# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2325 #======================================================== # SUBMISSION DETAILS _publ_contact_author ; Dr. Craig Rice Department of Chemistry and Biological Sciences University of Huddersfield Huddersfield HD1 3DH ; _publ_contact_author_fax '01484 472182' _publ_contact_author_email c.r.rice@hud.ac.uk _publ_contact_letter ; This CIF file contains details of the eight crystal structures in the paper 'New multidentate ligands for supramolecular coordination chemistry: double and triple helical complexes of ligands containing pyridyl and thiazolyl donor units' by Craig Rice, et al, submitted to Dalton Transactions for publication. ; #======================================================== data_jiffy1m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H27 Cu F12 N6 O2 P2 S3' _chemical_formula_weight 953.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' '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' 'S' 'S' 0.1246 0.1234 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 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 13.9497(14) _cell_length_b 23.133(2) _cell_length_c 22.485(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.792(2) _cell_angle_gamma 90.00 _cell_volume 7150.3(12) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19016 _diffrn_reflns_av_R_equivalents 0.1004 _diffrn_reflns_av_sigmaI/netI 0.1146 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6291 _reflns_number_gt 3197 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6291 _refine_ls_number_parameters 505 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.1655 _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.2807 _refine_ls_wR_factor_gt 0.2332 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _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 0.66657(8) 0.63095(4) 0.76312(5) 0.0347(3) Uani 1 1 d . . . N11 N 0.5959(6) 0.5587(3) 0.8011(3) 0.0441(19) Uani 1 1 d . . . C12 C 0.5313(7) 0.5485(4) 0.8409(4) 0.046(2) Uani 1 1 d . . . C13 C 0.5217(8) 0.4929(5) 0.8541(6) 0.069(3) Uani 1 1 d . . . H13 H 0.4789 0.4791 0.8783 0.083 Uiso 1 1 calc R . . S14 S 0.5978(2) 0.45032(12) 0.82098(17) 0.0718(10) Uani 1 1 d . . . C15 C 0.6361(7) 0.5099(4) 0.7873(4) 0.047(2) Uani 1 1 d . . . N21 N 0.7427(6) 0.5633(4) 0.7375(3) 0.048(2) Uani 1 1 d . . . C22 C 0.7148(7) 0.5100(4) 0.7511(4) 0.049(2) Uani 1 1 d . . . C23 C 0.7575(9) 0.4607(5) 0.7344(5) 0.066(3) Uani 1 1 d . . . H23 H 0.7345 0.4246 0.7436 0.079 Uiso 1 1 calc R . . C24 C 0.8358(9) 0.4652(6) 0.7035(5) 0.073(4) Uani 1 1 d . . . H24 H 0.8673 0.4324 0.6926 0.087 Uiso 1 1 calc R . . C25 C 0.8649(11) 0.5195(7) 0.6899(6) 0.097(5) Uani 1 1 d . . . H25 H 0.9163 0.5240 0.6688 0.116 Uiso 1 1 calc R . . C26 C 0.8172(9) 0.5679(5) 0.7077(5) 0.065(3) Uani 1 1 d . . . H26 H 0.8380 0.6045 0.6984 0.078 Uiso 1 1 calc R . . N31 N 0.5982(5) 0.6962(3) 0.8019(3) 0.0385(17) Uani 1 1 d . . . C32 C 0.6381(7) 0.7074(4) 0.8576(4) 0.042(2) Uani 1 1 d . . . S33 S 0.5931(2) 0.76651(11) 0.88828(12) 0.0540(7) Uani 1 1 d . . . C34 C 0.5144(7) 0.7778(4) 0.8214(5) 0.051(3) Uani 1 1 d . . . H34 H 0.4698 0.8080 0.8140 0.061 Uiso 1 1 calc R . . C35 C 0.5277(7) 0.7362(4) 0.7813(4) 0.041(2) Uani 1 1 d . . . N41 N 0.7575(6) 0.6359(3) 0.8526(4) 0.051(2) Uani 1 1 d . . . C42 C 0.7183(7) 0.6701(4) 0.8892(4) 0.049(2) Uani 1 1 d . . . C43 C 0.7452(9) 0.6718(5) 0.9515(5) 0.065(3) Uani 1 1 d . . . H43 H 0.7166 0.6977 0.9749 0.078 Uiso 1 1 calc R . . C44 C 0.8171(11) 0.6332(5) 0.9777(6) 0.088(4) Uani 1 1 d . . . H44 H 0.8330 0.6296 1.0194 0.106 Uiso 1 1 calc R . . C45 C 0.8651(11) 0.5998(5) 0.9391(6) 0.087(5) Uani 1 1 d . . . H45 H 0.9182 0.5770 0.9547 0.104 Uiso 1 1 calc R . . C46 C 0.8316(8) 0.6018(5) 0.8779(6) 0.067(3) Uani 1 1 d . . . H46 H 0.8615 0.5785 0.8528 0.081 Uiso 1 1 calc R . . N51 N 0.4151(6) 0.6315(3) 0.8306(3) 0.0430(18) Uani 1 1 d . . . C52 C 0.3765(7) 0.6675(4) 0.8648(4) 0.041(2) Uani 1 1 d . . . S53 S 0.4181(2) 0.66249(12) 0.94030(12) 0.0595(8) Uani 1 1 d . . . C54 C 0.4945(8) 0.6083(4) 0.9263(5) 0.057(3) Uani 1 1 d . . . H54 H 0.5380 0.5893 0.9558 0.069 Uiso 1 1 calc R . . C55 C 0.4831(7) 0.5969(4) 0.8666(5) 0.049(2) Uani 1 1 d . . . N61 N 0.2610(6) 0.6980(3) 0.7803(3) 0.047(2) Uani 1 1 d . . . C62 C 0.2994(7) 0.7085(4) 0.8375(4) 0.042(2) Uani 1 1 d . . . C63 C 0.2703(8) 0.7550(4) 0.8692(5) 0.052(3) Uani 1 1 d . . . H63 H 0.3001 0.7618 0.9088 0.062 Uiso 1 1 calc R . . C64 C 0.1987(9) 0.7906(5) 0.8424(5) 0.065(3) Uani 1 1 d . . . H64 H 0.1776 0.8215 0.8633 0.078 Uiso 1 1 calc R . . C65 C 0.1575(8) 0.7795(5) 0.7822(6) 0.068(3) Uani 1 1 d . . . H65 H 0.1071 0.8023 0.7623 0.082 Uiso 1 1 calc R . . C66 C 0.1937(9) 0.7340(5) 0.7533(5) 0.064(3) Uani 1 1 d . . . H66 H 0.1694 0.7282 0.7125 0.076 Uiso 1 1 calc R . . C71 C 0.6810(16) 0.4875(8) 0.0391(10) 0.118(6) Uani 1 1 d U . . C72 C 0.6077(18) 0.4978(8) 0.0048(9) 0.146(7) Uani 1 1 d U . . O73 O 0.6775(12) 0.4798(8) 0.0946(7) 0.181(7) Uani 1 1 d U . . C74 C 0.767(2) 0.4831(14) 0.0169(15) 0.235(14) Uani 1 1 d U . . C81 C 0.399(3) 0.8549(18) 0.0971(18) 0.257(16) Uani 1 1 d U . . C82 C 0.334(3) 0.864(2) 0.073(3) 0.31(2) Uani 1 1 d U . . O83 O 0.4367(17) 0.7981(8) 0.0469(7) 0.221(8) Uani 1 1 d U . . C84 C 0.304(2) 0.8248(9) 0.0206(11) 0.187(10) Uani 1 1 d U . . P1 P 0.6005(3) 0.66158(14) 0.10842(15) 0.0717(10) Uani 1 1 d . . . F11 F 0.4917(7) 0.6446(4) 0.0786(4) 0.131(4) Uani 1 1 d . . . F12 F 0.5562(6) 0.7145(4) 0.1393(3) 0.099(2) Uani 1 1 d . . . F13 F 0.5920(7) 0.6233(3) 0.1657(4) 0.114(3) Uani 1 1 d . . . F14 F 0.7016(6) 0.6802(5) 0.1431(5) 0.147(4) Uani 1 1 d . . . F15 F 0.6407(12) 0.6102(5) 0.0780(5) 0.189(6) Uani 1 1 d . . . F16 F 0.6038(8) 0.7000(4) 0.0502(4) 0.130(3) Uani 1 1 d . . . P2 