data_shelx _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 N10 Ni O10 W Y' _chemical_formula_weight 988.09 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' 'Ni' 'Ni' 0.3393 1.1124 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 '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/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9506(5) _cell_length_b 13.9237(6) _cell_length_c 27.4023(15) _cell_angle_alpha 90 _cell_angle_beta 93.252(4) _cell_angle_gamma 90 _cell_volume 3409.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 57563 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 32.63 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_F_000 1940 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_absorpt_coefficient_mu 5.669 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1450 _exptl_absorpt_correction_T_max 0.3411 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31808 _diffrn_reflns_av_unetI/netI 0.0641 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.670 _diffrn_reflns_theta_max 27.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 8193 _reflns_number_gt 6327 _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 'X-Area' _computing_cell_refinement 'X-Area' _computing_data_reduction 'X-Area' _computing_structure_solution 'SHELXS-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0482P)^2^+20.7845P] 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 SHELXL _refine_ls_extinction_coef 0.00070(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8193 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 C1 C 0.6513(14) 0.3353(11) 0.0222(4) 0.075(4) Uani 1 1 d . . . . . H1A H 0.6016 0.2886 0.0012 0.112 Uiso 1 1 calc R U . . . H1B H 0.6652 0.3935 0.0043 0.112 Uiso 1 1 calc R U . . . H1C H 0.7469 0.3107 0.0340 0.112 Uiso 1 1 calc R U . . . O9 O 0.2993(7) 0.2636(4) 0.2275(2) 0.0416(13) Uani 1 1 d . . . . . C2 C 0.6192(10) 0.4219(7) 0.0971(3) 0.0410(18) Uani 1 1 d . . . . . C3 C 0.7435(12) 0.4792(8) 0.0904(4) 0.056(3) Uani 1 1 d . . . . . H3 H 0.7939 0.4755 0.0618 0.067 Uiso 1 1 calc R U . . . C4 C 0.7900(12) 0.5412(9) 0.1269(4) 0.063(3) Uani 1 1 d . . . . . H4 H 0.8723 0.5805 0.1227 0.075 Uiso 1 1 calc R U . . . C5 C 0.7171(12) 0.5464(8) 0.1696(4) 0.060(3) Uani 1 1 d . . . . . H5 H 0.7527 0.5875 0.1944 0.072 Uiso 1 1 calc R U . . . C6 C 0.5901(11) 0.4908(6) 0.1762(3) 0.0437(19) Uani 1 1 d . . . . . C7 C 0.5398(9) 0.4257(6) 0.1394(3) 0.0375(17) Uani 1 1 d . . . . . C8 C 0.5170(12) 0.5032(7) 0.2222(3) 0.049(2) Uani 1 1 d . . . . . H8 H 0.5704 0.5382 0.2463 0.059 Uiso 1 1 calc R U . . . C9 C 0.3383(14) 0.5056(9) 0.2810(4) 0.066(3) Uani 1 1 d . . . . . H9A H 0.4159 0.4914 0.3062 0.079 Uiso 1 1 calc R U . . . H9B H 0.3268 0.5748 0.2797 0.079 Uiso 1 1 calc R U . . . C10 C 0.1992(17) 0.4641(10) 0.2956(4) 0.079(4) Uani 1 1 d . . . . . H10A H 0.1778 0.4907 0.3272 0.095 Uiso 1 1 calc R U . . . H10B H 0.2142 0.3956 0.3000 0.095 Uiso 1 1 calc R U . . . C11 C 0.0629(15) 0.4786(9) 0.2613(4) 0.067(3) Uani 1 1 d . . . . . H11A H -0.0263 0.4688 0.2792 0.080 Uiso 1 1 calc R U . . . H11B H 0.0616 0.5443 0.2496 0.080 Uiso 1 1 calc R U . . . C12 C -0.0583(11) 0.3655(7) 0.2093(3) 0.050(2) Uani 1 1 d . . . . . H12 H -0.1383 0.3766 0.2288 0.060 Uiso 1 1 calc R U . . . C13 C -0.0822(10) 0.2951(7) 0.1704(3) 0.0430(19) Uani 1 1 d . . . . . C14 C -0.2203(10) 0.2473(8) 0.1678(3) 0.050(2) Uani 1 1 d . . . . . H14 H -0.2907 0.2625 0.1903 0.060 Uiso 1 1 calc R U . . . C15 C -0.2543(12) 0.1786(9) 0.1331(4) 0.062(3) Uani 1 1 d . . . . . H15 H -0.3466 0.1478 0.1325 0.075 Uiso 1 1 calc R U . . . C16 C -0.1518(11) 0.1546(8) 0.0988(4) 0.054(2) Uani 1 1 d . . . . . H16 H -0.1744 0.1084 0.0750 0.065 Uiso 1 1 calc R U . . . C17 C -0.0152(10) 0.2015(7) 0.1010(3) 0.045(2) Uani 1 1 d . . . . . C18 C 0.0215(9) 0.2730(6) 0.1360(3) 0.0387(18) Uani 1 1 d . . . . . C19 C 0.0833(15) 0.0967(8) 0.0409(4) 0.069(3) Uani 1 1 d . . . . . H19A H 0.1657 0.0915 0.0201 0.104 Uiso 1 1 calc R U . . . H19B H 0.0837 0.0426 0.0627 0.104 Uiso 1 1 calc R U . . . H19C H -0.0090 0.0977 0.0213 0.104 Uiso 1 1 calc R U . . . C20 C 0.2043(9) 0.6086(6) 0.1383(3) 0.0376(17) Uani 1 1 d . . . . . C21 C 0.0779(10) 0.6757(7) 0.0618(3) 0.0437(19) Uani 1 1 d . . . . . C27 C 0.3348(10) 0.7501(7) 0.1865(3) 0.0423(19) Uani 1 1 d . . . . . C22 C 0.0311(9) 0.7388(6) 0.1772(3) 0.0369(16) Uani 1 1 d . . . . . N10 N 0.4170(10) 0.7475(7) 0.2192(3) 0.057(2) Uani 1 1 d . . . . . C23 C -0.0152(11) 0.8373(7) 0.0998(3) 0.046(2) Uani 1 1 d . . . . . C24 C 0.2342(12) 0.9028(6) 0.1477(3) 0.047(2) Uani 1 1 d . . . . . C25 C 0.2342(12) 0.8435(6) 0.0564(3) 0.044(2) Uani 1 1 d . . . . . C26 C 0.4067(10) 0.7223(8) 0.0966(3) 0.051(2) Uani 1 1 d . . . . . N1 N 0.3898(9) 0.4723(5) 0.2334(2) 0.0433(17) Uani 1 1 d . . . . . N2 N 0.0596(8) 0.4133(6) 0.2196(2) 0.0417(16) Uani 1 1 d . . . . . N3 N 0.2159(9) 0.5293(5) 0.1475(3) 0.0453(18) Uani 1 1 d . . . . . N4 N 0.0186(10) 0.6335(7) 0.0314(3) 0.054(2) Uani 1 1 d . . . . . N5 N -0.0541(9) 0.7280(6) 0.2070(3) 0.0492(18) Uani 1 1 d . . . . . N6 N -0.1229(11) 0.8776(7) 0.0871(3) 0.065(2) Uani 1 1 d . . . . . N7 N 0.2645(14) 0.9791(6) 0.1584(4) 0.073(3) Uani 1 1 d . . . . . N8 N 0.2621(12) 0.8872(7) 0.0233(3) 0.065(3) Uani 1 1 d . . . . . N9 N 0.5207(11) 0.7109(9) 0.0824(3) 0.078(3) Uani 1 1 d . . . . . Ni1 Ni 0.25241(12) 0.39916(8) 0.18551(4) 0.0357(2) Uani 1 1 d . . . . . O1 O 0.5604(7) 0.3550(5) 0.0635(2) 0.0477(15) Uani 1 1 d . . . . . O2 O 0.4235(7) 0.3679(4) 0.1419(2) 0.0397(13) Uani 1 1 d . . . . . O3 O 0.1533(6) 0.3156(4) 0.1331(2) 0.0378(12) Uani 1 1 d . . . . . O4 O 0.0974(7) 0.1845(5) 0.0691(2) 0.0470(15) Uani 1 1 d . . . . . O5 O 0.2114(9) 0.4208(5) 0.0488(2) 0.0596(19) Uani 1 1 d . . . . . O6 O 0.2886(7) 0.2709(5) -0.0078(2) 0.0523(16) Uani 1 1 d . . . . . O7 O 0.4548(9) 0.1382(5) 0.0487(3) 0.063(2) Uani 1 1 d . . . . . O8 O 0.3660(7) 0.1637(4) 0.1444(2) 0.0428(14) Uani 1 1 d . . . . . O10 O 0.5880(13) 0.9621(10) 0.0700(8) 0.200(9) Uani 1 1 d . . . . . W1 W 0.18773(4) 0.75975(2) 0.12089(2) 0.03246(11) Uani 1 1 d . . . . . Y1 Y 0.32800(9) 0.27482(6) 0.08002(3) 0.03573(18) Uani 1 1 d . . . . . 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 C1 0.061(7) 0.109(10) 0.057(6) -0.021(7) 0.025(5) -0.004(7) O9 0.048(3) 0.042(3) 0.035(3) 0.002(2) 0.000(2) 0.002(3) C2 0.039(5) 0.044(5) 0.040(4) -0.004(4) 0.000(3) -0.002(4) C3 0.047(6) 0.067(7) 0.055(5) 0.001(5) 0.012(4) -0.011(5) C4 0.043(6) 0.069(7) 0.076(7) 0.000(6) 0.003(5) -0.021(5) C5 0.048(6) 0.063(7) 0.068(7) -0.011(5) -0.008(5) -0.012(5) C6 0.045(5) 0.040(5) 0.045(5) -0.001(4) -0.006(4) -0.005(4) C7 0.036(4) 0.038(4) 0.038(4) 0.001(3) 0.001(3) -0.003(3) C8 0.055(6) 0.049(5) 0.042(5) -0.008(4) -0.006(4) -0.006(4) C9 0.082(8) 0.072(7) 0.043(5) -0.017(5) 0.011(5) -0.022(6) C10 0.113(11) 0.077(8) 0.050(6) -0.018(6) 0.017(7) -0.022(8) C11 0.084(9) 0.062(7) 0.056(6) -0.014(5) 0.015(6) 0.005(6) C12 0.050(6) 0.057(6) 0.044(5) 0.008(4) 0.011(4) 0.017(5) C13 0.042(5) 0.051(5) 0.036(4) 0.006(4) 0.004(3) -0.001(4) C14 0.034(4) 0.066(6) 0.050(5) 0.010(5) 0.005(4) 0.005(4) C15 0.044(5) 0.084(8) 0.058(6) 0.019(6) -0.007(5) -0.021(5) C16 0.050(6) 0.061(6) 0.049(5) 0.000(5) -0.009(4) -0.018(5) C17 0.043(5) 0.051(5) 0.041(4) 0.001(4) -0.005(4) -0.004(4) C18 0.037(4) 0.044(5) 0.035(4) 0.012(3) -0.001(3) 0.000(3) C19 0.083(8) 0.059(7) 0.065(7) -0.027(6) 0.001(6) -0.014(6) C20 0.035(4) 0.038(4) 0.040(4) -0.003(3) 0.001(3) -0.006(3) C21 0.042(5) 0.048(5) 0.039(4) -0.005(4) -0.006(4) 0.000(4) C27 0.041(4) 0.053(5) 0.031(4) -0.002(4) -0.010(3) 0.002(4) C22 0.037(4) 0.041(4) 0.034(4) 0.001(3) 0.013(3) -0.004(3) N10 0.056(5) 0.066(6) 0.049(4) -0.006(4) -0.003(4) 0.003(4) C23 0.047(5) 0.047(5) 0.043(5) 0.001(4) -0.001(4) 0.005(4) C24 0.071(7) 0.032(4) 0.038(4) 0.002(3) 0.001(4) -0.008(4) C25 0.064(6) 0.034(4) 0.036(4) 0.006(3) 0.009(4) -0.004(4) C26 0.033(4) 0.080(7) 0.043(5) 0.010(5) 0.009(3) 0.002(4) N1 0.051(5) 0.045(4) 0.034(3) -0.006(3) 0.000(3) -0.003(3) N2 0.042(4) 0.046(4) 0.038(4) 0.004(3) 0.007(3) 0.006(3) N3 0.059(5) 0.039(4) 0.038(4) -0.001(3) 0.004(3) 0.005(3) N4 0.056(5) 0.062(5) 0.043(4) -0.003(4) -0.006(4) -0.001(4) N5 0.054(5) 0.046(4) 0.048(4) -0.003(3) 0.008(3) -0.001(4) N6 0.062(6) 0.072(6) 0.062(5) 0.005(5) 0.004(4) 0.013(5) N7 0.108(9) 0.037(5) 0.074(6) -0.011(4) 0.011(6) -0.007(5) N8 0.086(7) 0.065(6) 0.045(4) 0.010(4) 0.009(4) -0.010(5) N9 0.052(5) 0.124(10) 0.058(5) 0.020(6) 0.013(4) 0.018(6) Ni1 0.0395(6) 0.0349(5) 0.0329(5) -0.0016(4) 0.0022(4) -0.0003(4) O1 0.039(3) 0.062(4) 0.043(3) -0.007(3) 0.013(3) -0.004(3) O2 0.039(3) 0.045(3) 0.035(3) -0.005(2) 0.003(2) -0.004(3) O3 0.031(3) 0.045(3) 0.038(3) -0.006(2) 0.004(2) 0.000(2) O4 0.052(4) 0.048(4) 0.040(3) -0.008(3) 0.002(3) -0.012(3) O5 0.078(5) 0.052(4) 0.048(4) 0.006(3) 0.002(3) 0.013(4) O6 0.048(4) 0.074(5) 0.035(3) -0.004(3) 0.002(3) 0.000(3) O7 0.081(5) 0.056(4) 0.052(4) -0.004(3) 0.012(4) 0.018(4) O8 0.051(4) 0.038(3) 0.039(3) 0.001(2) -0.001(3) 0.000(3) O10 0.066(8) 0.091(9) 0.43(3) 0.087(13) -0.044(12) -0.009(7) W1 0.03442(17) 0.03293(17) 0.02986(16) 0.00010(12) 0.00032(10) -0.00096(13) Y1 0.0370(4) 0.0383(4) 0.0318(3) -0.0022(3) 0.0009(3) -0.0017(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 C1 O1 1.456(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? O9 Ni1 2.238(6) . ? C2 C3 1.390(13) . ? C2 O1 1.392(10) . ? C2 C7 1.393(12) . ? C3 C4 1.367(15) . ? C3 H3 0.9300 . ? C4 C5 1.375(15) . ? C4 H4 0.9300 . ? C5 C6 1.395(13) . ? C5 H5 0.9300 . ? C6 C7 1.411(12) . ? C6 C8 1.463(13) . ? C7 O2 1.320(10) . ? C8 N1 1.271(12) . ? C8 H8 0.9300 . ? C9 C10 1.449(17) . ? C9 N1 1.482(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.509(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.460(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.266(12) . ? C12 C13 1.455(13) . ? C12 H12 0.9300 . ? C13 C18 1.395(12) . ? C13 C14 1.402(13) . ? C14 C15 1.370(15) . ? C14 H14 0.9300 . ? C15 C16 1.392(16) . ? C15 H15 0.9300 . ? C16 C17 1.385(13) . ? C16 H16 0.9300 . ? C17 O4 1.393(11) . ? C17 C18 1.407(13) . ? C18 O3 1.327(10) . ? C19 O4 1.448(11) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N3 1.137(11) . ? C20 W1 2.160(9) . ? C21 N4 1.128(11) . ? C21 W1 2.185(9) . ? C27 N10 1.127(11) . ? C27 W1 2.171(7) . ? C22 N5 1.157(11) . ? C22 W1 2.164(7) . ? C23 N6 1.152(13) . ? C23 W1 2.163(10) . ? C24 N7 1.131(12) . ? C24 W1 2.156(9) . ? C25 N8 1.132(11) . ? C25 W1 2.178(8) . ? C26 N9 1.123(12) . ? C26 W1 2.169(9) . ? N1 Ni1 2.023(7) . ? N2 Ni1 2.018(7) . ? N3 Ni1 2.106(8) . ? Ni1 O3 2.014(6) . ? Ni1 O2 2.043(6) . ? Ni1 Y1 3.4690(13) . ? O1 Y1 2.426(6) . ? O2 Y1 2.263(6) . ? O3 Y1 2.269(5) . ? O4 Y1 2.421(6) . ? O5 Y1 2.419(7) . ? O6 Y1 2.412(6) . ? O7 Y1 2.398(7) . ? O8 Y1 2.357(6) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.9(8) . . ? C3 C2 C7 122.5(8) . . ? O1 C2 C7 112.6(8) . . ? C4 C3 C2 118.7(9) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 121.0(10) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 120.7(10) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 119.6(9) . . ? C5 C6 C8 116.9(9) . . ? C7 C6 C8 123.5(8) . . ? O2 C7 C2 117.4(7) . . ? O2 C7 C6 125.1(8) . . ? C2 C7 C6 117.5(8) . . ? N1 C8 C6 128.2(9) . . ? N1 C8 H8 115.9 . . ? C6 C8 H8 115.9 . . ? C10 C9 N1 115.6(9) . . ? C10 C9 H9A 108.4 . . ? N1 C9 H9A 108.4 . . ? C10 C9 H9B 108.4 . . ? N1 C9 H9B 108.4 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 116.9(11) . . ? C9 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? C9 C10 H10B 108.1 . . ? C11 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? N2 C11 C10 112.6(10) . . ? N2 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? N2 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N2 C12 C13 127.1(9) . . ? N2 C12 H12 116.4 . . ? C13 C12 H12 116.4 . . ? C18 C13 C14 118.7(9) . . ? C18 C13 C12 124.6(9) . . ? C14 C13 C12 116.7(8) . . ? C15 C14 C13 121.8(9) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 120.6(9) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 118.1(10) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 O4 124.1(9) . . ? C16 C17 C18 122.4(9) . . ? O4 C17 C18 113.5(8) . . ? O3 C18 C13 124.7(8) . . ? O3 C18 C17 116.8(8) . . ? C13 C18 C17 118.5(8) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 W1 178.7(8) . . ? N4 C21 W1 178.5(9) . . ? N10 C27 W1 176.3(9) . . ? N5 C22 W1 179.1(8) . . ? N6 C23 W1 177.8(9) . . ? N7 C24 W1 174.4(9) . . ? N8 C25 W1 178.3(10) . . ? N9 C26 W1 173.8(11) . . ? C8 N1 C9 115.7(8) . . ? C8 N1 Ni1 122.2(6) . . ? C9 N1 Ni1 121.4(7) . . ? C12 N2 C11 118.8(8) . . ? C12 N2 Ni1 124.7(6) . . ? C11 N2 Ni1 116.3(7) . . ? C20 N3 Ni1 163.0(7) . . ? O3 Ni1 N2 91.9(3) . . ? O3 Ni1 N1 168.7(3) . . ? N2 Ni1 N1 98.9(3) . . ? O3 Ni1 O2 77.0(2) . . ? N2 Ni1 O2 168.8(3) . . ? N1 Ni1 O2 92.2(3) . . ? O3 Ni1 N3 95.4(3) . . ? N2 Ni1 N3 91.8(3) . . ? N1 Ni1 N3 87.7(3) . . ? O2 Ni1 N3 89.7(3) . . ? O3 Ni1 O9 86.7(2) . . ? N2 Ni1 O9 89.1(3) . . ? N1 Ni1 O9 90.1(3) . . ? O2 Ni1 O9 89.8(2) . . ? N3 Ni1 O9 177.7(3) . . ? O3 Ni1 Y1 38.44(16) . . ? N2 Ni1 Y1 130.3(2) . . ? N1 Ni1 Y1 130.7(2) . . ? O2 Ni1 Y1 38.54(16) . . ? N3 Ni1 Y1 92.8(2) . . ? O9 Ni1 Y1 88.18(15) . . ? C2 O1 C1 115.7(8) . . ? C2 O1 Y1 118.7(5) . . ? C1 O1 Y1 125.5(7) . . ? C7 O2 Ni1 121.3(5) . . ? C7 O2 Y1 125.1(5) . . ? Ni1 O2 Y1 107.2(3) . . ? C18 O3 Ni1 125.0(5) . . ? C18 O3 Y1 125.0(5) . . ? Ni1 O3 Y1 108.1(2) . . ? C17 O4 C19 115.7(8) . . ? C17 O4 Y1 118.4(5) . . ? C19 O4 Y1 123.6(6) . . ? C24 W1 C20 144.7(3) . . ? C24 W1 C23 76.8(4) . . ? C20 W1 C23 126.2(3) . . ? C24 W1 C22 90.1(3) . . ? C20 W1 C22 75.5(3) . . ? C23 W1 C22 71.9(3) . . ? C24 W1 C26 99.6(4) . . ? C20 W1 C26 77.4(4) . . ? C23 W1 C26 142.9(4) . . ? C22 W1 C26 145.1(3) . . ? C24 W1 C27 71.3(4) . . ? C20 W1 C27 74.1(3) . . ? C23 W1 C27 135.4(3) . . ? C22 W1 C27 77.7(3) . . ? C26 W1 C27 73.9(3) . . ? C24 W1 C25 74.9(3) . . ? C20 W1 C25 133.4(3) . . ? C23 W1 C25 73.3(4) . . ? C22 W1 C25 144.4(3) . . ? C26 W1 C25 70.3(4) . . ? C27 W1 C25 124.8(4) . . ? C24 W1 C21 144.8(3) . . ? C20 W1 C21 70.3(3) . . ? C23 W1 C21 74.6(4) . . ? C22 W1 C21 100.0(3) . . ? C26 W1 C21 91.2(4) . . ? C27 W1 C21 143.7(4) . . ? C25 W1 C21 77.6(3) . . ? O2 Y1 O3 67.7(2) . . ? O2 Y1 O8 77.4(2) . . ? O3 Y1 O8 76.1(2) . . ? O2 Y1 O7 123.8(3) . . ? O3 Y1 O7 141.8(2) . . ? O8 Y1 O7 72.3(2) . . ? O2 Y1 O6 142.0(2) . . ? O3 Y1 O6 125.4(2) . . ? O8 Y1 O6 137.6(2) . . ? O7 Y1 O6 70.8(2) . . ? O2 Y1 O5 85.5(2) . . ? O3 Y1 O5 73.6(2) . . ? O8 Y1 O5 149.0(2) . . ? O7 Y1 O5 138.0(2) . . ? O6 Y1 O5 68.3(2) . . ? O2 Y1 O4 132.3(2) . . ? O3 Y1 O4 66.2(2) . . ? O8 Y1 O4 80.7(2) . . ? O7 Y1 O4 87.8(3) . . ? O6 Y1 O4 77.8(2) . . ? O5 Y1 O4 92.6(3) . . ? O2 Y1 O1 65.5(2) . . ? O3 Y1 O1 129.3(2) . . ? O8 Y1 O1 110.7(2) . . ? O7 Y1 O1 82.5(3) . . ? O6 Y1 O1 84.4(2) . . ? O5 Y1 O1 84.5(3) . . ? O4 Y1 O1 161.8(2) . . ? O2 Y1 Ni1 34.22(15) . . ? O3 Y1 Ni1 33.49(14) . . ? O8 Y1 Ni1 74.36(15) . . ? O7 Y1 Ni1 144.33(17) . . ? O6 Y1 Ni1 144.89(18) . . ? O5 Y1 Ni1 77.00(16) . . ? O4 Y1 Ni1 99.05(15) . . ? O1 Y1 Ni1 97.80(15) . . ? _refine_diff_density_max 2.373 _refine_diff_density_min -2.289 _refine_diff_density_rms 0.162 _shelxl_version_number 2014-3 _shelx_res_file ; TITL tr12 in P 21/c CELL 0.71073 8.9506 13.9237 27.4023 90.000 93.252 90.000 ZERR 4.00 0.0005 0.0006 0.0015 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N NI O W Y UNIT 108 128 40 4 40 4 4 MERG 2 OMIT -3.00 56.00 OMIT -4 3 1 OMIT 3 5 1 OMIT 1 0 0 OMIT 1 0 2 OMIT -10 1 1 OMIT -4 4 9 OMIT -3 5 3 OMIT -1 0 2 FMAP 2 PLAN 20 ACTA BOND $H L.S. 8 WGHT 0.048200 20.784500 EXTI 0.000704 FVAR 0.44532 C1 1 0.651274 0.335282 0.022211 11.00000 0.06061 0.10878 = 0.05739 -0.02056 0.02534 -0.00425 AFIX 33 H1A 2 0.601635 0.288624 0.001210 11.00000 -1.50000 H1B 2 0.665212 0.393496 0.004255 11.00000 -1.50000 H1C 2 0.746881 0.310720 0.033957 11.00000 -1.50000 AFIX 0 O9 5 0.299280 0.263598 0.227548 11.00000 0.04755 0.04161 = 0.03524 0.00249 -0.00042 0.00167 C2 1 0.619181 0.421861 0.097147 11.00000 0.03934 0.04374 = 0.03983 -0.00422 0.00020 -0.00178 C3 1 0.743479 0.479231 0.090446 11.00000 0.04707 0.06676 = 0.05523 0.00137 0.01235 -0.01124 AFIX 43 H3 2 0.793940 0.475488 0.061760 11.00000 -1.20000 AFIX 0 C4 1 0.790018 0.541241 0.126864 11.00000 0.04291 0.06856 = 0.07639 -0.00032 0.00271 -0.02107 AFIX 43 H4 2 0.872312 0.580544 0.122663 11.00000 -1.20000 AFIX 0 C5 1 0.717070 0.546439 0.169632 11.00000 0.04776 0.06260 = 0.06751 -0.01063 -0.00846 -0.01244 AFIX 43 H5 2 0.752714 0.587473 0.194417 11.00000 -1.20000 AFIX 0 C6 1 0.590135 0.490784 0.176220 11.00000 0.04486 0.04024 = 0.04490 -0.00086 -0.00583 -0.00466 C7 1 0.539758 0.425712 0.139372 11.00000 0.03644 0.03794 = 0.03781 0.00093 0.00061 -0.00322 C8 1 0.517021 0.503226 0.222231 11.00000 0.05482 0.04899 = 0.04209 -0.00836 -0.00560 -0.00611 AFIX 43 H8 2 0.570359 0.538203 0.246316 11.00000 -1.20000 AFIX 0 C9 1 0.338312 0.505569 0.281045 11.00000 0.08190 0.07247 = 0.04319 -0.01661 0.01109 -0.02184 AFIX 23 H9A 2 0.415855 0.491351 0.306175 11.00000 -1.20000 H9B 2 0.326827 0.574808 0.279706 11.00000 -1.20000 AFIX 0 C10 1 0.199174 0.464147 0.295583 11.00000 0.11320 0.07671 = 0.04994 -0.01802 0.01676 -0.02221 AFIX 23 H10A 2 0.177761 0.490687 0.327162 11.00000 -1.20000 H10B 2 0.214233 0.395633 0.299976 11.00000 -1.20000 AFIX 0 C11 1 0.062939 0.478615 0.261349 11.00000 0.08355 0.06167 = 0.05629 -0.01352 0.01538 0.00493 AFIX 23 H11A 2 -0.026311 0.468801 0.279216 11.00000 -1.20000 H11B 2 0.061632 0.544314 0.249559 11.00000 -1.20000 AFIX 0 C12 1 -0.058257 0.365504 0.209326 11.00000 0.05043 0.05678 = 0.04395 0.00823 0.01109 0.01690 AFIX 43 H12 2 -0.138335 0.376561 0.228778 11.00000 -1.20000 AFIX 0 C13 1 -0.082216 0.295119 0.170405 11.00000 0.04220 0.05099 = 0.03614 0.00597 0.00418 -0.00085 C14 1 -0.220290 0.247251 0.167845 11.00000 0.03401 0.06646 = 0.05017 0.01049 0.00501 0.00539 AFIX 43 H14 2 -0.290681 0.262490 0.190310 11.00000 -1.20000 AFIX 0 C15 1 -0.254264 0.178622 0.133128 11.00000 0.04395 0.08409 = 0.05777 0.01871 -0.00707 -0.02062 AFIX 43 H15 2 -0.346566 0.147844 0.132515 11.00000 -1.20000 AFIX 0 C16 1 -0.151795 0.154592 0.098778 11.00000 0.05021 0.06107 = 0.04932 0.00043 -0.00915 -0.01791 AFIX 43 H16 2 -0.174419 0.108362 0.075001 11.00000 -1.20000 AFIX 0 C17 1 -0.015191 0.201520 0.101036 11.00000 0.04256 0.05150 = 0.04053 0.00119 -0.00522 -0.00376 C18 1 0.021500 0.273012 0.135982 11.00000 0.03717 0.04372 = 0.03491 0.01203 -0.00119 0.00025 C19 1 0.083258 0.096671 0.040909 11.00000 0.08291 0.05945 = 0.06542 -0.02735 0.00054 -0.01428 AFIX 33 H19A 2 0.165651 0.091455 0.020112 11.00000 -1.50000 H19B 2 0.083723 0.042649 0.062685 11.00000 -1.50000 H19C 2 -0.008995 0.097671 0.021255 11.00000 -1.50000 AFIX 0 C20 1 0.204292 0.608645 0.138256 11.00000 0.03484 0.03814 = 0.03975 -0.00280 0.00064 -0.00594 C21 1 0.077873 0.675654 0.061831 11.00000 0.04230 0.04840 = 0.03950 -0.00478 -0.00638 0.00026 C27 1 0.334811 0.750144 0.186496 11.00000 0.04129 0.05289 = 0.03120 -0.00229 -0.01002 0.00248 C22 1 0.031093 0.738769 0.177248 11.00000 0.03673 0.04107 = 0.03414 0.00144 0.01335 -0.00390 N10 3 0.416970 0.747522 0.219201 11.00000 0.05558 0.06629 = 0.04878 -0.00642 -0.00337 0.00316 C23 1 -0.015202 0.837337 0.099836 11.00000 0.04711 0.04707 = 0.04279 0.00082 -0.00094 0.00539 C24 1 0.234175 0.902843 0.147668 11.00000 0.07084 0.03216 = 0.03833 0.00182 0.00139 -0.00839 C25 1 0.234240 0.843535 0.056379 11.00000 0.06379 0.03426 = 0.03589 0.00579 0.00876 -0.00442 C26 1 0.406739 0.722269 0.096599 11.00000 0.03269 0.07976 = 0.04258 0.00960 0.00868 0.00217 N1 3 0.389811 0.472270 0.233445 11.00000 0.05071 0.04472 = 0.03419 -0.00596 -0.00018 -0.00313 N2 3 0.059617 0.413316 0.219603 11.00000 0.04165 0.04647 = 0.03759 0.00394 0.00696 0.00634 N3 3 0.215891 0.529318 0.147526 11.00000 0.05850 0.03950 = 0.03809 -0.00111 0.00442 0.00493 N4 3 0.018576 0.633480 0.031395 11.00000 0.05642 0.06221 = 0.04290 -0.00264 -0.00570 -0.00055 N5 3 -0.054146 0.728040 0.206971 11.00000 0.05388 0.04584 = 0.04844 -0.00250 0.00790 -0.00120 N6 3 -0.122945 0.877642 0.087133 11.00000 0.06176 0.07207 = 0.06215 0.00545 0.00364 0.01285 N7 3 0.264513 0.979119 0.158351 11.00000 0.10806 0.03729 = 0.07373 -0.01138 0.01096 -0.00691 N8 3 0.262116 0.887225 0.023266 11.00000 0.08645 0.06495 = 0.04513 0.00989 0.00891 -0.00976 N9 3 0.520659 0.710888 0.082396 11.00000 0.05186 0.12397 = 0.05833 0.01989 0.01280 0.01825 NI1 4 0.252409 0.399162 0.185512 11.00000 0.03946 0.03487 = 0.03289 -0.00160 0.00220 -0.00033 O1 5 0.560385 0.355014 0.063492 11.00000 0.03941 0.06192 = 0.04307 -0.00681 0.01285 -0.00365 O2 5 0.423542 0.367887 0.141897 11.00000 0.03881 0.04508 = 0.03542 -0.00506 0.00308 -0.00447 O3 5 0.153280 0.315643 0.133142 11.00000 0.03055 0.04493 = 0.03814 -0.00646 0.00428 -0.00006 O4 5 0.097429 0.184518 0.069077 11.00000 0.05244 0.04848 = 0.04012 -0.00830 0.00220 -0.01228 O5 5 0.211355 0.420803 0.048759 11.00000 0.07829 0.05217 = 0.04811 0.00646 0.00167 0.01306 O6 5 0.288630 0.270907 -0.007788 11.00000 0.04776 0.07379 = 0.03538 -0.00366 0.00203 0.00049 O7 5 0.454821 0.138205 0.048722 11.00000 0.08083 0.05573 = 0.05193 -0.00355 0.01195 0.01818 O8 5 0.366009 0.163684 0.144430 11.00000 0.05123 0.03769 = 0.03899 0.00068 -0.00058 0.00014 O10 5 0.587958 0.962111 0.070035 11.00000 0.06598 0.09144 = 0.43498 0.08681 -0.04379 -0.00938 W1 6 0.187728 0.759752 0.120886 11.00000 0.03442 0.03293 = 0.02986 0.00010 0.00032 -0.00096 Y1 7 0.327996 0.274821 0.080016 11.00000 0.03701 0.03828 = 0.03177 -0.00218 0.00085 -0.00173 HKLF 4 REM tr12 in P 21/c REM R1 = 0.0597 for 6327 Fo > 4sig(Fo) and 0.0840 for all 8193 data REM 452 parameters refined using 0 restraints END WGHT 0.0481 20.7870 REM Highest difference peak 2.373, deepest hole -2.289, 1-sigma level 0.162 Q1 1 0.1996 0.7614 0.1602 11.00000 0.05 2.37 Q2 1 0.2941 0.7610 0.1308 11.00000 0.05 2.25 Q3 1 0.1688 0.7623 0.0840 11.00000 0.05 2.16 Q4 1 0.0817 0.7614 0.1112 11.00000 0.05 2.01 Q5 1 0.1958 0.6981 0.1251 11.00000 0.05 1.83 Q6 1 0.3073 0.2788 0.0419 11.00000 0.05 1.07 Q7 1 0.1919 0.8180 0.1218 11.00000 0.05 1.07 Q8 1 0.3341 0.1994 0.0859 11.00000 0.05 0.95 Q9 1 0.2778 0.4009 0.2270 11.00000 0.05 0.86 Q10 1 0.6411 0.9761 0.0379 11.00000 0.05 0.84 Q11 1 0.1504 0.4030 0.1782 11.00000 0.05 0.83 Q12 1 0.3369 0.2786 0.1184 11.00000 0.05 0.83 Q13 1 0.2437 0.8463 0.1265 11.00000 0.05 0.78 Q14 1 0.2322 0.4016 0.1453 11.00000 0.05 0.77 Q15 1 0.4313 0.2772 0.0883 11.00000 0.05 0.75 Q16 1 0.3263 0.7092 0.1102 11.00000 0.05 0.74 Q17 1 0.2823 0.7241 0.1624 11.00000 0.05 0.72 Q18 1 0.2211 0.2781 0.0709 11.00000 0.05 0.70 Q19 1 0.3576 0.4008 0.1925 11.00000 0.05 0.68 Q20 1 0.0985 0.7197 0.1590 11.00000 0.05 0.67 ; _shelx_res_checksum 53008 _shelx_hkl_file ; -13 0 1 -22.51 61.86 13 0 -1 8.01 60.37 -13 0 2 216.64 69.01 13 0 -2 115.85 59.08 -13 0 3 23.28 60.04 13 0 -3 -13.23 59.00 13 0 -4 64.46 55.70 -13 0 4 13.99 59.19 -13 0 5 -6.27 60.53 13 0 -5 -28.10 58.05 13 0 -6 -53.24 57.69 -13 0 6 7.02 60.78 -13 0 7 -26.64 58.43 13 0 -7 47.47 54.17 -13 0 8 137.65 51.72 13 0 -8 91.48 55.82 -13 0 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55.91 -13 2 -9 131.09 64.02 13 2 9 104.93 55.57 -13 -2 -9 -1.47 61.54 -13 -2 -10 52.50 60.90 13 2 10 83.15 67.73 13 -2 10 21.42 66.98 13 -2 10 -35.81 55.73 13 2 10 38.03 56.57 -13 2 -10 66.20 55.67 -13 -2 -10 79.94 67.53 -13 -2 -11 130.17 58.82 13 2 11 81.61 65.54 13 -2 11 -12.57 65.29 -13 2 -11 63.80 62.34 13 2 11 52.09 54.54 -13 -2 -11 97.52 60.84 -13 3 0 30.23 57.46 13 -3 0 -31.50 60.40 13 3 0 -19.11 56.76 -13 -3 0 13.04 86.85 -13 -3 0 2.18 52.93 -13 3 -1 31.81 56.19 13 -3 1 98.63 67.70 13 3 1 29.84 57.75 -13 -3 -1 13.12 86.92 -13 -3 -1 186.56 60.74 -13 -3 -2 37.17 62.39 -13 3 -2 137.32 67.54 13 -3 2 197.89 60.87 13 3 2 159.96 57.75 -13 -3 -2 165.79 86.44 -13 -3 -3 -1.02 62.79 -13 3 -3 64.51 57.23 13 -3 3 19.90 59.96 13 3 3 26.22 48.40 -13 -3 -3 73.42 74.54 -13 -3 -4 15.18 60.98 13 -3 4 20.18 105.52 13 3 4 -32.07 72.19 -13 3 -4 30.60 63.84 13 -3 4 102.72 66.09 13 3 4 18.88 56.84 -13 -3 -4 -6.91 72.73 -13 -3 -5 -39.55 59.30 13 3 5 76.61 77.07 13 -3 5 90.49 98.19 -13 3 -5 125.37 62.35 13 -3 5 53.75 59.29 13 3 5 50.68 56.17 -13 -3 -5 96.03 72.54 -13 -3 -6 58.70 62.69 13 3 6 124.86 76.04 13 -3 6 152.68 97.03 -13 3 -6 85.80 58.53 13 -3 6 168.32 58.51 13 3 6 148.53 56.58 -13 -3 -6 200.63 75.36 -13 -3 -7 -87.66 61.27 13 3 7 -22.11 72.91 13 -3 7 -29.70 80.09 -13 3 -7 -42.02 62.31 13 -3 7 83.19 57.52 13 3 7 17.88 56.96 -13 -3 -7 33.15 69.31 -13 -3 -8 88.96 68.16 13 3 8 30.59 65.50 13 -3 8 27.60 81.08 -13 3 -8 40.83 61.12 13 -3 8 -44.05 56.59 13 3 8 81.49 54.18 -13 -3 -8 47.17 71.35 -13 -3 -9 -6.36 60.04 13 3 9 62.65 62.93 -13 3 -9 28.69 61.37 13 -3 9 27.60 72.66 13 3 9 6.73 53.72 -13 -3 -9 10.34 64.13 13 3 10 46.35 67.46 -13 3 -10 65.24 60.50 13 -3 10 27.31 67.92 13 3 10 48.85 54.60 -13 -3 -10 52.63 62.87 13 -3 11 81.13 65.70 13 3 11 38.72 55.22 -13 -4 0 119.25 60.73 13 -4 0 27.93 69.95 13 4 0 101.95 57.19 -13 -4 0 182.08 88.95 -13 4 0 132.95 58.43 -13 -4 -1 -95.35 59.46 13 -4 1 47.02 60.46 13 4 1 33.26 55.95 -13 -4 -1 72.06 81.79 -13 4 -1 -14.33 56.99 -13 -4 -2 72.38 59.51 13 -4 2 29.53 60.69 13 4 2 97.11 56.06 -13 -4 -2 10.66 83.12 -13 4 -2 24.43 58.03 -13 -4 -3 -62.15 61.11 13 -4 3 -8.86 67.29 13 4 3 -25.03 49.01 -13 -4 -3 101.51 76.50 -13 4 -3 43.96 56.50 -13 4 -4 -87.29 56.86 -13 -4 -4 43.89 61.20 13 -4 4 43.08 60.20 13 4 4 19.12 55.75 -13 -4 -4 30.01 76.65 -13 4 -5 23.60 57.21 -13 -4 -5 54.39 59.95 13 4 5 32.59 77.32 13 -4 5 42.10 105.05 13 -4 5 22.79 60.43 13 4 5 82.17 55.87 -13 -4 -5 -46.19 74.63 -13 4 -6 11.52 54.93 13 4 6 63.29 75.14 -13 -4 -6 -6.30 59.06 13 -4 6 46.44 96.52 13 -4 6 77.74 57.97 13 4 6 32.43 54.81 -13 -4 -6 79.07 75.77 -13 4 -7 46.58 61.38 13 4 7 -50.38 75.26 -13 -4 -7 65.86 59.54 13 -4 7 1.79 86.03 13 -4 7 -19.24 57.37 13 4 7 -42.14 54.96 -13 -4 -7 55.48 67.60 -13 4 -8 -62.85 61.88 13 4 8 16.91 65.50 -13 -4 -8 37.40 60.65 13 -4 8 40.70 74.37 13 -4 8 23.95 56.78 13 4 8 -2.27 56.65 -13 -4 -8 88.63 67.24 -13 4 -9 30.84 59.65 13 4 9 -43.51 63.29 13 -4 9 40.27 77.91 13 -4 9 28.44 55.39 13 4 9 89.88 55.47 -13 -4 -9 52.42 65.71 13 4 10 90.46 56.71 -13 -5 0 87.24 59.35 13 -5 0 0.31 59.88 -13 5 0 23.03 63.43 13 5 0 38.10 55.39 -13 -5 0 37.63 80.66 -13 -5 -1 -56.75 59.09 13 -5 1 147.09 61.57 13 5 1 -13.28 55.97 -13 5 -1 -56.43 56.26 -13 -5 -1 24.55 81.43 -13 -5 -2 39.93 61.15 13 -5 2 18.40 70.02 13 5 2 110.02 56.71 -13 5 -2 75.72 65.78 -13 -5 -2 178.69 84.32 -13 -5 -3 -5.51 58.14 13 -5 3 120.29 61.32 13 5 3 139.87 48.24 -13 5 -3 116.38 63.46 -13 -5 -3 84.71 80.23 -13 -5 -4 -37.74 51.43 13 -5 4 58.53 59.77 13 5 4 51.93 53.47 -13 5 -4 74.19 62.93 -13 -5 -4 16.86 71.21 13 5 5 102.38 63.81 13 -5 5 9.39 120.02 -13 -5 -5 -28.19 59.95 13 -5 5 24.95 57.28 13 5 5 31.56 55.11 -13 5 -5 -17.68 55.46 -13 -5 -5 129.83 80.09 13 5 6 60.17 70.16 13 -5 6 82.66 105.68 -13 -5 -6 -18.40 60.45 13 -5 6 86.04 58.31 13 5 6 79.28 56.12 -13 5 -6 144.97 63.25 -13 -5 -6 180.49 73.71 13 5 7 149.65 67.46 -13 -5 -7 34.49 58.62 13 -5 7 25.50 91.10 13 -5 7 46.95 57.39 13 5 7 -47.56 53.62 -13 5 -7 78.31 61.47 -13 -5 -7 55.43 77.05 13 -5 8 30.73 77.20 -13 -5 -8 -49.85 60.35 13 -5 8 24.85 55.92 13 5 8 104.37 47.23 -13 -5 -8 142.44 71.02 -13 6 0 95.79 57.73 -13 -6 0 105.26 58.20 13 -6 0 78.38 62.23 13 6 0 183.67 55.09 -13 -6 0 110.02 85.87 -13 6 -1 -49.08 58.19 -13 -6 -1 34.54 58.97 13 -6 1 126.91 69.59 13 6 1 77.55 55.03 -13 -6 -1 -7.82 83.04 -13 6 -2 56.33 57.80 13 -6 2 -5.29 68.50 -13 -6 -2 30.45 51.70 13 6 2 96.22 56.12 -13 -6 -2 112.58 85.62 -13 6 -3 136.64 62.57 13 -6 3 13.48 67.48 -13 -6 -3 -0.40 50.66 13 6 3 167.91 47.62 -13 -6 -3 -32.66 82.81 -13 6 -4 109.68 64.29 -13 -6 -4 27.82 57.97 13 -6 4 46.88 59.67 13 6 4 1.57 53.71 -13 -6 -4 76.65 76.65 -13 -6 -5 183.50 58.99 13 -6 5 -35.15 58.78 13 6 5 -6.14 55.37 -13 -6 -5 118.28 75.34 13 -6 6 45.53 122.26 13 6 6 97.97 47.70 -13 -6 -6 19.48 75.41 13 -7 0 25.27 62.31 -13 -7 0 58.51 49.15 13 7 0 36.19 53.97 -13 -7 0 76.99 78.71 -13 7 0 44.35 64.58 13 -7 1 132.08 67.02 -13 -7 -1 96.47 49.27 13 7 1 40.93 53.65 -13 -7 -1 5.95 80.03 ; _shelx_hkl_checksum 4706 data_shelx _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 Eu N10 Ni O10 W' _chemical_formula_weight 1051.14 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' 'Eu' 'Eu' -0.1578 3.6682 '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' 'Ni' 'Ni' 0.3393 1.1124 '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' 'W' 'W' -0.8490 6.8722 '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/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9747(3) _cell_length_b 13.9587(4) _cell_length_c 27.4653(9) _cell_angle_alpha 90 _cell_angle_beta 93.266(3) _cell_angle_gamma 90 _cell_volume 3435.13(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 63827 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 33.80 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.032 _exptl_crystal_F_000 2036 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_absorpt_coefficient_mu 5.755 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2503 _exptl_absorpt_correction_T_max 0.4927 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31923 _diffrn_reflns_av_unetI/netI 0.0374 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.082 _diffrn_reflns_theta_max 27.