2) . ? K1 Si7 3.684(2) . ? Si1 N1 1.718(6) . ? Si1 C8 1.869(9) . ? Si1 C9 1.878(11) . ? Si1 C10 1.886(9) . ? Si2 N1 1.703(6) . ? Si2 C12 1.859(9) . ? Si2 C11 1.869(7) . ? Si2 C13 1.870(9) . ? Si3 N2 1.684(6) . ? Si3 C16 1.878(7) . ? Si3 C14 1.881(7) . ? Si3 C15 1.882(8) . ? Si4 N2 1.729(5) . ? Si4 C19 1.866(10) . ? Si4 C18 1.875(7) . ? Si4 C17 1.881(9) . ? Si5 N3 1.726(5) . ? Si5 C22 1.854(9) . ? Si5 C20 1.877(8) . ? Si5 C21 1.888(8) . ? Si6 N3 1.720(5) . ? Si6 C25 1.867(7) . ? Si6 C23 1.877(6) . ? Si6 C24 1.878(7) . ? Si7 N4 1.713(6) . ? Si7 C26 1.857(8) . ? Si7 C27 1.872(8) . ? Si7 C28 1.883(8) . ? Si8 N4 1.717(6) . ? Si8 C31 1.865(8) . ? Si8 C29 1.878(7) . ? Si8 C30 1.882(8) . ? C1 C2 1.381(15) . ? C1 C7 1.413(13) . ? C2 C3 1.431(14) . ? C3 C4 1.449(13) . ? C4 C5 1.409(13) . ? C5 C6 1.406(13) . ? C6 C7 1.379(13) . ? C14 K1 3.205(7) 4_566 ? 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 105.67(18) . . ? N1 Er1 C4 127.2(3) . . ? N2 Er1 C4 112.3(3) . . ? N1 Er1 C7 122.5(3) . . ? N2 Er1 C7 110.0(3) . . ? C4 Er1 C7 76.7(2) . . ? N1 Er1 C1 96.0(2) . . ? N2 Er1 C1 140.4(3) . . ? C4 Er1 C1 77.1(2) . . ? C7 Er1 C1 32.1(3) . . ? N1 Er1 C3 99.1(2) . . ? N2 Er1 C3 144.3(3) . . ? C4 Er1 C3 32.9(3) . . ? C7 Er1 C3 76.0(2) . . ? C1 Er1 C3 59.0(3) . . ? N1 Er1 C6 153.4(3) . . ? N2 Er1 C6 92.5(2) . . ? C4 Er1 C6 58.8(3) . . ? C7 Er1 C6 31.0(3) . . ? C1 Er1 C6 58.4(3) . . ? C3 Er1 C6 75.1(2) . . ? N1 Er1 C5 158.1(2) . . ? N2 Er1 C5 93.1(2) . . ? C4 Er1 C5 31.7(3) . . ? C7 Er1 C5 58.4(3) . . ? C1 Er1 C5 75.5(2) . . ? C3 Er1 C5 59.1(3) . . ? C6 Er1 C5 31.2(3) . . ? N1 Er1 C2 87.7(2) . . ? N2 Er1 C2 166.1(2) . . ? C4 Er1 C2 60.0(3) . . ? C7 Er1 C2 58.1(3) . . ? C1 Er1 C2 30.8(3) . . ? C3 Er1 C2 31.9(3) . . ? C6 Er1 C2 73.7(2) . . ? C5 Er1 C2 74.7(2) . . ? N1 Er1 Si2 30.33(16) . . ? N2 Er1 Si2 100.75(14) . . ? C4 Er1 Si2 105.4(2) . . ? C7 Er1 Si2 145.8(2) . . ? C1 Er1 Si2 114.0(2) . . ? C3 Er1 Si2 87.78(15) . . ? C6 Er1 Si2 162.78(18) . . ? C5 Er1 Si2 135.7(2) . . ? C2 Er1 Si2 92.7(2) . . ? N1 Er1 Si3 89.45(14) . . ? N2 Er1 Si3 28.39(14) . . ? C4 Er1 Si3 138.4(3) . . ? C7 Er1 Si3 101.50(18) . . ? C1 Er1 Si3 122.8(2) . . ? C3 Er1 Si3 171.1(2) . . ? C6 Er1 Si3 98.33(16) . . ? C5 Er1 Si3 112.21(19) . . ? C2 Er1 Si3 152.5(3) . . ? Si2 Er1 Si3 98.55(5) . . ? N1 Er1 Er2 125.61(12) . . ? N2 Er1 Er2 128.49(13) . . ? C4 Er1 Er2 39.91(14) . . ? C7 Er1 Er2 39.42(16) . . ? C1 Er1 Er2 39.36(16) . . ? C3 Er1 Er2 38.89(15) . . ? C6 Er1 Er2 38.29(16) . . ? C5 Er1 Er2 38.63(15) . . ? C2 Er1 Er2 37.95(16) . . ? Si2 Er1 Er2 125.36(3) . . ? Si3 Er1 Er2 135.89(3) . . ? N3 Er2 N4 98.57(17) . . ? N3 Er2 C2 110.0(3) . . ? N4 Er2 C2 129.0(3) . . ? N3 Er2 C6 114.5(3) . . ? N4 Er2 C6 126.7(3) . . ? C2 Er2 C6 78.2(3) . . ? N3 Er2 C5 145.4(3) . . ? N4 Er2 C5 100.7(2) . . ? C2 Er2 C5 79.0(2) . . ? C6 Er2 C5 32.5(3) . . ? N3 Er2 C3 140.8(3) . . ? N4 Er2 C3 102.3(2) . . ? C2 Er2 C3 33.1(3) . . ? C6 Er2 C3 77.9(2) . . ? C5 Er2 C3 61.0(3) . . ? N3 Er2 C1 93.1(2) . . ? N4 Er2 C1 160.7(3) . . ? C2 Er2 C1 31.7(3) . . ? C6 Er2 C1 59.9(3) . . ? C5 Er2 C1 77.4(2) . . ? C3 Er2 C1 59.7(3) . . ? N3 Er2 C7 95.4(2) . . ? N4 Er2 C7 158.3(3) . . ? C2 Er2 C7 59.7(3) . . ? C6 Er2 C7 31.5(3) . . ? C5 Er2 C7 59.4(3) . . ? C3 Er2 C7 76.4(2) . . ? C1 Er2 C7 32.0(3) . . ? N3 Er2 C4 169.45(19) . . ? N4 Er2 C4 91.78(18) . . ? C2 Er2 C4 61.2(3) . . ? C6 Er2 C4 59.6(3) . . ? C5 Er2 C4 32.0(3) . . ? C3 Er2 C4 32.8(3) . . ? C1 Er2 C4 76.3(2) . . ? C7 Er2 C4 75.3(2) . . ? N3 Er2 Si8 100.38(13) . . ? N4 Er2 Si8 28.55(14) . . ? C2 Er2 Si8 146.7(3) . . ? C6 Er2 Si8 101.9(2) . . ? C5 Er2 Si8 83.88(16) . . ? C3 Er2 Si8 113.7(2) . . ? C1 Er2 Si8 160.90(19) . . ? C7 Er2 Si8 131.9(2) . . ? C4 Er2 Si8 89.68(17) . . ? N3 Er2 Si5 27.94(13) . . ? N4 Er2 Si5 99.98(13) . . ? C2 Er2 Si5 88.5(2) . . ? C6 Er2 Si5 128.8(3) . . ? C5 Er2 Si5 159.36(19) . . ? C3 Er2 Si5 114.8(2) . . ? C1 Er2 Si5 83.38(16) . . ? C7 Er2 Si5 100.1(2) . . ? C4 Er2 Si5 147.6(2) . . ? Si8 Er2 Si5 114.65(4) . . ? N3 Er2 K1 49.06(12) . . ? N4 Er2 K1 49.51(12) . . ? C2 Er2 K1 138.18(17) . . ? C6 Er2 K1 140.75(18) . . ? C5 Er2 K1 140.59(15) . . ? C3 Er2 K1 139.46(16) . . ? C1 Er2 K1 139.82(15) . . ? C7 Er2 K1 141.35(16) . . ? C4 Er2 K1 141.26(14) . . ? Si8 Er2 K1 57.74(4) . . ? Si5 Er2 K1 56.92(4) . . ? N3 K1 N4 73.66(13) . . ? N3 K1 C23 58.14(15) . . ? N4 K1 C23 113.05(18) . . ? N3 K1 C28 114.57(19) . . ? N4 K1 C28 57.63(17) . . ? C23 K1 C28 170.5(2) . . ? N3 K1 C14 155.12(17) . 4_665 ? N4 K1 C14 129.81(17) . 4_665 ? C23 K1 C14 109.48(18) . 4_665 ? C28 K1 C14 79.58(19) . 4_665 ? N3 K1 C21 55.49(16) . . ? N4 K1 C21 117.10(18) . . ? C23 K1 C21 70.7(2) . . ? C28 K1 C21 111.0(3) . . ? C14 K1 C21 101.0(2) 4_665 . ? N3 K1 C29 115.50(17) . . ? N4 K1 C29 54.92(16) . . ? C23 K1 C29 107.1(2) . . ? C28 K1 C29 69.7(3) . . ? C14 K1 C29 88.2(2) 4_665 . ? C21 K1 C29 170.76(19) . . ? N3 K1 Si5 29.64(10) . . ? N4 K1 Si5 86.70(11) . . ? C23 K1 Si5 73.78(14) . . ? C28 K1 Si5 102.7(2) . . ? C14 K1 Si5 130.75(16) 4_665 . ? C21 K1 Si5 31.49(14) . . ? C29 K1 Si5 139.44(13) . . ? N3 K1 Si8 85.78(10) . . ? N4 K1 Si8 29.15(11) . . ? C23 K1 Si8 99.96(17) . . ? C28 K1 Si8 72.56(18) . . ? C14 K1 Si8 118.73(15) 4_665 . ? C21 K1 Si8 139.67(14) . . ? C29 K1 Si8 31.13(13) . . ? Si5 K1 Si8 108.36(5) . . ? N3 K1 Si6 27.43(10) . . ? N4 K1 Si6 91.22(10) . . ? C23 K1 Si6 30.80(12) . . ? C28 K1 Si6 141.34(16) . . ? C14 K1 Si6 137.56(14) 4_665 . ? C21 K1 Si6 60.33(14) . . ? C29 K1 Si6 113.03(17) . . ? Si5 K1 Si6 48.63(5) . . ? Si8 K1 Si6 91.18(5) . . ? N3 K1 Si7 91.16(10) . . ? N4 K1 Si7 27.15(11) . . ? C23 K1 Si7 139.82(15) . . ? C28 K1 Si7 30.74(14) . . ? C14 K1 Si7 108.10(14) 4_665 . ? C21 K1 Si7 115.06(16) . . ? C29 K1 Si7 60.48(15) . . ? Si5 K1 Si7 92.09(6) . . ? Si8 K1 Si7 48.30(5) . . ? Si6 K1 Si7 114.33(5) . . ? N3 K1 Er2 36.76(9) . . ? N4 K1 Er2 36.90(9) . . ? C23 K1 Er2 85.00(12) . . ? C28 K1 Er2 85.83(14) . . ? C14 K1 Er2 165.27(14) 4_665 . ? C21 K1 Er2 86.02(14) . . ? C29 K1 Er2 84.84(13) . . ? Si5 K1 Er2 54.62(3) . . ? Si8 K1 Er2 53.74(3) . . ? Si6 K1 Er2 57.13(3) . . ? Si7 K1 Er2 57.20(3) . . ? N1 Si1 C8 113.8(3) . . ? N1 Si1 C9 114.1(5) . . ? C8 Si1 C9 104.6(5) . . ? N1 Si1 C10 113.4(4) . . ? C8 Si1 C10 106.0(5) . . ? C9 Si1 C10 103.8(5) . . ? N1 Si2 C12 114.5(4) . . ? N1 Si2 C11 114.4(4) . . ? C12 Si2 C11 108.5(4) . . ? N1 Si2 C13 109.4(3) . . ? C12 Si2 C13 104.6(5) . . ? C11 Si2 C13 104.4(4) . . ? N1 Si2 Er1 42.15(18) . . ? C12 Si2 Er1 115.5(3) . . ? C11 Si2 Er1 135.8(3) . . ? C13 Si2 Er1 68.6(3) . . ? N2 Si3 C16 109.3(3) . . ? N2 Si3 C14 112.5(3) . . ? C16 Si3 C14 109.7(3) . . ? N2 Si3 C15 117.4(4) . . ? C16 Si3 C15 104.0(4) . . ? C14 Si3 C15 103.5(4) . . ? N2 Si3 Er1 39.75(16) . . ? C16 Si3 Er1 72.8(2) . . ? C14 Si3 Er1 111.9(2) . . ? C15 Si3 Er1 143.5(3) . . ? N2 Si4 C19 114.8(4) . . ? N2 Si4 C18 111.2(3) . . ? C19 Si4 C18 104.9(4) . . ? N2 