P 0.4325(2) 0.92245(11) 0.89368(13) 0.0518(7) Uani 1 1 d . . . F21 F 0.3245(6) 0.9347(6) 0.8862(4) 0.159(5) Uani 1 1 d . . . F22 F 0.4442(6) 0.9430(4) 0.9612(3) 0.109(3) Uani 1 1 d . . . F23 F 0.4353(9) 0.8585(3) 0.9153(4) 0.134(4) Uani 1 1 d . . . F24 F 0.5454(6) 0.9121(5) 0.8988(4) 0.139(4) Uani 1 1 d . . . F25 F 0.4423(9) 0.9842(3) 0.8679(6) 0.154(4) Uani 1 1 d . . . F26 F 0.4194(9) 0.8997(4) 0.8276(3) 0.154(5) 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 0.0410(6) 0.0275(5) 0.0362(6) -0.0003(5) 0.0082(4) 0.0013(5) N11 0.050(5) 0.037(4) 0.043(5) -0.012(3) 0.001(4) 0.011(4) C12 0.044(6) 0.042(6) 0.049(6) -0.012(4) -0.003(5) 0.007(5) C13 0.068(7) 0.042(6) 0.106(10) -0.016(6) 0.039(7) -0.011(6) S14 0.0622(18) 0.0335(14) 0.125(3) -0.0176(15) 0.0312(18) 0.0001(13) C15 0.044(5) 0.033(5) 0.059(6) -0.008(4) -0.003(5) 0.009(4) N21 0.051(5) 0.054(5) 0.040(5) -0.004(4) 0.011(4) 0.010(4) C22 0.059(6) 0.049(6) 0.035(5) 0.002(4) -0.002(5) 0.020(5) C23 0.083(8) 0.059(7) 0.055(7) 0.002(5) 0.009(6) 0.035(6) C24 0.091(9) 0.071(8) 0.060(8) 0.007(6) 0.022(7) 0.035(7) C25 0.115(12) 0.114(13) 0.075(9) 0.014(8) 0.052(8) 0.061(10) C26 0.080(8) 0.054(7) 0.063(7) 0.012(6) 0.023(6) 0.017(6) N31 0.044(4) 0.025(4) 0.050(5) 0.004(3) 0.017(4) 0.002(3) C32 0.052(6) 0.037(5) 0.039(5) -0.005(4) 0.014(4) 0.004(4) S33 0.0716(18) 0.0396(13) 0.0508(15) -0.0090(11) 0.0106(13) 0.0111(13) C34 0.061(6) 0.031(5) 0.063(7) -0.004(4) 0.017(5) 0.007(5) C35 0.057(6) 0.028(5) 0.044(5) -0.001(4) 0.019(4) -0.007(4) N41 0.060(5) 0.037(4) 0.058(5) 0.001(4) 0.017(4) 0.012(4) C42 0.061(6) 0.037(5) 0.046(6) 0.006(4) 0.001(5) 0.000(5) C43 0.080(8) 0.048(6) 0.064(7) -0.006(5) 0.000(6) 0.004(6) C44 0.111(11) 0.065(8) 0.074(9) -0.004(7) -0.027(8) 0.016(8) C45 0.124(12) 0.060(8) 0.064(8) -0.003(6) -0.020(8) 0.048(8) C46 0.070(8) 0.052(7) 0.078(8) -0.001(6) 0.006(6) 0.020(6) N51 0.051(5) 0.038(4) 0.044(4) -0.005(4) 0.018(4) -0.002(4) C52 0.047(5) 0.036(5) 0.044(5) -0.012(4) 0.013(4) -0.002(4) S53 0.0784(19) 0.0543(16) 0.0436(15) -0.0100(12) 0.0045(13) 0.0186(15) C54 0.060(7) 0.047(6) 0.061(7) -0.015(5) -0.004(5) 0.013(5) C55 0.048(6) 0.039(5) 0.062(7) -0.016(5) 0.018(5) -0.002(5) N61 0.065(5) 0.041(4) 0.035(4) 0.006(4) 0.005(4) -0.003(4) C62 0.052(6) 0.035(5) 0.041(5) 0.001(4) 0.018(4) -0.014(4) C63 0.070(7) 0.043(6) 0.045(6) -0.008(5) 0.019(5) 0.011(5) C64 0.075(8) 0.058(7) 0.067(8) -0.002(6) 0.026(6) 0.011(6) C65 0.067(8) 0.062(8) 0.075(8) 0.013(6) 0.011(6) 0.009(6) C66 0.096(9) 0.044(6) 0.048(6) 0.000(5) 0.003(6) 0.007(6) C71 0.146(14) 0.093(12) 0.114(11) 0.006(11) 0.019(10) 0.032(12) C72 0.200(16) 0.080(11) 0.136(14) 0.014(11) -0.034(13) 0.007(13) O73 0.175(13) 0.232(17) 0.133(10) 0.044(12) 0.018(9) -0.035(12) C74 0.24(2) 0.22(3) 0.29(3) 0.07(2) 0.17(2) 0.09(2) C81 0.38(4) 0.20(2) 0.26(3) 0.00(2) 0.26(2) -0.10(3) C82 0.25(3) 0.26(3) 0.49(5) -0.16(3) 0.25(3) -0.17(2) O83 0.34(2) 0.196(16) 0.135(13) 0.009(11) 0.058(14) -0.018(16) C84 0.30(3) 0.114(14) 0.217(19) 0.041(14) 0.24(2) 0.034(16) P1 0.097(3) 0.0585(19) 0.0589(19) -0.0087(15) 0.0119(18) -0.0174(18) F11 0.162(9) 0.130(7) 0.084(6) 0.017(5) -0.032(6) -0.071(7) F12 0.121(6) 0.102(6) 0.070(5) -0.011(4) 0.009(4) 0.018(5) F13 0.165(8) 0.088(5) 0.078(5) 0.017(4) -0.008(5) -0.033(6) F14 0.083(6) 0.177(10) 0.190(10) -0.048(8) 0.046(6) -0.039(6) F15 0.334(18) 0.118(8) 0.116(8) -0.040(7) 0.038(10) 0.081(10) F16 0.195(9) 0.108(7) 0.102(6) 0.032(5) 0.071(7) -0.020(7) P2 0.0566(17) 0.0420(15) 0.0567(17) -0.0035(12) 0.0096(13) 0.0114(13) F21 0.059(5) 0.291(15) 0.120(7) -0.009(8) -0.007(5) 0.032(7) F22 0.118(6) 0.122(6) 0.079(5) -0.039(5) -0.006(5) 0.033(5) F23 0.234(12) 0.063(5) 0.113(7) 0.017(5) 0.056(7) -0.008(6) F24 0.072(5) 0.209(11) 0.143(8) 0.051(8) 0.043(5) 0.050(6) F25 0.177(10) 0.060(5) 0.238(12) 0.041(6) 0.069(9) 0.014(6) F26 0.264(12) 0.131(7) 0.050(4) -0.012(5) -0.019(6) 0.121(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 Cu1 N21 2.028(8) . ? Cu1 N31 2.056(7) . ? Cu1 N61 2.171(8) 2_656 ? Cu1 N11 2.187(8) . ? Cu1 N41 2.192(8) . ? Cu1 N51 2.219(8) 2_656 ? N11 C15 1.321(11) . ? N11 C12 1.393(12) . ? C12 C13 1.331(14) . ? C12 C55 1.474(12) . ? C13 S14 1.710(11) . ? S14 C15 1.703(10) . ? C15 C22 1.473(14) . ? N21 C26 1.334(13) . ? N21 C22 1.344(13) . ? C22 C23 1.367(13) . ? C23 C24 1.395(16) . ? C24 C25 1.371(19) . ? C25 C26 1.396(16) . ? N31 C32 1.308(11) . ? N31 C35 1.373(11) . ? C32 C42 1.494(13) . ? C32 S33 1.699(9) . ? S33 C34 1.724(11) . ? C34 C35 1.353(12) . ? C35 C35 1.486(18) 2_656 ? N41 C42 1.325(12) . ? N41 C46 1.346(12) . ? C42 C43 1.388(14) . ? C43 C44 1.396(16) . ? C44 C45 1.411(18) . ? C45 C46 1.378(16) . ? N51 C52 1.311(11) . ? N51 C55 1.390(12) . ? N51 Cu1 2.219(8) 2_656 ? C52 C62 1.485(13) . ? C52 S53 1.702(9) . ? S53 C54 1.709(10) . ? C54 C55 1.350(14) . ? N61 C66 1.324(13) . ? N61 C62 1.329(11) . ? N61 Cu1 2.171(8) 2_656 ? C62 C63 1.390(12) . ? C63 C64 1.354(14) . ? C64 C65 1.402(16) . ? C65 C66 1.377(15) . ? C71 C72 1.19(2) . ? C71 O73 1.27(2) . ? C71 C74 1.37(3) . ? C81 C82 1.00(8) . ? C81 O83 1.86(4) . ? C82 C84 1.49(5) . ? P1 F15 1.525(10) . ? P1 F14 1.552(10) . ? P1 F12 1.582(8) . ? P1 F13 1.585(8) . ? P1 F16 1.590(8) . ? P1 F11 1.600(9) . ? P2 F21 1.515(8) . ? P2 F23 1.556(8) . ? P2 F25 1.557(8) . ? P2 F26 1.558(8) . ? P2 F22 1.573(8) . ? P2 F24 1.577(8) . ? 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 N21 Cu1 N31 171.5(3) . . ? N21 Cu1 N61 96.7(3) . 2_656 ? N31 Cu1 N61 87.2(3) . 2_656 ? N21 Cu1 N11 79.2(3) . . ? N31 Cu1 N11 97.1(3) . . ? N61 Cu1 N11 175.4(3) 2_656 . ? N21 Cu1 N41 92.9(3) . . ? N31 Cu1 N41 79.1(3) . . ? N61 Cu1 N41 97.8(3) 2_656 . ? N11 Cu1 N41 84.8(3) . . ? N21 Cu1 N51 86.8(3) . 2_656 ? N31 Cu1 N51 101.4(3) . 