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.916 _diffrn_measured_fraction_theta_full 0.937 _diffrn_reflns_Laue_measured_fraction_max 0.916 _diffrn_reflns_Laue_measured_fraction_full 0.937 _diffrn_reflns_point_group_measured_fraction_max 0.916 _diffrn_reflns_point_group_measured_fraction_full 0.937 _reflns_number_total 7591 _reflns_number_gt 6471 _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 'X-Area' _computing_cell_refinement 'X-Area' _computing_data_reduction 'X-Area' _computing_structure_solution 'SHELXS-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0302P)^2^+12.8800P] 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 SHELXL _refine_ls_extinction_coef 0.00100(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7591 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 C1 C 0.6566(9) 0.3398(7) 0.0240(3) 0.061(2) Uani 1 1 d . . . . . H1A H 0.6093 0.2931 0.0026 0.092 Uiso 1 1 calc R U . . . H1B H 0.6701 0.3983 0.0064 0.092 Uiso 1 1 calc R U . . . H1C H 0.7520 0.3160 0.0362 0.092 Uiso 1 1 calc R U . . . C2 C 0.6207(6) 0.4246(4) 0.0983(2) 0.0299(12) Uani 1 1 d . . . . . C3 C 0.7433(7) 0.4811(5) 0.0922(2) 0.0422(16) Uani 1 1 d . . . . . H3 H 0.7946 0.4778 0.0638 0.051 Uiso 1 1 calc R U . . . C4 C 0.7890(8) 0.5434(5) 0.1297(3) 0.0482(17) Uani 1 1 d . . . . . H4 H 0.8718 0.5824 0.1262 0.058 Uiso 1 1 calc R U . . . C5 C 0.7137(7) 0.5481(5) 0.1715(3) 0.0463(17) Uani 1 1 d . . . . . H5 H 0.7469 0.5895 0.1964 0.056 Uiso 1 1 calc R U . . . C6 C 0.5876(7) 0.4914(4) 0.1776(2) 0.0304(12) Uani 1 1 d . . . . . C7 C 0.5395(6) 0.4274(4) 0.14041(19) 0.0256(11) Uani 1 1 d . . . . . C8 C 0.5140(7) 0.5036(4) 0.2232(2) 0.0344(13) Uani 1 1 d . . . . . H8 H 0.5656 0.5396 0.2471 0.041 Uiso 1 1 calc R U . . . C9 C 0.3390(9) 0.5038(6) 0.2815(2) 0.057(2) Uani 1 1 d . . . . . H9A H 0.4163 0.4885 0.3064 0.068 Uiso 1 1 calc R U . . . H9B H 0.3289 0.5729 0.2806 0.068 Uiso 1 1 calc R U . . . C10 C 0.1987(10) 0.4632(6) 0.2962(3) 0.064(2) Uani 1 1 d . . . . . H10A H 0.1776 0.4901 0.3276 0.077 Uiso 1 1 calc R U . . . H10B H 0.2127 0.3948 0.3007 0.077 Uiso 1 1 calc R U . . . C11 C 0.0608(9) 0.4784(6) 0.2613(3) 0.055(2) Uani 1 1 d . . . . . H11A H -0.0289 0.4689 0.2788 0.065 Uiso 1 1 calc R U . . . H11B H 0.0601 0.5438 0.2492 0.065 Uiso 1 1 calc R U . . . C12 C -0.0596(7) 0.3655(5) 0.2092(2) 0.0347(14) Uani 1 1 d . . . . . H12 H -0.1400 0.3777 0.2282 0.042 Uiso 1 1 calc R U . . . C13 C -0.0838(6) 0.2952(5) 0.1702(2) 0.0320(12) Uani 1 1 d . . . . . C14 C -0.2231(7) 0.2477(5) 0.1679(2) 0.0428(16) Uani 1 1 d . . . . . H14 H -0.2928 0.2629 0.1905 0.051 Uiso 1 1 calc R U . . . C15 C -0.2568(7) 0.1803(6) 0.1336(2) 0.0457(17) Uani 1 1 d . . . . . H15 H -0.3493 0.1500 0.1328 0.055 Uiso 1 1 calc R U . . . C16 C -0.1544(7) 0.1560(5) 0.0994(2) 0.0424(16) Uani 1 1 d . . . . . H16 H -0.1777 0.1099 0.0757 0.051 Uiso 1 1 calc R U . . . C17 C -0.0186(6) 0.2012(5) 0.10128(19) 0.0313(12) Uani 1 1 d . . . . . C18 C 0.0196(6) 0.2720(4) 0.13617(18) 0.0253(11) Uani 1 1 d . . . . . C19 C 0.0804(8) 0.0941(5) 0.0417(3) 0.0511(18) Uani 1 1 d . . . . . H19A H 0.1624 0.0883 0.0209 0.077 Uiso 1 1 calc R U . . . H19B H 0.0812 0.0410 0.0639 0.077 Uiso 1 1 calc R U . . . H19C H -0.0118 0.0944 0.0222 0.077 Uiso 1 1 calc R U . . . C20 C 0.2050(6) 0.6069(4) 0.13913(18) 0.0255(11) Uani 1 1 d . . . . . C21 C 0.0806(6) 0.6744(4) 0.06238(19) 0.0290(12) Uani 1 1 d . . . . . C22 C 0.0313(6) 0.7387(4) 0.17778(18) 0.0256(11) Uani 1 1 d . . . . . C23 C -0.0153(7) 0.8352(4) 0.0996(2) 0.0329(13) Uani 1 1 d . . . . . C24 C 0.2367(7) 0.9007(4) 0.1474(2) 0.0340(13) Uani 1 1 d . . . . . C25 C 0.2343(7) 0.8409(4) 0.0576(2) 0.0348(13) Uani 1 1 d . . . . . C26 C 0.4033(7) 0.7208(5) 0.0971(2) 0.0384(15) Uani 1 1 d . . . . . C27 C 0.3358(6) 0.7486(4) 0.18642(19) 0.0286(12) Uani 1 1 d . . . . . Eu1 Eu 0.32908(3) 0.27322(2) 0.07947(2) 0.02326(8) Uani 1 1 d . . . . . N1 N 0.3891(6) 0.4714(4) 0.23411(16) 0.0315(11) Uani 1 1 d . . . . . N2 N 0.0604(5) 0.4120(4) 0.22003(16) 0.0307(11) Uani 1 1 d . . . . . N3 N 0.2128(6) 0.5276(4) 0.14833(16) 0.0314(11) Uani 1 1 d . . . . . N4 N 0.0199(6) 0.6307(4) 0.03181(18) 0.0410(13) Uani 1 1 d . . . . . N5 N -0.0516(6) 0.7279(4) 0.20751(18) 0.0375(12) Uani 1 1 d . . . . . N6 N -0.1220(7) 0.8752(5) 0.0872(2) 0.0544(16) Uani 1 1 d . . . . . N7 N 0.2653(8) 0.9765(4) 0.1588(2) 0.0549(16) Uani 1 1 d . . . . . N8 N 0.2661(8) 0.8850(5) 0.0246(2) 0.0561(17) Uani 1 1 d . . . . . N9 N 0.5173(7) 0.7066(6) 0.0825(2) 0.068(2) Uani 1 1 d . . . . . N10 N 0.4197(6) 0.7452(4) 0.2191(2) 0.0455(14) Uani 1 1 d . . . . . Ni1 Ni 0.25149(8) 0.39811(5) 0.18582(2) 0.02325(15) Uani 1 1 d . . . . . O1 O 0.5639(4) 0.3577(3) 0.06439(14) 0.0358(10) Uani 1 1 d . . . . . O2 O 0.4230(4) 0.3684(3) 0.14261(12) 0.0257(8) Uani 1 1 d . . . . . O3 O 0.1513(4) 0.3147(3) 0.13369(12) 0.0253(8) Uani 1 1 d . . . . . O4 O 0.0944(5) 0.1826(3) 0.06897(14) 0.0341(9) Uani 1 1 d . . . . . O5 O 0.2059(6) 0.4210(3) 0.04760(16) 0.0475(12) Uani 1 1 d . . . . . O6 O 0.2890(5) 0.2688(4) -0.00980(14) 0.0423(11) Uani 1 1 d . . . . . O7 O 0.4570(6) 0.1329(4) 0.04740(16) 0.0500(12) Uani 1 1 d . . . . . O8 O 0.3654(5) 0.1605(3) 0.14556(13) 0.0320(9) Uani 1 1 d . . . . . O9 O 0.2986(4) 0.2624(3) 0.22774(13) 0.0283(8) Uani 1 1 d . . . . . O10 O 0.5853(8) 0.9581(6) 0.0708(5) 0.167(5) Uani 1 1 d . . . . . W1 W 0.18731(2) 0.75761(2) 0.12135(2) 0.02060(7) Uani 1 1 d . . . . . 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 C1 0.051(5) 0.086(7) 0.048(4) -0.021(4) 0.025(3) -0.016(4) C2 0.022(3) 0.031(3) 0.036(3) -0.001(2) 0.003(2) -0.002(2) C3 0.028(3) 0.050(4) 0.050(4) 0.001(3) 0.011(3) -0.014(3) C4 0.031(4) 0.047(4) 0.067(4) -0.004(3) 0.009(3) -0.023(3) C5 0.032(4) 0.045(4) 0.060(4) -0.009(3) -0.007(3) -0.013(3) C6 0.028(3) 0.025(3) 0.038(3) -0.004(2) -0.001(2) -0.006(2) C7 0.019(3) 0.025(3) 0.033(3) 0.002(2) 0.0005(19) -0.002(2) C8 0.040(4) 0.025(3) 0.037(3) -0.006(2) -0.009(2) -0.003(3) C9 0.072(5) 0.066(5) 0.034(3) -0.020(3) 0.012(3) -0.013(4) C10 0.086(6) 0.060(5) 0.048(4) -0.017(4) 0.024(4) -0.014(5) C11 0.066(5) 0.051(5) 0.049(4) -0.011(3) 0.019(3) 0.017(4) C12 0.028(3) 0.039(4) 0.039(3) 0.011(2) 0.014(2) 0.008(3) C13 0.026(3) 0.037(4) 0.033(3) 0.009(2) 0.003(2) -0.001(3) C14 0.023(3) 0.063(5) 0.042(3) 0.018(3) 0.005(2) -0.001(3) C15 0.028(3) 0.060(5) 0.049(4) 0.015(3) -0.004(3) -0.013(3) C16 0.035(4) 0.051(4) 0.040(3) 0.007(3) -0.007(3) -0.016(3) C17 0.028(3) 0.034(3) 0.032(3) 0.003(2) -0.001(2) -0.004(3) C18 0.020(3) 0.028(3) 0.028(2) 0.007(2) -0.0012(19) -0.003(2) C19 0.052(4) 0.044(4) 0.057(4) -0.020(3) 0.003(3) -0.017(4) C20 0.025(3) 0.024(3) 0.028(2) 0.001(2) 0.002(2) 0.001(2) C21 0.032(3) 0.026(3) 0.029(3) 0.000(2) 0.001(2) -0.001(2) C22 0.023(3) 0.027(3) 0.027(2) -0.002(2) 0.005(2) -0.001(2) C23 0.030(3) 0.031(3) 0.038(3) 0.005(2) 0.001(2) 0.006(3) C24 0.049(4) 0.020(3) 0.033(3) -0.008(2) 0.001(2) -0.008(3) C25 0.044(4) 0.030(3) 0.031(3) 0.002(2) 0.001(2) -0.003(3) C26 0.028(3) 0.058(5) 0.030(3) 0.006(3) 0.012(2) 0.010(3) C27 0.025(3) 0.032(3) 0.029(3) -0.001(2) -0.006(2) -0.002(2) Eu1 0.02238(14) 0.02338(16) 0.02417(13) -0.00222(9) 0.00269(9) -0.00221(11) N1 0.036(3) 0.031(3) 0.027(2) -0.0058(18) 0.0033(19) -0.003(2) N2 0.032(3) 0.030(3) 0.031(2) 0.0012(19) 0.0088(19) 0.007(2) N3 0.035(3) 0.026(3) 0.034(2) -0.0019(19) 0.0042(19) 0.002(2) N4 0.037(3) 0.045(3) 0.040(3) -0.006(2) -0.005(2) -0.005(3) N5 0.036(3) 0.036(3) 0.041(3) -0.006(2) 0.009(2) -0.004(2) N6 0.041(3) 0.065(5) 0.057(4) 0.010(3) 0.001(3) 0.020(3) N7 0.075(5) 0.031(3) 0.059(4) -0.003(3) 0.001(3) -0.008(3) N8 0.082(5) 0.049(4) 0.037(3) 0.011(3) 0.008(3) -0.011(3) N9 0.044(4) 0.111(6) 0.050(4) 0.020(4) 0.015(3) 0.022(4) N10 0.043(3) 0.052(4) 0.040(3) -0.004(2) -0.006(2) -0.005(3) Ni1 0.0241(4) 0.0214(4) 0.0245(3) -0.0012(2) 0.0038(2) -0.0004(3) O1 0.029(2) 0.047(3) 0.032(2) -0.0088(18) 0.0107(16) -0.0068(19) O2 0.024(2) 0.025(2) 0.0288(18) -0.0042(14) 0.0047(14) -0.0044(16) O3 0.0197(18) 0.026(2) 0.0305(18) -0.0036(14) 0.0039(14) -0.0040(16) O4 0.033(2) 0.035(3) 0.035(2) -0.0080(17) 0.0001(16) -0.0090(19) O5 0.062(3) 0.038(3) 0.042(2) 0.0044(19) -0.002(2) 0.014(2) O6 0.037(2) 0.062(3) 0.028(2) 0.0016(19) 0.0028(17) -0.006(2) O7 0.063(3) 0.045(3) 0.043(2) -0.006(2) 0.010(2) 0.019(3) O8 0.035(2) 0.027(2) 0.035(2) 0.0018(16) 0.0038(16) 0.0022(18) O9 0.029(2) 0.027(2) 0.0292(18) 0.0013(15) 0.0007(15) 0.0026(17) O10 0.053(4) 0.085(6) 0.358(15) 0.096(8) -0.045(7) -0.004(4) W1 0.02043(11) 0.01925(12) 0.02215(11) 0.00016(7) 0.00156(7) -0.00086(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.445(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.371(8) . ? C2 O1 1.395(7) . ? C2 C7 1.403(7) . ? C3 C4 1.392(9) . ? C3 H3 0.9300 . ? C4 C5 1.368(9) . ? C4 H4 0.9300 . ? C5 C6 1.398(9) . ? C5 H5 0.9300 . ? C6 C7 1.406(7) . ? C6 C8 1.459(8) . ? C7 O2 1.335(6) . ? C7 Eu1 3.262(5) . ? C8 N1 1.259(8) . ? C8 H8 0.9300 . ? C9 C10 1.458(11) . ? C9 N1 1.473(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.537(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.464(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.278(8) . ? C12 C13 1.459(9) . ? C12 H12 0.9300 . ? C13 C18 1.393(8) . ? C13 C14 1.414(8) . ? C14 C15 1.354(10) . ? C14 H14 0.9300 . ? C15 C16 1.393(10) . ? C15 H15 0.9300 . ? C16 C17 1.371(8) . ? C16 H16 0.9300 . ? C17 C18 1.405(8) . ? C17 O4 1.409(7) . ? C18 O3 1.329(6) . ? C18 Eu1 3.261(5) . ? C19 O4 1.446(8) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N3 1.137(7) . ? C20 W1 2.163(6) . ? C21 N4 1.150(7) . ? C21 W1 2.171(5) . ? C22 N5 1.146(7) . ? C22 W1 2.163(5) . ? C23 N6 1.144(8) . ? C23 W1 2.171(6) . ? C24 N7 1.129(8) . ? C24 W1 2.159(6) . ? C25 N8 1.146(8) . ? C25 W1 2.162(6) . ? C26 N9 1.138(8) . ? C26 W1 2.148(6) . ? C27 N10 1.140(7) . ? C27 W1 2.171(5) . ? Eu1 O2 2.306(3) . ? Eu1 O3 2.317(3) . ? Eu1 O8 2.410(4) . ? Eu1 O6 2.459(4) . ? Eu1 O7 2.459(4) . ? Eu1 O4 2.460(4) . ? Eu1 O1 2.470(4) . ? Eu1 O5 2.476(4) . ? Eu1 Ni1 3.5054(7) . ? N1 Ni1 2.036(5) . ? N2 Ni1 2.011(5) . ? N3 Ni1 2.100(5) . ? Ni1 O3 2.017(4) . ? Ni1 O2 2.039(4) . ? Ni1 O9 2.244(4) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.7(5) . . ? C3 C2 C7 122.9(6) . . ? O1 C2 C7 112.4(5) . . ? C2 C3 C4 118.3(6) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 120.8(6) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.0(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 119.4(5) . . ? C5 C6 C8 116.4(5) . . ? C7 C6 C8 124.2(5) . . ? O2 C7 C2 117.7(5) . . ? O2 C7 C6 124.6(5) . . ? C2 C7 C6 117.7(5) . . ? O2 C7 Eu1 35.3(2) . . ? C2 C7 Eu1 82.6(3) . . ? C6 C7 Eu1 159.5(4) . . ? N1 C8 C6 128.0(5) . . ? N1 C8 H8 116.0 . . ? C6 C8 H8 116.0 . . ? C10 C9 N1 115.9(6) . . ? C10 C9 H9A 108.3 . . ? N1 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? N1 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 116.8(7) . . ? C9 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? C9 C10 H10B 108.1 . . ? C11 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? N2 C11 C10 111.1(6) . . ? N2 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? N2 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N2 C12 C13 126.9(5) . . ? N2 C12 H12 116.6 . . ? C13 C12 H12 116.6 . . ? C18 C13 C14 118.8(6) . . ? C18 C13 C12 124.9(5) . . ? C14 C13 C12 116.3(5) . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 120.6(6) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 118.7(6) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 122.1(6) . . ? C16 C17 O4 124.1(5) . . ? C18 C17 O4 113.8(5) . . ? O3 C18 C13 123.9(5) . . ? O3 C18 C17 117.6(5) . . ? C13 C18 C17 118.4(5) . . ? O3 C18 Eu1 35.8(2) . . ? C13 C18 Eu1 159.6(4) . . ? C17 C18 Eu1 81.9(3) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 W1 179.3(5) . . ? N4 C21 W1 177.9(5) . . ? N5 C22 W1 179.4(5) . . ? N6 C23 W1 178.5(6) . . ? N7 C24 W1 176.5(6) . . ? N8 C25 W1 176.8(6) . . ? N9 C26 W1 175.5(7) . . ? N10 C27 W1 176.5(5) . . ? O2 Eu1 O3 66.96(12) . . ? O2 Eu1 O8 77.39(13) . . ? O3 Eu1 O8 75.37(13) . . ? O2 Eu1 O6 142.26(14) . . ? O3 Eu1 O6 125.46(14) . . ? O8 Eu1 O6 137.80(15) . . ? O2 Eu1 O7 124.76(15) . . ? O3 Eu1 O7 141.42(15) . . ? O8 Eu1 O7 72.78(14) . . ? O6 Eu1 O7 70.60(16) . . ? O2 Eu1 O4 131.19(13) . . ? O3 Eu1 O4 65.63(13) . . ? O8 Eu1 O4 80.25(14) . . ? O6 Eu1 O4 78.15(14) . . ? O7 Eu1 O4 87.85(16) . . ? O2 Eu1 O1 64.67(12) . . ? O3 Eu1 O1 127.88(13) . . ? O8 Eu1 O1 110.95(14) . . ? O6 Eu1 O1 85.56(14) . . ? O7 Eu1 O1 84.24(16) . . ? O4 Eu1 O1 163.49(12) . . ? O2 Eu1 O5 85.56(14) . . ? O3 Eu1 O5 73.10(14) . . ? O8 Eu1 O5 148.03(14) . . ? O6 Eu1 O5 68.36(15) . . ? O7 Eu1 O5 138.17(15) . . ? O4 Eu1 O5 91.44(16) . . ? O1 Eu1 O5 84.91(16) . . ? O2 Eu1 C18 85.92(13) . . ? O3 Eu1 C18 19.60(13) . . ? O8 Eu1 C18 73.68(13) . . ? O6 Eu1 C18 113.32(13) . . ? O7 Eu1 C18 126.48(16) . . ? O4 Eu1 C18 46.07(13) . . ? O1 Eu1 C18 147.22(14) . . ? O5 Eu1 C18 78.35(15) . . ? O2 Eu1 C7 19.55(12) . . ? O3 Eu1 C7 84.56(13) . . ? O8 Eu1 C7 89.70(13) . . ? O6 Eu1 C7 125.15(14) . . ? O7 Eu1 C7 116.17(16) . . ? O4 Eu1 C7 150.03(13) . . ? O1 Eu1 C7 45.31(13) . . ? O5 Eu1 C7 82.26(15) . . ? C18 Eu1 C7 104.03(13) . . ? O2 Eu1 Ni1 33.72(9) . . ? O3 Eu1 Ni1 33.24(9) . . ? O8 Eu1 Ni1 73.84(9) . . ? O6 Eu1 Ni1 144.95(11) . . ? O7 Eu1 Ni1 144.45(11) . . ? O4 Eu1 Ni1 98.28(9) . . ? O1 Eu1 Ni1 96.56(9) . . ? O5 Eu1 Ni1 76.96(10) . . ? C18 Eu1 Ni1 52.39(10) . . ? C7 Eu1 Ni1 51.75(9) . . ? C8 N1 C9 115.0(5) . . ? C8 N1 Ni1 122.6(4) . . ? C9 N1 Ni1 121.7(4) . . ? C12 N2 C11 117.8(5) . . ? C12 N2 Ni1 124.9(4) . . ? C11 N2 Ni1 117.3(4) . . ? C20 N3 Ni1 162.5(4) . . ? N2 Ni1 O3 91.70(17) . . ? N2 Ni1 N1 98.6(2) . . ? O3 Ni1 N1 169.11(18) . . ? N2 Ni1 O2 169.60(18) . . ? O3 Ni1 O2 77.90(14) . . ? N1 Ni1 O2 91.78(17) . . ? N2 Ni1 N3 91.41(19) . . ? O3 Ni1 N3 95.43(17) . . ? N1 Ni1 N3 87.95(19) . . ? O2 Ni1 N3 89.94(17) . . ? N2 Ni1 O9 88.97(17) . . ? O3 Ni1 O9 86.56(15) . . ? N1 Ni1 O9 90.02(17) . . ? O2 Ni1 O9 90.04(15) . . ? N3 Ni1 O9 177.96(17) . . ? N2 Ni1 Eu1 130.72(14) . . ? O3 Ni1 Eu1 39.02(10) . . ? N1 Ni1 Eu1 130.60(14) . . ? O2 Ni1 Eu1 38.88(10) . . ? N3 Ni1 Eu1 93.14(12) . . ? O9 Ni1 Eu1 88.12(10) . . ? C2 O1 C1 115.1(5) . . ? C2 O1 Eu1 119.4(3) . . ? C1 O1 Eu1 125.4(4) . . ? C7 O2 Ni1 121.3(3) . . ? C7 O2 Eu1 125.1(3) . . ? Ni1 O2 Eu1 107.39(16) . . ? C18 O3 Ni1 125.8(3) . . ? C18 O3 Eu1 124.6(3) . . ? Ni1 O3 Eu1 107.74(15) . . ? C17 O4 C19 116.1(5) . . ? C17 O4 Eu1 118.2(3) . . ? C19 O4 Eu1 123.3(4) . . ? C26 W1 C24 98.8(3) . . ? C26 W1 C25 69.9(2) . . ? C24 W1 C25 74.1(2) . . ? C26 W1 C20 77.4(2) . . ? C24 W1 C20 144.4(2) . . ? C25 W1 C20 133.7(2) . . ? C26 W1 C22 145.6(2) . . ? C24 W1 C22 90.3(2) . . ? C25 W1 C22 144.1(2) . . ? C20 W1 C22 76.2(2) . . ? C26 W1 C21 90.5(2) . . ? C24 W1 C21 144.7(2) . . ? C25 W1 C21 77.4(2) . . ? C20 W1 C21 70.8(2) . . ? C22 W1 C21 101.1(2) . . ? C26 W1 C23 142.3(2) . . ? C24 W1 C23 77.5(2) . . ? C25 W1 C23 73.1(2) . . ? C20 W1 C23 126.6(2) . . ? C22 W1 C23 72.0(2) . . ? C21 W1 C23 74.6(2) . . ? C26 W1 C27 73.7(2) . . ? C24 W1 C27 71.1(2) . . ? C25 W1 C27 123.9(2) . . ? C20 W1 C27 74.0(2) . . ? C22 W1 C27 78.2(2) . . ? C21 W1 C27 143.8(2) . . ? C23 W1 C27 136.1(2) . . ? _refine_diff_density_max 1.068 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.143 _shelxl_version_number 2014-3 _shelx_res_file ; TITL tr22 in P 21/c CELL 0.71073 8.9747 13.9587 27.4653 90.000 93.266 90.000 ZERR 4.00 0.0003 0.0004 0.0009 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H EU N NI O W UNIT 108 128 4 40 4 40 4 MERG 2 OMIT -3.00 56.00 OMIT -9 3 7 OMIT -8 1 1 OMIT -8 1 5 OMIT 4 13 2 OMIT 9 2 3 OMIT -9 1 3 OMIT -11 0 28 OMIT 11 3 3 OMIT -10 3 5 OMIT 5 7 7 OMIT -7 2 1 OMIT -10 1 1 OMIT 1 0 2 FMAP 2 PLAN 20 ACTA BOND $H L.S. 8 WGHT 0.030200 12.880000 EXTI 0.001002 FVAR 0.26490 C1 1 0.656593 0.339756 0.024025 11.00000 0.05138 0.08620 = 0.04841 -0.02069 0.02463 -0.01592 AFIX 33 H1A 2 0.609307 0.293074 0.002630 11.00000 -1.50000 H1B 2 0.670050 0.398265 0.006437 11.00000 -1.50000 H1C 2 0.751982 0.316036 0.036193 11.00000 -1.50000 AFIX 0 C2 1 0.620732 0.424620 0.098282 11.00000 0.02233 0.03121 = 0.03628 -0.00064 0.00269 -0.00245 C3 1 0.743300 0.481080 0.092212 11.00000 0.02794 0.05002 = 0.04970 0.00056 0.01123 -0.01357 AFIX 43 H3 2 0.794581 0.477790 0.063774 11.00000 -1.20000 AFIX 0 C4 1 0.789039 0.543431 0.129673 11.00000 0.03149 0.04701 = 0.06688 -0.00448 0.00885 -0.02266 AFIX 43 H4 2 0.871788 0.582424 0.126208 11.00000 -1.20000 AFIX 0 C5 1 0.713709 0.548054 0.171548 11.00000 0.03226 0.04532 = 0.06021 -0.00870 -0.00684 -0.01256 AFIX 43 H5 2 0.746893 0.589493 0.196369 11.00000 -1.20000 AFIX 0 C6 1 0.587605 0.491412 0.177576 11.00000 0.02850 0.02474 = 0.03752 -0.00404 -0.00074 -0.00570 C7 1 0.539477 0.427438 0.140411 11.00000 0.01885 0.02483 = 0.03316 0.00164 0.00054 -0.00233 C8 1 0.513989 0.503597 0.223181 11.00000 0.03964 0.02544 = 0.03688 -0.00646 -0.00886 -0.00295 AFIX 43 H8 2 0.565615 0.539579 0.247131 11.00000 -1.20000 AFIX 0 C9 1 0.338975 0.503755 0.281522 11.00000 0.07226 0.06559 = 0.03361 -0.01999 0.01206 -0.01271 AFIX 23 H9A 2 0.416279 0.488500 0.306438 11.00000 -1.20000 H9B 2 0.328942 0.572931 0.280569 11.00000 -1.20000 AFIX 0 C10 1 0.198676 0.463153 0.296178 11.00000 0.08590 0.06030 = 0.04785 -0.01691 0.02433 -0.01449 AFIX 23 H10A 2 0.177600 0.490055 0.327615 11.00000 -1.20000 H10B 2 0.212662 0.394758 0.300707 11.00000 -1.20000 AFIX 0 C11 1 0.060760 0.478446 0.261277 11.00000 0.06555 0.05118 = 0.04872 -0.01099 0.01943 0.01699 AFIX 23 H11A 2 -0.028855 0.468921 0.278823 11.00000 -1.20000 H11B 2 0.060117 0.543779 0.249234 11.00000 -1.20000 AFIX 0 C12 1 -0.059563 0.365498 0.209218 11.00000 0.02791 0.03853 = 0.03919 0.01072 0.01404 0.00827 AFIX 43 H12 2 -0.139972 0.377731 0.228210 11.00000 -1.20000 AFIX 0 C13 1 -0.083803 0.295246 0.170222 11.00000 0.02568 0.03698 = 0.03346 0.00861 0.00292 -0.00109 C14 1 -0.223052 0.247654 0.167927 11.00000 0.02310 0.06310 = 0.04239 0.01818 0.00482 -0.00134 AFIX 43 H14 2 -0.292844 0.262895 0.190463 11.00000 -1.20000 AFIX 0 C15 1 -0.256850 0.180301 0.133560 11.00000 0.02758 0.06026 = 0.04871 0.01464 -0.00351 -0.01276 AFIX 43 H15 2 -0.349262 0.150024 0.132783 11.00000 -1.20000 AFIX 0 C16 1 -0.154431 0.155960 0.099359 11.00000 0.03457 0.05123 = 0.04042 0.00674 -0.00711 -0.01597 AFIX 43 H16 2 -0.177730 0.109884 0.075678 11.00000 -1.20000 AFIX 0 C17 1 -0.018629 0.201226 0.101276 11.00000 0.02760 0.03374 = 0.03224 0.00337 -0.00147 -0.00390 C18 1 0.019582 0.271950 0.136171 11.00000 0.02034 0.02761 = 0.02770 0.00732 -0.00120 -0.00294 C19 1 0.080366 0.094132 0.041688 11.00000 0.05222 0.04413 = 0.05694 -0.02032 0.00284 -0.01719 AFIX 33 H19A 2 0.162360 0.088320 0.020910 11.00000 -1.50000 H19B 2 0.081250 0.040983 0.063886 11.00000 -1.50000 H19C 2 -0.011806 0.094373 0.022152 11.00000 -1.50000 AFIX 0 C20 1 0.204989 0.606949 0.139135 11.00000 0.02505 0.02370 = 0.02791 0.00092 0.00207 0.00109 C21 1 0.080596 0.674410 0.062385 11.00000 0.03227 0.02579 = 0.02894 -0.00033 0.00077 -0.00137 C22 1 0.031349 0.738651 0.177775 11.00000 0.02325 0.02700 = 0.02708 -0.00245 0.00517 -0.00069 C23 1 -0.015347 0.835186 0.099648 11.00000 0.02957 0.03132 = 0.03782 0.00461 0.00140 0.00612 C24 1 0.236705 0.900664 0.147433 11.00000 0.04875 0.02036 = 0.03280 -0.00759 0.00112 -0.00820 C25 1 0.234313 0.840921 0.057636 11.00000 0.04403 0.02961 = 0.03067 0.00238 0.00097 -0.00310 C26 1 0.403329 0.720813 0.097103 11.00000 0.02833 0.05801 = 0.03020 0.00606 0.01232 0.00978 C27 1 0.335836 0.748589 0.186417 11.00000 0.02480 0.03150 = 0.02862 -0.00149 -0.00642 -0.00233 EU1 3 0.329080 0.273222 0.079467 11.00000 0.02238 0.02338 = 0.02417 -0.00222 0.00269 -0.00221 N1 4 0.389138 0.471387 0.234106 11.00000 0.03608 0.03134 = 0.02735 -0.00578 0.00327 -0.00268 N2 4 0.060420 0.411975 0.220034 11.00000 0.03219 0.03015 = 0.03054 0.00116 0.00878 0.00669 N3 4 0.212788 0.527630 0.148331 11.00000 0.03510 0.02569 = 0.03382 -0.00193 0.00423 0.00174 N4 4 0.019872 0.630703 0.031806 11.00000 0.03741 0.04526 = 0.03964 -0.00612 -0.00454 -0.00512 N5 4 -0.051612 0.727854 0.207506 11.00000 0.03633 0.03582 = 0.04104 -0.00604 0.00916 -0.00389 N6 4 -0.122029 0.875222 0.087206 11.00000 0.04117 0.06457 = 0.05715 0.01024 0.00137 0.01963 N7 4 0.265258 0.976492 0.158820 11.00000 0.07457 0.03128 = 0.05863 -0.00328 0.00076 -0.00793 N8 4 0.266082 0.885028 0.024582 11.00000 0.08235 0.04949 = 0.03689 0.01072 0.00838 -0.01061 N9 4 0.517341 0.706637 0.082463 11.00000 0.04447 0.11086 = 0.04995 0.02010 0.01521 0.02246 N10 4 0.419681 0.745170 0.219126 11.00000 0.04337 0.05230 = 0.03988 -0.00353 -0.00562 -0.00465 NI1 5 0.251489 0.398115 0.185817 11.00000 0.02412 0.02141 = 0.02448 -0.00118 0.00376 -0.00038 O1 6 0.563936 0.357657 0.064388 11.00000 0.02887 0.04723 = 0.03246 -0.00876 0.01070 -0.00685 O2 6 0.423043 0.368411 0.142607 11.00000 0.02374 0.02508 = 0.02879 -0.00423 0.00470 -0.00439 O3 6 0.151272 0.314665 0.133688 11.00000 0.01972 0.02602 = 0.03047 -0.00359 0.00395 -0.00403 O4 6 0.094362 0.182555 0.068968 11.00000 0.03269 0.03487 = 0.03458 -0.00800 0.00009 -0.00896 O5 6 0.205900 0.420999 0.047600 11.00000 0.06226 0.03824 = 0.04154 0.00436 -0.00228 0.01407 O6 6 0.288974 0.268842 -0.009803 11.00000 0.03737 0.06155 = 0.02816 0.00157 0.00284 -0.00568 O7 6 0.457025 0.132887 0.047397 11.00000 0.06328 0.04494 = 0.04257 -0.00602 0.01045 0.01858 O8 6 0.365390 0.160538 0.145564 11.00000 0.03499 0.02659 = 0.03469 0.00182 0.00382 0.00223 O9 6 0.298562 0.262418 0.227740 11.00000 0.02889 0.02678 = 0.02919 0.00129 0.00070 0.00258 O10 6 0.585273 0.958095 0.070781 11.00000 0.05283 0.08477 = 0.35828 0.09592 -0.04544 -0.00361 W1 7 0.187314 0.757611 0.121347 11.00000 0.02043 0.01925 = 0.02215 0.00016 0.00156 -0.00086 HKLF 4 REM tr22 in P 21/c REM R1 = 0.0369 for 6471 Fo > 4sig(Fo) and 0.0467 for all 7591 data REM 452 parameters refined using 0 restraints END WGHT 0.0306 12.7066 REM Highest difference peak 1.068, deepest hole -0.985, 1-sigma level 0.143 Q1 1 0.1662 0.5392 0.2764 11.00000 0.05 1.07 Q2 1 0.2127 0.8384 0.0983 11.00000 0.05 0.92 Q3 1 0.5813 0.9787 0.0905 11.00000 0.05 0.90 Q4 1 0.3040 0.1954 0.1753 11.00000 0.05 0.82 Q5 1 0.1779 0.7562 0.0807 11.00000 0.05 0.80 Q6 1 0.3461 0.7481 0.1184 11.00000 0.05 0.79 Q7 1 0.2065 0.8404 0.1467 11.00000 0.05 0.76 Q8 1 0.1877 0.7559 0.1621 11.00000 0.05 0.72 Q9 1 0.2777 0.2001 0.1134 11.00000 0.05 0.71 Q10 1 0.1928 0.7582 0.0962 11.00000 0.05 0.71 Q11 1 0.3281 0.1031 0.1443 11.00000 0.05 0.70 Q12 1 0.3920 0.2759 0.2461 11.00000 0.05 0.69 Q13 1 0.2240 0.2585 0.2508 11.00000 0.05 0.69 Q14 1 0.2573 0.1842 0.0787 11.00000 0.05 0.69 Q15 1 0.3069 0.7204 0.0985 11.00000 0.05 0.68 Q16 1 0.2808 0.6782 0.1216 11.00000 0.05 0.67 Q17 1 0.0993 0.6802 0.1216 11.00000 0.05 0.67 Q18 1 0.3375 0.2807 0.1187 11.00000 0.05 0.66 Q19 1 0.2036 0.6718 0.1425 11.00000 0.05 0.66 Q20 1 0.3252 0.2836 0.1837 11.00000 0.05 0.63 ; _shelx_res_checksum 16598 _shelx_hkl_file ; -13 0 2 184.95 26.31 -13 0 3 -15.33 21.06 -13 0 4 314.74 24.57 -13 0 5 28.36 20.79 -13 0 6 15.57 22.05 -13 0 7 -18.98 21.93 -13 0 8 242.15 23.90 -13 0 9 0.44 21.82 -13 0 10 81.93 22.62 13 0 -10 91.03 27.36 13 0 -11 -16.67 26.26 -13 0 11 -10.24 21.16 13 0 -12 90.89 29.26 -13 0 12 116.05 22.32 -13 0 13 21.19 20.92 13 0 -13 3.67 27.14 -13 0 14 -22.27 21.98 13 0 -14 3.29 26.54 13 0 -15 12.77 27.66 -13 0 15 -6.57 22.20 -13 0 16 23.19 18.08 13 0 -16 14.06 27.65 -13 1 1 37.57 21.29 -13 1 2 67.68 21.49 -13 1 3 7.38 21.19 -13 1 4 25.11 21.26 -13 1 5 -4.62 20.52 -13 -1 6 -15.39 21.18 -13 1 6 35.92 20.77 -13 1 7 8.94 20.15 -13 -1 7 10.07 21.31 -13 1 8 136.68 24.94 -13 1 9 -13.16 20.61 -13 -1 10 152.26 22.87 13 -1 -10 136.56 27.39 -13 1 10 95.43 22.47 -13 1 11 1.40 20.79 13 -1 -11 28.39 26.36 -13 -1 11 1.88 22.32 13 1 -11 -23.27 27.56 13 1 -12 67.74 23.19 -13 -1 12 50.82 22.73 -13 1 12 83.90 21.89 13 -1 -12 74.49 31.47 -13 -1 13 -27.60 21.65 -13 1 13 4.60 21.79 13 1 -13 2.26 26.13 13 -1 -13 -2.71 26.29 13 1 -14 297.14 30.39 -13 -1 14 261.00 25.15 13 -1 -14 187.55 31.11 -13 1 14 220.59 26.00 -13 -1 15 6.22 21.73 13 -1 -15 29.08 27.45 13 1 -15 6.40 21.99 -13 1 15 -5.05 17.61 -13 -1 16 28.39 22.59 13 -1 -16 39.30 28.22 13 1 -16 -30.85 27.23 13 1 -17 37.12 28.39 -13 2 1 12.46 21.51 -13 2 2 149.65 26.01 -13 2 3 5.43 22.30 -13 2 4 397.24 28.23 -13 2 5 0.00 19.95 -13 2 6 8.49 22.47 -13 2 7 3.61 20.36 -13 2 8 292.40 27.11 -13 2 9 13.50 20.45 -13 2 10 51.27 24.47 -13 -2 10 19.42 21.89 -13 2 11 2.88 20.95 -13 -2 11 4.38 22.21 13 -2 -11 13.10 30.30 13 2 -12 54.99 27.02 13 -2 -12 40.66 27.54 -13 2 12 45.90 21.86 -13 -2 12 36.55 21.90 -13 -2 13 22.51 21.35 13 -2 -13 -5.45 27.18 13 2 -13 6.15 20.58 -13 2 13 19.97 16.81 -13 -2 14 -10.95 17.91 13 -2 -14 35.96 28.44 13 2 -14 -22.60 26.46 13 2 -15 20.59 27.46 -13 -2 15 7.64 22.07 13 -2 -15 18.84 27.01 13 -2 -16 47.36 27.74 13 2 -16 14.36 27.66 -13 -2 16 39.10 22.75 -13 3 1 16.71 24.05 -13 3 2 16.09 23.92 -13 3 3 -1.97 24.20 -13 3 4 17.40 23.21 -13 3 5 6.30 20.12 -13 3 6 0.76 23.72 -13 3 7 20.03 23.95 -13 3 8 70.55 21.86 -13 3 9 46.82 24.18 13 3 -10 120.20 26.83 13 -3 -10 146.13 29.72 -13 3 10 160.05 24.07 -13 -3 11 21.28 23.00 13 -3 -11 25.45 31.74 13 3 -11 7.22 21.88 13 -3 -12 46.27 31.75 13 3 -12 26.76 26.61 -13 -3 12 59.41 23.15 13 3 -13 -15.82 26.94 -13 -3 13 39.42 23.30 13 -3 -13 -10.44 27.27 13 -3 -14 184.28 29.16 -13 -3 14 293.00 25.44 13 -3 -14 193.25 32.13 13 3 -14 267.24 30.89 13 -3 -15 19.86 21.29 -13 -3 15 23.55 22.70 13 -3 -15 -12.14 28.10 13 3 -15 -10.68 22.83 13 -3 -16 30.53 28.00 -13 4 1 62.43 24.02 -13 4 2 96.94 21.92 -13 4 3 4.82 24.30 -13 4 4 465.48 29.19 -13 4 5 27.54 25.18 -13 4 6 1.72 24.12 -13 4 7 25.76 22.40 13 -4 -9 -22.94 31.13 13 -4 -10 28.47 31.33 13 -4 -11 -18.46 25.32 13 -4 -11 13.38 32.13 13 4 -11 10.70 25.34 -13 -4 12 -2.68 23.03 13 -4 -12 41.98 31.76 13 4 -12 63.29 24.80 13 -4 -12 33.15 22.14 13 -4 -13 24.60 21.78 13 -4 -13 38.89 31.91 -13 -4 13 -17.93 22.60 13 4 -13 14.29 21.27 13 -4 -14 11.14 28.86 -13 -4 14 3.31 22.38 13 -4 -14 17.46 25.23 13 4 -14 35.97 21.74 13 -4 -15 19.77 32.85 13 4 -15 19.27 25.88 -13 5 1 5.16 27.23 -13 5 2 52.85 25.56 13 -5 -7 25.85 24.34 13 -5 -8 51.36 25.91 13 -5 -8 37.04 31.49 13 -5 -9 -11.33 24.86 13 -5 -9 13.79 31.54 13 -5 -10 128.58 34.36 13 -5 -10 36.62 23.65 13 -5 -11 58.50 29.07 13 -5 -11 28.94 26.30 13 5 -11 50.93 25.89 13 -5 -12 63.67 29.15 13 -5 -12 33.39 26.66 13 5 -12 31.97 22.02 13 5 -13 -0.06 21.40 13 -5 -13 3.39 28.29 13 -5 -13 20.38 25.26 13 -6 -1 19.73 31.66 13 -6 -2 138.10 28.62 13 -6 -2 115.55 33.09 13 -6 -3 42.21 32.37 13 -6 -3 12.73 27.75 13 -6 -4 38.37 30.19 13 -6 -5 52.42 29.78 13 -6 -6 -3.62 28.67 13 -6 -6 23.38 34.21 13 -6 -7 44.04 34.98 13 -6 -7 37.37 26.49 13 -6 -8 156.03 27.46 13 -6 -8 105.57 33.54 13 -6 -9 8.11 34.52 13 -6 -9 13.03 24.86 13 -6 -10 27.01 25.81 13 -6 -10 20.22 32.06 13 6 -10 0.86 26.16 13 6 -11 -8.10 22.37 13 -7 -1 38.45 38.48 13 -7 -1 21.56 36.14 13 -7 -2 58.28 33.62 13 -7 -2 78.50 39.48 13 -7 -3 -2.38 33.80 13 -7 -3 12.74 30.61 13 -7 -4 22.68 33.51 13 -7 -4 19.06 33.02 13 -7 -5 -1.01 35.74 13 -7 -5 9.09 30.94 13 -7 -6 55.27 34.28 13 -7 -6 43.52 32.23 13 -7 -7 10.07 36.46 -12 0 12 270.25 22.00 12 0 -12 306.95 27.28 12 0 -13 11.88 24.06 -12 0 13 8.88 19.73 -12 0 14 115.07 20.73 12 0 -14 180.11 25.67 12 0 -15 26.81 24.30 -12 0 15 -5.65 20.24 12 0 -16 39.53 24.72 -12 0 16 27.01 19.92 12 0 -17 19.24 25.72 -12 0 17 12.77 16.26 -12 0 18 19.63 16.34 12 0 -18 2.52 20.83 12 0 -19 -12.14 21.50 12 0 -20 16.72 25.98 12 0 -21 15.19 21.89 12 0 -21 23.94 27.33 12 0 -22 35.93 23.20 12 0 -22 -8.84 23.18 12 0 -23 18.58 27.58 12 0 -23 16.32 21.33 -12 1 9 11.31 18.90 -12 1 10 67.73 19.70 -12 1 11 46.83 19.50 -12 1 12 126.29 20.39 12 -1 -12 148.97 25.26 12 -1 -13 35.08 23.75 12 1 -13 20.19 19.39 -12 1 13 13.37 19.60 -12 -1 14 31.50 16.96 12 -1 -14 13.60 26.10 -12 1 14 25.74 16.06 12 1 -14 -13.43 24.53 12 -1 -15 32.12 24.27 -12 1 15 -7.28 19.74 12 1 -15 -8.88 24.49 -12 -1 15 6.85 19.59 12 1 -16 411.92 28.88 -12 1 16 396.39 23.36 12 -1 -16 450.15 32.14 -12 -1 16 378.76 26.04 12 -1 -17 17.27 24.57 12 1 -17 -14.06 24.44 -12 -1 17 30.31 21.20 12 -1 -18 83.63 27.72 -12 -1 18 87.64 22.05 12 1 -18 31.70 27.16 12 -1 -19 25.22 27.03 -12 -1 19 37.95 21.06 12 -1 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21.14 12 -2 -18 6.74 20.45 12 -2 -18 18.25 26.11 12 -2 -19 5.00 20.87 12 2 -19 -1.55 26.00 12 -2 -19 8.69 26.21 -12 -2 19 -5.43 21.85 -12 -2 20 14.17 16.90 12 -2 -20 -15.45 23.51 12 2 -20 27.02 25.04 12 -2 -20 -9.77 22.06 12 -2 -21 -11.80 28.53 12 -2 -21 -0.59 22.08 12 2 -21 13.50 25.89 12 -2 -22 34.89 24.96 12 2 -22 88.41 27.22 12 -2 -22 47.83 22.44 12 2 -23 -4.70 26.41 -12 3 1 22.10 23.30 -12 3 2 36.82 19.84 -12 3 3 66.73 21.67 -12 3 4 22.97 22.47 -12 3 5 29.36 18.21 -12 3 6 40.84 22.59 -12 3 7 -6.91 18.83 -12 3 8 32.72 19.28 -12 3 9 17.35 21.75 -12 3 10 14.53 19.21 -12 3 11 -0.02 23.10 12 -3 -11 6.85 24.46 12 -3 -12 283.50 29.07 12 -3 -13 52.94 24.41 12 3 -13 63.12 25.30 12 -3 -14 7.03 28.85 12 3 -14 41.83 20.29 12 -3 -15 28.79 25.21 12 3 -15 26.18 24.57 12 -3 -15 -21.75 19.99 12 -3 -16 288.11 25.82 12 -3 -16 297.84 35.94 12 3 -16 324.72 28.98 -12 -3 17 26.70 17.76 12 -3 -17 -10.34 25.84 12 3 -17 16.01 24.64 12 -3 -17 22.10 20.27 12 -3 -18 17.40 20.43 -12 -3 18 33.03 21.20 12 -3 -18 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31.80 10 7 -23 132.75 19.50 -10 -7 23 118.11 19.15 10 -7 -23 70.34 34.32 10 7 -24 56.16 21.79 10 -7 -24 18.30 24.01 10 -7 -24 37.99 29.68 10 -7 -24 25.24 33.09 -10 -7 24 1.96 21.81 10 -7 -25 -3.40 21.22 10 -7 -25 15.38 28.73 -10 -7 25 4.54 17.92 10 -7 -25 8.72 30.56 10 7 -25 19.12 18.60 10 -7 -26 123.24 32.04 10 -7 -26 15.86 32.03 10 -7 -26 8.51 26.30 10 7 -26 66.14 19.74 10 7 -27 19.95 23.32 10 -7 -27 -12.93 21.15 10 -7 -27 -9.05 30.09 10 -7 -27 27.56 28.76 10 -8 -1 101.96 27.02 10 -8 -1 117.94 41.90 10 -8 -1 113.06 40.15 10 -8 -2 63.57 34.45 10 -8 -2 68.20 36.57 10 -8 -2 51.40 28.46 10 -8 -3 -2.66 30.53 10 -8 -3 10.38 28.01 10 -8 -4 71.96 32.12 10 -8 -4 103.88 29.22 10 -8 -5 37.98 27.56 10 -8 -5 45.90 28.86 10 -8 -6 225.83 32.60 10 -8 -6 245.89 32.89 10 -8 -7 85.01 30.22 10 -8 -7 68.38 27.13 10 -8 -8 300.59 32.08 10 -8 -8 333.86 34.89 10 -8 -9 275.18 36.26 10 -8 -9 242.84 29.45 10 -8 -10 256.73 35.39 10 -8 -10 192.69 28.60 10 -8 -11 49.23 28.35 10 -8 -11 67.03 35.54 10 -8 -11 66.88 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31.64 10 -9 -22 -8.90 26.79 10 -9 -23 6.14 24.12 10 -9 -23 -21.16 34.60 10 -9 -23 155.70 29.53 10 9 -23 88.27 20.08 -10 -9 24 -5.46 22.98 10 -9 -24 33.45 33.55 10 9 -24 0.15 18.21 10 -9 -24 20.73 27.80 10 -9 -24 22.36 21.68 -10 -9 25 20.75 18.85 10 -9 -25 -0.80 25.79 10 -9 -25 15.45 35.34 10 9 -25 31.06 23.06 10 -9 -25 27.62 28.51 -10 -10 1 16.76 34.41 -10 -10 1 31.95 40.52 10 -10 -1 -11.26 24.59 10 -10 -2 214.27 26.65 -10 -10 2 160.31 40.69 -10 -10 2 197.02 46.98 10 -10 -3 19.54 25.27 -10 -10 3 21.52 41.80 -10 -10 3 19.79 47.86 10 -10 -4 125.40 26.04 10 -10 -5 11.79 24.60 10 -10 -6 260.23 31.61 10 -10 -7 153.54 29.21 10 -10 -8 94.55 30.96 10 -10 -9 119.52 45.22 10 -10 -9 165.78 30.59 10 -10 -9 137.50 41.43 10 -10 -10 46.19 29.60 10 -10 -10 37.38 34.35 10 -10 -10 36.65 37.96 10 -10 -11 12.01 31.25 10 -10 -11 2.47 30.57 10 -10 -11 21.83 36.07 10 -10 -12 113.55 33.90 10 -10 -12 122.93 36.92 10 -10 -12 93.71 31.85 10 -10 -13 330.98 34.07 10 -10 -13 367.92 38.58 10 -10 -13 260.53 41.92 10 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16.28 30.62 -10 -13 11 -0.19 39.89 10 -13 -12 39.21 31.08 -10 -13 12 3.22 38.35 -10 -13 13 -3.87 38.35 10 -13 -13 20.11 31.64 -10 -13 14 125.50 41.88 10 -13 -14 169.96 34.82 -10 -13 15 6.14 41.79 10 -13 -15 -2.50 33.79 10 13 -15 -16.66 18.13 10 -13 -16 13.30 33.76 -10 -13 16 14.26 40.52 10 13 -16 21.32 18.22 10 -14 -1 9.08 29.88 10 -14 -2 48.87 26.62 10 -14 -3 11.01 29.57 -10 -14 3 82.94 36.89 -10 -14 4 88.44 37.84 10 -14 -4 54.33 28.36 10 -14 -5 28.44 31.14 -10 -14 5 26.30 36.75 -10 -14 6 20.45 37.21 10 -14 -6 0.06 26.55 10 -14 -7 29.10 30.98 -10 -14 7 15.44 37.77 -10 -14 8 111.18 41.18 10 -14 -8 137.87 29.08 10 14 -9 161.61 25.40 -10 -14 9 62.58 40.21 10 -14 -9 135.89 34.19 -10 -14 10 29.41 37.35 10 14 -10 -2.14 22.55 10 -14 -10 18.41 32.28 -10 -14 11 8.96 40.66 10 14 -11 0.80 19.36 10 -14 -11 31.27 31.95 10 14 -12 3.32 19.92 10 -14 -12 44.91 28.72 -10 -14 12 38.49 41.99 9 0 -3 42.17 20.43 9 0 -4 644.97 22.17 9 0 -15 -3.20 17.14 9 0 -16 57.40 21.46 9 0 -17 2.63 20.58 9 0 -18 1111.38 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18.62 4 6 -28 6.96 13.57 4 6 -28 -0.92 20.15 4 6 -28 -1.62 18.91 -4 -6 28 19.56 15.13 4 6 -29 95.67 17.38 -4 -6 29 135.44 17.44 4 -6 -29 111.74 24.63 4 -6 -29 107.49 20.33 4 6 -29 166.62 18.76 4 6 -29 79.81 16.15 4 -6 -29 131.52 14.14 -4 -6 30 457.87 19.91 4 -6 -30 273.16 26.72 4 -6 -30 321.96 22.27 4 6 -30 463.14 20.77 4 6 -30 311.36 19.81 4 6 -30 322.02 23.05 4 -6 -30 463.30 19.96 4 6 -31 149.31 22.48 -4 -6 31 206.12 18.47 4 -6 -31 216.11 15.50 4 -6 -31 133.04 18.06 4 6 -31 254.15 18.93 4 -6 -31 269.18 24.94 4 6 -31 170.05 21.11 4 -6 -32 110.68 24.89 4 6 -32 200.82 19.62 4 6 -32 143.07 20.96 4 -6 -32 222.85 18.57 4 6 -32 103.37 18.82 -4 -6 32 173.89 19.15 4 -6 -32 127.48 16.83 4 -6 -33 127.97 25.37 4 -6 -33 189.35 18.57 4 6 -33 182.88 18.79 4 6 -33 115.23 22.11 4 6 -33 117.32 23.09 4 -6 -33 113.71 21.46 4 6 -34 378.06 18.84 4 -6 -34 219.42 22.67 4 6 -34 230.01 21.19 4 6 -34 252.71 22.92 4 -6 -34 205.63 23.86 4 -6 -34 341.96 21.25 4 6 -35 5.19 18.64 4 6 -35 21.32 20.75 4 6 -35 6.59 22.13 4 -6 -35 6.20 23.88 4 -6 -35 3.91 17.60 4 -6 -35 9.29 20.61 4 6 -36 161.77 21.75 4 -6 -36 350.39 18.67 4 -6 -36 58.94 19.27 4 6 -36 337.79 22.81 4 -6 -36 129.44 22.77 4 6 -36 204.84 20.43 4 6 -37 48.30 22.73 4 -6 -37 28.62 25.05 4 -6 -37 -17.20 17.65 4 6 -37 4.56 17.36 4 -6 -37 52.36 18.88 4 6 -37 4.70 19.87 4 -6 -38 27.86 22.21 4 -6 -38 13.99 20.57 4 6 -38 43.45 23.60 4 -6 -38 48.96 24.69 4 6 -38 48.30 20.61 4 6 -38 31.78 21.61 4 -6 -39 60.21 17.78 4 6 -39 57.90 21.25 4 -6 -39 45.95 23.00 4 -6 -39 32.30 22.33 4 6 -39 75.35 22.58 4 6 -39 -7.36 20.84 -4 -7 1 313.80 20.81 4 7 -1 279.41 17.94 4 -7 -2 39.42 40.67 -4 -7 2 91.42 18.17 4 -7 -2 50.88 39.26 4 7 -2 62.93 15.61 -4 -7 3 1216.05 24.55 4 -7 -3 1327.05 54.11 4 -7 -3 1282.20 50.24 4 7 -3 1276.90 27.19 -4 -7 4 407.28 18.04 4 -7 -4 461.57 37.46 4 -7 -4 401.31 31.66 4 7 -4 413.08 18.60 4 -7 -5 225.99 28.92 -4 -7 5 256.81 19.40 4 -7 -5 212.62 27.47 -4 -7 5 269.43 25.18 4 7 -5 223.31 16.32 4 -7 -6 1093.38 35.40 4 -7 -6 1078.68 40.08 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17.31 4 7 -33 24.48 21.16 4 -7 -33 29.98 24.19 -4 -7 33 40.98 17.97 4 -7 -33 36.27 19.66 4 -7 -33 38.13 18.03 4 7 -33 