Supplementary data for CrystEngComm, paper b304201d This journal is © The Royal Society of Chemistry 2003 data_1 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C26 H28 Fe N4 O4 S' _chemical_formula_weight 548.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c (15)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.731(4) _cell_length_b 10.588(2) _cell_length_c 11.685(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.50(3) _cell_angle_gamma 90.00 _cell_volume 2518.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3732 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 11645 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2448 _reflns_number_observed 1596 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2448 _refine_ls_number_parameters 165 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_obs 0.0358 _refine_ls_wR_factor_all 0.0817 _refine_ls_wR_factor_obs 0.0739 _refine_ls_goodness_of_fit_all 0.895 _refine_ls_restrained_S_all 0.895 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.5000 0.0000 0.5000 0.02663(16) Uani 1 2 d S . . N2 N 0.10628(9) 0.5505(2) 0.59685(18) 0.0310(5) Uani 1 1 d . . . C8 C 0.31488(12) 0.6222(2) 0.7724(3) 0.0401(7) Uani 1 1 d . . . H8A H 0.3242 0.6395 0.8584 0.048 Uiso 1 1 calc R . . H8B H 0.3266 0.6968 0.7364 0.048 Uiso 1 1 calc R . . C3 C 0.39211(13) 0.3778(2) 0.6145(2) 0.0360(6) Uani 1 1 d . . . C2 C 0.44598(13) 0.3943(3) 0.5781(3) 0.0443(7) Uani 1 1 d . . . H2 H 0.4606 0.4753 0.5701 0.053 Uiso 1 1 calc R . . C13 C 0.13683(12) 0.6433(2) 0.5593(2) 0.0353(6) Uani 1 1 d . . . H13 H 0.1121 0.6933 0.4940 0.042 Uiso 1 1 calc R . . N1 N 0.46224(10) 0.1714(2) 0.56793(18) 0.0349(5) Uani 1 1 d . . . C9 C 0.24231(12) 0.5986(2) 0.7119(2) 0.0322(6) Uani 1 1 d . . . C12 C 0.20328(13) 0.6684(2) 0.6129(2) 0.0359(6) Uani 1 1 d . . . H12 H 0.2220 0.7330 0.5820 0.043 Uiso 1 1 calc R . . C1 C 0.47781(13) 0.2906(3) 0.5538(3) 0.0432(7) Uani 1 1 d . . . H1 H 0.5123 0.3048 0.5258 0.052 Uiso 1 1 calc R . . C5 C 0.41330(14) 0.1563(3) 0.6109(3) 0.0472(8) Uani 1 1 d . . . H5 H 0.4029 0.0746 0.6271 0.057 Uiso 1 1 calc R . . C4 C 0.37733(14) 0.2544(3) 0.6327(3) 0.0483(8) Uani 1 1 d . . . H4 H 0.3428 0.2374 0.6599 0.058 Uiso 1 1 calc R . . C6 C 0.35102(13) 0.4875(2) 0.6296(2) 0.0417(7) Uani 1 1 d . . . H6A H 0.3052 0.4706 0.5827 0.050 Uiso 1 1 calc R . . H6B H 0.3637 0.5629 0.5962 0.050 Uiso 1 1 calc R . . C11 C 0.14400(12) 0.4825(2) 0.6920(2) 0.0366(7) Uani 1 1 d . . . H11 H 0.1244 0.4170 0.7198 0.044 Uiso 1 1 calc R . . C7 C 0.35809(12) 0.5120(2) 0.7611(2) 0.0395(7) Uani 1 1 d . . . H7A H 0.4037 0.5309 0.8080 0.047 Uiso 1 1 calc R . . H7B H 0.3460 0.4365 0.7952 0.047 Uiso 1 1 calc R . . C10 C 0.21026(12) 0.5036(2) 0.7514(2) 0.0387(6) Uani 1 1 d . . . H10 H 0.2336 0.4540 0.8182 0.046 Uiso 1 1 calc R . . S S 0.5000 -0.18022(8) 0.7500 0.0277(2) Uani 1 2 d SD . . O1 O 0.49835(9) -0.09706(18) 0.64811(15) 0.0474(5) Uani 1 1 d D . . O2 O 0.55932(10) -0.2545(2) 0.78761(18) 0.0679(7) Uani 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 Fe 0.0240(3) 0.0306(3) 0.0284(3) 0.0015(2) 0.0130(2) -0.0002(2) N2 0.0282(12) 0.0328(12) 0.0339(13) 0.0006(10) 0.0134(10) -0.0010(10) C8 0.0254(15) 0.0420(17) 0.0517(17) -0.0127(14) 0.0119(14) 0.0008(12) C3 0.0404(16) 0.0361(16) 0.0333(15) -0.0052(12) 0.0152(13) 0.0000(13) C2 0.0424(17) 0.0318(16) 0.064(2) -0.0054(14) 0.0250(16) -0.0066(13) C13 0.0318(16) 0.0366(16) 0.0369(16) 0.0038(12) 0.0114(13) -0.0003(12) N1 0.0354(13) 0.0352(13) 0.0384(13) -0.0005(10) 0.0185(11) 0.0007(10) C9 0.0281(14) 0.0302(15) 0.0417(16) -0.0094(12) 0.0165(13) -0.0003(12) C12 0.0355(16) 0.0356(16) 0.0410(16) -0.0027(13) 0.0189(13) -0.0076(13) C1 0.0338(16) 0.0408(18) 0.0612(19) -0.0030(15) 0.0245(15) -0.0057(14) C5 0.062(2) 0.0346(17) 0.063(2) 0.0004(14) 0.0445(17) -0.0003(15) C4 0.058(2) 0.0423(18) 0.066(2) -0.0024(15) 0.0488(18) -0.0017(15) C6 0.0377(16) 0.0409(17) 0.0466(17) -0.0024(14) 0.0150(13) 0.0051(14) C11 0.0345(15) 0.0311(16) 0.0490(17) 0.0057(13) 0.0206(13) 0.0003(12) C7 0.0276(14) 0.0407(17) 0.0488(17) -0.0053(14) 0.0117(13) 0.0025(13) C10 0.0296(14) 0.0387(16) 0.0462(16) 0.0059(14) 0.0115(13) 0.0055(14) S 0.0309(5) 0.0252(5) 0.0287(5) 0.000 0.0124(4) 0.000 O1 0.0417(11) 0.0677(14) 0.0347(11) 0.0150(10) 0.0157(9) -0.0082(10) O2 0.0655(15) 0.0613(14) 0.0642(15) -0.0046(11) 0.0069(12) 0.0425(12) _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 Fe O1 2.0238(16) 5_656 ? Fe O1 2.0239(16) . ? Fe N1 2.248(2) . ? Fe N1 2.248(2) 5_656 ? Fe N2 2.252(2) 7_556 ? Fe N2 2.252(2) 3_545 ? N2 C11 1.337(3) . ? N2 C13 1.343(3) . ? N2 Fe 2.252(2) 3_455 ? C8 C9 1.506(3) . ? C8 C7 1.532(3) . ? C3 C4 1.379(4) . ? C3 C2 1.390(4) . ? C3 C6 1.512(3) . ? C2 C1 1.379(4) . ? C13 C12 1.384(3) . ? N1 C1 1.332(3) . ? N1 C5 1.335(3) . ? C9 C12 1.385(3) . ? C9 C10 1.391(3) . ? C5 C4 1.376(4) . ? C6 C7 1.513(3) . ? C11 C10 1.380(3) . ? S O2 1.4409(18) 2_656 ? S O2 1.4409(18) . ? S O1 1.4712(17) 2_656 ? S O1 1.4712(17) . ? 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 Fe O1 180.0 5_656 . ? O1 Fe N1 90.57(8) 5_656 . ? O1 Fe N1 89.43(8) . . ? O1 Fe N1 89.43(8) 5_656 5_656 ? O1 Fe N1 90.57(8) . 5_656 ? N1 Fe N1 180.000(1) . 5_656 ? O1 Fe N2 90.74(8) 5_656 7_556 ? O1 Fe N2 89.26(8) . 7_556 ? N1 Fe N2 86.11(7) . 7_556 ? N1 Fe N2 93.89(7) 5_656 7_556 ? O1 Fe N2 89.26(8) 5_656 3_545 ? O1 Fe N2 90.74(8) . 3_545 ? N1 Fe N2 93.89(7) . 3_545 ? N1 Fe N2 86.11(7) 5_656 3_545 ? N2 Fe N2 180.00(6) 7_556 3_545 ? C11 N2 C13 115.9(2) . . ? C11 N2 Fe 120.82(17) . 3_455 ? C13 N2 Fe 123.17(16) . 3_455 ? C9 C8 C7 114.0(2) . . ? C4 C3 C2 115.7(2) . . ? C4 C3 C6 122.0(2) . . ? C2 C3 C6 122.3(2) . . ? C1 C2 C3 120.0(2) . . ? N2 C13 C12 123.4(2) . . ? C1 N1 C5 115.5(2) . . ? C1 N1 Fe 125.54(17) . . ? C5 N1 Fe 118.25(18) . . ? C12 C9 C10 115.6(2) . . ? C12 C9 C8 122.5(2) . . ? C10 C9 C8 121.9(2) . . ? C13 C12 C9 120.8(2) . . ? N1 C1 C2 124.2(2) . . ? N1 C5 C4 123.9(3) . . ? C5 C4 C3 120.5(2) . . ? C3 C6 C7 113.3(2) . . ? N2 C11 C10 124.0(2) . . ? C6 C7 C8 111.8(2) . . ? C11 C10 C9 120.4(2) . . ? O2 S O2 113.9(2) 2_656 . ? O2 S O1 109.82(12) 2_656 2_656 ? O2 S O1 108.31(11) . 2_656 ? O2 S O1 108.31(11) 2_656 . ? O2 S O1 109.82(12) . . ? O1 S O1 106.47(16) 2_656 . ? S O1 Fe 173.35(13) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.297 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.054 data_2 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C12 H8 Cd N2 O4 S' _chemical_formula_weight 388.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P-421m (113)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' 'y+1/2, x+1/2, z' '-y+1/2, -x+1/2, z' '-y, x, -z' 'y, -x, -z' _cell_length_a 6.8307(10) _cell_length_b 6.8307(10) _cell_length_c 14.404(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 672.06(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 732 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 1.793 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 10709 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 30.54 _reflns_number_total 1124 _reflns_number_observed 1051 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.27(5) _refine_ls_number_reflns 1124 _refine_ls_number_parameters 65 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_obs 0.0208 _refine_ls_wR_factor_all 0.0483 _refine_ls_wR_factor_obs 0.0479 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_restrained_S_all 1.044 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd -0.5000 0.0000 -0.966057(15) 0.01517(8) Uani 1 4 d S . . S S -0.5000 -0.5000 -1.0000 0.01495(14) Uani 1 4 d S . . O O -0.5106(7) -0.32883(19) -0.93978(10) 0.0503(5) Uani 1 1 d . . . N1 N -0.5000 0.0000 -0.79896(19) 0.0222(6) Uani 1 4 d S . . C2 C -0.6157(4) -0.1157(4) -0.7516(3) 0.0533(13) Uani 1 2 d S . . H2 H -0.6988 -0.1988 -0.7842 0.064 Uiso 1 2 calc SR . . C3 C -0.6208(4) -0.1208(4) -0.6549(3) 0.0624(16) Uani 1 2 d S . . H3 H -0.7056 -0.2056 -0.6243 0.075 Uiso 1 2 calc SR . . C4 C -0.5000 0.0000 -0.6053(3) 0.0335(11) Uani 1 4 d S . . C5 C -0.5000 0.0000 -0.5052(3) 0.0408(12) Uani 1 4 d S . . C6 C -0.5000 0.0000 -0.4226(3) 0.0376(10) Uani 1 4 d S . . C7 C -0.5000 0.0000 -0.3230(2) 0.0282(8) Uani 1 4 d S . . C8 C -0.6212(4) -0.1212(4) -0.2731(3) 0.0605(15) Uani 1 2 d S . . H8 H -0.7060 -0.2060 -0.3036 0.073 Uiso 1 2 calc SR . . C9 C -0.6162(4) -0.1162(4) -0.1763(3) 0.0522(13) Uani 1 2 d S . . H9 H -0.6994 -0.1994 -0.1438 0.063 Uiso 1 2 calc SR . . N10 N -0.5000 0.0000 -0.1285(2) 0.0234(7) Uani 1 4 d S . . 