2_656 ? N61 Cu1 N51 76.8(3) 2_656 2_656 ? N11 Cu1 N51 100.5(3) . 2_656 ? N41 Cu1 N51 174.5(3) . 2_656 ? C15 N11 C12 110.7(8) . . ? C15 N11 Cu1 108.9(6) . . ? C12 N11 Cu1 139.8(6) . . ? C13 C12 N11 114.1(9) . . ? C13 C12 C55 125.1(10) . . ? N11 C12 C55 120.8(8) . . ? C12 C13 S14 111.4(9) . . ? C15 S14 C13 89.6(5) . . ? N11 C15 C22 121.0(9) . . ? N11 C15 S14 114.1(8) . . ? C22 C15 S14 124.5(7) . . ? C26 N21 C22 117.9(9) . . ? C26 N21 Cu1 124.9(7) . . ? C22 N21 Cu1 117.3(6) . . ? N21 C22 C23 123.1(10) . . ? N21 C22 C15 113.5(8) . . ? C23 C22 C15 123.4(10) . . ? C22 C23 C24 119.3(12) . . ? C25 C24 C23 117.8(11) . . ? C24 C25 C26 119.8(12) . . ? N21 C26 C25 122.1(12) . . ? C32 N31 C35 110.6(7) . . ? C32 N31 Cu1 113.6(6) . . ? C35 N31 Cu1 135.2(6) . . ? N31 C32 C42 120.2(8) . . ? N31 C32 S33 115.0(7) . . ? C42 C32 S33 124.8(7) . . ? C32 S33 C34 89.6(5) . . ? C35 C34 S33 109.5(7) . . ? C34 C35 N31 115.3(8) . . ? C34 C35 C35 121.5(8) . 2_656 ? N31 C35 C35 123.1(7) . 2_656 ? C42 N41 C46 117.2(9) . . ? C42 N41 Cu1 111.5(6) . . ? C46 N41 Cu1 129.7(7) . . ? N41 C42 C43 125.1(10) . . ? N41 C42 C32 113.8(8) . . ? C43 C42 C32 121.0(10) . . ? C42 C43 C44 117.2(11) . . ? C43 C44 C45 118.2(12) . . ? C46 C45 C44 118.7(11) . . ? N41 C46 C45 123.1(11) . . ? C52 N51 C55 109.4(8) . . ? C52 N51 Cu1 111.4(6) . 2_656 ? C55 N51 Cu1 137.6(6) . 2_656 ? N51 C52 C62 120.3(8) . . ? N51 C52 S53 115.9(7) . . ? C62 C52 S53 123.8(7) . . ? C52 S53 C54 89.1(5) . . ? C55 C54 S53 110.8(8) . . ? C54 C55 N51 114.8(8) . . ? C54 C55 C12 123.7(10) . . ? N51 C55 C12 121.4(9) . . ? C66 N61 C62 117.9(9) . . ? C66 N61 Cu1 126.2(7) . 2_656 ? C62 N61 Cu1 115.1(6) . 2_656 ? N61 C62 C63 122.2(9) . . ? N61 C62 C52 115.3(8) . . ? C63 C62 C52 122.5(8) . . ? C64 C63 C62 120.1(10) . . ? C63 C64 C65 117.9(11) . . ? C66 C65 C64 118.3(11) . . ? N61 C66 C65 123.5(10) . . ? C72 C71 O73 119(2) . . ? C72 C71 C74 119(3) . . ? O73 C71 C74 122(2) . . ? C82 C81 O83 98(5) . . ? C81 C82 C84 114(6) . . ? F15 P1 F14 94.0(7) . . ? F15 P1 F12 178.6(7) . . ? F14 P1 F12 87.4(5) . . ? F15 P1 F13 90.7(6) . . ? F14 P1 F13 86.2(6) . . ? F12 P1 F13 89.3(5) . . ? F15 P1 F16 90.2(6) . . ? F14 P1 F16 96.2(6) . . ? F12 P1 F16 89.8(5) . . ? F13 P1 F16 177.4(6) . . ? F15 P1 F11 90.9(7) . . ? F14 P1 F11 174.0(6) . . ? F12 P1 F11 87.7(5) . . ? F13 P1 F11 90.4(5) . . ? F16 P1 F11 87.2(5) . . ? F21 P2 F23 100.6(7) . . ? F21 P2 F25 86.3(7) . . ? F23 P2 F25 171.9(6) . . ? F21 P2 F26 90.3(6) . . ? F23 P2 F26 88.3(5) . . ? F25 P2 F26 87.6(6) . . ? F21 P2 F22 89.3(5) . . ? F23 P2 F22 89.6(5) . . ? F25 P2 F22 94.7(6) . . ? F26 P2 F22 177.7(6) . . ? F21 P2 F24 177.0(6) . . ? F23 P2 F24 82.0(6) . . ? F25 P2 F24 90.9(6) . . ? F26 P2 F24 88.4(6) . . ? F22 P2 F24 92.2(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.992 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.129 #=END data_nolifem _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H58 Cl4 Cu2 N20 O17 S4' _chemical_formula_weight 1920.54 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' 'Cl' 'Cl' 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4641(13) _cell_length_b 15.0528(15) _cell_length_c 21.859(2) _cell_angle_alpha 80.685(2) _cell_angle_beta 81.242(2) _cell_angle_gamma 77.288(2) _cell_volume 4233.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description orange _exptl_crystal_colour rod _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22820 _diffrn_reflns_av_R_equivalents 0.1418 _diffrn_reflns_av_sigmaI/netI 0.1624 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 20.00 _reflns_number_total 7887 _reflns_number_gt 4102 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1442P)^2^+14.6259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7887 _refine_ls_number_parameters 677 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1853 _refine_ls_R_factor_gt 0.0984 _refine_ls_wR_factor_ref 0.2884 _refine_ls_wR_factor_gt 0.2353 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.016 _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 0.24196(14) 0.90261(14) 0.15647(9) 0.0302(6) Uani 1 1 d . . . N101 N 0.1956(9) 0.7610(9) 0.1716(6) 0.034(4) Uani 1 1 d . . . C102 C 0.0967(13) 0.7737(11) 0.1658(7) 0.032(4) Uiso 1 1 d . . . S103 S 0.0548(3) 0.6782(3) 0.1578(2) 0.0460(13) Uani 1 1 d . . . C104 C 0.1731(13) 0.6156(12) 0.1629(8) 0.044(5) Uiso 1 1 d . . . H104 H 0.1921 0.5514 0.1612 0.053 Uiso 1 1 calc R . . C105 C 0.2387(12) 0.6699(11) 0.1698(7) 0.029(4) Uiso 1 1 d . . . N111 N 0.3060(9) 0.8658(8) 0.2474(5) 0.025(3) Uani 1 1 d . . . C112 C 0.4046(12) 0.8709(10) 0.2386(7) 0.027(4) Uiso 1 1 d . . . S113 S 0.4602(3) 0.8625(3) 0.3057(2) 0.0394(12) Uani 1 1 d . . . C114 C 0.3461(13) 0.8493(11) 0.3478(8) 0.043(5) Uiso 1 1 d . . . H114 H 0.3342 0.8404 0.3921 0.052 Uiso 1 1 calc R . . C115 C 0.2731(12) 0.8533(11) 0.3091(7) 0.032(4) Uiso 1 1 d . . . N121 N 0.3915(9) 0.8852(9) 0.1324(5) 0.029(3) Uani 1 1 d . . . C122 C 0.4254(12) 0.8879(11) 0.0707(7) 0.033(4) Uiso 1 1 d . . . C123 C 0.3480(12) 0.8985(10) 0.0309(7) 0.029(4) Uiso 1 1 d . . . N124 N 0.2501(8) 0.9089(9) 0.0587(5) 0.029(3) Uani 1 1 d . . . C125 C 0.1776(14) 0.9199(11) 0.0214(8) 0.039(5) Uiso 1 1 d . . . H125 H 0.1081 0.9267 0.0396 0.047 Uiso 1 1 calc R . . C126 C 0.1993(13) 0.9218(11) -0.0438(8) 0.043(5) Uiso 1 1 d . . . H126 H 0.1448 0.9305 -0.0685 0.052 Uiso 1 1 calc R . . C127 C 0.3009(14) 0.9109(12) -0.0724(9) 0.049(5) Uiso 1 1 d . . . H127 H 0.3173 0.9112 -0.1163 0.059 Uiso 1 1 calc R . . C128 C 0.3775(13) 0.8997(11) -0.0331(7) 0.036(4) Uiso 1 1 d . . . C129 C 0.4856(13) 0.8886(11) -0.0565(8) 0.043(5) Uiso 1 1 d . . . H129 H 0.5060 0.8912 -0.1002 0.052 Uiso 1 1 calc R . . C130 C 0.5584(13) 0.8746(11) -0.0173(7) 0.040(5) Uiso 1 1 d . . . H130 H 0.6288 0.8659 -0.0338 0.048 Uiso 1 1 