24.82 18.87 4 7 -33 12.19 19.35 -4 -7 34 12.35 18.18 4 7 -34 13.80 17.02 4 -7 -34 28.53 20.17 4 7 -34 21.13 18.88 4 -7 -34 21.78 20.19 4 7 -34 7.78 19.91 4 -7 -34 39.52 17.42 4 -7 -35 18.11 15.44 4 7 -35 25.20 19.22 4 -7 -35 52.73 24.97 4 -7 -35 3.38 17.28 4 7 -35 17.34 21.15 4 7 -35 10.01 21.48 4 -7 -36 19.48 21.12 4 -7 -36 16.25 18.43 4 7 -36 8.46 19.56 4 7 -36 12.56 19.01 4 -7 -36 11.10 17.53 4 7 -36 5.06 21.06 4 -7 -37 28.16 21.66 4 7 -37 29.23 20.34 4 -7 -37 31.12 26.89 4 7 -37 5.33 23.59 4 7 -37 12.54 21.37 4 -7 -37 18.87 15.59 4 7 -38 8.91 18.02 4 -7 -38 54.88 23.12 4 7 -38 38.37 20.83 4 -7 -38 57.21 20.72 4 -7 -38 22.18 27.39 4 7 -38 -5.94 19.66 -4 -8 1 112.19 15.29 4 8 -1 111.56 17.49 -4 -8 2 1290.92 25.38 4 8 -2 1257.60 28.17 4 -8 -3 1057.63 54.91 4 8 -3 1005.21 25.60 4 -8 -3 1080.20 58.23 -4 -8 3 1014.93 23.69 -4 -8 4 84.59 19.35 4 8 -4 59.43 19.24 4 -8 -4 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21.06 4 12 -27 162.94 21.91 4 12 -27 124.82 18.95 4 -12 -27 100.76 29.08 4 12 -28 81.86 23.23 4 -12 -28 121.16 16.64 4 -12 -28 53.63 21.41 -4 -12 28 48.67 20.50 4 -12 -28 55.85 28.58 4 12 -28 83.49 21.12 4 12 -29 109.63 24.32 4 -12 -29 195.99 20.34 4 12 -29 153.14 22.17 4 -12 -29 82.23 22.08 4 -12 -29 65.96 30.62 -4 -12 29 101.00 21.49 4 12 -30 54.86 18.99 -4 -12 30 59.85 20.97 4 -12 -30 34.17 22.02 4 -12 -30 59.54 30.25 4 -12 -30 85.83 18.86 4 12 -30 48.27 23.42 -4 -12 31 140.93 21.37 4 -12 -31 75.00 31.57 4 -12 -31 123.91 16.63 4 -12 -31 40.70 22.67 4 12 -31 107.09 22.27 4 12 -31 75.15 20.79 4 -12 -32 3.65 21.99 -4 -12 32 45.40 16.30 4 12 -32 35.33 22.83 4 -12 -32 39.91 19.97 4 12 -32 48.35 24.24 4 -12 -32 -21.59 30.30 4 -12 -33 0.94 32.45 4 -12 -33 120.45 21.28 -4 -12 33 145.42 22.61 4 -12 -33 -7.02 24.06 4 12 -33 69.03 18.63 4 12 -33 46.97 25.05 -4 -13 1 344.09 18.63 4 -13 -6 9.35 37.03 4 -13 -6 13.34 30.80 4 -13 -7 48.53 35.39 4 -13 -7 64.80 29.44 4 -13 -8 1009.86 40.02 4 -13 -8 898.11 49.54 -4 -13 8 1039.84 22.97 -4 -13 9 31.46 19.05 4 -13 -9 6.33 26.43 4 -13 -9 6.04 33.95 4 -13 -10 87.08 32.36 -4 -13 10 89.93 16.29 4 -13 -10 111.81 26.05 4 -13 -11 238.41 28.88 4 -13 -11 191.91 36.18 4 -13 -12 1339.61 36.83 4 -13 -12 989.50 47.51 4 -13 -13 78.07 24.09 4 -13 -13 72.69 30.83 4 -13 -14 60.49 22.07 4 -13 -14 26.26 29.41 4 -13 -15 1.48 21.41 4 -13 -15 18.64 30.11 -4 -13 16 201.02 17.08 4 -13 -16 174.44 24.06 4 -13 -16 103.76 29.30 -4 -13 16 205.21 16.84 4 -13 -17 454.15 26.28 4 -13 -17 243.71 30.44 4 -13 -18 27.55 21.65 4 -13 -18 -2.65 26.67 4 13 -19 453.51 22.83 4 -13 -19 189.84 33.34 4 -13 -19 366.84 25.61 4 -13 -20 62.13 22.48 4 13 -20 43.59 19.41 4 -13 -20 1.04 31.35 4 13 -21 260.80 21.21 4 -13 -21 178.72 21.84 4 -13 -21 141.07 29.11 4 -13 -22 30.07 20.23 4 -13 -22 8.69 29.41 4 13 -22 26.72 19.35 4 -13 -23 312.65 23.87 4 -13 -23 226.36 31.28 4 13 -23 387.61 22.65 4 -13 -24 91.12 23.58 4 -13 -24 50.41 28.41 4 13 -24 108.33 16.27 4 13 -25 9.33 21.31 4 -13 -25 9.16 19.64 -4 -13 25 37.63 19.54 4 -13 -25 21.86 31.61 4 13 -25 18.18 20.13 4 -13 -26 4.13 19.80 4 13 -26 57.79 22.26 4 13 -26 35.66 20.54 -4 -13 26 25.93 19.88 4 -13 -26 9.63 28.71 4 -13 -27 47.61 28.14 4 13 -27 57.07 22.89 4 13 -27 89.85 20.95 4 -13 -27 31.33 21.65 -4 -13 27 75.78 20.87 4 -13 -28 86.31 22.76 4 13 -28 104.62 24.60 4 13 -28 109.83 22.79 -4 -13 28 92.89 21.87 4 -13 -28 64.19 30.44 4 13 -29 67.09 23.70 4 -13 -29 126.95 19.77 4 13 -29 81.78 22.00 4 -13 -29 45.80 22.89 -4 -13 29 95.80 21.61 4 -13 -29 12.29 34.90 -4 -13 30 40.16 21.92 4 -13 -30 41.98 15.90 4 -13 -30 1.86 22.19 4 13 -30 43.97 22.21 4 -13 -30 13.46 30.01 4 13 -30 13.39 22.34 -4 -13 31 1.12 20.58 4 13 -31 24.92 17.86 4 -13 -31 7.64 22.47 4 -13 -31 26.88 19.33 4 13 -31 -2.79 22.94 4 -13 -31 123.58 31.57 4 13 -32 57.09 22.62 4 -13 -32 5.83 23.47 -4 -13 32 71.20 22.77 4 -13 -32 88.50 21.47 4 13 -32 -0.40 24.00 4 -13 -32 19.74 30.64 4 -14 -6 810.41 67.79 -4 -14 6 870.50 22.45 4 -14 -7 752.99 57.70 4 -14 -8 6.65 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20.93 23.36 2 6 -37 17.30 20.44 2 -6 -37 54.39 21.80 2 6 -37 42.41 21.11 2 -6 -38 22.83 23.19 2 6 -38 47.42 18.69 2 6 -38 17.60 16.95 2 -6 -38 -7.78 20.96 2 -6 -38 30.19 15.57 2 6 -38 21.43 24.42 2 -6 -39 -1.82 18.57 2 6 -39 48.89 18.98 2 -6 -39 58.82 16.30 2 6 -39 2.68 24.82 2 6 -39 35.56 21.52 2 -6 -39 4.48 23.91 2 -6 -40 -36.73 19.55 2 6 -40 133.21 23.41 2 -6 -40 213.42 21.52 2 6 -40 191.86 17.93 2 6 -40 8.72 22.01 2 -6 -40 65.98 25.10 -2 -7 1 1908.79 34.33 2 -7 -1 1919.63 59.43 -2 7 1 1964.90 73.48 2 7 -1 1965.05 35.74 2 7 -2 828.78 27.27 -2 -7 2 818.04 26.45 -2 7 2 783.80 48.58 2 -7 -2 762.67 40.43 2 -7 -3 3454.57 62.96 -2 -7 3 3409.81 42.21 2 7 -3 3408.94 43.13 -2 7 3 3482.02 73.37 -2 -7 4 632.28 24.46 2 -7 -4 629.86 33.42 2 7 -4 636.04 25.08 -2 7 4 603.63 37.69 2 7 -5 463.17 23.62 2 -7 -5 356.72 25.51 -2 7 5 333.82 32.69 -2 -7 5 390.04 19.90 -2 -7 5 450.92 23.27 2 -7 -6 4731.04 59.19 2 7 -6 4314.88 44.66 -2 -7 6 4394.83 44.74 -2 -7 6 4742.00 48.70 -2 7 6 4783.52 69.68 -2 -7 7 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600.33 24.80 -2 15 18 442.60 32.43 -2 15 19 6.30 27.65 -2 -15 19 27.65 14.97 2 -15 -19 33.41 18.50 2 15 -19 -9.05 23.66 -2 15 20 -4.41 27.02 2 -15 -20 3.12 19.03 2 15 -20 7.72 19.28 -2 15 21 30.95 26.74 2 -15 -21 15.84 19.07 2 15 -21 22.85 19.47 -2 15 22 269.37 29.70 2 15 -22 168.50 25.15 2 -15 -22 230.04 22.07 2 15 -22 262.02 24.53 2 15 -23 121.16 25.36 2 15 -23 214.67 22.21 -2 15 23 146.72 28.53 2 -15 -23 180.68 25.35 2 15 -24 26.72 23.03 -2 15 24 10.30 27.42 2 -15 -24 11.27 20.86 2 15 -24 13.59 20.70 2 -15 -25 -3.16 20.28 2 15 -25 30.42 20.18 -2 15 25 22.75 28.24 2 15 -25 18.43 26.42 -2 -15 26 43.87 20.61 2 -15 -26 10.03 21.17 2 15 -26 52.90 20.97 -2 15 26 24.23 27.36 2 15 -26 77.46 29.67 -2 -15 27 428.28 24.61 2 -15 -27 16.75 24.04 -2 15 27 218.71 32.63 2 15 -27 333.35 29.14 2 15 -27 312.92 30.65 2 -15 -28 -32.04 22.42 -2 -15 28 9.25 20.48 2 15 -28 -7.94 21.17 2 15 -28 16.38 25.40 2 -15 -29 37.61 22.13 -2 -15 29 41.37 17.40 2 15 -29 17.18 21.52 2 15 -29 31.54 26.37 2 -15 -30 12.03 21.16 2 -15 -30 14.12 22.21 2 15 -30 4.38 21.43 2 15 -30 34.55 26.50 -2 -15 30 -15.66 21.65 -2 16 1 169.73 44.24 -2 16 2 410.10 49.24 -2 -16 3 65.78 18.80 -2 16 3 14.79 37.70 -2 16 4 258.79 42.25 -2 16 5 11.44 37.30 -2 -16 6 190.13 20.99 -2 16 6 110.26 36.54 -2 16 7 114.85 37.89 -2 16 8 770.84 48.84 -2 16 9 28.28 31.04 2 -16 -10 5.34 22.19 -2 16 10 17.95 30.88 2 -16 -11 92.94 22.35 -2 16 11 82.22 31.28 2 -16 -12 278.90 27.61 -2 16 12 223.25 33.67 -2 16 13 322.08 37.12 2 -16 -13 426.96 27.24 2 -16 -14 21.15 22.15 2 16 -14 -23.82 23.14 -2 16 14 12.20 30.17 2 16 -15 10.04 19.55 2 -16 -15 26.27 23.83 -2 16 15 -0.32 30.30 -2 16 16 3.98 31.17 -2 -16 16 20.72 14.67 2 16 -16 14.31 22.82 2 -16 -16 7.68 20.51 2 16 -17 654.31 27.85 -2 -16 17 586.76 21.09 -2 16 17 371.02 34.48 2 -16 -17 578.92 29.30 -2 16 18 -6.47 27.20 2 -16 -18 -18.62 20.15 2 16 -18 -12.12 22.96 -2 16 19 101.64 29.19 2 16 -19 180.28 22.52 2 -16 -19 158.41 26.28 -2 16 20 8.20 27.40 2 16 -20 22.16 20.11 2 -16 -20 33.13 24.06 -2 16 21 155.41 32.81 2 16 -21 103.10 29.58 2 -16 -21 129.04 25.16 2 16 -21 153.75 25.33 2 -16 -22 56.34 23.68 -2 16 22 -4.13 28.23 2 16 -22 4.74 28.44 2 16 -22 25.14 25.21 2 16 -23 85.77 28.57 2 -16 -23 50.90 21.42 2 16 -23 82.20 25.61 -2 16 23 49.01 28.30 2 -16 -24 29.01 23.28 -2 16 24 70.98 30.41 2 16 -24 152.78 26.75 2 16 -24 131.98 30.55 -2 16 25 7.95 27.12 -2 -16 25 8.57 21.04 2 16 -25 14.79 23.55 2 -16 -25 10.59 23.90 2 16 -25 33.11 28.11 2 -16 -26 -3.36 22.44 -2 16 26 34.60 29.12 -2 -16 26 77.22 21.37 2 16 -26 66.87 21.67 2 16 -26 10.63 30.77 2 -16 -27 -5.72 22.00 -2 -16 27 -7.22 17.39 2 16 -27 19.69 21.90 2 16 -27 30.95 26.56 2 -16 -28 -28.78 24.04 -2 -16 28 161.13 23.92 2 16 -28 90.48 24.08 2 16 -28 80.62 29.32 -2 17 1 23.99 44.63 -2 17 2 175.09 47.59 -2 17 3 463.71 52.22 -2 17 4 5.80 39.55 -2 17 5 14.24 34.57 -2 17 6 6.73 38.56 -2 17 7 356.50 43.80 -2 17 8 46.34 35.76 2 -17 -9 128.08 28.09 -2 17 9 115.72 32.96 2 -17 -10 0.61 22.69 -2 17 10 0.48 30.43 -2 -17 10 14.02 15.66 2 -17 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30.67 -2 17 25 8.02 28.96 2 17 -25 6.34 22.15 -2 -17 25 2.11 17.55 2 17 -25 -0.29 31.03 2 -17 -25 17.20 21.95 2 18 -1 29.60 26.42 2 -18 -1 42.03 44.40 -2 18 1 30.07 48.93 2 18 -2 372.19 30.14 -2 18 2 249.47 52.09 2 18 -3 57.03 26.70 -2 18 3 29.19 42.13 -2 18 4 240.14 46.58 -2 18 5 11.15 39.94 -2 18 6 94.19 40.47 2 18 -7 91.67 25.45 -2 18 7 3.09 33.28 2 18 -8 512.07 30.95 -2 18 8 234.83 42.11 -2 18 9 70.26 38.09 2 18 -9 174.53 24.45 2 -18 -9 170.57 29.82 2 18 -10 12.90 21.49 2 -18 -10 10.26 25.74 -2 18 10 25.69 31.32 -2 18 11 3.03 34.04 2 -18 -11 16.78 22.72 2 18 -11 -16.44 25.38 2 18 -12 117.03 26.63 2 -18 -12 137.31 25.70 -2 18 12 68.13 33.30 2 18 -13 344.77 29.47 2 -18 -13 252.47 31.94 -2 18 13 155.95 36.88 2 18 -14 32.08 25.00 -2 18 14 26.87 31.54 2 -18 -14 16.11 27.14 2 18 -15 -1.96 21.47 2 -18 -15 28.53 24.00 -2 18 15 18.23 31.10 -2 18 16 0.10 32.00 2 18 -16 -7.26 25.43 2 -18 -16 10.00 24.43 -2 18 17 49.79 29.68 2 18 -17 131.90 23.93 2 -18 -17 92.65 27.22 -2 18 18 34.35 32.30 2 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14.44 0 5 -26 199.36 16.23 0 5 27 26.40 19.59 0 -5 27 4.55 15.69 0 -5 -27 12.77 15.69 0 -5 -27 8.88 19.16 0 5 -27 3.31 15.83 0 5 -27 -16.93 16.43 0 5 -27 -2.71 16.60 0 5 28 -13.83 19.88 0 -5 28 1.25 12.31 0 -5 -28 8.26 15.38 0 5 -28 14.40 15.26 0 -5 -28 3.00 12.29 0 5 -28 9.54 21.23 0 5 -28 7.39 17.16 0 5 29 26.75 16.27 0 -5 29 46.26 15.92 0 -5 -29 33.83 15.49 0 -5 -29 39.24 19.39 0 5 -29 40.48 15.58 0 5 -29 18.97 21.03 0 5 -29 41.10 17.41 0 -5 30 573.41 19.66 0 -5 -30 537.21 16.99 0 -5 -30 514.68 23.72 0 5 30 362.01 20.93 0 5 -30 531.35 16.77 0 5 -30 497.77 25.81 0 5 -30 387.33 18.66 0 5 31 112.50 17.93 0 -5 -31 173.18 16.85 0 -5 31 168.55 14.65 0 -5 -31 101.59 17.71 0 5 -31 179.60 14.76 0 5 -31 147.37 19.42 0 5 -31 196.68 18.92 0 5 32 105.24 17.39 0 -5 -32 210.76 16.88 0 -5 32 186.38 16.97 0 5 -32 160.97 14.28 0 5 -32 92.97 19.38 0 5 -32 113.25 15.95 0 -5 -32 115.55 20.45 0 -5 -33 170.59 19.10 0 5 33 157.75 18.79 0 -5 -33 232.33 15.31 0 -5 33 282.97 18.32 0 5 -33 150.24 24.83 0 5 -33 308.30 18.53 0 5 -33 168.51 20.51 0 -5 34 657.02 18.98 0 -5 -34 762.85 19.45 0 -5 -34 509.23 26.09 0 5 -34 752.66 18.56 0 5 -34 388.37 29.01 0 5 -34 549.54 24.72 0 -5 -35 79.31 17.39 0 -5 35 68.45 13.82 0 -5 -35 37.84 17.29 0 5 -35 70.82 17.76 0 5 -35 67.10 23.87 0 5 -35 63.24 19.59 0 5 -36 171.47 25.82 0 -5 -36 136.81 24.20 0 5 -36 336.88 20.28 0 -5 -36 371.98 19.03 0 5 -36 205.44 19.86 0 5 -37 -0.27 14.42 0 -5 -37 32.07 18.10 0 -5 -37 33.44 15.13 0 -5 -37 39.34 21.88 0 5 -37 22.40 24.83 0 5 -37 21.56 19.82 0 5 -38 72.71 16.25 0 5 -38 141.42 19.44 0 -5 -38 92.36 16.11 0 -5 -38 55.63 19.22 0 -5 -38 64.60 23.26 0 5 -38 36.36 25.97 0 5 -39 20.43 20.02 0 -5 -39 24.12 22.57 0 -5 -39 1.52 22.43 0 -5 -39 72.23 18.53 0 5 -39 61.81 15.88 0 5 -39 42.04 22.18 0 5 -40 167.49 21.96 0 -5 -40 114.77 20.40 0 5 -40 8.05 22.86 0 5 -40 213.68 21.49 0 -5 -40 74.13 24.64 0 -5 -40 183.81 20.58 0 -5 -41 72.60 23.99 0 5 -41 10.69 16.96 0 -5 -41 16.93 19.71 0 5 -41 17.35 21.40 0 5 -41 23.42 15.71 0 -5 -41 13.84 19.11 0 6 0 9566.77 96.69 0 -6 0 9380.83 89.92 0 6 -1 182.59 29.35 0 6 1 186.97 30.74 0 -6 -1 184.09 27.27 0 -6 1 168.74 26.80 0 -6 2 14.70 24.05 0 6 2 7.11 22.87 0 -6 -2 4.95 25.59 0 6 -2 20.57 23.04 0 -6 -3 1976.79 42.68 0 6 3 1950.62 44.28 0 6 -3 1953.63 46.88 0 -6 3 1918.36 43.92 0 -6 -4 2606.92 46.20 0 6 4 2638.47 48.92 0 6 -4 2500.23 47.61 0 -6 4 2502.29 36.22 0 -6 4 2597.00 48.33 0 -6 5 420.28 26.51 0 -6 -5 403.45 25.79 0 6 -5 400.27 27.59 0 6 5 403.02 28.83 0 -6 5 417.79 22.85 0 -6 6 123.58 25.33 0 -6 -6 120.47 21.79 0 6 -6 131.06 21.36 0 6 6 196.23 25.24 0 -6 6 114.79 19.16 0 6 -7 1080.25 33.13 0 -6 -7 1111.92 31.07 0 -6 7 1084.61 26.90 0 6 7 1132.29 33.39 0 -6 7 1113.15 33.02 0 -6 8 409.03 21.81 0 6 -8 362.36 23.14 0 -6 8 369.04 24.62 0 -6 -8 401.82 24.55 0 6 8 410.74 26.65 0 -6 -9 2.31 16.40 0 -6 9 11.20 18.58 0 6 9 6.20 18.39 0 -6 9 6.02 17.61 0 6 -9 -2.63 17.14 0 -6 -10 1181.02 27.02 0 -6 10 1263.83 26.15 0 6 -10 1203.78 23.86 0 6 10 1275.28 32.75 0 6 -10 1241.72 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33.73 0 -6 -20 2312.53 28.21 0 6 -20 2628.57 30.42 0 -6 -20 2323.19 32.52 0 -6 20 2521.21 29.80 0 6 -20 2484.32 38.25 0 6 20 2549.35 37.22 0 -6 -21 640.00 24.22 0 6 -21 513.53 19.42 0 -6 -21 640.18 20.20 0 6 -21 569.47 17.67 0 6 -21 550.99 25.85 0 -6 21 588.74 19.51 0 6 21 570.94 26.38 0 -6 -22 -3.84 18.94 0 -6 -22 27.41 14.93 0 6 -22 37.96 15.59 0 -6 22 21.56 12.92 0 6 -22 6.51 19.84 0 6 22 12.51 16.37 0 6 -22 10.68 17.34 0 -6 -23 1153.80 26.00 0 6 -23 1000.31 29.65 0 -6 -23 1163.10 22.48 0 -6 23 1053.31 19.82 0 6 -23 1124.85 22.40 0 6 23 1113.63 27.72 0 6 -23 1136.00 25.82 0 6 24 1274.43 29.62 0 -6 -24 1266.67 21.32 0 -6 24 1473.64 23.87 0 -6 -24 1216.65 25.11 0 6 -24 1256.20 21.38 0 6 -24 1354.72 31.11 0 6 -24 1342.29 27.01 0 -6 -25 55.88 15.86 0 -6 25 61.82 15.66 0 -6 -25 17.96 16.45 0 6 -25 26.78 17.28 0 6 -25 29.83 17.53 0 6 -25 49.07 16.09 0 6 25 23.64 17.32 0 -6 26 1048.91 20.18 0 -6 -26 892.02 24.47 0 -6 -26 1069.82 20.58 0 6 -26 1144.07 22.99 0 6 -26 998.60 30.66 0 6 26 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1 1415.87 37.72 0 -7 -1 1357.98 35.23 0 -7 2 525.42 26.59 0 7 2 535.30 28.49 0 -7 -2 563.10 29.51 0 7 -2 554.36 30.17 0 7 3 24.09 22.14 0 7 -3 1.92 23.02 0 -7 -3 2.97 19.83 0 -7 3 7.86 22.29 0 -7 -4 8.10 20.18 0 7 4 11.16 25.91 0 7 -4 11.94 18.97 0 -7 4 4.69 22.34 0 -7 -5 170.90 21.54 0 7 5 164.64 28.08 0 -7 5 181.46 24.55 0 7 -5 154.99 21.56 0 -7 5 244.19 21.24 0 -7 -6 4949.08 54.69 0 -7 6 5045.34 61.65 0 7 -6 4618.91 56.58 0 7 6 5035.13 58.76 0 -7 6 4946.25 46.95 0 7 7 1951.80 40.67 0 -7 -7 1943.98 36.75 0 7 -7 1907.23 38.70 0 -7 7 1949.08 31.25 0 -7 7 1968.61 40.82 0 7 -8 40.40 17.87 0 7 8 35.60 22.21 0 -7 8 43.51 21.93 0 -7 8 36.20 14.36 0 7 -9 232.09 19.93 0 -7 9 382.10 21.30 0 7 9 293.35 24.89 0 -7 9 248.15 21.98 0 7 -10 6328.40 59.29 0 -7 -10 6371.18 56.71 0 -7 10 6745.96 65.61 0 -7 10 6501.00 49.03 0 7 10 6270.09 59.11 0 -7 11 1152.92 25.31 0 -7 -11 1168.31 28.62 0 -7 11 1228.19 31.44 0 7 11 1182.39 30.80 0 7 -11 1100.19 28.73 0 -7 12 149.25 21.42 0 -7 -12 131.33 19.45 0 -7 12 126.64 17.18 0 7 12 140.73 21.99 0 7 -12 141.34 19.47 0 -7 13 1894.20 28.32 0 -7 -13 1766.97 31.40 0 7 13 1908.51 34.97 0 7 -13 1757.23 32.27 0 7 -14 1630.44 37.40 0 -7 -14 1643.27 30.15 0 -7 14 1698.35 27.00 0 7 -14 1614.11 31.36 0 7 14 1682.25 32.76 0 7 -15 -3.22 18.83 0 -7 15 -4.46 13.82 0 7 -15 5.17 17.26 0 7 15 6.81 20.11 0 -7 -15 -0.46 17.81 0 7 -16 395.50 23.97 0 -7 -16 409.91 20.93 0 -7 16 366.38 16.60 0 7 -16 371.30 20.28 0 7 16 364.05 20.39 0 7 17 726.35 26.00 0 -7 17 715.15 21.22 0 7 -17 701.83 23.10 0 -7 -17 638.11 20.23 0 7 -17 679.64 18.91 0 7 -17 650.27 25.84 0 -7 -18 579.42 23.54 0 -7 18 520.02 17.86 0 7 -18 580.06 21.87 0 7 -18 533.30 18.30 0 7 18 528.59 22.44 0 7 -18 507.32 24.88 0 7 -19 411.00 20.25 0 -7 -19 358.76 18.96 0 7 -19 418.00 17.41 0 7 19 414.03 24.09 0 -7 19 407.26 16.80 0 7 -19 355.97 20.32 0 7 20 745.89 24.24 0 7 -20 760.20 22.93 0 -7 20 714.23 18.57 0 -7 -20 760.63 25.01 0 7 -20 798.77 21.79 0 7 -20 756.99 28.09 0 7 21 66.08 21.30 0 7 -21 56.48 18.23 0 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0 8 -4 1313.89 34.51 0 -8 -4 1300.40 32.45 0 8 5 86.41 23.70 0 -8 5 94.89 21.40 0 -8 5 105.44 14.83 0 8 -5 91.44 21.55 0 -8 -5 100.98 23.87 0 -8 -6 66.31 19.47 0 8 6 54.73 25.56 0 -8 6 82.03 18.76 0 -8 6 73.46 18.01 0 8 -6 72.40 20.10 0 8 7 135.95 23.15 0 8 -7 120.00 21.82 0 -8 7 124.04 18.91 0 -8 7 141.48 22.12 0 8 -8 713.33 27.34 0 -8 8 670.59 20.89 0 -8 8 753.06 27.19 0 8 8 683.65 28.78 0 -8 9 581.56 28.08 0 8 -9 530.02 26.53 0 -8 9 480.10 18.03 0 8 9 554.79 27.03 0 8 -10 459.60 23.00 0 -8 10 445.61 20.34 0 8 10 475.18 23.42 0 -8 10 499.79 27.50 0 -8 -10 456.49 23.46 0 -8 11 87.11 20.35 0 -8 -11 76.18 19.81 0 -8 11 45.28 17.40 0 8 11 83.00 23.23 0 -8 12 702.01 26.93 0 -8 -12 659.50 24.73 0 -8 12 649.78 19.34 0 8 12 694.51 27.94 0 -8 -13 15.80 15.00 0 -8 13 6.06 14.07 0 8 13 18.33 20.43 0 8 14 48.61 20.48 0 -8 -14 75.65 17.90 0 -8 14 66.76 17.43 0 8 -15 10.00 19.77 0 8 15 12.71 16.12 0 -8 -15 14.59 17.48 0 -8 15 19.34 14.03 0 8 -15 22.68 19.45 0 8 -16 753.61 29.80 0 -8 -16 768.45 24.06 0 8 16 742.09 27.11 0 8 -16 775.32 23.79 0 8 -17 1215.94 30.97 0 -8 -17 1115.45 24.49 0 8 17 1239.19 29.42 0 8 -17 1203.72 27.25 0 8 -17 1195.22 22.54 0 8 -18 5.02 20.11 0 -8 -18 -4.15 18.71 0 -8 18 19.70 14.84 0 8 -18 11.19 15.05 0 8 -18 -4.37 17.40 0 8 18 17.04 17.60 0 8 -19 87.23 17.51 0 8 -19 76.65 15.38 0 -8 -19 70.35 20.25 0 8 19 73.09 22.63 0 -8 19 62.48 14.39 0 8 -19 62.79 20.96 0 -8 -20 1520.23 30.32 0 8 -20 1705.38 30.33 0 8 -20 1632.62 24.74 0 8 20 1497.14 31.18 0 8 -20 1606.41 34.68 0 8 -21 1171.40 26.65 0 8 -21 1248.62 24.20 0 -8 -21 1034.94 24.36 0 8 21 1095.34 29.00 0 8 -21 1005.77 30.36 0 -8 -22 47.58 19.05 0 8 -22 70.89 18.12 0 8 -22 67.26 16.88 0 8 -22 50.86 21.78 0 8 22 40.54 21.58 0 8 -23 385.91 20.24 0 8 -23 403.39 17.04 0 -8 -23 351.15 22.12 0 8 -23 369.96 24.78 0 8 23 314.88 20.85 0 -8 -24 743.03 20.76 0 8 -24 731.82 21.43 0 -8 24 672.85 18.04 0 -8 -24 544.51 24.83 0 8 -24 618.14 23.15 0 8 -24 553.40 27.70 0 8 24 661.16 26.12 0 8 25 64.38 21.41 0 -8 25 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39.40 0 -9 11 1922.30 29.52 0 9 11 1886.77 36.56 0 -9 -12 496.32 19.76 0 -9 12 529.54 19.27 0 -9 12 589.48 26.52 0 9 12 572.02 26.22 0 -9 13 1643.75 35.21 0 -9 -13 1558.22 29.26 0 -9 13 1637.00 28.27 0 9 13 1567.60 33.13 0 -9 -14 1704.07 27.81 0 9 14 1940.16 34.41 0 9 -15 63.40 18.37 0 9 -15 47.84 20.97 0 -9 -15 77.10 18.39 0 9 15 66.80 21.83 0 9 -16 399.55 24.88 0 -9 -16 404.73 20.40 0 9 16 367.17 20.54 0 -9 16 370.06 17.70 0 9 -16 418.49 21.55 0 9 -17 563.03 29.17 0 -9 -17 537.42 20.02 0 9 17 598.85 25.88 0 9 -17 616.38 25.32 0 -9 -18 738.09 21.65 0 9 18 799.61 27.93 0 9 -18 918.86 25.30 0 9 -18 865.37 29.21 0 -9 19 716.34 18.80 0 -9 -19 703.69 23.43 0 9 -19 684.64 27.08 0 9 19 673.26 27.89 0 9 -19 699.33 23.39 0 -9 -20 146.99 16.85 0 -9 20 176.38 15.12 0 9 -20 185.02 18.38 0 9 -20 153.30 21.21 0 9 20 143.20 21.92 0 9 -20 162.58 21.02 0 9 -21 143.77 20.68 0 -9 -21 94.77 19.59 0 9 -21 135.94 21.60 0 -9 21 140.47 15.30 0 9 -21 149.71 18.04 0 9 21 145.94 22.72 0 -9 -22 294.62 18.51 0 9 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47.50 16.04 0 9 -36 33.91 26.90 0 -9 37 158.93 21.17 0 -9 -37 151.79 20.89 0 -9 -37 50.28 24.16 0 9 -37 67.13 29.39 0 9 -37 172.26 20.86 0 9 -37 114.13 18.42 0 -9 38 32.37 19.90 0 -9 -38 16.91 19.23 0 -9 -38 30.14 16.60 0 9 -38 -0.55 28.83 0 9 -38 27.59 20.53 0 9 -38 50.22 22.04 0 10 0 1357.81 37.86 0 -10 0 1328.43 33.90 0 -10 1 1393.50 34.17 0 10 -1 1386.98 35.43 0 10 1 1441.51 38.46 0 -10 -1 1435.91 34.56 0 -10 2 205.00 23.78 0 10 -2 232.67 27.82 0 10 2 224.50 27.78 0 -10 -2 189.21 23.58 0 10 -3 2172.70 42.94 0 10 3 2136.46 40.80 0 -10 -3 2060.57 36.68 0 -10 3 2156.18 40.48 0 10 -4 1501.09 37.46 0 10 4 1491.37 36.40 0 -10 4 1605.55 37.96 0 -10 -4 1481.97 32.68 0 -10 5 98.57 18.66 0 -10 5 60.56 19.57 0 10 5 60.67 24.07 0 -10 -5 48.43 23.69 0 10 -5 57.22 23.52 0 -10 6 406.10 21.50 0 -10 6 380.58 25.92 0 10 6 364.08 26.38 0 10 -6 352.23 24.42 0 -10 -6 328.40 21.57 0 -10 7 977.83 32.77 0 10 7 910.11 31.28 0 -10 7 872.22 21.97 0 10 -7 848.91 29.20 0 -10 -7 846.42 26.95 0 -10 -8 1938.71 34.08 0 -10 8 1768.95 26.63 0 10 -8 1791.37 35.18 0 -10 8 1972.23 37.77 0 10 8 1985.85 38.53 0 -10 -9 543.80 23.25 0 -10 9 614.97 28.23 0 -10 9 548.81 21.95 0 10 9 583.52 26.87 0 10 -9 526.86 26.30 0 -10 -10 -3.54 18.21 0 10 10 30.47 21.70 0 -10 10 -9.49 18.93 0 -10 10 -4.20 18.70 0 -10 -11 241.38 20.51 0 -10 11 197.92 16.99 0 10 11 253.87 24.16 0 -10 -12 964.45 25.64 0 10 12 951.55 29.68 0 -10 12 975.66 24.24 0 -10 -13 11.39 17.66 0 10 13 11.40 21.02 0 -10 13 14.00 14.45 0 -10 -14 -5.42 16.63 0 -10 14 -9.49 17.45 0 10 14 9.73 20.49 0 -10 -15 128.95 15.97 0 -10 15 144.51 15.19 0 10 15 143.12 18.35 0 10 -16 475.23 24.50 0 -10 -16 447.33 21.58 0 10 16 479.47 25.27 0 10 -17 1131.54 29.00 0 -10 -17 1128.68 26.56 0 10 -17 1097.76 33.38 0 10 17 1029.36 30.86 0 10 -18 220.47 23.34 0 10 -18 259.72 20.05 0 -10 -18 207.99 15.92 0 10 18 206.57 22.47 0 -10 -19 189.82 20.22 0 -10 19 223.45 15.99 0 10 -19 216.34 22.50 0 10 19 225.14 23.59 0 10 -19 218.28 22.67 0 -10 -20 490.99 21.93 0 10 20 448.87 26.41 0 -10 20 552.34 18.82 0 10 -20 512.32 25.66 0 10 -20 506.32 21.67 0 -10 -21 417.94 20.17 0 -10 21 499.63 18.10 0 10 21 481.82 22.85 0 10 -21 554.58 27.40 0 10 -21 563.83 23.10 0 -10 -22 429.87 22.70 0 10 22 386.55 26.15 0 10 -22 346.83 26.08 0 10 -22 390.77 21.82 0 -10 -23 748.67 26.69 0 10 -23 829.99 34.38 0 10 23 766.01 30.18 0 10 -23 971.97 25.64 0 -10 -24 595.06 21.14 0 10 -24 637.65 24.05 0 10 -24 631.33 30.22 0 10 24 595.51 24.15 0 -10 -25 -10.68 18.58 0 -10 25 34.77 17.62 0 10 25 -3.71 22.14 0 10 -25 15.62 22.64 0 10 -25 21.59 17.73 0 -10 -26 113.71 16.60 0 -10 -26 96.74 20.76 0 -10 26 109.11 18.64 0 10 -26 47.05 27.29 0 10 -26 130.71 18.75 0 10 -26 79.40 18.56 0 10 26 102.35 23.07 0 -10 -27 604.26 20.71 0 -10 -27 473.82 24.43 0 -10 27 586.25 18.50 0 10 -27 635.40 21.73 0 10 -27 325.97 28.38 0 10 -27 565.93 23.89 0 10 27 451.06 24.28 0 -10 -28 419.98 17.26 0 -10 -28 258.31 22.63 0 10 28 271.36 21.62 0 -10 28 356.75 18.93 0 10 -28 422.15 17.32 0 10 -28 215.54 31.61 0 10 -28 317.29 24.89 0 -10 -29 115.18 17.86 0 -10 -29 102.22 20.55 0 -10 29 127.44 18.53 0 10 -29 114.46 16.07 0 10 -29 45.54 24.37 0 10 -29 101.45 19.51 0 10 29 57.18 23.70 0 10 30 61.29 24.03 0 -10 -30 62.11 21.41 0 -10 -30 63.01 17.05 0 10 -30 96.16 17.79 0 -10 30 58.78 15.35 0 10 -30 51.50 27.36 0 10 -30 39.60 18.70 0 10 31 17.00 23.47 0 -10 -31 33.00 13.55 0 -10 31 33.57 18.03 0 10 -31 36.66 17.60 0 -10 -31 9.21 20.32 0 10 -31 3.65 25.25 0 10 -31 -1.56 19.35 0 10 32 46.33 22.85 0 -10 32 39.98 15.42 0 -10 -32 47.80 17.32 0 -10 -32 26.53 21.01 0 10 -32 93.02 18.73 0 10 -32 6.19 24.92 0 10 -32 -12.46 19.26 0 10 33 65.18 20.28 0 -10 -33 64.08 18.05 0 -10 33 92.35 19.50 0 10 -33 103.83 18.69 0 10 -33 54.41 25.11 0 -10 -33 79.02 14.80 0 10 -33 40.72 20.22 0 10 34 141.03 21.32 0 -10 34 127.47 17.43 0 -10 -34 127.78 19.72 0 -10 -34 58.37 19.07 0 10 -34 156.18 19.94 0 10 -34 0.34 27.46 0 10 -34 44.61 21.38 0 -10 -35 20.65 14.51 0 10 35 0.95 19.99 0 -10 35 -16.23 18.51 0 10 -35 20.19 18.90 0 -10 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23.46 0 -11 8 167.31 19.65 0 -11 8 154.29 23.69 0 -11 9 254.21 16.77 0 -11 9 294.70 25.50 0 11 9 289.46 25.03 0 -11 -10 352.36 21.78 0 -11 10 402.13 26.45 0 -11 10 397.90 20.03 0 11 10 340.66 25.55 0 -11 -11 432.00 22.30 0 -11 11 404.56 17.37 0 11 11 420.57 25.75 0 -11 11 433.17 24.12 0 -11 -12 402.22 21.94 0 -11 12 461.48 24.45 0 -11 12 546.15 22.24 0 11 12 383.28 25.42 0 -11 -13 2543.01 36.50 0 -11 13 2959.86 44.50 0 -11 13 2528.34 29.51 0 11 13 2882.81 42.79 0 -11 -14 1363.47 29.62 0 11 14 1277.62 34.21 0 -11 -15 -10.01 18.96 0 11 15 23.96 21.89 0 11 -16 262.01 25.87 0 -11 -16 272.80 20.91 0 11 -16 286.82 22.62 0 11 16 288.34 24.96 0 -11 16 279.32 16.47 0 11 -17 1295.54 33.04 0 -11 -17 1257.26 27.38 0 11 -17 1279.61 30.60 0 11 17 1018.66 27.39 0 -11 17 1175.72 22.81 0 11 -18 1277.49 36.92 0 -11 -18 1306.16 27.47 0 11 -18 1327.43 29.42 0 11 18 1239.70 32.94 0 11 -19 118.26 21.59 0 -11 -19 110.05 16.01 0 11 19 124.54 19.40 0 11 -19 81.26 26.15 0 11 -20 89.76 18.08 0 -11 -20 76.38 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70.11 19.93 0 11 29 27.39 19.60 0 -11 -30 190.25 18.33 0 -11 -30 140.47 21.72 0 -11 30 172.22 19.48 0 11 30 140.52 20.69 0 11 -30 76.93 26.57 0 11 -30 91.44 20.26 0 -11 -31 105.84 18.99 0 -11 -31 62.95 22.23 0 -11 31 161.29 16.58 0 11 31 55.41 25.18 0 11 -31 45.38 26.44 0 11 -31 114.17 20.87 0 11 32 13.93 24.97 0 -11 -32 60.06 14.87 0 -11 -32 15.67 22.10 0 -11 32 60.78 19.98 0 11 -32 16.89 26.36 0 11 -32 50.89 20.76 0 11 33 101.34 26.27 0 -11 -33 122.40 23.94 0 -11 33 164.37 17.54 0 11 -33 53.63 27.54 0 -11 -33 179.67 19.86 0 11 -33 164.37 21.97 0 11 34 62.60 26.24 0 -11 -34 119.83 16.34 0 -11 -34 38.73 23.49 0 11 -34 68.29 27.35 0 -11 34 129.93 20.60 0 11 -34 103.87 21.31 0 11 35 -11.64 21.55 0 -11 35 20.97 17.00 0 -11 -35 35.79 19.46 0 -11 -35 -1.15 19.32 0 11 -35 4.24 26.78 0 11 -35 5.89 20.80 0 11 36 -5.88 20.66 0 -11 -36 7.51 23.08 0 -11 -36 14.46 19.30 0 11 -36 51.57 27.66 0 -11 36 12.12 19.87 0 11 -36 0.71 20.65 0 -12 0 1244.78 32.55 0 -12 1 195.13 20.77 0 12 -1 199.58 23.78 0 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270.97 16.28 0 12 -18 277.87 25.22 0 -12 -18 256.43 20.32 0 12 -18 266.47 20.70 0 12 18 233.17 25.40 0 -12 -19 228.17 20.63 0 12 -19 216.96 23.44 0 -12 19 263.32 15.81 0 12 19 181.27 21.34 0 12 -19 188.52 26.35 0 -12 -20 258.06 18.64 0 12 -20 339.85 20.35 0 -12 20 296.25 16.97 0 12 20 358.25 25.97 0 12 -20 306.84 29.11 0 -12 -21 178.41 20.98 0 -12 21 212.57 16.85 0 12 -21 226.98 20.55 0 12 21 206.26 25.25 0 12 -21 238.05 27.86 0 -12 -22 9.21 19.09 0 12 -22 4.72 18.22 0 12 22 36.67 18.59 0 12 -22 25.93 26.33 0 -12 -23 689.10 27.06 0 12 -23 991.39 27.58 0 12 -23 986.47 33.42 0 12 23 883.91 31.04 0 -12 -24 61.07 20.06 0 12 -24 88.19 20.20 0 12 24 51.31 24.63 0 12 -24 54.84 24.53 0 12 25 19.27 19.12 0 -12 25 15.92 17.72 0 12 -25 7.01 18.82 0 -12 -25 21.34 19.73 0 12 -25 14.56 26.45 0 12 -26 30.46 21.92 0 -12 -26 17.02 16.51 0 -12 26 50.45 14.84 0 12 -26 22.96 24.36 0 12 26 30.94 23.99 0 12 -27 264.16 22.01 0 -12 -27 298.75 23.13 0 -12 27 324.60 17.38 0 12 -27 184.92 27.15 0 12 27 253.48 27.00 0 -12 -28 112.24 15.66 0 12 -28 116.42 20.54 0 -12 -28 99.29 22.09 0 -12 28 131.61 19.38 0 12 -28 81.01 29.96 0 12 28 72.73 25.73 0 12 -29 45.18 19.73 0 -12 -29 76.79 17.79 0 -12 -29 40.33 21.43 0 -12 29 91.34 19.28 0 12 -29 22.44 24.55 0 12 29 23.91 20.53 0 12 30 56.83 21.47 0 -12 -30 78.74 21.58 0 12 -30 93.66 20.35 0 -12 30 62.81 16.28 0 12 -30 44.19 30.13 0 -12 -30 84.52 18.60 0 12 31 3.76 23.46 0 -12 -31 4.04 14.82 0 -12 -31 -7.35 20.48 0 -12 31 8.96 18.06 0 12 -31 -2.79 24.43 0 12 -31 14.05 19.46 0 12 32 86.50 27.94 0 12 -32 88.06 21.77 0 -12 -32 147.68 19.99 0 -12 -32 47.30 24.36 0 -12 32 172.91 18.06 0 12 -32 94.02 32.20 0 12 -33 33.97 21.45 0 -12 -33 51.42 14.84 0 -12 -33 20.01 22.68 0 -12 33 31.29 20.77 0 12 33 31.21 26.01 0 12 -33 1.91 27.88 0 12 34 46.45 25.52 0 12 -34 38.38 24.62 0 -12 -34 2.80 22.33 0 -12 -34 46.79 19.17 0 -12 34 15.13 21.00 0 12 -34 -16.79 27.99 0 12 -35 49.98 24.34 0 -12 -35 7.94 19.77 0 -12 -35 9.51 15.58 0 -12 35 -14.43 16.90 0 12 35 -7.60 26.65 0 12 -35 21.83 27.98 0 -13 0 14.46 20.02 0 -13 1 165.00 22.47 0 -13 -1 128.97 21.59 0 -13 -2 1093.53 30.17 0 -13 2 1101.48 30.99 0 -13 -3 418.24 22.18 0 -13 3 472.42 26.13 0 -13 -4 237.65 22.37 0 -13 4 275.97 22.24 0 -13 5 142.44 26.90 0 13 5 -6.37 21.72 0 -13 -5 37.15 18.29 0 13 6 1177.21 33.30 0 -13 6 1090.06 23.36 0 -13 6 1355.81 36.13 0 -13 -6 1095.74 28.63 0 -13 7 1664.59 36.71 0 -13 8 101.73 24.57 0 13 9 223.15 27.23 0 -13 9 242.44 16.24 0 -13 10 433.96 17.82 0 13 10 426.69 27.22 0 13 11 524.83 28.03 0 13 12 46.05 22.90 0 -13 -12 15.56 21.33 0 13 13 1523.95 37.11 0 -13 -13 1430.30 29.72 0 -13 -14 267.10 20.41 0 13 14 259.59 24.72 0 -13 14 239.84 15.96 0 -13 -15 4.44 17.67 0 13 15 9.47 21.81 0 -13 15 17.04 13.50 0 -13 -16 15.03 17.52 0 13 -16 6.76 23.45 0 13 16 7.55 17.65 0 13 -16 -0.27 16.61 0 -13 16 -3.59 13.81 0 13 -17 761.60 29.83 0 -13 -17 729.33 24.71 0 -13 17 695.14 19.51 0 13 -17 803.06 27.80 0 13 17 717.56 28.67 0 13 -18 170.40 27.17 0 -13 -18 188.38 19.83 0 13 -18 201.84 20.74 0 -13 18 205.55 16.37 0 13 18 168.08 24.21 0 -13 -19 64.39 19.71 0 -13 19 65.92 15.49 0 13 -19 90.78 21.93 0 13 19 67.36 23.88 0 13 -19 68.37 26.19 0 -13 -20 223.11 19.96 0 13 -20 210.60 23.79 0 -13 20 197.16 16.83 0 13 20 169.06 24.33 0 13 -20 170.81 28.85 0 -13 -21 25.43 15.72 0 13 -21 3.53 18.82 0 13 21 4.49 18.97 0 13 -21 -11.51 26.73 0 -13 -22 226.61 21.70 0 13 22 289.63 25.85 0 13 -22 351.23 24.75 0 13 -22 278.54 31.26 0 -13 -23 46.66 19.52 0 13 -23 18.51 22.03 0 13 -23 19.86 27.64 0 13 23 44.20 24.41 0 -13 -24 130.94 20.07 0 13 -24 141.10 23.25 0 13 -24 77.30 25.19 0 13 24 107.54 25.32 0 -13 -25 64.94 20.14 0 13 -25 28.29 22.00 0 -13 25 -12.88 18.34 0 13 -25 4.50 23.90 0 13 25 -0.75 18.87 0 -13 -26 175.15 22.39 0 13 -26 242.33 24.97 0 -13 26 249.09 17.06 0 13 -26 136.97 31.74 0 13 26 146.40 26.49 0 -13 -27 27.70 17.61 0 13 -27 44.46 20.87 0 13 -27 43.71 25.82 0 -13 27 58.77 19.42 0 13 27 -3.06 23.89 0 -13 -28 51.98 15.57 0 -13 -28 33.71 21.65 0 13 -28 58.00 24.68 0 -13 28 68.54 19.61 0 13 -28 11.93 25.39 0 13 28 -3.19 25.90 0 -13 -29 32.51 18.20 0 -13 -29 -5.67 21.83 0 13 -29 56.42 20.24 0 13 29 44.55 20.34 0 -13 29 38.11 15.63 0 13 -29 42.65 30.24 0 13 30 7.80 20.90 0 -13 -30 -2.62 21.30 0 -13 30 11.14 19.68 0 13 -30 19.38 19.78 0 13 -30 12.51 25.15 0 -13 -30 32.90 14.89 0 13 31 56.50 25.82 0 -13 -31 51.27 18.52 0 -13 -31 27.07 22.81 0 13 -31 45.62 21.81 0 -13 31 81.89 20.45 0 13 -31 55.76 31.78 0 -13 -32 69.45 18.70 0 -13 -32 25.74 23.14 0 13 -32 41.57 24.50 0 13 32 57.50 27.17 0 -13 32 54.67 17.58 0 13 -32 21.24 28.68 0 13 33 90.76 27.75 0 -13 -33 -10.37 25.09 0 -13 -33 134.28 17.35 0 13 -33 111.45 23.03 0 -13 33 145.18 22.54 0 13 -33 72.23 34.09 0 13 34 27.31 27.22 0 -14 0 721.83 26.24 0 -14 -1 868.92 29.54 0 -14 1 914.92 30.85 0 14 2 149.16 26.37 0 -14 2 265.13 26.26 0 14 3 1239.86 36.82 0 -14 3 1324.18 35.38 0 -14 -4 466.25 23.07 0 14 4 487.66 30.23 0 -14 4 577.00 28.86 0 -14 5 38.29 23.16 0 -14 -5 11.97 17.61 0 14 5 -32.26 24.15 0 -14 6 300.46 26.68 0 -14 -6 224.95 20.47 0 14 6 225.58 24.58 0 14 7 454.57 28.27 0 -14 7 457.82 18.33 0 -14 8 501.36 18.30 0 14 8 599.64 28.31 0 -14 9 143.41 15.25 0 14 9 132.44 23.94 0 14 10 30.27 26.36 0 14 11 33.44 22.42 0 -14 -11 8.53 21.28 0 14 12 821.16 30.39 0 -14 -12 778.59 26.95 0 14 13 9.87 25.82 0 -14 -13 -4.61 18.48 0 14 14 265.53 25.11 0 14 -14 333.85 25.22 0 -14 -14 298.96 21.49 0 14 15 16.19 23.26 0 14 -15 32.57 21.53 0 -14 -15 13.17 18.28 0 14 -16 852.60 35.86 0 14 -16 837.88 30.54 0 14 16 696.71 30.31 0 -14 -16 714.44 25.13 0 -14 -17 292.05 21.83 0 14 -17 272.09 32.51 0 14 -17 313.40 25.59 0 14 17 266.56 26.21 0 -14 -18 56.32 20.27 0 14 -18 46.40 28.02 0 14 -18 73.09 22.93 0 14 18 41.39 24.41 0 -14 -19 136.50 21.02 0 14 -19 139.79 25.50 0 14 19 102.22 24.16 0 14 -19 147.84 23.75 0 -14 -20 111.64 20.48 0 14 -20 125.52 25.58 0 14 -20 152.58 23.71 0 14 20 150.71 25.86 0 -14 -21 326.85 22.69 0 14 -21 359.14 24.10 0 14 21 343.92 27.10 0 14 -21 359.52 28.96 0 -14 -22 28.09 19.73 0 14 -22 26.33 22.82 0 14 22 38.66 24.15 0 14 -22 -2.90 23.85 0 -14 -23 213.97 22.72 0 14 -23 354.10 27.21 0 14 23 263.71 23.36 0 14 -23 233.94 30.22 0 -14 -24 6.11 19.79 0 14 -24 11.27 20.31 0 14 -24 6.45 28.88 0 14 24 23.43 24.31 0 14 25 24.43 23.90 0 -14 -25 22.98 18.76 0 14 -25 6.29 20.67 0 14 -25 16.89 29.71 0 -14 -26 40.34 19.88 0 -14 26 30.08 16.24 0 14 -26 31.02 20.46 0 14 -26 23.99 29.23 0 14 26 31.77 24.93 0 -14 -27 187.73 23.95 0 -14 27 349.97 22.73 0 14 -27 296.43 28.34 0 14 -27 152.59 30.25 0 14 27 159.29 29.29 0 -14 -28 80.65 21.96 0 -14 28 113.24 21.35 0 14 -28 50.71 25.17 0 14 -28 -0.12 31.62 0 14 28 54.02 22.44 0 -14 -29 12.03 18.91 0 -14 -29 -10.54 18.10 0 14 -29 29.77 20.55 0 -14 29 20.61 16.23 0 14 -29 -5.96 27.63 0 14 29 24.78 25.63 0 14 30 27.62 26.35 0 -14 -30 -2.13 16.00 0 -14 -30 3.75 21.49 0 -14 30 43.74 20.98 0 14 -30 8.49 25.03 0 14 -30 -6.22 31.86 0 -14 -31 0.52 22.06 0 -14 -31 51.27 19.18 0 -14 31 65.37 21.46 0 14 -31 43.21 21.68 0 14 -31 16.43 29.11 0 14 31 13.53 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27.28 11 -10 3 35.18 25.27 11 -10 4 81.93 28.84 11 -10 5 31.59 28.58 -11 -10 -5 23.07 42.27 -11 -10 -5 14.36 47.89 11 -10 6 15.26 27.38 -11 -10 -6 -3.15 37.69 -11 -10 -6 2.52 42.26 11 -10 7 18.53 24.88 -11 -10 -7 20.55 