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 Cd 0.01567(9) 0.01567(9) 0.01417(11) 0.000 0.000 -0.0003(3) S 0.01231(19) 0.01231(19) 0.0202(3) 0.000 0.000 0.000 O 0.1099(17) 0.0141(6) 0.0269(7) -0.0036(5) 0.0015(18) 0.0047(19) N1 0.0261(9) 0.0261(9) 0.0145(12) 0.000 0.000 -0.005(5) C2 0.069(2) 0.069(2) 0.0215(17) -0.0011(10) -0.0011(10) -0.045(3) C3 0.082(2) 0.082(2) 0.0221(19) 0.0050(11) 0.0050(11) -0.055(3) C4 0.0418(17) 0.0418(17) 0.0168(15) 0.000 0.000 0.017(7) C5 0.051(2) 0.051(2) 0.0208(17) 0.000 0.000 0.012(11) C6 0.0461(15) 0.0461(15) 0.0206(18) 0.000 0.000 -0.006(10) C7 0.0341(13) 0.0341(13) 0.0165(15) 0.000 0.000 -0.006(8) C8 0.080(2) 0.080(2) 0.0218(18) -0.0036(11) -0.0036(11) -0.056(3) C9 0.066(2) 0.066(2) 0.0244(18) 0.0022(10) 0.0022(10) -0.046(2) N10 0.0264(11) 0.0264(11) 0.0174(12) 0.000 0.000 0.016(5) _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 Cd O 2.2789(14) 6_445 ? Cd O 2.2789(14) 2_455 ? Cd O 2.2789(14) 5_455 ? Cd O 2.2789(14) . ? Cd N10 2.339(3) 1_554 ? Cd N1 2.407(3) . ? S O 1.4576(13) 7_453 ? S O 1.4576(13) 8_543 ? S O 1.4576(13) 2_445 ? S O 1.4576(13) . ? N1 C2 1.309(4) 2_455 ? N1 C2 1.309(4) . ? C2 C3 1.395(5) . ? C3 C4 1.368(5) . ? C4 C3 1.368(5) 2_455 ? C4 C5 1.443(6) . ? C5 C6 1.189(6) . ? C6 C7 1.435(5) . ? C7 C8 1.374(4) 2_455 ? C7 C8 1.374(4) . ? C8 C9 1.395(5) . ? C9 N10 1.317(4) . ? N10 C9 1.317(4) 2_455 ? N10 Cd 2.339(3) 1_556 ? 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 O Cd O 84.8(2) 6_445 2_455 ? O Cd O 160.88(8) 6_445 5_455 ? O Cd O 92.0(2) 2_455 5_455 ? O Cd O 92.0(2) 6_445 . ? O Cd O 160.88(8) 2_455 . ? O Cd O 84.8(2) 5_455 . ? O Cd N10 99.56(4) 6_445 1_554 ? O Cd N10 99.56(4) 2_455 1_554 ? O Cd N10 99.56(4) 5_455 1_554 ? O Cd N10 99.56(4) . 1_554 ? O Cd N1 80.44(4) 6_445 . ? O Cd N1 80.44(4) 2_455 . ? O Cd N1 80.44(4) 5_455 . ? O Cd N1 80.44(4) . . ? N10 Cd N1 180.000(1) 1_554 . ? O S O 106.97(12) 7_453 8_543 ? O S O 110.74(6) 7_453 2_445 ? O S O 110.74(6) 8_543 2_445 ? O S O 110.74(6) 7_453 . ? O S O 110.74(6) 8_543 . ? O S O 106.97(12) 2_445 . ? S O Cd 133.65(9) . . ? C2 N1 C2 117.2(4) 2_455 . ? C2 N1 Cd 121.38(19) 2_455 . ? C2 N1 Cd 121.38(19) . . ? N1 C2 C3 123.4(4) . . ? C4 C3 C2 119.4(4) . . ? C3 C4 C3 117.1(4) . 2_455 ? C3 C4 C5 121.4(2) . . ? C3 C4 C5 121.4(2) 2_455 . ? C6 C5 C4 180.000(1) . . ? C5 C6 C7 180.000(1) . . ? C8 C7 C8 116.9(4) 2_455 . ? C8 C7 C6 121.6(2) 2_455 . ? C8 C7 C6 121.6(2) . . ? C7 C8 C9 119.6(4) . . ? N10 C9 C8 123.5(4) . . ? C9 N10 C9 116.9(4) . 2_455 ? C9 N10 Cd 121.5(2) . 1_556 ? C9 N10 Cd 121.5(2) 2_455 1_556 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.511 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.089 data_3 _exptl_absorpt_correction_nazim 3 _diffrn_measurement_domega 1.1+0.35tg(theta) _diffrn_measurement_rtime 60 _chemical_formula_sum 'C12 H18 Cu N2 O7 S' _chemical_formula_weight 397.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 (2)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.399(3) _cell_length_b 9.496(3) _cell_length_c 10.073(4) _cell_angle_alpha 62.11(2) _cell_angle_beta 89.18(2) _cell_angle_gamma 73.00(2) _cell_volume 751.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 12 _exptl_crystal_description column _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 410 _exptl_absorpt_coefficient_mu 1.630 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method omega-scan _diffrn_standards_number 3 _diffrn_standards_interval_time 2h _diffrn_standards_decay_% 0 _diffrn_reflns_number 2620 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2620 _reflns_number_observed 2001 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+1.6800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2620 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_obs 0.0439 _refine_ls_wR_factor_all 0.1312 _refine_ls_wR_factor_obs 0.1199 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.0000 0.5000 0.0210(2) Uani 1 2 d S . . Cu2 Cu -0.5000 0.5000 0.5000 0.0251(2) Uani 1 2 d S . . N1 N 0.3867(4) 0.0629(5) 0.6454(4) 0.0221(8) Uani 1 1 d . . . C11 C 0.4511(5) 0.1072(6) 0.7311(5) 0.0242(10) Uani 1 1 d . . . H11 H 0.5468 0.1159 0.7166 0.029 Uiso 1 1 calc R . . C12 C 0.3828(5) 0.1404(6) 0.8392(5) 0.0240(10) Uani 1 1 d . . . H12 H 0.4317 0.1715 0.8956 0.029 Uiso 1 1 calc R . . C13 C 0.2409(5) 0.1276(6) 0.8641(5) 0.0232(10) Uani 1 1 d . . . C14 C 0.1718(6) 0.0865(6) 0.7722(5) 0.0274(11) Uani 1 1 d . . . H14 H 0.0754 0.0791 0.7832 0.033 Uiso 1 1 calc R . . C15 C 0.2472(5) 0.0568(6) 0.6647(5) 0.0262(10) Uani 1 1 d . . . H15 H 0.1988 0.0313 0.6029 0.031 Uiso 1 1 calc R . . C1 C 0.1675(6) 0.1558(7) 0.9876(5) 0.0309(12) Uani 1 1 d . . . H1A H 0.2453 0.1221 1.0688 0.037 Uiso 1 1 calc R . . H1B H 0.1053 0.0839 1.0289 0.037 Uiso 1 1 calc R . . C2 C 0.0701(6) 0.3388(7) 0.9341(6) 0.0314(12) Uani 1 1 d . . . H2A H 0.0418 0.3521 1.0215 0.038 Uiso 1 1 calc R . . H2B H 0.1279 0.4131 0.8813 0.038 Uiso 1 1 calc R . . N2 N -0.3207(5) 0.4519(5) 0.6394(5) 0.0293(9) Uani 1 1 d . . . C21 C -0.2083(6) 0.5093(6) 0.5845(6) 0.0297(11) Uani 1 1 d . . . H21 H -0.2140 0.5713 0.4798 0.036 Uiso 1 1 calc R . . C22 C -0.0829(6) 0.4817(7) 0.6749(6) 0.0310(12) Uani 1 1 d . . . H22 H -0.0080 0.5267 0.6310 0.037 Uiso 1 1 calc R . . C23 C -0.0698(6) 0.3875(6) 0.8297(6) 0.0288(11) Uani 1 1 d . . . C24 C -0.1890(6) 0.3298(8) 0.8884(6) 0.0370(13) Uani 1 1 d . . . H24 H -0.1857 0.2670 0.9928 0.044 Uiso 1 1 calc R . . C25 C -0.3119(6) 0.3666(7) 0.7904(6) 0.0372(13) Uani 1 1 d . . . H25 H -0.3921 0.3305 0.8312 0.045 Uiso 1 1 calc R . . S S -0.30695(13) 0.32469(14) 0.35208(13) 0.0206(3) Uani 1 1 d . . . O1 O -0.3696(4) 0.4903(4) 0.3506(4) 0.0269(8) Uani 1 1 d . . . O2 O -0.3906(4) 0.2142(4) 0.4465(4) 0.0331(8) Uani 1 1 d . . . O3 O -0.3236(4) 0.3585(5) 0.1949(4) 0.0369(9) Uani 1 1 d . . . O4 O -0.1474(4) 0.2511(5) 0.4168(4) 0.0353(9) Uani 1 1 d . . . O1S O 0.6711(4) -0.1652(4) 0.6667(4) 0.0279(8) Uani 1 1 d . . . O1W O 0.9152(4) -0.0742(5) 0.6767(4) 0.0375(9) Uani 1 1 d . . . O2W O 0.5632(5) -0.3177(5) 0.9316(4) 0.0408(9) 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 Cu1 0.0170(4) 0.0243(5) 0.0215(4) -0.0125(3) 0.0023(3) -0.0040(3) Cu2 0.0180(4) 0.0246(5) 0.0323(5) -0.0148(4) 0.0018(3) -0.0046(3) N1 0.021(2) 0.024(2) 0.022(2) -0.0120(17) 0.0032(16) -0.0067(17) C11 0.020(2) 0.027(3) 0.027(2) -0.012(2) 0.0015(19) -0.010(2) C12 0.027(3) 0.024(2) 0.023(2) -0.011(2) -0.001(2) -0.010(2) C13 0.020(2) 0.024(2) 0.023(2) -0.011(2) 0.0013(19) -0.004(2) C14 0.020(2) 0.034(3) 0.033(3) -0.019(2) 0.007(2) -0.011(2) C15 0.023(3) 0.031(3) 0.029(3) -0.017(2) 0.002(2) -0.011(2) C1 0.023(3) 0.044(3) 0.024(2) -0.018(2) 0.000(2) -0.005(2) C2 0.028(3) 0.040(3) 0.036(3) -0.027(2) 0.004(2) -0.010(2) N2 0.021(2) 0.032(2) 0.033(2) -0.0152(19) 0.0034(18) -0.0069(18) C21 0.025(3) 0.030(3) 0.032(3) -0.014(2) 0.003(2) -0.008(2) C22 0.025(3) 0.037(3) 0.034(3) -0.019(2) 0.005(2) -0.011(2) C23 0.022(2) 0.030(3) 0.034(3) -0.019(2) 0.001(2) -0.001(2) C24 0.029(3) 0.049(3) 0.027(3) -0.014(2) 0.003(2) -0.012(3) C25 0.027(3) 0.048(3) 0.038(3) -0.018(3) 0.010(2) -0.018(3) S 0.0182(6) 0.0201(6) 0.0248(6) -0.0117(5) 0.0035(4) -0.0066(5) O1 0.0237(18) 0.0246(18) 0.0362(19) -0.0176(15) 0.0061(14) -0.0080(14) O2 0.031(2) 0.032(2) 0.040(2) -0.0163(17) 0.0125(16) -0.0177(16) O3 0.043(2) 0.041(2) 0.0302(19) -0.0192(17) 0.0068(17) -0.0149(19) O4 0.0187(18) 0.035(2) 0.049(2) -0.0207(18) -0.0013(16) -0.0022(15) O1S 0.0215(17) 0.0284(19) 0.0283(18) -0.0120(15) -0.0001(14) -0.0037(15) O1W 0.0232(19) 0.050(2) 0.035(2) -0.0186(18) 0.0047(15) -0.0098(17) O2W 0.049(2) 0.041(2) 0.034(2) -0.0128(18) 0.0056(18) -0.0257(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1S 2.001(3) 2_656 ? Cu1 O1S 2.001(3) . ? Cu1 N1 2.010(4) . ? Cu1 N1 2.010(4) 2_656 ? Cu1 O2 2.381(3) 1_655 ? Cu1 O2 2.381(3) 2_556 ? Cu2 O1 1.946(3) 2_466 ? Cu2 O1 1.946(3) . ? Cu2 N2 2.009(4) . ? Cu2 N2 2.009(4) 2_466 ? Cu2 O2 2.904(4) 2_466 ? Cu2 O2 2.904(4) . ? N1 C15 1.337(6) . ? N1 C11 1.339(6) . ? C11 C12 1.371(7) . ? C12 C13 1.383(7) . ? C13 C14 1.391(7) . ? C13 C1 1.508(6) . ? C14 C15 1.379(7) . ? C1 C2 1.535(7) . ? C2 C23 1.509(7) . ? N2 C21 1.326(7) . ? N2 C25 1.338(7) . ? C21 C22 1.383(7) . ? C22 C23 1.372(7) . ? C23 C24 1.394(8) . ? C24 C25 1.380(8) . ? S O3 1.462(4) . ? S O2 1.466(3) . ? S O4 1.467(4) . ? S O1 1.502(3) . ? O2 Cu1 2.381(3) 1_455 ? 