calc R . . C131 C 0.5300(13) 0.8729(11) 0.0487(8) 0.038(5) Uiso 1 1 d . . . C132 C 0.6005(13) 0.8642(11) 0.0930(7) 0.039(5) Uiso 1 1 d . . . H132 H 0.6719 0.8589 0.0797 0.046 Uiso 1 1 calc R . . C133 C 0.5633(12) 0.8638(10) 0.1551(7) 0.035(4) Uiso 1 1 d . . . H133 H 0.6097 0.8553 0.1852 0.042 Uiso 1 1 calc R . . C134 C 0.4573(12) 0.8757(10) 0.1746(7) 0.025(4) Uiso 1 1 d . . . N141 N 0.2112(9) 1.0447(9) 0.1682(5) 0.029(3) Uani 1 1 d . . . C142 C 0.1089(12) 1.0791(11) 0.1759(7) 0.031(4) Uiso 1 1 d . . . C143 C 0.0444(12) 1.0155(11) 0.1787(7) 0.027(4) Uiso 1 1 d . . . N144 N 0.0897(8) 0.9284(9) 0.1721(5) 0.028(3) Uani 1 1 d . . . C145 C 0.0345(12) 0.8660(10) 0.1734(7) 0.024(4) Uiso 1 1 d . . . C146 C -0.0750(12) 0.8899(11) 0.1838(7) 0.033(4) Uiso 1 1 d . . . H146 H -0.1152 0.8450 0.1848 0.039 Uiso 1 1 calc R . . C147 C -0.1198(13) 0.9761(11) 0.1920(7) 0.036(4) Uiso 1 1 d . . . H147 H -0.1924 0.9914 0.2005 0.043 Uiso 1 1 calc R . . C148 C -0.0638(12) 1.0441(11) 0.1887(7) 0.030(4) Uiso 1 1 d . . . C149 C -0.1030(14) 1.1406(12) 0.1944(8) 0.045(5) Uiso 1 1 d . . . H149 H -0.1751 1.1604 0.2035 0.054 Uiso 1 1 calc R . . C150 C -0.0455(13) 1.2019(13) 0.1877(8) 0.046(5) Uiso 1 1 d . . . H150 H -0.0766 1.2648 0.1886 0.055 Uiso 1 1 calc R . . C151 C 0.0666(13) 1.1743(12) 0.1787(8) 0.040(5) Uiso 1 1 d . . . C152 C 0.1303(13) 1.2356(13) 0.1749(8) 0.047(5) Uiso 1 1 d . . . H152 H 0.1037 1.2993 0.1763 0.057 Uiso 1 1 calc R . . C153 C 0.2355(14) 1.2002(13) 0.1689(8) 0.052(5) Uiso 1 1 d . . . H153 H 0.2820 1.2402 0.1665 0.062 Uiso 1 1 calc R . . C154 C 0.2736(14) 1.1063(12) 0.1663(8) 0.046(5) Uiso 1 1 d . . . H154 H 0.3457 1.0843 0.1630 0.055 Uiso 1 1 calc R . . Cu2 Cu 0.26770(14) 0.59714(14) 0.34047(9) 0.0316(6) Uani 1 1 d . . . N201 N 0.3602(9) 0.6310(8) 0.2477(6) 0.030(3) Uani 1 1 d . . . C202 C 0.4559(13) 0.6217(11) 0.2540(7) 0.033(4) Uiso 1 1 d . . . S203 S 0.5386(3) 0.6193(4) 0.1865(2) 0.0493(14) Uani 1 1 d . . . C204 C 0.4354(13) 0.6369(12) 0.1458(9) 0.047(5) Uiso 1 1 d . . . H204 H 0.4389 0.6435 0.1016 0.056 Uiso 1 1 calc R . . C205 C 0.3488(14) 0.6402(12) 0.1857(8) 0.045(5) Uiso 1 1 d . . . N211 N 0.1649(9) 0.7409(9) 0.3267(5) 0.031(4) Uani 1 1 d U . . C212 C 0.0708(12) 0.7301(10) 0.3325(7) 0.030(4) Uiso 1 1 d . . . S213 S -0.0195(3) 0.8303(3) 0.3437(2) 0.0445(13) Uani 1 1 d . . . C214 C 0.0771(12) 0.8894(12) 0.3356(7) 0.039(5) Uiso 1 1 d . . . H214 H 0.0669 0.9536 0.3369 0.046 Uiso 1 1 calc R . . C215 C 0.1723(12) 0.8320(11) 0.3268(7) 0.025(4) Uiso 1 1 d . . . N221 N 0.4004(9) 0.6095(8) 0.3618(6) 0.030(3) Uani 1 1 d . . . C222 C 0.4100(13) 0.6096(11) 0.4220(8) 0.039(5) Uiso 1 1 d . . . C223 C 0.3186(13) 0.6030(11) 0.4648(7) 0.034(4) Uiso 1 1 d . . . N224 N 0.2356(9) 0.5970(9) 0.4398(5) 0.027(3) Uani 1 1 d . . . C225 C 0.1496(14) 0.5901(11) 0.4777(8) 0.044(5) Uiso 1 1 d . . . H225 H 0.0906 0.5856 0.4603 0.053 Uiso 1 1 calc R . . C226 C 0.1432(14) 0.5892(12) 0.5425(8) 0.049(5) Uiso 1 1 d . . . H226 H 0.0813 0.5829 0.5686 0.058 Uiso 1 1 calc R . . C227 C 0.2291(13) 0.5977(12) 0.5681(9) 0.049(5) Uiso 1 1 d . . . H227 H 0.2261 0.5992 0.6117 0.059 Uiso 1 1 calc R . . C228 C 0.3194(12) 0.6041(11) 0.5281(7) 0.033(4) Uiso 1 1 d . . . C229 C 0.4138(13) 0.6103(11) 0.5488(8) 0.045(5) Uiso 1 1 d . . . H229 H 0.4176 0.6063 0.5922 0.054 Uiso 1 1 calc R . . C230 C 0.4967(13) 0.6215(11) 0.5077(8) 0.042(5) Uiso 1 1 d . . . H230 H 0.5551 0.6310 0.5234 0.050 Uiso 1 1 calc R . . C231 C 0.5028(13) 0.6202(11) 0.4414(8) 0.038(5) Uiso 1 1 d . . . C232 C 0.5842(14) 0.6258(12) 0.3959(8) 0.050(5) Uiso 1 1 d . . . H232 H 0.6477 0.6311 0.4073 0.059 Uiso 1 1 calc R . . C233 C 0.5764(12) 0.6240(10) 0.3344(7) 0.030(4) Uiso 1 1 d . . . H233 H 0.6333 0.6300 0.3035 0.037 Uiso 1 1 calc R . . C234 C 0.4831(12) 0.6132(10) 0.3173(7) 0.028(4) Uiso 1 1 d . . . N241 N 0.3074(9) 0.4561(9) 0.3271(6) 0.033(4) Uani 1 1 d . . . C242 C 0.2221(12) 0.4246(10) 0.3202(7) 0.029(4) Uiso 1 1 d . . . C243 C 0.1284(11) 0.4912(10) 0.3214(7) 0.025(4) Uiso 1 1 d . . . N244 N 0.1336(9) 0.5760(8) 0.3282(5) 0.023(3) Uiso 1 1 d . . . C245 C 0.0494(11) 0.6431(10) 0.3299(6) 0.022(4) Uiso 1 1 d . . . C246 C -0.0441(13) 0.6195(12) 0.3217(7) 0.040(5) Uiso 1 1 d . . . H246 H -0.1047 0.6658 0.3214 0.048 Uiso 1 1 calc R . . C247 C -0.0491(13) 0.5348(11) 0.3143(7) 0.042(5) Uiso 1 1 d . . . H247 H -0.1131 0.5225 0.3087 0.051 Uiso 1 1 calc R . . C248 C 0.0390(13) 0.4615(11) 0.3146(7) 0.038(5) Uiso 1 1 d . . . C249 C 0.0390(14) 0.3726(11) 0.3078(7) 0.043(5) Uiso 1 1 d . . . H249 H -0.0232 0.3559 0.3031 0.052 Uiso 1 1 calc R . . C250 C 0.1275(13) 0.3078(12) 0.3077(8) 0.047(5) Uiso 1 1 d . . . H250 H 0.1267 0.2463 0.3031 0.056 Uiso 1 1 calc R . . C251 C 0.2217(12) 0.3326(11) 0.3145(7) 0.035(4) Uiso 1 1 d . . . C252 C 0.3162(14) 0.2716(13) 0.3127(8) 0.050(5) Uiso 1 1 d . . . H252 H 0.3212 0.2095 0.3071 0.060 Uiso 1 1 calc R . . C253 C 0.4019(15) 0.3030(13) 0.3192(8) 0.057(6) Uiso 1 1 d . . . H253 H 0.4664 0.2619 0.3203 0.068 Uiso 1 1 calc R . . C254 C 0.3939(13) 0.3944(11) 0.3242(7) 0.033(4) Uiso 1 1 d . . . H254 H 0.4554 0.4147 0.3257 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.7281(3) 0.3992(4) 0.2557(2) 0.0492(13) Uani 1 1 d . . . O1 O 0.6312(9) 0.3870(11) 0.2865(6) 0.080(5) Uani 1 1 d . . . O2 O 0.8048(10) 0.3319(11) 0.2860(6) 0.081(5) Uani 1 1 d . . . O3 O 0.7425(11) 0.4888(10) 0.2637(7) 0.084(5) Uani 1 1 d . . . O4 O 0.7391(11) 0.3912(11) 0.1910(6) 0.081(5) Uani 1 1 d . . . Cl2 Cl 0.5622(3) 0.0854(3) 0.2502(2) 0.0446(13) Uani 1 1 d . . . O5 O 0.4767(11) 0.1200(14) 0.2162(7) 0.117(7) Uani 1 1 d . . . O6 O 0.6173(11) -0.0018(9) 0.2330(7) 0.082(5) Uani 1 1 d . . . O7 O 0.6319(10) 0.1467(9) 0.2353(7) 0.075(4) Uani 1 1 d . . . O8 O 0.5241(11) 0.0763(9) 0.3152(6) 0.072(4) Uani 1 