Si4 C17 112.4(4) . . ? C19 Si4 C17 105.2(6) . . ? C18 Si4 C17 107.7(5) . . ? N3 Si5 C22 115.9(3) . . ? N3 Si5 C20 109.5(3) . . ? C22 Si5 C20 105.3(4) . . ? N3 Si5 C21 113.2(4) . . ? C22 Si5 C21 107.0(5) . . ? C20 Si5 C21 105.0(4) . . ? N3 Si5 Er2 39.06(16) . . ? C22 Si5 Er2 109.5(3) . . ? C20 Si5 Er2 75.1(3) . . ? C21 Si5 Er2 142.0(3) . . ? N3 Si5 K1 57.09(17) . . ? C22 Si5 K1 171.5(3) . . ? C20 Si5 K1 82.3(3) . . ? C21 Si5 K1 73.8(3) . . ? Er2 Si5 K1 68.46(4) . . ? N3 Si6 C25 114.3(3) . . ? N3 Si6 C23 110.8(3) . . ? C25 Si6 C23 106.6(4) . . ? N3 Si6 C24 115.7(3) . . ? C25 Si6 C24 105.0(4) . . ? C23 Si6 C24 103.5(4) . . ? N3 Si6 K1 51.72(16) . . ? C25 Si6 K1 123.7(3) . . ? C23 Si6 K1 59.3(3) . . ? C24 Si6 K1 130.9(3) . . ? N4 Si7 C26 115.6(3) . . ? N4 Si7 C27 114.7(4) . . ? C26 Si7 C27 103.7(4) . . ? N4 Si7 C28 111.4(3) . . ? C26 Si7 C28 105.9(4) . . ? C27 Si7 C28 104.6(4) . . ? N4 Si7 K1 51.76(17) . . ? C26 Si7 K1 121.7(3) . . ? C27 Si7 K1 134.3(3) . . ? C28 Si7 K1 60.3(3) . . ? N4 Si8 C31 109.7(3) . . ? N4 Si8 C29 113.2(4) . . ? C31 Si8 C29 105.5(4) . . ? N4 Si8 C30 115.3(3) . . ? C31 Si8 C30 105.2(4) . . ? C29 Si8 C30 107.1(4) . . ? N4 Si8 Er2 40.39(16) . . ? C31 Si8 Er2 73.4(2) . . ? C29 Si8 Er2 141.9(3) . . ? C30 Si8 Er2 109.8(3) . . ? N4 Si8 K1 56.77(17) . . ? C31 Si8 K1 83.8(2) . . ? C29 Si8 K1 73.5(3) . . ? C30 Si8 K1 170.1(3) . . ? Er2 Si8 K1 68.53(4) . . ? Si2 N1 Si1 119.1(3) . . ? Si2 N1 Er1 107.5(3) . . ? Si1 N1 Er1 133.2(3) . . ? Si3 N2 Si4 119.5(3) . . ? Si3 N2 Er1 111.9(3) . . ? Si4 N2 Er1 128.6(3) . . ? Si6 N3 Si5 117.7(3) . . ? Si6 N3 Er2 125.8(3) . . ? Si5 N3 Er2 113.0(2) . . ? Si6 N3 K1 100.8(2) . . ? Si5 N3 K1 93.3(2) . . ? Er2 N3 K1 94.17(16) . . ? Si7 N4 Si8 118.6(3) . . ? Si7 N4 Er2 126.5(3) . . ? Si8 N4 Er2 111.1(3) . . ? Si7 N4 K1 101.1(2) . . ? Si8 N4 K1 94.1(2) . . ? Er2 N4 K1 93.59(16) . . ? C2 C1 C7 128.1(7) . . ? C2 C1 Er2 71.1(4) . . ? C7 C1 Er2 74.3(4) . . ? C2 C1 Er1 77.2(4) . . ? C7 C1 Er1 73.0(4) . . ? Er2 C1 Er1 101.2(2) . . ? C1 C2 C3 128.8(7) . . ? C1 C2 Er2 77.1(5) . . ? C3 C2 Er2 75.4(4) . . ? C1 C2 Er1 72.0(4) . . ? C3 C2 Er1 72.2(4) . . ? Er2 C2 Er1 101.4(3) . . ? C2 C3 C4 127.5(7) . . ? C2 C3 Er2 71.5(4) . . ? C4 C3 Er2 75.6(4) . . ? C2 C3 Er1 75.9(4) . . ? C4 C3 Er1 71.9(4) . . ? Er2 C3 Er1 101.4(2) . . ? C5 C4 C3 127.6(6) . . ? C5 C4 Er1 77.2(4) . . ? C3 C4 Er1 75.2(4) . . ? C5 C4 Er2 71.2(4) . . ? C3 C4 Er2 71.6(4) . . ? Er1 C4 Er2 101.1(2) . . ? C6 C5 C4 128.1(7) . . ? C6 C5 Er2 73.2(4) . . ? C4 C5 Er2 76.8(4) . . ? C6 C5 Er1 74.3(4) . . ? C4 C5 Er1 71.1(4) . . ? Er2 C5 Er1 100.9(2) . . ? C7 C6 C5 129.3(8) . . ? C7 C6 Er2 76.8(4) . . ? C5 C6 Er2 74.3(4) . . ? C7 C6 Er1 71.6(4) . . ? C5 C6 Er1 74.5(4) . . ? Er2 C6 Er1 101.4(3) . . ? C6 C7 C1 129.5(7) . . ? C6 C7 Er1 77.4(5) . . ? C1 C7 Er1 74.9(4) . . ? C6 C7 Er2 71.7(4) . . ? C1 C7 Er2 73.7(4) . . ? Er1 C7 Er2 101.6(3) . . ? Si3 C14 K1 169.0(4) . 4_566 ? Si5 C21 K1 74.7(3) . . ? Si6 C23 K1 89.9(3) . . ? Si7 C28 K1 89.0(3) . . ? Si8 C29 K1 75.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Si2 N1 Si1 -73.9(5) . . . . ? C11 Si2 N1 Si1 52.4(5) . . . . ? C13 Si2 N1 Si1 169.1(4) . . . . ? Er1 Si2 N1 Si1 -175.5(5) . . . . ? C12 Si2 N1 Er1 101.6(5) . . . . ? C11 Si2 N1 Er1 -132.1(4) . . . . ? C13 Si2 N1 Er1 -15.4(4) . . . . ? C8 Si1 N1 Si2 148.5(5) . . . . ? C9 Si1 N1 Si2 28.4(5) . . . . ? C10 Si1 N1 Si2 -90.2(5) . . . . ? C8 Si1 N1 Er1 -25.6(6) . . . . ? C9 Si1 N1 Er1 -145.7(5) . . . . ? C10 Si1 N1 Er1 95.7(5) . . . . ? C16 Si3 N2 Si4 -153.5(4) . . . . ? C14 Si3 N2 Si4 84.4(4) . . . . ? C15 Si3 N2 Si4 -35.5(5) . . . . ? Er1 Si3 N2 Si4 -178.0(5) . . . . ? C16 Si3 N2 Er1 24.5(4) . . . . ? C14 Si3 N2 Er1 -97.6(3) . . . . ? C15 Si3 N2 Er1 142.5(4) . . . . ? C19 Si4 N2 Si3 -165.0(4) . . . . ? C18 Si4 N2 Si3 -46.1(5) . . . . ? C17 Si4 N2 Si3 74.8(6) . . . . ? C19 Si4 N2 Er1 17.4(6) . . . . ? C18 Si4 N2 Er1 136.3(4) . . . . ? C17 Si4 N2 Er1 -102.8(5) . . . . ? C25 Si6 N3 Si5 -145.6(3) . . . . ? C23 Si6 N3 Si5 93.9(4) . . . . ? C24 Si6 N3 Si5 -23.5(4) . . . . ? K1 Si6 N3 Si5 99.6(3) . . . . ? C25 Si6 N3 Er2 11.5(4) . . . . ? C23 Si6 N3 Er2 -108.9(4) . . . . ? C24 Si6 N3 Er2 133.7(4) . . . . ? K1 Si6 N3 Er2 -103.3(3) . . . . ? C25 Si6 N3 K1 114.8(3) . . . . ? C23 Si6 N3 K1 -5.7(4) . . . . ? C24 Si6 N3 K1 -123.1(3) . . . . ? C22 Si5 N3 Si6 70.5(5) . . . . ? C20 Si5 N3 Si6 -170.6(4) . . . . ? C21 Si5 N3 Si6 -53.7(4) . . . . ? Er2 Si5 N3 Si6 160.0(4) . . . . ? K1 Si5 N3 Si6 -104.1(3) . . . . ? C22 Si5 N3 Er2 -89.5(4) . . . . ? C20 Si5 N3 Er2 29.4(4) . . . . ? C21 Si5 N3 Er2 146.3(3) . . . . ? K1 Si5 N3 Er2 95.9(2) . . . . ? C22 Si5 N3 K1 174.6(3) . . . . ? C20 Si5 N3 K1 -66.5(3) . . . . ? C21 Si5 N3 K1 50.3(4) . . . . ? Er2 Si5 N3 K1 -95.9(2) . . . . ? C26 Si7 N4 Si8 -147.7(4) . . . . ? C27 Si7 N4 Si8 -27.1(5) . . . . ? C28 Si7 N4 Si8 91.4(5) . . . . ? K1 Si7 N4 Si8 100.9(3) . . . . ? C26 Si7 N4 Er2 8.4(5) . . . . ? C27 Si7 N4 Er2 129.0(4) . . . . ? C28 Si7 N4 Er2 -112.5(5) . . . . ? K1 Si7 N4 Er2 -103.0(3) . . . . ? C26 Si7 N4 K1 111.4(3) . . . . ? C27 Si7 N4 K1 -128.0(3) . . . . ? C28 Si7 N4 K1 -9.5(4) . . . . ? C31 Si8 N4 Si7 -173.2(4) . . . . ? C29 Si8 N4 Si7 -55.6(5) . . . . ? C30 Si8 N4 Si7 68.3(5) . . . . ? Er2 Si8 N4 Si7 159.6(5) . . . . ? K1 Si8 N4 Si7 -105.0(3) . . . . ? C31 Si8 N4 Er2 27.2(4) . . . . ? C29 Si8 N4 Er2 144.8(4) . . . . ? C30 Si8 N4 Er2 -91.3(4) . . . . ? K1 Si8 N4 Er2 95.4(2) . . . . ? C31 Si8 N4 K1 -68.2(3) . . . . ? C29 Si8 N4 K1 49.4(4) . . . . ? C30 Si8 N4 K1 173.3(3) . . . . ? Er2 Si8 N4 K1 -95.4(2) . . . . ? C7 C1 C2 C3 -8.3(12) . . . . ? Er2 C1 C2 C3 -59.0(7) . . . . ? Er1 C1 C2 C3 47.7(7) . . . . ? C7 C1 C2 Er2 50.7(7) . . . . ? Er1 C1 C2 Er2 106.7(2) . . . . ? C7 C1 C2 Er1 -56.0(7) . . . . ? Er2 C1 C2 Er1 -106.7(2) . . . . ? C1 C2 C3 C4 5.8(12) . . . . ? Er2 C2 C3 C4 -54.0(6) . . . . ? Er1 C2 C3 C4 53.4(6) . . . . ? C1 C2 C3 Er2 59.7(7) . . . . ? Er1 C2 C3 Er2 107.3(2) . . . . ? C1 C2 C3 Er1 -47.6(7) . . . . ? Er2 C2 C3 Er1 -107.3(2) . . . . ? C2 C3 C4 C5 5.6(11) . . . . ? Er2 C3 C4 C5 -46.7(6) . . . . ? Er1 C3 C4 C5 60.6(6) . . . . ? C2 C3 C4 Er1 -55.0(7) . . . . ? Er2 C3 C4 Er1 -107.3(2) . . . . ? C2 C3 C4 Er2 52.4(6) . . . . ? Er1 C3 C4 Er2 107.3(2) . . . . ? C3 C4 C5 C6 -8.9(11) . . . . ? Er1 C4 C5 C6 50.8(7) . . . . ? Er2 C4 C5 C6 -55.8(6) . . . . ? C3 C4 C5 Er2 46.9(6) . . . . ? Er1 C4 C5 Er2 106.6(2) . . . . ? C3 C4 C5 Er1 -59.7(6) . . . . ? Er2 C4 C5 Er1 -106.6(2) . . . . ? C4 C5 C6 C7 -0.2(12) . . . . ? Er2 C5 C6 C7 -57.5(7) . . . . ? Er1 C5 C6 C7 49.4(7) . . . . ? C4 C5 C6 Er2 57.3(7) . . . . ? Er1 C5 C6 Er2 106.9(2) . . . . ? C4 C5 C6 Er1 -49.6(6) . . . . ? Er2 C5 C6 Er1 -106.9(2) . . . . ? C5 C6 C7 C1 7.5(13) . . . . ? Er2 C6 C7 C1 -49.0(7) . . . . ? Er1 C6 C7 C1 58.0(7) . . . . ? C5 C6 C7 Er1 -50.4(7) . . . . ? Er2 C6 C7 Er1 -107.0(2) . . . . ? C5 C6 C7 Er2 56.5(7) . . . . ? Er1 C6 C7 Er2 107.0(2) . . . . ? C2 C1 C7 C6 -1.3(12) . . . . ? Er2 C1 C7 C6 48.3(7) . . . . ? Er1 C1 C7 C6 -59.0(7) . . . . ? C2 C1 C7 Er1 57.7(7) . . . . ? Er2 C1 C7 Er1 107.3(2) . . . . ? C2 C1 C7 Er2 -49.6(7) . . . . ? Er1 C1 C7 Er2 -107.3(2) . . . . ? N2 Si3 C14 K1 -87(2) . . . 