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 O1S Cu1 O1S 180.0 2_656 . ? O1S Cu1 N1 89.74(15) 2_656 . ? O1S Cu1 N1 90.26(15) . . ? O1S Cu1 N1 90.26(15) 2_656 2_656 ? O1S Cu1 N1 89.74(15) . 2_656 ? N1 Cu1 N1 180.0 . 2_656 ? O1S Cu1 O2 90.59(14) 2_656 1_655 ? O1S Cu1 O2 89.41(14) . 1_655 ? N1 Cu1 O2 88.22(14) . 1_655 ? N1 Cu1 O2 91.78(14) 2_656 1_655 ? O1S Cu1 O2 89.41(14) 2_656 2_556 ? O1S Cu1 O2 90.59(13) . 2_556 ? N1 Cu1 O2 91.78(14) . 2_556 ? N1 Cu1 O2 88.22(14) 2_656 2_556 ? O2 Cu1 O2 180.0 1_655 2_556 ? O1 Cu2 O1 180.000(1) 2_466 . ? O1 Cu2 N2 90.51(16) 2_466 . ? O1 Cu2 N2 89.49(16) . . ? O1 Cu2 N2 89.49(16) 2_466 2_466 ? O1 Cu2 N2 90.51(16) . 2_466 ? N2 Cu2 N2 180.0 . 2_466 ? O1 Cu2 O2 55.22(12) 2_466 2_466 ? O1 Cu2 O2 124.78(12) . 2_466 ? N2 Cu2 O2 80.95(14) . 2_466 ? N2 Cu2 O2 99.05(14) 2_466 2_466 ? O1 Cu2 O2 124.78(12) 2_466 . ? O1 Cu2 O2 55.22(12) . . ? N2 Cu2 O2 99.05(14) . . ? N2 Cu2 O2 80.95(14) 2_466 . ? O2 Cu2 O2 180.0 2_466 . ? C15 N1 C11 117.4(4) . . ? C15 N1 Cu1 121.9(3) . . ? C11 N1 Cu1 120.7(3) . . ? N1 C11 C12 123.1(4) . . ? C11 C12 C13 119.8(4) . . ? C12 C13 C14 117.2(4) . . ? C12 C13 C1 120.4(4) . . ? C14 C13 C1 122.5(4) . . ? C15 C14 C13 119.6(4) . . ? N1 C15 C14 122.8(4) . . ? C13 C1 C2 113.9(4) . . ? C23 C2 C1 111.1(4) . . ? C21 N2 C25 117.3(5) . . ? C21 N2 Cu2 120.9(3) . . ? C25 N2 Cu2 121.8(3) . . ? N2 C21 C22 123.4(5) . . ? N2 C21 Cu2 36.2(2) . . ? C22 C21 Cu2 159.6(4) . . ? C23 C22 C21 119.6(5) . . ? C22 C23 C24 117.3(5) . . ? C22 C23 C2 122.4(5) . . ? C24 C23 C2 120.2(5) . . ? C25 C24 C23 119.4(5) . . ? N2 C25 C24 122.9(5) . . ? N2 C25 Cu2 35.5(2) . . ? C24 C25 Cu2 158.3(4) . . ? O3 S O2 112.2(2) . . ? O3 S O4 110.1(2) . . ? O2 S O4 110.2(2) . . ? O3 S O1 107.5(2) . . ? O2 S O1 108.1(2) . . ? O4 S O1 108.6(2) . . ? O3 S Cu2 129.62(16) . . ? O2 S Cu2 73.42(15) . . ? O4 S Cu2 114.17(16) . . ? O1 S Cu2 35.62(13) . . ? S O1 Cu2 117.68(19) . . ? S O2 Cu1 150.9(2) . 1_455 ? S O2 Cu2 77.64(15) . . ? Cu1 O2 Cu2 127.62(13) 1_455 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.982 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.117 data_4 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C38 H44 Co2 N6 O10 S2' _chemical_formula_weight 926.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c (15)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.350(11) _cell_length_b 19.882(9) _cell_length_c 13.644(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.29(2) _cell_angle_gamma 90.00 _cell_volume 6080(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 872 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 0.17 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% decomposition _diffrn_reflns_number 4869 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.1218 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.08 _reflns_number_total 2960 _reflns_number_observed 1671 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2960 _refine_ls_number_parameters 264 _refine_ls_number_restraints 209 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_obs 0.0679 _refine_ls_wR_factor_all 0.1921 _refine_ls_wR_factor_obs 0.1807 _refine_ls_goodness_of_fit_all 0.939 _refine_ls_restrained_S_all 0.966 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.2500 0.5000 0.0322(5) Uani 1 2 d SU . . Co2 Co 0.0000 0.81207(7) 0.7500 0.0384(5) Uani 1 2 d SU . . S S 0.37835(8) 0.35186(11) 0.5614(2) 0.0450(7) Uani 1 1 d DU . . O1 O 0.43259(19) 0.3152(3) 0.6126(4) 0.0472(17) Uani 1 1 d DU . . O2 O 0.32826(19) 0.3051(3) 0.5335(4) 0.0433(16) Uani 1 1 d DU . . N1 N 0.1984(2) 0.3404(3) 0.5016(6) 0.0396(19) Uani 1 1 d U . . O3 O 0.3663(2) 0.4009(3) 0.6358(5) 0.071(2) Uani 1 1 d DU . . N3 N 0.2424(3) 0.2596(3) 0.3381(6) 0.044(2) Uani 1 1 d U . . O1S O 0.0485(2) 0.8842(3) 0.6939(5) 0.065(2) Uani 1 1 d U . . O4 O 0.3840(3) 0.3854(3) 0.4709(5) 0.091(3) Uani 1 1 d DU . . C10 C 0.0831(3) 0.6944(4) 0.7488(8) 0.053(3) Uani 1 1 d U . . H10 H 0.0925 0.7019 0.8188 0.063 Uiso 1 1 calc R . . C9 C 0.1115(4) 0.6433(5) 0.7167(10) 0.067(3) Uani 1 1 d U . . H9 H 0.1376 0.6156 0.7635 0.081 Uiso 1 1 calc R . . C3 C 0.1350(4) 0.4566(4) 0.5250(9) 0.068(3) Uani 1 1 d DU . . N2 N 0.0440(3) 0.7338(3) 0.6902(6) 0.045(2) Uani 1 1 d U . . C13 C 0.2110(4) 0.2135(5) 0.2708(7) 0.055(3) Uani 1 1 d U . . H13 H 0.1935 0.1780 0.2961 0.066 Uiso 1 1 calc R . . C8 C 0.1011(4) 0.6329(4) 0.6135(9) 0.063(3) Uani 1 1 d DU . . C4 C 0.1879(4) 0.4589(5) 0.5042(10) 0.080(3) Uani 1 1 d U . . H4 H 0.2047 0.5006 0.4988 0.096 Uiso 1 1 calc R . . C17 C 0.2696(4) 0.3064(5) 0.2997(8) 0.051(3) Uani 1 1 d U . . H17 H 0.2939 0.3368 0.3445 0.061 Uiso 1 1 calc R . . C1 C 0.1467(4) 0.3391(4) 0.5185(8) 0.061(3) Uani 1 1 d U . . H1 H 0.1304 0.2967 0.5213 0.073 Uiso 1 1 calc R . . C5 C 0.2186(4) 0.4010(5) 0.4904(8) 0.064(3) Uani 1 1 d U . . H5 H 0.2541 0.4053 0.4728 0.076 Uiso 1 1 calc R . . C6 C 0.1001(4) 0.5166(4) 0.5444(11) 0.096(4) Uani 1 1 d DU . . H6A H 0.0682 0.5255 0.4827 0.116 Uiso 1 1 calc R . . H6B H 0.0816 0.5047 0.5975 0.116 Uiso 1 1 calc R . . C14 C 0.2038(4) 0.2164(5) 0.1711(8) 0.064(3) Uani 1 1 d U . . H14 H 0.1798 0.1844 0.1291 0.077 Uiso 1 1 calc R . . C15 C 0.2310(4) 0.2653(5) 0.1273(6) 0.052(3) Uani 1 1 d DU . . C12 C 0.0618(4) 0.6730(5) 0.5505(10) 0.081(4) Uani 1 1 d U . . H12 H 0.0529 0.6670 0.4802 0.098 Uiso 1 1 calc R . . C2 C 0.1129(4) 0.3931(5) 0.5328(10) 0.080(3) Uani 1 1 d U . . H2 H 0.0765 0.3870 0.5471 0.096 Uiso 1 1 calc R . . C11 C 0.0342(4) 0.7237(5) 0.5905(9) 0.061(3) Uani 1 1 d U . . H11 H 0.0077 0.7521 0.5454 0.073 Uiso 1 1 calc R . . C7 C 0.1345(4) 0.5793(4) 0.5749(9) 0.079(4) Uani 1 1 d DU . . H7A H 0.1459 0.5967 0.5167 0.095 Uiso 1 1 calc R . . H7B H 0.1708 0.5689 0.6279 0.095 Uiso 1 1 calc R . . C16 C 0.2642(4) 0.3130(5) 0.1970(9) 0.062(3) Uani 1 1 d U . . H16 H 0.2824 0.3488 0.1736 0.074 Uiso 1 1 calc R . . C18 C 0.2265(3) 0.2715(5) 0.0157(6) 0.079(3) Uani 1 1 d DU . . H18A H 0.2316 0.3183 -0.0002 0.095 Uiso 1 1 calc R . . H18B H 0.1870 0.2576 -0.0240 0.095 Uiso 1 1 calc R . . C1S C 0.0338(6) 0.9330(7) 0.6214(13) 0.152(6) Uani 1 1 d U . . H1S1 H 0.0693 0.9559 0.6175 0.183 Uiso 1 1 calc R . . H1S2 H 0.0072 0.9645 0.6390 0.183 Uiso 1 1 calc R . . H1S3 H 0.0145 0.9130 0.5565 0.183 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0317(8) 0.0458(10) 0.0212(11) -0.0036(8) 0.0109(7) 0.0029(6) Co2 0.0322(8) 0.0454(10) 0.0372(12) 0.000 0.0092(8) 0.000 S 0.0379(11) 0.0497(15) 0.0436(18) 0.0043(12) 0.0055(12) -0.0018(9) O1 0.033(3) 0.070(4) 0.037(4) -0.007(3) 0.007(3) 0.013(2) O2 0.040(3) 0.067(4) 0.026(4) -0.010(3) 0.015(3) -0.003(2) N1 0.033(3) 0.044(4) 0.043(5) 0.000(3) 0.012(3) 0.002(3) O3 0.073(4) 0.065(4) 0.066(5) -0.027(4) 0.001(4) 0.020(3) N3 0.039(3) 0.052(4) 0.040(5) -0.003(4) 0.010(4) -0.002(3) O1S 0.075(4) 0.072(4) 0.041(4) 0.027(3) 0.005(3) -0.011(3) O4 0.081(4) 0.091(5) 0.091(6) 0.036(5) 0.009(4) -0.022(4) C10 0.048(4) 0.060(5) 0.047(6) 0.000(5) 0.009(4) 0.016(4) C9 0.056(5) 0.063(6) 0.077(7) 0.005(5) 0.010(5) 