1 d . . . Cl3 Cl 0.0995(4) 0.1795(4) 0.9950(2) 0.0506(14) Uani 1 1 d . . . O9 O 0.1888(9) 0.1468(10) 1.0240(6) 0.067(4) Uani 1 1 d . . . O10 O 0.0270(11) 0.1263(11) 1.0235(9) 0.107(6) Uani 1 1 d . . . O11 O 0.0607(13) 0.2728(11) 1.0042(8) 0.107(6) Uani 1 1 d . . . O12 O 0.1279(13) 0.1742(14) 0.9297(7) 0.124(7) Uani 1 1 d . . . Cl4 Cl 0.1806(4) 0.3278(4) 0.4992(2) 0.0521(14) Uani 1 1 d . . . O13 O 0.0980(12) 0.3882(12) 0.4691(9) 0.121(7) Uani 1 1 d . . . O14 O 0.2649(14) 0.3607(16) 0.4763(12) 0.173(11) Uani 1 1 d . . . O15 O 0.2026(18) 0.2384(15) 0.4814(13) 0.183(11) Uani 1 1 d . . . O16A O 0.192(2) 0.3292(19) 0.5635(13) 0.096(9) Uiso 0.60 1 d P . . O16B O 0.120(4) 0.292(3) 0.553(2) 0.122(16) Uiso 0.40 1 d P . . N1 N 0.3332(16) 0.4146(13) 0.1661(9) 0.087(6) Uiso 1 1 d . . . C2 C 0.416(2) 0.3892(16) 0.1550(11) 0.081(7) Uiso 1 1 d . . . C3 C 0.528(2) 0.3528(18) 0.1447(12) 0.104(9) Uiso 1 1 d . . . N4 N 0.255(2) 0.2433(19) 0.7416(13) 0.152(10) Uiso 1 1 d . . . C5 C 0.2751(19) 0.1854(17) 0.6983(12) 0.091(8) Uiso 1 1 d . . . C6 C 0.299(2) 0.127(2) 0.6321(13) 0.121(10) Uiso 1 1 d . . . N7 N 0.1978(16) 0.8296(13) 0.4826(9) 0.084(6) Uiso 1 1 d . . . C8 C 0.114(2) 0.8388(16) 0.5001(11) 0.082(7) Uiso 1 1 d . . . C9 C 0.002(2) 0.848(2) 0.5299(14) 0.130(11) Uiso 1 1 d . . . N10 N 0.869(2) 0.031(2) 0.3778(13) 0.152(10) Uiso 1 1 d . . . C11 C 0.807(2) 0.092(2) 0.3743(13) 0.104(9) Uiso 1 1 d . . . C12 C 0.713(2) 0.166(2) 0.3778(13) 0.124(10) Uiso 1 1 d . . . N13 N 0.3338(17) 0.6804(14) 1.0139(10) 0.106(7) Uiso 1 1 d . . . C14 C 0.263(2) 0.6746(16) 0.9875(11) 0.088(8) Uiso 1 1 d . . . C15 C 0.190(2) 0.6765(18) 0.9464(12) 0.101(8) Uiso 1 1 d . . . N16 N -0.016(2) 0.529(2) 0.8591(14) 0.168(11) Uiso 1 1 d . . . C17 C 0.076(3) 0.478(2) 0.8539(16) 0.149(12) Uiso 1 1 d . . . C18 C 0.1744(19) 0.3969(16) 0.8580(11) 0.087(7) Uiso 1 1 d . . . N19 N 0.1710(19) 0.0740(16) 0.3398(12) 0.122(8) Uiso 1 1 d . . . C20 C 0.219(2) 0.0632(19) 0.3795(14) 0.106(9) Uiso 1 1 d . . . C21 C 0.286(3) 0.049(3) 0.4274(19) 0.185(15) Uiso 1 1 d . . . N22 N 0.647(3) 0.590(2) 1.0335(15) 0.179(12) Uiso 1 1 d D . . C23 C 0.713(3) 0.604(3) 0.991(2) 0.22(2) Uiso 1 1 d D . . C24 C 0.829(3) 0.566(3) 0.966(2) 0.25(2) Uiso 1 1 d D . . O17 O 0.4991(18) 0.8652(16) 0.4586(11) 0.173(9) Uiso 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 0.0154(12) 0.0452(14) 0.0287(12) -0.0024(10) -0.0027(9) -0.0054(10) N101 0.024(8) 0.050(10) 0.028(8) -0.010(7) -0.003(6) -0.006(7) S103 0.027(3) 0.056(3) 0.059(3) -0.002(3) -0.013(2) -0.014(2) N111 0.019(8) 0.030(8) 0.027(8) 0.003(7) -0.004(6) -0.012(6) S113 0.024(3) 0.062(3) 0.035(3) -0.001(2) -0.012(2) -0.011(2) N121 0.013(8) 0.053(9) 0.024(8) -0.011(7) 0.009(6) -0.014(7) N124 0.004(7) 0.048(9) 0.028(8) 0.009(7) -0.001(6) -0.004(6) N141 0.017(8) 0.046(9) 0.021(7) -0.007(7) -0.001(6) -0.001(7) N144 0.004(7) 0.048(9) 0.029(8) -0.010(7) -0.001(6) -0.001(7) Cu2 0.0143(12) 0.0455(14) 0.0338(12) -0.0047(11) -0.0034(9) -0.0032(10) N201 0.018(8) 0.036(8) 0.036(8) -0.010(7) 0.002(6) -0.004(6) S203 0.021(3) 0.072(4) 0.049(3) -0.004(3) 0.002(2) -0.006(2) N211 0.005(7) 0.066(10) 0.023(7) -0.002(7) 0.003(6) -0.015(7) S213 0.021(3) 0.054(3) 0.051(3) -0.003(3) -0.001(2) 0.005(2) N221 0.013(8) 0.036(8) 0.036(8) 0.012(7) -0.012(6) 0.003(6) N224 0.018(8) 0.049(9) 0.019(7) -0.010(7) -0.002(6) -0.013(7) N241 0.012(8) 0.056(10) 0.033(8) -0.010(7) -0.001(6) -0.008(7) Cl1 0.028(3) 0.067(4) 0.054(3) -0.023(3) -0.008(2) 0.001(3) O1 0.027(8) 0.135(14) 0.077(10) -0.007(10) 0.015(7) -0.036(8) O2 0.044(9) 0.124(13) 0.074(10) -0.044(10) -0.022(8) 0.017(9) O3 0.087(12) 0.082(11) 0.088(11) -0.039(10) -0.007(9) -0.007(9) O4 0.073(11) 0.128(13) 0.055(9) -0.055(9) 0.001(8) -0.024(9) Cl2 0.034(3) 0.061(3) 0.042(3) -0.015(3) -0.002(2) -0.012(3) O5 0.050(11) 0.24(2) 0.073(11) -0.035(12) -0.029(9) -0.022(12) O6 0.089(12) 0.067(10) 0.087(11) -0.044(9) 0.044(9) -0.023(9) O7 0.065(10) 0.058(9) 0.111(12) -0.022(9) 0.002(9) -0.035(8) O8 0.078(11) 0.081(11) 0.050(9) -0.010(8) 0.008(8) -0.007(8) Cl3 0.032(3) 0.067(4) 0.054(3) -0.011(3) -0.007(3) -0.011(3) O9 0.032(8) 0.117(12) 0.051(8) -0.002(8) -0.008(7) -0.016(8) O10 0.047(10) 0.101(13) 0.177(18) 0.004(12) -0.025(11) -0.031(10) O11 0.103(14) 0.070(11) 0.139(15) -0.046(11) 0.023(11) -0.002(10) O12 0.108(14) 0.186(19) 0.063(11) -0.060(12) -0.025(10) 0.045(13) Cl4 0.042(3) 0.075(4) 0.041(3) 0.000(3) 0.000(2) -0.023(3) O13 0.052(11) 0.129(15) 0.192(19) -0.043(14) -0.065(12) 0.011(10) O14 0.057(13) 0.20(2) 0.26(3) 0.06(2) -0.068(15) -0.056(14) O15 0.17(2) 0.121(18) 0.28(3) -0.10(2) -0.05(2) -0.002(16) _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 N121 1.972(11) . ? Cu1 N144 1.987(11) . ? Cu1 N124 2.111(12) . ? Cu1 N141 2.138(13) . ? Cu1 N111 2.226(12) . ? Cu1 N101 2.311(13) . ? N101 C102 1.325(19) . ? N101 C105 1.370(19) . ? C102 C145 1.48(2) . ? C102 S103 1.697(16) . ? S103 C104 1.673(18) . ? C104 C105 1.37(2) . ? C105 C205 1.53(2) . ? N111 C112 1.330(18) . ? N111 C115 1.351(19) . ? C112 C134 1.47(2) . ? C112 S113 1.720(15) . ? S113 C114 1.700(17) . ? C114 C115 1.38(2) . ? C115 C215 1.44(2) . ? N121 C134 1.345(18) . ? N121 C122 1.353(19) . ? C122 C131 1.40(2) . ? C122 C123 1.42(2) . ? C123 N124 1.352(18) . ? C123 C128 1.39(2) . ? N124 C125 1.331(19) . ? C125 C126 1.41(2) . ? C126 C127 1.40(2) . ? C127 C128 1.41(2) . ? C128 C129 1.45(2) . ? C129 C130 1.36(2) . ? C130 C131 1.43(2) . ? C131 C132 1.43(2) . ? C132 C133 1.37(2) . ? C133 C134 1.41(2) . ? N141 C142 1.356(19) . ? N141 C154 1.37(2) . ? C142 C143 1.42(2) . ? C142 C151 1.43(2) . ? C143 N144 1.339(19) . ? C143 C148 1.42(2) . ? N144 C145 1.315(18) . ? C145 C146 1.43(2) . ? C146 C147 1.33(2) . ? C147 C148 1.39(2) . ? C148 C149 1.45(2) . ? C149 C150 1.31(2) . ? C150 