4_566 ? C16 Si3 C14 K1 151.1(19) . . . 4_566 ? C15 Si3 C14 K1 41(2) . . . 4_566 ? Er1 Si3 C14 K1 -130.1(19) . . . 4_566 ? N3 Si5 C21 K1 -42.3(3) . . . . ? C22 Si5 C21 K1 -171.2(3) . . . . ? C20 Si5 C21 K1 77.2(3) . . . . ? Er2 Si5 C21 K1 -7.7(4) . . . . ? N3 Si6 C23 K1 5.2(3) . . . . ? C25 Si6 C23 K1 -119.7(3) . . . . ? C24 Si6 C23 K1 129.8(3) . . . . ? N4 Si7 C28 K1 8.6(4) . . . . ? C26 Si7 C28 K1 -117.8(3) . . . . ? C27 Si7 C28 K1 133.0(3) . . . . ? N4 Si8 C29 K1 -41.5(3) . . . . ? C31 Si8 C29 K1 78.6(3) . . . . ? C30 Si8 C29 K1 -169.7(3) . . . . ? Er2 Si8 C29 K1 -4.2(5) . . . . ? _refine_diff_density_max 3.653 _refine_diff_density_min -2.021 _refine_diff_density_rms 0.173 _shelx_res_file ; mm466_5.res created by SHELXL-2014/7 TITL mm466_4 in P2(1)/n CELL 0.71073 14.09460 14.29650 25.10550 90.0000 95.1701 90.0000 ZERR 4.00 0.00070 0.00080 0.00130 0.0000 0.0027 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N SI K ER UNIT 124 316 16 32 4 8 TEMP -73.150 SIZE 0.43 0.543 0.80 L.S. 80 ACTA CONF LIST 0 BOND FMAP 2 PLAN 5 OMIT 1 1 32 OMIT -1 1 30 OMIT 3 1 20 OMIT -1 1 22 OMIT -12 1 5 OMIT 0 2 23 OMIT 0 2 31 OMIT 5 1 28 OMIT 0 0 2 OMIT -12 1 13 OMIT -13 1 18 OMIT 3 1 26 OMIT -2 2 29 OMIT 14 1 2 OMIT 2 2 31 OMIT -6 2 3 OMIT 4 2 27 OMIT 2 2 23 OMIT 1 1 26 OMIT 12 3 8 OMIT 1 1 24 OMIT 5 6 27 OMIT 5 6 27 OMIT 2 5 21 OMIT -13 1 10 OMIT -15 1 16 OMIT 3 1 34 OMIT 16 2 4 OMIT 3 1 32 OMIT 13 2 9 OMIT -11 1 12 OMIT 3 4 1 OMIT 5 10 13 OMIT -3 1 28 OMIT 12 1 8 OMIT -2 13 6 OMIT 6 5 17 OMIT 4 11 12 OMIT -1 2 21 OMIT 16 0 4 OMIT 6 1 29 OMIT 1 4 4 OMIT 6 4 17 OMIT 14 3 10 OMIT 1 2 1 OMIT 9 2 20 OMIT -3 1 7 OMIT 8 3 19 OMIT -17 1 6 OMIT -1 1 24 WGHT 0.057100 21.348400 BASF 0.35221 FVAR 0.13048 ER1 6 0.172125 0.231051 1.066947 11.00000 0.02367 0.02770 = 0.01755 -0.00068 0.00762 0.00015 ER2 6 0.302787 0.225585 0.933887 11.00000 0.02287 0.02523 = 0.01457 -0.00170 0.00566 -0.00227 K1 5 0.434660 0.217070 0.805309 11.00000 0.04942 0.05078 = 0.02713 -0.01807 0.01746 -0.02047 SI1 4 0.317662 0.207242 1.194516 11.00000 0.03386 0.06396 = 0.02580 0.01105 0.00497 0.00710 SI2 4 0.176484 0.066060 1.154225 11.00000 0.05510 0.02911 = 0.03636 0.00750 0.02330 0.00431 SI3 4 0.051700 0.386782 1.129807 11.00000 0.03489 0.02799 = 0.02868 0.00088 0.01164 0.00617 SI4 4 -0.078288 0.287198 1.050497 11.00000 0.02553 0.05338 = 0.03251 0.00632 0.00499 -0.00175 SI5 4 0.542188 0.250422 0.934430 11.00000 0.02286 0.03006 = 0.04009 -0.00216 0.00544 0.00087 SI6 4 0.442221 0.421009 0.894156 11.00000 0.03265 0.02916 = 0.02441 0.00081 0.00706 -0.00563 SI7 4 0.289957 0.021231 0.848446 11.00000 0.04348 0.03000 = 0.03162 -0.00848 0.00996 -0.00647 SI8 4 0.187861 0.193245 0.812475 11.00000 0.03566 0.04270 = 0.02231 0.00048 0.00050 -0.00502 N1 3 0.230122 0.171435 1.146845 11.00000 0.03266 0.03722 = 0.02537 0.01184 0.01016 0.01003 N2 3 0.034465 0.303990 1.082189 11.00000 0.02038 0.03821 = 0.02604 -0.00059 0.00919 0.00544 N3 3 0.437175 0.304608 0.910987 11.00000 0.02355 0.02433 = 0.02610 -0.00354 0.01054 -0.00572 N4 3 0.271330 0.138708 0.855878 11.00000 0.03342 0.02676 = 0.02524 -0.01085 0.00579 -0.00882 C1 1 0.334715 0.266242 1.033142 11.00000 0.03459 0.10667 = 0.02686 -0.01602 0.01285 -0.03384 AFIX 43 H1A 2 0.389406 0.288772 1.054135 11.00000 -1.20000 AFIX 0 C2 1 0.327720 0.170270 1.027873 11.00000 0.04972 0.11129 = 0.02973 0.02310 0.01875 0.04206 AFIX 43 H2A 2 0.382200 0.135804 1.041528 11.00000 -1.20000 AFIX 0 C3 1 0.249542 0.115737 1.004636 11.00000 0.10613 0.02343 = 0.04381 0.01143 0.04362 0.01666 AFIX 43 H3A 2 0.256049 0.049779 1.007770 11.00000 -1.20000 AFIX 0 C4 1 0.161587 0.149455 0.976875 11.00000 0.06736 0.07111 = 0.03133 -0.03566 0.02986 -0.05592 AFIX 43 H4A 2 0.114723 0.103446 0.966834 11.00000 -1.20000 AFIX 0 C5 1 0.137436 0.242533 0.963030 11.00000 0.02684 0.10344 = 0.01967 -0.00286 0.00536 0.00619 AFIX 43 H5A 2 0.080461 0.250784 0.940273 11.00000 -1.20000 AFIX 0 C6 1 0.187173 0.324677 0.978707 11.00000 0.07541 0.05061 = 0.04346 0.01479 0.03653 0.02953 AFIX 43 H6A 2 0.159199 0.381146 0.964914 11.00000 -1.20000 AFIX 0 C7 1 0.270714 0.335137 1.011218 11.00000 0.08314 0.03670 = 0.03974 -0.01584 0.03949 -0.02273 AFIX 43 H7A 2 0.287738 0.397852 1.020193 11.00000 -1.20000 AFIX 0 C8 1 0.411303 0.281618 1.167539 11.00000 0.04557 0.11155 = 0.03420 0.00799 -0.00448 -0.02817 AFIX 33 H8A 2 0.458718 0.299453 1.196728 11.00000 -1.50000 H8B 2 0.442461 0.246366 1.140527 11.00000 -1.50000 H8C 2 0.381835 0.338037 1.151214 11.00000 -1.50000 AFIX 0 C9 1 0.385324 0.108844 1.229956 11.00000 0.05599 0.10833 = 0.09122 0.03614 -0.00350 0.02276 AFIX 33 H9A 2 0.433773 0.134537 1.256405 11.00000 -1.50000 H9B 2 0.341214 0.069501 1.248060 11.00000 -1.50000 H9C 2 0.416294 0.071150 1.203898 11.00000 -1.50000 AFIX 0 C10 1 0.270876 0.276723 1.250395 11.00000 0.06260 0.10596 = 0.02976 -0.01884 0.00448 0.00392 AFIX 33 H10A 2 0.324039 0.294988 1.276149 11.00000 -1.50000 H10B 2 0.238465 0.332913 1.235660 11.00000 -1.50000 H10C 2 0.225812 0.238376 1.268413 11.00000 -1.50000 AFIX 0 C11 1 0.128305 0.048932 1.220501 11.00000 0.06197 0.05552 = 0.04251 0.01275 0.02415 -0.00260 AFIX 33 H11A 2 0.098736 -0.012996 1.221615 11.00000 -1.50000 H11B 2 0.180342 0.053635 1.249018 11.00000 -1.50000 H11C 2 0.080573 0.097174 1.225621 11.00000 -1.50000 AFIX 0 C12 1 0.251249 -0.036846 1.140579 11.00000 0.11749 0.04033 = 0.09307 0.01654 0.05793 0.03024 AFIX 33 H12A 2 0.215433 -0.094421 1.145679 11.00000 -1.50000 H12B 2 0.268439 -0.033943 1.103651 11.00000 -1.50000 H12C 2 0.309280 -0.036411 1.165214 11.00000 -1.50000 AFIX 0 C13 1 0.069852 0.056284 1.104543 11.00000 0.07985 0.04765 = 0.04200 -0.00162 0.01086 -0.02636 AFIX 33 H13A 2 0.038896 -0.004320 1.108735 11.00000 -1.50000 H13B 2 0.024934 0.106685 1.110592 11.00000 -1.50000 H13C 2 0.089837 0.061363 1.068265 11.00000 -1.50000 AFIX 0 C14 1 0.023525 0.343855 1.197428 11.00000 0.05080 0.04086 = 0.03252 -0.00076 0.01154 0.00953 AFIX 33 H14A 2 0.034598 0.394292 1.223688 11.00000 -1.50000 H14B 2 -0.043337 0.324348 1.195702 11.00000 -1.50000 H14C 2 0.064636 0.290559 1.208126 11.00000 -1.50000 AFIX 0 C15 1 -0.020092 0.497460 1.120386 11.00000 0.06636 0.03487 = 0.06871 0.00763 0.01348 0.01621 AFIX 33 H15A 2 -0.003632 0.539659 1.150572 11.00000 -1.50000 H15B 2 -0.005910 0.528010 1.087071 11.00000 -1.50000 H15C 2 -0.088125 0.482355 1.118609 11.00000 -1.50000 AFIX 0 C16 1 0.178610 0.428031 1.133417 11.00000 0.04293 0.03153 = 0.04037 -0.00363 0.00221 -0.00965 AFIX 33 H16A 2 0.188819 0.476219 1.161102 11.00000 -1.50000 H16B 2 0.221432 0.375176 1.142257 11.00000 -1.50000 H16C 2 0.191808 