34.47 -11 -10 -8 134.45 25.95 11 -10 8 167.94 26.36 -11 -10 -8 99.86 34.30 -11 -10 -9 136.91 26.74 11 -10 9 217.84 27.25 -11 -10 -9 118.69 35.53 -11 -10 -10 21.25 24.58 11 -10 10 -0.75 24.50 -11 -10 -10 -8.35 29.54 11 -10 11 24.14 25.51 -11 -10 -11 -1.97 26.05 -11 -10 -11 16.09 29.40 11 -10 12 157.02 25.10 -11 -10 -12 123.71 27.06 -11 -10 -12 121.31 30.72 11 -10 13 34.07 23.70 -11 -10 -13 43.05 26.90 -11 -10 -13 95.58 28.26 11 -10 14 -7.49 21.31 -11 -10 -14 1.90 26.80 -11 -10 -14 38.42 31.05 11 -11 0 6.25 29.86 11 -11 1 54.57 27.99 11 -11 2 104.41 31.11 -11 -11 -3 92.68 49.79 11 -11 3 153.84 32.47 -11 -11 -3 102.03 55.32 -11 -11 -4 0.65 39.19 11 -11 4 14.83 27.16 -11 -11 -4 6.18 46.79 11 -11 5 189.14 28.39 -11 -11 -5 81.94 38.26 -11 -11 -5 108.61 43.35 -11 -11 -6 136.78 26.85 11 -11 6 115.47 28.46 -11 -11 -6 87.75 35.57 -11 -11 -6 77.36 42.80 -11 -11 -7 28.74 25.31 11 -11 7 5.85 25.97 -11 -11 -7 10.66 33.65 -11 -11 -7 63.47 41.73 -11 -11 -8 23.93 24.82 11 -11 8 24.72 25.60 -11 -11 -8 19.84 33.48 -11 -11 -9 3.21 20.42 11 -11 9 34.88 26.29 -11 -11 -9 39.59 33.32 -11 -11 -10 66.16 22.17 11 -11 10 51.25 24.63 -11 -11 -10 61.56 31.75 -11 -11 -11 25.52 22.21 11 -11 11 -3.08 25.98 -11 -11 -11 10.07 30.37 11 -11 12 22.04 26.25 -11 -11 -12 19.00 31.47 11 -12 0 154.20 30.05 -11 -12 -1 9.47 50.74 11 -12 1 12.55 27.97 -11 -12 -1 20.72 55.73 -11 -12 -2 18.62 45.42 11 -12 2 9.39 31.75 -11 -12 -2 9.81 46.13 -11 -12 -3 2.90 40.79 11 -12 3 23.53 29.08 -11 -12 -3 8.49 45.57 -11 -12 -4 97.80 42.60 11 -12 4 103.87 30.07 -11 -12 -4 119.53 42.98 -11 -12 -5 5.67 34.63 11 -12 5 42.60 28.16 -11 -12 -5 14.29 38.16 -11 -12 -6 -0.65 34.16 11 -12 6 26.46 28.50 -11 -12 -6 12.54 38.19 -11 -12 -7 -0.05 32.10 11 -12 7 -0.56 27.88 -11 -12 -7 22.25 38.73 -11 -12 -8 52.52 36.15 11 -12 8 22.58 28.62 -11 -12 -9 12.74 32.86 -11 -13 0 19.69 46.26 -11 -13 0 39.44 53.05 -11 -13 -1 15.09 43.11 11 -13 1 39.81 31.77 -11 -13 -1 -0.77 47.09 -11 -13 -2 14.66 39.30 -11 -13 -2 23.88 42.56 -12 0 -8 100.39 23.90 -12 0 -9 1.59 22.57 -12 0 -10 111.83 24.70 -12 0 -11 -9.25 23.59 -12 0 -12 24.20 27.60 -12 0 -13 20.86 24.43 -12 0 -14 178.18 29.31 -12 0 -15 -30.23 26.67 -12 0 -16 68.73 31.47 -12 0 -17 95.00 32.91 -12 0 -18 48.02 31.25 -12 0 -19 24.67 29.30 12 0 19 7.77 23.15 -12 1 -4 526.72 28.06 -12 1 -5 99.41 23.12 -12 1 -6 57.83 24.94 -12 1 -7 19.69 22.39 -12 1 -8 376.08 29.88 -12 -1 -8 371.75 27.31 -12 1 -9 22.66 26.97 -12 -1 -9 30.43 23.11 -12 -1 -10 208.48 28.99 -12 1 -10 162.33 25.72 -12 -1 -11 30.36 25.21 -12 1 -11 5.36 23.43 -12 -1 -12 36.25 26.14 -12 1 -12 55.82 27.88 -12 1 -13 -16.47 24.14 -12 -1 -13 20.24 25.69 -12 1 -14 31.19 28.68 -12 -1 -14 20.79 26.45 -12 1 -15 12.57 28.35 -12 -1 -15 8.55 26.53 -12 1 -16 28.61 26.20 -12 -1 -16 4.60 26.02 -12 1 -17 18.27 26.34 -12 -1 -17 6.15 27.42 -12 1 -18 -8.63 27.92 -12 -1 -18 30.94 29.50 12 -1 18 2.91 25.87 -12 1 -19 13.38 28.12 -12 -1 -19 -4.61 29.86 -12 -1 -19 22.70 33.97 12 -1 19 5.90 26.58 -12 2 0 105.61 23.72 -12 2 -1 21.43 20.54 -12 2 -2 38.74 21.51 -12 2 -3 3.28 23.91 -12 2 -6 29.23 24.03 -12 2 -7 21.54 25.32 -12 2 -8 29.11 22.61 -12 -2 -8 24.42 23.84 -12 2 -9 14.69 25.12 -12 2 -10 183.48 28.37 -12 -2 -11 -4.81 24.99 -12 2 -11 -9.56 26.58 -12 -2 -12 43.55 26.04 -12 2 -12 5.49 22.11 -12 -2 -13 42.43 26.28 -12 2 -13 -19.84 24.15 -12 2 -14 330.09 30.23 -12 -2 -14 291.41 31.90 -12 2 -15 23.69 28.48 -12 -2 -15 7.99 29.30 -12 2 -16 31.84 28.27 -12 -2 -16 27.51 28.98 12 -2 16 -3.82 25.74 -12 2 -17 19.05 30.05 -12 -2 -17 30.04 29.19 -12 -2 -17 31.03 38.47 12 -2 17 11.15 26.21 -12 2 -18 27.23 29.14 -12 -2 -18 109.40 33.04 -12 -2 -18 -11.74 35.42 12 -2 18 129.05 29.31 -12 -2 -19 20.59 34.57 -12 3 0 451.48 28.34 -12 3 -1 44.33 24.42 -12 3 -2 26.08 23.79 -12 3 -3 13.19 23.86 -12 3 -4 1032.40 35.52 -12 3 -5 127.16 27.92 -12 3 -6 21.00 20.90 -12 3 -7 29.85 24.08 -12 -3 -8 272.54 27.54 -12 3 -8 214.77 28.29 -12 -3 -9 51.61 25.35 -12 3 -9 59.81 24.55 -12 -3 -10 134.65 26.11 -12 3 -10 87.27 26.61 -12 -3 -11 -2.20 27.45 -12 3 -11 7.91 25.38 -12 -3 -12 49.86 27.92 -12 3 -12 44.74 29.01 -12 -3 -13 -8.47 27.38 -12 3 -13 7.15 26.69 -12 -3 -14 44.35 22.92 12 -3 14 63.97 26.11 -12 3 -14 20.92 28.11 -12 -3 -15 -2.42 23.70 12 -3 15 3.19 25.26 -12 3 -15 28.46 26.43 -12 -3 -16 -27.54 29.63 -12 -3 -16 -4.10 40.44 12 -3 16 11.63 25.82 -12 3 -16 16.78 27.88 -12 3 -17 10.58 31.84 -12 -3 -17 10.30 30.46 -12 -3 -17 -6.52 37.34 12 -3 17 -15.11 26.07 -12 3 -18 22.63 29.26 -12 -3 -18 20.17 30.65 -12 -3 -18 0.14 34.90 12 -3 18 14.43 25.54 -12 4 0 32.83 22.46 -12 4 -1 18.05 22.50 -12 4 -2 33.41 23.40 -12 4 -3 26.51 25.87 -12 4 -4 19.14 23.28 -12 4 -5 11.01 22.94 -12 -4 -5 4.91 23.36 -12 4 -6 20.90 23.44 -12 4 -7 14.23 23.09 -12 -4 -8 36.93 25.03 -12 4 -8 35.53 24.06 -12 4 -9 13.38 23.18 -12 4 -10 103.18 26.07 -12 -4 -11 5.09 26.62 -12 4 -11 11.48 25.99 -12 -4 -12 12.68 26.54 -12 4 -12 8.11 25.32 12 -4 12 29.79 25.21 -12 -4 -13 -12.97 28.12 12 -4 13 10.45 25.55 -12 4 -13 22.42 26.65 -12 -4 -14 184.03 31.20 12 -4 14 192.18 30.32 -12 4 -14 205.88 33.52 -12 -4 -15 11.70 29.01 -12 -4 -15 33.94 44.28 12 -4 15 34.37 28.96 -12 4 -15 2.47 31.55 -12 -4 -16 14.63 29.70 -12 -4 -16 -10.12 40.64 12 -4 16 20.77 28.48 -12 4 -16 10.97 30.41 -12 -4 -17 25.43 30.74 -12 -4 -17 -2.21 38.18 12 -4 17 -3.33 25.61 -12 4 -17 20.43 27.77 -12 -4 -18 -11.55 34.38 -12 5 0 358.41 30.11 -12 5 -1 83.78 25.33 -12 5 -2 35.99 25.51 -12 5 -3 82.90 26.17 -12 5 -4 487.68 29.66 -12 5 -5 107.99 25.83 12 -5 6 51.45 28.09 -12 5 -6 54.13 26.74 -12 -5 -6 50.75 25.72 12 -5 7 54.34 28.71 -12 5 -7 45.63 26.37 12 -5 8 246.81 30.70 -12 5 -8 192.01 29.62 -12 5 -9 2.61 27.15 12 -5 9 12.55 28.02 -12 -5 -10 76.34 27.84 -12 5 -10 84.64 28.96 12 -5 10 88.31 27.00 -12 -5 -11 -0.66 26.16 -12 5 -11 -4.08 27.73 12 -5 11 6.62 27.50 -12 -5 -12 51.91 27.58 -12 5 -12 48.75 28.16 12 -5 12 37.98 29.27 -12 -5 -13 40.43 28.76 -12 5 -13 11.52 28.72 12 -5 13 31.84 28.45 -12 -5 -14 17.52 29.30 -12 5 -14 32.46 28.24 -12 -5 -14 23.61 48.14 12 -5 14 19.11 28.57 -12 -5 -15 27.85 29.47 -12 -5 -15 10.30 44.03 -12 5 -15 -0.78 27.75 12 -5 15 -4.25 27.42 -12 -5 -16 20.58 29.72 -12 -5 -16 0.98 41.44 -12 5 -16 10.81 29.01 12 -5 16 12.36 30.85 -12 6 -1 18.39 27.88 -12 6 -2 178.23 30.82 -12 6 -3 49.26 28.84 12 -6 3 31.47 31.52 -12 6 -4 13.67 28.08 12 -6 4 9.80 29.86 -12 6 -5 6.92 27.94 12 -6 5 4.38 29.29 12 -6 6 84.27 32.64 -12 6 -6 77.55 31.64 12 -6 7 6.58 29.82 -12 6 -7 9.27 27.66 -12 -6 -8 39.07 25.30 -12 6 -8 22.36 28.91 12 -6 8 57.53 32.83 -12 -6 -9 -2.41 26.40 -12 6 -9 15.14 27.83 12 -6 9 15.29 31.79 -12 -6 -10 81.45 27.19 -12 6 -10 86.90 32.58 12 -6 10 71.58 34.40 -12 -6 -11 48.34 27.09 -12 6 -11 43.79 32.66 12 -6 11 61.24 33.58 -12 -6 -12 12.34 27.05 -12 6 -12 9.17 34.10 12 -6 12 12.25 32.96 -12 -6 -13 -4.69 22.05 -12 -6 -13 -0.12 56.18 12 -6 13 11.19 33.55 -12 6 -13 19.50 34.31 -12 6 -14 177.02 36.08 -12 -6 -14 24.12 29.08 -12 -6 -14 -17.39 46.75 12 -6 14 148.43 36.43 -12 6 -15 33.14 33.20 -12 -6 -15 -20.27 30.46 -12 -6 -15 22.70 40.68 12 -6 15 15.10 34.01 -12 -6 -16 -8.80 38.32 12 -7 0 131.21 34.64 12 -7 0 175.23 36.85 12 -7 1 77.56 35.14 12 -7 1 108.27 36.95 12 -7 2 28.46 35.33 12 -7 2 17.08 37.77 12 -7 3 8.23 35.75 12 -7 3 24.21 37.39 12 -7 4 186.73 46.16 12 -7 5 35.95 44.19 12 -7 6 36.99 50.94 12 -7 6 0.23 11.90 -12 -7 -8 142.96 27.67 -12 -7 -9 7.52 26.75 -12 -7 -10 120.29 27.75 -12 -7 -11 22.52 28.52 -12 -7 -12 116.96 29.50 -12 -7 -13 29.82 24.46 -12 -7 -13 1.58 51.39 -12 -7 -14 6.90 45.86 -12 -8 -8 13.45 26.48 -12 -8 -9 8.36 26.63 -12 -8 -10 36.40 27.33 -12 -8 -10 1.26 17.12 -12 -8 -11 39.88 29.20 -12 -8 -12 31.08 29.68 -12 -8 -12 18.60 57.00 12 -9 2 5.95 38.25 12 -9 3 22.86 36.10 12 -9 4 173.06 39.36 -12 -9 -4 30.18 26.83 12 -9 5 40.24 31.39 12 -9 6 17.86 31.03 12 -9 7 193.31 34.94 -12 -9 -8 66.32 28.25 12 -9 8 98.43 30.33 -12 -9 -9 41.23 28.14 12 -9 9 -1.54 28.39 -12 -9 -9 0.62 23.41 -12 -9 -10 13.37 27.58 12 -10 0 17.15 39.92 12 -10 1 38.18 38.76 12 -10 2 72.79 36.08 12 -10 3 10.57 35.04 12 -10 4 24.64 32.58 -12 -10 -4 -3.86 25.63 12 -10 5 5.19 32.85 -12 -10 -5 -15.11 25.88 -13 0 -1 -2.94 22.12 -13 0 -2 249.70 28.25 -13 0 -3 24.82 22.89 -13 0 -4 45.02 26.47 -13 0 -5 28.89 22.57 -13 0 -6 34.82 23.95 -13 0 -7 11.28 24.02 -13 0 -8 -0.49 23.60 -13 0 -9 -6.13 27.52 -13 0 -10 -7.46 24.87 -13 0 -11 9.42 24.59 -13 0 -12 27.27 26.19 -13 1 0 39.75 21.37 -13 1 -1 22.23 24.57 -13 1 -2 274.18 24.11 -13 1 -3 -5.09 25.66 -13 1 -4 -11.64 21.19 -13 1 -5 -0.67 25.04 -13 -1 -5 5.73 23.07 -13 1 -6 298.05 26.21 -13 -1 -6 296.69 27.69 -13 1 -7 13.98 27.63 -13 -1 -7 34.74 25.15 -13 1 -8 119.00 25.46 -13 -1 -8 110.88 26.47 -13 1 -9 11.50 24.21 -13 -1 -9 75.63 30.01 -13 1 -10 120.77 28.62 -13 -1 -10 121.74 28.10 -13 1 -11 7.27 25.74 -13 -1 -11 14.61 26.62 -13 1 -12 98.27 31.92 -13 -1 -12 122.82 29.88 -13 2 0 153.83 26.63 -13 2 -1 16.75 21.26 -13 2 -2 150.19 27.11 -13 2 -3 18.80 25.67 -13 2 -4 26.55 21.64 -13 -2 -4 0.03 23.94 -13 2 -5 25.67 25.28 -13 -2 -5 9.97 25.08 -13 2 -6 37.00 22.24 -13 -2 -6 34.40 24.70 -13 2 -7 14.52 26.44 -13 -2 -7 -19.43 25.61 -13 2 -8 7.26 26.62 -13 -2 -8 18.81 25.89 -13 2 -9 28.45 26.34 -13 -2 -9 -1.59 26.15 -13 2 -10 0.69 26.59 -13 -2 -10 4.59 27.53 -13 2 -11 25.54 24.18 -13 -2 -11 0.72 27.65 -13 2 -12 82.19 29.58 -13 3 0 -7.13 20.40 -13 3 -1 20.91 24.10 -13 3 -2 313.34 27.11 -13 3 -3 55.77 25.79 -13 3 -4 19.79 24.78 -13 3 -5 -1.10 24.90 -13 -3 -5 19.76 25.61 -13 3 -6 379.71 29.79 -13 -3 -6 248.04 29.29 -13 3 -7 28.39 26.20 -13 -3 -7 55.09 27.50 -13 3 -8 27.30 26.60 -13 -3 -8 20.41 27.13 -13 3 -9 41.59 26.91 -13 -3 -9 31.17 27.11 -13 3 -10 32.65 31.67 -13 -3 -10 41.00 27.97 -13 3 -11 6.37 27.59 -13 -3 -11 1.36 28.77 -13 4 0 215.83 28.73 -13 4 -1 16.88 24.55 -13 4 -2 99.77 26.13 -13 4 -3 18.73 24.65 -13 4 -4 -12.19 24.61 -13 4 -5 41.09 25.17 -13 4 -6 80.52 28.37 -13 -4 -6 103.90 26.67 -13 -4 -7 33.71 25.92 -13 4 -7 8.11 28.26 13 -4 8 17.34 27.10 -13 -4 -8 0.55 26.80 -13 4 -8 20.67 28.14 -13 4 -9 2.92 27.95 13 -4 9 9.79 31.13 -13 -4 -9 -2.61 27.46 -13 4 -10 18.78 25.94 -13 5 0 12.31 27.10 -13 5 -1 6.63 24.07 -13 5 -2 291.66 30.87 13 -5 3 99.01 31.97 -13 5 -3 62.90 28.39 -13 -5 -3 84.52 26.89 13 -5 4 17.83 29.98 -13 5 -4 11.89 27.17 13 -5 5 40.43 29.65 -13 5 -5 7.17 30.42 -13 5 -6 185.35 30.03 13 -5 6 144.73 31.85 -13 -5 -6 113.14 28.36 -13 5 -7 54.08 25.97 13 -5 7 46.03 34.10 -13 -5 -7 101.06 28.53 -13 5 -8 65.86 28.19 13 -5 8 18.72 29.77 -13 -5 -8 35.10 23.07 13 -6 0 139.84 32.52 13 -6 1 6.73 33.93 13 -6 2 102.24 35.55 13 -6 3 41.53 33.81 13 -6 4 58.11 33.10 -13 -6 -4 78.04 27.20 -13 6 -5 20.13 35.27 13 -6 5 38.07 35.17 13 -6 6 19.48 35.64 -13 6 -6 16.99 32.96 13 -7 0 12.88 39.31 13 -7 0 14.19 38.54 13 -7 1 7.10 42.00 13 -7 1 1.76 41.75 13 -7 2 76.16 51.20 -13 -7 -2 81.20 26.02 13 -7 2 59.36 45.55 ; _shelx_hkl_checksum 48294 data_global _audit_creation_date "2016-04-05" _audit_creation_method CRYSTALS_ver_14.61 _oxford_structure_analysis_title 'THIS IS THE DEFAULT SETTING FOR THE TITLE, P' _chemical_name_systematic ? _chemical_melting_point ? #looking for refcif # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; ; _publ_contact_author_name '' _publ_contact_author_address ; ; _publ_contact_author_phone '' _publ_contact_author_fax '' _publ_contact_author_email '' _publ_requested_journal '' _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name '' _publ_section_title # Title of paper - generally just the systematic or trivial name ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Other, Anthony N.' # Author 1 ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Else, S. O.' # Author 2 ; ? # Address 2 ; ; ? # Footnote 2 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; The H atoms were refined with riding constraints (Cooper et al, 2010). Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100-1107. Hydrogen atoms could not be located on the 6 H2O molecules ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # data_1 _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 8.9103(3) _cell_length_b 13.9215(5) _cell_length_c 27.2730(10) _cell_angle_alpha 90 _cell_angle_beta 93.553(4) _cell_angle_gamma 90 _cell_volume 3376.6(2) _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.1653 3.9035 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C27 H32 Gd1 N10 Ni1 O10 W1 # Dc = 2.08 Fooo = 1992.00 Mu = 59.61 M = 1056.42 # Found Formula = C27 H20 Gd1 N10 Ni1 O10 W1 # Dc = 2.05 FOOO = 1992.00 Mu = 59.60 M = 1044.33 _chemical_formula_sum 'C27 H32 Gd1 N10 Ni1 O10 W1' _chemical_formula_moiety 'C27 H30 Gd1 N10 Ni1 O9 W1, H2 O' _chemical_compound_source ? _chemical_formula_weight 1056.42 _cell_measurement_reflns_used 13133 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 180 _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_min 0.120 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 2.078 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 5.961 # Sheldrick geometric approximatio 0.41 0.49 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)' _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_T_max 0.52 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)' _computing_data_reduction 'XRED (Stoe & Cie 1996)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 180 _diffrn_reflns_number 31324 _reflns_number_total 8942 _diffrn_reflns_av_R_equivalents 0.080 # Number of reflections without Friedels Law is 8942 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 9117 _diffrn_reflns_theta_min 2.679 _diffrn_reflns_theta_max 29.219 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.635 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 37 _atom_sites_solution_primary direct #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -2.89 _refine_diff_density_max 4.00 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>1.7\s(I) _refine_ls_number_reflns 4623 _refine_ls_number_restraints 0 _refine_ls_number_parameters 460 _oxford_refine_ls_R_factor_ref 0.0449 _refine_ls_wR_factor_ref 0.0545 _refine_ls_goodness_of_fit_ref 0.9978 _refine_ls_shift/su_max 0.0005720 _refine_ls_shift/su_mean 0.0000271 # The values computed with all filters except I/sigma _oxford_reflns_number_all 9054 _refine_ls_R_factor_all 0.0936 _refine_ls_wR_factor_all 0.1360 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4341 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_gt 0.0532 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed # WARNING. The IUCr will not accept pure Unit Weights for F-squared refinements _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Quasi-Unit weights W = 1.0 or 1./4Fsq ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Agilent (2011). CrysAlisPro. Oxford Diffraction, (2002). Xcalibur User Manual. Stoe & Cie (1996). IPDS Software. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens W1 W 0.18710(6) 0.74315(4) 0.121097(17) 0.0151 1.0000 Uani . . . . . . Gd1 Gd 0.32921(7) 1.22830(4) 0.07970(2) 0.0166 1.0000 Uani . . . . . . Ni1 Ni 0.2516(2) 1.10273(11) 0.18592(6) 0.0172 1.0000 Uani . . . . . . C1 C 0.2049(16) 0.8929(10) 0.1391(5) 0.0236 1.0000 Uani . . . . . . C2 C 0.4039(15) 0.7825(12) 0.0965(4) 0.0278 1.0000 Uani . . . . . . C3 C 0.3361(15) 0.7528(10) 0.1864(5) 0.0252 1.0000 Uani . . . . . . C4 C 0.2336(18) 0.6008(10) 0.1476(5) 0.0271 1.0000 Uani . . . . . . C5 C 0.2341(19) 0.6582(11) 0.0577(5) 0.0320 1.0000 Uani . . . . . . C6 C -0.0185(19) 0.6665(10) 0.0990(5) 0.0289 1.0000 Uani . . . . . . C7 C 0.0291(14) 0.7632(9) 0.1784(4) 0.0221 1.0000 Uani . . . . . . C8 C 0.0823(15) 0.8270(9) 0.0614(5) 0.0206 1.0000 Uani . . . . . . C9 C 0.082(2) 1.4080(12) 0.0417(6) 0.0390 1.0000 Uani . . . . . . C10 C -0.0206(17) 1.3013(11) 0.1015(5) 0.0259 1.0000 Uani . . . . . . C11 C -0.1556(17) 1.3473(12) 0.0994(6) 0.0325 1.0000 Uani . . . . . . C12 C -0.2602(16) 1.3230(12) 0.1335(6) 0.0328 1.0000 Uani . . . . . . C13 C -0.2227(15) 1.2532(13) 0.1682(5) 0.0339 1.0000 Uani . . . . . . C14 C -0.0882(16) 1.2055(11) 0.1705(5) 0.0264 1.0000 Uani . . . . . . C15 C 0.0185(13) 1.2290(9) 0.1351(5) 0.0205 1.0000 Uani . . . . . . C16 C -0.0612(16) 1.1352(10) 0.2087(5) 0.0260 1.0000 Uani . . . . . . C17 C 0.062(2) 1.0201(11) 0.2614(6) 0.0376 1.0000 Uani . . . . . . C18 C 0.194(2) 1.0382(13) 0.2960(6) 0.0430 1.0000 Uani . . . . . . C19 C 0.339(2) 0.9954(12) 0.2816(6) 0.0425 1.0000 Uani . . . . . . C20 C 0.5157(17) 0.9961(10) 0.2235(5) 0.0262 1.0000 Uani . . . . . . C21 C 0.5901(16) 1.0089(9) 0.1772(5) 0.0212 1.0000 Uani . . . . . . C22 C 0.5416(13) 1.0734(9) 0.1408(5) 0.0173 1.0000 Uani . . . . . . C23 C 0.7149(18) 0.9532(11) 0.1708(6) 0.0320 1.0000 Uani . . . . . . C24 C 0.7904(18) 0.9567(12) 0.1287(6) 0.0375 1.0000 Uani . . . . . . C25 C 0.7468(16) 1.0204(11) 0.0920(6) 0.0286 1.0000 Uani . . . . . . C26 C 0.6239(15) 1.0777(9) 0.0979(5) 0.0217 1.0000 Uani . . . . . . C27 C 0.6583(17) 1.1648(13) 0.0251(5) 0.0351 1.0000 Uani . . . . . . N1 N 0.2116(14) 0.9734(7) 0.1475(4) 0.0239 1.0000 Uani . . . . . . N2 N 0.5193(16) 0.7977(14) 0.0824(5) 0.0552 1.0000 Uani . . . . . . N3 N 0.4219(14) 0.7560(11) 0.2197(4) 0.0357 1.0000 Uani . . . . . . N4 N 0.2619(18) 0.5242(9) 0.1581(5) 0.0378 1.0000 Uani . . . . . . N5 N 0.2635(19) 0.6124(10) 0.0243(5) 0.0457 1.0000 Uani . . . . . . N6 N -0.1239(16) 0.6267(10) 0.0866(5) 0.0372 1.0000 Uani . . . . . . N7 N -0.0514(14) 0.7735(9) 0.2077(4) 0.0281 1.0000 Uani . . . . . . N8 N 0.0182(14) 0.8700(10) 0.0312(4) 0.0293 1.0000 Uani . . . . . . N9 N 0.0584(14) 1.0877(8) 0.2198(4) 0.0227 1.0000 Uani . . . . . . N10 N 0.3886(14) 1.0293(8) 0.2340(4) 0.0235 1.0000 Uani . . . . . . O1 O 0.0947(12) 1.3188(7) 0.0692(3) 0.0271 1.0000 Uani . . . . . . O2 O 0.1507(11) 1.1855(6) 0.1334(3) 0.0219 1.0000 Uani . . . . . . O3 O 0.4247(10) 1.1328(6) 0.1432(3) 0.0179 1.0000 Uani . . . . . . O4 O 0.5635(11) 1.1453(7) 0.0647(3) 0.0251 1.0000 Uani . . . . . . O5 O 0.2114(13) 1.0807(7) 0.0478(4) 0.0351 1.0000 Uani . . . . . . O6 O 0.2901(11) 1.2334(8) -0.0097(3) 0.0305 1.0000 Uani . . . . . . O7 O 0.4573(14) 1.3690(8) 0.0481(4) 0.0396 1.0000 Uani . . . . . . O8 O 0.3663(11) 1.3397(7) 0.1458(3) 0.0217 1.0000 Uani . . . . . . O9 O 0.2978(10) 1.2376(7) 0.2273(3) 0.0204 1.0000 Uani . . . . . . O10 O 0.581(3) 0.5308(19) 0.0873(12) 0.0532 0.5000 Uani . . . . . . O11 O 0.590(3) 0.5530(18) 0.0545(10) 0.0478 0.5000 Uani . . . . . . H93 H 0.1643 1.4132 0.0210 0.0620 1.0000 Uiso R . . . . . H92 H 0.0833 1.4618 0.0637 0.0620 1.0000 Uiso R . . . . . H91 H -0.0110 1.4078 0.0219 0.0620 1.0000 Uiso R . . . . . H111 H -0.1773 1.3945 0.0759 0.0390 1.0000 Uiso R . . . . . H121 H -0.3533 1.3533 0.1327 0.0400 1.0000 Uiso R . . . . . H131 H -0.2920 1.2375 0.1910 0.0410 1.0000 Uiso R . . . . . H161 H -0.1412 1.1228 0.2279 0.0320 1.0000 Uiso R . . . . . H171 H -0.0295 1.0267 0.2783 0.0460 1.0000 Uiso R . . . . . H172 H 0.0701 0.9551 0.2490 0.0460 1.0000 Uiso R . . . . . H181 H 0.2075 1.1072 0.2985 0.0540 1.0000 Uiso R . . . . . H182 H 0.1725 1.0122 0.3277 0.0540 1.0000 Uiso R . . . . . H191 H 0.4180 1.0105 0.3066 0.0510 1.0000 Uiso R . . . . . H192 H 0.3255 0.9265 0.2798 0.0510 1.0000 Uiso R . . . . . H201 H 0.5668 0.9590 0.2477 0.0310 1.0000 Uiso R . . . . . H231 H 0.7487 0.9120 0.1958 0.0380 1.0000 Uiso R . . . . . H241 H 0.8714 0.9160 0.1249 0.0430 1.0000 Uiso R . . . . . H251 H 0.7991 1.0246 0.0636 0.0341 1.0000 Uiso R . . . . . H273 H 0.6161 1.2171 0.0061 0.0530 1.0000 Uiso R . . . . . H272 H 0.7575 1.1816 0.0382 0.0529 1.0000 Uiso R . . . . . H271 H 0.6628 1.1085 0.0049 0.0530 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0202(2) 0.0159(2) 0.0094(2) 0.00008(19) 0.00364(17) 0.0014(2) Gd1 0.0205(3) 0.0199(3) 0.0097(3) 0.0009(2) 0.0043(2) 0.0016(2) Ni1 0.0237(9) 0.0168(7) 0.0116(7) 0.0004(6) 0.0056(6) -0.0001(6) C1 0.021(7) 0.038(8) 0.012(6) 0.011(5) 0.007(5) 0.001(6) C2 0.016(6) 0.059(9) 0.009(5) -0.014(6) -0.003(5) -0.009(6) C3 0.027(7) 0.027(7) 0.022(6) 0.003(6) 0.012(5) -0.001(6) C4 0.036(9) 0.030(8) 0.016(7) -0.007(5) 0.012(6) 0.005(6) C5 0.047(10) 0.030(8) 0.020(7) -0.001(6) 0.018(7) 0.007(7) C6 0.048(10) 0.026(7) 0.013(6) -0.002(5) 0.003(6) 0.000(7) C7 0.026(7) 0.023(6) 0.017(5) -0.003(5) 0.003(5) -0.002(5) C8 0.014(6) 0.025(6) 0.024(7) -0.004(5) 0.005(5) 0.001(5) C9 0.046(10) 0.039(9) 0.033(9) 0.006(7) 0.010(8) 0.013(8) C10 0.030(8) 0.037(8) 0.010(6) -0.004(5) 0.002(5) 0.000(6) C11 0.032(9) 0.043(9) 0.023(7) -0.007(6) -0.003(6) 0.012(7) C12 0.014(7) 0.050(9) 0.034(8) -0.019(7) -0.003(6) 0.006(6) C13 0.020(6) 0.054(9) 0.028(7) -0.018(8) 0.000(5) 0.003(7) C14 0.024(7) 0.038(8) 0.018(6) -0.013(6) 0.009(5) -0.005(6) C15 0.012(5) 0.024(6) 0.026(6) -0.004(5) 0.001(5) 0.003(5) C16 0.023(7) 0.035(8) 0.021(7) -0.010(6) 0.014(6) -0.006(6) C17 0.055(11) 0.033(8) 0.028(8) 0.002(6) 0.026(8) -0.012(7) C18 0.062(12) 0.045(10) 0.023(8) 0.012(7) 0.013(8) 0.007(9) C19 0.070(13) 0.041(9) 0.019(7) 0.015(6) 0.014(8) 0.018(9) C20 0.031(8) 0.026(7) 0.021(7) 0.002(5) -0.006(6) 0.009(6) C21 0.022(7) 0.025(6) 0.016(6) 0.002(5) 0.002(5) 0.001(5) C22 0.007(5) 0.026(6) 0.017(6) 0.000(5) -0.003(5) 0.001(5) C23 0.032(8) 0.030(8) 0.034(8) 0.003(6) -0.004(7) 0.008(6) C24 0.031(9) 0.040(9) 0.042(9) 0.003(7) 0.015(7) 0.017(7) C25 0.020(7) 0.032(7) 0.035(8) 0.000(6) 0.009(6) 0.010(6) C26 0.021(7) 0.022(6) 0.023(7) 0.001(5) 0.004(5) 0.006(5) C27 0.027(8) 0.057(10) 0.023(8) 0.008(7) 0.015(6) 0.006(7) N1 0.038(7) 0.013(5) 0.022(6) 0.001(4) 0.011(5) -0.002(4) N2 0.026(8) 0.113(15) 0.028(7) -0.015(8) 0.013(6) -0.015(8) N3 0.038(7) 0.048(8) 0.021(6) 0.004(6) 0.000(5) 0.001(7) N4 0.061(10) 0.019(6) 0.035(8) 0.002(5) 0.014(7) 0.015(6) N5 0.073(11) 0.038(8) 0.025(7) -0.001(6) 0.002(7) 0.015(7) N6 0.037(8) 0.046(8) 0.028(7) -0.006(6) 0.001(6) -0.018(6) N7 0.033(7) 0.032(6) 0.020(6) 0.000(5) 0.008(5) 0.003(5) N8 0.021(6) 0.045(7) 0.021(6) 0.006(5) -0.003(5) 0.004(5) N9 0.034(7) 0.021(5) 0.014(6) -0.003(4) 0.011(5) -0.005(5) N10 0.039(7) 0.023(5) 0.009(5) 0.002(4) 0.007(5) -0.004(5) O1 0.039(6) 0.025(5) 0.018(5) 0.001(4) 0.005(4) 0.009(4) O2 0.027(5) 0.018(4) 0.022(5) -0.002(3) 0.014(4) 0.001(4) O3 0.016(5) 0.026(5) 0.012(4) 0.004(3) 0.005(4) 0.006(4) O4 0.022(5) 0.038(5) 0.016(5) 0.006(4) 0.009(4) 0.003(4) O5 0.055(8) 0.027(5) 0.024(5) -0.003(4) 0.009(5) -0.003(5) O6 0.038(6) 0.041(6) 0.014(4) 0.001(4) 0.008(4) 0.005(5) O7 0.059(8) 0.033(6) 0.030(6) -0.002(5) 0.019(6) -0.011(5) O8 0.024(5) 0.026(5) 0.015(4) -0.006(4) 0.005(4) -0.001(4) O9 0.024(4) 0.027(5) 0.010(4) -0.002(4) 0.005(3) -0.002(4) O10 0.047(17) 0.043(15) 0.07(2) 0.001(14) 0.003(15) 0.016(12) O11 0.049(16) 0.041(14) 0.051(16) 0.022(13) -0.018(14) -0.014(12) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 . C1 . 2.145(15) yes W1 . C2 . 2.154(13) yes W1 . C3 . 2.159(14) yes W1 . C4 . 2.140(15) yes W1 . C5 . 2.156(14) yes W1 . C6 . 2.173(16) yes W1 . C7 . 2.185(12) yes W1 . C8 . 2.167(14) yes Gd1 . O1 . 2.442(10) yes Gd1 . O2 . 2.307(9) yes Gd1 . O3 . 2.305(8) yes Gd1 . O4 . 2.442(9) yes Gd1 . O5 . 2.444(10) yes Gd1 . O6 . 2.442(9) yes Gd1 . O7 . 2.450(10) yes Gd1 . O8 . 2.386(9) yes Ni1 . N1 . 2.102(11) yes Ni1 . N9 . 2.015(11) yes Ni1 . N10 . 2.015(12) yes Ni1 . O2 . 2.006(10) yes Ni1 . O3 . 2.033(9) yes Ni1 . O9 . 2.216(9) yes C1 . N1 . 1.144(18) yes C2 . N2 . 1.140(18) yes C3 . N3 . 1.149(17) yes C4 . N4 . 1.129(19) yes C5 . N5 . 1.157(19) yes C6 . N6 . 1.125(19) yes C7 . N7 . 1.117(16) yes C8 . N8 . 1.143(17) yes C9 . O1 . 1.452(18) yes C9 . H93 . 0.956 no C9 . H92 . 0.960 no C9 . H91 . 0.959 no C10 . C11 . 1.36(2) yes C10 . C15 . 1.392(19) yes C10 . O1 . 1.414(17) yes C11 . C12 . 1.40(2) yes C11 . H111 . 0.931 no C12 . C13 . 1.38(2) yes C12 . H121 . 0.929 no C13 . C14 . 1.37(2) yes C13 . H131 . 0.927 no C14 . C15 . 1.432(17) yes C14 . C16 . 1.44(2) yes C15 . O2 . 1.328(14) yes C16 . N9 . 1.274(18) yes C16 . H161 . 0.926 no C17 . C18 . 1.48(2) yes C17 . N9 . 1.472(18) yes C17 . H171 . 0.967 no C17 . H172 . 0.969 no C18 . C19 . 1.50(2) yes C18 . H181 . 0.969 no C18 . H182 . 0.969 no C19 . N10 . 1.473(17) yes C19 . H191 . 0.971 no C19 . H192 . 0.969 no C20 . C21 . 1.474(18) yes C20 . N10 . 1.272(18) yes C20 . H201 . 0.932 no C21 . C22 . 1.387(17) yes C21 . C23 . 1.375(19) yes C22 . C26 . 1.420(17) yes C22 . O3 . 1.334(14) yes C23 . C24 . 1.37(2) yes C23 . H231 . 0.927 no C24 . C25 . 1.38(2) yes C24 . H241 . 0.929 no C25 . C26 . 1.373(18) yes C25 . H251 . 0.930 no C26 . O4 . 1.391(16) yes C27 . O4 . 1.437(15) yes C27 . H273 . 0.957 no C27 . H272 . 0.961 no C27 . H271 . 0.961 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . W1 . C2 . 76.7(5) yes C1 . W1 . C3 . 73.6(5) yes C2 . W1 . C3 . 74.0(4) yes C1 . W1 . C4 . 144.3(5) yes C2 . W1 . C4 . 100.5(6) yes C3 . W1 . C4 . 71.5(6) yes C1 . W1 . C5 . 134.5(5) yes C2 . W1 . C5 . 70.6(6) yes C3 . W1 . C5 . 123.7(6) yes C4 . W1 . C5 . 73.7(5) yes C1 . W1 . C6 . 126.1(6) yes C2 . W1 . C6 . 142.7(5) yes C3 . W1 . C6 . 136.4(5) yes C4 . W1 . C6 . 77.4(6) yes C5 . W1 . C6 . 73.2(6) yes C1 . W1 . C7 . 75.7(5) yes C2 . W1 . C7 . 145.1(5) yes C3 . W1 . C7 . 78.0(5) yes C4 . W1 . C7 . 89.9(5) yes C5 . W1 . C7 . 144.0(5) yes C1 . W1 . C8 . 70.8(5) yes C2 . W1 . C8 . 89.0(5) yes C3 . W1 . C8 . 143.2(5) yes C4 . W1 . C8 . 144.8(5) yes C5 . W1 . C8 . 77.8(5) yes C6 . W1 . C7 . 72.0(5) yes C6 . W1 . C8 . 74.9(5) yes C7 . W1 . C8 . 101.6(5) yes O1 . Gd1 . O2 . 65.7(3) yes O1 . Gd1 . O3 . 131.2(3) yes O2 . Gd1 . O3 . 67.1(3) yes O1 . Gd1 . O4 . 163.5(3) yes O2 . Gd1 . O4 . 127.9(3) yes O3 . Gd1 . O4 . 64.7(3) yes O1 . Gd1 . O5 . 92.7(4) yes O2 . Gd1 . O5 . 73.2(3) yes O3 . Gd1 . O5 . 85.0(3) yes O4 . Gd1 . O5 . 84.0(4) yes O1 . Gd1 . O6 . 78.5(3) yes O2 . Gd1 . O6 . 125.5(3) yes O3 . Gd1 . O6 . 142.2(3) yes O4 . Gd1 . O6 . 85.3(3) yes O5 . Gd1 . O6 . 68.7(3) yes O1 . Gd1 . O7 . 87.7(4) yes O2 . Gd1 . O7 . 141.7(3) yes O3 . Gd1 . O7 . 124.6(4) yes O4 . Gd1 . O7 . 84.1(4) yes O5 . Gd1 . O7 . 138.3(3) yes O1 . Gd1 . O8 . 80.3(3) yes O2 . Gd1 . O8 . 75.9(3) yes O3 . Gd1 . O8 . 77.2(3) yes O4 . Gd1 . O8 . 110.7(3) yes O5 . Gd1 . O8 . 148.5(3) yes O6 . Gd1 . O7 . 70.5(4) yes O6 . Gd1 . O8 . 137.7(3) yes O7 . Gd1 . O8 . 72.6(3) yes N1 . Ni1 . N9 . 90.9(4) yes N1 . Ni1 . N10 . 88.1(5) yes N9 . Ni1 . N10 . 98.6(5) yes N1 . Ni1 . O2 . 94.7(4) yes N9 . Ni1 . O2 . 91.7(4) yes N10 . Ni1 . O2 . 169.3(4) yes N1 . Ni1 . O3 . 90.1(4) yes N9 . Ni1 . O3 . 169.9(4) yes N10 . Ni1 . O3 . 91.5(4) yes O2 . Ni1 . O3 . 78.2(4) yes N1 . Ni1 . O9 . 178.8(4) yes N9 . Ni1 . O9 . 89.5(4) yes N10 . Ni1 . O9 . 90.7(4) yes O2 . Ni1 . O9 . 86.5(3) yes O3 . Ni1 . O9 . 89.7(3) yes W1 . C1 . N1 . 178.0(13) yes W1 . C2 . N2 . 175.8(15) yes W1 . C3 . N3 . 176.1(11) yes W1 . C4 . N4 . 174.8(13) yes W1 . C5 . N5 . 178.0(16) yes W1 . C6 . N6 . 178.5(13) yes W1 . C7 . N7 . 179.8(12) yes W1 . C8 . N8 . 175.5(12) yes O1 . C9 . H93 . 109.3 no O1 . C9 . H92 . 110.3 no H93 . C9 . H92 . 109.2 no O1 . C9 . H91 . 109.0 no H93 . C9 . H91 . 109.6 no H92 . C9 . H91 . 109.5 no C11 . C10 . C15 . 123.5(14) yes C11 . C10 . O1 . 124.6(13) yes C15 . C10 . O1 . 111.9(12) yes C10 . C11 . C12 . 118.9(15) yes C10 . C11 . H111 . 120.4 no C12 . C11 . H111 . 120.7 no C11 . C12 . C13 . 118.8(13) yes C11 . C12 . H121 . 120.5 no C13 . C12 . H121 . 120.7 no C12 . C13 . C14 . 123.0(14) yes C12 . C13 . H131 . 118.7 no C14 . C13 . H131 . 118.3 no C13 . C14 . C15 . 118.4(14) yes C13 . C14 . C16 . 118.0(13) yes C15 . C14 . C16 . 123.7(13) yes C14 . C15 . C10 . 117.3(12) yes C14 . C15 . O2 . 123.1(12) yes C10 . C15 . O2 . 119.5(12) yes C14 . C16 . N9 . 128.7(13) yes C14 . C16 . H161 . 115.9 no N9 . C16 . H161 . 115.4 no C18 . C17 . N9 . 111.2(12) yes C18 . C17 . H171 . 110.0 no N9 . C17 . H171 . 109.0 no C18 . C17 . H172 . 108.0 no N9 . C17 . H172 . 109.1 no H171 . C17 . H172 . 109.5 no C17 . C18 . C19 . 115.4(15) yes C17 . C18 . H181 . 107.6 no C19 . C18 . H181 . 108.0 no C17 . C18 . H182 . 108.1 no C19 . C18 . H182 . 108.0 no H181 . C18 . H182 . 109.6 no C18 . C19 . N10 . 114.4(13) yes C18 . C19 . H191 . 109.1 no N10 . C19 . H191 . 108.0 no C18 . C19 . H192 . 107.3 no N10 . C19 . H192 . 108.4 no H191 . C19 . H192 . 109.6 no C21 . C20 . N10 . 127.0(12) yes C21 . C20 . H201 . 116.5 no N10 . C20 . H201 . 116.5 no C20 . C21 . C22 . 123.8(12) yes C20 . C21 . C23 . 116.7(12) yes C22 . C21 . C23 . 119.5(13) yes C21 . C22 . C26 . 117.6(11) yes C21 . C22 . O3 . 125.1(11) yes C26 . C22 . O3 . 117.4(11) yes C21 . C23 . C24 . 122.0(14) yes C21 . C23 . H231 . 119.0 no C24 . C23 . H231 . 118.9 no C23 . C24 . C25 . 120.2(14) yes C23 . C24 . H241 . 120.0 no C25 . C24 . H241 . 119.8 no C24 . C25 . C26 . 118.7(14) yes C24 . C25 . H251 . 120.9 no C26 . C25 . H251 . 120.4 no C22 . C26 . C25 . 122.0(13) yes C22 . C26 . O4 . 111.5(11) yes C25 . C26 . O4 . 126.6(12) yes O4 . C27 . H273 . 108.7 no O4 . C27 . H272 . 109.7 no H273 . C27 . H272 . 109.8 no O4 . C27 . H271 . 108.9 no H273 . C27 . H271 . 109.8 no H272 . C27 . H271 . 109.9 no Ni1 . N1 . C1 . 160.7(11) yes C17 . N9 . C16 . 119.7(12) yes C17 . N9 . Ni1 . 116.1(10) yes C16 . N9 . Ni1 . 124.2(9) yes C19 . N10 . C20 . 113.6(12) yes C19 . N10 . Ni1 . 122.3(10) yes C20 . N10 . Ni1 . 123.4(9) yes C9 . O1 . C10 . 115.6(11) yes C9 . O1 . Gd1 . 122.8(9) yes C10 . O1 . Gd1 . 119.2(8) yes C15 . O2 . Gd1 . 123.5(8) yes C15 . O2 . Ni1 . 126.6(8) yes Gd1 . O2 . Ni1 . 107.8(4) yes C22 . O3 . Ni1 . 121.5(8) yes C22 . O3 . Gd1 . 124.9(7) yes Ni1 . O3 . Gd1 . 106.9(4) yes C27 . O4 . C26 . 113.3(11) yes C27 . O4 . Gd1 . 125.8(8) yes C26 . O4 . Gd1 . 120.7(7) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C9 . H91 . N5 2_575 172.0 0.959 2.525 3.48(2) yes C12 . H121 . O8 1_455 147.0 0.929 2.552 3.37(2) yes data_shelx _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 Dy N10 Ni O10 W' _chemical_formula_weight 1061.68 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' 'Dy' 'Dy' -0.1892 4.4098 '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' 'Ni' 'Ni' 0.3393 1.1124 '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' 'W' 'W' -0.8490 6.8722 '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/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9520(2) _cell_length_b 13.9264(3) _cell_length_c 27.3934(6) _cell_angle_alpha 90 _cell_angle_beta 93.261(2) _cell_angle_gamma 90 _cell_volume 3409.58(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 102111 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 33.82 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.068 _exptl_crystal_F_000 2048 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_absorpt_coefficient_mu 6.150 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1232 _exptl_absorpt_correction_T_max 0.2800 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46283 _diffrn_reflns_av_unetI/netI 0.0455 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.087 _diffrn_reflns_theta_max 27.