C151 1.47(2) . ? C151 C152 1.38(2) . ? C152 C153 1.39(2) . ? C153 C154 1.40(2) . ? Cu2 N244 1.965(12) . ? Cu2 N221 1.968(12) . ? Cu2 N241 2.129(14) . ? Cu2 N224 2.148(11) . ? Cu2 N201 2.258(12) . ? Cu2 N211 2.299(13) . ? N201 C202 1.292(19) . ? N201 C205 1.37(2) . ? C202 C234 1.46(2) . ? C202 S203 1.707(17) . ? S203 C204 1.712(18) . ? C204 C205 1.34(2) . ? N211 C212 1.297(18) . ? N211 C215 1.398(19) . ? C212 C245 1.41(2) . ? C212 S213 1.743(16) . ? S213 C214 1.703(17) . ? C214 C215 1.39(2) . ? N221 C222 1.34(2) . ? N221 C234 1.368(19) . ? C222 C231 1.43(2) . ? C222 C223 1.44(2) . ? C223 N224 1.342(19) . ? C223 C228 1.39(2) . ? N224 C225 1.33(2) . ? C225 C226 1.40(2) . ? C226 C227 1.40(2) . ? C227 C228 1.40(2) . ? C228 C229 1.44(2) . ? C229 C230 1.35(2) . ? C230 C231 1.44(2) . ? C231 C232 1.37(2) . ? C232 C233 1.37(2) . ? C233 C234 1.41(2) . ? N241 C254 1.320(19) . ? N241 C242 1.373(19) . ? C242 C251 1.41(2) . ? C242 C243 1.43(2) . ? C243 N244 1.328(17) . ? C243 C248 1.41(2) . ? N244 C245 1.342(17) . ? C245 C246 1.42(2) . ? C246 C247 1.33(2) . ? C247 C248 1.43(2) . ? C248 C249 1.37(2) . ? C249 C250 1.36(2) . ? C250 C251 1.43(2) . ? C251 C252 1.39(2) . ? C252 C253 1.37(2) . ? C253 C254 1.38(2) . ? Cl1 O1 1.410(12) . ? Cl1 O4 1.422(13) . ? Cl1 O2 1.436(14) . ? Cl1 O3 1.444(15) . ? Cl2 O5 1.421(14) . ? Cl2 O7 1.425(12) . ? Cl2 O8 1.431(13) . ? Cl2 O6 1.436(14) . ? Cl3 O9 1.400(12) . ? Cl3 O10 1.407(15) . ? Cl3 O11 1.422(15) . ? Cl3 O12 1.429(15) . ? Cl4 O14 1.333(18) . ? Cl4 O15 1.42(2) . ? Cl4 O16B 1.43(5) . ? Cl4 O16A 1.44(3) . ? Cl4 O13 1.444(15) . ? O16A O16B 1.28(5) . ? N1 C2 1.10(3) . ? C2 C3 1.49(3) . ? N4 C5 1.35(3) . ? C5 C6 1.77(4) . ? N7 C8 1.12(3) . ? C8 C9 1.53(4) . ? N10 C11 1.09(3) . ? C11 C12 1.49(4) . ? N13 C14 1.22(3) . ? C14 C15 1.42(3) . ? N16 C17 1.30(4) . ? C17 C18 1.60(4) . ? N19 C20 1.13(3) . ? C20 C21 1.45(4) . ? N22 C23 1.208(19) . ? C23 C24 1.60(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 N121 Cu1 N144 173.9(5) . . ? N121 Cu1 N124 79.3(5) . . ? N144 Cu1 N124 95.6(5) . . ? N121 Cu1 N141 98.7(5) . . ? N144 Cu1 N141 79.2(5) . . ? N124 Cu1 N141 102.1(5) . . ? N121 Cu1 N111 76.3(5) . . ? N144 Cu1 N111 109.3(5) . . ? N124 Cu1 N111 154.1(4) . . ? N141 Cu1 N111 90.0(4) . . ? N121 Cu1 N101 108.7(5) . . ? N144 Cu1 N101 74.3(5) . . ? N124 Cu1 N101 91.1(5) . . ? N141 Cu1 N101 151.4(4) . . ? N111 Cu1 N101 88.8(4) . . ? C102 N101 C105 108.6(13) . . ? C102 N101 Cu1 108.7(10) . . ? C105 N101 Cu1 140.3(10) . . ? N101 C102 C145 116.6(14) . . ? N101 C102 S103 115.5(12) . . ? C145 C102 S103 127.6(12) . . ? C104 S103 C102 89.9(9) . . ? C105 C104 S103 110.5(14) . . ? C104 C105 N101 115.5(15) . . ? C104 C105 C205 128.2(15) . . ? N101 C105 C205 115.6(14) . . ? C112 N111 C115 110.0(12) . . ? C112 N111 Cu1 109.6(9) . . ? C115 N111 Cu1 139.4(10) . . ? N111 C112 C134 118.2(13) . . ? N111 C112 S113 115.3(11) . . ? C134 C112 S113 126.3(12) . . ? C114 S113 C112 88.6(8) . . ? C115 C114 S113 111.0(13) . . ? N111 C115 C114 115.1(15) . . ? N111 C115 C215 117.0(14) . . ? C114 C115 C215 127.2(15) . . ? C134 N121 C122 120.8(13) . . ? C134 N121 Cu1 122.0(10) . . ? C122 N121 Cu1 117.1(10) . . ? N121 C122 C131 121.8(14) . . ? N121 C122 C123 115.3(14) . . ? C131 C122 C123 122.7(15) . . ? N124 C123 C128 124.9(14) . . ? N124 C123 C122 116.6(14) . . ? C128 C123 C122 118.5(15) . . ? C125 N124 C123 116.6(13) . . ? C125 N124 Cu1 131.7(10) . . ? C123 N124 Cu1 111.7(9) . . ? N124 C125 C126 123.0(16) . . ? C127 C126 C125 120.2(17) . . ? C126 C127 C128 116.9(17) . . ? C123 C128 C127 118.5(16) . . ? C123 C128 C129 118.9(15) . . ? C127 C128 C129 122.7(16) . . ? C130 C129 C128 121.4(16) . . ? C129 C130 C131 120.6(16) . . ? C122 C131 C132 117.6(15) . . ? C122 C131 C130 117.7(15) . . ? C132 C131 C130 124.5(15) . . ? C133 C132 C131 118.8(16) . . ? C132 C133 C134 120.8(15) . . ? N121 C134 C133 119.9(14) . . ? N121 C134 C112 111.6(13) . . ? C133 C134 C112 128.2(14) . . ? C142 N141 C154 116.0(14) . . ? C142 N141 Cu1 111.0(10) . . ? C154 N141 Cu1 132.8(11) . . ? N141 C142 C143 116.2(14) . . ? N141 C142 C151 123.0(15) . . ? C143 C142 C151 120.8(15) . . ? N144 C143 C142 117.3(14) . . ? N144 C143 C148 122.2(14) . . ? C142 C143 C148 120.5(15) . . ? C145 N144 C143 120.6(13) . . ? C145 N144 Cu1 123.2(11) . . ? C143 N144 Cu1 116.2(10) . . ? N144 C145 C146 120.2(14) . . ? N144 C145 C102 113.5(14) . . ? C146 C145 C102 126.2(14) . . ? C147 C146 C145 119.0(15) . . ? C146 C147 C148 122.1(16) . . ? C147 C148 C143 115.9(15) . . ? C147 C148 C149 127.5(15) . . ? C143 C148 C149 116.6(15) . . ? C150 C149 C148 124.1(18) . . ? C149 C150 C151 120.5(17) . . ? C152 C151 C142 120.2(16) . . ? C152 C151 C150 122.5(16) . . ? C142 C151 C150 117.3(15) . . ? C151 C152 C153 117.1(18) . . ? C152 C153 C154 120.8(18) . . ? N141 C154 C153 122.9(17) . . ? N244 Cu2 N221 173.6(5) . . ? N244 Cu2 N241 79.5(5) . . ? N221 Cu2 N241 98.2(5) . . ? N244 Cu2 N224 96.3(5) . . ? N221 Cu2 N224 78.4(5) . . ? N241 Cu2 N224 105.3(5) . . ? N244 Cu2 N201 110.7(5) . . ? N221 Cu2 N201 75.2(5) . . ? N241 Cu2 N201 88.8(5) . . ? N224 Cu2 N201 151.6(5) . . ? N244 Cu2 N211 74.7(5) . . ? N221 Cu2 N211 108.6(5) . . ? N241 Cu2 N211 151.6(5) . . ? N224 Cu2 N211 89.3(4) . . ? N201 Cu2 N211 89.3(4) . . ? C202 N201 C205 109.6(13) . . ? C202 N201 Cu2 111.0(10) . . ? C205 N201 Cu2 137.6(11) . . ? N201 C202 C234 117.7(14) . . ? N201 C202 S203 115.8(12) . . ? C234 C202 S203 126.5(13) . . ? C202 S203 C204 88.7(9) . . ? C205 C204 S203 109.7(14) . . ? C204 C205 N201 116.0(16) . . ? C204 C205 C105 127.3(16) . . ? N201 C205 C105 115.7(14) . . ? C212 N211 C215 112.9(13) . . ? C212 N211 Cu2 107.5(10) . . ? C215 N211 Cu2 137.9(9) . . ? N211 C212 C245 120.4(14) . . ? N211 C212 S213 113.5(12) . . ? C245 C212 