0.454223 1.098774 11.00000 -1.50000 AFIX 0 C17 1 -0.113347 0.382135 1.000692 11.00000 0.05588 0.10513 = 0.06827 0.05016 -0.01576 -0.01551 AFIX 33 H17A 2 -0.177521 0.369682 0.983810 11.00000 -1.50000 H17B 2 -0.112672 0.442648 1.019061 11.00000 -1.50000 H17C 2 -0.068111 0.383536 0.973259 11.00000 -1.50000 AFIX 0 C18 1 -0.170333 0.283410 1.099901 11.00000 0.03048 0.05578 = 0.04910 0.00742 0.01061 0.00308 AFIX 33 H18A 2 -0.233410 0.273848 1.080890 11.00000 -1.50000 H18B 2 -0.156039 0.231789 1.125032 11.00000 -1.50000 H18C 2 -0.169667 0.342614 1.119607 11.00000 -1.50000 AFIX 0 C19 1 -0.094286 0.175653 1.012163 11.00000 0.04060 0.09467 = 0.05796 -0.03178 -0.00038 -0.01001 AFIX 33 H19A 2 -0.159814 0.171761 0.995564 11.00000 -1.50000 H19B 2 -0.049871 0.174006 0.984308 11.00000 -1.50000 H19C 2 -0.081577 0.122601 1.036483 11.00000 -1.50000 AFIX 0 C20 1 0.522242 0.120962 0.938952 11.00000 0.05111 0.02901 = 0.06839 0.00097 0.01473 0.00401 AFIX 33 H20A 2 0.581899 0.090284 0.952263 11.00000 -1.50000 H20B 2 0.473489 0.108593 0.963524 11.00000 -1.50000 H20C 2 0.500924 0.096417 0.903431 11.00000 -1.50000 AFIX 0 C21 1 0.639737 0.263908 0.888188 11.00000 0.03755 0.04735 = 0.08247 -0.00725 0.02882 0.00011 AFIX 33 H21A 2 0.697296 0.231856 0.903545 11.00000 -1.50000 H21B 2 0.619007 0.236391 0.853318 11.00000 -1.50000 H21C 2 0.653555 0.330479 0.883694 11.00000 -1.50000 AFIX 0 C22 1 0.592931 0.286173 1.002058 11.00000 0.04721 0.05100 = 0.05616 -0.00046 -0.01521 0.00163 AFIX 33 H22A 2 0.652072 0.251587 1.011560 11.00000 -1.50000 H22B 2 0.606432 0.353422 1.002233 11.00000 -1.50000 H22C 2 0.547114 0.272411 1.028131 11.00000 -1.50000 AFIX 0 C23 1 0.455969 0.435195 0.820906 11.00000 0.06872 0.06551 = 0.02077 0.00787 0.00909 -0.01826 AFIX 33 H23A 2 0.458689 0.501905 0.812193 11.00000 -1.50000 H23B 2 0.514897 0.404640 0.812252 11.00000 -1.50000 H23C 2 0.401497 0.406446 0.800037 11.00000 -1.50000 AFIX 0 C24 1 0.545846 0.488178 0.927278 11.00000 0.04344 0.03493 = 0.05852 -0.00196 0.00773 -0.01103 AFIX 33 H24A 2 0.542348 0.553352 0.915164 11.00000 -1.50000 H24B 2 0.543754 0.486065 0.966171 11.00000 -1.50000 H24C 2 0.605502 0.460164 0.917780 11.00000 -1.50000 AFIX 0 C25 1 0.334707 0.489854 0.908246 11.00000 0.04300 0.02922 = 0.04581 0.00299 0.00464 0.00135 AFIX 33 H25A 2 0.342871 0.555128 0.897647 11.00000 -1.50000 H25B 2 0.278305 0.463570 0.887923 11.00000 -1.50000 H25C 2 0.326520 0.486996 0.946563 11.00000 -1.50000 AFIX 0 C26 1 0.323764 -0.044230 0.911191 11.00000 0.06238 0.03276 = 0.04858 -0.00411 0.00286 0.00154 AFIX 33 H26A 2 0.332798 -0.110416 0.902834 11.00000 -1.50000 H26B 2 0.383212 -0.018645 0.928573 11.00000 -1.50000 H26C 2 0.273121 -0.038172 0.935276 11.00000 -1.50000 AFIX 0 C27 1 0.184737 -0.044857 0.816951 11.00000 0.08127 0.04030 = 0.04859 -0.00366 -0.00913 -0.01941 AFIX 33 H27A 2 0.201292 -0.111148 0.814184 11.00000 -1.50000 H27B 2 0.131223 -0.038270 0.839031 11.00000 -1.50000 H27C 2 0.166624 -0.019742 0.781155 11.00000 -1.50000 AFIX 0 C28 1 0.387425 -0.001852 0.803551 11.00000 0.08918 0.03808 = 0.07269 -0.02235 0.04674 -0.00599 AFIX 33 H28A 2 0.396413 -0.069479 0.800076 11.00000 -1.50000 H28B 2 0.369735 0.025219 0.768185 11.00000 -1.50000 H28C 2 0.446853 0.026689 0.819027 11.00000 -1.50000 AFIX 0 C29 1 0.209438 0.176943 0.740309 11.00000 0.07820 0.06918 = 0.02044 0.00034 0.00020 -0.01232 AFIX 33 H29A 2 0.159755 0.209488 0.717583 11.00000 -1.50000 H29B 2 0.271898 0.202739 0.734070 11.00000 -1.50000 H29C 2 0.207920 0.110098 0.731627 11.00000 -1.50000 AFIX 0 C30 1 0.060653 0.158913 0.819345 11.00000 0.03650 0.06825 = 0.05454 0.00600 -0.00456 -0.01115 AFIX 33 H30A 2 0.018417 0.193383 0.793109 11.00000 -1.50000 H30B 2 0.052987 0.091586 0.813005 11.00000 -1.50000 H30C 2 0.044308 0.173891 0.855497 11.00000 -1.50000 AFIX 0 C31 1 0.192328 0.322074 0.824155 11.00000 0.04333 0.04423 = 0.04751 0.00487 -0.00063 0.00654 AFIX 33 H31A 2 0.144610 0.352955 0.799321 11.00000 -1.50000 H31B 2 0.178871 0.335369 0.861021 11.00000 -1.50000 H31C 2 0.255851 0.345587 0.818259 11.00000 -1.50000 AFIX 0 HKLF 5 REM mm466_4 in P2(1)/n REM R1 = 0.0443 for 12527 Fo > 4sig(Fo) and 0.0648 for all 15164 data REM 416 parameters refined using 0 restraints END WGHT 0.0344 21.3450 REM Highest difference peak 3.653, deepest hole -2.021, 1-sigma level 0.173 Q1 1 0.0409 0.2393 1.2004 11.00000 0.05 3.65 Q2 1 0.3449 0.2233 0.9238 11.00000 0.05 2.09 Q3 1 0.2778 0.2658 0.9656 11.00000 0.05 2.00 Q4 1 0.1847 0.2745 1.0470 11.00000 0.05 1.82 Q5 1 0.2193 0.2323 1.0448 11.00000 0.05 1.72 ; _shelx_res_checksum 75421 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mm422 _database_code_depnum_ccdc_archive 'CCDC 1454171' _audit_update_record ; 2016-02-18 deposited with the CCDC. 2016-08-08 downloaded from the CCDC. ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H95 Er2 K N4 O2 Si8' _chemical_formula_weight 1250.52 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' 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 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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+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 20.1042(7) _cell_length_b 18.7574(6) _cell_length_c 16.5696(6) _cell_angle_alpha 90 _cell_angle_beta 107.8505(17) _cell_angle_gamma 90 _cell_volume 5947.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 28.38 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_density_meas n/a _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_F_000 2560 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.677 _exptl_crystal_size_mid 0.530 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 3.066 _shelx_estimated_absorpt_T_min 0.231 _shelx_estimated_absorpt_T_max 0.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4772 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23004 _diffrn_reflns_av_unetI/netI 0.0285 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.520 _diffrn_reflns_theta_max 28.381 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_point_group_measured_fraction_full 0.981 _reflns_number_total 7321 _reflns_number_gt 6576 _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 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-03 (Sheldrick, 2003)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0827P)^2^+27.3690P] 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 7321 _refine_ls_number_parameters 286 _refine_ls_number_restraints 657 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _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 0.5000 0.28621(2) 0.2500 0.02486(9) Uani 1 2 d S TU P A . Er2 Er 0.5000 0.49787(2) 0.2500 0.02297(9) Uani 1 2 d S TU P . . K1 K 0.5000 0.07739(7) 0.2500 0.0410(3) Uani 1 2 d S TU P A . Si1 Si 0.41306(7) 0.18800(7) 0.07984(8) 0.0343(3) Uani 1 1 d . U . . . Si2 Si 0.56302(7) 0.19393(7) 0.09638(9) 0.0340(3) Uani 1 1 d . U . . . Si3 