0.017(4) C3 0.045(5) 0.066(6) 0.098(8) -0.012(5) 0.029(5) 0.007(4) N2 0.042(4) 0.053(4) 0.037(5) -0.004(4) 0.009(4) 0.005(3) C13 0.065(5) 0.076(6) 0.021(6) -0.009(5) 0.010(5) -0.008(4) C8 0.049(5) 0.065(6) 0.076(8) -0.010(5) 0.019(5) 0.015(4) C4 0.072(6) 0.059(6) 0.116(9) -0.007(6) 0.038(6) 0.001(4) C17 0.054(5) 0.070(6) 0.029(6) -0.005(5) 0.012(5) 0.000(4) C1 0.054(5) 0.051(5) 0.080(7) -0.015(5) 0.024(5) -0.002(4) C5 0.055(5) 0.059(6) 0.078(7) -0.001(5) 0.022(5) 0.014(4) C6 0.084(6) 0.089(7) 0.131(9) -0.025(6) 0.055(6) 0.013(5) C14 0.080(6) 0.069(6) 0.037(6) -0.009(5) 0.004(5) -0.012(5) C15 0.060(5) 0.079(6) 0.023(6) 0.001(5) 0.018(5) 0.014(4) C12 0.078(6) 0.085(7) 0.081(8) -0.019(6) 0.022(6) 0.023(5) C2 0.062(5) 0.072(6) 0.118(8) -0.026(6) 0.043(5) 0.003(5) C11 0.057(5) 0.063(6) 0.059(7) 0.000(5) 0.012(5) 0.012(4) C7 0.076(5) 0.086(7) 0.083(8) -0.020(6) 0.035(5) 0.010(5) C16 0.066(5) 0.076(6) 0.052(7) 0.012(5) 0.029(5) 0.005(4) C18 0.091(6) 0.089(7) 0.052(7) 0.004(5) 0.014(6) 0.016(5) C1S 0.133(8) 0.168(9) 0.148(10) 0.028(8) 0.027(7) -0.046(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 Co1 O2 2.068(4) . ? Co1 O2 2.068(4) 7_556 ? Co1 N1 2.168(6) . ? Co1 N1 2.168(6) 7_556 ? Co1 N3 2.175(8) 7_556 ? Co1 N3 2.175(8) . ? Co2 O1 2.083(5) 3_455 ? Co2 O1 2.083(5) 4_556 ? Co2 O1S 2.101(6) 2_556 ? Co2 O1S 2.101(6) . ? Co2 N2 2.148(7) 2_556 ? Co2 N2 2.148(7) . ? S O4 1.441(7) . ? S O2 1.459(5) . ? S O1 1.459(4) . ? S O3 1.491(6) . ? O1 Co2 2.083(5) 3_545 ? N1 C1 1.290(11) . ? N1 C5 1.319(11) . ? N3 C17 1.316(12) . ? N3 C13 1.357(10) . ? O1S C1S 1.358(14) . ? C10 N2 1.296(9) . ? C10 C9 1.351(13) . ? C9 C8 1.376(15) . ? C3 C4 1.343(13) . ? C3 C2 1.380(13) . ? C3 C6 1.509(8) . ? N2 C11 1.330(13) . ? C13 C14 1.324(14) . ? C8 C12 1.332(12) . ? C8 C7 1.500(8) . ? C4 C5 1.395(13) . ? C17 C16 1.377(14) . ? C1 C2 1.381(12) . ? C6 C7 1.479(8) . ? C14 C15 1.386(13) . ? C15 C16 1.411(12) . ? C15 C18 1.502(9) . ? C12 C11 1.388(14) . ? C18 C18 1.543(9) 7 ? 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 O2 Co1 O2 180.0(3) . 7_556 ? O2 Co1 N1 91.0(2) . . ? O2 Co1 N1 89.0(2) 7_556 . ? O2 Co1 N1 89.0(2) . 7_556 ? O2 Co1 N1 91.0(2) 7_556 7_556 ? N1 Co1 N1 180.000(1) . 7_556 ? O2 Co1 N3 90.4(2) . 7_556 ? O2 Co1 N3 89.6(2) 7_556 7_556 ? N1 Co1 N3 87.1(3) . 7_556 ? N1 Co1 N3 92.9(3) 7_556 7_556 ? O2 Co1 N3 89.6(2) . . ? O2 Co1 N3 90.4(2) 7_556 . ? N1 Co1 N3 92.9(3) . . ? N1 Co1 N3 87.1(3) 7_556 . ? N3 Co1 N3 180.0 7_556 . ? O1 Co2 O1 176.6(3) 3_455 4_556 ? O1 Co2 O1S 87.7(2) 3_455 2_556 ? O1 Co2 O1S 90.0(2) 4_556 2_556 ? O1 Co2 O1S 90.0(2) 3_455 . ? O1 Co2 O1S 87.7(2) 4_556 . ? O1S Co2 O1S 93.9(4) 2_556 . ? O1 Co2 N2 92.4(3) 3_455 2_556 ? O1 Co2 N2 90.0(2) 4_556 2_556 ? O1S Co2 N2 89.6(3) 2_556 2_556 ? O1S Co2 N2 175.8(2) . 2_556 ? O1 Co2 N2 90.0(2) 3_455 . ? O1 Co2 N2 92.4(2) 4_556 . ? O1S Co2 N2 175.8(2) 2_556 . ? O1S Co2 N2 89.6(3) . . ? N2 Co2 N2 87.1(4) 2_556 . ? O4 S O2 109.4(3) . . ? O4 S O1 111.5(4) . . ? O2 S O1 109.3(3) . . ? O4 S O3 111.1(4) . . ? O2 S O3 107.7(4) . . ? O1 S O3 107.8(3) . . ? S O1 Co2 141.4(4) . 3_545 ? S O2 Co1 171.5(4) . . ? C1 N1 C5 115.0(7) . . ? C1 N1 Co1 122.3(6) . . ? C5 N1 Co1 122.6(6) . . ? C17 N3 C13 115.9(8) . . ? C17 N3 Co1 123.7(6) . . ? C13 N3 Co1 120.2(6) . . ? C1S O1S Co2 134.4(7) . . ? N2 C10 C9 125.4(10) . . ? C10 C9 C8 118.9(9) . . ? C4 C3 C2 115.7(8) . . ? C4 C3 C6 125.8(9) . . ? C2 C3 C6 118.4(9) . . ? C10 N2 C11 115.5(8) . . ? C10 N2 Co2 122.2(6) . . ? C11 N2 Co2 122.3(5) . . ? C14 C13 N3 123.7(9) . . ? C12 C8 C9 117.5(8) . . ? C12 C8 C7 122.1(10) . . ? C9 C8 C7 120.4(9) . . ? C3 C4 C5 122.6(10) . . ? N3 C17 C16 123.7(9) . . ? N1 C1 C2 127.6(9) . . ? N1 C5 C4 121.6(10) . . ? C7 C6 C3 115.9(8) . . ? C13 C14 C15 122.1(9) . . ? C14 C15 C16 114.4(8) . . ? C14 C15 C18 125.7(9) . . ? C16 C15 C18 119.8(9) . . ? C8 C12 C11 119.6(11) . . ? C1 C2 C3 117.3(10) . . ? N2 C11 C12 123.1(9) . . ? C6 C7 C8 113.7(8) . . ? C17 C16 C15 119.8(9) . . ? C15 C18 C18 112.5(8) . 7 ? _diffrn_measured_fraction_theta_max 0.695 _diffrn_reflns_theta_full 23.08 _diffrn_measured_fraction_theta_full 0.695 _refine_diff_density_max 0.609 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.085 data_5 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 54 _chemical_formula_sum 'C120 H152 N20 Ni6 O40 S6' _chemical_formula_weight 3059.24 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c (14)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.485(3) _cell_length_b 27.235(4) _cell_length_c 26.925(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.240(10) _cell_angle_gamma 90.00 _cell_volume 15755(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 976 _cell_measurement_theta_min 3 _cell_measurement_theta_max 19 _exptl_crystal_description block _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6384 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 3 _diffrn_reflns_number 55661 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.1397 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 21.05 _reflns_number_total 16820 _reflns_number_observed 8930 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1830P)^2^+173.5657P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 16820 _refine_ls_number_parameters 830 _refine_ls_number_restraints 1015 _refine_ls_R_factor_all 0.1647 _refine_ls_R_factor_obs 0.1123 _refine_ls_wR_factor_all 0.3173 _refine_ls_wR_factor_obs 0.2802 _refine_ls_goodness_of_fit_all 0.881 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.00145(11) 1.13153(6) 0.25772(7) 0.0266(5) Uani 1 1 d . . . Ni2 Ni 0.50592(11) 1.26360(7) 0.49167(7) 0.0373(6) Uani 1 1 d . . . Ni3 Ni 0.22755(11) 0.00783(6) 0.99379(7) 0.0345(6) Uani 1 1 d . . . Ni4 Ni 0.24966(12) -0.49429(7) 0.99315(6) 0.0321(6) Uani 1 1 d . . . Ni5 Ni 0.50129(11) 0.85910(6) 0.26212(7) 0.0266(6) Uani 1 1 d . . . Ni6 Ni 0.98708(11) 0.75794(7) -0.00654(8) 0.0403(7) Uani 1 1 d . . . N2 N -0.0003(5) 0.7106(5) 0.2428(5) 0.034(3) Uiso 1 1 d D . . N3 N 0.0966(6) 1.1334(5) 0.2820(5) 0.028(3) Uiso 1 1 d . . . N4 N 0.4555(7) 1.2363(5) 0.4304(5) 0.038(4) Uiso 1 1 d . . . N5 N -0.0935(6) 1.1330(5) 0.2327(5) 0.032(3) Uiso 1 1 d . . . N6 N -0.4445(7) 1.2143(5) 0.0543(5) 0.039(4) Uiso 1 1 d . . . N7 N 0.2245(7) 0.0040(5) 0.9153(5) 0.038(4) Uiso 1 1 d . . . N8 N 0.2500(6) -0.0049(5) 0.5714(4) 0.030(3) Uiso 1 1 d . . . N9 N 0.2493(7) -0.0076(5) 1.4150(4) 0.035(3) Uiso 1 1 d . . . N10 N 0.2305(7) 0.0128(5) 1.0705(5) 0.041(4) Uiso 1 1 d . . . N11 N 0.2364(6) -0.4159(5) 0.9953(5) 0.031(3) Uiso 1 1 d . . . N12 N 0.2297(6) -0.0700(5) 0.9974(5) 0.037(3) Uiso 1 1 d . . . N13 N 0.2666(6) 0.4263(5) 0.9897(4) 0.033(3) Uiso 1 1 d D . . N14 N 0.2321(6) 0.0846(5) 0.9875(5) 0.038(4) Uiso 1 1 d D . . N15 N 1.0394(6) 0.7323(5) -0.0667(5) 0.036(4) Uiso 1 1 d . . . N16 N 0.4102(6) 0.8574(5) 0.2868(5) 0.038(4) Uiso 1 1 d . . . N17 N 0.9336(7) 0.7789(5) 0.0567(5) 0.042(4) Uiso 1 1 d . . . N18 N 0.5946(7) 0.8591(5) 0.2424(5) 0.039(4) Uiso 1 1 d . . . N19 N 0.5041(6) 0.7808(4) 0.2653(5) 0.029(3) Uiso 1 1 d . . . N20 N 0.4958(6) 0.9369(4) 0.2567(4) 0.024(3) Uiso 1 1 d . . . C25 C -0.0139(7) 0.7369(7) 0.2815(7) 0.057(6) Uiso 1 1 d D . . H25 H -0.0214 0.7194 0.3105 0.068 Uiso 1 1 calc R . . C1B C 0.2797(10) 1.1479(9) 0.3398(9) 0.105(9) Uiso 1 1 d D . . H1B1 H 0.2721 1.1568 0.3742 0.126 Uiso 1 1 calc R . . H1B2 H 0.2990 1.1157 0.3401 0.126 Uiso 1 1 calc R . . C2B C 0.3244(8) 1.1817(7) 0.3209(8) 0.066(6) Uiso 1 1 d D . . H2B1 H 0.3023 1.2097 0.3072 0.079 Uiso 1 1 calc R . . H2B2 H 0.3462 1.1659 0.2937 0.079 Uiso 1 1 calc R . . C1C C -0.2621(11) 1.1490(12) 0.1583(11) 0.156(14) Uiso 1 1 d D . . H1C1 H -0.2739 1.1162 0.1479 0.188 Uiso 1 1 calc R . . H1C2 H -0.2509 1.1667 0.1284 0.188 Uiso 1 1 calc R . . C2C C -0.3172(9) 1.1716(11) 0.1766(10) 0.114(10) Uiso 1 1 d D . . H2C1 H -0.3059 1.2011 0.1949 0.137 Uiso 1 1 calc R . . H2C2 H -0.3375 1.1494 0.1995 0.137 Uiso 1 1 calc R . . C1D C 0.2092(14) -0.0056(13) 0.7588(9) 