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 8196 _reflns_number_gt 7597 _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 'X-Area' _computing_cell_refinement 'X-Area' _computing_data_reduction 'X-Area' _computing_structure_solution 'SHELXS-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0464P)^2^+9.7041P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00071(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8196 _refine_ls_number_parameters 476 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.190 _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 C1 C 0.6538(9) 0.3359(8) 0.0233(3) 0.062(3) Uani 1 1 d . . . . . H1A H 0.6048 0.2892 0.0022 0.093 Uiso 1 1 calc R U . . . H1B H 0.6694 0.3938 0.0053 0.093 Uiso 1 1 calc R U . . . H1C H 0.7485 0.3111 0.0358 0.093 Uiso 1 1 calc R U . . . C2 C 0.6200(6) 0.4239(4) 0.0974(2) 0.0282(11) Uani 1 1 d . . . . . C3 C 0.7424(7) 0.4795(6) 0.0907(3) 0.0405(15) Uani 1 1 d . . . . . H3 H 0.7929 0.4753 0.0621 0.049 Uiso 1 1 calc R U . . . C4 C 0.7902(7) 0.5429(6) 0.1278(3) 0.0469(17) Uani 1 1 d . . . . . H4 H 0.8735 0.5815 0.1239 0.056 Uiso 1 1 calc R U . . . C5 C 0.7147(7) 0.5486(6) 0.1699(3) 0.0447(16) Uani 1 1 d . . . . . H5 H 0.7477 0.5912 0.1943 0.054 Uiso 1 1 calc R U . . . C6 C 0.5883(6) 0.4912(4) 0.1768(2) 0.0299(11) Uani 1 1 d . . . . . C7 C 0.5388(5) 0.4269(4) 0.13983(19) 0.0229(10) Uani 1 1 d . . . . . C8 C 0.5168(7) 0.5042(5) 0.2224(2) 0.0326(12) Uani 1 1 d . . . . . H8 H 0.5695 0.5403 0.2462 0.039 Uiso 1 1 calc R U . . . C9 C 0.3399(10) 0.5058(7) 0.2812(3) 0.054(2) Uani 1 1 d . . . . . H9A H 0.4186 0.4929 0.3061 0.065 Uiso 1 1 calc R U . . . H9B H 0.3266 0.5748 0.2795 0.065 Uiso 1 1 calc R U . . . C10 C 0.2009(10) 0.4628(7) 0.2967(3) 0.058(2) Uani 1 1 d . . . . . H10A H 0.1804 0.4886 0.3285 0.069 Uiso 1 1 calc R U . . . H10B H 0.2163 0.3942 0.3005 0.069 Uiso 1 1 calc R U . . . C11 C 0.0609(9) 0.4791(6) 0.2615(3) 0.0500(18) Uani 1 1 d . . . . . H11A H -0.0289 0.4689 0.2790 0.060 Uiso 1 1 calc R U . . . H11B H 0.0600 0.5448 0.2498 0.060 Uiso 1 1 calc R U . . . C12 C -0.0589(6) 0.3652(5) 0.2092(2) 0.0336(13) Uani 1 1 d . . . . . H12 H -0.1393 0.3765 0.2285 0.040 Uiso 1 1 calc R U . . . C13 C -0.0823(6) 0.2957(5) 0.1705(2) 0.0312(12) Uani 1 1 d . . . . . C14 C -0.2218(6) 0.2474(5) 0.1680(2) 0.0382(15) Uani 1 1 d . . . . . H14 H -0.2922 0.2625 0.1905 0.046 Uiso 1 1 calc R U . . . C15 C -0.2546(7) 0.1796(6) 0.1335(3) 0.0444(17) Uani 1 1 d . . . . . H15 H -0.3471 0.1490 0.1328 0.053 Uiso 1 1 calc R U . . . C16 C -0.1521(7) 0.1551(6) 0.0992(2) 0.0402(15) Uani 1 1 d . . . . . H16 H -0.1746 0.1081 0.0758 0.048 Uiso 1 1 calc R U . . . C17 C -0.0158(6) 0.2024(5) 0.1009(2) 0.0286(11) Uani 1 1 d . . . . . C18 C 0.0201(6) 0.2728(4) 0.1359(2) 0.0276(11) Uani 1 1 d . . . . . C19 C 0.0829(9) 0.0967(6) 0.0412(3) 0.0519(19) Uani 1 1 d . . . . . H19A H 0.1653 0.0913 0.0204 0.078 Uiso 1 1 calc R U . . . H19B H 0.0836 0.0430 0.0632 0.078 Uiso 1 1 calc R U . . . H19C H -0.0093 0.0973 0.0215 0.078 Uiso 1 1 calc R U . . . C20 C 0.2051(6) 0.6085(4) 0.13878(19) 0.0250(10) Uani 1 1 d . . . . . C21 C 0.0793(6) 0.6760(4) 0.0621(2) 0.0279(11) Uani 1 1 d . . . . . C22 C 0.0302(6) 0.7391(4) 0.1776(2) 0.0242(10) Uani 1 1 d . . . . . C23 C -0.0171(6) 0.8369(5) 0.0992(2) 0.0319(12) Uani 1 1 d . . . . . C24 C 0.2349(7) 0.9024(4) 0.1474(2) 0.0318(12) Uani 1 1 d . . . . . C25 C 0.2337(7) 0.8427(5) 0.0568(2) 0.0325(12) Uani 1 1 d . . . . . C26 C 0.4054(7) 0.7227(6) 0.0965(2) 0.0372(14) Uani 1 1 d . . . . . C27 C 0.3344(6) 0.7500(4) 0.1866(2) 0.0270(11) Uani 1 1 d . . . . . Dy1 Dy 0.32822(2) 0.27465(2) 0.07991(2) 0.02110(8) Uani 1 1 d . . . . . N1 N 0.3906(6) 0.4722(4) 0.23366(17) 0.0303(10) Uani 1 1 d . . . . . N2 N 0.0614(5) 0.4133(4) 0.21987(18) 0.0290(10) Uani 1 1 d . . . . . N3 N 0.2139(5) 0.5295(4) 0.14796(18) 0.0293(10) Uani 1 1 d . . . . . N4 N 0.0188(6) 0.6328(5) 0.0314(2) 0.0401(13) Uani 1 1 d . . . . . N5 N -0.0524(6) 0.7291(4) 0.2069(2) 0.0371(12) Uani 1 1 d . . . . . N6 N -0.1228(7) 0.8776(6) 0.0870(2) 0.0523(16) Uani 1 1 d . . . . . N7 N 0.2654(8) 0.9782(5) 0.1583(3) 0.0533(16) Uani 1 1 d . . . . . N8 N 0.2637(9) 0.8871(5) 0.0235(2) 0.0543(17) Uani 1 1 d . . . . . N9 N 0.5215(7) 0.7106(7) 0.0826(3) 0.065(2) Uani 1 1 d . . . . . N10 N 0.4191(7) 0.7470(5) 0.2195(2) 0.0448(14) Uani 1 1 d . . . . . Ni1 Ni 0.25235(7) 0.39921(5) 0.18568(2) 0.02113(14) Uani 1 1 d . . . . . O1 O 0.5617(4) 0.3564(4) 0.06351(15) 0.0337(9) Uani 1 1 d . . . . . O2 O 0.4228(4) 0.3681(3) 0.14234(13) 0.0239(7) Uani 1 1 d . . . . . O3 O 0.1527(4) 0.3160(3) 0.13338(13) 0.0233(7) Uani 1 1 d . . . . . O4 O 0.0968(4) 0.1847(3) 0.06888(15) 0.0319(9) Uani 1 1 d . . . . . O5 O 0.2101(6) 0.4202(4) 0.04860(19) 0.0460(12) Uani 1 1 d D . . . . O6 O 0.2891(5) 0.2705(4) -0.00800(15) 0.0378(10) Uani 1 1 d . . . . . O7 O 0.4541(7) 0.1377(4) 0.04849(19) 0.0512(13) Uani 1 1 d D . . . . O8 O 0.3666(5) 0.1637(3) 0.14437(16) 0.0308(8) Uani 1 1 d D . . . . O9 O 0.2997(4) 0.2633(3) 0.22766(14) 0.0271(8) Uani 1 1 d . . . . . O10 O 0.5848(9) 0.9615(7) 0.0703(7) 0.185(8) Uani 1 1 d . . . . . W1 W 0.18758(2) 0.75945(2) 0.12094(2) 0.01832(8) Uani 1 1 d . . . . . H7W H 0.357(8) 0.197(5) 0.1689(17) 0.04(2) Uiso 1 1 d D . . . . H8W H 0.336(8) 0.109(2) 0.149(3) 0.04(2) Uiso 1 1 d D . . . . H1W H 0.159(7) 0.434(6) 0.0239(16) 0.04(2) Uiso 1 1 d D . . . . H6W H 0.489(10) 0.086(3) 0.058(3) 0.06(3) Uiso 1 1 d D . . . . H2W H 0.201(12) 0.444(8) 0.0757(18) 0.09(4) Uiso 1 1 d D . . . . H5W H 0.451(9) 0.123(6) 0.0195(8) 0.05(2) Uiso 1 1 d D . . . . 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 C1 0.047(4) 0.096(7) 0.046(4) -0.022(5) 0.027(3) -0.017(4) C2 0.024(2) 0.031(3) 0.030(3) 0.001(2) 0.0038(19) -0.003(2) C3 0.032(3) 0.052(4) 0.037(3) 0.004(3) 0.008(2) -0.014(3) C4 0.028(3) 0.050(4) 0.064(5) -0.001(4) 0.006(3) -0.018(3) C5 0.034(3) 0.050(4) 0.050(4) -0.006(3) -0.002(3) -0.015(3) C6 0.027(2) 0.030(3) 0.033(3) -0.004(2) -0.002(2) -0.004(2) C7 0.018(2) 0.025(3) 0.026(2) 0.002(2) 0.0014(17) -0.0019(18) C8 0.036(3) 0.029(3) 0.032(3) -0.008(2) -0.007(2) -0.006(2) C9 0.067(5) 0.065(5) 0.032(3) -0.021(3) 0.010(3) -0.011(4) C10 0.076(5) 0.062(6) 0.036(4) -0.006(4) 0.017(4) -0.017(4) C11 0.064(4) 0.041(4) 0.046(4) -0.011(3) 0.016(3) 0.012(3) C12 0.030(3) 0.040(3) 0.033(3) 0.009(3) 0.015(2) 0.010(2) C13 0.022(2) 0.041(3) 0.030(3) 0.015(3) 0.0017(19) -0.004(2) C14 0.022(3) 0.057(4) 0.036(3) 0.017(3) 0.004(2) -0.002(2) C15 0.027(3) 0.061(5) 0.044(4) 0.017(3) -0.004(2) -0.018(3) C16 0.033(3) 0.053(4) 0.033(3) 0.004(3) -0.005(2) -0.019(3) C17 0.025(2) 0.034(3) 0.025(3) 0.004(2) -0.0033(19) -0.006(2) C18 0.024(2) 0.034(3) 0.024(3) 0.007(2) -0.0027(19) -0.004(2) C19 0.058(4) 0.054(5) 0.044(4) -0.017(3) 0.001(3) -0.020(4) C20 0.027(2) 0.025(3) 0.022(2) -0.002(2) 0.0002(18) -0.0015(19) C21 0.028(2) 0.029(3) 0.026(3) 0.001(2) -0.0001(19) 0.000(2) C22 0.023(2) 0.024(3) 0.026(3) -0.001(2) 0.0051(19) -0.0008(18) C23 0.030(3) 0.034(3) 0.031(3) 0.005(2) -0.001(2) 0.008(2) C24 0.046(3) 0.018(3) 0.031(3) 0.000(2) 0.000(2) -0.003(2) C25 0.046(3) 0.030(3) 0.022(3) 0.003(2) 0.005(2) -0.001(2) C26 0.029(3) 0.057(4) 0.027(3) 0.008(3) 0.009(2) 0.011(3) C27 0.030(3) 0.030(3) 0.021(2) -0.002(2) -0.001(2) -0.003(2) Dy1 0.02191(12) 0.02290(15) 0.01862(13) -0.00207(8) 0.00217(8) -0.00194(8) N1 0.039(2) 0.032(3) 0.020(2) -0.0065(19) -0.0005(18) 0.000(2) N2 0.033(2) 0.030(3) 0.024(2) 0.002(2) 0.0074(17) 0.0031(19) N3 0.036(2) 0.022(2) 0.030(2) 0.0004(19) 0.0058(18) 0.0003(19) N4 0.041(3) 0.049(4) 0.030(3) -0.006(2) -0.006(2) -0.004(2) N5 0.039(3) 0.043(3) 0.030(3) -0.004(2) 0.012(2) -0.004(2) N6 0.046(3) 0.060(4) 0.051(4) 0.007(3) 0.002(3) 0.018(3) N7 0.077(4) 0.027(3) 0.056(4) -0.005(3) 0.001(3) -0.011(3) N8 0.080(5) 0.049(4) 0.034(3) 0.011(3) 0.008(3) -0.013(3) N9 0.042(3) 0.110(7) 0.043(4) 0.014(4) 0.010(3) 0.024(4) N10 0.042(3) 0.059(4) 0.033(3) -0.003(3) -0.008(2) 0.000(3) Ni1 0.0241(3) 0.0207(3) 0.0188(3) -0.0014(2) 0.0031(2) -0.0006(2) O1 0.0272(18) 0.046(3) 0.029(2) -0.0076(19) 0.0115(15) -0.0087(17) O2 0.0228(16) 0.026(2) 0.0235(17) -0.0030(15) 0.0024(13) -0.0057(14) O3 0.0187(15) 0.027(2) 0.0248(17) -0.0033(15) 0.0042(13) -0.0016(14) O4 0.0329(19) 0.034(2) 0.029(2) -0.0074(17) 0.0007(15) -0.0102(17) O5 0.063(3) 0.042(3) 0.032(2) 0.004(2) -0.001(2) 0.013(2) O6 0.034(2) 0.058(3) 0.0210(19) 0.0002(19) 0.0000(16) 0.001(2) O7 0.069(3) 0.049(3) 0.036(3) -0.004(2) 0.008(2) 0.024(3) O8 0.041(2) 0.021(2) 0.030(2) 0.0008(17) 0.0027(17) -0.0016(17) O9 0.0320(19) 0.030(2) 0.0197(17) 0.0011(15) 0.0027(14) 0.0028(15) O10 0.054(4) 0.082(7) 0.41(2) 0.095(10) -0.062(8) -0.005(4) W1 0.02011(11) 0.01848(13) 0.01642(11) 0.00026(7) 0.00142(7) -0.00105(6) _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 C1 O1 1.440(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.362(8) . ? C2 O1 1.400(7) . ? C2 C7 1.407(7) . ? C3 C4 1.394(10) . ? C3 H3 0.9300 . ? C4 C5 1.372(11) . ? C4 H4 0.9300 . ? C5 C6 1.408(8) . ? C5 H5 0.9300 . ? C6 C7 1.404(8) . ? C6 C8 1.445(9) . ? C7 O2 1.328(6) . ? C8 N1 1.269(8) . ? C8 H8 0.9300 . ? C9 C10 1.466(11) . ? C9 N1 1.478(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.554(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.462(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.288(8) . ? C12 C13 1.441(10) . ? C12 H12 0.9300 . ? C13 C18 1.392(8) . ? C13 C14 1.417(8) . ? C14 C15 1.357(11) . ? C14 H14 0.9300 . ? C15 C16 1.392(10) . ? C15 H15 0.9300 . ? C16 C17 1.386(7) . ? C16 H16 0.9300 . ? C17 O4 1.396(7) . ? C17 C18 1.396(8) . ? C18 O3 1.336(6) . ? C19 O4 1.443(8) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N3 1.130(8) . ? C20 W1 2.162(6) . ? C21 N4 1.146(8) . ? C21 W1 2.170(6) . ? C22 N5 1.131(8) . ? C22 W1 2.172(5) . ? C23 N6 1.136(8) . ? C23 W1 2.180(5) . ? C24 N7 1.127(9) . ? C24 W1 2.152(6) . ? C25 N8 1.147(9) . ? C25 W1 2.163(6) . ? C26 N9 1.139(9) . ? C26 W1 2.159(6) . ? C27 N10 1.145(8) . ? C27 W1 2.170(5) . ? Dy1 O2 2.274(4) . ? Dy1 O3 2.282(4) . ? Dy1 O8 2.357(4) . ? Dy1 O7 2.400(5) . ? Dy1 O6 2.414(4) . ? Dy1 O5 2.420(5) . ? Dy1 O4 2.425(4) . ? Dy1 O1 2.444(4) . ? Dy1 Ni1 3.4768(7) . ? N1 Ni1 2.027(5) . ? N2 Ni1 2.005(5) . ? N3 Ni1 2.106(5) . ? Ni1 O3 2.011(4) . ? Ni1 O2 2.033(4) . ? Ni1 O9 2.242(4) . ? O5 H1W 0.820(5) . ? O5 H2W 0.820(5) . ? O7 H6W 0.820(5) . ? O7 H5W 0.820(5) . ? O8 H7W 0.821(5) . ? O8 H8W 0.820(5) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.4(5) . . ? C3 C2 C7 123.4(6) . . ? O1 C2 C7 112.2(5) . . ? C2 C3 C4 118.6(6) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 120.3(6) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.2(6) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 119.1(6) . . ? C7 C6 C8 124.5(5) . . ? C5 C6 C8 116.4(5) . . ? O2 C7 C6 124.8(5) . . ? O2 C7 C2 117.8(5) . . ? C6 C7 C2 117.4(5) . . ? N1 C8 C6 127.6(5) . . ? N1 C8 H8 116.2 . . ? C6 C8 H8 116.2 . . ? C10 C9 N1 115.7(6) . . ? C10 C9 H9A 108.3 . . ? N1 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? N1 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 115.4(7) . . ? C9 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? C9 C10 H10B 108.4 . . ? C11 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? N2 C11 C10 110.7(6) . . ? N2 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N2 C12 C13 126.9(5) . . ? N2 C12 H12 116.5 . . ? C13 C12 H12 116.5 . . ? C18 C13 C14 118.1(6) . . ? C18 C13 C12 125.5(5) . . ? C14 C13 C12 116.4(6) . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 121.0(6) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 118.3(6) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C16 C17 O4 124.2(6) . . ? C16 C17 C18 121.6(6) . . ? O4 C17 C18 114.2(5) . . ? O3 C18 C13 123.6(5) . . ? O3 C18 C17 116.8(5) . . ? C13 C18 C17 119.6(5) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 W1 179.7(6) . . ? N4 C21 W1 178.4(5) . . ? N5 C22 W1 179.5(6) . . ? N6 C23 W1 178.7(6) . . ? N7 C24 W1 175.1(6) . . ? N8 C25 W1 177.3(6) . . ? N9 C26 W1 174.7(8) . . ? N10 C27 W1 175.6(6) . . ? O2 Dy1 O3 67.25(13) . . ? O2 Dy1 O8 77.26(15) . . ? O3 Dy1 O8 76.17(15) . . ? O2 Dy1 O7 124.22(17) . . ? O3 Dy1 O7 141.74(18) . . ? O8 Dy1 O7 72.32(17) . . ? O2 Dy1 O6 142.23(16) . . ? O3 Dy1 O6 125.46(14) . . ? O8 Dy1 O6 137.59(16) . . ? O7 Dy1 O6 70.59(18) . . ? O2 Dy1 O5 85.64(16) . . ? O3 Dy1 O5 73.33(17) . . ? O8 Dy1 O5 148.93(17) . . ? O7 Dy1 O5 137.99(18) . . ? O6 Dy1 O5 68.33(17) . . ? O2 Dy1 O4 131.94(13) . . ? O3 Dy1 O4 66.17(14) . . ? O8 Dy1 O4 80.89(15) . . ? O7 Dy1 O4 87.69(19) . . ? O6 Dy1 O4 77.82(15) . . ? O5 Dy1 O4 92.03(18) . . ? O2 Dy1 O1 65.54(13) . . ? O3 Dy1 O1 128.87(14) . . ? O8 Dy1 O1 110.71(15) . . ? O7 Dy1 O1 83.2(2) . . ? O6 Dy1 O1 84.53(15) . . ? O5 Dy1 O1 84.59(18) . . ? O4 Dy1 O1 162.01(14) . . ? O2 Dy1 Ni1 33.87(9) . . ? O3 Dy1 Ni1 33.38(9) . . ? O8 Dy1 Ni1 74.32(11) . . ? O7 Dy1 Ni1 144.43(13) . . ? O6 Dy1 Ni1 144.98(12) . . ? O5 Dy1 Ni1 77.02(13) . . ? O4 Dy1 Ni1 98.96(10) . . ? O1 Dy1 Ni1 97.49(10) . . ? C8 N1 C9 115.2(5) . . ? C8 N1 Ni1 122.5(4) . . ? C9 N1 Ni1 121.5(4) . . ? C12 N2 C11 117.6(5) . . ? C12 N2 Ni1 124.5(4) . . ? C11 N2 Ni1 117.8(4) . . ? C20 N3 Ni1 162.7(5) . . ? N2 Ni1 O3 91.93(18) . . ? N2 Ni1 N1 98.8(2) . . ? O3 Ni1 N1 168.70(18) . . ? N2 Ni1 O2 169.11(18) . . ? O3 Ni1 O2 77.20(14) . . ? N1 Ni1 O2 91.99(17) . . ? N2 Ni1 N3 91.4(2) . . ? O3 Ni1 N3 95.35(18) . . ? N1 Ni1 N3 87.9(2) . . ? O2 Ni1 N3 90.25(18) . . ? N2 Ni1 O9 89.10(18) . . ? O3 Ni1 O9 86.69(15) . . ? N1 Ni1 O9 90.02(18) . . ? O2 Ni1 O9 89.62(15) . . ? N3 Ni1 O9 177.87(18) . . ? N2 Ni1 Dy1 130.56(15) . . ? O3 Ni1 Dy1 38.63(10) . . ? N1 Ni1 Dy1 130.51(14) . . ? O2 Ni1 Dy1 38.57(10) . . ? N3 Ni1 Dy1 93.16(14) . . ? O9 Ni1 Dy1 88.06(10) . . ? C2 O1 C1 115.5(5) . . ? C2 O1 Dy1 118.8(3) . . ? C1 O1 Dy1 125.5(4) . . ? C7 O2 Ni1 120.9(3) . . ? C7 O2 Dy1 125.0(3) . . ? Ni1 O2 Dy1 107.55(15) . . ? C18 O3 Ni1 125.6(3) . . ? C18 O3 Dy1 124.5(4) . . ? Ni1 O3 Dy1 107.98(15) . . ? C17 O4 C19 115.9(5) . . ? C17 O4 Dy1 118.2(3) . . ? C19 O4 Dy1 123.5(4) . . ? Dy1 O5 H1W 135(6) . . ? Dy1 O5 H2W 95(8) . . ? H1W O5 H2W 125(10) . . ? Dy1 O7 H6W 140(7) . . ? Dy1 O7 H5W 124(6) . . ? H6W O7 H5W 95(8) . . ? Dy1 O8 H7W 103(6) . . ? Dy1 O8 H8W 134(5) . . ? H7W O8 H8W 109(8) . . ? C24 W1 C26 99.2(3) . . ? C24 W1 C20 144.4(2) . . ? C26 W1 C20 77.5(2) . . ? C24 W1 C25 74.6(2) . . ? C26 W1 C25 70.0(2) . . ? C20 W1 C25 133.6(2) . . ? C24 W1 C21 144.7(2) . . ? C26 W1 C21 90.9(2) . . ? C20 W1 C21 70.8(2) . . ? C25 W1 C21 77.4(2) . . ? C24 W1 C27 71.3(2) . . ? C26 W1 C27 74.2(2) . . ? C20 W1 C27 73.8(2) . . ? C25 W1 C27 124.8(2) . . ? C21 W1 C27 143.8(2) . . ? C24 W1 C22 90.2(2) . . ? C26 W1 C22 145.5(2) . . ? C20 W1 C22 75.7(2) . . ? C25 W1 C22 144.2(2) . . ? C21 W1 C22 100.4(2) . . ? C27 W1 C22 77.7(2) . . ? C24 W1 C23 77.3(2) . . ? C26 W1 C23 142.4(2) . . ? C20 W1 C23 126.3(2) . . ? C25 W1 C23 73.1(2) . . ? C21 W1 C23 74.2(2) . . ? C27 W1 C23 135.8(2) . . ? C22 W1 C23 72.0(2) . . ? _refine_diff_density_max 2.665 _refine_diff_density_min -3.743 _refine_diff_density_rms 0.203 _shelxl_version_number 2014-3 _shelx_res_file ; TITL tr16 in P 21/c CELL 0.71073 8.9520 13.9264 27.3934 90.000 93.261 90.000 ZERR 4.00 0.0002 0.0003 0.0006 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H DY N NI O W UNIT 108 128 4 40 4 40 4 MERG 2 OMIT -3.00 56.00 OMIT 1 0 2 OMIT -4 3 1 OMIT -3 5 3 OMIT -9 1 3 OMIT -1 0 2 DFIX 0.820 0.005 O8 H7W O8 H8W DFIX 0.820 0.005 O5 H1W O5 H2W O7 H5W O7 H6W FMAP 2 PLAN 40 ACTA BOND $H L.S. 8 WGHT 0.046400 9.704100 EXTI 0.000710 FVAR 0.37504 C1 1 0.653780 0.335947 0.023349 11.00000 0.04719 0.09588 = 0.04597 -0.02242 0.02735 -0.01719 AFIX 33 H1A 2 0.604829 0.289219 0.002222 11.00000 -1.50000 H1B 2 0.669361 0.393827 0.005296 11.00000 -1.50000 H1C 2 0.748527 0.311135 0.035762 11.00000 -1.50000 AFIX 0 C2 1 0.619999 0.423891 0.097366 11.00000 0.02410 0.03099 = 0.02989 0.00060 0.00381 -0.00272 C3 1 0.742367 0.479516 0.090706 11.00000 0.03241 0.05244 = 0.03719 0.00389 0.00810 -0.01443 AFIX 43 H3 2 0.792930 0.475299 0.062051 11.00000 -1.20000 AFIX 0 C4 1 0.790155 0.542897 0.127774 11.00000 0.02753 0.04958 = 0.06400 -0.00148 0.00585 -0.01830 AFIX 43 H4 2 0.873495 0.581453 0.123934 11.00000 -1.20000 AFIX 0 C5 1 0.714731 0.548611 0.169886 11.00000 0.03362 0.04979 = 0.05021 -0.00611 -0.00217 -0.01550 AFIX 43 H5 2 0.747739 0.591244 0.194308 11.00000 -1.20000 AFIX 0 C6 1 0.588300 0.491157 0.176836 11.00000 0.02706 0.02964 = 0.03267 -0.00401 -0.00246 -0.00396 C7 1 0.538847 0.426948 0.139827 11.00000 0.01832 0.02476 = 0.02572 0.00163 0.00139 -0.00186 C8 1 0.516813 0.504208 0.222357 11.00000 0.03615 0.02884 = 0.03171 -0.00792 -0.00694 -0.00573 AFIX 43 H8 2 0.569471 0.540282 0.246163 11.00000 -1.20000 AFIX 0 C9 1 0.339944 0.505774 0.281166 11.00000 0.06697 0.06466 = 0.03176 -0.02145 0.01045 -0.01131 AFIX 23 H9A 2 0.418632 0.492862 0.306116 11.00000 -1.20000 H9B 2 0.326631 0.574843 0.279489 11.00000 -1.20000 AFIX 0 C10 1 0.200904 0.462774 0.296664 11.00000 0.07644 0.06240 = 0.03585 -0.00633 0.01673 -0.01661 AFIX 23 H10A 2 0.180402 0.488591 0.328483 11.00000 -1.20000 H10B 2 0.216307 0.394185 0.300517 11.00000 -1.20000 AFIX 0 C11 1 0.060881 0.479077 0.261477 11.00000 0.06377 0.04144 = 0.04611 -0.01130 0.01578 0.01200 AFIX 23 H11A 2 -0.028936 0.468918 0.279003 11.00000 -1.20000 H11B 2 0.060038 0.544822 0.249772 11.00000 -1.20000 AFIX 0 C12 1 -0.058931 0.365173 0.209189 11.00000 0.02972 0.03963 = 0.03284 0.00873 0.01490 0.01032 AFIX 43 H12 2 -0.139302 0.376477 0.228479 11.00000 -1.20000 AFIX 0 C13 1 -0.082252 0.295689 0.170546 11.00000 0.02227 0.04105 = 0.03018 0.01457 0.00168 -0.00387 C14 1 -0.221774 0.247410 0.168047 11.00000 0.02215 0.05684 = 0.03596 0.01700 0.00383 -0.00212 AFIX 43 H14 2 -0.292237 0.262507 0.190510 11.00000 -1.20000 AFIX 0 C15 1 -0.254648 0.179580 0.133532 11.00000 0.02749 0.06088 = 0.04403 0.01673 -0.00396 -0.01809 AFIX 43 H15 2 -0.347090 0.148979 0.132764 11.00000 -1.20000 AFIX 0 C16 1 -0.152135 0.155077 0.099244 11.00000 0.03330 0.05305 = 0.03338 0.00387 -0.00501 -0.01940 AFIX 43 H16 2 -0.174602 0.108140 0.075817 11.00000 -1.20000 AFIX 0 C17 1 -0.015791 0.202414 0.100921 11.00000 0.02544 0.03443 = 0.02541 0.00372 -0.00328 -0.00614 C18 1 0.020070 0.272821 0.135937 11.00000 0.02436 0.03388 = 0.02400 0.00697 -0.00272 -0.00393 C19 1 0.082928 0.096724 0.041153 11.00000 0.05781 0.05370 = 0.04381 -0.01737 0.00068 -0.02043 AFIX 33 H19A 2 0.165289 0.091260 0.020361 11.00000 -1.50000 H19B 2 0.083574 0.043049 0.063153 11.00000 -1.50000 H19C 2 -0.009342 0.097345 0.021500 11.00000 -1.50000 AFIX 0 C20 1 0.205085 0.608478 0.138783 11.00000 0.02708 0.02528 = 0.02247 -0.00189 0.00018 -0.00147 C21 1 0.079275 0.676038 0.062117 11.00000 0.02800 0.02946 = 0.02620 0.00097 -0.00007 -0.00005 C22 1 0.030249 0.739147 0.177566 11.00000 0.02280 0.02448 = 0.02565 -0.00126 0.00512 -0.00079 C23 1 -0.017084 0.836874 0.099169 11.00000 0.03034 0.03395 = 0.03107 0.00538 -0.00091 0.00846 C24 1 0.234881 0.902376 0.147363 11.00000 0.04590 0.01817 = 0.03117 0.00018 -0.00031 -0.00311 C25 1 0.233662 0.842658 0.056824 11.00000 0.04560 0.03012 = 0.02210 0.00267 0.00464 -0.00136 C26 1 0.405443 0.722657 0.096507 11.00000 0.02882 0.05703 = 0.02665 0.00768 0.00948 0.01106 C27 1 0.334378 0.749998 0.186594 11.00000 0.02973 0.03041 = 0.02063 -0.00225 -0.00087 -0.00289 DY1 3 0.328223 0.274654 0.079915 11.00000 0.02191 0.02290 = 0.01862 -0.00207 0.00217 -0.00194 N1 4 0.390621 0.472221 0.233657 11.00000 0.03908 0.03151 = 0.01995 -0.00651 -0.00049 -0.00033 N2 4 0.061387 0.413315 0.219871 11.00000 0.03330 0.03015 = 0.02431 0.00195 0.00739 0.00310 N3 4 0.213908 0.529471 0.147965 11.00000 0.03625 0.02211 = 0.02994 0.00042 0.00584 0.00031 N4 4 0.018848 0.632830 0.031356 11.00000 0.04111 0.04864 = 0.02978 -0.00570 -0.00579 -0.00427 N5 4 -0.052378 0.729131 0.206904 11.00000 0.03902 0.04293 = 0.03050 -0.00440 0.01224 -0.00444 N6 4 -0.122759 0.877553 0.086989 11.00000 0.04557 0.06021 = 0.05111 0.00750 0.00152 0.01755 N7 4 0.265371 0.978195 0.158341 11.00000 0.07658 0.02716 = 0.05577 -0.00485 0.00065 -0.01099 N8 4 0.263746 0.887105 0.023530 11.00000 0.08035 0.04884 = 0.03419 0.01092 0.00795 -0.01279 N9 4 0.521468 0.710572 0.082628 11.00000 0.04227 0.10976 = 0.04279 0.01404 0.00982 0.02444 N10 4 0.419074 0.746988 0.219485 11.00000 0.04201 0.05885 = 0.03256 -0.00280 -0.00751 0.00024 NI1 5 0.252353 0.399214 0.185679 11.00000 0.02411 0.02068 = 0.01882 -0.00143 0.00312 -0.00056 O1 6 0.561684 0.356443 0.063513 11.00000 0.02720 0.04587 = 0.02924 -0.00758 0.01147 -0.00868 O2 6 0.422790 0.368085 0.142340 11.00000 0.02275 0.02564 = 0.02351 -0.00295 0.00243 -0.00567 O3 6 0.152681 0.316023 0.133379 11.00000 0.01868 0.02678 = 0.02475 -0.00331 0.00420 -0.00164 O4 6 0.096850 0.184685 0.068879 11.00000 0.03291 0.03394 = 0.02867 -0.00743 0.00067 -0.01016 O5 6 0.210065 0.420169 0.048599 11.00000 0.06346 0.04166 = 0.03231 0.00376 -0.00101 0.01335 O6 6 0.289135 0.270526 -0.007996 11.00000 0.03432 0.05786 = 0.02103 0.00024 0.00002 0.00069 O7 6 0.454052 0.137685 0.048493 11.00000 0.06917 0.04912 = 0.03588 -0.00446 0.00794 0.02421 O8 6 0.366562 0.163714 0.144369 11.00000 0.04087 0.02115 = 0.03033 0.00079 0.00273 -0.00160 O9 6 0.299658 0.263309 0.227656 11.00000 0.03204 0.02975 = 0.01973 0.00106 0.00266 0.00277 O10 6 0.584761 0.961478 0.070345 11.00000 0.05353 0.08214 = 0.40977 0.09481 -0.06168 -0.00485 W1 7 0.187582 0.759446 0.120942 11.00000 0.02011 0.01848 = 0.01642 0.00026 0.00142 -0.00105 H7W 2 0.357115 0.196642 0.168857 11.00000 0.03685 H8W 2 0.335789 0.109345 0.149359 11.00000 0.03729 H1W 2 0.158735 0.434389 0.023900 11.00000 0.04050 H6W 2 0.489196 0.086154 0.057982 11.00000 0.05872 H2W 2 0.200998 0.443863 0.075683 11.00000 0.08688 H5W 2 0.450657 0.123068 0.019462 11.00000 0.04537 HKLF 4 REM tr16 in P 21/c REM R1 = 0.0413 for 7597 Fo > 4sig(Fo) and 0.0454 for all 8196 data REM 476 parameters refined using 6 restraints END WGHT 0.0464 9.7042 REM Highest difference peak 2.665, deepest hole -3.743, 1-sigma level 0.203 Q1 1 0.1718 0.7604 0.0903 11.00000 0.05 2.66 Q2 1 0.2014 0.7617 0.1519 11.00000 0.05 2.58 Q3 1 0.1941 0.6983 0.1217 11.00000 0.05 2.29 Q4 1 0.2025 0.8208 0.1213 11.00000 0.05 2.29 Q5 1 0.3092 0.2769 0.0480 11.00000 0.05 2.14 Q6 1 0.3406 0.2770 0.1121 11.00000 0.05 2.06 Q7 1 0.3215 0.3343 0.0803 11.00000 0.05 1.79 Q8 1 0.3002 0.2143 0.0828 11.00000 0.05 1.61 Q9 1 0.3601 0.2127 0.0784 11.00000 0.05 1.56 Q10 1 0.5906 0.9788 0.0912 11.00000 0.05 1.09 Q11 1 0.1683 0.5387 0.2761 11.00000 0.05 1.07 Q12 1 0.6298 0.9671 0.0372 11.00000 0.05 1.03 Q13 1 0.2424 0.3990 0.1568 11.00000 0.05 0.98 Q14 1 0.2414 0.3362 0.1845 11.00000 0.05 0.83 Q15 1 0.2715 0.3946 0.2182 11.00000 0.05 0.83 Q16 1 0.2445 0.4588 0.1879 11.00000 0.05 0.82 Q17 1 0.1289 0.6853 0.1499 11.00000 0.05 0.78 Q18 1 0.5985 0.4030 0.0105 11.00000 0.05 0.72 Q19 1 0.3923 0.1928 0.0506 11.00000 0.05 0.65 Q20 1 0.2375 0.2524 0.2540 11.00000 0.05 0.64 Q21 1 0.2430 0.6853 0.0947 11.00000 0.05 0.64 Q22 1 0.3430 0.7353 0.1087 11.00000 0.05 0.60 Q23 1 0.2644 0.9218 0.1763 11.00000 0.05 0.60 Q24 1 0.3051 0.2861 -0.0354 11.00000 0.05 0.59 Q25 1 0.2706 0.2278 -0.0088 11.00000 0.05 0.59 Q26 1 0.0087 0.2553 0.1200 11.00000 0.05 0.58 Q27 1 0.5779 0.9315 0.0505 11.00000 0.05 0.58 Q28 1 0.5262 0.2780 -0.0378 11.00000 0.05 0.57 Q29 1 0.2668 0.4768 0.1524 11.00000 0.05 0.55 Q30 1 0.2646 0.3541 0.1076 11.00000 0.05 0.54 Q31 1 0.3245 0.2626 0.1783 11.00000 0.05 0.54 Q32 1 0.3116 0.1791 0.1808 11.00000 0.05 0.53 Q33 1 0.3304 0.2657 0.2572 11.00000 0.05 0.52 Q34 1 0.2161 0.7420 0.0294 11.00000 0.05 0.50 Q35 1 0.6702 0.9415 0.0767 11.00000 0.05 0.50 Q36 1 0.3150 0.0952 0.1297 11.00000 0.05 0.50 Q37 1 0.1595 0.7755 0.2159 11.00000 0.05 0.49 Q38 1 0.1547 0.6457 0.1713 11.00000 0.05 0.49 Q39 1 0.0257 0.6297 0.0610 11.00000 0.05 0.48 Q40 1 -0.1689 0.2941 0.2502 11.00000 0.05 0.48 ; _shelx_res_checksum 74236 _shelx_hkl_file ; 13 0 -1 4.08 20.35 13 0 -1 11.33 22.75 13 0 -1 5.27 17.58 13 0 -2 377.74 26.07 13 0 -2 448.49 25.33 13 0 -2 359.09 20.53 13 0 -3 22.97 23.09 13 0 -3 26.53 17.67 13 0 -3 36.26 20.60 13 0 -4 561.18 28.03 13 0 -4 618.15 23.02 13 0 -4 647.93 28.56 13 0 -5 10.66 23.13 13 0 -5 16.89 17.43 13 0 -5 34.58 26.43 13 0 -6 9.86 18.67 13 0 -6 -14.54 17.67 13 0 -6 25.22 25.69 13 0 -7 11.06 19.42 13 0 -7 16.88 20.93 13 0 -7 7.83 17.84 13 0 -8 454.02 27.03 13 0 -8 523.04 24.48 13 0 -8 619.58 32.94 13 0 -9 14.15 27.39 13 0 -9 31.26 18.31 13 0 -9 -27.17 18.96 13 0 -10 286.51 29.84 13 0 -10 232.24 26.09 13 0 -10 241.97 20.72 13 0 -11 17.33 24.11 13 0 -11 15.31 22.27 13 0 -11 9.00 27.09 13 0 -12 196.08 22.63 13 0 -12 153.37 20.66 13 0 -12 208.82 30.48 13 0 -13 -18.58 22.98 13 0 -13 4.46 23.89 13 0 -13 22.84 26.21 13 0 -14 0.65 20.38 13 0 -14 3.18 26.73 13 0 -14 -7.09 18.30 13 0 -15 -2.34 19.23 13 0 -15 -17.42 20.57 13 0 -15 7.26 30.74 13 0 -16 -9.94 23.07 13 0 -16 37.72 29.80 13 0 -16 40.86 25.03 13 0 -17 16.17 18.57 13 1 -1 1.24 17.85 13 -1 -1 3.19 23.29 13 -1 -1 -6.40 17.26 13 -1 -1 33.22 26.58 13 1 -1 7.91 18.05 13 1 -1 24.56 24.83 13 -1 -2 26.38 24.32 13 1 -2 126.82 19.18 13 1 -2 143.68 25.71 13 1 -2 106.52 18.96 13 -1 -2 89.67 23.12 13 -1 -2 128.33 26.43 13 -1 -3 -16.49 24.06 13 -1 -3 6.60 26.07 13 -1 -3 -16.72 22.08 13 1 -3 30.12 25.13 13 1 -3 41.50 17.94 13 1 -3 33.48 18.38 13 1 -4 6.18 16.99 13 1 -4 30.42 18.24 13 -1 -4 19.09 17.00 13 1 -4 51.78 25.30 13 -1 -4 -27.90 26.81 13 -1 -4 40.65 22.15 13 1 -5 2.22 21.24 13 -1 -5 -6.54 26.20 13 -1 -5 -11.15 23.32 13 1 -5 30.41 18.06 13 1 -5 35.67 18.29 13 -1 -5 17.86 17.28 13 1 -6 -1.58 18.42 13 1 -6 9.58 22.40 13 1 -6 11.78 26.07 13 -1 -6 43.67 19.38 13 -1 -6 46.74 21.18 13 -1 -6 31.69 18.26 13 -1 -7 11.80 19.36 13 1 -7 36.36 21.47 13 1 -7 2.84 18.86 13 1 -7 9.01 17.60 13 -1 -7 -16.67 18.06 13 -1 -7 38.72 25.75 13 1 -8 174.00 20.00 13 1 -8 199.59 20.94 13 1 -8 238.36 29.78 13 -1 -8 170.22 19.28 13 -1 -8 255.71 28.40 13 -1 -8 195.86 21.88 13 1 -9 20.21 19.03 13 -1 -9 23.21 19.43 13 1 -9 8.36 22.83 13 -1 -9 25.97 21.91 13 -1 -9 -10.87 22.16 13 1 -9 44.46 26.81 13 1 -10 221.56 29.62 13 -1 -10 212.44 29.51 13 1 -10 122.41 20.66 13 1 -10 114.46 25.84 13 -1 -10 207.36 26.23 13 -1 -10 126.93 19.49 13 1 -11 22.13 27.09 13 -1 -11 10.13 18.57 13 1 -11 -2.17 18.14 13 1 -11 -7.53 23.35 13 -1 -11 5.05 26.15 13 -1 -11 -19.30 20.99 13 1 -12 92.22 19.75 13 1 -12 188.14 21.04 13 -1 -12 119.82 28.59 13 1 -12 210.95 29.55 13 -1 -12 115.59 20.11 13 -1 -12 132.69 21.54 13 1 -13 44.72 19.98 13 -1 -13 22.60 27.02 13 -1 -13 3.13 24.59 13 -1 -13 19.09 18.30 13 1 -13 29.54 18.58 13 1 -13 11.43 30.65 13 1 -14 432.98 29.47 13 1 -14 359.40 23.82 13 1 -14 391.53 35.70 13 -1 -14 342.22 23.77 13 -1 -14 608.46 34.95 13 -1 -14 442.54 27.08 13 1 -15 6.10 18.80 13 1 -15 -13.84 19.76 13 1 -15 13.67 29.99 13 -1 -15 -24.03 25.05 13 -1 -15 -9.32 26.78 13 -1 -15 1.38 22.75 13 -1 -16 31.25 20.42 13 1 -16 10.51 30.03 13 -1 -16 7.97 18.61 13 -1 -16 14.04 30.77 13 1 -16 26.57 19.32 13 1 -16 45.02 25.95 13 1 -17 20.91 23.54 13 -2 -1 76.27 27.48 13 2 -1 67.31 20.73 13 -2 -1 33.26 18.49 13 2 -1 58.18 21.31 13 2 -1 62.54 18.76 13 -2 -1 62.73 24.96 13 2 -2 284.61 21.18 13 -2 -2 243.56 25.35 13 -2 -2 245.16 20.18 13 2 -2 272.62 23.67 13 -2 -2 280.85 29.38 13 2 -2 185.68 20.00 13 2 -3 76.61 25.55 13 2 -3 17.73 17.86 13 -2 -3 -1.67 18.11 13 -2 -3 10.20 26.55 13 -2 -3 29.46 24.17 13 2 -3 -17.28 18.65 13 -2 -4 730.32 28.57 13 2 -4 620.36 23.97 13 2 -4 975.47 34.26 13 2 -4 671.03 25.01 13 -2 -4 793.29 33.84 13 -2 -4 616.15 30.81 13 2 -5 -6.11 21.50 13 -2 -5 32.72 20.45 13 2 -5 16.55 18.29 13 2 -5 10.27 17.37 13 -2 -5 36.97 22.83 13 -2 -5 16.07 26.66 13 -2 -6 36.41 17.98 13 2 -6 20.62 25.66 13 -2 -6 -17.15 26.18 13 -2 -6 -3.29 19.36 13 2 -6 2.55 17.18 13 2 -6 33.08 18.85 13 2 -7 27.97 18.80 13 -2 -7 0.91 26.65 13 -2 -7 39.72 18.35 13 2 -7 5.49 19.09 13 2 -7 23.22 21.70 13 -2 -7 39.07 20.34 13 -2 -8 672.23 26.32 13 2 -8 807.31 34.85 13 2 -8 622.42 25.45 13 -2 -8 672.64 29.75 13 -2 -8 516.58 27.94 13 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135.66 29.25 12 7 -6 28.49 18.12 -12 -7 6 -16.89 33.64 12 7 -6 -11.84 27.11 12 -7 -6 39.16 28.75 12 7 -6 14.00 19.55 12 -7 -6 11.47 19.95 12 -7 -6 -3.26 17.99 12 7 -7 80.30 19.73 12 7 -7 12.59 17.55 12 7 -7 35.97 26.70 12 -7 -7 1.17 22.71 12 -7 -7 45.19 23.74 12 -7 -7 58.06 24.27 -12 -7 7 -31.71 34.41 12 -7 -8 118.75 24.21 12 -7 -8 70.31 19.56 12 7 -8 139.05 28.58 -12 -7 8 81.42 37.34 12 7 -8 99.21 19.75 12 7 -8 129.21 19.01 12 -7 -8 89.42 20.73 12 -7 -9 -20.62 24.02 12 7 -9 -15.29 21.74 -12 -7 9 59.52 36.88 12 7 -9 33.45 18.85 12 -7 -9 16.80 21.99 12 -7 -9 3.37 18.16 12 7 -9 3.13 27.25 12 -7 -10 53.65 23.15 12 -7 -10 22.58 20.42 12 -7 -10 44.14 22.97 12 7 -10 11.95 26.24 12 7 -10 46.98 18.14 12 7 -10 48.31 19.08 12 -7 -11 50.72 22.65 12 -7 -11 54.61 19.65 12 7 -11 30.49 30.90 12 7 -11 45.89 18.72 12 -7 -11 46.57 24.78 12 7 -11 47.11 19.74 12 -7 -12 157.34 23.74 12 7 -12 71.23 23.68 12 -7 -12 74.98 24.44 12 7 -12 92.61 20.81 12 7 -12 158.38 32.57 12 -7 -12 119.18 21.49 12 7 -13 121.37 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350.18 22.04 11 8 -10 409.05 29.92 11 8 -11 817.58 24.96 11 -8 -11 717.27 29.47 11 8 -11 866.20 26.53 -11 -8 11 1082.85 49.90 11 -8 -11 900.32 33.01 11 -8 -11 912.07 31.79 11 8 -11 1113.55 36.82 11 -8 -12 502.32 32.65 11 -8 -12 375.08 28.29 11 8 -12 522.02 35.84 -11 -8 12 505.05 44.42 11 8 -12 412.58 26.43 11 -8 -12 450.42 26.92 11 8 -12 463.59 23.66 11 -8 -12 401.46 26.18 11 -8 -13 21.94 24.53 11 -8 -13 27.86 23.33 11 -8 -13 5.84 18.68 11 8 -13 3.37 19.06 11 8 -13 -2.80 24.04 11 -8 -13 20.28 21.50 11 8 -13 11.32 24.77 11 8 -14 363.74 36.14 11 -8 -14 290.20 21.99 11 -8 -14 310.27 27.84 11 -8 -14 281.85 24.72 11 8 -14 293.85 22.76 11 8 -14 247.84 25.57 11 -8 -14 347.15 26.64 11 -8 -15 324.27 29.10 11 8 -15 279.09 22.56 11 8 -15 352.86 32.64 11 -8 -15 322.34 26.93 11 8 -15 344.37 22.36 11 -8 -15 250.93 25.88 11 -8 -15 302.30 28.94 11 -8 -16 75.28 24.08 11 -8 -16 66.44 26.67 11 -8 -16 139.78 25.12 11 -8 -16 76.20 26.17 11 8 -16 95.15 30.76 11 8 -16 77.93 21.29 11 8 -17 128.61 37.25 11 -8 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17.81 26.12 11 -9 -3 22.62 18.25 -11 -9 3 -4.00 25.12 11 -9 -3 -17.61 19.87 11 -9 -3 61.62 29.90 11 9 -4 98.08 21.45 11 9 -4 93.79 26.76 11 -9 -4 103.47 24.55 11 -9 -4 125.50 23.52 -11 -9 4 34.80 26.50 11 9 -4 116.33 18.14 11 -9 -4 133.54 24.07 11 9 -5 162.18 27.27 11 -9 -5 148.50 20.83 11 9 -5 153.65 18.15 11 9 -5 142.61 22.15 11 -9 -5 222.29 30.07 11 -9 -5 122.01 19.55 -11 -9 5 148.41 28.16 11 9 -6 273.35 28.64 11 -9 -6 244.65 22.61 11 9 -6 228.33 20.02 11 9 -6 274.75 22.76 -11 -9 6 217.47 35.93 11 -9 -6 348.30 25.19 11 -9 -6 218.88 24.40 11 9 -7 119.81 21.14 -11 -9 7 77.27 35.13 11 -9 -7 179.39 29.11 11 -9 -7 75.31 19.48 11 9 -7 126.21 27.18 11 -9 -7 87.13 20.39 11 9 -7 108.26 18.97 11 9 -8 107.28 22.29 -11 -9 8 126.78 35.15 11 -9 -8 105.70 24.16 11 9 -8 139.13 28.00 11 9 -8 131.06 20.64 11 -9 -8 60.72 23.14 11 -9 -8 159.57 29.82 11 -9 -9 71.10 19.36 11 -9 -9 100.51 23.55 11 9 -9 51.62 25.55 11 -9 -9 77.47 23.06 11 9 -9 88.79 20.95 11 9 -9 21.63 23.15 -11 -9 9 46.12 35.87 11 9 -10 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43.25 27.85 11 -10 -16 58.78 27.24 11 10 -16 30.21 32.15 11 -10 -16 37.33 25.16 11 10 -16 48.71 20.82 11 -10 -16 71.57 28.70 11 -10 -17 148.63 23.73 11 -10 -17 168.24 31.18 11 -10 -17 141.90 25.98 11 -10 -17 153.58 30.93 11 10 -17 145.71 22.65 11 10 -17 205.28 41.21 11 -10 -18 170.04 30.36 11 -10 -18 60.59 26.13 11 -10 -18 71.37 28.19 11 10 -18 119.04 22.67 11 -10 -18 137.42 32.17 11 11 -1 269.60 23.92 11 11 -1 307.36 19.59 -11 -11 1 159.91 33.18 11 -11 -1 313.67 27.69 11 -11 -1 318.57 28.40 11 11 -1 367.02 25.28 11 -11 -1 247.57 22.14 11 11 -2 192.72 27.77 11 -11 -2 85.36 20.25 -11 -11 2 49.71 26.95 11 11 -2 94.11 17.71 11 11 -2 127.06 23.77 11 -11 -2 150.62 30.98 11 -11 -2 141.99 21.37 11 11 -3 94.28 26.80 11 -11 -3 46.14 23.68 11 11 -3 52.52 17.56 11 -11 -3 14.96 21.19 11 11 -3 9.81 21.40 -11 -11 3 22.34 26.58 11 -11 -3 109.65 25.17 11 11 -4 66.81 25.62 11 -11 -4 26.91 19.24 11 11 -4 25.10 17.47 11 11 -4 2.81 26.27 -11 -11 4 45.54 32.10 11 -11 -4 65.11 24.94 11 -11 -4 89.64 30.20 11 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11 11 -10 160.70 29.83 11 -11 -10 109.08 20.25 11 -11 -11 6.05 23.19 11 11 -11 36.82 26.75 11 -11 -11 13.10 20.06 11 -11 -11 -23.15 28.56 11 -11 -11 31.87 20.62 -11 -11 11 18.56 35.81 11 11 -11 43.61 21.21 11 -11 -12 69.02 24.82 11 -11 -12 38.42 27.70 11 11 -12 105.50 28.60 -11 -11 12 17.59 43.85 11 11 -12 103.26 22.38 11 -11 -12 115.94 25.86 11 -11 -12 96.64 23.89 11 -11 -13 0.67 20.53 11 11 -13 32.49 20.82 11 -11 -13 17.56 21.98 11 11 -13 -4.77 23.43 -11 -11 13 23.93 41.71 11 -11 -13 3.63 23.16 11 -11 -13 7.33 22.97 11 11 -14 58.75 22.14 11 11 -14 127.64 29.11 11 -11 -14 66.95 23.71 -11 -11 14 71.09 49.53 11 -11 -14 91.59 27.75 11 -11 -14 103.89 24.14 11 -11 -14 59.80 24.59 11 -11 -15 80.92 30.14 11 -11 -15 72.63 24.19 11 11 -15 184.66 34.53 11 -11 -15 91.99 25.37 -11 -11 15 162.87 47.33 11 11 -15 140.17 23.49 11 -11 -15 164.18 29.51 11 -12 -1 28.68 24.76 -11 -12 1 -18.64 24.95 11 12 -1 22.34 26.84 11 -12 -1 24.68 20.41 11 12 -1 34.06 21.51 11 -12 -1 38.42 21.95 11 