Si 0.61326(8) 0.61633(7) 0.23005(9) 0.0366(3) Uani 1 1 d . U . . . Si4 Si 0.65568(7) 0.56301(7) 0.40593(9) 0.0344(3) Uani 1 1 d . U . . . O1 O 0.5917(3) -0.0304(2) 0.2845(3) 0.0620(12) Uani 1 1 d . U . . . N1 N 0.4963(2) 0.20846(18) 0.1398(2) 0.0274(7) Uani 1 1 d . U . . . N2 N 0.59579(19) 0.56619(18) 0.3066(2) 0.0276(7) Uani 1 1 d . U . . . C1 C 0.4864(8) 0.3932(5) 0.1475(6) 0.0280(19) Uani 0.5 1 d D U P A -1 H1A H 0.4770 0.3990 0.0881 0.034 Uiso 0.5 1 calc R U P A -1 C2 C 0.4269(6) 0.3875(5) 0.1758(8) 0.0286(19) Uani 0.5 1 d D U P A -1 H2A H 0.3834 0.3824 0.1327 0.034 Uiso 0.5 1 calc R U P A -1 C3 C 0.4239(6) 0.3885(5) 0.2597(10) 0.0278(18) Uani 0.5 1 d D U P A -1 H3A H 0.3785 0.3849 0.2657 0.033 Uiso 0.5 1 calc R U P A -1 C4 C 0.4800(8) 0.3942(5) 0.3364(8) 0.0288(19) Uani 0.5 1 d D U P A -1 H4A H 0.4669 0.4008 0.3864 0.035 Uiso 0.5 1 calc R U P A -1 C5 C 0.5534(7) 0.3913(4) 0.3482(7) 0.0298(19) Uani 0.5 1 d D U P A -1 H5A H 0.5829 0.3928 0.4053 0.036 Uiso 0.5 1 calc R U P A -1 C6 C 0.5876(5) 0.3864(5) 0.2849(9) 0.0293(18) Uani 0.5 1 d D U P A -1 H6A H 0.6366 0.3787 0.3049 0.035 Uiso 0.5 1 calc R U P A -1 C7 C 0.5575(7) 0.3914(5) 0.1954(9) 0.0305(18) Uani 0.5 1 d D U P A -1 H7A H 0.5897 0.3940 0.1639 0.037 Uiso 0.5 1 calc R U P A -1 C8 C 0.3540(3) 0.1902(4) 0.1483(4) 0.0516(14) Uani 1 1 d . U . . . H8A H 0.3114 0.1631 0.1209 0.077 Uiso 1 1 calc R U . . . H8B H 0.3417 0.2397 0.1563 0.077 Uiso 1 1 calc R U . . . H8C H 0.3781 0.1689 0.2036 0.077 Uiso 1 1 calc R U . . . C9 C 0.3705(3) 0.2492(3) -0.0106(4) 0.0511(13) Uani 1 1 d . U . . . H9A H 0.3452 0.2210 -0.0603 0.077 Uiso 1 1 calc R U . . . H9B H 0.4064 0.2779 -0.0242 0.077 Uiso 1 1 calc R U . . . H9C H 0.3378 0.2808 0.0054 0.077 Uiso 1 1 calc R U . . . C10 C 0.4062(4) 0.0955(3) 0.0331(4) 0.0559(15) Uani 1 1 d . U . . . H10A H 0.3698 0.0950 -0.0221 0.084 Uiso 1 1 calc R U . A . H10B H 0.3940 0.0616 0.0713 0.084 Uiso 1 1 calc R U . . . H10C H 0.4511 0.0820 0.0258 0.084 Uiso 1 1 calc R U . . . C11 C 0.5374(4) 0.2099(4) -0.0216(4) 0.0559(15) Uani 1 1 d . U . . . H11A H 0.5203 0.2588 -0.0341 0.084 Uiso 1 1 calc R U . . . H11B H 0.5005 0.1763 -0.0508 0.084 Uiso 1 1 calc R U . . . H11C H 0.5782 0.2027 -0.0413 0.084 Uiso 1 1 calc R U . . . C12 C 0.6413(3) 0.2511(3) 0.1389(4) 0.0477(12) Uani 1 1 d . U . . . H12A H 0.6589 0.2460 0.2007 0.072 Uiso 1 1 calc R U . . . H12B H 0.6287 0.3010 0.1243 0.072 Uiso 1 1 calc R U . . . H12C H 0.6776 0.2365 0.1141 0.072 Uiso 1 1 calc R U . . . C13 C 0.5958(4) 0.0993(3) 0.1134(4) 0.0517(14) Uani 1 1 d . U . . . H13A H 0.6101 0.0882 0.1742 0.077 Uiso 1 1 calc R U . A . H13B H 0.6358 0.0938 0.0920 0.077 Uiso 1 1 calc R U . . . H13C H 0.5584 0.0667 0.0830 0.077 Uiso 1 1 calc R U . . . C14 C 0.5493(3) 0.5932(3) 0.1252(3) 0.0401(10) Uani 1 1 d . U . . . H14A H 0.5602 0.6205 0.0804 0.060 Uiso 1 1 calc R U . . . H14B H 0.5019 0.6049 0.1257 0.060 Uiso 1 1 calc R U . . . H14C H 0.5522 0.5421 0.1144 0.060 Uiso 1 1 calc R U . . . C15 C 0.6039(6) 0.7140(3) 0.2442(5) 0.083(3) Uani 1 1 d . U . . . H15A H 0.6438 0.7390 0.2352 0.124 Uiso 1 1 calc R U . . . H15B H 0.6025 0.7233 0.3019 0.124 Uiso 1 1 calc R U . . . H15C H 0.5606 0.7309 0.2031 0.124 Uiso 1 1 calc R U . . . C16 C 0.7020(4) 0.6003(5) 0.2175(6) 0.081(2) Uani 1 1 d . U . . . H16A H 0.7241 0.6461 0.2132 0.121 Uiso 1 1 calc R U . . . H16B H 0.6970 0.5724 0.1659 0.121 Uiso 1 1 calc R U . . . H16C H 0.7312 0.5740 0.2668 0.121 Uiso 1 1 calc R U . . . C17 C 0.7003(4) 0.6497(3) 0.4417(4) 0.0566(15) Uani 1 1 d . U . . . H17A H 0.6653 0.6866 0.4396 0.085 Uiso 1 1 calc R U . . . H17B H 0.7278 0.6631 0.4044 0.085 Uiso 1 1 calc R U . . . H17C H 0.7314 0.6450 0.5000 0.085 Uiso 1 1 calc R U . . . C18 C 0.7276(3) 0.4974(4) 0.4133(5) 0.0628(18) Uani 1 1 d . U . . . H18A H 0.7499 0.5083 0.3698 0.094 Uiso 1 1 calc R U . . . H18B H 0.7082 0.4491 0.4043 0.094 Uiso 1 1 calc R U . . . H18C H 0.7623 0.5005 0.4695 0.094 Uiso 1 1 calc R U . . . C19 C 0.6178(3) 0.5381(4) 0.4919(4) 0.0551(15) Uani 1 1 d . U . . . H19A H 0.5795 0.5707 0.4909 0.083 Uiso 1 1 calc R U . . . H19B H 0.6541 0.5414 0.5470 0.083 Uiso 1 1 calc R U . . . H19C H 0.6000 0.4892 0.4829 0.083 Uiso 1 1 calc R U . . . C20 C 0.5817(5) -0.0817(4) 0.2182(5) 0.0682(18) Uani 1 1 d . U . . . H20A H 0.5517 -0.0621 0.1637 0.082 Uiso 1 1 calc R U . A . H20B H 0.5597 -0.1255 0.2316 0.082 Uiso 1 1 calc R U . . . C21 C 0.6527(5) -0.0969(4) 0.2140(5) 0.0690(18) Uani 1 1 d . U . . . H21A H 0.6680 -0.0601 0.1807 0.083 Uiso 1 1 calc R U . . . H21B H 0.6549 -0.1443 0.1887 0.083 Uiso 1 1 calc R U . . . C22 C 0.6960(5) -0.0949(5) 0.3055(6) 0.087(3) Uani 1 1 d . U . . . H22A H 0.7442 -0.0787 0.3118 0.104 Uiso 1 1 calc R U . . . H22B H 0.6979 -0.1424 0.3322 0.104 Uiso 1 1 calc R U . . . C23 C 0.6581(5) -0.0421(5) 0.3439(5) 0.086(3) Uani 1 1 d . U . . . H23A H 0.6531 -0.0611 0.3974 0.104 Uiso 1 1 calc R U . . . H23B H 0.6846 0.0032 0.3565 0.104 Uiso 1 1 calc R U . . . 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 0.02932(15) 0.01535(13) 0.02986(15) 0.000 0.00902(11) 0.000 Er2 0.02196(14) 0.01560(13) 0.03230(16) 0.000 0.00971(11) 0.000 K1 0.0556(9) 0.0223(6) 0.0395(7) 0.000 0.0064(7) 0.000 Si1 0.0348(6) 0.0329(6) 0.0322(6) 0.0026(5) 0.0056(5) -0.0084(5) Si2 0.0391(7) 0.0278(6) 0.0387(7) -0.0027(5) 0.0173(6) 0.0021(5) Si3 0.0400(7) 0.0356(7) 0.0371(7) 0.0004(5) 0.0163(6) -0.0170(5) Si4 0.0269(6) 0.0355(6) 0.0383(7) 0.0013(5) 0.0063(5) -0.0047(5) O1 0.075(3) 0.046(2) 0.054(2) -0.0069(18) 0.003(2) 0.018(2) N1 0.0300(17) 0.0226(16) 0.0285(17) -0.0013(12) 0.0072(14) -0.0025(13) N2 0.0267(16) 0.0224(15) 0.0364(17) 0.0013(13) 0.0135(14) -0.0030(13) C1 0.037(5) 0.019(4) 0.024(3) -0.003(2) 0.004(4) 0.000(4) C2 0.030(4) 0.020(4) 0.032(5) -0.003(3) 0.003(3) -0.003(3) C3 0.025(4) 0.027(4) 0.032(4) 0.003(4) 0.008(4) -0.001(3) C4 0.037(5) 0.018(4) 0.034(4) -0.003(3) 0.016(4) -0.002(4) C5 0.037(5) 0.016(3) 0.036(4) -0.005(3) 0.011(3) -0.003(3) C6 0.024(3) 0.021(4) 0.039(5) -0.001(4) 0.004(4) 0.002(3) C7 0.033(5) 0.025(4) 0.037(5) -0.002(3) 0.015(4) -0.002(3) C8 0.037(3) 0.069(4) 0.047(3) 0.009(3) 0.010(2) -0.009(3) C9 0.050(3) 0.055(3) 0.040(3) 0.010(2) 0.001(2) -0.001(3) C10 0.068(4) 0.042(3) 0.051(3) -0.008(2) 0.009(3) -0.020(3) C11 0.065(4) 0.066(4) 0.042(3) 0.001(2) 0.024(3) 0.001(3) C12 0.040(3) 0.047(3) 0.062(3) -0.009(2) 0.025(2) -0.003(2) C13 0.061(4) 0.035(2) 0.064(4) -0.003(2) 0.028(3) 0.011(2) C14 0.047(3) 0.041(2) 0.037(2) 0.001(2) 0.019(2) -0.007(2) C15 0.153(8) 0.033(3) 0.059(4) 0.002(3) 0.027(5) -0.024(3) C16 0.045(3) 0.135(7) 0.072(5) 0.003(4) 0.031(3) -0.026(4) C17 0.061(4) 0.052(3) 0.052(3) -0.005(3) 0.010(3) -0.025(3) C18 0.034(3) 0.065(4) 0.075(4) -0.009(3) -0.006(3) 0.007(2) C19 0.057(3) 0.066(4) 0.041(3) 0.008(3) 0.012(3) -0.017(3) C20 0.092(5) 0.043(3) 0.066(4) -0.010(3) 0.019(3) 0.001(3) C21 0.093(5) 0.048(3) 0.071(4) -0.007(3) 0.031(4) -0.007(3) C22 