0.164(15) Uiso 1 1 d D . . H1D1 H 0.2010 -0.0400 0.7521 0.197 Uiso 1 1 calc R . . H1D2 H 0.1723 0.0129 0.7496 0.197 Uiso 1 1 calc R . . C2D C 0.2600(11) 0.0102(10) 0.7290(7) 0.095(8) Uiso 1 1 d D . . H2D1 H 0.2976 -0.0057 0.7409 0.113 Uiso 1 1 calc R . . H2D2 H 0.2653 0.0453 0.7334 0.113 Uiso 1 1 calc R . . C1E C 0.2313(10) 0.0241(6) 1.2314(6) 0.065(6) Uiso 1 1 d D . . H1E1 H 0.2595 0.0499 1.2417 0.078 Uiso 1 1 calc R . . H1E2 H 0.1900 0.0328 1.2427 0.078 Uiso 1 1 calc R . . C2E C 0.2498(11) -0.0209(7) 1.2545(6) 0.075(7) Uiso 1 1 d D . . H2E1 H 0.2907 -0.0301 1.2428 0.091 Uiso 1 1 calc R . . H2E2 H 0.2209 -0.0466 1.2452 0.091 Uiso 1 1 calc R . . C1F C 0.2134(8) -0.2585(5) 1.0056(7) 0.053(5) Uiso 1 1 d D . . H1F1 H 0.1716 -0.2502 0.9946 0.063 Uiso 1 1 calc R . . H1F2 H 0.2161 -0.2512 1.0408 0.063 Uiso 1 1 calc R . . C2F C 0.2569(11) -0.2276(6) 0.9796(10) 0.102(9) Uiso 1 1 d D . . H2F1 H 0.2534 -0.2341 0.9443 0.123 Uiso 1 1 calc R . . H2F2 H 0.2988 -0.2362 0.9899 0.123 Uiso 1 1 calc R . . C1G C 0.2901(9) 0.2715(6) 0.9868(7) 0.076(7) Uiso 1 1 d D . . H1G1 H 0.3126 0.2645 0.9565 0.092 Uiso 1 1 calc R . . H1G2 H 0.3179 0.2639 1.0142 0.092 Uiso 1 1 calc R . . C2G C 0.2394(14) 0.2380(10) 0.9893(14) 0.29(3) Uiso 1 1 d D . . H2G1 H 0.2202 0.2428 1.0215 0.350 Uiso 1 1 calc R . . H2G2 H 0.2093 0.2487 0.9647 0.350 Uiso 1 1 calc R . . C1H C 0.1771(7) 0.8170(8) 0.3277(7) 0.065(6) Uiso 1 1 d D . . H1H1 H 0.1877 0.7899 0.3060 0.078 Uiso 1 1 calc R . . H1H2 H 0.1616 0.8436 0.3071 0.078 Uiso 1 1 calc R . . C2H C 0.2320(6) 0.8331(6) 0.3532(6) 0.046(5) Uiso 1 1 d D . . H2H1 H 0.2429 0.8079 0.3772 0.055 Uiso 1 1 calc R . . H2H2 H 0.2211 0.8623 0.3718 0.055 Uiso 1 1 calc R . . C1I C 0.8034(11) 0.8061(8) 0.1761(10) 0.108(9) Uiso 1 1 d D . . H1I1 H 0.7675 0.7872 0.1653 0.129 Uiso 1 1 calc R . . H1I2 H 0.8179 0.7929 0.2076 0.129 Uiso 1 1 calc R . . C2I C 0.7868(13) 0.8567(8) 0.1817(11) 0.126(11) Uiso 1 1 d D . . H2I1 H 0.7859 0.8731 0.1497 0.151 Uiso 1 1 calc R . . H2I2 H 0.8164 0.8735 0.2031 0.151 Uiso 1 1 calc R . . C1L C 0.4893(10) 0.6236(7) 0.2688(8) 0.071(6) Uiso 1 1 d D . . H1L1 H 0.4949 0.6120 0.3027 0.086 Uiso 1 1 calc R . . H1L2 H 0.4466 0.6169 0.2592 0.086 Uiso 1 1 calc R . . C2L C 0.5300(10) 0.5962(6) 0.2370(8) 0.073(7) Uiso 1 1 d D . . H2L1 H 0.5725 0.6042 0.2460 0.087 Uiso 1 1 calc R . . H2L2 H 0.5233 0.6073 0.2032 0.087 Uiso 1 1 calc R . . C11B C -0.0357(8) 1.0261(7) 0.2840(6) 0.049(5) Uiso 1 1 d D . . H11B H -0.0637 1.0419 0.3049 0.059 Uiso 1 1 calc R . . N1 N -0.0009(7) 1.0542(5) 0.2550(5) 0.036(4) Uiso 1 1 d D . . C11 C 0.2813(9) -0.3851(6) 0.9863(6) 0.040(5) Uiso 1 1 d . . . H11 H 0.3200 -0.3984 0.9788 0.048 Uiso 1 1 calc R . . C12 C -0.0340(9) 0.9774(8) 0.2858(8) 0.071(7) Uiso 1 1 d D . . H12 H -0.0560 0.9608 0.3102 0.086 Uiso 1 1 calc R . . C13 C -0.0017(14) 0.9529(9) 0.2532(10) 0.099(9) Uiso 1 1 d D . . C14 C 0.0362(17) 0.9787(15) 0.2214(14) 0.157(14) Uiso 1 1 d D . . H14 H 0.0632 0.9638 0.1990 0.188 Uiso 1 1 calc R . . C15 C 0.0300(13) 1.0280(11) 0.2261(10) 0.102(9) Uiso 1 1 d D . . H15 H 0.0532 1.0458 0.2033 0.122 Uiso 1 1 calc R . . C1A C 0.0193(18) 0.8932(10) 0.2686(12) 0.179(17) Uiso 1 1 d D . . H1A1 H 0.0642 0.8892 0.2685 0.215 Uiso 1 1 calc R . . H1A2 H 0.0033 0.8840 0.3009 0.215 Uiso 1 1 calc R . . C2A C -0.0091(12) 0.8651(9) 0.2299(12) 0.163(14) Uiso 1 1 d D . . H2A1 H 0.0132 0.8700 0.1991 0.196 Uiso 1 1 calc R . . H2A2 H -0.0518 0.8759 0.2251 0.196 Uiso 1 1 calc R . . C21 C 0.0109(7) 0.7357(8) 0.2011(8) 0.065(6) Uiso 1 1 d D . . H21 H 0.0212 0.7189 0.1722 0.078 Uiso 1 1 calc R . . C22 C 0.0074(8) 0.7871(9) 0.2004(9) 0.084(7) Uiso 1 1 d D . . H22 H 0.0150 0.8055 0.1720 0.101 Uiso 1 1 calc R . . C23 C -0.0082(8) 0.8079(10) 0.2446(12) 0.128(11) Uiso 1 1 d D . . C24 C -0.0188(8) 0.7886(9) 0.2856(9) 0.077(7) Uiso 1 1 d D . . H24 H -0.0285 0.8055 0.3146 0.092 Uiso 1 1 calc R . . C31 C 0.1162(8) 1.1082(6) 0.3192(6) 0.031(4) Uiso 1 1 d . . . H31 H 0.0881 1.0870 0.3342 0.037 Uiso 1 1 calc R . . C32 C 0.1726(8) 1.1102(6) 0.3376(6) 0.034(4) Uiso 1 1 d . . . H32 H 0.1830 1.0906 0.3647 0.040 Uiso 1 1 calc R . . C33 C 0.2198(7) 1.1428(6) 0.3160(7) 0.045(5) Uiso 1 1 d D . . C34 C 0.1987(9) 1.1648(7) 0.2764(7) 0.050(5) Uiso 1 1 d . . . H34 H 0.2268 1.1840 0.2587 0.060 Uiso 1 1 calc R . . C35 C 0.1373(8) 1.1622(6) 0.2579(7) 0.039(5) Uiso 1 1 d . . . H35 H 0.1254 1.1799 0.2299 0.047 Uiso 1 1 calc R . . C41 C 0.4495(8) 1.1874(6) 0.4241(6) 0.038(5) Uiso 1 1 d . . . H41 H 0.4734 1.1657 0.4429 0.046 Uiso 1 1 calc R . . C42 C 0.4057(9) 1.1693(7) 0.3879(7) 0.052(5) Uiso 1 1 d . . . H42 H 0.3999 1.1356 0.3850 0.063 Uiso 1 1 calc R . . C43 C 0.3719(7) 1.2004(6) 0.3572(6) 0.038(5) Uiso 1 1 d D . . C44 C 0.3847(9) 1.2484(8) 0.3628(8) 0.060(6) Uiso 1 1 d . . . H44 H 0.3650 1.2710 0.3422 0.072 Uiso 1 1 calc R . . C45 C 0.4265(9) 1.2653(8) 0.3986(7) 0.055(6) Uiso 1 1 d . . . H45 H 0.4345 1.2988 0.4002 0.067 Uiso 1 1 calc R . . C51 C -0.1101(9) 1.1079(6) 0.1919(6) 0.040(5) Uiso 1 1 d . . . H51 H -0.0825 1.0847 0.1794 0.048 Uiso 1 1 calc R . . C52 C -0.1627(10) 1.1142(8) 0.1693(8) 0.067(6) Uiso 1 1 d . . . H52 H -0.1698 1.0972 0.1398 0.080 Uiso 1 1 calc R . . C53 C -0.2073(8) 1.1439(7) 0.1860(8) 0.058(6) Uiso 1 1 d D . . C54 C -0.1954(10) 1.1689(8) 0.2297(8) 0.065(6) Uiso 1 1 d . . . H54 H -0.2249 1.1897 0.2437 0.078 Uiso 1 1 calc R . . C55 C -0.1353(8) 1.1614(6) 0.2527(7) 0.042(5) Uiso 1 1 d . . . H55 H -0.1262 1.1772 0.2825 0.050 Uiso 1 1 calc R . . C61 C -0.4369(9) 1.1654(7) 0.0658(7) 0.048(5) Uiso 1 1 d . . . H61 H -0.4607 1.1420 0.0493 0.058 Uiso 1 1 calc R . . C62 C -0.3943(9) 1.1505(8) 0.1017(7) 0.059(6) Uiso 1 1 d . . . H62 H -0.3853 1.1172 0.1051 0.071 Uiso 1 1 calc R . . C63 C -0.3638(9) 1.1855(8) 0.1339(8) 0.063(6) Uiso 1 1 d D . . C64 C -0.3743(10) 1.2344(8) 0.1252(8) 0.067(6) Uiso 1 1 d . . . H64 H -0.3556 1.2585 0.1447 0.081 Uiso 1 1 calc R . . C65 C -0.4163(8) 1.2474(7) 0.0839(6) 0.043(5) Uiso 1 1 d . . . H65 H -0.4238 1.2805 0.0778 0.051 Uiso 1 1 calc R . . C71 C 0.1735(9) 0.0192(6) 0.8927(7) 0.045(5) Uiso 1 1 d . . . H71 H 0.1385 0.0296 0.9100 0.054 Uiso 1 1 calc R . . C72 C 0.1755(12) 0.0184(9) 0.8394(9) 0.089(8) Uiso 1 1 d . . . H72 H 0.1419 0.0311 0.8218 0.107 Uiso 1 1 calc R . . C73 C 0.2215(13) 0.0010(10) 0.8153(7) 0.091(8) Uiso 1 1 d D . . C74 C 0.2735(14) -0.0147(10) 0.8379(10) 0.104(9) Uiso 1 1 d . . . H74 H 0.3070 -0.0263 0.8196 0.125 Uiso 1 1 calc R . . C75 C 0.2760(10) -0.0132(7) 0.8910(7) 0.058(6) Uiso 1 1 d . . . H75 H 0.3112 -0.0235 0.9083 0.070 Uiso 1 1 calc R . . C81 C 0.2806(8) -0.0396(7) 0.5975(6) 0.043(5) Uiso 1 1 d . . . H81 H 0.2994 -0.0656 0.5809 0.051 Uiso 1 1 calc R . . C82 C 0.2841(9) -0.0370(7) 0.6469(7) 0.051(5) Uiso 1 1 d . . . H82 H 0.3077 -0.0601 0.6641 0.061 Uiso 1 1 calc R . . C83 C 0.2531(12) -0.0004(9) 0.6739(7) 0.080(7) Uiso 1 1 d D . . C84 C 0.2222(9) 0.0330(7) 0.6476(7) 0.053(5) Uiso 1 1 d . . . H84 H 0.1998 0.0574 0.6639 0.064 Uiso 1 1 calc R . . C85 C 0.2231(8) 0.0320(6) 0.5946(6) 0.041(5) Uiso 1 1 d . . . H85 H 0.2047 0.0572 0.5765 0.049 Uiso 1 1 calc R . . C91 C 0.2958(8) 0.0099(6) 1.3900(6) 0.041(5) Uiso 1 1 d . . . H91 H 0.3274 0.0264 1.4068 0.050 Uiso 1 1 calc R . . C92 C 0.2995(10) 0.0049(7) 1.3396(7) 0.057(6) Uiso 1 1 d . . . H92 H 0.3349 0.0158 1.3231 0.068 Uiso 1 1 calc R . . C93 C 0.2514(9) -0.0162(6) 1.3126(5) 0.049(5) Uiso 1 1 d D . . C94 C 0.1975(9) -0.0302(7) 1.3375(7) 0.052(5) Uiso 1 1 d . . . H94 H 0.1623 -0.0415 1.3210 0.063 Uiso 1 1 calc R . . C95 C 0.2002(8) -0.0257(6) 1.3905(6) 0.038(5) Uiso 1 1 d . . . H95 H 0.1660 -0.0360 1.4088 0.046 Uiso 1 1 calc R . . C101 C 0.2696(9) 0.0410(7) 1.0951(7) 0.050(5) Uiso 1 1 d . . . H101 H 0.2971 0.0593 1.0760 0.060 Uiso 1 1 calc R . . C102 C 0.2746(11) 0.0465(8) 1.1449(8) 0.076(7) Uiso 1 1 d . . . H102 H 0.3054 0.0660 1.1591 0.091 Uiso 1 1 calc R . . C103 C 0.2309(10) 0.0212(7) 1.1741(6) 0.057(6) Uiso 1 1 d D . . C104 C 0.1899(9) -0.0127(7) 1.1500(7) 0.057(6) Uiso 1 