12 -1 53.13 22.19 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2 -9 262.70 26.68 10 -2 -9 197.15 18.63 10 -2 -9 246.22 25.97 10 -2 -9 200.28 24.06 10 2 -9 177.03 18.90 10 -2 -10 1904.75 37.69 10 -2 -10 1644.47 30.04 10 2 -10 1687.79 28.05 10 2 -10 1560.91 29.56 10 2 -10 1890.75 38.51 10 -2 -10 1490.87 26.86 10 2 -11 -10.27 25.06 10 -2 -11 26.59 17.96 10 -2 -11 31.71 27.06 10 -2 -11 -14.14 18.75 10 2 -11 -18.16 21.43 10 2 -11 -20.27 23.16 10 2 -12 1295.55 36.90 10 -2 -12 1066.12 26.69 10 2 -12 1136.47 25.96 10 2 -12 968.06 23.54 10 -2 -12 1161.91 29.72 10 -2 -12 1269.30 34.56 10 -2 -13 114.58 18.72 10 2 -13 172.93 24.18 10 -2 -13 176.23 23.73 10 2 -13 129.35 17.78 10 -2 -13 162.83 27.51 10 2 -13 198.64 30.97 10 -2 -14 492.06 23.98 10 2 -14 554.04 22.64 10 -2 -14 636.82 30.51 10 2 -14 584.29 32.84 10 2 -14 517.31 24.15 10 2 -15 7.21 17.09 10 -2 -15 -8.94 18.80 10 2 -15 3.31 28.76 10 -2 -15 22.18 30.81 10 2 -15 9.90 18.96 10 -2 -16 3141.27 55.04 10 2 -16 2898.18 39.69 10 2 -16 2418.65 34.27 10 -2 -16 2745.74 35.80 10 2 -16 3049.90 52.82 10 -2 -16 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3 -27 51.36 20.57 10 3 -27 5.76 25.39 10 3 -28 15.66 24.90 10 -3 -28 7.92 25.70 10 3 -28 1.90 25.03 10 -3 -28 31.87 26.05 10 3 -29 61.35 26.11 10 -3 -29 38.78 29.15 10 -3 -29 57.17 27.37 10 3 -29 48.51 26.02 10 -3 -30 349.46 37.24 10 3 -30 397.87 30.87 10 -3 -30 233.90 34.42 10 3 -30 284.49 30.73 10 4 -1 15.54 19.06 10 -4 -1 -13.78 18.22 10 4 -1 21.66 21.32 10 -4 -1 -13.77 25.88 -10 -4 1 41.86 20.69 10 4 -1 -7.63 20.00 10 -4 -1 -33.42 17.02 10 -4 -2 100.32 18.18 10 -4 -2 97.74 21.31 10 -4 -2 128.73 22.61 10 4 -2 90.83 21.21 10 4 -2 91.53 25.05 10 4 -2 116.67 18.53 -10 -4 2 103.87 22.22 10 4 -3 45.51 24.07 10 -4 -3 37.11 17.45 10 -4 -3 12.59 26.30 10 4 -3 42.20 17.25 -10 -4 3 46.65 22.01 10 -4 -3 9.36 18.40 10 4 -3 9.67 22.83 10 -4 -4 28.32 16.98 10 4 -4 7.59 22.07 10 -4 -4 -11.44 20.17 10 -4 -4 12.46 19.00 10 4 -4 29.25 17.01 -10 -4 4 9.80 27.62 10 4 -4 35.87 20.03 -10 -4 5 47.38 29.05 10 4 -5 80.21 19.29 10 -4 -5 61.60 18.67 10 4 -5 112.70 24.87 10 4 -5 49.92 18.40 10 -4 -5 70.60 21.52 10 -4 -5 60.48 24.19 10 -4 -6 1341.76 33.73 10 4 -6 1191.18 25.18 10 -4 -6 1356.08 28.67 10 -4 -6 1260.63 28.82 -10 -4 6 1287.95 40.40 10 4 -6 1478.73 35.49 10 4 -6 1336.01 26.96 10 -4 -7 426.18 27.00 10 -4 -7 422.83 24.36 10 4 -7 437.04 29.12 10 4 -7 378.98 20.06 -10 -4 7 456.89 33.56 10 4 -7 382.42 21.73 10 -4 -7 477.49 29.63 10 4 -8 11.14 22.86 10 -4 -8 41.66 18.26 -10 -4 8 58.72 31.43 10 4 -8 38.76 17.52 10 -4 -8 60.57 20.87 10 4 -8 56.00 25.69 10 -4 -8 25.96 23.71 10 -4 -9 290.96 21.14 10 4 -9 260.21 19.90 -10 -4 9 312.26 33.83 10 4 -9 247.64 18.97 10 -4 -9 232.28 22.08 10 -4 -9 225.76 19.28 10 4 -9 292.27 27.02 10 4 -10 1465.58 36.33 10 -4 -10 1308.00 27.69 10 -4 -10 1311.82 30.15 10 4 -10 1187.43 27.81 10 4 -10 1380.55 26.14 10 -4 -10 1271.58 28.85 10 4 -11 -11.60 18.22 10 -4 -11 56.24 24.67 10 -4 -11 29.52 18.48 10 -4 -11 26.52 21.13 10 4 -11 48.25 29.81 10 4 -11 54.02 18.67 10 4 -12 1387.40 35.54 10 -4 -12 1349.26 33.63 10 -4 -12 1414.57 31.41 10 -4 -12 1191.88 25.50 10 4 -12 1108.14 24.37 10 4 -12 1309.73 26.29 10 4 -13 405.12 21.00 10 4 -13 449.85 26.14 10 4 -13 489.95 29.34 10 -4 -13 430.60 24.59 10 -4 -13 486.99 29.29 10 -4 -13 510.63 26.49 10 -4 -14 354.89 20.44 10 4 -14 419.16 21.68 10 -4 -14 414.04 27.98 10 4 -14 425.55 31.94 10 4 -14 341.26 24.37 10 -4 -14 432.69 26.83 10 4 -15 182.75 24.46 10 -4 -15 193.09 26.22 10 4 -15 180.26 30.03 10 -4 -15 121.29 22.42 10 -4 -15 159.91 25.49 10 4 -15 141.21 18.77 10 4 -16 2307.87 35.01 10 4 -16 2743.78 35.57 10 4 -16 2991.55 58.35 10 -4 -16 2816.04 46.49 10 -4 -16 2762.84 38.51 10 -4 -16 3677.43 59.75 10 4 -17 124.81 37.24 10 -4 -17 141.13 20.15 10 4 -17 127.98 24.90 10 -4 -17 176.94 30.96 10 4 -17 113.55 20.76 10 -4 -17 198.35 29.90 10 -4 -18 37.55 19.54 10 4 -18 48.53 22.06 10 -4 -18 31.34 27.04 10 -4 -18 43.97 22.17 10 4 -18 35.46 37.37 10 -4 -18 30.37 25.27 10 4 -18 43.49 18.86 10 -4 -19 154.12 26.55 10 4 -19 145.62 21.03 10 -4 -19 190.81 33.62 10 4 -19 129.30 19.97 10 4 -19 136.76 48.96 10 -4 -19 159.94 23.39 10 -4 -20 1193.50 32.43 10 -4 -20 1291.94 40.10 10 4 -20 974.78 27.30 10 4 -20 1238.44 28.81 10 -4 -20 1579.33 42.17 10 4 -21 8.28 18.91 10 -4 -21 3.33 26.12 10 -4 -21 21.95 29.83 10 -4 -21 -3.34 22.82 10 -4 -22 50.34 19.22 10 -4 -22 36.51 30.44 10 4 -22 43.82 23.50 10 -4 -22 23.89 29.52 10 -4 -23 18.97 29.05 10 -4 -23 -3.25 23.34 10 -4 -23 5.40 30.00 10 4 -23 -22.84 19.49 10 -4 -24 57.55 34.39 10 4 -24 63.37 19.94 10 -4 -24 53.76 32.93 10 -4 -24 63.27 24.09 10 -4 -24 36.05 24.38 10 4 -25 66.27 25.01 10 -4 -25 43.87 25.14 10 -4 -25 42.90 24.74 10 -4 -25 36.88 32.65 10 -4 -25 46.10 37.90 10 4 -26 9.64 24.20 10 -4 -26 9.75 25.43 10 -4 -26 6.63 34.82 10 -4 -26 17.11 40.87 10 -4 -27 30.55 45.48 10 4 -27 15.88 20.42 10 -4 -27 4.24 47.68 10 -4 -27 7.94 25.85 10 -4 -28 15.02 26.49 10 4 -28 39.02 20.79 10 -4 -28 32.61 26.77 10 -4 -29 -1.51 29.03 10 -4 -29 26.52 26.37 10 4 -29 -17.94 25.41 10 5 -1 182.02 20.50 10 5 -1 185.03 23.13 10 5 -1 232.64 25.09 10 -5 -1 149.79 23.76 -10 -5 1 184.12 28.88 10 -5 -1 148.26 21.80 10 -5 -1 166.97 23.51 10 5 -2 1537.33 26.04 10 -5 -2 1659.50 32.09 10 -5 -2 1560.03 29.96 10 -5 -2 1537.29 30.90 -10 -5 2 1705.01 38.19 10 5 -2 1611.19 30.66 10 5 -2 1789.70 32.72 -10 -5 3 394.50 29.53 10 5 -3 292.39 19.22 10 -5 -3 279.67 24.34 10 5 -3 380.50 25.00 10 -5 -3 364.05 24.94 10 -5 -3 295.11 26.72 10 5 -3 338.96 27.67 10 -5 -4 626.29 26.40 10 -5 -4 516.02 24.38 -10 -5 4 604.56 28.98 10 -5 -4 499.74 21.45 10 5 -4 547.76 21.03 10 5 -4 632.25 25.69 10 5 -4 635.47 26.47 10 5 -5 510.87 22.88 10 -5 -5 586.98 28.71 10 -5 -5 481.64 22.09 10 -5 -5 609.75 30.96 10 5 -5 535.09 22.20 10 5 -5 621.02 29.89 -10 -5 5 552.65 33.75 10 -5 -6 2320.59 32.76 10 5 -6 2390.99 31.59 10 -5 -6 2667.88 38.80 10 -5 -6 2420.82 36.52 10 5 -6 2861.10 43.69 -10 -5 6 2684.35 48.48 10 5 -6 2407.76 33.31 10 5 -7 254.80 20.55 10 5 -7 300.02 21.44 10 5 -7 335.61 28.62 10 -5 -7 267.11 27.90 10 -5 -7 380.21 29.69 10 -5 -7 269.36 25.03 -10 -5 7 303.33 34.02 10 -5 -8 68.58 21.76 -10 -5 8 15.31 32.06 10 5 -8 42.34 22.76 10 5 -8 10.64 25.14 10 -5 -8 -1.55 26.18 10 -5 -8 -28.94 22.55 10 5 -8 27.19 18.15 10 -5 -9 595.09 22.18 10 -5 -9 653.84 29.45 10 5 -9 604.75 22.32 10 5 -9 724.83 30.28 10 5 -9 577.10 21.02 -10 -5 9 694.01 37.02 10 -5 -9 618.98 24.31 10 5 -10 465.64 20.23 10 -5 -10 447.59 24.83 10 5 -10 558.50 21.35 10 5 -10 572.41 29.98 10 -5 -10 502.22 23.27 -10 -5 10 590.49 39.04 10 -5 -10 615.29 29.20 10 -5 -11 14.71 17.67 10 5 -11 14.47 21.36 10 5 -11 14.73 27.92 -10 -5 11 -7.81 33.22 10 -5 -11 -1.68 24.00 10 5 -11 17.84 18.56 10 -5 -11 -26.55 26.23 10 5 -12 31.38 17.91 10 -5 -12 19.69 21.39 10 5 -12 32.34 28.48 10 5 -12 -6.75 17.28 10 -5 -12 16.02 24.65 10 -5 -13 -14.34 16.78 10 5 -13 -3.87 27.67 10 5 -13 35.73 17.26 10 5 -13 13.97 17.88 10 -5 -13 31.44 24.90 10 5 -14 98.29 22.14 10 -5 -14 116.27 22.84 10 5 -14 91.19 23.13 10 -5 -14 176.68 25.41 10 -5 -14 107.88 24.84 10 5 -14 113.19 28.66 10 5 -15 64.18 17.42 10 -5 -15 57.65 18.29 10 5 -15 65.09 28.85 10 -5 -15 103.36 28.21 10 -5 -15 38.25 24.56 10 5 -15 64.77 18.95 10 -5 -15 80.54 24.63 10 -5 -16 203.33 31.02 10 -5 -16 178.75 23.05 10 -5 -16 234.18 29.65 10 5 -16 220.03 34.74 10 -5 -16 183.00 21.09 10 5 -16 237.34 24.68 10 -5 -17 305.70 25.14 10 -5 -17 281.72 27.79 10 5 -17 318.40 38.16 10 -5 -17 375.75 31.37 10 -5 -17 268.79 22.42 10 5 -17 257.21 20.98 10 5 -18 79.44 38.15 10 -5 -18 138.97 27.63 10 -5 -18 88.07 29.20 10 5 -18 30.61 19.57 10 -5 -18 53.64 18.79 10 5 -19 -3.25 19.38 10 -5 -19 27.56 25.26 10 -5 -19 22.84 18.33 10 -5 -19 34.13 26.56 10 -5 -20 389.20 33.94 10 -5 -20 313.29 25.55 10 -5 -20 291.88 27.90 10 5 -20 296.40 25.94 10 -5 -21 9.61 23.35 10 5 -21 14.39 18.88 10 -5 -21 7.90 26.83 10 -5 -21 14.20 24.68 10 -5 -22 604.16 32.53 10 5 -22 526.09 27.29 10 -5 -22 677.93 37.71 10 -5 -22 482.28 28.78 10 -5 -23 268.24 27.09 10 -5 -23 253.71 32.59 10 5 -23 268.43 22.40 10 -5 -23 272.54 34.50 10 -5 -24 90.59 26.39 10 -5 -24 128.55 22.40 10 -5 -24 126.48 32.05 10 -5 -24 128.39 32.61 10 5 -24 149.82 21.21 10 -5 -25 71.92 34.55 10 -5 -25 73.44 35.56 10 -5 -25 96.45 25.96 10 5 -25 81.41 25.59 10 -5 -26 802.37 36.09 10 5 -26 860.80 27.97 10 -5 -26 829.03 45.87 10 -5 -26 738.70 49.64 10 -5 -27 255.20 31.63 10 5 -27 291.99 28.48 10 -5 -27 244.30 30.42 10 -5 -27 288.55 38.59 10 -5 -27 234.15 45.33 10 -5 -28 15.57 38.03 10 -5 -28 9.71 40.70 10 -5 -28 15.79 26.53 10 5 -28 4.77 25.65 10 -5 -28 13.71 28.62 10 -5 -29 38.98 32.85 10 5 -29 68.19 21.84 10 -5 -29 45.07 30.54 10 -6 -1 42.04 26.53 -10 -6 1 47.57 27.30 10 -6 -1 17.10 17.77 10 6 -1 -18.33 20.02 10 6 -1 8.73 23.01 10 6 -1 50.39 23.37 10 -6 -1 38.85 19.09 10 -6 -2 31.64 22.27 10 6 -2 31.54 19.28 10 6 -2 37.02 20.80 -10 -6 2 -6.82 26.82 10 6 -2 -7.74 23.27 10 -6 -2 6.89 18.62 10 -6 -2 27.53 19.49 10 6 -3 198.81 19.37 10 -6 -3 214.25 23.39 10 -6 -3 165.90 24.40 -10 -6 3 179.05 28.72 10 6 -3 200.34 24.86 10 -6 -3 161.27 18.85 10 6 -3 184.93 17.70 -10 -6 4 22.99 29.74 10 -6 -4 63.98 19.52 10 6 -4 82.65 20.00 10 -6 -4 52.81 22.31 10 -6 -4 67.26 21.49 10 6 -4 42.87 17.40 10 6 -4 97.42 18.34 10 -6 -5 -3.45 17.72 10 -6 -5 -10.90 23.83 -10 -6 5 62.73 29.19 10 6 -5 56.49 24.80 10 6 -5 31.16 18.87 10 -6 -5 -18.01 27.86 10 6 -5 6.66 16.97 10 6 -6 251.70 20.28 10 6 -6 236.39 27.34 10 6 -6 224.59 18.90 10 -6 -6 224.63 21.60 -10 -6 6 282.10 33.24 10 -6 -6 223.24 19.63 10 -6 -6 235.00 23.21 10 6 -7 926.93 24.41 10 6 -7 950.61 32.41 10 6 -7 765.84 22.14 10 -6 -7 974.91 32.98 -10 -6 7 884.51 38.13 10 -6 -7 748.83 25.29 10 -6 -7 805.74 26.99 10 -6 -8 806.18 33.01 10 6 -8 805.86 30.58 10 -6 -8 660.76 29.47 -10 -6 8 832.79 37.48 10 6 -8 724.92 23.24 10 -6 -8 693.83 26.57 10 6 -8 660.37 21.48 -10 -6 9 207.98 35.61 10 6 -9 153.36 19.04 10 6 -9 241.72 27.40 10 -6 -9 150.05 19.50 10 -6 -9 202.36 24.76 10 -6 -9 196.35 20.69 10 6 -9 190.69 25.10 10 6 -10 1511.92 39.48 -10 -6 10 1409.27 46.64 10 -6 -10 1159.64 29.54 10 6 -10 1186.15 28.78 10 -6 -10 1288.56 30.94 10 6 -10 1246.68 26.15 10 -6 -10 1261.52 28.96 10 -6 -11 78.85 19.69 10 6 -11 50.09 19.69 10 6 -11 82.05 28.98 10 6 -11 28.62 23.10 10 -6 -11 74.65 21.17 10 -6 -11 68.43 25.83 -10 -6 11 83.21 37.45 10 -6 -12 1197.15 28.16 10 6 -12 1010.40 24.29 10 -6 -12 1312.77 33.97 10 6 -12 1195.61 25.52 10 6 -12 1344.33 39.17 10 -6 -12 1094.37 29.95 -10 -6 12 1461.90 49.38 10 6 -13 682.46 24.31 10 6 -13 825.15 33.42 10 -6 -13 620.16 23.31 10 -6 -13 760.49 26.12 10 -6 -13 810.40 31.52 10 6 -14 569.26 34.48 10 -6 -14 600.93 31.56 10 -6 -14 455.77 24.19 10 -6 -14 549.56 29.16 10 -6 -14 429.50 22.17 10 6 -14 516.35 22.14 10 -6 -15 248.88 26.78 10 6 -15 193.42 21.21 10 -6 -15 238.53 23.99 10 6 -15 249.13 30.51 10 -6 -15 227.34 22.23 10 -6 -15 287.55 29.58 10 -6 -16 1053.74 32.43 10 6 -16 952.92 25.70 10 -6 -16 1253.27 37.09 10 -6 -16 1030.08 30.09 10 6 -16 1120.36 45.31 10 6 -17 332.97 37.59 10 6 -17 344.21 21.66 10 -6 -17 383.13 30.57 10 -6 -17 288.26 21.50 10 -6 -17 292.57 27.86 10 6 -18 8.35 36.29 10 -6 -18 -3.54 22.47 10 -6 -18 -1.38 24.30 10 6 -18 -6.00 24.06 10 -6 -18 23.85 28.29 10 -6 -18 22.90 19.83 10 -6 -19 536.39 32.94 10 -6 -19 384.81 26.84 10 -6 -19 504.67 29.11 10 -6 -19 479.31 28.72 10 6 -19 470.37 23.88 10 -6 -20 615.01 26.60 10 -6 -20 544.97 28.71 10 -6 -20 633.71 34.77 -10 -6 20 586.31 23.53 10 6 -20 657.38 29.23 10 -6 -20 714.10 34.77 10 -6 -21 5.01 23.45 -10 -6 21 -12.18 18.32 10 -6 -21 8.86 24.92 10 -6 -21 33.19 24.13 10 6 -21 14.68 20.38 10 -6 -21 17.76 26.20 10 6 -22 20.35 24.42 10 -6 -22 23.80 24.07 -10 -6 22 31.36 23.21 10 -6 -22 37.50 24.75 10 -6 -22 34.25 28.08 10 6 -23 48.81 20.48 10 -6 -23 45.72 25.30 -10 -6 23 61.62 24.59 10 -6 -23 54.51 29.22 10 -6 -23 60.42 31.68 -10 -6 24 288.34 26.12 10 6 -24 266.00 27.58 10 -6 -24 318.46 32.61 10 -6 -24 274.46 28.62 10 -6 -24 342.20 35.89 10 -6 -24 277.41 30.34 10 -6 -25 59.81 27.71 10 -6 -25 33.21 26.44 10 -6 -25 53.37 30.65 10 6 -25 97.07 21.13 10 -6 -25 101.31 31.69 -10 -6 25 71.03 25.31 10 -6 -26 19.77 30.37 10 6 -26 -6.22 26.35 10 -6 -26 24.27 28.08 10 -6 -26 24.01 31.54 -10 -6 26 53.34 21.66 10 -6 -26 34.29 30.85 10 6 -27 42.77 21.14 10 -6 -27 32.94 26.65 -10 -6 27 41.49 25.93 10 -6 -27 19.26 34.88 10 -6 -27 11.35 28.72 10 -6 -27 23.31 33.67 10 -6 -28 142.31 38.36 10 -6 -28 123.35 29.27 10 6 -28 141.22 22.80 -10 -6 28 126.44 27.88 10 -6 -28 121.18 41.31 10 -7 -1 112.42 22.88 10 7 -1 69.39 20.80 10 7 -1 90.64 21.68 10 -7 -1 70.43 21.47 10 -7 -1 68.30 23.02 10 7 -1 94.37 17.64 -10 -7 1 46.44 28.25 10 -7 -2 952.75 25.93 -10 -7 2 1087.57 35.90 10 -7 -2 1112.90 32.38 10 -7 -2 1278.14 31.76 10 7 -2 966.85 27.04 10 7 -2 1265.02 33.05 10 7 -2 1108.75 26.31 10 7 -3 1701.39 30.04 10 7 -3 1780.39 30.66 -10 -7 3 1846.74 40.61 10 -7 -3 1586.52 30.28 10 -7 -3 2067.54 40.99 10 -7 -3 1672.53 32.99 10 7 -3 1921.04 33.16 10 -7 -4 566.99 24.81 10 7 -4 720.44 25.25 -10 -7 4 742.72 36.66 10 7 -4 779.88 26.88 10 -7 -4 829.94 30.60 10 -7 -4 646.88 30.78 10 7 -4 567.89 21.69 10 7 -5 224.83 18.33 10 7 -5 256.88 27.06 10 -7 -5 308.79 30.37 10 -7 -5 196.18 22.36 -10 -7 5 235.04 32.32 10 7 -5 251.82 21.36 10 -7 -5 203.01 24.15 10 -7 -6 840.01 30.18 10 7 -6 656.60 22.00 10 -7 -6 938.98 32.37 -10 -7 6 822.04 31.53 10 7 -6 960.13 32.33 10 -7 -6 715.04 24.17 10 7 -6 845.82 25.12 10 -7 -7 194.48 23.77 10 -7 -7 269.75 25.39 10 -7 -7 212.56 21.89 -10 -7 7 256.67 34.25 10 7 -7 279.59 27.32 10 7 -7 279.67 21.38 10 7 -7 199.26 18.60 10 -7 -8 92.84 20.05 10 7 -8 72.65 25.57 10 7 -8 96.61 19.76 10 7 -8 43.52 22.03 -10 -7 8 77.62 32.27 10 -7 -8 80.41 27.96 10 -7 -8 64.24 18.44 10 7 -9 666.27 33.89 10 -7 -9 542.67 25.08 -10 -7 9 612.11 38.46 10 -7 -9 495.24 28.15 10 7 -9 519.21 24.86 10 7 -9 489.98 25.86 10 -7 -9 612.90 31.71 10 7 -10 188.33 24.52 10 -7 -10 181.21 25.20 10 -7 -10 150.66 20.12 -10 -7 10 187.19 35.08 10 7 -10 179.05 25.69 10 -7 -10 190.10 22.82 10 -7 -11 32.32 21.91 10 7 -11 80.33 25.38 10 -7 -11 48.62 24.18 10 -7 -11 50.93 21.97 10 7 -11 53.20 18.44 -10 -7 11 24.74 40.09 10 7 -12 29.60 18.19 -10 -7 12 51.47 35.72 10 -7 -12 11.15 17.96 10 -7 -12 22.69 24.41 10 7 -12 37.03 28.21 10 -7 -12 49.38 25.90 10 -7 -13 79.16 25.99 10 7 -13 86.21 19.16 10 -7 -13 147.19 26.92 -10 -7 13 105.71 38.30 10 7 -13 101.19 29.38 10 -7 -13 86.36 23.90 10 -7 -13 94.11 22.66 10 -7 -14 187.79 27.35 10 7 -14 224.98 29.73 10 -7 -14 181.47 25.82 10 -7 -14 175.96 26.11 10 7 -14 196.53 24.27 10 -7 -14 168.63 23.75 10 7 -15 -3.92 30.38 10 7 -15 55.07 19.12 10 -7 -15 -0.14 23.58 10 -7 -15 -5.65 24.49 10 -7 -15 13.13 20.65 10 -7 -15 -8.72 17.39 -10 -7 16 25.63 18.82 10 -7 -16 13.51 20.06 10 7 -16 28.77 28.60 10 -7 -16 -6.89 18.05 10 -7 -16 14.46 26.17 10 -7 -16 15.91 24.40 10 7 -16 59.62 19.52 10 7 -17 128.05 25.27 10 -7 -17 136.57 27.06 -10 -7 17 150.29 19.90 10 -7 -17 135.97 23.48 10 7 -17 139.25 35.85 10 -7 -17 121.40 22.06 10 -7 -18 240.88 25.09 -10 -7 18 312.84 20.97 10 -7 -18 279.25 27.13 10 7 -18 297.86 21.15 10 7 -18 292.34 48.80 10 -7 -18 382.82 30.31 10 -7 -19 179.63 27.43 10 -7 -19 231.57 29.77 10 7 -19 232.79 21.65 10 -7 -19 231.57 26.54 10 -7 -19 189.76 25.13 -10 -7 19 150.56 21.34 -10 -7 20 201.86 20.25 10 -7 -20 209.73 26.32 10 7 -20 226.21 26.53 10 -7 -20 240.74 26.55 10 -7 -20 280.16 30.72 10 -7 -21 73.75 25.38 10 -7 -21 76.95 24.86 -10 -7 21 92.23 24.83 10 7 -21 85.50 21.37 10 -7 -21 99.82 27.93 10 -7 -22 272.82 30.00 -10 -7 22 282.29 23.28 10 -7 -22 269.91 27.88 10 -7 -22 296.15 28.42 10 7 -22 280.51 27.26 10 -7 -22 361.32 31.73 10 7 -23 451.71 23.84 10 -7 -23 372.26 32.39 10 -7 -23 493.64 34.31 -10 -7 23 356.94 23.67 10 -7 -23 400.62 29.89 10 -7 -23 372.06 30.49 10 -7 -24 59.37 33.41 10 -7 -24 64.72 28.72 10 -7 -24 101.61 30.26 -10 -7 24 53.08 20.99 10 -7 -24 43.57 26.20 10 7 -24 65.21 22.12 10 -7 -25 7.95 28.21 10 -7 -25 7.36 25.42 10 -7 -25 11.81 26.63 -10 -7 25 6.12 20.47 10 7 -25 24.66 21.14 10 -7 -25 49.86 27.89 10 -7 -26 179.21 35.00 10 7 -26 265.81 24.68 10 -7 -26 189.66 34.61 -10 -7 26 209.04 23.82 10 -7 -26 338.58 35.27 10 -7 -26 332.94 36.67 10 -7 -27 63.99 36.30 10 -7 -27 105.26 32.49 10 -7 -27 81.39 27.79 10 7 -27 108.09 22.18 -10 -7 27 53.06 22.74 10 8 -1 281.76 26.14 10 -8 -1 270.69 22.04 10 8 -1 283.40 20.93 -10 -8 1 255.90 24.78 10 -8 -1 269.54 30.07 10 -8 -1 204.44 20.29 10 8 -1 225.85 17.78 -10 -8 2 149.58 24.88 10 -8 -2 105.41 20.76 10 8 -2 157.37 21.41 10 -8 -2 153.60 24.61 10 8 -2 135.01 17.35 10 -8 -2 135.34 24.69 10 8 -2 141.23 20.27 10 -8 -3 4.57 18.74 10 -8 -3 36.99 28.56 10 8 -3 31.39 24.30 -10 -8 3 23.76 28.41 10 8 -3 16.17 16.73 10 8 -3 19.76 19.80 10 -8 -3 1.77 24.59 10 -8 -4 227.52 25.75 10 -8 -4 156.98 19.98 10 8 -4 246.29 26.82 10 8 -4 202.21 20.94 10 8 -4 230.64 18.01 -10 -8 4 238.94 31.27 10 -8 -4 227.47 21.44 10 -8 -5 126.14 24.66 -10 -8 5 124.08 30.41 10 -8 -5 95.94 23.41 10 8 -5 135.48 20.21 10 -8 -5 108.26 29.71 10 8 -5 69.53 18.00 10 8 -5 124.00 25.57 10 -8 -6 350.30 22.74 10 8 -6 503.10 29.22 10 8 -6 339.81 19.69 -10 -8 6 457.18 29.18 10 -8 -6 350.08 21.13 10 8 -6 423.89 22.46 10 -8 -6 416.06 26.07 10 -8 -7 213.54 30.59 10 8 -7 191.60 21.02 10 -8 -7 180.91 23.54 -10 -8 7 208.30 33.52 10 -8 -7 194.63 24.89 10 8 -7 160.63 18.98 10 8 -7 213.19 26.73 10 -8 -8 554.93 23.33 10 -8 -8 742.15 27.99 -10 -8 8 708.20 38.42 10 8 -8 753.19 31.29 10 -8 -8 615.16 28.97 10 8 -8 592.81 22.62 10 8 -8 753.40 24.60 10 -8 -9 724.54 28.56 10 8 -9 845.67 32.89 10 -8 -9 672.06 27.38 10 8 -9 758.20 24.78 -10 -8 9 845.21 40.32 10 -8 -9 727.62 25.87 10 -8 -10 409.40 30.22 10 8 -10 417.56 26.44 10 8 -10 435.52 28.39 10 -8 -10 330.48 22.83 -10 -8 10 456.04 38.46 10 -8 -10 312.75 21.37 10 -8 -11 160.34 20.59 10 -8 -11 139.33 19.16 10 8 -11 188.82 29.61 10 -8 -11 142.09 28.53 -10 -8 11 190.08 38.22 10 8 -11 187.52 24.90 10 8 -12 846.80 25.56 10 -8 -12 809.68 28.69 10 -8 -12 856.02 27.37 10 8 -12 1016.72 33.78 10 -8 -12 929.57 31.27 -10 -8 12 1107.03 53.30 10 -8 -12 921.40 28.56 10 -8 -13 1391.61 32.68 10 -8 -13 1444.10 36.64 10 8 -13 1406.56 28.59 10 -8 -13 1282.82 33.06 10 -8 -13 1333.95 32.90 -10 -8 13 1814.49 62.87 -10 -8 13 1203.65 26.11 10 8 -13 1615.57 43.60 -10 -8 14 261.89 48.70 10 -8 -14 177.53 26.80 10 8 -14 184.72 22.12 10 -8 -14 244.72 27.61 -10 -8 14 206.42 20.80 10 -8 -14 184.43 20.65 10 8 -14 246.93 33.11 10 -8 -14 240.39 24.10 10 -8 -15 -8.35 22.26 -10 -8 15 20.26 18.75 10 8 -15 18.52 19.89 10 8 -15 29.30 28.96 10 -8 -15 34.38 25.95 10 -8 -15 25.71 20.28 10 -8 -16 719.88 26.75 -10 -8 16 697.60 24.10 10 -8 -16 851.23 32.53 10 -8 -16 652.96 28.25 10 8 -16 715.35 28.97 10 8 -16 746.53 39.90 10 -8 -17 250.97 27.48 10 -8 -17 196.13 24.87 10 8 -17 238.49 22.17 10 -8 -17 256.45 29.00 10 8 -17 224.81 35.38 -10 -8 17 231.70 25.03 10 -8 -18 15.32 26.67 -10 -8 18 12.63 19.61 10 -8 -18 5.93 22.45 10 8 -18 18.70 20.60 10 -8 -18 11.04 24.74 10 8 -19 544.72 28.79 10 -8 -19 521.29 29.81 10 -8 -19 593.69 32.99 10 -8 -19 424.02 33.16 -10 -8 19 380.42 28.27 10 -8 -19 407.80 28.71 10 -8 -20 436.79 29.43 -10 -8 20 458.93 22.90 10 -8 -20 520.67 34.77 10 8 -20 422.70 24.47 10 -8 -20 385.21 29.01 10 -8 -21 21.41 29.48 10 8 -21 58.80 21.15 10 -8 -21 25.85 24.08 -10 -8 21 11.02 20.59 10 -8 -21 23.57 25.58 10 -8 -22 37.03 28.60 10 8 -22 4.20 25.71 10 -8 -22 23.56 24.55 10 -8 -22 20.80 24.36 -10 -8 22 37.27 20.38 10 -8 -23 245.64 32.47 10 -8 -23 188.51 31.62 10 8 -23 232.49 22.51 -10 -8 23 183.38 22.96 10 -8 -23 194.46 27.85 10 8 -24 159.71 23.65 10 -8 -24 145.17 27.94 -10 -8 24 127.99 26.49 10 -8 -24 185.79 31.41 10 -8 -24 95.32 28.08 10 -8 -25 8.06 29.11 10 -8 -25 35.32 25.29 10 -8 -25 22.01 28.72 10 8 -25 61.06 26.18 -10 -8 25 13.13 25.91 10 -8 -25 -0.86 25.26 10 -8 -26 8.44 30.12 10 -8 -26 5.97 32.61 -10 -8 26 -12.07 25.81 10 -8 -26 18.72 30.23 10 -8 -26 23.95 35.30 10 8 -26 9.23 21.56 10 -9 -1 100.72 29.67 10 9 -1 85.63 25.79 -10 -9 1 49.11 29.29 10 -9 -1 71.89 19.94 10 9 -1 82.85 25.34 10 9 -1 87.63 17.98 10 9 -2 520.95 29.66 10 -9 -2 418.59 26.38 -10 -9 2 436.15 33.10 10 9 -2 383.18 20.13 10 -9 -2 390.36 24.39 10 9 -2 463.16 28.78 10 -9 -2 529.91 27.95 10 -9 -3 1847.30 35.69 10 9 -3 2392.36 40.30 -10 -9 3 1854.05 39.49 10 -9 -3 2310.42 42.62 10 9 -3 2019.94 37.15 10 -9 -3 1526.97 32.56 10 9 -3 1788.52 32.06 -10 -9 4 59.00 25.01 10 9 -4 115.06 26.27 10 9 -4 60.94 21.47 10 9 -4 64.65 22.45 10 -9 -4 43.73 20.69 10 -9 -4 56.46 25.83 10 -9 -4 98.63 26.03 10 9 -5 232.22 22.70 10 9 -5 285.40 27.10 10 -9 -5 196.62 21.64 -10 -9 5 216.07 27.54 10 -9 -5 164.51 24.74 10 9 -5 201.08 23.22 10 -9 -5 225.93 24.85 10 -9 -6 542.13 29.01 10 -9 -6 556.24 23.86 10 9 -6 652.99 24.77 -10 -9 6 711.11 37.23 10 9 -6 590.38 25.02 10 9 -6 826.98 30.23 10 -9 -6 678.20 29.43 10 -9 -7 266.01 29.95 10 9 -7 275.63 23.08 10 -9 -7 218.11 24.40 10 -9 -7 203.66 21.44 -10 -9 7 245.34 34.89 10 9 -7 206.44 21.29 -10 -9 8 110.19 35.34 10 -9 -8 139.63 23.24 10 -9 -8 99.10 22.96 10 9 -8 131.03 26.59 10 -9 -8 78.14 19.50 10 9 -8 101.23 20.37 10 9 -9 361.30 22.44 -10 -9 9 357.88 36.68 10 -9 -9 262.25 20.45 10 -9 -9 320.55 25.60 10 -9 -9 361.65 30.18 10 9 -9 400.37 28.84 10 -9 -10 483.79 31.82 10 -9 -10 385.46 26.04 10 9 -10 486.76 23.62 10 9 -10 536.96 29.21 10 -9 -10 514.37 28.14 -10 -9 10 578.28 40.57 10 -9 -10 458.56 27.42 -10 -9 11 107.77 36.14 10 9 -11 130.09 21.47 10 9 -11 124.80 24.61 10 -9 -11 89.80 22.36 10 -9 -11 82.60 24.31 10 -9 -11 111.50 22.35 10 -9 -11 102.68 25.91 10 -9 -12 80.10 18.31 10 -9 -12 95.98 24.58 10 9 -12 103.53 28.11 10 9 -12 126.40 25.26 -10 -9 12 118.40 42.83 10 -9 -12 121.69 20.36 -10 -9 12 80.40 19.65 10 -9 -12 108.04 22.28 10 9 -13 100.20 27.17 10 -9 -13 101.14 19.90 10 -9 -13 79.46 18.12 10 9 -13 83.90 24.01 10 -9 -13 78.77 24.41 -10 -9 13 68.27 41.23 10 -9 -13 101.22 27.04 -10 -9 13 94.03 19.50 10 9 -14 85.84 20.84 -10 -9 14 148.87 49.03 10 -9 -14 124.71 25.64 10 -9 -14 169.91 27.01 10 -9 -14 90.58 22.76 -10 -9 14 102.50 19.06 10 -9 -14 112.01 25.46 10 9 -14 123.17 27.54 10 9 -15 25.15 25.24 10 -9 -15 20.78 25.39 -10 -9 15 56.23 50.02 10 9 -15 51.79 20.26 -10 -9 15 29.21 19.45 10 -9 -15 -0.97 25.10 10 -9 -15 34.29 22.24 10 -9 -15 68.04 25.28 10 9 -16 64.82 20.18 10 -9 -16 61.84 22.24 10 -9 -16 38.50 25.50 -10 -9 16 74.53 19.36 10 -9 -16 39.94 25.33 10 -9 -16 56.33 25.75 10 9 -16 49.15 28.36 10 -9 -17 102.62 27.62 -10 -9 17 62.41 19.47 10 9 -17 76.77 34.71 10 -9 -17 60.47 23.67 10 -9 -17 47.22 25.39 10 9 -17 115.92 20.96 10 -9 -17 96.40 26.39 10 9 -18 32.54 25.74 10 -9 -18 39.47 22.87 -10 -9 18 0.50 20.39 10 -9 -18 52.83 21.97 10 -9 -18 24.19 24.72 10 9 -19 229.58 23.28 10 -9 -19 188.99 27.58 -10 -9 19 206.24 26.27 10 -9 -19 207.77 25.78 10 -9 -19 237.80 30.64 10 9 -20 33.88 20.50 10 -9 -20 2.60 28.25 10 -9 -20 -2.63 24.76 10 -9 -20 -1.16 28.48 10 -9 -20 20.67 23.45 -10 -9 20 -4.85 20.50 10 -9 -21 97.75 25.26 10 -9 -21 118.94 30.23 10 -9 -21 77.98 30.17 10 9 -21 127.32 22.46 10 -9 -21 101.31 28.52 -10 -9 21 79.10 20.45 -10 -9 22 209.92 23.18 10 -9 -22 190.43 28.11 10 -9 -22 282.14 32.61 10 9 -22 276.30 29.42 10 -9 -22 243.47 28.80 10 -9 -23 400.47 29.66 10 -9 -23 459.56 35.65 10 9 -23 495.93 25.73 -10 -9 23 275.09 28.48 10 -9 -23 348.48 34.46 10 -9 -24 0.47 30.06 10 -9 -24 1.03 25.11 10 -9 -24 -7.00 29.50 10 -9 -24 32.27 29.30 -10 -9 24 36.92 25.89 10 9 -24 9.96 22.04 10 -9 -25 50.22 29.98 10 -9 -25 17.63 35.10 -10 -10 1 6.92 28.36 10 10 -1 13.23 19.77 10 -10 -1 -8.71 20.24 10 10 -1 45.75 16.84 10 10 -1 24.19 20.85 10 -10 -1 26.86 23.15 10 10 -2 287.14 19.15 -10 -10 2 404.18 32.03 10 -10 -2 397.67 22.18 10 10 -2 417.16 23.26 10 10 -2 512.58 24.21 10 -10 -2 462.90 26.72 10 -10 -3 29.05 23.44 10 10 -3 76.16 25.02 -10 -10 3 37.27 24.89 10 -10 -3 56.95 21.38 10 -10 -3 59.30 28.99 10 10 -3 76.23 20.73 10 10 -3 54.88 25.53 10 10 -4 370.10 27.86 10 10 -4 281.14 22.46 10 -10 -4 330.00 25.83 -10 -10 4 258.24 33.17 10 -10 -4 305.02 26.59 10 -10 -4 245.52 20.83 10 10 -4 280.61 27.07 10 10 -5 24.48 20.69 10 -10 -5 23.19 19.41 -10 -10 5 40.14 30.74 10 -10 -5 18.68 18.45 10 -10 -5 5.86 28.12 10 10 -5 -5.77 19.73 10 10 -5 22.70 20.72 10 -10 -6 430.38 26.60 10 -10 -6 378.31 26.20 -10 -10 6 456.99 36.38 10 10 -6 463.26 24.39 10 10 -6 532.25 29.49 10 -10 -6 468.13 27.10 10 -10 -7 293.45 21.96 -10 -10 7 342.94 35.92 10 -10 -7 360.33 30.01 10 10 -7 451.70 28.62 10 -10 -7 291.58 21.26 10 10 -7 353.85 23.26 10 -10 -8 226.13 26.30 10 -10 -8 197.85 21.06 10 -10 -8 165.82 24.67 -10 -10 8 200.72 36.27 10 10 -8 221.81 21.12 10 10 -8 211.79 27.28 10 -10 -8 232.38 22.52 10 10 -9 392.31 22.50 -10 -10 9 461.48 38.04 10 10 -9 454.25 28.44 10 -10 -9 392.48 26.48 10 -10 -9 389.19 25.99 10 -10 -9 376.12 27.03 10 -10 -9 356.10 25.38 10 -10 -10 15.37 22.58 -10 -10 10 58.62 19.10 10 -10 -10 74.30 28.34 10 -10 -10 46.90 22.92 10 10 -10 56.78 28.01 10 -10 -10 51.14 20.51 -10 -10 10 41.72 34.94 10 10 -10 65.79 20.79 10 -10 -11 88.63 26.89 -10 -10 11 41.27 35.83 10 -10 -11 42.83 18.05 10 -10 -11 59.86 23.42 10 10 -11 49.87 24.20 10 -10 -11 59.28 19.17 10 10 -11 53.87 20.32 -10 -10 11 45.97 22.34 10 -10 -12 217.97 24.18 -10 -10 12 293.69 38.99 10 -10 -12 234.67 26.77 10 -10 -12 218.83 26.14 10 -10 -12 289.84 24.50 -10 -10 12 233.09 20.16 10 10 -12 264.96 22.76 10 10 -12 281.59 29.19 10 -10 -13 766.88 29.90 10 10 -13 1130.76 37.80 -10 -10 13 1209.03 57.84 10 -10 -13 977.73 30.07 -10 -10 13 890.27 24.51 10 -10 -13 1050.96 34.65 10 -10 -13 858.78 27.41 10 10 -13 983.74 28.36 10 -10 -14 36.91 26.98 -10 -10 14 15.87 42.28 10 -10 -14 -14.81 22.78 10 -10 -14 -9.27 25.73 10 -10 -14 21.17 20.05 10 10 -14 14.28 20.80 -10 -10 14 12.81 18.95 10 10 -14 12.04 25.31 -10 -10 15 182.52 51.35 10 10 -15 223.41 21.88 10 10 -15 195.95 27.98 10 -10 -15 119.66 21.73 10 -10 -15 210.99 27.96 -10 -10 15 166.94 20.05 10 -10 -15 147.92 27.36 10 -10 -15 138.07 24.11 10 -10 -16 386.70 30.87 10 -10 -16 385.25 28.79 10 -10 -16 381.55 29.59 10 10 -16 435.66 35.51 -10 -10 16 487.86 58.18 -10 -10 16 336.04 22.44 10 10 -16 454.95 28.68 10 -10 -16 271.41 26.76 10 -10 -17 379.80 32.58 10 -10 -17 387.48 28.68 10 -10 -17 320.31 27.47 -10 -10 17 381.36 22.92 10 10 -17 461.06 29.17 10 -10 -17 367.05 30.10 10 -10 -18 67.76 23.23 10 -10 -18 51.75 23.51 10 -10 -18 57.42 25.62 10 10 -18 34.12 21.52 10 -10 -18 8.44 29.30 -10 -10 18 17.97 19.75 -10 -10 19 342.87 27.81 10 -10 -19 385.37 27.83 10 10 -19 520.19 26.00 10 -10 -19 374.57 24.96 10 -10 -19 263.93 32.42 10 -10 -20 240.58 28.46 10 10 -20 263.21 25.11 10 -10 -20 331.02 32.91 10 -10 -20 203.84 27.84 -10 -10 20 306.56 22.57 10 -10 -21 -6.18 24.56 10 -10 -21 21.45 30.02 10 10 -21 13.74 21.98 10 -10 -21 23.61 25.12 10 -10 -21 27.85 29.51 -10 -10 21 -17.75 20.84 10 10 -22 22.94 27.90 10 -10 -22 23.72 29.12 -10 -10 22 40.90 21.74 10 -10 -22 17.60 29.16 10 -10 -22 31.91 30.14 10 -10 -23 76.64 31.93 -10 -10 23 51.27 27.77 10 10 -23 114.54 23.77 10 -10 -23 72.17 26.95 10 -10 -23 63.92 30.45 10 11 -1 165.28 18.70 10 -11 -1 219.76 28.79 10 11 -1 171.85 27.39 -10 -11 1 140.29 30.21 10 11 -1 240.06 22.33 10 -11 -1 131.41 24.74 10 11 -2 144.00 22.05 10 11 -2 198.93 22.25 10 -11 -2 173.13 24.49 10 -11 -2 119.56 20.62 -10 -11 2 180.92 30.95 10 11 -2 155.52 18.29 10 -11 -3 894.11 30.28 10 -11 -3 753.32 26.82 10 11 -3 988.35 28.42 10 -11 -3 600.09 30.00 10 11 -3 876.45 26.99 -10 -11 3 675.43 32.38 10 11 -3 765.54 26.51 10 11 -4 33.68 21.11 10 11 -4 54.25 21.49 10 -11 -4 43.50 19.20 10 -11 -4 31.30 23.74 10 11 -4 52.92 25.82 10 -11 -4 46.19 29.31 -10 -11 4 77.54 31.80 10 -11 -5 133.24 20.08 -10 -11 5 214.50 32.72 10 -11 -5 143.26 21.25 10 11 -5 233.25 26.41 10 -11 -5 238.95 24.80 10 11 -5 249.20 26.42 10 -11 -6 251.57 25.53 10 11 -6 368.48 24.02 10 -11 -6 390.53 30.34 10 -11 -6 305.64 23.66 10 11 -6 397.60 27.58 -10 -11 6 300.47 35.31 10 -11 -6 269.84 26.47 10 -11 -7 239.95 25.42 10 -11 -7 166.46 21.37 10 -11 -7 168.58 26.47 10 -11 -7 191.50 24.01 10 11 -7 286.68 27.87 10 11 -7 236.16 22.66 -10 -11 7 200.06 34.82 10 -11 -8 147.06 19.65 10 -11 -8 193.79 21.77 -10 -11 8 166.05 35.41 10 11 -8 269.86 22.43 10 -11 -8 137.86 20.52 10 -11 -8 223.36 29.36 10 11 -8 230.61 26.21 10 11 -9 371.15 23.96 10 -11 -9 215.77 21.11 10 -11 -9 347.12 26.12 10 -11 -9 294.38 26.19 10 11 -9 418.54 26.96 -10 -11 9 282.71 20.16 10 -11 -9 368.23 29.72 -10 -11 9 335.87 37.61 -10 -11 10 350.31 24.67 10 -11 -10 251.48 24.25 10 -11 -10 337.89 27.10 10 11 -10 389.97 26.33 10 -11 -10 295.14 22.38 10 -11 -10 320.07 26.08 10 11 -10 341.09 23.48 -10 -11 10 396.28 43.80 -10 -11 11 0.27 40.03 -10 -11 11 24.49 18.15 10 11 -11 2.38 25.98 10 -11 -11 1.50 23.50 10 -11 -11 -15.14 22.69 10 11 -11 40.70 20.74 10 -11 -11 43.93 24.68 10 -11 -11 -15.75 22.58 -10 -11 12 131.62 43.52 10 11 -12 174.04 21.72 10 11 -12 202.62 25.16 10 -11 -12 150.94 20.90 10 -11 -12 166.71 25.83 10 -11 -12 151.31 23.64 10 -11 -12 214.75 28.61 -10 -11 12 171.87 20.39 10 11 -13 11.11 25.72 10 -11 -13 46.21 24.72 10 -11 -13 -5.37 21.85 -10 -11 13 42.21 23.10 10 -11 -13 37.44 24.42 -10 -11 13 18.21 40.88 10 -11 -13 5.33 27.19 10 11 -13 -15.98 20.90 10 -11 -14 196.20 22.98 10 -11 -14 139.50 24.16 10 -11 -14 170.09 25.90 10 11 -14 197.85 22.32 -10 -11 14 125.95 45.13 10 11 -14 203.76 28.58 -10 -11 14 154.60 20.12 10 -11 -14 170.72 27.68 10 -11 -15 -29.88 21.42 10 11 -15 17.38 27.80 10 -11 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52.27 23.29 9 11 -21 60.13 22.19 9 -11 -21 43.70 33.00 9 -11 -21 51.00 20.54 9 11 -22 110.16 22.51 9 -11 -22 47.45 35.00 9 -11 -22 46.42 29.60 -9 -11 22 72.21 20.62 9 -11 -22 54.78 24.80 9 -11 -22 84.19 29.47 9 -11 -23 21.54 32.45 9 -11 -23 17.95 24.94 -9 -11 23 -0.75 21.26 9 -11 -23 16.93 38.66 9 11 -23 -25.63 22.67 9 -11 -23 3.79 28.82 9 -11 -24 149.97 22.99 9 -11 -24 223.29 43.59 -9 -11 24 156.03 23.03 9 11 -24 250.17 29.56 9 -11 -24 185.42 37.82 9 -11 -24 202.72 32.70 9 -11 -25 248.37 44.37 9 -11 -25 249.02 33.48 9 -11 -25 206.90 28.69 -9 -11 25 179.04 24.21 9 -11 -25 185.33 50.79 9 11 -25 273.31 25.78 -9 -12 1 803.98 29.75 9 -12 -1 805.57 26.19 9 12 -1 1102.96 28.07 -9 12 1 1163.29 29.08 9 12 -1 1032.72 31.95 9 -12 -1 911.68 28.10 -9 -12 2 291.91 31.04 -9 12 2 351.26 27.71 9 12 -2 357.68 28.26 9 -12 -2 276.82 22.90 9 -12 -2 330.63 28.80 9 12 -2 426.71 22.51 -9 12 3 21.16 24.21 9 12 -3 10.87 19.63 -9 -12 3 26.04 23.68 9 12 -3 28.81 19.47 9 -12 -3 28.33 21.98 9 -12 -3 48.80 23.02 9 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606.64 24.53 9 -12 -10 655.96 29.90 9 12 -10 839.60 29.80 -9 -12 10 564.23 22.49 9 12 -10 766.11 26.53 9 -12 -10 689.51 27.80 -9 -12 10 794.38 41.33 9 -12 -10 535.43 27.00 9 -12 -11 350.08 24.14 9 -12 -11 366.33 25.93 -9 -12 11 282.81 20.28 9 12 -11 404.83 24.07 9 -12 -11 312.10 27.58 9 12 -11 448.50 26.48 -9 -12 11 418.65 43.27 9 -12 -11 253.38 25.10 -9 -12 12 21.09 39.19 -9 -12 12 -13.59 22.68 9 12 -12 6.08 21.78 9 12 -12 22.07 21.02 9 -12 -12 27.00 19.26 9 -12 -12 8.77 24.16 9 -12 -12 21.95 21.57 9 -12 -12 15.47 25.95 -9 -12 13 30.17 39.52 9 -12 -13 24.29 19.38 9 12 -13 48.17 25.51 9 -12 -13 38.52 22.40 9 12 -13 27.06 21.21 -9 -12 13 41.94 19.66 9 -12 -13 10.34 24.59 9 -12 -13 14.94 22.09 9 -12 -14 183.38 25.53 -9 -12 14 209.89 49.11 9 12 -14 234.06 28.03 9 -12 -14 179.10 22.69 9 12 -14 225.53 27.71 9 -12 -14 163.48 28.52 9 -12 -14 123.77 23.65 -9 -12 14 115.13 20.88 9 -12 -15 566.88 29.28 9 -12 -15 726.33 26.17 -9 -12 15 693.99 24.94 9 12 -15 1008.94 39.28 9 -12 -15 858.59 32.93 -9 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30.47 8 -7 -28 161.97 33.85 8 7 -28 270.36 22.09 -8 -7 28 163.00 26.61 8 -7 -28 159.82 42.69 8 -7 -28 113.82 28.36 8 -7 -29 124.89 28.71 8 -7 -29 179.91 34.68 8 7 -29 270.68 28.32 8 -7 -29 231.80 44.50 -8 -7 29 258.89 26.35 8 -7 -29 149.27 31.64 8 -7 -30 532.56 50.68 8 -7 -30 373.78 40.13 8 -7 -30 399.96 43.31 8 -7 -30 415.96 36.02 8 7 -30 573.81 26.32 -8 -7 30 450.45 26.02 -8 -7 31 72.94 23.60 8 -7 -31 66.05 34.96 8 -7 -31 67.90 31.92 8 7 -31 82.17 21.90 8 -7 -31 73.89 41.59 8 7 -32 238.92 28.44 -8 -7 32 140.00 29.56 8 -7 -32 175.38 39.24 8 -7 -32 207.47 52.62 8 -7 -32 148.00 42.27 8 -7 -33 332.23 52.84 8 -7 -33 298.76 49.17 -8 -7 33 224.32 27.10 8 8 -1 60.38 19.49 -8 8 1 36.83 20.21 8 -8 -1 40.72 20.22 -8 -8 1 62.04 26.76 8 8 -1 35.37 24.72 8 -8 -1 64.23 28.12 -8 8 2 175.15 24.49 8 -8 -2 157.70 19.55 8 8 -2 152.00 20.46 8 8 -2 176.73 25.34 -8 -8 2 95.55 28.08 8 -8 -2 159.53 28.41 8 -8 -3 1377.67 31.28 8 8 -3 1483.82 33.43 8 8 -3 1449.63 27.92 -8 8 3 1576.60 30.00 -8 -8 3 1187.28 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7 -1 -30 513.46 33.48 -7 -1 30 380.13 26.10 7 -1 -30 359.66 28.18 7 1 -30 424.01 30.61 -7 -1 31 33.46 20.30 7 1 -31 31.44 28.49 7 -1 -31 93.23 29.93 7 -1 -31 68.39 25.40 7 1 -32 1660.18 40.44 -7 -1 32 1399.98 35.17 7 -1 -32 1478.95 42.65 7 -1 -32 1042.50 38.98 7 -1 -33 -11.70 27.48 7 1 -33 -17.68 29.80 -7 -1 33 21.22 25.97 7 -1 -33 40.44 36.01 7 -1 -34 1156.38 42.80 -7 -1 34 1083.83 34.80 7 1 -34 1096.29 38.72 7 -1 -34 863.77 35.12 -7 -1 35 15.64 27.21 7 -1 -35 39.65 31.99 7 -1 -35 24.73 30.56 7 1 -35 10.61 30.17 7 1 -36 246.92 33.79 -7 -1 36 166.52 30.92 7 -1 -36 170.89 34.28 7 -1 -36 249.81 34.44 7 -1 -37 -2.90 31.54 7 -1 -37 18.48 31.61 7 1 -37 49.47 35.29 7 2 -1 237.03 19.61 -7 -2 1 89.70 27.89 7 2 -1 121.58 26.05 7 -2 -1 33.87 20.04 -7 -2 2 7197.68 65.63 7 2 -2 7183.61 49.69 7 -2 -2 7251.26 55.16 7 2 -2 7665.56 52.52 7 2 -2 7167.07 62.20 7 -2 -2 6785.84 60.43 7 -2 -3 109.17 26.83 7 2 -3 216.45 29.11 -7 -2 3 184.70 24.50 7 -2 -3 129.78 19.70 7 2 -3 183.24 21.06 7 2 -3 195.67 20.25 7 2 -4 3321.84 43.51 7 -2 -4 3193.94 42.72 7 -2 -4 3189.56 36.99 -7 -2 4 3108.83 45.48 7 -2 -4 3124.55 35.29 -7 -2 5 828.93 31.73 7 2 -5 831.58 29.70 7 -2 -5 738.94 22.08 7 -2 -5 767.59 25.91 7 2 -6 1128.15 26.80 7 2 -6 1157.66 31.71 -7 -2 6 1105.72 33.22 7 -2 -6 1140.72 31.06 7 2 -7 183.38 25.11 7 2 -7 167.39 17.85 -7 -2 7 185.62 21.06 7 -2 -7 147.37 20.96 -7 -2 8 755.83 31.84 7 -2 -8 772.87 21.50 7 2 -8 770.27 30.42 7 -2 -8 773.76 27.15 7 2 -8 784.50 21.37 7 -2 -9 37.96 23.18 7 -2 -9 29.10 16.32 -7 -2 9 53.61 26.47 7 2 -9 39.23 25.02 7 2 -9 90.65 17.96 7 -2 -10 21.91 20.49 7 -2 -10 40.87 23.37 7 2 -10 42.75 23.90 7 2 -10 44.39 16.72 -7 -2 11 98.97 16.26 7 2 -11 113.75 18.87 7 -2 -11 130.46 18.42 7 2 -11 146.48 30.61 7 -2 -11 112.36 25.46 -7 -2 12 9.55 15.95 7 -2 -12 37.04 22.66 7 2 -12 16.24 30.17 7 -2 -12 2.96 28.16 7 -2 -13 1206.25 36.24 7 -2 -13 1184.96 26.13 -7 -2 13 1105.35 23.11 7 2 -13 1228.64 40.27 7 -2 -14 257.86 24.11 7 -2 -14 234.61 32.03 -7 -2 14 250.05 18.91 7 2 -14 279.83 35.17 7 -2 -14 243.48 23.55 7 -2 -15 7.13 23.81 7 -2 -15 13.34 20.96 7 -2 -15 33.30 20.68 7 2 -15 7.13 33.62 -7 -2 15 25.45 20.80 7 -2 -16 19.64 21.05 7 -2 -16 14.26 20.64 7 -2 -16 35.37 28.55 7 2 -16 37.78 33.47 -7 -2 16 22.15 19.79 7 -2 -16 29.73 26.71 7 2 -17 338.19 41.46 7 -2 -17 277.06 20.53 7 -2 -17 301.72 20.44 7 -2 -17 375.71 28.61 -7 -2 17 305.61 19.60 7 -2 -17 344.77 27.73 7 2 -17 313.32 20.29 7 -2 -18 4152.58 47.54 7 2 -18 4444.52 120.39 7 -2 -18 4024.92 44.03 7 -2 -18 4982.78 70.75 -7 -2 18 4057.24 42.35 7 2 -18 3965.25 41.49 7 -2 -18 4746.25 73.13 -7 -2 19 -0.14 18.23 7 -2 -19 -15.82 36.60 7 -2 -19 -5.30 21.81 7 2 -19 9.72 19.07 7 -2 -19 -33.54 19.19 7 -2 -19 19.52 27.35 -7 -2 20 315.91 21.94 7 2 -20 312.18 19.68 7 -2 -20 320.99 30.92 7 -2 -20 292.45 22.98 7 -2 -20 301.83 22.80 7 -2 -20 401.17 36.23 -7 -2 21 371.92 23.65 7 -2 -21 417.26 41.63 7 -2 -21 386.49 25.00 7 -2 -21 372.94 34.91 7 -2 -21 325.51 20.16 7 2 -21 345.56 24.98 7 -2 -22 2467.17 61.52 7 -2 -22 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47.35 4 13 -8 2667.55 35.73 -4 -13 9 16.20 20.51 4 13 -9 6.71 26.97 4 -13 -9 41.62 30.74 4 -13 -9 26.94 27.46 -4 13 9 12.98 23.51 -4 -13 9 -0.40 25.22 -4 -13 10 221.83 21.60 4 -13 -10 262.57 36.04 4 -13 -10 270.60 22.94 -4 13 10 330.31 28.26 4 13 -10 401.70 27.90 -4 -13 10 204.28 26.00 -4 13 11 323.77 31.03 -4 -13 11 198.89 26.69 -4 -13 11 237.89 27.25 4 -13 -11 236.94 38.24 4 -13 -11 277.58 29.12 4 13 -11 387.54 24.76 4 -13 -12 2677.98 38.62 -4 13 12 3508.06 64.37 -4 -13 12 2114.40 39.65 4 13 -12 3772.40 39.24 4 -13 -12 2536.31 60.50 -4 -13 12 2285.92 33.65 4 13 -13 307.35 22.66 4 -13 -13 186.73 32.19 4 -13 -13 207.89 40.72 -4 -13 13 168.61 26.06 -4 -13 13 191.09 27.04 -4 -13 14 96.19 21.08 4 -13 -14 162.69 24.13 4 -13 -14 193.69 35.56 4 13 -14 221.76 26.25 4 -13 -14 146.96 41.86 -4 -13 14 156.53 29.05 -4 -13 15 14.82 20.55 4 -13 -15 14.36 22.58 4 -13 -15 0.62 45.36 4 -13 -15 4.81 37.04 -4 -13 15 10.25 24.21 4 13 -15 17.92 24.70 -4 -13 16 218.40 25.52 4 -13 -16 353.01 50.44 4 -13 -16 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62.01 20.57 0 -9 38 102.52 30.76 0 10 0 1792.56 37.65 0 -10 0 1455.12 36.73 0 10 -1 3158.45 41.50 0 -10 1 2776.97 38.57 0 -10 1 2473.73 41.03 0 -10 -1 2639.19 49.18 0 10 1 3171.18 43.27 0 10 -2 307.47 23.24 0 10 2 278.06 30.93 0 -10 2 310.93 32.96 0 -10 -2 301.29 30.01 0 -10 2 345.51 29.47 0 10 3 5468.90 62.59 0 -10 3 4046.56 50.61 0 -10 -3 4050.15 56.21 0 10 -3 4935.40 49.88 0 -10 3 4516.96 48.76 0 10 4 2484.87 45.99 0 -10 -4 1954.51 47.53 0 10 -4 2345.03 35.52 0 -10 4 2171.83 37.64 0 -10 4 2054.03 41.90 0 10 5 128.72 26.73 0 10 -5 89.96 20.67 0 -10 5 123.40 23.15 0 -10 5 121.52 24.94 0 -10 -5 127.87 25.69 0 10 6 568.08 31.15 0 10 -6 511.82 24.24 0 10 6 576.80 23.05 0 -10 -6 410.42 28.90 0 -10 6 421.15 25.75 0 -10 6 395.32 31.22 0 -10 -6 394.11 22.91 0 10 -7 2481.84 36.60 0 -10 -7 1999.89 34.65 0 10 7 2785.23 34.17 0 -10 7 2148.67 42.19 0 -10 7 1716.05 37.04 0 -10 -7 2005.63 44.89 0 10 7 2812.33 51.97 0 10 -8 3817.19 44.66 0 10 8 4396.34 65.31 0 -10 8 2620.05 39.60 0 10 8 4080.72 39.42 0 -10 8 3376.45 48.71 0 -10 -8 2747.65 34.45 0 -10 -8 3256.75 54.60 0 -10 -9 1055.73 40.59 0 10 -9 1064.86 28.20 0 10 9 1176.56 25.10 0 -10 9 967.32 35.64 0 -10 -9 741.67 23.39 0 10 9 1306.49 42.64 0 -10 9 744.44 28.41 0 -10 -10 7.10 30.03 0 10 -10 5.84 20.19 0 -10 10 -13.96 20.94 0 10 10 44.95 22.26 0 -10 -10 -10.40 18.88 0 10 10 19.15 31.18 0 -10 11 140.41 22.73 0 10 11 324.99 20.95 0 10 11 370.62 40.19 0 -10 -11 227.51 19.27 0 -10 -11 327.60 35.48 0 10 -11 323.86 22.42 0 -10 -12 1978.02 58.16 0 10 12 2454.86 69.21 0 10 -12 2113.56 32.66 0 10 12 2101.70 30.72 0 -10 12 1959.05 37.16 0 -10 -12 1501.31 30.82 0 -10 12 1375.23 30.13 0 10 -13 7.79 20.42 0 10 13 26.76 22.23 0 -10 13 -15.55 26.55 0 -10 13 36.24 21.41 0 -10 -13 -8.49 17.78 0 10 -14 33.04 24.44 0 -10 14 15.31 24.49 0 10 14 21.56 17.96 0 -10 14 1.07 21.16 0 -10 -14 15.68 17.86 0 10 -15 266.38 22.00 0 -10 -15 215.04 23.30 0 10 15 261.56 19.62 0 -10 15 201.78 25.93 0 -10 15 245.60 27.33 0 10 -16 834.17 29.81 0 -10 16 792.42 32.07 0 10 16 836.49 26.44 0 -10 16 713.25 29.58 0 -10 16 573.13 24.33 0 -10 -16 566.34 20.96 0 10 -17 2326.30 32.42 0 -10 17 2267.19 42.46 0 -10 17 1967.32 38.23 0 10 17 2328.33 34.50 0 -10 -17 1719.03 28.58 0 -10 17 1720.26 30.94 0 10 -18 751.28 24.06 0 -10 18 572.20 30.22 0 10 18 732.52 23.48 0 -10 18 581.47 24.08 0 -10 -18 567.61 26.00 0 -10 18 663.84 30.21 0 10 -19 597.65 22.99 0 -10 19 521.54 29.14 0 -10 19 445.58 27.23 0 10 19 561.49 22.57 0 -10 19 444.80 23.64 0 -10 -19 464.89 20.74 0 10 -20 799.13 27.80 0 -10 20 636.18 31.25 0 10 20 638.46 23.60 0 -10 20 566.19 28.68 0 -10 20 586.89 30.19 0 -10 -20 569.09 21.81 0 10 -21 1448.96 27.37 0 -10 -21 1115.95 28.03 0 -10 21 1352.93 38.15 0 -10 21 1139.06 32.20 0 10 21 1359.80 27.17 0 -10 21 1141.96 28.19 0 -10 22 847.74 36.22 0 10 22 867.33 25.23 0 -10 22 676.55 29.19 0 -10 22 658.56 25.74 0 -10 -22 643.26 26.16 0 10 -22 882.70 23.95 0 -10 23 2951.20 59.01 0 10 23 2795.80 39.43 0 -10 23 2242.56 43.02 0 -10 23 2169.42 33.03 0 -10 -23 2118.05 31.82 0 10 -23 2680.13 32.21 0 -10 24 1036.02 35.11 0 10 24 1430.64 32.67 0 -10 24 1047.08 27.39 0 10 -24 1287.62 25.34 0 -10 -24 993.60 24.87 0 -10 24 1455.16 49.02 0 -10 25 6.61 39.77 0 10 -25 32.03 18.42 0 -10 25 -14.59 26.09 0 10 25 22.86 20.50 0 -10 25 36.32 26.07 0 -10 -25 12.79 22.98 0 -10 26 210.06 43.71 0 -10 26 170.16 23.56 0 10 26 168.39 26.58 0 -10 26 141.85 26.89 0 -10 -26 154.53 24.00 0 10 -26 192.38 23.96 0 -10 27 2351.66 68.37 0 10 27 2179.60 37.60 0 -10 27 1611.11 43.27 0 -10 27 1732.41 32.57 0 -10 -27 1535.81 28.62 0 10 -27 2003.17 32.21 0 10 28 847.33 28.01 0 -10 28 648.99 36.47 0 -10 28 1014.18 56.52 0 -10 28 648.36 26.81 0 10 -28 764.04 26.23 0 -10 -28 587.08 23.77 0 10 29 328.68 29.25 0 -10 29 262.35 32.57 0 -10 -29 298.73 24.99 0 -10 29 394.41 29.41 0 10 -29 357.63 24.04 0 -10 29 494.80 52.16 0 10 30 162.19 28.43 0 -10 30 90.43 32.03 0 10 -30 131.09 23.19 0 -10 30 111.88 23.61 0 -10 -30 113.05 23.74 0 -10 30 130.23 54.18 0 10 31 188.52 29.10 0 -10 31 100.74 36.58 0 10 -31 122.17 18.63 0 -10 31 150.32 24.62 0 -10 -31 97.20 24.33 0 -10 32 62.06 23.97 0 -10 -32 95.12 24.31 0 10 32 59.25 30.66 0 -10 32 62.19 38.50 0 10 -32 99.84 22.16 0 -10 -33 229.06 22.43 0 -10 33 336.73 26.97 0 -10 33 273.41 49.00 0 10 -33 330.74 24.39 0 10 33 420.62 28.67 0 -10 33 378.47 65.64 0 -10 -34 298.81 23.07 0 -10 34 462.83 26.72 0 -10 34 414.40 59.07 0 10 -34 450.44 25.03 0 10 34 600.92 31.01 0 -10 34 447.23 68.50 0 10 -35 22.91 22.62 0 -10 -35 -3.08 23.58 0 10 35 35.40 31.99 0 -10 35 19.94 24.15 0 10 -36 110.58 23.16 0 10 36 103.74 34.32 0 -10 36 27.81 24.08 0 -10 -36 70.28 24.73 0 10 -37 14.58 19.04 0 10 37 36.10 34.59 0 -10 37 -41.35 24.01 0 -10 -37 25.78 24.64 0 11 0 36.55 23.58 0 -11 0 56.82 23.90 0 -11 0 44.11 20.40 0 11 -1 381.54 23.74 0 -11 -1 322.12 24.72 0 11 1 370.58 23.29 0 -11 -1 352.00 30.78 0 -11 1 338.51 26.23 0 -11 1 357.72 28.39 0 11 -2 2502.92 37.42 0 11 2 2710.65 42.75 0 -11 2 2356.01 38.29 0 -11 -2 2148.47 33.23 0 -11 2 1945.28 37.99 0 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960.84 39.55 0 11 -10 385.97 23.23 0 11 10 422.53 21.14 0 -11 10 331.56 28.90 0 -11 -10 301.13 24.17 0 -11 -10 400.43 35.41 0 -11 10 246.94 28.41 0 11 10 487.25 34.88 0 11 -11 1095.81 27.55 0 11 11 1307.72 46.15 0 -11 -11 1086.90 41.28 0 11 11 1129.74 25.40 0 -11 11 724.46 31.61 0 -11 -11 707.65 23.04 0 -11 11 903.15 29.35 0 -11 -12 517.58 28.00 0 -11 -12 753.73 44.09 0 11 12 963.27 47.83 0 11 12 840.78 30.19 0 11 -12 792.27 32.29 0 -11 12 574.61 34.51 0 -11 12 439.57 33.50 0 -11 -13 4959.24 45.02 0 11 13 8088.28 143.91 0 11 -13 7368.82 55.24 0 11 13 7414.73 55.09 0 -11 13 5906.74 58.86 0 -11 13 4699.04 47.25 0 -11 -14 1290.68 32.69 0 11 -14 2040.52 36.42 0 11 14 1964.60 31.65 0 -11 14 1696.22 40.53 0 -11 14 1327.41 31.61 0 11 -15 24.49 21.87 0 11 15 33.98 19.49 0 -11 15 -4.82 22.12 0 -11 15 25.13 22.12 0 -11 -15 2.69 18.74 0 11 -16 437.18 23.82 0 -11 16 340.66 29.38 0 11 16 450.10 21.97 0 -11 16 299.06 23.81 0 -11 -16 348.69 20.43 0 11 -17 3881.73 39.54 0 -11 17 2998.93 46.70 0 11 17 3668.95 39.39 0 -11 17 2544.73 35.18 0 -11 -17 2592.43 33.78 0 -11 17 3574.24 54.43 0 11 -18 2452.31 33.34 0 -11 -18 1704.31 29.06 0 -11 18 2214.90 44.60 0 11 18 2463.08 35.84 0 -11 18 1982.12 39.16 0 -11 18 1733.11 31.83 0 11 -19 384.34 26.24 0 -11 19 279.44 28.34 0 11 19 327.27 24.82 0 -11 19 289.59 26.93 0 -11 19 270.52 25.53 0 -11 -19 229.87 23.85 0 11 -20 148.86 19.78 0 -11 20 106.69 26.81 0 -11 20 99.62 23.42 0 11 20 137.68 24.20 0 -11 20 138.62 20.95 0 -11 -20 107.12 19.42 0 -11 21 42.58 30.43 0 11 21 58.99 23.18 0 -11 21 29.10 22.68 0 -11 21 3.04 25.39 0 -11 -21 29.63 17.61 0 11 -21 39.50 18.98 0 -11 22 711.38 33.63 0 11 22 822.51 28.37 0 -11 22 596.08 28.12 0 -11 22 598.49 24.41 0 -11 -22 590.59 26.66 0 11 -22 743.29 23.60 0 -11 23 71.80 32.74 0 11 23 68.87 19.98 0 -11 23 49.39 26.59 0 -11 -23 34.54 18.69 0 11 -23 73.40 23.04 0 -11 23 63.96 26.05 0 -11 24 257.65 31.50 0 11 24 253.69 21.49 0 -11 24 172.84 23.75 0 11 -24 308.50 23.99 0 -11 24 193.06 22.79 0 -11 -24 194.96 19.39 0 -11 25 147.44 39.39 0 11 25 105.71 20.97 0 -11 25 95.49 26.39 0 -11 -25 121.57 23.00 0 -11 25 90.65 22.53 0 11 -25 121.51 18.82 0 -11 26 214.84 28.47 0 -11 -26 199.07 19.15 0 11 26 337.25 26.67 0 -11 26 315.70 42.65 0 11 -26 304.75 20.31 0 -11 26 211.91 23.07 0 -11 27 121.38 44.04 0 11 27 150.86 21.65 0 -11 27 106.05 27.27 0 -11 27 163.23 23.25 0 -11 -27 91.63 19.32 0 11 -27 148.69 18.78 0 -11 28 720.32 51.66 0 11 28 675.73 25.77 0 -11 28 453.25 33.82 0 -11 -28 457.02 26.32 0 -11 28 492.67 24.73 0 11 -28 566.13 21.80 0 11 29 385.41 29.63 0 -11 -29 287.72 20.65 0 -11 29 263.95 30.62 0 -11 29 308.71 28.94 0 11 -29 326.83 19.64 0 -11 29 375.02 50.97 0 11 30 333.41 25.21 0 -11 -30 188.76 20.85 0 -11 30 245.65 34.72 0 -11 30 350.13 55.88 0 11 -30 283.66 19.99 0 -11 30 237.65 24.68 0 -11 -31 350.58 21.99 0 11 31 520.50 27.19 0 -11 31 406.37 39.48 0 11 -31 433.78 25.71 0 -11 31 400.61 26.98 0 -11 31 504.01 59.86 0 -11 32 171.64 42.48 0 11 -32 193.76 23.70 0 -11 -32 182.72 24.94 0 -11 32 187.52 25.78 0 -11 32 232.70 60.78 0 11 32 194.20 31.47 0 11 33 939.67 33.20 0 -11 33 651.56 55.35 0 11 -33 737.24 27.32 0 -11 33 733.46 34.17 0 -11 33 756.87 65.92 0 -11 -33 566.48 28.73 0 11 -34 166.99 23.81 0 11 34 307.48 34.55 0 -11 34 182.73 54.36 0 -11 34 205.19 61.46 0 -11 34 235.15 30.67 0 -11 -34 138.47 25.66 0 11 35 85.49 34.01 0 11 -35 29.77 18.46 0 -11 35 83.78 30.00 0 -11 -35 37.52 24.78 0 11 36 88.62 35.21 0 11 -36 55.63 18.86 0 -11 36 101.56 24.54 0 -11 -36 50.16 19.53 0 12 0 1900.99 36.55 0 -12 0 1492.91 31.66 0 -12 0 1422.55 35.40 0 12 1 713.55 26.66 0 12 -1 721.42 26.63 0 -12 -1 674.76 31.94 0 -12 1 593.50 25.78 0 -12 1 567.56 31.09 0 -12 -1 651.77 34.12 0 12 2 194.38 27.17 0 12 -2 226.56 30.83 0 -12 -2 285.72 31.52 0 -12 2 154.83 26.27 0 -12 -2 269.77 30.56 0 -12 2 337.74 32.37 0 12 3 7129.85 67.77 0 12 -3 6451.21 58.69 0 -12 3 5449.09 51.64 0 -12 3 4798.48 53.95 0 -12 -3 5159.01 47.96 0 -12 -3 5286.12 58.75 0 12 4 1317.57 35.81 0 12 -4 1123.50 32.71 0 -12 -4 988.51 28.48 0 -12 4 1099.25 31.77 0 -12 -4 1048.77 33.97 0 -12 4 1015.79 38.01 0 12 -5 203.62 25.88 0 -12 5 210.69 28.64 0 -12 5 174.20 24.98 0 -12 -5 169.52 26.47 0 -12 -5 158.34 22.96 0 12 5 217.41 31.26 0 12 -6 115.16 24.82 0 -12 -6 49.87 26.69 0 12 6 75.14 26.19 0 -12 6 10.77 30.85 0 -12 6 75.88 30.14 0 -12 -6 80.85 26.57 0 12 6 88.11 27.73 0 -12 7 3110.13 43.66 0 12 -7 3621.41 42.44 0 12 7 4342.52 43.52 0 -12 -7 2688.31 34.99 0 -12 7 2533.72 39.11 0 -12 -7 2851.97 46.54 0 12 7 4145.42 57.17 0 12 -8 1421.18 29.15 0 -12 -8 1311.73 40.60 0 -12 8 1347.84 33.68 0 12 8 1768.59 32.43 0 -12 -8 1100.10 26.71 0 -12 8 1011.60 30.61 0 12 8 1832.13 43.35 0 -12 -9 37.74 28.76 0 12 -9 46.40 20.43 0 -12 9 50.54 22.22 0 12 9 40.25 19.31 0 12 9 42.56 29.95 0 -12 -9 23.89 23.94 0 -12 9 29.83 27.19 0 12 -10 111.42 20.08 0 -12 -10 101.88 31.53 0 12 10 91.19 18.96 0 12 10 122.99 33.15 0 -12 10 63.36 27.54 0 -12 -10 54.17 18.61 0 -12 10 41.46 26.46 0 12 -11 103.92 25.91 0 -12 11 30.85 21.71 0 12 11 70.02 23.75 0 12 11 90.12 34.50 0 -12 -11 70.11 19.02 0 -12 11 19.56 28.37 0 -12 -11 74.99 31.83 0 12 -12 2259.60 32.76 0 -12 -12 2111.68 56.70 0 12 12 2613.63 65.05 0 12 12 2373.04 31.06 0 -12 12 1864.67 37.61 0 -12 -12 1526.12 26.37 0 -12 12 1514.45 34.51 0 12 13 772.41 52.60 0 12 -13 684.21 24.06 0 -12 -13 631.68 46.53 0 -12 13 530.97 26.19 0 12 13 701.81 26.63 0 -12 13 483.33 29.63 0 -12 -13 393.44 20.73 0 12 -14 617.75 24.11 0 12 14 576.83 22.16 0 -12 14 446.51 28.14 0 -12 14 349.89 28.55 0 -12 -14 421.12 23.91 0 12 -15 363.82 23.10 0 -12 -15 229.35 19.45 0 12 15 378.00 21.30 0 -12 15 249.52 28.37 0 -12 15 211.70 23.22 0 12 -16 1206.60 27.56 0 12 16 1202.26 29.26 0 -12 16 931.89 32.55 0 -12 16 767.90 26.07 0 -12 -16 867.68 26.92 0 12 -17 907.26 29.17 0 -12 17 754.65 32.36 0 12 17 873.81 24.63 0 -12 17 596.55 29.18 0 -12 17 515.05 24.40 0 -12 -17 570.44 21.66 0 -12 -18 576.16 25.50 0 -12 18 712.93 30.85 0 12 -18 812.09 24.46 0 12 18 821.14 24.27 0 -12 18 582.20 29.14 0 -12 18 576.71 28.28 0 -12 19 561.23 29.85 0 12 19 624.74 22.89 0 -12 19 463.72 26.89 0 -12 19 425.12 22.93 0 -12 -19 411.15 20.69 0 12 -19 681.77 26.87 0 -12 20 423.77 28.83 0 -12 -20 333.64 25.21 0 -12 20 330.77 25.75 0 12 20 474.83 21.97 0 -12 20 355.83 22.77 0 12 -20 490.00 22.85 0 -12 21 558.84 31.27 0 12 21 634.77 22.86 0 -12 -21 461.16 20.61 0 -12 21 435.59 27.02 0 -12 21 468.97 23.79 0 12 -21 724.08 23.65 0 -12 22 38.31 31.09 0 12 22 27.66 20.84 0 -12 22 26.77 27.35 0 -12 22 42.52 20.48 0 -12 -22 29.26 18.92 0 12 -22 39.07 19.71 0 -12 -23 1979.67 33.87 0 -12 23 2460.87 50.67 0 12 -23 2786.56 35.50 0 12 23 2682.41 35.84 0 -12 23 1998.23 38.90 0 -12 23 1985.36 32.23 0 -12 24 75.89 35.37 0 12 24 62.47 20.70 0 -12 24 71.17 27.96 0 -12 24 69.94 22.10 0 -12 -24 55.05 19.76 0 12 -24 102.98 20.27 0 -12 25 46.45 31.12 0 12 25 40.94 25.80 0 -12 25 32.81 22.41 0 12 -25 76.66 19.66 0 -12 25 41.34 22.54 0 -12 -25 46.08 22.28 0 -12 26 89.42 39.13 0 12 -26 69.27 18.62 0 12 26 53.92 25.08 0 -12 26 17.54 24.38 0 -12 26 44.13 26.17 0 -12 -26 69.32 19.56 0 12 27 1293.52 29.81 0 -12 27 975.86 36.81 0 -12 27 1259.79 55.60 0 -12 27 969.15 27.88 0 12 -27 1276.97 28.50 0 -12 -27 837.31 25.04 0 -12 28 268.81 47.31 0 -12 28 188.70 31.05 0 12 28 278.06 28.71 0 -12 28 190.45 23.94 0 12 -28 267.10 23.07 0 -12 -28 183.16 23.94 0 -12 29 184.93 47.90 0 12 29 244.99 23.71 0 -12 29 148.01 34.61 0 -12 29 133.29 27.90 0 12 -29 146.40 19.29 0 -12 -29 107.51 19.33 0 -12 30 204.63 23.89 0 12 -30 202.73 20.07 0 -12 30 153.20 32.15 0 12 30 287.11 30.12 0 -12 -30 140.67 20.62 0 -12 30 260.95 50.84 0 -12 31 68.63 25.32 0 12 31 52.65 29.90 0 -12 31 34.59 36.27 0 -12 -31 44.65 23.93 0 -12 31 64.09 53.71 0 12 -31 23.47 19.20 0 -12 -32 358.13 27.74 0 -12 32 384.43 31.58 0 12 32 646.06 34.16 0 -12 32 425.43 46.82 0 -12 32 458.82 60.49 0 12 -32 502.36 21.74 0 12 33 314.07 28.33 0 -12 33 199.99 49.34 0 12 -33 274.77 19.73 0 -12 33 187.01 30.78 0 -12 33 174.93 62.46 0 -12 -33 107.48 21.44 0 12 34 123.28 34.05 0 -12 34 114.67 56.80 0 12 -34 101.62 19.44 0 -12 34 117.88 62.24 0 -12 34 107.70 24.60 0 -12 -34 38.63 21.03 0 12 35 52.58 33.79 0 -12 35 -15.44 24.46 0 -12 -35 31.11 24.54 0 13 0 50.27 24.16 0 -13 0 37.65 23.32 0 -13 0 28.90 22.33 0 13 1 179.91 26.64 0 13 -1 127.79 20.81 0 -13 1 127.51 23.92 0 -13 -1 138.43 23.00 0 -13 1 149.31 25.35 0 -13 -1 173.38 28.98 0 13 2 2364.58 40.40 0 13 -2 2249.79 37.21 0 -13 -2 1760.08 39.38 0 -13 2 1754.88 33.42 0 -13 -2 1748.05 32.00 0 -13 2 1654.06 35.26 0 13 -3 1081.42 31.00 0 -13 3 879.59 29.53 0 -13 3 851.86 30.28 0 -13 -3 895.84 33.58 0 -13 -3 927.21 27.07 0 13 3 1254.59 34.98 0 13 -4 857.06 30.09 0 -13 4 653.78 34.08 0 -13 4 722.40 28.06 0 -13 -4 655.11 25.27 0 -13 -4 694.79 33.99 0 13 4 949.70 32.33 0 13 -5 4.74 21.00 0 -13 -5 51.19 28.24 0 -13 5 70.82 25.89 0 -13 5 30.74 29.69 0 13 5 91.16 30.89 0 -13 -5 -3.24 26.49 0 13 -6 1800.81 31.97 0 -13 -6 1409.84 37.49 0 -13 6 1575.63 38.78 0 -13 -6 1427.10 34.67 0 -13 6 1337.64 39.49 0 13 6 2184.24 44.55 0 13 -7 3614.41 40.68 0 -13 -7 2957.23 46.76 0 -13 7 3105.70 41.37 0 -13 -7 2793.75 35.59 0 -13 7 2518.36 40.52 0 13 7 4373.94 58.52 0 13 -8 273.20 27.06 0 -13 -8 259.68 31.90 0 13 8 305.08 22.37 0 13 8 368.73 31.52 0 -13 8 210.55 25.89 0 -13 8 232.42 25.56 0 -13 -8 199.31 22.25 0 13 -9 755.26 28.09 0 -13 -9 662.24 35.70 0 13 9 831.50 23.92 0 -13 9 572.59 30.96 0 -13 -9 493.10 22.77 0 13 9 953.70 39.80 0 -13 9 440.17 30.58 0 13 -10 590.67 22.90 0 -13 -10 540.57 35.51 0 -13 -10 408.62 26.31 0 13 10 616.50 27.17 0 -13 10 439.34 26.72 0 13 10 660.57 38.70 0 -13 10 350.65 25.39 0 13 -11 1575.07 29.21 0 -13 -11 1085.35 25.88 0 13 11 1698.70 28.67 0 -13 -11 1522.11 48.57 0 13 11 1971.66 51.16 0 -13 11 1375.03 35.32 0 -13 11 1046.09 29.13 0 13 -12 159.89 22.68 0 13 12 187.20 39.13 0 -13 -12 52.96 21.04 0 -13 -12 124.10 36.84 0 -13 12 15.65 23.63 0 -13 12 26.05 24.77 0 13 12 132.32 21.82 0 13 -13 3893.81 40.20 0 13 13 4659.72 96.77 0 -13 -13 2806.32 37.23 0 -13 -13 3714.26 79.98 0 -13 13 3300.14 45.76 0 13 13 4297.22 40.90 0 -13 13 2589.86 36.58 0 13 -14 303.24 22.76 0 13 14 304.64 26.00 0 -13 14 188.63 29.61 0 -13 14 168.07 23.15 0 -13 -14 143.95 20.41 0 13 -15 96.60 25.23 0 -13 15 30.09 21.01 0 -13 15 76.59 25.53 0 13 15 57.54 19.08 0 -13 -15 32.22 17.61 0 13 -16 72.43 20.19 0 13 16 98.53 24.10 0 -13 16 11.49 25.16 0 -13 16 13.77 25.21 0 -13 -16 41.97 22.06 0 -13 -17 1445.53 27.46 0 -13 17 1626.65 35.59 0 13 17 2297.74 35.10 0 -13 17 1443.36 28.76 0 -13 17 1940.31 36.41 0 13 -17 2365.00 34.82 0 -13 18 228.00 22.05 0 -13 18 278.11 28.99 0 13 18 367.62 22.01 0 -13 18 225.89 26.12 0 -13 -18 169.29 23.79 0 13 -18 370.53 22.50 0 -13 19 132.68 22.23 0 -13 19 218.73 27.04 0 13 19 215.00 20.84 0 -13 19 161.88 25.96 0 -13 -19 124.07 18.76 0 13 -19 271.18 21.47 0 -13 20 312.53 28.01 0 13 20 379.93 22.96 0 -13 20 267.62 25.82 0 -13 20 206.51 22.40 0 -13 -20 294.17 24.52 0 13 -20 349.25 22.01 0 13 -21 93.22 20.33 0 -13 21 103.09 26.85 0 13 21 68.64 19.77 0 -13 21 60.24 28.26 0 -13 21 51.23 21.08 0 -13 -21 30.82 19.14 0 -13 22 720.85 36.90 0 13 22 820.48 24.97 0 -13 22 645.48 29.09 0 -13 22 596.67 29.38 0 -13 -22 594.33 26.41 0 13 -22 966.21 28.62 0 -13 23 75.10 28.43 0 13 23 112.75 19.88 0 -13 23 84.80 24.37 0 -13 23 148.13 20.99 0 -13 -23 70.61 18.66 0 13 -23 128.26 20.10 0 -13 24 389.52 33.41 0 13 24 502.84 27.78 0 -13 24 371.58 27.38 0 -13 24 369.03 27.65 0 -13 -24 343.49 25.64 0 13 -24 473.01 20.82 0 -13 -25 4.85 18.73 0 13 25 -27.54 26.45 0 -13 25 62.37 34.50 0 -13 25 49.33 20.91 0 13 -25 25.07 19.29 0 -13 25 24.42 27.36 0 -13 26 529.90 39.27 0 13 26 627.44 25.28 0 -13 26 405.32 32.69 0 -13 26 453.70 29.00 0 13 -26 653.78 26.61 0 -13 -26 406.33 26.02 0 -13 -27 58.14 20.37 0 13 27 98.85 23.10 0 -13 27 115.53 40.99 0 -13 27 75.43 29.49 0 -13 27 80.62 21.89 0 13 -27 125.36 19.37 0 -13 28 220.39 47.38 0 -13 -28 151.65 20.77 0 13 28 226.30 28.91 0 -13 28 163.05 32.44 0 13 -28 229.18 19.81 0 -13 28 137.08 22.93 0 13 29 134.62 25.40 0 -13 29 98.70 31.36 0 -13 29 158.48 47.27 0 -13 29 124.52 27.40 0 -13 -29 114.79 24.97 0 13 -29 181.55 19.59 0 13 30 47.51 30.53 0 -13 30 12.41 35.53 0 13 -30 20.48 19.60 0 -13 30 -14.98 23.89 0 -13 -30 15.49 19.57 0 -13 30 17.64 46.79 0 13 31 258.42 27.58 0 -13 31 181.48 40.68 0 13 -31 205.55 20.73 0 -13 31 183.65 25.72 0 -13 -31 87.45 25.88 0 -13 31 192.24 56.37 0 -13 32 116.48 29.51 0 13 32 178.19 33.50 0 -13 32 117.28 46.39 0 13 -32 200.46 24.23 0 -13 -32 87.60 25.93 0 13 33 560.03 33.80 0 -13 33 389.79 53.06 0 13 -33 452.35 27.38 0 -13 33 513.86 27.88 0 -13 -33 309.88 24.54 0 -14 0 860.33 34.62 0 -14 0 670.75 30.73 0 14 0 873.30 32.63 0 -14 1 2034.30 40.48 0 -14 -1 2025.72 38.77 0 -14 1 1843.79 38.02 0 -14 -1 1990.73 42.55 0 14 1 2549.71 41.73 0 14 -1 2461.04 41.06 0 14 -2 526.33 28.87 0 -14 2 437.14 29.56 0 -14 2 424.43 27.29 0 -14 -2 469.84 31.89 0 -14 -2 453.44 33.49 0 14 2 552.94 30.77 0 14 -3 3035.35 42.47 0 -14 3 2470.70 37.88 0 -14 -3 2594.78 39.73 0 -14 3 2432.78 44.19 0 -14 -3 2381.89 43.78 0 14 3 3600.23 49.24 0 14 -4 626.36 28.40 0 -14 4 550.26 28.27 0 -14 -4 583.80 32.15 0 -14 -4 580.65 31.29 0 -14 4 536.02 33.05 0 14 4 717.40 32.65 0 14 5 14.73 26.55 0 14 -5 10.25 20.67 0 -14 -5 11.62 27.47 0 -14 -5 49.07 26.25 0 -14 5 4.51 25.99 0 -14 5 21.51 29.34 0 -14 -6 523.15 24.96 0 -14 6 588.65 27.91 0 14 -6 747.19 25.27 0 -14 6 540.60 33.04 0 14 6 958.93 34.58 0 -14 -6 606.80 30.58 0 14 -7 1215.43 27.48 0 14 7 1474.86 40.33 0 -14 7 913.28 29.68 0 -14 -7 869.14 25.99 0 -14 7 863.68 29.65 0 -14 -7 906.51 33.63 0 14 -8 1150.85 26.73 0 -14 8 792.06 33.56 0 -14 8 966.07 33.25 0 -14 -8 746.82 24.99 0 14 8 1413.73 41.28 0 -14 -8 937.41 35.32 0 14 -9 262.60 21.57 0 -14 -9 276.45 31.48 0 -14 9 231.08 28.82 0 -14 -9 232.97 20.95 0 -14 9 208.67 25.04 0 14 9 353.87 35.46 0 14 -10 63.75 24.29 0 -14 -10 51.65 28.63 0 -14 10 32.17 26.38 0 -14 -10 46.08 19.79 0 14 10 73.30 31.12 0 -14 10 19.62 23.36 0 -14 -11 55.08 29.64 0 -14 -11 35.05 24.23 0 14 -11 81.65 27.35 0 14 11 98.14 34.71 0 -14 11 40.23 24.23 0 14 11 77.30 21.45 0 -14 11 50.66 22.78 0 14 -12 1754.88 30.38 0 14 12 2106.02 59.52 0 -14 12 1385.66 34.76 0 14 12 2002.91 33.31 0 -14 -12 1102.01 25.65 0 -14 12 1114.50 29.33 0 -14 -12 1650.47 53.26 0 14 -13 9.92 19.79 0 14 13 10.16 40.70 0 -14 -13 2.60 36.03 0 14 13 0.05 19.67 0 -14 13 -3.31 27.81 0 -14 -13 -0.10 19.23 0 -14 13 -3.27 21.25 0 14 14 958.96 72.74 0 14 14 972.89 27.89 0 -14 14 654.61 25.54 0 -14 -14 536.55 21.87 0 -14 14 504.78 25.28 0 14 -14 903.47 29.26 0 14 15 139.25 21.10 0 -14 15 104.99 27.12 0 -14 -15 100.97 23.46 0 -14 15 84.29 22.17 0 14 -15 132.12 21.09 0 14 16 1529.82 28.50 0 -14 16 1035.23 32.09 0 -14 -16 886.55 25.03 0 -14 16 916.58 26.33 0 14 -16 1523.24 31.56 0 -14 17 595.94 30.39 0 14 17 799.29 24.71 0 -14 -17 490.97 21.82 0 -14 17 546.35 28.18 0 14 -17 850.73 24.00 0 -14 18 214.93 27.08 0 -14 18 191.52 26.76 0 14 18 297.61 27.34 0 -14 -18 184.60 24.00 0 -14 18 187.81 20.75 0 14 -18 326.06 24.89 0 14 19 568.81 27.60 0 -14 19 393.34 27.24 0 -14 -19 370.32 21.23 0 -14 19 384.16 22.25 0 14 -19 565.03 23.10 0 -14 19 429.16 24.64 0 -14 20 140.43 26.93 0 14 20 160.34 20.95 0 -14 20 118.58 25.52 0 -14 20 125.52 21.97 0 -14 -20 121.30 23.75 0 14 -20 210.86 24.81 0 14 21 1000.06 26.34 0 -14 21 762.05 32.63 0 -14 21 707.66 29.71 0 -14 21 668.54 29.07 0 -14 -21 657.55 23.51 0 14 -21 994.84 25.88 0 -14 22 25.59 26.57 0 -14 -22 51.78 19.63 0 14 22 19.70 25.58 0 -14 22 15.49 24.48 0 -14 22 64.07 20.50 0 14 -22 53.98 20.10 0 14 23 1143.63 30.92 0 -14 23 850.43 34.05 0 -14 23 694.59 24.82 0 -14 -23 750.74 24.42 0 14 -23 1182.99 26.94 0 -14 23 942.55 36.19 0 -14 -24 19.46 18.85 0 -14 24 40.00 33.71 0 14 24 65.67 26.28 0 -14 24 17.52 23.83 0 -14 24 5.02 21.80 0 14 -24 24.74 19.78 0 -14 25 -10.67 29.89 0 14 25 35.63 26.40 0 -14 25 -22.34 28.76 0 -14 25 -6.67 20.42 0 -14 -25 18.59 24.09 0 14 -25 -24.29 19.84 0 -14 26 41.83 32.99 0 -14 -26 16.39 20.28 0 -14 26 32.25 21.53 0 14 26 45.57 22.54 0 -14 26 10.83 29.53 0 14 -26 44.51 23.99 0 -14 27 1049.92 52.45 0 14 27 1232.13 30.89 0 -14 27 857.87 39.20 0 14 -27 1225.32 26.96 0 -14 27 993.02 31.25 0 -14 -27 733.32 25.48 0 -14 -28 110.82 21.67 0 -14 28 146.45 44.92 0 -14 28 150.06 23.45 0 14 28 203.92 30.26 0 -14 28 113.14 32.82 0 14 -28 205.21 21.49 0 -14 29 106.60 46.30 0 14 29 138.35 24.97 0 -14 -29 97.01 21.21 0 -14 29 75.13 32.98 0 14 -29 148.63 20.44 0 -14 29 42.20 28.62 0 -14 30 75.69 48.81 0 14 30 41.68 30.94 0 -14 30 50.75 34.55 0 14 -30 35.42 24.86 0 -14 -30 27.87 25.72 0 -14 30 73.54 22.69 0 14 31 366.27 28.96 0 -14 31 217.89 42.31 0 14 -31 253.25 26.25 0 -14 -31 142.47 22.69 0 -14 31 97.52 26.59 0 -14 31 266.32 52.84 0 -14 32 218.28 31.50 0 -14 -32 140.78 27.99 0 -14 32 366.49 49.18 0 -15 0 74.14 23.83 0 -15 0 64.41 29.59 0 15 0 29.80 26.61 0 -15 -1 38.69 22.95 0 -15 1 92.80 30.67 0 -15 1 66.07 24.75 0 -15 -1 50.64 29.42 0 15 1 29.70 25.87 0 15 -1 32.43 27.06 0 -15 2 2037.50 40.32 0 -15 -2 1969.06 33.57 0 -15 2 1892.11 36.32 0 15 2 2745.36 43.24 0 -15 -2 2009.55 40.10 0 15 -2 2586.29 37.15 0 -15 3 211.78 31.87 0 -15 3 195.72 25.50 0 -15 -3 233.59 23.29 0 15 3 262.80 27.85 0 -15 -3 206.72 28.54 0 15 -3 256.55 27.10 0 -15 4 477.70 32.32 0 -15 -4 519.99 29.65 0 -15 -4 449.42 24.49 0 -15 4 487.65 26.26 0 15 4 703.45 32.40 0 15 -4 655.20 28.53 0 -15 -5 274.93 27.96 0 -15 5 279.53 26.02 0 -15 -5 255.81 23.54 0 -15 5 294.26 30.17 0 15 5 428.71 30.10 0 15 -5 353.00 21.78 0 -15 -6 244.06 23.48 0 15 -6 367.48 24.22 0 -15 6 272.60 27.87 0 15 6 511.28 36.88 0 -15 6 254.11 33.75 0 -15 -6 288.54 28.89 0 -15 7 1822.10 35.73 0 -15 -7 1605.52 30.89 0 15 7 2845.84 50.79 0 -15 7 1594.80 33.67 0 -15 -7 1883.05 44.70 0 15 -7 2212.24 32.86 0 -15 -8 386.30 35.05 0 15 -8 423.39 24.53 0 15 8 613.59 38.88 0 -15 -8 327.75 23.58 0 -15 8 382.01 30.91 0 -15 8 373.69 32.44 0 -15 -9 848.63 38.53 0 -15 9 624.34 28.13 0 15 9 1377.93 44.88 0 -15 9 726.58 28.14 0 -15 -9 677.53 24.63 0 15 -9 956.29 25.79 0 -15 -10 35.73 22.28 0 -15 -10 35.82 35.87 0 15 10 38.92 34.10 0 -15 10 0.41 24.72 0 -15 10 20.56 25.14 0 15 -10 75.72 21.61 0 -15 -11 1781.87 52.99 0 15 11 2542.16 62.95 0 -15 11 1535.38 36.27 0 -15 -11 1241.14 27.78 0 -15 11 1241.71 31.62 0 15 -11 1915.91 31.44 0 -15 -12 21.87 33.46 0 15 12 48.46 34.76 0 -15 12 -29.09 24.38 0 -15 12 -18.15 22.58 0 -15 -12 26.13 25.35 0 15 -12 39.84 24.36 0 -15 13 948.70 28.68 0 -15 -13 1299.10 53.30 0 -15 13 1095.89 29.03 0 -15 -13 1000.15 28.55 0 15 -13 1431.38 28.42 0 15 13 1813.46 65.50 0 15 14 96.87 54.67 0 -15 14 48.45 27.08 0 -15 -14 50.94 19.23 0 -15 14 101.50 22.80 0 15 -14 117.40 21.24 0 -15 15 18.78 25.63 0 -15 -15 -2.15 19.06 0 -15 15 4.68 21.27 0 15 -15 9.56 25.47 0 15 16 68.36 19.91 0 -15 16 60.24 25.29 0 -15 -16 47.98 18.62 0 -15 16 34.84 20.68 0 15 -16 47.22 21.05 0 -15 17 558.14 30.05 0 15 17 823.79 24.66 0 -15 -17 451.11 21.95 0 -15 17 489.31 23.57 0 15 -17 852.14 24.97 0 -15 18 505.91 28.51 0 -15 -18 431.74 21.98 0 15 18 821.79 25.36 0 -15 18 471.16 24.44 0 15 -18 714.77 24.65 0 -15 -19 229.56 21.27 0 15 19 505.79 27.26 0 -15 19 318.76 26.69 0 -15 19 329.58 27.02 0 -15 19 307.95 27.46 0 15 -19 472.39 23.08 0 15 20 55.72 25.25 0 -15 20 24.84 25.39 0 -15 -20 50.02 23.37 0 -15 20 -8.55 20.03 0 15 -20 0.41 19.59 0 15 21 609.85 28.12 0 -15 21 338.36 28.67 0 -15 -21 322.00 21.51 0 -15 21 309.86 22.34 0 15 -21 578.54 23.04 0 -15 22 796.47 34.31 0 15 22 1078.31 31.59 0 -15 22 745.76 31.72 0 -15 -22 594.56 23.75 0 -15 22 662.72 29.03 0 15 -22 1021.90 25.07 0 -15 23 9.79 26.93 0 15 23 46.26 26.05 0 -15 23 31.33 25.65 0 -15 -23 32.44 18.67 0 -15 23 22.34 19.75 0 15 -23 60.17 24.57 0 15 24 249.67 27.46 0 -15 24 119.64 30.17 0 -15 24 143.37 26.47 0 -15 24 123.23 21.36 0 -15 -24 137.88 20.69 0 15 -24 218.92 20.93 0 15 25 95.72 23.20 0 -15 25 100.03 30.72 0 15 -25 97.44 20.16 0 -15 -25 48.77 25.31 0 -15 25 67.84 20.58 0 -15 26 165.93 22.60 0 15 26 271.41 24.53 0 -15 26 167.31 32.48 0 15 -26 248.03 26.44 0 -15 -26 139.43 21.51 0 -15 27 126.11 36.79 0 -15 27 77.36 33.83 0 15 -27 180.01 20.57 0 -15 -27 106.17 26.05 0 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60.57 20.55 0 -16 -5 52.81 25.82 0 -16 -6 186.05 27.89 0 -16 6 163.13 24.62 0 16 6 325.49 32.39 0 -16 6 214.36 31.05 0 -16 -6 145.56 22.29 0 16 -6 248.45 21.48 0 -16 -7 693.30 36.37 0 -16 -7 610.45 24.70 0 -16 7 739.27 33.80 0 16 7 1142.63 43.02 0 -16 7 594.85 28.56 0 16 -7 814.41 26.08 0 -16 -8 1353.86 44.11 0 -16 8 1220.00 31.83 0 -16 -8 1115.52 28.69 0 16 8 2270.63 52.92 0 -16 8 1099.36 36.95 0 16 -8 1541.19 29.20 0 -16 -9 54.00 31.12 0 -16 -9 39.35 21.57 0 16 9 98.28 34.74 0 -16 9 51.26 28.41 0 -16 9 46.72 29.98 0 16 -9 79.08 21.69 0 16 10 82.87 39.46 0 -16 10 35.22 22.20 0 -16 -10 16.38 21.30 0 -16 10 16.20 23.97 0 -16 -10 31.61 32.14 0 16 -10 69.28 21.10 0 -16 -11 445.68 40.64 0 16 11 661.79 42.63 0 -16 11 342.16 30.78 0 -16 -11 343.90 23.32 0 -16 11 300.27 26.06 0 16 -11 518.41 23.64 0 -16 12 1304.65 34.79 0 -16 -12 1101.78 26.65 0 16 12 2226.39 67.05 0 -16 12 1099.16 29.91 0 -16 -12 1501.42 54.33 0 16 -12 1798.66 30.41 0 -16 -13 15.75 37.62 0 -16 13 -34.98 27.89 0 -16 -13 11.15 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7 7 2 776.88 23.90 -7 -7 -3 488.10 27.43 7 7 3 646.13 26.16 7 -7 3 619.52 30.67 7 7 3 580.24 19.72 -7 7 -3 636.90 23.27 7 -7 3 530.54 22.95 7 7 3 573.00 22.47 -7 -7 -4 761.36 28.99 7 7 4 1022.04 28.71 7 7 4 874.98 21.77 7 -7 4 1008.45 32.76 7 -7 4 843.26 24.35 -7 7 -4 1001.89 25.32 7 7 4 953.03 27.87 -7 -7 -5 819.06 28.87 7 7 5 1111.19 30.02 7 -7 5 1035.33 28.50 7 7 5 989.18 22.78 7 -7 5 863.21 25.39 7 7 5 1002.35 25.29 -7 7 -5 1063.25 24.75 7 7 6 1742.90 27.40 -7 -7 -6 1608.39 32.59 7 7 6 2085.37 35.70 7 -7 6 2018.26 33.26 7 -7 6 1761.64 30.05 7 7 6 1913.42 29.56 -7 7 -6 2002.42 29.32 -7 -7 -7 175.11 24.61 7 7 7 268.33 25.85 7 -7 7 278.79 23.10 7 7 7 259.68 20.87 7 -7 7 221.13 19.78 -7 7 -7 255.21 19.99 -7 -7 -8 640.23 23.57 -7 7 -8 760.08 22.88 7 7 8 906.33 30.13 7 -7 8 821.65 32.43 7 7 8 847.71 24.36 7 -7 8 688.92 22.77 -7 -7 -9 1915.36 31.04 -7 7 -9 2319.06 32.88 7 -7 9 2429.21 36.01 7 7 9 2598.19 34.61 7 7 9 2477.30 32.51 7 -7 9 2137.60 33.48 7 7 9 2208.56 30.27 -7 -7 -10 25.51 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32 385.84 33.01 7 7 32 