0.077(5) 0.082(5) 0.085(5) -0.024(4) 0.000(4) 0.023(4) C23 0.083(5) 0.092(6) 0.061(4) -0.018(4) -0.012(3) 0.034(4) _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 2.321(4) 2_655 ? Er1 N1 2.321(4) . ? Er1 C2 2.485(9) . ? Er1 C3 2.490(9) . ? Er1 C6 2.518(9) . ? Er1 C5 2.572(9) . ? Er1 C4 2.582(9) . ? Er1 C7 2.587(9) . ? Er1 C1 2.589(10) . ? Er1 Si1 3.3729(13) . ? Er1 Si1 3.3730(13) 2_655 ? Er1 K1 3.9169(14) . ? Er2 N2 2.263(4) 2_655 ? Er2 N2 2.264(4) . ? Er2 C4 2.520(9) . ? Er2 C1 2.555(9) . ? Er2 C5 2.594(10) . ? Er2 C3 2.594(9) . ? Er2 C7 2.604(9) . ? Er2 C2 2.617(9) . ? Er2 C6 2.681(9) . ? Er2 Si3 3.2700(12) . ? Er2 Si3 3.2700(12) 2_655 ? K1 O1 2.676(4) 2_655 ? K1 O1 2.677(4) . ? K1 N1 3.050(4) 2_655 ? K1 N1 3.050(4) . ? K1 C13 3.415(6) . ? K1 C13 3.415(6) 2_655 ? K1 Si1 3.5053(16) . ? K1 Si1 3.5053(16) 2_655 ? K1 C20 3.522(7) . ? K1 C20 3.522(7) 2_655 ? K1 C10 3.526(7) 2_655 ? K1 C10 3.526(7) . ? Si1 N1 1.708(4) . ? Si1 C9 1.874(6) . ? Si1 C8 1.878(6) . ? Si1 C10 1.887(6) . ? Si2 N1 1.726(4) . ? Si2 C12 1.856(6) . ? Si2 C13 1.884(6) . ? Si2 C11 1.887(6) . ? Si3 N2 1.700(4) . ? Si3 C15 1.863(7) . ? Si3 C14 1.869(6) . ? Si3 C16 1.884(7) . ? Si4 N2 1.716(4) . ? Si4 C17 1.864(6) . ? Si4 C19 1.869(6) . ? Si4 C18 1.874(6) . ? O1 C23 1.413(9) . ? O1 C20 1.427(8) . ? C1 C7 1.408(10) . ? C1 C2 1.415(10) . ? C2 C3 1.410(10) . ? C3 C4 1.421(11) . ? C4 C5 1.429(11) . ? C5 C6 1.423(11) . ? C6 C7 1.423(11) . ? C20 C21 1.478(12) . ? C21 C22 1.501(12) . ? C22 C23 1.504(11) . ? 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 N1 102.12(17) 2_655 . ? N1 Er1 C2 137.8(4) 2_655 . ? N1 Er1 C2 102.7(3) . . ? N1 Er1 C3 107.8(3) 2_655 . ? N1 Er1 C3 131.5(4) . . ? C2 Er1 C3 32.9(2) . . ? N1 Er1 C6 115.9(3) 2_655 . ? N1 Er1 C6 120.1(3) . . ? C2 Er1 C6 79.0(3) . . ? C3 Er1 C6 79.1(3) . . ? N1 Er1 C5 94.4(3) 2_655 . ? N1 Er1 C5 152.4(3) . . ? C2 Er1 C5 78.2(3) . . ? C3 Er1 C5 60.9(3) . . ? C6 Er1 C5 32.4(2) . . ? N1 Er1 C4 91.7(2) 2_655 . ? N1 Er1 C4 163.1(3) . . ? C2 Er1 C4 60.4(3) . . ? C3 Er1 C4 32.5(2) . . ? C6 Er1 C4 60.3(3) . . ? C5 Er1 C4 32.2(2) . . ? N1 Er1 C7 147.7(4) 2_655 . ? N1 Er1 C7 96.6(3) . . ? C2 Er1 C7 60.2(3) . . ? C3 Er1 C7 77.5(3) . . ? C6 Er1 C7 32.3(2) . . ? C5 Er1 C7 59.5(3) . . ? C4 Er1 C7 76.0(3) . . ? N1 Er1 C1 167.2(3) 2_655 . ? N1 Er1 C1 90.0(2) . . ? C2 Er1 C1 32.3(2) . . ? C3 Er1 C1 60.1(3) . . ? C6 Er1 C1 59.9(3) . . ? C5 Er1 C1 76.2(3) . . ? C4 Er1 C1 75.7(3) . . ? C7 Er1 C1 31.6(2) . . ? N1 Er1 Si1 101.41(9) 2_655 . ? N1 Er1 Si1 27.82(10) . . ? C2 Er1 Si1 85.9(2) . . ? C3 Er1 Si1 107.7(3) . . ? C6 Er1 Si1 138.3(3) . . ? C5 Er1 Si1 163.0(2) . . ? C4 Er1 Si1 139.7(4) . . ? C7 Er1 Si1 107.3(3) . . ? C1 Er1 Si1 87.2(2) . . ? N1 Er1 Si1 27.82(10) 2_655 2_655 ? N1 Er1 Si1 101.41(9) . 2_655 ? C2 Er1 Si1 155.2(3) . 2_655 ? C3 Er1 Si1 122.6(3) . 2_655 ? C6 Er1 Si1 93.9(3) . 2_655 ? C5 Er1 Si1 83.2(2) . 2_655 ? C4 Er1 Si1 95.4(3) . 2_655 ? C7 Er1 Si1 122.4(3) . 2_655 ? C1 Er1 Si1 153.6(3) . 2_655 ? Si1 Er1 Si1 113.79(5) . 2_655 ? N1 Er1 K1 51.06(9) 2_655 . ? N1 Er1 K1 51.06(9) . . ? C2 Er1 K1 139.9(2) . . ? C3 Er1 K1 140.4(2) . . ? C6 Er1 K1 138.2(2) . . ? C5 Er1 K1 140.0(2) . . ? C4 Er1 K1 141.7(2) . . ? C7 Er1 K1 139.7(2) . . ? C1 Er1 K1 140.8(2) . . ? Si1 Er1 K1 56.89(2) . . ? Si1 Er1 K1 56.89(2) 2_655 . ? N2 Er2 N2 111.03(18) 2_655 . ? N2 Er2 C4 114.1(3) 2_655 . ? N2 Er2 C4 117.7(4) . . ? N2 Er2 C1 104.8(3) 2_655 . ? N2 Er2 C1 127.9(4) . . ? C4 Er2 C1 77.4(3) . . ? N2 Er2 C5 146.3(3) 2_655 . ? N2 Er2 C5 92.3(3) . . ? C4 Er2 C5 32.4(2) . . ? C1 Er2 C5 76.4(3) . . ? N2 Er2 C3 91.7(3) 2_655 . ? N2 Er2 C3 149.9(3) . . ? C4 Er2 C3 32.2(2) . . ? C1 Er2 C3 59.2(3) . . ? C5 Er2 C3 59.3(3) . . ? N2 Er2 C7 134.6(4) 2_655 . ? N2 Er2 C7 99.6(3) . . ? C4 Er2 C7 76.8(3) . . ? C1 Er2 C7 31.7(2) . . ? C5 Er2 C7 59.0(3) . . ? C3 Er2 C7 75.4(3) . . ? N2 Er2 C2 88.2(2) 2_655 . ? N2 Er2 C2 157.9(3) . . ? C4 Er2 C2 59.5(3) . . ? C1 Er2 C2 31.7(2) . . ? C5 Er2 C2 75.5(3) . . ? C3 Er2 C2 31.4(2) . . ? C7 Er2 C2 58.4(3) . . ? N2 Er2 C6 161.9(2) 2_655 . ? N2 Er2 C6 86.2(2) . . ? C4 Er2 C6 58.9(3) . . ? C1 Er2 C6 58.2(3) . . ? C5 Er2 C6 31.3(2) . . ? C3 Er2 C6 74.4(3) . . ? C7 Er2 C6 31.2(2) . . ? C2 Er2 C6 73.8(3) . . ? N2 Er2 Si3 95.95(9) 2_655 . ? N2 Er2 Si3 29.18(10) . . ? C4 Er2 Si3 145.0(4) . . ? C1 Er2 Si3 113.0(3) . . ? C5 Er2 Si3 114.9(3) . . ? C3 Er2 Si3 170.4(2) . . ? C7 Er2 Si3 95.1(2) . . ? C2 Er2 Si3 142.9(3) . . ? C6 Er2 Si3 96.9(2) . . ? N2 Er2 Si3 29.17(10) 2_655 2_655 ? N2 Er2 Si3 95.95(9) . 2_655 ? C4 Er2 Si3 103.3(3) . 2_655 ? C1 Er2 Si3 130.8(3) . 2_655 ? C5 Er2 Si3 128.8(3) . 2_655 ? C3 Er2 Si3 95.1(2) . 2_655 ? C7 Er2 Si3 162.4(3) . 2_655 ? C2 Er2 Si3 106.1(3) . 2_655 ? C6 Er2 Si3 160.1(3) . 2_655 ? Si3 Er2 Si3 94.39(5) . 2_655 ? O1 K1 O1 81.9(2) 2_655 . ? O1 K1 N1 128.70(14) 2_655 2_655 ? O1 K1 N1 126.31(12) . 2_655 ? O1 K1 N1 126.31(12) 2_655 . ? O1 K1 N1 128.70(14) . . ? N1 K1 N1 72.57(14) 2_655 . ? O1 K1 C13 116.14(16) 2_655 . ? O1 K1 C13 75.00(15) . . ? N1 K1 C13 112.61(12) 2_655 . ? N1 K1 C13 54.64(12) . . ? O1 K1 C13 75.01(15) 2_655 2_655 ? O1 K1 C13 116.15(16) . 2_655 ? N1 K1 C13 54.64(12) 2_655 2_655 ? N1 K1 C13 112.61(12) . 2_655 ? C13 K1 C13 166.16(18) . 2_655 ? O1 K1 Si1 97.71(10) 2_655 . ? O1 K1 Si1 139.44(11) . . ? N1 K1 Si1 85.36(8) 2_655 . ? N1 K1 Si1 29.16(7) . . ? C13 K1 Si1 68.85(11) . . ? C13 K1 Si1 102.60(12) 2_655 . ? O1 K1 Si1 139.44(11) 2_655 2_655 ? O1 K1 Si1 97.71(10) . 2_655 ? N1 K1 Si1 29.16(7) 2_655 2_655 ? N1 K1 Si1 85.36(8) . 2_655 ? C13 K1 Si1 102.61(12) . 2_655 ? C13 K1 Si1 68.85(11) 2_655 2_655 ? Si1 K1 Si1 107.42(6) . 2_655 ? O1 K1 C20 69.55(19) 2_655 . ? O1 K1 C20 21.59(16) . . ? N1 K1 C20 147.73(15) 2_655 . ? N1 K1 C20 121.34(15) . . ? C13 K1 C20 67.65(16) . . ? C13 K1 C20 125.76(17) 2_655 . ? Si1 K1 C20 121.43(13) . . ? Si1 K1 C20 118.76(14) 2_655 . ? O1 K1 C20 21.59(16) 2_655 2_655 ? O1 K1 C20 69.55(19) . 2_655 ? N1 K1 C20 121.34(15) 2_655 2_655 ? N1 K1 C20 147.73(15) . 2_655 ? C13 K1 C20 125.76(17) . 2_655 ? C13 K1 C20 67.65(16) 2_655 2_655 ? Si1 K1 C20 118.77(14) . 2_655 ? Si1 K1 C20 121.43(13) 2_655 2_655 ? C20 K1 C20 64.2(3) . 2_655 ? O1 K1 C10 114.14(15) 2_655 2_655 ? O1 K1 C10 74.74(14) . 2_655 ? N1 K1 C10 53.47(12) 2_655 2_655 ? N1 K1 C10 116.08(13) . 2_655 ? C13 K1 C10 115.43(18) . 2_655 ? C13 K1 C10 63.09(17) 2_655 2_655 ? Si1 K1 C10 137.88(11) . 2_655 ? Si1 K1 C10 31.13(10) 2_655 2_655 ? C20 K1 C10 96.07(16) . 