1 d . . . H104 H 0.1623 -0.0317 1.1683 0.068 Uiso 1 1 calc R . . C105 C 0.1922(9) -0.0167(7) 1.0984(7) 0.048(5) Uiso 1 1 d . . . H105 H 0.1673 -0.0398 1.0825 0.058 Uiso 1 1 calc R . . C112 C 0.2770(9) -0.3341(6) 0.9869(6) 0.045(5) Uiso 1 1 d . . . H112 H 0.3116 -0.3150 0.9793 0.054 Uiso 1 1 calc R . . C113 C 0.2230(8) -0.3126(5) 0.9985(6) 0.039(4) Uiso 1 1 d D . . C114 C 0.1733(9) -0.3439(6) 1.0072(6) 0.042(5) Uiso 1 1 d . . . H114 H 0.1341 -0.3314 1.0145 0.051 Uiso 1 1 calc R . . C115 C 0.1833(10) -0.3953(7) 1.0049(7) 0.055(5) Uiso 1 1 d . . . H115 H 0.1494 -0.4157 1.0107 0.065 Uiso 1 1 calc R . . C121 C 0.2775(9) -0.0933(7) 1.0160(7) 0.053(5) Uiso 1 1 d . . . H121 H 0.3064 -0.0742 1.0331 0.064 Uiso 1 1 calc R . . C122 C 0.2904(12) -0.1433(9) 1.0134(9) 0.091(8) Uiso 1 1 d . . . H122 H 0.3263 -0.1565 1.0274 0.110 Uiso 1 1 calc R . . C123 C 0.2468(9) -0.1729(5) 0.9886(7) 0.055(5) Uiso 1 1 d D . . C124 C 0.1944(9) -0.1478(7) 0.9665(7) 0.054(6) Uiso 1 1 d . . . H124 H 0.1648 -0.1653 0.9484 0.065 Uiso 1 1 calc R . . C125 C 0.1888(9) -0.0984(6) 0.9724(6) 0.043(5) Uiso 1 1 d . . . H125 H 0.1543 -0.0831 0.9582 0.051 Uiso 1 1 calc R . . C131 C 0.2227(10) 0.3482(8) 0.9733(6) 0.064(6) Uiso 1 1 d D . . H131 H 0.1892 0.3292 0.9626 0.076 Uiso 1 1 calc R . . C13O C 0.2159(10) 0.3988(7) 0.9743(6) 0.061(6) Uiso 1 1 d D . . H13O H 0.1788 0.4138 0.9649 0.073 Uiso 1 1 calc R . . C133 C 0.2787(10) 0.3240(7) 0.9879(6) 0.067(6) Uiso 1 1 d D . . C134 C 0.3273(9) 0.3544(7) 1.0018(6) 0.054(5) Uiso 1 1 d D . . H134 H 0.3656 0.3413 1.0109 0.064 Uiso 1 1 calc R . . C135 C 0.3183(8) 0.4035(6) 1.0018(5) 0.040(5) Uiso 1 1 d D . . H135 H 0.3519 0.4230 1.0113 0.048 Uiso 1 1 calc R . . C141 C 0.2738(9) 0.1082(7) 0.9605(6) 0.057(6) Uiso 1 1 d D . . H141 H 0.3009 0.0888 0.9420 0.068 Uiso 1 1 calc R . . C142 C 0.2811(10) 0.1550(8) 0.9569(7) 0.067(6) Uiso 1 1 d D . . H142 H 0.3115 0.1671 0.9357 0.080 Uiso 1 1 calc R . . C143 C 0.2458(10) 0.1873(6) 0.9832(8) 0.076(7) Uiso 1 1 d D . . C144 C 0.1998(10) 0.1650(8) 1.0135(8) 0.073(7) Uiso 1 1 d D . . H144 H 0.1739 0.1841 1.0332 0.087 Uiso 1 1 calc R . . C145 C 0.1944(8) 0.1148(7) 1.0133(6) 0.048(5) Uiso 1 1 d D . . H145 H 0.1628 0.1007 1.0320 0.057 Uiso 1 1 calc R . . C151 C 1.0719(8) 0.7645(6) -0.0971(6) 0.036(5) Uiso 1 1 d . . . H151 H 1.0651 0.7981 -0.0939 0.044 Uiso 1 1 calc R . . C152 C 0.1129(8) 0.7514(6) 0.3690(7) 0.041(5) Uiso 1 1 d . . . H152 H 0.1335 0.7288 0.3491 0.049 Uiso 1 1 calc R . . C153 C 0.1250(6) 0.8005(6) 0.3633(7) 0.041(5) Uiso 1 1 d D . . C154 C 0.0932(9) 0.8310(7) 0.3916(7) 0.054(6) Uiso 1 1 d . . . H154 H 0.0996 0.8645 0.3879 0.065 Uiso 1 1 calc R . . C155 C 0.0516(9) 0.8153(7) 0.4259(7) 0.044(5) Uiso 1 1 d . . . H155 H 0.0307 0.8385 0.4450 0.053 Uiso 1 1 calc R . . C161 C 0.3893(8) 0.8833(6) 0.3254(6) 0.032(4) Uiso 1 1 d . . . H161 H 0.4154 0.9066 0.3396 0.039 Uiso 1 1 calc R . . C162 C 0.3327(9) 0.8773(7) 0.3444(7) 0.051(5) Uiso 1 1 d . . . H162 H 0.3220 0.8961 0.3720 0.061 Uiso 1 1 calc R . . C163 C 0.2875(7) 0.8442(7) 0.3252(7) 0.048(5) Uiso 1 1 d D . . C164 C 0.3074(8) 0.8210(6) 0.2821(6) 0.040(5) Uiso 1 1 d . . . H164 H 0.2802 0.8008 0.2645 0.049 Uiso 1 1 calc R . . C165 C 0.3653(8) 0.8277(6) 0.2659(6) 0.034(4) Uiso 1 1 d . . . H165 H 0.3766 0.8104 0.2375 0.041 Uiso 1 1 calc R . . C171 C 0.9219(9) 0.8251(8) 0.0663(8) 0.059(6) Uiso 1 1 d . . . H171 H 0.9388 0.8494 0.0462 0.070 Uiso 1 1 calc R . . C172 C 0.8829(11) 0.8388(9) 0.1079(8) 0.076(7) Uiso 1 1 d . . . H172 H 0.8752 0.8715 0.1154 0.091 Uiso 1 1 calc R . . C173 C 0.8587(10) 0.8028(8) 0.1346(8) 0.076(7) Uiso 1 1 d D . . C174 C 0.8729(10) 0.7546(9) 0.1239(9) 0.075(7) Uiso 1 1 d . . . H174 H 0.8573 0.7292 0.1433 0.090 Uiso 1 1 calc R . . C175 C 0.9097(9) 0.7453(8) 0.0851(7) 0.056(6) Uiso 1 1 d . . . H175 H 0.9188 0.7127 0.0779 0.067 Uiso 1 1 calc R . . C181 C 0.6140(9) 0.8865(6) 0.2013(7) 0.044(5) Uiso 1 1 d . . . H181 H 0.5850 0.9061 0.1849 0.053 Uiso 1 1 calc R . . C182 C 0.6744(10) 0.8856(8) 0.1840(8) 0.063(6) Uiso 1 1 d . . . H182 H 0.6863 0.9047 0.1571 0.076 Uiso 1 1 calc R . . C183 C 0.7155(9) 0.8562(8) 0.2074(8) 0.072(7) Uiso 1 1 d D . . C184 C 0.6981(12) 0.8254(9) 0.2481(9) 0.086(8) Uiso 1 1 d . . . H184 H 0.7257 0.8034 0.2627 0.103 Uiso 1 1 calc R . . C185 C 0.6373(9) 0.8306(7) 0.2641(7) 0.046(5) Uiso 1 1 d . . . H185 H 0.6253 0.8129 0.2921 0.055 Uiso 1 1 calc R . . C191 C 0.5121(9) 0.7553(7) 0.3068(7) 0.049(5) Uiso 1 1 d . . . H191 H 0.5174 0.7732 0.3359 0.059 Uiso 1 1 calc R . . C192 C 0.5133(10) 0.7059(7) 0.3108(8) 0.062(6) Uiso 1 1 d . . . H192 H 0.5228 0.6905 0.3408 0.074 Uiso 1 1 calc R . . C193 C 0.4997(9) 0.6788(6) 0.2679(7) 0.054(5) Uiso 1 1 d D . . C194 C 0.4908(9) 0.7036(7) 0.2243(7) 0.049(5) Uiso 1 1 d . . . H194 H 0.4838 0.6862 0.1952 0.058 Uiso 1 1 calc R . . C195 C 0.4922(8) 0.7524(6) 0.2232(7) 0.042(5) Uiso 1 1 d . . . H195 H 0.4850 0.7682 0.1931 0.051 Uiso 1 1 calc R . . C201 C 0.5360(9) 0.9658(7) 0.2823(7) 0.052(5) Uiso 1 1 d . . . H201 H 0.5694 0.9509 0.2985 0.062 Uiso 1 1 calc R . . C202 C 0.5301(11) 1.0179(9) 0.2859(9) 0.078(7) Uiso 1 1 d . . . H202 H 0.5593 1.0368 0.3029 0.094 Uiso 1 1 calc R . . C203 C 0.4770(9) 1.0395(7) 0.2621(7) 0.054(6) Uiso 1 1 d . . . C204 C 0.4391(10) 1.0082(7) 0.2345(7) 0.057(6) Uiso 1 1 d . . . H204 H 0.4062 1.0215 0.2165 0.069 Uiso 1 1 calc R . . C205 C 0.4483(9) 0.9593(7) 0.2329(7) 0.049(5) Uiso 1 1 d . . . H205 H 0.4207 0.9402 0.2145 0.059 Uiso 1 1 calc R . . O11L O 0.0315(5) 1.1330(4) 0.1840(4) 0.047(3) Uiso 1 1 d . . . O12L O -0.0288(5) 1.1323(4) 0.3315(4) 0.030(3) Uiso 1 1 d . . . O21L O 0.4335(5) 1.3148(4) 0.5037(5) 0.052(3) Uiso 1 1 d . . . O22L O 0.4574(5) 1.2125(4) 0.5369(4) 0.033(3) Uiso 1 1 d . . . O23L O 0.5512(6) 1.3152(4) 0.4481(5) 0.052(3) Uiso 1 1 d . . . O24L O 0.5797(5) 1.2142(4) 0.4772(4) 0.044(3) Uiso 1 1 d . . . O31L O 0.3252(5) 0.0085(4) 0.9950(5) 0.052(3) Uiso 1 1 d . . . O32L O 0.1279(5) 0.0092(4) 0.9961(4) 0.043(3) Uiso 1 1 d . . . O41L O 0.3441(5) -0.4849(4) 0.9960(4) 0.034(3) Uiso 1 1 d . . . O42L O 0.1542(5) -0.5039(4) 0.9955(4) 0.044(3) Uiso 1 1 d . . . O51L O 0.5318(5) 0.8629(4) 0.3370(4) 0.031(3) Uiso 1 1 d . . . O52L O 0.4725(5) 0.8574(4) 0.1870(4) 0.038(3) Uiso 1 1 d . . . O61L O 1.0360(5) 0.7100(4) 0.0398(4) 0.037(3) Uiso 1 1 d . . . O62L O 0.9181(6) 0.7077(5) -0.0225(5) 0.060(4) Uiso 1 1 d . . . O63L O 0.9407(5) 0.8056(4) -0.0533(4) 0.039(3) Uiso 1 1 d . . . O64L O 1.0535(5) 0.8131(4) 0.0095(4) 0.045(3) Uiso 1 1 d . . . O11 O 0.3404(7) 0.7585(5) 0.6861(4) 0.099(5) Uiso 1 1 d D . . O12 O 0.2779(7) 0.7097(7) 0.6322(8) 0.216(13) Uiso 1 1 d D . . O13 O 0.3872(7) 0.6975(5) 0.6339(6) 0.106(6) Uiso 1 1 d D . . O14 O 0.3447(9) 0.7704(6) 0.5980(5) 0.138(8) Uiso 1 1 d D . . O21 O 0.4259(5) 0.9387(3) 0.4370(4) 0.046(3) Uiso 1 1 d D . . O22 O 0.4791(5) 0.8623(3) 0.4278(4) 0.048(3) Uiso 1 1 d D . . O23 O 0.5233(5) 0.9267(4) 0.4786(4) 0.058(4) Uiso 1 1 d D . . O24 O 0.4327(5) 0.8833(4) 0.5054(3) 0.053(3) Uiso 1 1 d D . . O31 O 0.9837(6) 0.0915(5) 0.0083(4) 0.098(5) Uiso 1 1 d D . . O32 O 1.0584(4) 0.0578(4) 0.0655(5) 0.070(4) Uiso 1 1 d D . . O33 O 0.9851(5) 0.1186(4) 0.0925(4) 0.053(3) Uiso 1 1 d D . . O34 O 0.9508(5) 0.0376(4) 0.0720(5) 0.076(4) Uiso 1 1 d D . . O41 O 0.0268(5) 0.1322(3) 0.4234(4) 0.047(3) Uiso 1 1 d D . . O42 O -0.0202(5) 0.0714(5) 0.4749(5) 0.082(5) Uiso 1 1 d D . . O43 O 0.0727(5) 0.1122(4) 0.5022(4) 0.056(4) Uiso 1 1 d D . . O44 O 0.0759(5) 0.0542(4) 0.4345(4) 0.051(3) Uiso 1 1 d D . . O51 O 0.4932(14) 0.4275(12) 0.3785(8) 0.304(19) Uiso 1 1 d D . . O52 O 0.5033(13) 0.4236(12) 0.4664(9) 0.35(2) Uiso 1 1 d D . . O53 O 0.4164(11) 0.4649(8) 0.4294(10) 0.213(13) Uiso 1 1 d D . . O54 O 0.4237(13) 0.3774(8) 0.4255(13) 0.32(2) Uiso 1 1 d D . . O61 O 0.8201(9) 0.7342(7) 0.8139(5) 0.130(7) Uiso 1 1 d D . . O62 O 0.8710(9) 0.7925(8) 0.8664(9) 0.193(11) Uiso 1 1 d D . . O63 O 0.8300(13) 0.7200(8) 0.9020(7) 0.232(14) Uiso 1 1 d D . . O64 O 0.7609(9) 0.7819(11) 0.8712(12) 