S213 126.1(12) . . ? C214 S213 C212 89.7(8) . . ? C215 C214 S213 111.4(13) . . ? C214 C215 N211 112.3(14) . . ? C214 C215 C115 130.5(15) . . ? N211 C215 C115 116.5(13) . . ? C222 N221 C234 120.1(13) . . ? C222 N221 Cu2 118.5(11) . . ? C234 N221 Cu2 121.4(10) . . ? N221 C222 C231 122.1(15) . . ? N221 C222 C223 115.1(15) . . ? C231 C222 C223 122.8(16) . . ? N224 C223 C228 123.6(15) . . ? N224 C223 C222 116.5(14) . . ? C228 C223 C222 120.0(16) . . ? C225 N224 C223 118.5(14) . . ? C225 N224 Cu2 129.9(11) . . ? C223 N224 Cu2 111.6(10) . . ? N224 C225 C226 122.1(17) . . ? C227 C226 C225 119.2(18) . . ? C228 C227 C226 118.3(17) . . ? C223 C228 C227 118.3(16) . . ? C223 C228 C229 117.9(15) . . ? C227 C228 C229 123.8(16) . . ? C230 C229 C228 121.2(17) . . ? C229 C230 C231 124.3(17) . . ? C232 C231 C222 116.8(16) . . ? C232 C231 C230 129.5(17) . . ? C222 C231 C230 113.7(15) . . ? C233 C232 C231 121.9(17) . . ? C232 C233 C234 119.4(15) . . ? N221 C234 C233 119.5(14) . . ? N221 C234 C202 112.3(14) . . ? C233 C234 C202 127.2(14) . . ? C254 N241 C242 114.9(14) . . ? C254 N241 Cu2 134.4(11) . . ? C242 N241 Cu2 110.7(10) . . ? N241 C242 C251 124.5(14) . . ? N241 C242 C243 115.6(14) . . ? C251 C242 C243 119.9(14) . . ? N244 C243 C248 125.8(14) . . ? N244 C243 C242 116.9(14) . . ? C248 C243 C242 117.3(14) . . ? C243 N244 C245 121.1(13) . . ? C243 N244 Cu2 117.2(10) . . ? C245 N244 Cu2 121.6(10) . . ? N244 C245 C212 113.1(13) . . ? N244 C245 C246 116.8(14) . . ? C212 C245 C246 129.6(14) . . ? C247 C246 C245 122.0(16) . . ? C246 C247 C248 122.1(17) . . ? C249 C248 C243 122.7(16) . . ? C249 C248 C247 125.1(16) . . ? C243 C248 C247 112.2(15) . . ? C250 C249 C248 120.6(17) . . ? C249 C250 C251 119.9(17) . . ? C252 C251 C242 116.8(16) . . ? C252 C251 C250 123.7(16) . . ? C242 C251 C250 119.4(15) . . ? C253 C252 C251 118.9(18) . . ? C252 C253 C254 119.6(18) . . ? N241 C254 C253 125.1(17) . . ? O1 Cl1 O4 112.6(9) . . ? O1 Cl1 O2 107.9(9) . . ? O4 Cl1 O2 110.4(9) . . ? O1 Cl1 O3 108.7(9) . . ? O4 Cl1 O3 109.7(9) . . ? O2 Cl1 O3 107.5(9) . . ? O5 Cl2 O7 109.4(10) . . ? O5 Cl2 O8 107.6(9) . . ? O7 Cl2 O8 111.7(9) . . ? O5 Cl2 O6 111.1(11) . . ? O7 Cl2 O6 106.8(8) . . ? O8 Cl2 O6 110.2(8) . . ? O9 Cl3 O10 107.8(9) . . ? O9 Cl3 O11 109.0(10) . . ? O10 Cl3 O11 109.3(10) . . ? O9 Cl3 O12 107.0(9) . . ? O10 Cl3 O12 114.2(13) . . ? O11 Cl3 O12 109.4(11) . . ? O14 Cl4 O15 103.8(16) . . ? O14 Cl4 O16B 147(2) . . ? O15 Cl4 O16B 87(2) . . ? O14 Cl4 O16A 94.7(16) . . ? O15 Cl4 O16A 113.9(16) . . ? O16B Cl4 O16A 53(2) . . ? O14 Cl4 O13 106.0(12) . . ? O15 Cl4 O13 112.5(13) . . ? O16B Cl4 O13 98(2) . . ? O16A Cl4 O13 122.0(14) . . ? O16B O16A Cl4 63(3) . . ? O16A O16B Cl4 64(3) . . ? N1 C2 C3 176(3) . . ? N4 C5 C6 170(2) . . ? N7 C8 C9 175(3) . . ? N10 C11 C12 170(3) . . ? N13 C14 C15 169(3) . . ? N16 C17 C18 166(3) . . ? N19 C20 C21 176(4) . . ? N22 C23 C24 142(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.229 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.128 #=END data_jolly _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 N4 S2' _chemical_formula_weight 322.40 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.882(5) _cell_length_b 9.871(4) _cell_length_c 24.086(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2825(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.377 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details 0.85 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11085 _diffrn_reflns_av_R_equivalents 0.1817 _diffrn_reflns_av_sigmaI/netI 0.1061 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 22.49 _reflns_number_total 1851 _reflns_number_gt 1171 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1851 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1360 _refine_ls_R_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.2307 _refine_ls_wR_factor_gt 0.2110 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 S2 S 0.48445(17) 1.0493(2) 0.61842(8) 0.0293(7) Uani 1 1 d . . . S1 S 0.14214(17) 0.6875(2) 0.76695(8) 0.0297(7) Uani 1 1 d . . . N1 N 0.2447(5) 0.4922(6) 0.8433(2) 0.0253(16) Uani 1 1 d . . . N2 N 0.3490(6) 0.7420(6) 0.7463(2) 0.0255(16) Uani 1 1 d . . . N3 N 0.2761(5) 0.9999(6) 0.6413(2) 0.0257(16) Uani 1 1 d . . . N4 N 0.3795(6) 1.2360(7) 0.5389(3) 0.0327(18) Uani 1 1 d . . . C1 C 0.3248(6) 0.5668(7) 0.8187(3) 0.0224(18) Uani 1 1 d . . . C2 C 0.2777(7) 0.4028(8) 0.8819(3) 0.030(2) Uani 1 1 d . . . H2 H 0.2222 0.3484 0.8995 0.036 Uiso 1 1 calc R . . C3 C 0.3900(7) 0.3866(8) 0.8973(3) 0.0268(19) Uani 1 1 d . . . H3 H 0.4104 0.3218 0.9247 0.032 Uiso 1 1 calc R . . C4 C 0.4705(7) 0.4653(8) 0.8725(3) 0.030(2) Uani 1 1 d . . . H4 H 0.5472 0.4574 0.8832 0.036 Uiso 1 1 calc R . . C5 C 0.4392(7) 0.5559(8) 0.8320(3) 0.028(2) Uani 1 1 d . . . H5 H 0.4938 0.6098 0.8134 0.033 Uiso 1 1 calc R . . C6 C 0.2850(6) 0.6637(7) 0.7770(3) 0.0234(18) Uani 1 1 d . . . C7 C 0.2858(6) 0.8221(8) 0.7121(3) 0.0229(19) Uani 1 1 d . . . C8 C 0.1707(6) 0.8065(8) 0.7190(3) 0.028(2) Uani 1 1 d . . . H8 H 0.1153 0.8565 0.6993 0.033 Uiso 1 1 calc R . . C9 C 0.3411(6) 0.9148(7) 0.6742(3) 0.0206(18) Uani 1 1 d . . . C10 C 0.4568(6) 0.9285(8) 0.6670(3) 0.0260(19) Uani 1 1 d . . . H10 H 0.5122 0.8778 0.6864 0.031 Uiso 1 1 calc R . . C11 C 0.3409(6) 1.0763(8) 0.6094(3) 0.0236(19) Uani 1 1 d . . . C12 C 0.2998(7) 1.1758(8) 0.5699(3) 0.0256(19) Uani 1 1 d . . . C13 C 0.3446(7) 1.3302(8) 0.5025(3) 0.034(2) Uani 1 1 d . . . H13 H 0.3994 1.3754 0.4806 0.041 Uiso 1 1 calc R . . C14 C 0.2316(7) 1.3647(8) 0.4953(3) 0.034(2) Uani 1 1 d . . . H14 H 0.2106 1.4321 0.4691 0.041 Uiso 1 1 calc R . . C15 C 0.1507(7) 1.2999(7) 0.5267(3) 0.032(2) Uani 1 1 d . . . H15 H 0.0732 1.3204 0.5221 0.039 Uiso 1 1 calc R . . C16 C 0.1850(7) 