670.93 31.85 7 -7 32 396.97 34.56 7 -8 0 294.23 24.37 -7 8 0 201.34 20.88 7 -8 0 196.96 20.86 7 8 0 207.24 25.03 7 8 0 239.23 21.23 -7 -8 0 147.17 22.33 7 -8 1 1056.47 29.12 -7 -8 -1 739.71 25.48 -7 8 -1 1098.12 26.06 7 8 1 1038.54 25.62 7 -8 1 972.12 26.93 7 8 1 1059.30 25.30 7 -8 2 2241.03 33.92 -7 8 -2 2480.66 36.36 7 8 2 2245.97 32.39 7 -8 2 2131.19 31.94 7 8 2 2327.42 31.06 -7 -8 -2 1568.44 30.34 7 8 3 527.49 22.57 7 -8 3 504.94 25.11 7 8 3 480.83 19.64 7 8 3 495.68 26.38 7 -8 3 486.32 21.44 -7 8 -3 552.43 22.47 -7 -8 -3 355.10 26.23 7 8 4 -9.59 19.65 7 -8 4 -15.99 22.04 7 8 4 4.96 16.88 7 8 4 -20.75 18.97 7 -8 4 41.11 20.03 -7 8 -4 20.36 18.99 -7 -8 -4 -18.79 23.94 7 8 5 2768.83 38.17 7 8 5 2543.91 32.82 7 -8 5 2753.34 37.03 7 8 5 2555.40 33.92 7 -8 5 2370.72 33.66 -7 8 -5 2678.96 33.37 -7 -8 -5 1880.14 31.46 7 8 6 1823.53 33.98 -7 8 -6 1695.56 27.99 7 8 6 1655.45 27.24 7 -8 6 1763.22 36.80 7 8 6 1809.09 32.90 7 -8 6 1459.35 28.40 -7 -8 -6 1326.87 28.68 7 8 7 104.85 24.14 -7 8 -7 100.52 18.79 7 8 7 90.96 23.79 7 -8 7 113.48 18.44 7 -8 7 106.21 22.80 -7 -8 -7 91.47 20.07 7 8 8 24.65 22.66 7 -8 8 23.38 22.22 -7 8 -8 -26.54 22.47 7 8 8 -18.68 18.52 7 -8 8 11.73 18.03 -7 -8 -8 20.29 19.05 7 8 9 569.84 22.06 7 -8 9 559.04 25.42 -7 8 -9 448.96 21.03 7 8 9 496.30 18.43 7 8 9 567.68 22.19 7 -8 9 417.72 21.18 -7 -8 -9 431.77 26.84 -7 -8 -10 558.68 22.44 7 8 10 745.81 27.73 7 -8 10 816.46 30.39 -7 8 -10 677.96 21.36 7 8 10 779.51 24.30 7 -8 10 679.72 22.41 -7 -8 -11 36.35 19.75 7 8 11 36.95 22.34 7 -8 11 19.41 22.78 -7 8 -11 38.53 20.85 7 8 11 33.16 19.20 7 -8 11 11.78 18.11 -7 -8 -12 10.77 24.74 7 8 12 25.58 23.49 7 -8 12 57.28 21.47 7 8 12 42.80 19.71 -7 8 -12 -6.68 17.52 7 8 12 47.09 23.65 7 -8 12 15.01 17.57 -7 -8 -13 412.91 22.70 7 -8 13 413.07 20.43 7 8 13 521.43 26.00 7 -8 13 516.91 25.07 -7 8 -13 451.08 19.76 7 8 13 414.45 19.06 7 8 13 571.64 27.40 -7 -8 -14 431.88 22.96 7 -8 14 449.05 24.00 7 8 14 541.60 27.20 7 -8 14 507.32 25.57 -7 8 -14 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-25.23 20.50 -13 -5 -1 32.39 30.85 13 -5 1 18.02 25.94 13 -5 1 -25.96 18.75 13 5 1 15.13 17.54 13 5 1 12.71 26.66 13 -5 1 8.25 29.73 13 5 2 364.01 23.76 -13 -5 -2 23.97 29.90 13 -5 2 348.33 27.85 13 -5 2 375.13 21.49 13 5 2 352.35 21.22 13 5 2 410.53 30.06 13 -5 2 380.13 28.69 13 5 3 79.19 26.96 -13 -5 -3 89.12 26.60 13 -5 3 109.03 21.50 13 -5 3 158.46 19.61 13 5 3 179.29 24.15 13 5 3 176.36 22.64 13 -5 3 178.26 27.00 13 5 4 12.70 20.44 -13 -5 -4 -2.57 29.95 13 -5 4 2.33 19.36 13 -5 4 20.36 17.52 13 5 4 41.67 22.66 13 5 4 -5.11 20.37 13 -5 4 -19.05 24.00 13 5 5 74.75 21.67 -13 -5 -5 49.99 24.75 13 -5 5 56.79 20.21 13 -5 5 46.15 22.96 13 5 5 58.50 20.53 13 5 5 27.06 18.74 13 -5 5 127.84 25.25 13 5 6 268.90 23.46 -13 -5 -6 134.55 31.51 13 -5 6 273.33 26.41 13 -5 6 265.30 24.43 13 5 6 248.50 22.56 13 5 6 232.45 20.93 13 -5 6 368.20 33.70 13 5 7 22.03 23.00 -13 -5 -7 67.73 23.96 13 -5 7 109.44 19.34 13 -5 7 88.91 22.67 13 5 7 66.79 20.48 13 5 7 73.70 18.73 13 -5 7 133.63 25.20 13 5 8 59.90 25.74 -13 -5 -8 35.62 23.59 13 -5 8 53.34 18.85 13 -5 8 57.19 18.60 13 -5 8 154.38 25.23 13 5 8 75.98 18.20 13 6 0 191.96 26.95 -13 -6 0 88.43 28.34 13 -6 0 265.19 23.13 13 6 0 107.85 19.06 13 -6 0 191.36 20.85 13 6 0 204.74 29.04 13 -6 0 207.29 26.65 13 6 1 30.04 25.94 -13 -6 -1 53.09 32.03 13 -6 1 54.49 21.16 13 6 1 9.13 18.98 13 -6 1 2.23 18.41 13 6 1 91.66 27.23 13 -6 1 8.09 25.63 13 6 2 276.79 23.88 -13 -6 -2 169.68 34.14 13 -6 2 203.71 23.90 13 6 2 148.25 21.26 13 -6 2 233.66 21.59 13 6 2 297.39 25.35 13 -6 2 343.63 34.00 13 6 3 8.60 21.16 -13 -6 -3 62.25 24.73 13 -6 3 -8.19 20.77 13 -6 3 38.30 22.93 13 6 3 9.62 18.35 13 6 3 3.21 25.92 13 -6 3 61.73 24.94 13 6 4 134.93 27.33 -13 -6 -4 77.60 30.53 13 -6 4 78.34 25.78 13 -6 4 95.13 19.72 13 6 4 96.88 18.90 13 6 4 110.37 26.69 13 -6 4 82.78 31.54 13 6 5 17.05 24.15 -13 -6 -5 11.76 24.84 13 -6 5 56.87 21.03 13 -6 5 106.04 19.63 13 6 5 113.81 18.90 13 6 5 110.88 26.07 13 -6 5 37.65 26.85 13 6 6 1.13 27.24 -13 -6 -6 -0.49 30.24 13 -6 6 6.41 18.63 13 6 6 54.23 22.67 -13 -7 0 -5.32 26.95 13 -7 0 60.12 26.07 13 7 0 11.59 18.82 13 -7 0 14.69 19.19 13 7 0 6.08 21.88 -13 -7 -1 23.56 26.26 13 7 1 -14.86 22.36 13 -7 1 -11.70 18.91 -13 -7 -2 46.64 32.65 13 7 2 50.16 23.03 13 -7 2 50.11 23.56 13 -7 3 114.19 20.26 ; _shelx_hkl_checksum 88543 data_shelx _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 Lu N10 Ni O10 W' _chemical_formula_weight 1074.15 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' 'Lu' 'Lu' -0.4720 5.8584 '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' 'Ni' 'Ni' 0.3393 1.1124 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.9298(4) _cell_length_b 13.9422(7) _cell_length_c 30.8112(19) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3836.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26423 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 30.80 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_F_000 2068 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_absorpt_coefficient_mu 6.092 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4766 _exptl_absorpt_correction_T_max 0.6352 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19721 _diffrn_reflns_av_unetI/netI 0.0738 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.375 _diffrn_reflns_theta_max 27.995 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.914 _diffrn_measured_fraction_theta_full 0.886 _diffrn_reflns_Laue_measured_fraction_max 0.914 _diffrn_reflns_Laue_measured_fraction_full 0.886 _diffrn_reflns_point_group_measured_fraction_max 0.929 _diffrn_reflns_point_group_measured_fraction_full 0.906 _reflns_number_total 7808 _reflns_number_gt 6462 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.818 _reflns_Friedel_fraction_max 0.949 _reflns_Friedel_fraction_full 0.931 _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 'X-Area' _computing_cell_refinement 'X-Area' _computing_data_reduction 'X-Area' _computing_structure_solution 'SHELXS-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion 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^)+(0.1597P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.0113(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.13(4) _chemical_absolute_configuration ? _refine_ls_number_reflns 7808 _refine_ls_number_parameters 453 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0984 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2316 _refine_ls_wR_factor_gt 0.2182 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 C1 C 0.326(4) 0.049(3) 0.9538(9) 0.079(12) Uani 1 1 d . . . . . H1A H 0.3780 -0.0005 0.9696 0.119 Uiso 1 1 calc R U . . . H1B H 0.3126 0.1037 0.9721 0.119 Uiso 1 1 calc R U . . . H1C H 0.2306 0.0253 0.9445 0.119 Uiso 1 1 calc R U . . . C2 C 0.353(3) 0.1473(19) 0.8900(11) 0.052(7) Uani 1 1 d . . . . . C3 C 0.218(3) 0.194(2) 0.8989(14) 0.063(9) Uani 1 1 d . . . . . H3 H 0.1597 0.1815 0.9233 0.076 Uiso 1 1 calc R U . . . C4 C 0.178(4) 0.266(3) 0.8655(15) 0.081(13) Uani 1 1 d . . . . . H4 H 0.0881 0.2993 0.8690 0.098 Uiso 1 1 calc R U . . . C5 C 0.259(4) 0.286(2) 0.8317(14) 0.068(10) Uani 1 1 d . . . . . H5 H 0.2330 0.3371 0.8140 0.081 Uiso 1 1 calc R U . . . C6 C 0.388(3) 0.230(3) 0.8212(10) 0.057(8) Uani 1 1 d . . . . . C7 C 0.434(4) 0.156(2) 0.8528(9) 0.051(7) Uani 1 1 d . . . . . C8 C 0.461(4) 0.256(3) 0.7823(13) 0.073(11) Uani 1 1 d . . . . . H8 H 0.4137 0.3007 0.7647 0.088 Uiso 1 1 calc R U . . . C9 C 0.625(5) 0.260(3) 0.7249(16) 0.079(13) Uani 1 1 d . . . . . H9A H 0.6300 0.3292 0.7256 0.094 Uiso 1 1 calc R U . . . H9B H 0.5469 0.2415 0.7046 0.094 Uiso 1 1 calc R U . . . C10 C 0.779(4) 0.218(2) 0.7090(13) 0.065(9) Uani 1 1 d . . . . . H10A H 0.7690 0.1495 0.7060 0.078 Uiso 1 1 calc R U . . . H10B H 0.7994 0.2442 0.6804 0.078 Uiso 1 1 calc R U . . . C11 C 0.909(4) 0.238(3) 0.7367(11) 0.065(9) Uani 1 1 d . . . . . H11A H 0.9023 0.3032 0.7474 0.078 Uiso 1 1 calc R U . . . H11B H 0.9993 0.2334 0.7192 0.078 Uiso 1 1 calc R U . . . C12 C 1.040(3) 0.124(2) 0.7793(11) 0.053(6) Uani 1 1 d . . . . . H12 H 1.1155 0.1349 0.7591 0.064 Uiso 1 1 calc R U . . . C13 C 1.070(3) 0.056(2) 0.8124(9) 0.047(6) Uani 1 1 d . . . . . C14 C 1.212(3) 0.008(2) 0.8124(9) 0.049(5) Uani 1 1 d . . . . . H14 H 1.2826 0.0241 0.7916 0.058 Uiso 1 1 calc R U . . . C15 C 1.246(3) -0.063(3) 0.8423(11) 0.058(7) Uani 1 1 d . . . . . H15 H 1.3371 -0.0950 0.8402 0.070 Uiso 1 1 calc R U . . . C16 C 1.145(3) -0.090(2) 0.8764(15) 0.070(10) Uani 1 1 d . . . . . H16 H 1.1686 -0.1355 0.8972 0.084 Uiso 1 1 calc R U . . . C17 C 1.004(4) -0.0393(19) 0.8759(9) 0.050(6) Uani 1 1 d . . . . . C18 C 0.975(3) 0.0332(17) 0.8438(11) 0.049(7) Uani 1 1 d . . . . . C19 C 0.930(4) -0.145(3) 0.9331(14) 0.071(10) Uani 1 1 d . . . . . H19A H 0.8438 -0.1539 0.9513 0.106 Uiso 1 1 calc R U . . . H19B H 0.9482 -0.2023 0.9167 0.106 Uiso 1 1 calc R U . . . H19C H 1.0158 -0.1312 0.9509 0.106 Uiso 1 1 calc R U . . . C20 C 0.776(3) 0.353(2) 0.8494(9) 0.045(6) Uani 1 1 d . . . . . C21 C 0.961(4) 0.486(2) 0.8178(10) 0.058(7) Uani 1 1 d . . . . . C22 C 0.897(4) 0.415(2) 0.9202(9) 0.051(6) Uani 1 1 d . . . . . C23 C 1.009(4) 0.589(3) 0.8878(10) 0.058(7) Uani 1 1 d . . . . . C24 C 0.759(6) 0.578(7) 0.9300(18) 0.15(3) Uani 1 1 d . . . . . C25 C 0.773(4) 0.652(2) 0.8452(10) 0.054(7) Uani 1 1 d . . . . . C26 C 0.574(5) 0.482(4) 0.895(2) 0.139(18) Uani 1 1 d D U . . . C27 C 0.646(4) 0.514(2) 0.8154(10) 0.073(8) Uani 1 1 d D U . . . Lu1 Lu 0.65955(11) 0.01658(8) 0.89751(3) 0.0413(3) Uani 1 1 d . . . . . N1 N 0.587(3) 0.2226(18) 0.7693(7) 0.048(5) Uani 1 1 d . . . . . N2 N 0.923(3) 0.1707(16) 0.7749(9) 0.052(6) Uani 1 1 d . . . . . N3 N 0.762(2) 0.2855(18) 0.8401(7) 0.044(5) Uani 1 1 d . . . . . N4 N 1.047(3) 0.480(2) 0.7901(9) 0.061(7) Uani 1 1 d . . . . . N5 N 0.941(4) 0.371(2) 0.9481(10) 0.069(8) Uani 1 1 d . . . . . N6 N 1.109(4) 0.620(3) 0.8990(18) 0.100(14) Uani 1 1 d . . . . . N7 N 0.735(4) 0.6382(18) 0.9571(10) 0.071(9) Uani 1 1 d . . . . . N8 N 0.766(9) 0.734(3) 0.8379(14) 0.15(3) Uani 1 1 d . . . . . N9 N 0.475(4) 0.445(3) 0.910(2) 0.129(17) Uani 1 1 d D U . . . N10 N 0.566(4) 0.515(3) 0.7875(10) 0.077(8) Uani 1 1 d D U . . . Ni1 Ni 0.7306(4) 0.1523(2) 0.80734(11) 0.0399(7) Uani 1 1 d . . . . . O1 O 0.413(2) 0.0757(17) 0.9165(7) 0.055(5) Uani 1 1 d . . . . . O2 O 0.561(2) 0.1086(15) 0.8469(5) 0.046(4) Uani 1 1 d . . . . . O3 O 0.836(2) 0.0724(11) 0.8526(5) 0.039(3) Uani 1 1 d . . . . . O4 O 0.903(2) -0.0625(18) 0.9025(8) 0.063(6) Uani 1 1 d . . . . . O5 O 0.722(3) 0.1665(15) 0.9251(7) 0.067(7) Uani 1 1 d . . . . . O6 O 0.687(3) 0.000(2) 0.9745(7) 0.077(7) Uani 1 1 d . . . . . O7 O 0.552(3) -0.1217(17) 0.9188(8) 0.066(6) Uani 1 1 d . . . . . O8 O 0.637(3) -0.0815(15) 0.8380(7) 0.053(5) Uani 1 1 d . . . . . O9 O 0.696(2) 0.0138(14) 0.7666(5) 0.047(4) Uani 1 1 d . . . . . O10 O 0.789(5) 0.123(3) 1.0303(11) 0.103(11) Uani 1 1 d . . . . . W1 W 0.80111(10) 0.50880(7) 0.86987(3) 0.0418(3) Uani 1 1 d . . . . . 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 C1 0.07(2) 0.14(3) 0.029(12) 0.013(14) 0.003(12) -0.05(2) C2 0.032(10) 0.037(13) 0.09(2) -0.009(11) 0.011(12) -0.009(9) C3 0.041(13) 0.051(16) 0.10(3) -0.026(16) 0.017(15) 0.005(11) C4 0.047(17) 0.09(3) 0.11(3) -0.03(2) -0.016(19) 0.032(17) C5 0.057(18) 0.039(15) 0.11(3) -0.008(15) -0.013(18) 0.023(13) C6 0.035(12) 0.08(2) 0.052(16) -0.011(14) -0.006(10) 0.025(13) C7 0.072(18) 0.040(13) 0.041(12) -0.006(9) 0.009(12) 0.028(12) C8 0.07(2) 0.08(3) 0.07(2) 0.04(2) -0.011(17) 0.019(18) C9 0.07(2) 0.06(2) 0.10(3) 0.05(2) 0.00(2) 0.013(18) C10 0.08(2) 0.038(15) 0.08(2) 0.005(13) 0.013(17) 0.015(14) C11 0.066(19) 0.08(2) 0.053(18) 0.014(14) 0.032(15) 0.010(16) C12 0.036(12) 0.061(18) 0.063(17) -0.009(13) -0.002(11) -0.011(11) C13 0.039(12) 0.062(16) 0.041(12) -0.022(11) -0.003(9) -0.001(10) C14 0.036(10) 0.048(14) 0.062(14) -0.015(11) 0.004(9) 0.000(10) C15 0.044(13) 0.07(2) 0.058(17) -0.018(14) -0.021(13) 0.004(12) C16 0.042(14) 0.036(14) 0.13(3) -0.004(16) -0.020(17) 0.017(11) C17 0.061(15) 0.038(13) 0.052(15) 0.013(10) -0.013(12) 0.015(10) C18 0.034(11) 0.026(12) 0.09(2) 0.007(10) 0.007(11) -0.019(8) C19 0.057(18) 0.07(2) 0.09(3) 0.030(19) -0.005(17) 0.002(15) C20 0.048(14) 0.046(14) 0.040(12) -0.015(10) -0.003(10) -0.001(10) C21 0.067(16) 0.053(16) 0.053(14) 0.005(13) -0.008(12) 0.009(14) C22 0.066(17) 0.046(15) 0.041(13) -0.004(10) 0.015(12) -0.010(12) C23 0.059(17) 0.07(2) 0.046(15) -0.011(12) -0.008(12) -0.012(15) C24 0.06(3) 0.31(10) 0.08(3) 0.03(5) 0.05(3) 0.01(4) C25 0.071(19) 0.047(15) 0.045(14) 0.013(10) -0.016(13) 0.005(13) C26 0.10(2) 0.09(3) 0.22(5) 0.07(3) 0.08(3) -0.01(2) C27 0.11(2) 0.030(11) 0.080(17) 0.012(12) -0.001(15) -0.037(14) Lu1 0.0423(5) 0.0392(5) 0.0425(5) 0.0030(4) -0.0008(3) -0.0020(4) N1 0.058(14) 0.049(13) 0.038(11) 0.009(8) -0.017(10) 0.004(10) N2 0.058(14) 0.026(10) 0.071(16) -0.002(9) 0.015(12) 0.004(8) N3 0.038(10) 0.061(15) 0.034(10) 0.004(9) -0.001(8) 0.003(9) N4 0.053(12) 0.058(15) 0.074(17) 0.019(13) 0.024(11) 0.006(12) N5 0.072(18) 0.07(2) 0.061(17) 0.006(13) -0.016(14) 0.005(15) N6 0.07(2) 0.08(3) 0.15(4) 0.01(3) -0.03(3) -0.006(18) N7 0.11(3) 0.036(12) 0.063(16) -0.026(11) 0.023(16) -0.028(14) N8 0.34(9) 0.041(16) 0.08(2) -0.003(15) -0.02(4) -0.04(3) N9 0.08(2) 0.07(2) 0.24(5) 0.04(3) 0.08(3) -0.008(17) N10 0.087(17) 0.058(14) 0.084(17) 0.016(14) -0.036(13) -0.020(14) Ni1 0.0395(15) 0.0373(15) 0.0430(15) 0.0024(11) 0.0016(12) 0.0007(11) O1 0.044(10) 0.063(13) 0.059(13) 0.007(9) 0.005(8) 0.006(9) O2 0.047(9) 0.067(12) 0.025(7) 0.002(7) 0.005(6) 0.018(9) O3 0.042(8) 0.028(7) 0.046(9) 0.006(6) 0.009(7) -0.003(6) O4 0.050(11) 0.072(15) 0.068(15) 0.016(11) -0.016(10) 0.009(10) O5 0.12(2) 0.043(11) 0.034(9) -0.007(7) 0.012(11) -0.001(12) O6 0.095(17) 0.098(19) 0.038(9) 0.020(11) -0.014(10) 0.006(18) O7 0.087(17) 0.057(14) 0.053(13) -0.004(9) -0.002(11) -0.025(12) O8 0.058(12) 0.046(11) 0.054(11) 0.009(8) 0.012(9) 0.003(9) O9 0.055(9) 0.044(9) 0.041(8) 0.003(7) 0.000(7) 0.001(9) O10 0.15(3) 0.10(2) 0.067(19) -0.007(15) 0.02(2) 0.01(2) W1 0.0407(4) 0.0354(5) 0.0492(5) -0.0013(4) -0.0004(3) 0.0021(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 C1 O1 1.44(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.36(4) . ? C2 C3 1.40(3) . ? C2 O1 1.40(4) . ? C3 C4 1.48(6) . ? C3 H3 0.9300 . ? C4 C5 1.30(6) . ? C4 H4 0.9300 . ? C5 C6 1.43(4) . ? C5 H5 0.9300 . ? C6 C8 1.41(5) . ? C6 C7 1.48(4) . ? C7 O2 1.33(3) . ? C8 N1 1.28(5) . ? C8 H8 0.9300 . ? C9 N1 1.50(4) . ? C9 C10 1.57(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.47(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.51(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.23(4) . ? C12 C13 1.42(5) . ? C12 H12 0.9300 . ? C13 C18 1.32(4) . ? C13 C14 1.44(3) . ? C14 C15 1.39(5) . ? C14 H14 0.9300 . ? C15 C16 1.43(6) . ? C15 H15 0.9300 . ? C16 C17 1.44(3) . ? C16 H16 0.9300 . ? C17 O4 1.26(4) . ? C17 C18 1.44(4) . ? C18 O3 1.38(3) . ? C19 O4 1.51(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N3 0.99(3) . ? C20 W1 2.28(3) . ? C21 N4 1.16(4) . ? C21 W1 2.17(3) . ? C22 N5 1.13(4) . ? C22 W1 2.20(3) . ? C23 N6 1.06(5) . ? C23 W1 2.23(3) . ? C24 N7 1.21(8) . ? C24 W1 2.12(7) . ? C25 N8 1.17(5) . ? C25 W1 2.15(3) . ? C26 N9 1.122(7) . ? C26 W1 2.21(3) . ? C27 N10 1.122(7) . ? C27 W1 2.17(2) . ? Lu1 O2 2.201(18) . ? Lu1 O3 2.236(16) . ? Lu1 O7 2.25(2) . ? Lu1 O8 2.30(2) . ? Lu1 O5 2.32(2) . ? Lu1 O6 2.397(19) . ? Lu1 O1 2.42(2) . ? Lu1 O4 2.44(2) . ? Lu1 Ni1 3.421(3) . ? N1 Ni1 2.00(2) . ? N2 Ni1 2.01(2) . ? N3 Ni1 2.13(3) . ? Ni1 O3 2.019(17) . ? Ni1 O2 2.03(2) . ? Ni1 O9 2.32(2) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 126(3) . . ? C7 C2 O1 110(2) . . ? C3 C2 O1 124(3) . . ? C2 C3 C4 113(3) . . ? C2 C3 H3 123.5 . . ? C4 C3 H3 123.5 . . ? C5 C4 C3 124(3) . . ? C5 C4 H4 117.9 . . ? C3 C4 H4 117.9 . . ? C4 C5 C6 121(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C8 C6 C5 115(3) . . ? C8 C6 C7 128(3) . . ? C5 C6 C7 117(3) . . ? O2 C7 C2 122(3) . . ? O2 C7 C6 120(3) . . ? C2 C7 C6 118(2) . . ? N1 C8 C6 125(3) . . ? N1 C8 H8 117.3 . . ? C6 C8 H8 117.3 . . ? N1 C9 C10 111(3) . . ? N1 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 116(3) . . ? C11 C10 H10A 108.2 . . ? C9 C10 H10A 108.2 . . ? C11 C10 H10B 108.2 . . ? C9 C10 H10B 108.2 . . ? H10A C10 H10B 107.3 . . ? C10 C11 N2 114(3) . . ? C10 C11 H11A 108.8 . . ? N2 C11 H11A 108.8 . . ? C10 C11 H11B 108.8 . . ? N2 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N2 C12 C13 126(3) . . ? N2 C12 H12 117.0 . . ? C13 C12 H12 117.0 . . ? C18 C13 C12 125(3) . . ? C18 C13 C14 117(3) . . ? C12 C13 C14 119(3) . . ? C15 C14 C13 122(3) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C16 122(3) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C15 C16 C17 115(3) . . ? C15 C16 H16 122.6 . . ? C17 C16 H16 122.6 . . ? O4 C17 C18 120(2) . . ? O4 C17 C16 120(3) . . ? C18 C17 C16 120(3) . . ? C13 C18 O3 128(3) . . ? C13 C18 C17 124(3) . . ? O3 C18 C17 108(2) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 W1 178(3) . . ? N4 C21 W1 176(3) . . ? N5 C22 W1 175(3) . . ? N6 C23 W1 173(4) . . ? N7 C24 W1 163(6) . . ? N8 C25 W1 170(3) . . ? N9 C26 W1 161(5) . . ? N10 C27 W1 179(3) . . ? O2 Lu1 O3 68.9(7) . . ? O2 Lu1 O7 122.4(9) . . ? O3 Lu1 O7 141.2(8) . . ? O2 Lu1 O8 75.4(7) . . ? O3 Lu1 O8 77.0(7) . . ? O7 Lu1 O8 71.7(8) . . ? O2 Lu1 O5 80.2(8) . . ? O3 Lu1 O5 75.2(8) . . ? O7 Lu1 O5 140.0(8) . . ? O8 Lu1 O5 148.1(7) . . ? O2 Lu1 O6 143.0(8) . . ? O3 Lu1 O6 124.9(8) . . ? O7 Lu1 O6 70.9(9) . . ? O8 Lu1 O6 137.9(9) . . ? O5 Lu1 O6 72.5(9) . . ? O2 Lu1 O1 67.1(7) . . ? O3 Lu1 O1 132.1(7) . . ? O7 Lu1 O1 80.4(9) . . ? O8 Lu1 O1 108.5(8) . . ? O5 Lu1 O1 79.7(9) . . ? O6 Lu1 O1 83.6(8) . . ? O2 Lu1 O4 131.5(8) . . ? O3 Lu1 O4 64.5(8) . . ? O7 Lu1 O4 88.6(10) . . ? O8 Lu1 O4 81.9(9) . . ? O5 Lu1 O4 99.8(10) . . ? O6 Lu1 O4 78.6(9) . . ? O1 Lu1 O4 161.3(8) . . ? O2 Lu1 Ni1 34.5(5) . . ? O3 Lu1 Ni1 34.4(5) . . ? O7 Lu1 Ni1 142.1(6) . . ? O8 Lu1 Ni1 72.4(5) . . ? O5 Lu1 Ni1 75.8(5) . . ? O6 Lu1 Ni1 146.9(7) . . ? O1 Lu1 Ni1 100.1(5) . . ? O4 Lu1 Ni1 97.8(6) . . ? C8 N1 C9 111(3) . . ? C8 N1 Ni1 124(2) . . ? C9 N1 Ni1 124(2) . . ? C12 N2 C11 119(3) . . ? C12 N2 Ni1 127(2) . . ? C11 N2 Ni1 113.3(19) . . ? C20 N3 Ni1 169(2) . . ? N1 Ni1 N2 101.4(11) . . ? N1 Ni1 O3 167.7(9) . . ? N2 Ni1 O3 90.9(9) . . ? N1 Ni1 O2 91.2(9) . . ? N2 Ni1 O2 166.8(9) . . ? O3 Ni1 O2 76.5(7) . . ? N1 Ni1 N3 86.3(10) . . ? N2 Ni1 N3 90.7(9) . . ? O3 Ni1 N3 95.3(8) . . ? O2 Ni1 N3 94.2(8) . . ? N1 Ni1 O9 90.3(9) . . ? N2 Ni1 O9 87.1(8) . . ? O3 Ni1 O9 88.6(7) . . ? O2 Ni1 O9 88.7(7) . . ? N3 Ni1 O9 175.6(7) . . ? N1 Ni1 Lu1 129.0(8) . . ? N2 Ni1 Lu1 129.4(8) . . ? O3 Ni1 Lu1 38.7(5) . . ? O2 Ni1 Lu1 37.8(5) . . ? N3 Ni1 Lu1 97.0(6) . . ? O9 Ni1 Lu1 87.4(4) . . ? C2 O1 C1 116(3) . . ? C2 O1 Lu1 117.1(16) . . ? C1 O1 Lu1 127(2) . . ? C7 O2 Ni1 124.7(18) . . ? C7 O2 Lu1 122.2(16) . . ? Ni1 O2 Lu1 107.7(8) . . ? C18 O3 Ni1 120.0(16) . . ? C18 O3 Lu1 128.1(14) . . ? Ni1 O3 Lu1 106.9(8) . . ? C17 O4 C19 119(2) . . ? C17 O4 Lu1 118.7(17) . . ? C19 O4 Lu1 122(2) . . ? C24 W1 C25 82(2) . . ? C24 W1 C21 146.0(19) . . ? C25 W1 C21 87.2(13) . . ? C24 W1 C27 123(2) . . ? C25 W1 C27 67.9(11) . . ? C21 W1 C27 81.4(14) . . ? C24 W1 C22 74(2) . . ? C25 W1 C22 147.5(11) . . ? C21 W1 C22 100.3(11) . . ? C27 W1 C22 144.2(10) . . ? C24 W1 C26 67(3) . . ? C25 W1 C26 99.9(18) . . ? C21 W1 C26 147(2) . . ? C27 W1 C26 72(2) . . ? C22 W1 C26 90.6(19) . . ? C24 W1 C23 72.8(18) . . ? C25 W1 C23 73.7(14) . . ? C21 W1 C23 73.2(12) . . ? C27 W1 C23 134.6(12) . . ? C22 W1 C23 78.3(12) . . ? C26 W1 C23 139(2) . . ? C24 W1 C20 131(2) . . ? C25 W1 C20 141.1(10) . . ? C21 W1 C20 73.8(12) . . ? C27 W1 C20 75.8(11) . . ? C22 W1 C20 70.6(10) . . ? C26 W1 C20 81.3(19) . . ? C23 W1 C20 129.0(12) . . ? _refine_diff_density_max 3.956 _refine_diff_density_min -1.685 _refine_diff_density_rms 0.324 _shelxl_version_number 2014-3 _shelx_res_file ; TITL tr49 in P 21 21 21 CELL 0.71073 8.9298 13.9422 30.8112 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0007 0.0019 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H LU N NI O W UNIT 108 128 4 40 4 40 4 MERG 2 OMIT -3.00 56.00 OMIT 0 12 2 OMIT 0 12 6 OMIT -1 12 4 OMIT 0 9 1 OMIT 0 9 3 OMIT 0 6 2 OMIT 0 10 2 OMIT 0 2 4 OMIT 2 8 13 OMIT -1 2 2 OMIT 1 6 4 OMIT 1 0 2 OMIT 1 7 0 OMIT 0 5 1 OMIT 2 11 2 OMIT 1 2 2 OMIT 0 12 8 OMIT -4 9 6 OMIT 0 2 2 TWIN DFIX 1.120 0.005 N9 C26 N10 C27 SIMU 0.01 N9 C26 SIMU 0.01 N10 C27 FMAP 2 PLAN 10 ACTA BOND $H L.S. 8 WGHT 0.159700 EXTI 0.011261 BASF 0.13099 FVAR 0.26084 C1 1 0.326426 0.048830 0.953765 11.00000 0.07279 0.13581 = 0.02935 0.01280 0.00324 -0.04681 AFIX 33 H1A 2 0.377952 -0.000472 0.969580 11.00000 -1.50000 H1B 2 0.312633 0.103744 0.972132 11.00000 -1.50000 H1C 2 0.230576 0.025292 0.944511 11.00000 -1.50000 AFIX 0 C2 1 0.352600 0.147253 0.889994 11.00000 0.03155 0.03700 = 0.08693 -0.00935 0.01111 -0.00881 C3 1 0.217936 0.194122 0.898921 11.00000 0.04108 0.05078 = 0.09814 -0.02580 0.01732 0.00527 AFIX 43 H3 2 0.159669 0.181506 0.923278 11.00000 -1.20000 AFIX 0 C4 1 0.177583 0.266040 0.865536 11.00000 0.04682 0.08721 = 0.11007 -0.02998 -0.01606 0.03161 AFIX 43 H4 2 0.088052 0.299264 0.868963 11.00000 -1.20000 AFIX 0 C5 1 0.259308 0.285775 0.831699 11.00000 0.05676 0.03879 = 0.10808 -0.00821 -0.01255 0.02306 AFIX 43 H5 2 0.232969 0.337138 0.814019 11.00000 -1.20000 AFIX 0 C6 1 0.388369 0.230220 0.821211 11.00000 0.03464 0.08400 = 0.05206 -0.01104 -0.00618 0.02453 C7 1 0.434062 0.155974 0.852826 11.00000 0.07155 0.03980 = 0.04122 -0.00633 0.00862 0.02782 C8 1 0.460994 0.255903 0.782333 11.00000 0.06713 0.08037 = 0.07292 0.03504 -0.01142 0.01920 AFIX 43 H8 2 0.413701 0.300729 0.764676 11.00000 -1.20000 AFIX 0 C9 1 0.624999 0.259730 0.724870 11.00000 0.07435 0.06391 = 0.09792 0.04823 0.00361 0.01333 AFIX 23 H9A 2 0.630007 0.329210 0.725610 11.00000 -1.20000 H9B 2 0.546917 0.241504 0.704597 11.00000 -1.20000 AFIX 0 C10 1 0.779021 0.218443 0.708997 11.00000 0.08057 0.03844 = 0.07667 0.00455 0.01254 0.01541 AFIX 23 H10A 2 0.768967 0.149484 0.706012 11.00000 -1.20000 H10B 2 0.799381 0.244202 0.680354 11.00000 -1.20000 AFIX 0 C11 1 0.909212 0.237938 0.736695 11.00000 0.06603 0.07513 = 0.05282 0.01420 0.03228 0.01038 AFIX 23 H11A 2 0.902322 0.303184 0.747440 11.00000 -1.20000 H11B 2 0.999281 0.233387 0.719218 11.00000 -1.20000 AFIX 0 C12 1 1.040006 0.124280 0.779316 11.00000 0.03583 0.06102 = 0.06251 -0.00914 -0.00173 -0.01116 AFIX 43 H12 2 1.115488 0.134903 0.759083 11.00000 -1.20000 AFIX 0 C13 1 1.069640 0.056173 0.812435 11.00000 0.03889 0.06222 = 0.04079 -0.02161 -0.00303 -0.00052 C14 1 1.211517 0.007512 0.812366 11.00000 0.03566 0.04783 = 0.06231 -0.01471 0.00395 -0.00007 AFIX 43 H14 2 1.282568 0.024086 0.791611 11.00000 -1.20000 AFIX 0 C15 1 1.245642 -0.063464 0.842346 11.00000 0.04436 0.07330 = 0.05783 -0.01753 -0.02117 0.00400 AFIX 43 H15 2 1.337084 -0.095041 0.840214 11.00000 -1.20000 AFIX 0 C16 1 1.144998 -0.089637 0.876371 11.00000 0.04202 0.03606 = 0.13258 -0.00443 -0.01955 0.01695 AFIX 43 H16 2 1.168592 -0.135528 0.897182 11.00000 -1.20000 AFIX 0 C17 1 1.003912 -0.039310 0.875919 11.00000 0.06072 0.03792 = 0.05237 0.01333 -0.01281 0.01458 C18 1 0.974982 0.033188 0.843760 11.00000 0.03398 0.02629 = 0.08591 0.00695 0.00748 -0.01923 C19 1 0.930186 -0.144957 0.933138 11.00000 0.05677 0.06592 = 0.08918 0.03001 -0.00521 0.00166 AFIX 33 H19A 2 0.843850 -0.153868 0.951260 11.00000 -1.50000 H19B 2 0.948232 -0.202333 0.916726 11.00000 -1.50000 H19C 2 1.015801 -0.131216 0.950926 11.00000 -1.50000 AFIX 0 C20 1 0.775852 0.352643 0.849444 11.00000 0.04840 0.04602 = 0.04025 -0.01487 -0.00301 -0.00067 C21 1 0.960525 0.486058 0.817828 11.00000 0.06672 0.05287 = 0.05299 0.00509 -0.00814 0.00852 C22 1 0.897384 0.415460 0.920185 11.00000 0.06601 0.04648 = 0.04087 -0.00363 0.01528 -0.00991 C23 1 1.008564 0.588903 0.887793 11.00000 0.05886 0.06851 = 0.04554 -0.01084 -0.00801 -0.01160 C24 1 0.758769 0.577783 0.929984 11.00000 0.06129 0.31262 = 0.08079 0.02739 0.04978 0.00700 C25 1 0.773076 0.651995 0.845225 11.00000 0.07101 0.04714 = 0.04495 0.01303 -0.01603 0.00510 C26 1 0.573840 0.482479 0.895284 11.00000 0.10425 0.08966 = 0.22334 0.06556 0.07825 -0.00716 C27 1 0.646436 0.513784 0.815410 11.00000 0.10757 0.03045 = 0.07953 0.01247 -0.00067 -0.03668 LU1 3 0.659555 0.016585 0.897511 11.00000 0.04226 0.03924 = 0.04247 0.00296 -0.00078 -0.00198 N1 4 0.586814 0.222564 0.769319 11.00000 0.05821 0.04928 = 0.03769 0.00907 -0.01699 0.00443 N2 4 0.923483 0.170693 0.774866 11.00000 0.05800 0.02610 = 0.07097 -0.00215 0.01541 0.00391 N3 4 0.761799 0.285547 0.840146 11.00000 0.03845 0.06076 = 0.03363 0.00413 -0.00057 0.00315 N4 4 1.047272 0.479651 0.790052 11.00000 0.05260 0.05784 = 0.07372 0.01934 0.02430 0.00587 N5 4 0.941152 0.371324 0.948080 11.00000 0.07239 0.07191 = 0.06123 0.00628 -0.01601 0.00452 N6 4 1.109222 0.619947 0.899005 11.00000 0.07482 0.07942 = 0.14596 0.00588 -0.03285 -0.00598 N7 4 0.734834 0.638151 0.957122 11.00000 0.11428 0.03571 = 0.06338 -0.02601 0.02251 -0.02776 N8 4 0.765918 0.733982 0.837882 11.00000 0.34270 0.04142 = 0.07720 -0.00260 -0.01899 -0.04409 N9 4 0.475308 0.445270 0.910341 11.00000 0.08100 0.07052 = 0.23587 0.04194 0.07829 -0.00794 N10 4 0.565740 0.514993 0.787486 11.00000 0.08709 0.05802 = 0.08440 0.01606 -0.03620 -0.02004 NI1 5 0.730637 0.152311 0.807338 11.00000 0.03954 0.03729 = 0.04296 0.00236 0.00156 0.00073 O1 6 0.413419 0.075660 0.916453 11.00000 0.04389 0.06309 = 0.05948 0.00676 0.00497 0.00578 O2 6 0.561476 0.108638 0.846904 11.00000 0.04671 0.06711 = 0.02469 0.00181 0.00477 0.01811 O3 6 0.836043 0.072425 0.852649 11.00000 0.04226 0.02783 = 0.04642 0.00578 0.00871 -0.00318 O4 6 0.902989 -0.062470 0.902529 11.00000 0.05017 0.07214 = 0.06770 0.01587 -0.01640 0.00933 O5 6 0.721529 0.166483 0.925072 11.00000 0.12256 0.04345 = 0.03366 -0.00726 0.01160 -0.00097 O6 6 0.687384 0.000064 0.974516 11.00000 0.09536 0.09775 = 0.03757 0.02023 -0.01378 0.00568 O7 6 0.552017 -0.121705 0.918809 11.00000 0.08668 0.05681 = 0.05339 -0.00400 -0.00175 -0.02457 O8 6 0.637209 -0.081512 0.838006 11.00000 0.05820 0.04579 = 0.05439 0.00860 0.01157 0.00279 O9 6 0.696389 0.013830 0.766609 11.00000 0.05458 0.04431 = 0.04078 0.00300 -0.00011 0.00076 O10 6 0.788528 0.122634 1.030270 11.00000 0.14540 0.09547 = 0.06747 -0.00660 0.01945 0.00687 W1 7 0.801109 0.508801 0.869874 11.00000 0.04068 0.03541 = 0.04925 -0.00126 -0.00037 0.00212 HKLF 4 REM tr49 in P 21 21 21 REM R1 = 0.0840 for 6462 Fo > 4sig(Fo) and 0.0984 for all 7808 data REM 453 parameters refined using 14 restraints END WGHT 0.1597 0.0000 REM Highest difference peak 3.956, deepest hole -1.685, 1-sigma level 0.324 Q1 1 0.6596 0.0061 0.8686 11.00000 0.05 3.96 Q2 1 0.7857 0.5085 0.8426 11.00000 0.05 3.57 Q3 1 0.7927 0.5020 0.8960 11.00000 0.05 3.29 Q4 1 0.6725 0.0104 0.9233 11.00000 0.05 2.95 Q5 1 0.8442 -0.0038 0.8940 11.00000 0.05 2.79 Q6 1 0.7227 0.4862 0.8738 11.00000 0.05 2.56 Q7 1 0.4107 -0.2934 0.8932 11.00000 0.05 1.96 Q8 1 0.5647 0.2552 0.9910 11.00000 0.05 1.93 Q9 1 0.7600 0.0135 0.8577 11.00000 0.05 1.70 Q10 1 0.8307 0.4926 0.9294 11.00000 0.05 1.41 ; _shelx_res_checksum 40676 _shelx_hkl_file ; 13 -7 4 -3.35 22.82 -13 -7 -4 19.64 27.71 13 -7 3 -3.18 22.57 13 7 -3 20.20 33.68 -13 -7 -3 1.61 28.42 -13 -7 -2 4.38 27.94 13 -7 2 26.67 22.76 13 7 -2 11.88 32.90 13 -7 2 22.23 29.35 13 -7 2 -1.51 29.97 -13 -7 -1 8.37 28.47 13 7 -1 18.58 28.91 13 -7 1 5.07 22.36 13 -7 1 30.49 29.26 13 -7 1 28.21 24.72 -13 -7 0 0.89 29.05 -13 -6 -10 1.31 28.22 -13 -6 -9 -10.86 22.54 13 6 -8 12.74 46.74 13 -6 8 -7.53 28.83 13 -6 8 29.87 23.11 13 -6 8 35.17 23.99 -13 -6 -8 -13.37 27.51 13 -6 7 22.15 24.24 13 -6 7 4.15 24.18 13 -6 7 -1.24 22.82 -13 -6 -7 0.29 22.18 13 6 -7 9.87 37.84 13 6 -6 -5.37 36.86 13 -6 6 5.11 22.44 13 -6 6 39.57 23.91 -13 -6 -6 15.27 27.23 13 -6 6 -32.99 23.70 13 -6 5 14.59 23.65 13 6 -5 41.65 34.37 13 -6 5 13.37 22.21 -13 -6 -5 26.62 27.93 13 -6 5 29.59 23.93 13 -6 4 42.33 29.25 -13 -6 -4 24.39 28.33 13 -6 4 27.37 22.09 13 6 -4 28.74 32.34 13 -6 4 2.43 23.95 13 -6 3 51.46 28.60 -13 -6 -3 -18.83 28.25 13 -6 3 6.20 22.39 13 -6 3 10.50 28.92 13 6 -3 44.72 33.79 13 -6 2 39.40 22.14 -13 -6 -2 0.56 27.88 13 6 -2 13.83 32.52 13 -6 2 -0.62 29.14 13 -6 2 13.39 29.40 13 -6 1 29.95 22.66 13 -6 1 23.25 30.39 -13 -6 -1 18.74 28.14 13 6 -1 32.36 28.78 13 -6 1 41.18 30.70 -13 -6 0 28.51 28.96 -13 -5 -11 42.75 28.10 13 -5 11 38.00 22.57 13 -5 10 36.36 28.80 13 -5 10 21.07 23.52 -13 -5 -10 -7.32 22.46 13 -5 10 20.65 28.55 -13 -5 -9 0.79 27.16 13 -5 9 59.24 29.98 13 -5 9 9.06 28.15 13 -5 9 18.09 22.13 -13 -5 -8 10.49 22.38 13 -5 8 32.81 21.52 13 -5 8 7.78 23.11 13 5 -8 4.97 47.23 13 5 -8 14.57 46.19 13 -5 8 41.39 23.97 13 -5 7 -5.46 24.40 13 -5 7 7.19 23.17 -13 -5 -7 5.97 28.18 13 5 -7 17.58 41.09 13 -5 7 23.26 21.59 13 5 -7 27.72 41.44 13 -5 6 22.99 21.74 -13 -5 -6 1.27 27.14 13 -5 6 18.81 23.52 13 5 -6 14.79 36.89 13 -5 6 26.53 24.24 -13 -5 -5 -25.06 27.45 13 -5 5 3.55 24.06 13 -5 5 18.74 21.23 13 -5 5 -9.94 28.86 13 5 -5 18.62 37.17 13 -5 4 36.24 22.24 13 -5 4 34.07 29.01 13 5 -4 26.64 32.74 -13 -5 -4 37.02 27.32 13 -5 4 11.54 28.23 13 -5 3 -31.05 20.76 13 -5 3 35.71 28.44 13 5 -3 14.98 33.05 13 -5 3 -30.07 28.39 -13 -5 -3 24.12 27.80 13 5 -2 21.89 31.83 -13 -5 -2 -20.00 27.60 13 -5 2 20.33 23.22 13 -5 2 42.84 21.61 13 -5 2 23.95 28.76 13 -5 1 4.69 28.42 -13 -5 -1 20.09 27.29 13 -5 1 0.40 21.07 13 5 -1 33.24 31.18 13 -5 1 -4.02 28.52 -13 -5 0 13.39 27.79 13 -4 13 57.61 22.48 -13 -4 -13 -7.39 22.60 -13 -4 -12 9.96 27.88 13 -4 12 4.05 22.79 13 -4 12 2.30 21.84 13 -4 11 6.13 28.98 -13 -4 -11 22.96 22.81 13 -4 11 -30.77 22.08 -13 -4 -10 -19.67 28.35 13 -4 10 -2.83 20.84 13 -4 10 20.85 22.63 13 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14.28 21.28 13 -3 14 29.68 22.96 13 -3 13 -10.58 20.99 -13 -3 -13 5.33 22.51 13 -3 13 -23.60 23.15 13 -3 12 -4.35 21.08 -13 -3 -12 11.91 21.77 13 -3 12 23.11 28.09 13 -3 11 24.84 28.70 13 -3 11 19.07 26.27 -13 -3 -11 43.03 27.53 -13 -3 -10 19.44 21.89 13 -3 10 21.45 22.82 13 -3 10 38.99 26.43 13 -3 9 -15.05 21.32 13 -3 9 25.64 22.39 13 3 -9 5.28 51.39 13 3 -9 -3.37 53.27 -13 -3 -9 41.93 27.31 13 3 -8 5.31 43.83 13 3 -8 -2.08 42.12 -13 -3 -8 20.74 27.26 13 -3 8 34.03 22.94 13 -3 8 41.48 21.21 13 -3 7 49.93 20.63 13 3 -7 27.86 33.64 13 3 -7 -8.37 37.58 13 -3 7 15.37 22.42 -13 -3 -7 1.51 26.54 13 -3 6 42.91 29.16 -13 -3 -6 1.36 21.23 13 3 -6 -4.24 38.18 13 3 -6 20.09 36.04 13 -3 6 -12.62 22.87 13 3 -5 20.43 36.20 13 -3 5 5.18 23.07 13 -3 5 58.50 29.45 13 3 -5 40.24 35.49 -13 -3 -5 3.66 22.28 13 -3 4 45.52 28.07 -13 -3 -4 8.80 22.37 13 3 -4 19.74 32.40 13 -3 4 44.15 30.18 -13 -3 -3 19.83 22.16 13 3 -3 24.15 31.94 13 -3 3 -10.12 23.00 13 -3 3 41.36 28.23 13 -3 2 7.22 27.53 -13 -3 -2 16.36 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52.16 29.33 9 12 24 58.30 27.73 9 -12 -24 30.16 27.60 9 -12 -24 18.26 34.65 9 -13 0 37.43 27.00 9 -13 0 26.28 20.74 9 13 0 65.09 21.07 9 -13 0 26.00 21.88 9 -13 -1 58.50 30.88 -9 -13 1 18.74 26.06 9 -13 -1 22.99 25.22 9 13 1 43.38 25.32 9 -13 -1 47.13 21.62 9 -13 -2 65.81 31.23 -9 -13 2 36.40 26.43 9 -13 -2 45.59 20.24 9 -13 -2 31.10 27.29 9 13 2 49.69 21.71 9 -13 -3 76.83 31.89 -9 -13 3 39.48 26.63 9 -13 -3 43.17 21.42 9 -13 -3 39.10 22.72 9 13 3 82.42 25.87 9 -13 -4 63.80 31.64 -9 -13 4 42.09 26.79 9 -13 -4 22.27 21.01 9 -13 -4 46.77 27.58 9 13 4 46.34 25.46 9 -13 -5 28.32 32.31 -9 -13 5 48.86 26.97 9 -13 -5 29.54 22.87 9 -13 -5 32.95 21.02 9 13 5 35.35 20.95 9 13 6 7.93 20.18 9 -13 -6 0.30 31.52 -9 -13 6 13.03 26.35 9 -13 -6 15.67 21.25 9 -13 -6 9.04 19.54 9 13 7 32.79 20.50 9 -13 -7 38.58 32.79 -9 -13 7 42.36 31.27 9 -13 -7 43.37 28.05 9 13 8 60.75 21.31 9 -13 -8 30.66 36.07 -9 -13 8 43.82 27.74 9 -13 -8 12.74 22.60 9 -13 -9 17.42 25.05 9 13 9 37.63 25.16 9 -13 -9 25.09 31.70 -9 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