2_655 ? C20 K1 C10 93.31(17) 2_655 2_655 ? O1 K1 C10 74.74(14) 2_655 . ? O1 K1 C10 114.14(15) . . ? N1 K1 C10 116.08(13) 2_655 . ? N1 K1 C10 53.47(12) . . ? C13 K1 C10 63.09(17) . . ? C13 K1 C10 115.43(18) 2_655 . ? Si1 K1 C10 31.13(10) . . ? Si1 K1 C10 137.88(11) 2_655 . ? C20 K1 C10 93.31(17) . . ? C20 K1 C10 96.08(16) 2_655 . ? C10 K1 C10 168.9(2) 2_655 . ? N1 Si1 C9 116.9(2) . . ? N1 Si1 C8 109.4(2) . . ? C9 Si1 C8 104.6(3) . . ? N1 Si1 C10 112.4(3) . . ? C9 Si1 C10 106.1(3) . . ? C8 Si1 C10 106.7(3) . . ? N1 Si1 Er1 39.36(12) . . ? C9 Si1 Er1 109.0(2) . . ? C8 Si1 Er1 75.2(2) . . ? C10 Si1 Er1 143.0(2) . . ? N1 Si1 K1 60.47(12) . . ? C9 Si1 K1 177.3(2) . . ? C8 Si1 K1 77.2(2) . . ? C10 Si1 K1 75.0(2) . . ? Er1 Si1 K1 69.39(3) . . ? N1 Si2 C12 115.3(2) . . ? N1 Si2 C13 111.5(2) . . ? C12 Si2 C13 105.7(3) . . ? N1 Si2 C11 114.0(3) . . ? C12 Si2 C11 103.4(3) . . ? C13 Si2 C11 106.0(3) . . ? N1 Si2 K1 50.18(12) . . ? C12 Si2 K1 119.3(2) . . ? C13 Si2 K1 62.4(2) . . ? C11 Si2 K1 137.2(2) . . ? N2 Si3 C15 113.4(3) . . ? N2 Si3 C14 109.0(2) . . ? C15 Si3 C14 106.2(3) . . ? N2 Si3 C16 114.4(3) . . ? C15 Si3 C16 107.8(5) . . ? C14 Si3 C16 105.4(3) . . ? N2 Si3 Er2 40.46(13) . . ? C15 Si3 Er2 123.7(3) . . ? C14 Si3 Er2 68.54(15) . . ? C16 Si3 Er2 128.0(3) . . ? N2 Si4 C17 113.7(3) . . ? N2 Si4 C19 114.2(2) . . ? C17 Si4 C19 104.2(3) . . ? N2 Si4 C18 112.7(3) . . ? C17 Si4 C18 105.4(3) . . ? C19 Si4 C18 105.8(4) . . ? C23 O1 C20 108.1(6) . . ? C23 O1 K1 135.1(4) . . ? C20 O1 K1 114.8(4) . . ? Si1 N1 Si2 118.1(2) . . ? Si1 N1 Er1 112.82(19) . . ? Si2 N1 Er1 125.85(19) . . ? Si1 N1 K1 90.37(14) . . ? Si2 N1 K1 104.06(16) . . ? Er1 N1 K1 92.65(12) . . ? Si3 N2 Si4 119.3(2) . . ? Si3 N2 Er2 110.36(19) . . ? Si4 N2 Er2 129.45(19) . . ? C7 C1 C2 128.8(10) . . ? C7 C1 Er2 76.1(6) . . ? C2 C1 Er2 76.5(5) . . ? C7 C1 Er1 74.1(6) . . ? C2 C1 Er1 69.8(5) . . ? Er2 C1 Er1 101.0(3) . . ? C3 C2 C1 128.5(9) . . ? C3 C2 Er1 73.7(5) . . ? C1 C2 Er1 77.9(6) . . ? C3 C2 Er2 73.4(5) . . ? C1 C2 Er2 71.7(5) . . ? Er1 C2 Er2 102.2(3) . . ? C2 C3 C4 128.4(9) . . ? C2 C3 Er1 73.4(5) . . ? C4 C3 Er1 77.3(5) . . ? C2 C3 Er2 75.2(5) . . ? C4 C3 Er2 71.0(5) . . ? Er1 C3 Er2 102.7(3) . . ? C3 C4 C5 128.5(9) . . ? C3 C4 Er2 76.8(5) . . ? C5 C4 Er2 76.6(6) . . ? C3 C4 Er1 70.2(5) . . ? C5 C4 Er1 73.5(5) . . ? Er2 C4 Er1 102.2(3) . . ? C6 C5 C4 127.9(10) . . ? C6 C5 Er1 71.7(5) . . ? C4 C5 Er1 74.3(5) . . ? C6 C5 Er2 77.8(6) . . ? C4 C5 Er2 71.0(6) . . ? Er1 C5 Er2 100.5(4) . . ? C7 C6 C5 128.1(10) . . ? C7 C6 Er1 76.5(6) . . ? C5 C6 Er1 75.9(6) . . ? C7 C6 Er2 71.4(5) . . ? C5 C6 Er2 71.0(6) . . ? Er1 C6 Er2 99.5(3) . . ? C1 C7 C6 128.6(10) . . ? C1 C7 Er1 74.3(6) . . ? C6 C7 Er1 71.2(5) . . ? C1 C7 Er2 72.3(5) . . ? C6 C7 Er2 77.4(6) . . ? Er1 C7 Er2 99.8(3) . . ? Si1 C10 K1 73.8(2) . . ? Si2 C13 K1 88.3(2) . . ? O1 C20 C21 104.9(6) . . ? O1 C20 K1 43.6(3) . . ? C21 C20 K1 132.2(5) . . ? C20 C21 C22 102.5(7) . . ? C21 C22 C23 103.4(7) . . ? O1 C23 C22 107.5(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Si1 N1 Si2 -73.2(3) . . . . ? C8 Si1 N1 Si2 168.2(3) . . . . ? C10 Si1 N1 Si2 49.8(3) . . . . ? Er1 Si1 N1 Si2 -160.8(3) . . . . ? K1 Si1 N1 Si2 106.2(2) . . . . ? C9 Si1 N1 Er1 87.6(3) . . . . ? C8 Si1 N1 Er1 -31.0(3) . . . . ? C10 Si1 N1 Er1 -149.4(2) . . . . ? K1 Si1 N1 Er1 -93.03(17) . . . . ? C9 Si1 N1 K1 -179.4(2) . . . . ? C8 Si1 N1 K1 62.0(3) . . . . ? C10 Si1 N1 K1 -56.4(3) . . . . ? Er1 Si1 N1 K1 93.03(17) . . . . ? C12 Si2 N1 Si1 153.8(3) . . . . ? C13 Si2 N1 Si1 -85.7(3) . . . . ? C11 Si2 N1 Si1 34.4(3) . . . . ? K1 Si2 N1 Si1 -98.1(2) . . . . ? C12 Si2 N1 Er1 -4.2(4) . . . . ? C13 Si2 N1 Er1 116.3(3) . . . . ? C11 Si2 N1 Er1 -123.7(3) . . . . ? K1 Si2 N1 Er1 103.9(3) . . . . ? C12 Si2 N1 K1 -108.1(3) . . . . ? C13 Si2 N1 K1 12.4(3) . . . . ? C11 Si2 N1 K1 132.5(2) . . . . ? C15 Si3 N2 Si4 -74.5(4) . . . . ? C14 Si3 N2 Si4 167.5(3) . . . . ? C16 Si3 N2 Si4 49.8(4) . . . . ? Er2 Si3 N2 Si4 170.4(3) . . . . ? C15 Si3 N2 Er2 115.1(4) . . . . ? C14 Si3 N2 Er2 -2.9(3) . . . . ? C16 Si3 N2 Er2 -120.6(3) . . . . ? C17 Si4 N2 Si3 37.7(4) . . . . ? C19 Si4 N2 Si3 157.0(3) . . . . ? C18 Si4 N2 Si3 -82.2(3) . . . . ? C17 Si4 N2 Er2 -154.0(3) . . . . ? C19 Si4 N2 Er2 -34.7(4) . . . . ? C18 Si4 N2 Er2 86.1(3) . . . . ? C7 C1 C2 C3 9.6(16) . . . . ? Er2 C1 C2 C3 -49.8(9) . . . . ? Er1 C1 C2 C3 57.6(9) . . . . ? C7 C1 C2 Er1 -48.0(9) . . . . ? Er2 C1 C2 Er1 -107.3(3) . . . . ? C7 C1 C2 Er2 59.3(9) . . . . ? Er1 C1 C2 Er2 107.3(3) . . . . ? C1 C2 C3 C4 -1.2(17) . . . . ? Er1 C2 C3 C4 58.1(9) . . . . ? Er2 C2 C3 C4 -50.3(9) . . . . ? C1 C2 C3 Er1 -59.3(9) . . . . ? Er2 C2 C3 Er1 -108.4(3) . . . . ? C1 C2 C3 Er2 49.1(9) . . . . ? Er1 C2 C3 Er2 108.4(3) . . . . ? C2 C3 C4 C5 -8.7(16) . . . . ? Er1 C3 C4 C5 47.8(9) . . . . ? Er2 C3 C4 C5 -60.6(9) . . . . ? C2 C3 C4 Er2 51.9(9) . . . . ? Er1 C3 C4 Er2 108.4(3) . . . . ? C2 C3 C4 Er1 -56.5(9) . . . . ? Er2 C3 C4 Er1 -108.4(3) . . . . ? C3 C4 C5 C6 4.2(16) . . . . ? Er2 C4 C5 C6 -56.4(9) . . . . ? Er1 C4 C5 C6 50.8(9) . . . . ? C3 C4 C5 Er1 -46.6(9) . . . . ? Er2 C4 C5 Er1 -107.2(3) . . . . ? C3 C4 C5 Er2 60.7(9) . . . . ? Er1 C4 C5 Er2 107.2(3) . . . . ? C4 C5 C6 C7 8.0(16) . . . . ? Er1 C5 C6 C7 59.8(9) . . . . ? Er2 C5 C6 C7 -45.7(9) . . . . ? C4 C5 C6 Er1 -51.8(9) . . . . ? Er2 C5 C6 Er1 -105.5(3) . . . . ? C4 C5 C6 Er2 53.7(9) . . . . ? Er1 C5 C6 Er2 105.5(3) . . . . ? C2 C1 C7 C6 -2.8(16) . . . . ? Er2 C1 C7 C6 56.7(9) . . . . ? Er1 C1 C7 C6 -49.2(9) . . . . ? C2 C1 C7 Er1 46.4(9) . . . . ? Er2 C1 C7 Er1 106.0(2) . . . . ? C2 C1 C7 Er2 -59.5(9) . . . . ? Er1 C1 C7 Er2 -106.0(2) . . . . ? C5 C6 C7 C1 -9.1(16) . . . . ? Er1 C6 C7 C1 50.4(9) . . . . ? Er2 C6 C7 C1 -54.7(9) . . . . ? C5 C6 C7 Er1 -59.5(9) . . . . ? Er2 C6 C7 Er1 -105.1(2) . . . . ? C5 C6 C7 Er2 45.6(9) . . . . ? Er1 C6 C7 Er2 105.1(2) . . . . ? N1 Si1 C10 K1 48.6(2) . . . . ? C9 Si1 C10 K1 177.5(2) . . . . ? C8 Si1 C10 K1 -71.4(2) . . . . ? Er1 Si1 C10 K1 16.1(4) . . . . ? N1 Si2 C13 K1 -10.7(3) . . . . ? C12 Si2 C13 K1 115.3(2) . . . . ? C11 Si2 C13 K1 -135.4(2) . . . . ? C23 O1 C20 C21 -29.8(9) . . . . ? K1 O1 C20 C21 136.8(5) . . . . ? C23 O1 C20 K1 -166.6(8) . . . . ? O1 C20 C21 C22 37.2(8) . . . . ? K1 C20 C21 C22 76.8(8) . . . . ? C20 C21 C22 C23 -30.4(10) . . . . ? C20 O1 C23 C22 9.8(10) . . . . ? K1 O1 C23 C22 -152.8(6) . . . . ? C21 C22 C23 O1 13.5(11) . . . . ? _refine_diff_density_max 1.380 _refine_diff_density_min -2.107 _refine_diff_density_rms 0.172 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mm422 in C2/c CELL 0.71073 20.10420 18.75740 16.56960 90.0000 107.8505 90.0000 ZERR 4.00 0.00070 0.00060 0.00060 0.0000 0.0017 0.0000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O Si K ER UNIT 156 380 16 8 32 4 8 TEMP -73.150 SIZE 0.20 0.53 0.677 L.S. 80 ACTA CONF BOND FMAP 2 PLAN 5 LIST 0 SADI C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C1 SIMU RIGU OMIT 8 2 6 OMIT 10 0 14 OMIT 11 1 10 OMIT 9 1 6 OMIT 9 5 6 OMIT 10 0 16 OMIT 11 1 14 OMIT 10 4 10 OMIT 11 1 16 OMIT 10 4 15 OMIT 10 6 15 OMIT 4 4 2 OMIT 7 3 4 OMIT 11 5 14 OMIT 9 5 16 OMIT 12 0 14 OMIT 12 0 12 OMIT 2 4 2 OMIT 11 1 8 OMIT 10 4 16 OMIT 8 6 15 OMIT 8 10 16 OMIT 5 1 2 OMIT 9 5 9 OMIT 12 4 14 OMIT 9 9 14 OMIT 9 9 12 OMIT 8 4 10 OMIT 7 1 7 OMIT 8 10 14 OMIT 9 1 17 OMIT 8 