0.37(3) Uiso 1 1 d D . . S1 S 0.3393(3) 0.7349(2) 0.63827(19) 0.076(2) Uani 1 1 d D . . S2 S 0.4657(2) 0.90286(15) 0.46245(15) 0.0379(12) Uani 1 1 d D . . S3 S 0.9955(3) 0.07596(15) 0.05988(14) 0.0423(13) Uani 1 1 d D . . S4 S 0.0381(3) 0.09197(15) 0.45882(17) 0.0461(14) Uani 1 1 d D . . S5 S 0.4582(3) 0.42326(19) 0.4258(2) 0.0734(19) Uani 1 1 d D . . S6 S 0.8199(5) 0.7565(3) 0.8626(3) 0.134(4) Uani 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 Ni1 0.0463(14) 0.0091(10) 0.0245(11) -0.0003(8) -0.0042(11) -0.0023(11) Ni2 0.0577(16) 0.0279(12) 0.0261(12) 0.0011(10) -0.0098(12) -0.0094(12) Ni3 0.0857(18) 0.0081(10) 0.0095(10) -0.0009(9) -0.0032(11) -0.0047(11) Ni4 0.0834(17) 0.0078(10) 0.0050(9) -0.0013(8) 0.0005(12) -0.0026(10) Ni5 0.0512(15) 0.0103(10) 0.0185(11) -0.0023(8) 0.0051(11) -0.0048(11) Ni6 0.0587(17) 0.0197(11) 0.0427(14) -0.0031(10) 0.0157(13) 0.0012(11) S1 0.135(6) 0.059(4) 0.035(3) 0.018(3) 0.012(3) 0.008(4) S2 0.064(4) 0.024(2) 0.026(2) -0.005(2) 0.004(2) -0.005(2) S3 0.079(4) 0.026(2) 0.022(2) -0.0104(19) -0.003(3) -0.008(3) S4 0.081(4) 0.024(2) 0.034(3) 0.010(2) 0.015(3) 0.006(3) S5 0.135(6) 0.038(3) 0.048(3) -0.015(3) 0.009(4) -0.003(4) S6 0.229(11) 0.059(4) 0.114(7) 0.009(5) 0.016(7) -0.044(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 Ni1 O11L 2.089(12) . ? Ni1 O12L 2.094(10) . ? Ni1 N1 2.108(13) . ? Ni1 N3 2.145(13) . ? Ni1 N5 2.147(13) . ? Ni1 N2 2.154(13) 2 ? Ni2 O23L 2.074(12) . ? Ni2 N6 2.079(14) 4_686 ? Ni2 N4 2.105(14) . ? Ni2 O24L 2.116(12) . ? Ni2 O21L 2.116(12) . ? Ni2 O22L 2.125(10) . ? Ni3 N10 2.071(13) . ? Ni3 O31L 2.099(12) . ? Ni3 N14 2.101(13) . ? Ni3 N7 2.116(13) . ? Ni3 N12 2.123(13) . ? Ni3 O32L 2.141(11) . ? Ni4 O41L 2.047(11) . ? Ni4 O42L 2.069(11) . ? Ni4 N9 2.104(12) 4 ? Ni4 N8 2.108(11) 4_556 ? Ni4 N11 2.156(13) . ? Ni4 N13 2.195(13) 1_545 ? Ni5 N16 2.070(14) . ? Ni5 N18 2.077(14) . ? Ni5 O52L 2.114(11) . ? Ni5 O51L 2.121(10) . ? Ni5 N20 2.127(12) . ? Ni5 N19 2.134(12) . ? Ni6 O62L 2.060(13) . ? Ni6 O63L 2.063(11) . ? Ni6 O61L 2.087(11) . ? Ni6 N15 2.096(13) . ? Ni6 O64L 2.115(12) . ? Ni6 N17 2.136(14) . ? N2 C25 1.30(2) . ? N2 C21 1.34(2) . ? N2 Ni1 2.154(13) 2_545 ? N3 C31 1.283(19) . ? N3 C35 1.34(2) . ? N4 C45 1.32(2) . ? N4 C41 1.35(2) . ? N5 C55 1.30(2) . ? N5 C51 1.34(2) . ? N6 C65 1.35(2) . ? N6 C61 1.38(2) . ? N6 Ni2 2.079(14) 4_485 ? N7 C71 1.32(2) . ? N7 C75 1.37(2) . ? N8 C85 1.32(2) . ? N8 C81 1.35(2) . ? N8 Ni4 2.108(11) 4 ? N9 C91 1.30(2) . ? N9 C95 1.34(2) . ? N9 Ni4 2.104(12) 4_556 ? N10 C101 1.32(2) . ? N10 C105 1.38(2) . ? N11 C115 1.30(2) . ? N11 C11 1.303(19) . ? N12 C121 1.31(2) . ? N12 C125 1.35(2) . ? N13 C135 1.31(2) . ? N13 C13O 1.38(2) . ? N13 Ni4 2.195(13) 1_565 ? N14 C141 1.32(2) . ? N14 C145 1.35(2) . ? N15 C155 1.34(2) 4_675 ? N15 C151 1.39(2) . ? N16 C161 1.33(2) . ? N16 C165 1.38(2) . ? N17 C175 1.30(2) . ? N17 C171 1.31(2) . ? N18 C185 1.34(2) . ? N18 C181 1.40(2) . ? N19 C191 1.33(2) . ? N19 C195 1.40(2) . ? N20 C205 1.35(2) . ? N20 C201 1.36(2) . ? C25 C24 1.42(3) . ? C1B C2B 1.426(12) . ? C1B C33 1.44(2) . ? C2B C43 1.50(2) . ? C1C C53 1.40(3) . ? C1C C2C 1.424(12) . ? C2C C63 1.57(3) . ? C1D C2D 1.424(12) . ? C1D C73 1.55(3) . ? C2D C83 1.52(3) . ? C1E C2E 1.429(12) . ? C1E C103 1.55(2) . ? C2E C93 1.57(2) . ? C1F C2F 1.440(12) . ? C1F C113 1.50(2) . ? C2F C123 1.53(2) . ? C1G C2G 1.422(12) . ? C1G C133 1.45(2) . ? C2G C143 1.40(3) . ? C1H C2H 1.431(12) . ? C1H C153 1.54(2) . ? C2H C163 1.445(18) . ? C1I C2I 1.432(12) . ? C1I C173 1.64(3) . ? C2I C183 1.69(3) . ? C1L C2L 1.434(12) . ? C1L C193 1.52(2) . ? C2L C203 1.55(3) 2_645 ? C11B C12 1.33(3) . ? C11B N1 1.33(2) . ? N1 C15 1.25(3) . ? C11 C112 1.39(2) . ? C12 C13 1.30(3) . ? C13 C14 1.38(4) . ? C13 C1A 1.74(4) . ? C14 C15 1.35(4) . ? C1A C2A 1.426(12) . ? C2A C23 1.61(4) . ? C21 C22 1.40(3) . ? C22 C23 1.36(3) . ? C23 C24 1.25(3) . ? C31 C32 1.31(2) . ? C32 C33 1.47(2) . ? C33 C34 1.30(2) . ? C34 C35 1.41(2) . ? C41 C42 1.44(2) . ? C42 C43 1.39(2) . ? C43 C44 1.34(2) . ? C44 C45 1.39(3) . ? C51 C52 1.29(2) . ? C52 C53 1.33(2) . ? C53 C54 1.38(3) . ? C54 C55 1.44(3) . ? C61 C62 1.39(3) . ? C62 C63 1.45(3) . ? C63 C64 1.37(3) . ? C64 C65 1.47(3) . ? C71 C72 1.43(3) . ? C72 C73 1.28(3) . ? C73 C74 1.34(3) . ? C74 C75 1.43(3) . ? C81 C82 1.34(2) . ? C82 C83 1.40(3) . ? C83 C84 1.33(3) . ? C84 C85 1.43(2) . ? C91 C92 1.37(2) . ? C92 C93 1.39(3) . ? C93 C94 1.39(2) . ? C94 C95 1.43(2) . ? C101 C102 1.35(3) . ? C102 C103 1.41(3) . ? C103 C104 1.43(3) . ? C104 C105 1.39(3) . ? C112 C113 1.34(2) . ? C113 C114 1.39(2) . ? C114 C115 1.42(2) . ? C121 C122 1.39(3) . ? C122 C123 1.40(3) . ? C123 C124 1.44(3) . ? C124 C125 1.36(2) . ? C131 C13O 1.39(3) . ? C131 C133 1.43(3) . ? C133 C134 1.38(3) . ? C134 C135 1.35(2) . ? C141 C142 1.29(3) . ? C142 C143 1.36(3) . ? C143 C144 1.42(3) . ? C144 C145 1.37(3) . ? C151 C152 1.34(2) 4_675 ? C152 C151 1.34(2) 4_476 ? C152 C153 1.37(2) . ? C153 C154 1.32(2) . ? C154 C155 1.36(2) . ? C155 N15 1.34(2) 4_476 ? C161 C162 1.33(2) . ? C162 C163 1.42(2) . ? C163 C164 1.39(2) . ? C164 C165 1.33(2) . ? C171 C172 1.45(3) . ? C172 C173 1.32(3) . ? C173 C174 1.38(3) . ? C174 C175 1.34(3) . ? C181 C182 1.38(3) . ? C182 C183 1.34(3) . ? C183 C184 1.43(3) . ? C184 C185 1.38(3) . ? C191 C192 1.35(2) . ? C192 C193 1.40(2) . ? C193 C194 1.36(2) . ? C194 C195 1.33(2) . ? C201 C202 1.43(3) . ? C202 C203 1.43(3) . ? C203 C204 1.39(3) . ? C203 C2L 1.55(3) 2_655 ? C204 C205 1.34(2) . ? O11 S1 1.440(10) . ? O12 S1 1.497(11) . ? O13 S1 1.453(13) . ? O14 S1 1.457(10) . ? O21 S2 1.466(8) . ? O22 S2 1.474(8) . ? O23 S2 1.461(10) . ? O24 S2 1.460(8) . ? O31 S3 1.473(9) . ? O32 S3 1.447(9) . ? O33 S3 1.473(10) . ? O34 S3 1.456(9) . ? O41 S4 1.472(8) . ? O42 S4 1.440(9) . ? O43 S4 1.488(10) . ? O44 S4 1.467(8) . ? O51 S5 1.485(13) . ? O52 S5 1.456(13) . ? O53 S5 1.451(19) . ? O54 S5 1.453(13) . ? O61 S6 1.446(11) . ? O62 S6 1.476(12) . ? O63 S6 1.470(18) . ? O64 S6 1.463(12) . ? 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 O11L Ni1 O12L 178.3(4) . . ? O11L Ni1 N1 89.7(5) . . ? O12L Ni1 N1 92.0(5) . . ? O11L Ni1 N3 89.5(5) . . ? O12L Ni1 N3 90.6(4) . . ? N1 Ni1 N3 93.3(5) . . ? O11L Ni1 N5 89.9(5) . . ? O12L Ni1 N5 90.0(5) . . ? N1 Ni1 N5 89.2(5) . . ? N3 Ni1 N5 177.5(5) . . ? O11L Ni1 N2 88.8(5) . 2 ? O12L Ni1 N2 89.6(4) . 2 ? N1 Ni1 N2 176.9(5) . 2 ? N3 Ni1 N2 89.4(5) . 2 ? N5 Ni1 N2 88.2(5) . 2 ? O23L Ni2 N6 91.3(5) . 4_686 ? O23L Ni2 N4 92.1(5) . . ? N6 Ni2 N4 176.1(5) 4_686 . ? O23L Ni2 O24L 88.5(5) . . ? N6 Ni2 O24L 87.2(5) 4_686 . ? N4 Ni2 O24L 90.9(5) . . ? O23L Ni2 O21L 89.2(5) . . ? N6 Ni2 O21L 93.4(5) 4_686 . ? N4 Ni2 O21L 88.6(5) . . ? O24L Ni2 O21L 177.6(5) . . ? O23L Ni2 O22L 178.1(5) . . ? N6 Ni2 O22L 88.6(5) 4_686 . ? N4 Ni2 O22L 88.1(5) . . ? O24L Ni2 O22L 93.4(4) . . ? O21L Ni2 O22L 88.9(4) . . ? N10 Ni3 O31L 87.6(5) . . ? N10 Ni3 N14 90.8(5) . . ? O31L Ni3 N14 86.9(5) . . ? N10 Ni3 N7 179.0(5) . . ? O31L Ni3 N7 92.5(5) . . ? N14 Ni3 N7 88.2(5) . . ? N10 Ni3 N12 91.1(5) . . ? O31L Ni3 N12 89.2(5) . . ? N14 Ni3 N12 175.6(5) . . ? N7 Ni3 N12 89.8(5) . . ? N10 Ni3 O32L 89.8(5) . . ? O31L Ni3 O32L 177.0(5) . . ? N14 Ni3 O32L 91.8(5) . . ? N7 Ni3 O32L 90.2(5) . . ? N12 Ni3 O32L 92.2(5) . . ? O41L Ni4 O42L 176.1(4) . . ? O41L Ni4 N9 91.9(5) . 4 ? O42L Ni4 N9 92.0(5) . 4 ? O41L Ni4 N8 88.0(5) . 4_556 ? O42L Ni4 N8 88.1(5) . 4_556 ? N9 Ni4 N8 179.2(5) 4 4_556 ? O41L Ni4 N11 90.4(4) . . ? O42L Ni4 N11 89.6(5) . . ? N9 Ni4 N11 90.1(5) 4 . ? N8 Ni4 N11 89.1(5) 4_556 . ? O41L Ni4 N13 87.7(5) . 1_545 ? O42L Ni4 N13 92.4(5) . 1_545 ? N9 Ni4 N13 89.0(5) 4 1_545 ? N8 Ni4 N13 91.8(5) 4_556 1_545 ? N11 Ni4 N13 177.9(5) . 