0 4 OMIT 7 9 16 OMIT 7 5 14 OMIT 8 10 13 OMIT 8 4 11 OMIT 9 9 10 OMIT 3 1 1 OMIT 10 0 6 OMIT 9 3 5 OMIT 9 1 15 OMIT 8 10 9 OMIT 8 0 12 OMIT 8 4 16 OMIT 8 4 12 OMIT 9 1 5 OMIT 6 10 16 OMIT 11 3 9 OMIT 3 3 3 OMIT 12 0 10 WGHT 0.082700 27.368996 FVAR 0.04891 ER1 7 0.500000 0.286209 0.250000 10.50000 0.02932 0.01535 = 0.02986 0.00000 0.00902 0.00000 ER2 7 0.500000 0.497865 0.250000 10.50000 0.02196 0.01560 = 0.03230 0.00000 0.00971 0.00000 K1 6 0.500000 0.077391 0.250000 10.50000 0.05557 0.02233 = 0.03946 0.00000 0.00636 0.00000 SI1 5 0.413064 0.187997 0.079843 11.00000 0.03482 0.03289 = 0.03217 0.00255 0.00565 -0.00842 SI2 5 0.563020 0.193928 0.096384 11.00000 0.03909 0.02776 = 0.03867 -0.00269 0.01730 0.00212 SI3 5 0.613263 0.616327 0.230054 11.00000 0.04004 0.03561 = 0.03708 0.00040 0.01632 -0.01704 SI4 5 0.655676 0.563009 0.405933 11.00000 0.02687 0.03547 = 0.03835 0.00126 0.00630 -0.00473 O1 4 0.591701 -0.030352 0.284505 11.00000 0.07510 0.04577 = 0.05374 -0.00686 0.00300 0.01831 N1 3 0.496336 0.208457 0.139783 11.00000 0.02997 0.02260 = 0.02852 -0.00128 0.00722 -0.00247 N2 3 0.595789 0.566186 0.306629 11.00000 0.02667 0.02236 = 0.03644 0.00131 0.01353 -0.00298 PART -1 C1 1 0.486355 0.393210 0.147463 10.50000 0.03722 0.01933 = 0.02399 -0.00298 0.00407 -0.00046 AFIX 43 H1A 2 0.476965 0.399001 0.088055 10.50000 -1.20000 AFIX 0 C2 1 0.426914 0.387522 0.175790 10.50000 0.02983 0.01970 = 0.03180 -0.00270 0.00279 -0.00258 AFIX 43 H2A 2 0.383383 0.382391 0.132656 10.50000 -1.20000 AFIX 0 C3 1 0.423890 0.388479 0.259696 10.50000 0.02475 0.02660 = 0.03155 0.00293 0.00771 -0.00129 AFIX 43 H3A 2 0.378514 0.384853 0.265711 10.50000 -1.20000 AFIX 0 C4 1 0.479962 0.394168 0.336410 10.50000 0.03670 0.01849 = 0.03426 -0.00267 0.01557 -0.00239 AFIX 43 H4A 2 0.466936 0.400751 0.386386 10.50000 -1.20000 AFIX 0 C5 1 0.553355 0.391286 0.348239 10.50000 0.03720 0.01557 = 0.03648 -0.00457 0.01118 -0.00312 AFIX 43 H5A 2 0.582879 0.392848 0.405278 10.50000 -1.20000 AFIX 0 C6 1 0.587594 0.386359 0.284940 10.50000 0.02433 0.02127 = 0.03892 -0.00125 0.00450 0.00179 AFIX 43 H6A 2 0.636647 0.378722 0.304939 10.50000 -1.20000 AFIX 0 C7 1 0.557530 0.391444 0.195443 10.50000 0.03294 0.02502 = 0.03656 -0.00242 0.01526 -0.00219 AFIX 43 H7A 2 0.589726 0.393984 0.163872 10.50000 -1.20000 AFIX 0 PART 0 C8 1 0.353986 0.190168 0.148346 11.00000 0.03663 0.06905 = 0.04725 0.00888 0.01003 -0.00936 AFIX 33 H8A 2 0.311367 0.163067 0.120908 11.00000 -1.50000 H8B 2 0.341706 0.239677 0.156260 11.00000 -1.50000 H8C 2 0.378056 0.168892 0.203615 11.00000 -1.50000 AFIX 0 C9 1 0.370534 0.249249 -0.010600 11.00000 0.05004 0.05462 = 0.04002 0.00997 0.00111 -0.00121 AFIX 33 H9A 2 0.345160 0.221049 -0.060289 11.00000 -1.50000 H9B 2 0.406402 0.277948 -0.024216 11.00000 -1.50000 H9C 2 0.337797 0.280785 0.005404 11.00000 -1.50000 AFIX 0 C10 1 0.406152 0.095544 0.033102 11.00000 0.06810 0.04174 = 0.05136 -0.00832 0.00887 -0.02041 AFIX 33 H10A 2 0.369842 0.094967 -0.022105 11.00000 -1.50000 H10B 2 0.393963 0.061618 0.071287 11.00000 -1.50000 H10C 2 0.451062 0.082031 0.025850 11.00000 -1.50000 AFIX 0 C11 1 0.537447 0.209866 -0.021629 11.00000 0.06475 0.06556 = 0.04240 0.00064 0.02364 0.00113 AFIX 33 H11A 2 0.520337 0.258814 -0.034093 11.00000 -1.50000 H11B 2 0.500501 0.176339 -0.050761 11.00000 -1.50000 H11C 2 0.578223 0.202723 -0.041320 11.00000 -1.50000 AFIX 0 C12 1 0.641317 0.251088 0.138898 11.00000 0.04003 0.04707 = 0.06239 -0.00939 0.02505 -0.00313 AFIX 33 H12A 2 0.658943 0.246003 0.200685 11.00000 -1.50000 H12B 2 0.628733 0.300976 0.124348 11.00000 -1.50000 H12C 2 0.677623 0.236470 0.114111 11.00000 -1.50000 AFIX 0 C13 1 0.595755 0.099324 0.113448 11.00000 0.06111 0.03547 = 0.06424 -0.00324 0.02782 0.01100 AFIX 33 H13A 2 0.610098 0.088237 0.174155 11.00000 -1.50000 H13B 2 0.635812 0.093801 0.092032 11.00000 -1.50000 H13C 2 0.558386 0.066714 0.083035 11.00000 -1.50000 AFIX 0 C14 1 0.549291 0.593201 0.125178 11.00000 0.04708 0.04081 = 0.03682 0.00089 0.01943 -0.00738 AFIX 33 H14A 2 0.560175 0.620487 0.080380 11.00000 -1.50000 H14B 2 0.501919 0.604887 0.125718 11.00000 -1.50000 H14C 2 0.552232 0.542099 0.114435 11.00000 -1.50000 AFIX 0 C15 1 0.603914 0.713959 0.244231 11.00000 0.15312 0.03316 = 0.05851 0.00162 0.02748 -0.02359 AFIX 33 H15A 2 0.643797 0.739024 0.235164 11.00000 -1.50000 H15B 2 0.602470 0.723327 0.301857 11.00000 -1.50000 H15C 2 0.560557 0.730880 0.203130 11.00000 -1.50000 AFIX 0 C16 1 0.702049 0.600297 0.217479 11.00000 0.04525 0.13476 = 0.07167 0.00349 0.03122 -0.02577 AFIX 33 H16A 2 0.724111 0.646134 0.213180 11.00000 -1.50000 H16B 2 0.697012 0.572398 0.165939 11.00000 -1.50000 H16C 2 0.731219 0.574019 0.266776 11.00000 -1.50000 AFIX 0 C17 1 0.700324 0.649701 0.441710 11.00000 0.06084 0.05234 = 0.05160 -0.00463 0.00976 -0.02495 AFIX 33 H17A 2 0.665285 0.686570 0.439564 11.00000 -1.50000 H17B 2 0.727793 0.663145 0.404386 11.00000 -1.50000 H17C 2 0.731367 0.644961 0.499988 11.00000 -1.50000 AFIX 0 C18 1 0.727595 0.497414 0.413256 11.00000 0.03366 0.06463 = 0.07508 -0.00860 -0.00555 0.00676 AFIX 33 H18A 2 0.749909 0.508321 0.369772 11.00000 -1.50000 H18B 2 0.708158 0.449100 0.404332 11.00000 -1.50000 H18C 2 0.762329 0.500517 0.469493 11.00000 -1.50000 AFIX 0 C19 1 0.617816 0.538115 0.491919 11.00000 0.05654 0.06591 = 0.04087 0.00829 0.01216 -0.01743 AFIX 33 H19A 2 0.579498 0.570731 0.490948 11.00000 -1.50000 H19B 2 0.654102 0.541378 0.546986 11.00000 -1.50000 H19C 2 0.599993 0.489180 0.482915 11.00000 -1.50000 AFIX 0 C20 1 0.581682 -0.081662 0.218227 11.00000 0.09232 0.04317 = 0.06585 -0.00994 0.01937 0.00125 AFIX 23 H20A 2 0.551702 -0.062090 0.163718 11.00000 -1.20000 H20B 2 0.559675 -0.125467 0.231602 11.00000 -1.20000 AFIX 0 C21 1 0.652681 -0.096877 0.213967 11.00000 0.09259 0.04759 = 0.07079 -0.00721 0.03112 -0.00713 AFIX 23 H21A 2 0.668037 -0.060100 0.180666 11.00000 -1.20000 H21B 2 0.654885 -0.144305 0.188697 11.00000 -1.20000 AFIX 0 C22 1 0.696001 -0.094882 0.305545 11.00000 0.07659 0.08151 = 0.08514 -0.02408 0.00044 0.02349 AFIX 23 H22A 2 0.744198 -0.078701 0.311813 11.00000 -1.20000 H22B 2 0.697905 -0.142385 0.332198 11.00000 -1.20000 AFIX 0 C23 1 0.658140 -0.042074 0.343906 11.00000 0.08261 0.09241 = 0.06084 -0.01841 -0.01211 0.03354 AFIX 23 H23A 2 0.653072 -0.061121 0.397434 11.00000 -1.20000 H23B 2 0.684596 0.003218 0.356490 11.00000 -1.20000 AFIX 0 HKLF 4 REM mm422 in C2/c REM R1 = 0.0384 for 6576 Fo > 4sig(Fo) and 0.0438 for all 7321 data REM 286 parameters refined using 657 restraints END WGHT 0.0787 30.5382 REM Highest difference peak 1.380, deepest hole -2.107, 1-sigma level 0.172 Q1 1 0.4864 0.2865 0.2948 11.00000 0.05 1.38 Q2 1 0.5125 0.5054 0.2035 11.00000 0.05 1.38 Q3 1 0.5562 0.5008 0.2539 11.00000 0.05 1.28 Q4 1 0.4477 0.2776 0.2398 11.00000 0.05 1.13 Q5 1 0.5448 0.5019 0.3227 11.00000 0.05 1.07 ; _shelx_res_checksum 89475