1_545 ? N16 Ni5 N18 175.9(6) . . ? N16 Ni5 O52L 91.9(5) . . ? N18 Ni5 O52L 91.9(5) . . ? N16 Ni5 O51L 89.1(5) . . ? N18 Ni5 O51L 87.0(5) . . ? O52L Ni5 O51L 178.1(4) . . ? N16 Ni5 N20 89.5(5) . . ? N18 Ni5 N20 92.1(5) . . ? O52L Ni5 N20 86.5(4) . . ? O51L Ni5 N20 91.9(4) . . ? N16 Ni5 N19 89.5(5) . . ? N18 Ni5 N19 89.1(5) . . ? O52L Ni5 N19 91.4(4) . . ? O51L Ni5 N19 90.2(4) . . ? N20 Ni5 N19 177.7(5) . . ? O62L Ni6 O63L 86.9(5) . . ? O62L Ni6 O61L 94.0(5) . . ? O63L Ni6 O61L 178.6(4) . . ? O62L Ni6 N15 90.3(5) . . ? O63L Ni6 N15 89.8(5) . . ? O61L Ni6 N15 89.0(5) . . ? O62L Ni6 O64L 176.3(5) . . ? O63L Ni6 O64L 90.1(4) . . ? O61L Ni6 O64L 89.1(4) . . ? N15 Ni6 O64L 91.8(5) . . ? O62L Ni6 N17 87.5(5) . . ? O63L Ni6 N17 93.4(5) . . ? O61L Ni6 N17 87.9(5) . . ? N15 Ni6 N17 176.0(5) . . ? O64L Ni6 N17 90.7(5) . . ? C25 N2 C21 115.7(16) . . ? C25 N2 Ni1 123.6(12) . 2_545 ? C21 N2 Ni1 120.5(12) . 2_545 ? C31 N3 C35 118.5(15) . . ? C31 N3 Ni1 122.2(11) . . ? C35 N3 Ni1 119.2(11) . . ? C45 N4 C41 117.7(16) . . ? C45 N4 Ni2 122.5(13) . . ? C41 N4 Ni2 119.7(12) . . ? C55 N5 C51 117.5(15) . . ? C55 N5 Ni1 122.4(12) . . ? C51 N5 Ni1 119.7(11) . . ? C65 N6 C61 117.4(16) . . ? C65 N6 Ni2 120.9(12) . 4_485 ? C61 N6 Ni2 121.6(12) . 4_485 ? C71 N7 C75 123.9(16) . . ? C71 N7 Ni3 118.0(12) . . ? C75 N7 Ni3 118.1(12) . . ? C85 N8 C81 120.3(13) . . ? C85 N8 Ni4 118.8(11) . 4 ? C81 N8 Ni4 120.8(11) . 4 ? C91 N9 C95 119.1(14) . . ? C91 N9 Ni4 120.7(12) . 4_556 ? C95 N9 Ni4 120.1(11) . 4_556 ? C101 N10 C105 116.6(16) . . ? C101 N10 Ni3 123.9(12) . . ? C105 N10 Ni3 119.4(12) . . ? C115 N11 C11 114.3(15) . . ? C115 N11 Ni4 123.4(12) . . ? C11 N11 Ni4 122.3(11) . . ? C121 N12 C125 115.1(16) . . ? C121 N12 Ni3 121.3(12) . . ? C125 N12 Ni3 122.3(12) . . ? C135 N13 C13O 118.9(15) . . ? C135 N13 Ni4 126.6(11) . 1_565 ? C13O N13 Ni4 114.5(12) . 1_565 ? C141 N14 C145 113.5(16) . . ? C141 N14 Ni3 124.0(12) . . ? C145 N14 Ni3 122.4(12) . . ? C155 N15 C151 115.2(15) 4_675 . ? C155 N15 Ni6 122.9(12) 4_675 . ? C151 N15 Ni6 121.1(11) . . ? C161 N16 C165 113.0(14) . . ? C161 N16 Ni5 124.1(12) . . ? C165 N16 Ni5 122.9(11) . . ? C175 N17 C171 119.0(17) . . ? C175 N17 Ni6 119.7(13) . . ? C171 N17 Ni6 121.2(13) . . ? C185 N18 C181 116.8(15) . . ? C185 N18 Ni5 123.3(12) . . ? C181 N18 Ni5 119.5(12) . . ? C191 N19 C195 114.6(14) . . ? C191 N19 Ni5 124.1(11) . . ? C195 N19 Ni5 121.1(11) . . ? C205 N20 C201 117.3(15) . . ? C205 N20 Ni5 121.7(11) . . ? C201 N20 Ni5 120.5(11) . . ? N2 C25 C24 129(2) . . ? C2B C1B C33 120.3(18) . . ? C1B C2B C43 116.3(15) . . ? C53 C1C C2C 124(2) . . ? C1C C2C C63 112.3(18) . . ? C2D C1D C73 113(2) . . ? C1D C2D C83 115.0(17) . . ? C2E C1E C103 113.1(14) . . ? C1E C2E C93 111.8(14) . . ? C2F C1F C113 115.0(13) . . ? C1F C2F C123 113.6(16) . . ? C2G C1G C133 120.2(18) . . ? C143 C2G C1G 124(3) . . ? C2H C1H C153 113.0(14) . . ? C1H C2H C163 119.8(13) . . ? C2I C1I C173 107.7(16) . . ? C1I C2I C183 105.2(16) . . ? C2L C1L C193 114.5(15) . . ? C1L C2L C203 116.7(18) . 2_645 ? C12 C11B N1 126(2) . . ? C15 N1 C11B 109.8(19) . . ? C15 N1 Ni1 125.4(17) . . ? C11B N1 Ni1 124.8(12) . . ? N11 C11 C112 126.2(17) . . ? C13 C12 C11B 120(2) . . ? C12 C13 C14 118(3) . . ? C12 C13 C1A 117(3) . . ? C14 C13 C1A 118(3) . . ? C15 C14 C13 113(3) . . ? N1 C15 C14 133(3) . . ? C2A C1A C13 102.6(19) . . ? C1A C2A C23 110(2) . . ? N2 C21 C22 121(2) . . ? C23 C22 C21 115(2) . . ? C24 C23 C22 130(3) . . ? C24 C23 C2A 129(2) . . ? C22 C23 C2A 101(3) . . ? C23 C24 C25 110(2) . . ? N3 C31 C32 125.0(16) . . ? C31 C32 C33 121.0(16) . . ? C34 C33 C1B 128.7(15) . . ? C34 C33 C32 111.3(15) . . ? C1B C33 C32 120.0(16) . . ? C33 C34 C35 125.9(18) . . ? N3 C35 C34 118.0(17) . . ? N4 C41 C42 119.0(17) . . ? C43 C42 C41 122.3(18) . . ? C44 C43 C42 114.8(17) . . ? C44 C43 C2B 122.8(18) . . ? C42 C43 C2B 122.4(15) . . ? C43 C44 C45 122(2) . . ? N4 C45 C44 124(2) . . ? C52 C51 N5 123.0(19) . . ? C51 C52 C53 123(2) . . ? C52 C53 C54 117.1(19) . . ? C52 C53 C1C 119(2) . . ? C54 C53 C1C 123.9(18) . . ? C53 C54 C55 117.3(19) . . ? N5 C55 C54 121.4(18) . . ? N6 C61 C62 121.2(18) . . ? C61 C62 C63 121.4(19) . . ? C64 C63 C62 117.6(19) . . ? C64 C63 C2C 118(2) . . ? C62 C63 C2C 124.6(19) . . ? C63 C64 C65 118(2) . . ? N6 C65 C64 124.1(17) . . ? N7 C71 C72 115.4(19) . . ? C73 C72 C71 123(3) . . ? C72 C73 C74 122(2) . . ? C72 C73 C1D 114(3) . . ? C74 C73 C1D 123(2) . . ? C73 C74 C75 118(2) . . ? N7 C75 C74 117(2) . . ? C82 C81 N8 120.3(17) . . ? C81 C82 C83 122(2) . . ? C84 C83 C82 116.6(18) . . ? C84 C83 C2D 116(2) . . ? C82 C83 C2D 127(2) . . ? C83 C84 C85 120.7(19) . . ? N8 C85 C84 119.8(17) . . ? N9 C91 C92 121.8(18) . . ? C91 C92 C93 121.1(19) . . ? C92 C93 C94 118.6(16) . . ? C92 C93 C2E 124.8(18) . . ? C94 C93 C2E 116.3(18) . . ? C93 C94 C95 115.3(18) . . ? N9 C95 C94 123.5(17) . . ? N10 C101 C102 128(2) . . ? C101 C102 C103 117(2) . . ? C102 C103 C104 118.4(18) . . ? C102 C103 C1E 122.1(19) . . ? C104 C103 C1E 119.1(17) . . ? C105 C104 C103 118.5(18) . . ? N10 C105 C104 121.5(18) . . ? C113 C112 C11 119.7(17) . . ? C112 C113 C114 116.2(15) . . ? C112 C113 C1F 125.3(14) . . ? C114 C113 C1F 118.4(15) . . ? C113 C114 C115 118.8(17) . . ? N11 C115 C114 124.7(18) . . ? N12 C121 C122 128(2) . . ? C121 C122 C123 117(2) . . ? C122 C123 C124 116.3(18) . . ? C122 C123 C2F 123(2) . . ? C124 C123 C2F 120.5(18) . . ? C125 C124 C123 119.3(18) . . ? N12 C125 C124 124.5(18) . . ? C13O C131 C133 123(2) . . ? N13 C13O C131 117(2) . . ? C134 C133 C131 115.6(18) . . ? C134 C133 C1G 118(2) . . ? C131 C133 C1G 126.3(18) . . ? C135 C134 C133 119.1(19) . . ? N13 C135 C134 126.1(18) . . ? C142 C141 N14 127(2) . . ? C141 C142 C143 122(2) . . ? C142 C143 C2G 139(2) . . ? C142 C143 C144 114.4(18) . . ? C2G C143 C144 107(2) . . ? C145 C144 C143 119(2) . . ? N14 C145 C144 123.8(19) . . ? C152 C151 N15 121.8(16) 4_675 . ? C151 C152 C153 121.2(17) 4_476 . ? C154 C153 C152 116.8(16) . . ? C154 C153 C1H 123.6(16) . . ? C152 C153 C1H 119.5(17) . . ? C153 C154 C155 122.7(19) . . ? N15 C155 C154 122.3(18) 4_476 . ? C162 C161 N16 123.1(17) . . ? C161 C162 C163 124.2(18) . . ? C164 C163 C162 112.3(15) . . ? C164 C163 C2H 126.6(14) . . ? C162 C163 C2H 120.6(16) . . ? C165 C164 C163 120.1(17) . . ? C164 C165 N16 126.8(16) . . ? N17 C171 C172 121(2) . . ? C173 C172 C171 117(2) . . ? C172 C173 C174 120(2) . . ? C172 C173 C1I 128.3(17) . . ? C174 C173 C1I 111(2) . . ? C175 C174 C173 118(2) . . ? N17 C175 C174 124(2) . . ? C182 C181 N18 122.6(18) . . ? C183 C182 C181 118(2) . . ? C182 C183 C184 122(2) . . ? C182 C183 C2I 114(2) . . ? C184 C183 C2I 124.1(19) . . ? C185 C184 C183 115(2) . . ? N18 C185 C184 125(2) . . ? N19 C191 C192 126.3(19) . . ? C191 C192 C193 117.0(19) . . ? C194 C193 C192 118.4(16) . . ? C194 C193 C1L 119.0(17) . . ? C192 C193 C1L 122.4(18) . . ? C195 C194 C193 120.8(18) . . ? C194 C195 N19 122.6(17) . . ? N20 C201 C202 124(2) . . ? C201 C202 C203 117(2) . . ? C204 C203 C202 117(2) . . ? C204 C203 C2L 124(2) . 2_655 ? C202 C203 C2L 118.6(19) . 2_655 ? C205 C204 C203 123(2) . . ? C204 C205 N20 122.8(19) . . ? O11 S1 O13 112.1(8) . . ? O11 S1 O14 111.7(8) . . ? O13 S1 O14 110.3(8) . . ? O11 S1 O12 108.3(9) . . ? O13 S1 O12 107.0(9) . . ? O14 S1 O12 107.2(9) . . ? O24 S2 O23 109.9(6) . . ? O24 S2 O21 109.1(6) . . ? O23 S2 O21 109.5(6) . . ? O24 S2 O22 108.9(6) . . ? O23 S2 O22 110.7(6) . . ? O21 S2 O22 108.6(6) . . ? O32 S3 O34 110.3(7) . . ? O32 S3 O31 110.6(7) . . ? O34 S3 O31 107.8(7) . . ? O32 S3 O33 110.6(7) . . ? O34 S3 O33 109.3(6) . . ? O31 S3 O33 108.1(7) . . ? O42 S4 O44 110.2(7) . . ? O42 S4 O41 110.1(7) . . ? O44 S4 O41 108.9(6) . . ? O42 S4 O43 109.8(7) . . ? O44 S4 O43 109.5(6) . . ? O41 S4 O43 108.3(6) . . ? O53 S5 O54 110.9(11) . . ? O53 S5 O52 110.8(11) . . ? O54 S5 O52 110.3(12) . . ? O53 S5 O51 108.1(11) . . ? O54 S5 O51 108.8(11) . . ? O52 S5 O51 107.8(11) . . ? O61 S6 O64 110.4(11) . . ? O61 S6 O63 111.5(10) . . ? O64 S6 O63 109.4(11) . . ? O61 S6 O62 109.7(10) . . ? O64 S6 O62 108.7(11) . . ? O63 S6 O62 107.0(11) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 21.05 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.313 _refine_diff_density_min -0.911 _refine_diff_density_rms 0.159 # * END