1.2049(7) 0.5650(3) 0.028(2) Uani 1 1 d . . . H16 H 0.1315 1.1598 0.5877 0.034 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 S2 0.0153(11) 0.0346(13) 0.0380(12) 0.0034(10) -0.0010(9) -0.0008(9) S1 0.0131(11) 0.0412(14) 0.0348(12) 0.0041(10) 0.0008(9) -0.0008(10) N1 0.020(4) 0.022(4) 0.034(4) 0.000(3) 0.001(3) -0.006(3) N2 0.018(4) 0.031(4) 0.028(3) -0.002(3) -0.002(3) -0.003(3) N3 0.023(4) 0.031(4) 0.023(3) -0.008(3) -0.005(3) 0.009(3) N4 0.028(4) 0.037(4) 0.033(4) 0.009(3) -0.001(4) -0.010(3) C1 0.018(5) 0.025(4) 0.024(4) -0.004(4) 0.002(4) -0.002(4) C2 0.016(4) 0.040(5) 0.033(4) 0.008(4) 0.005(4) -0.004(4) C3 0.025(5) 0.030(5) 0.025(4) 0.000(3) 0.005(4) 0.008(4) C4 0.018(5) 0.049(6) 0.024(4) -0.003(4) 0.001(4) 0.013(4) C5 0.017(4) 0.036(5) 0.030(4) -0.010(4) 0.004(4) -0.004(4) C6 0.016(4) 0.021(4) 0.033(4) -0.007(4) -0.002(4) 0.001(3) C7 0.023(5) 0.026(4) 0.020(4) 0.001(4) -0.008(4) 0.003(4) C8 0.017(5) 0.034(5) 0.032(4) 0.002(4) -0.006(4) 0.006(4) C9 0.024(5) 0.014(4) 0.024(4) -0.004(3) -0.003(4) -0.001(3) C10 0.016(4) 0.032(5) 0.031(4) 0.001(4) -0.012(4) -0.001(4) C11 0.013(4) 0.030(5) 0.027(4) -0.007(4) 0.003(4) 0.004(4) C12 0.022(5) 0.027(5) 0.027(4) -0.004(4) -0.003(4) 0.001(4) C13 0.036(5) 0.029(5) 0.038(5) 0.008(4) 0.005(4) 0.000(4) C14 0.033(5) 0.029(5) 0.039(5) 0.010(4) -0.005(5) -0.004(4) C15 0.033(5) 0.030(5) 0.034(5) 0.005(4) -0.010(4) 0.000(4) C16 0.022(5) 0.027(5) 0.035(5) -0.004(4) -0.003(4) 0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S2 C10 1.704(8) . ? S2 C11 1.740(8) . ? S1 C8 1.682(8) . ? S1 C6 1.731(8) . ? N1 C2 1.341(9) . ? N1 C1 1.341(9) . ? N2 C6 1.314(9) . ? N2 C7 1.366(9) . ? N3 C11 1.323(9) . ? N3 C9 1.390(9) . ? N4 C13 1.344(9) . ? N4 C12 1.345(10) . ? C1 C5 1.401(11) . ? C1 C6 1.464(10) . ? C2 C3 1.394(11) . ? C3 C4 1.370(11) . ? C4 C5 1.375(10) . ? C7 C8 1.386(10) . ? C7 C9 1.450(10) . ? C9 C10 1.392(11) . ? C11 C12 1.452(10) . ? C12 C16 1.399(11) . ? C13 C14 1.396(11) . ? C14 C15 1.380(11) . ? C15 C16 1.376(10) . ? 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 C10 S2 C11 90.2(4) . . ? C8 S1 C6 89.6(4) . . ? C2 N1 C1 117.4(7) . . ? C6 N2 C7 111.2(7) . . ? C11 N3 C9 110.6(7) . . ? C13 N4 C12 116.8(7) . . ? N1 C1 C5 123.1(7) . . ? N1 C1 C6 115.6(7) . . ? C5 C1 C6 121.3(7) . . ? N1 C2 C3 122.7(7) . . ? C4 C3 C2 119.2(7) . . ? C3 C4 C5 119.3(8) . . ? C4 C5 C1 118.3(7) . . ? N2 C6 C1 125.7(7) . . ? N2 C6 S1 114.1(6) . . ? C1 C6 S1 120.1(6) . . ? N2 C7 C8 114.0(7) . . ? N2 C7 C9 119.7(7) . . ? C8 C7 C9 126.3(7) . . ? C7 C8 S1 111.0(6) . . ? N3 C9 C10 114.8(7) . . ? N3 C9 C7 119.3(7) . . ? C10 C9 C7 126.0(7) . . ? C9 C10 S2 110.1(6) . . ? N3 C11 C12 124.8(7) . . ? N3 C11 S2 114.3(6) . . ? C12 C11 S2 121.0(6) . . ? N4 C12 C16 123.2(7) . . ? N4 C12 C11 115.2(7) . . ? C16 C12 C11 121.5(7) . . ? N4 C13 C14 123.2(8) . . ? C15 C14 C13 119.2(8) . . ? C16 C15 C14 118.5(8) . . ? C15 C16 C12 119.0(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.923 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.139 #=END data_inxs0 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H42 Cl4 N16 O24 S6 Zn2' _chemical_formula_weight 1739.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 '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 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 13.329(3) _cell_length_b 23.158(3) _cell_length_c 22.379(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.357(19) _cell_angle_gamma 90.00 _cell_volume 6815.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.71 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)'_diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21828 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7794 _reflns_number_gt 5451 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1852P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7794 _refine_ls_number_parameters 515 _refine_ls_number_restraints 189 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2630 _refine_ls_wR_factor_gt 0.2483 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.006 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 Zn1 Zn 0.17463(4) 0.12490(2) 0.76521(2) 0.0388(2) Uani 1 1 d . . . N11 N 0.0975(3) 0.05139(15) 0.79998(17) 0.0374(8) Uani 1 1 d . . . C12 C 0.0279(4) 0.04257(19) 0.8386(2) 0.0411(11) Uani 1 1 d . . . C13 C 0.0164(5) -0.0136(2) 0.8544(3) 0.0541(14) Uani 1 1 d . . . H13 H -0.0283 -0.0266 0.8794 0.065 Uiso 1 1 calc R . . S14 S 0.09731(14) -0.05679(6) 0.82113(8) 0.0606(4) Uani 1 1 d . . . C15 C 0.1411(4) 0.00192(19) 0.7879(2) 0.0433(11) Uani 1 1 d . . . N21 N 0.2620(3) 0.05305(19) 0.7411(2) 0.0485(10) Uani 1 1 d . . . C22 C 0.2239(4) 0.0007(2) 0.7516(2) 0.0451(11) Uani 1 1 d . . . C23 C 0.2613(5) -0.0496(2) 0.7305(3) 0.0556(14) Uani 1 1 d . . . H23 H 0.2324 -0.0850 0.7373 0.067 Uiso 1 1 calc R . . C24 C 0.3415(5) -0.0466(3) 0.6993(3) 0.0686(18) Uani 1 1 d . . . H24 H 0.3679 -0.0799 0.6847 0.082 Uiso 1 1 calc R . . C25 C 0.3822(5) 0.0065(3) 0.6902(3) 0.0662(17) Uani 1 1 d . . . H25 H 0.4376 0.0093 0.6699 0.079 Uiso 1 1 calc R . . C26 C 0.3406(4) 0.0559(3) 0.7110(3) 0.0582(14) Uani 1 1 d . . . H26 H 0.3680 0.0917 0.7040 0.070 Uiso 1 1 calc R . . N31 N 0.0956(3) 0.19604(15) 0.80306(17) 0.0364(8) Uani 1 1 d . . . C32 C 0.1388(4) 0.2076(2) 0.8587(2) 0.0458(12) Uani 1 1 d . . . S33 S 0.10052(13) 0.27132(6) 0.88742(6) 0.0589(4) Uani 1 1 d . . . C34 C 0.0223(4) 0.2836(2) 0.8208(2) 0.0491(12) Uani 1 1 d . . . H34 H -0.0187 0.3160 0.8125 0.059 Uiso 1 1 calc R . . C35 C 0.0278(4) 0.23915(18) 0.7806(2) 0.0372(10) Uani 1 1 d . . . N41 N 0.2581(4) 0.13314(18) 0.8562(2) 0.0535(12) Uani 1 1 d . . . C42 C 0.2177(4) 0.1700(2) 0.8916(3) 0.0522(14) Uani 1 1 d . . . C43 C 0.2456(6) 0.1716(3) 0.9538(3) 0.074(2) Uani 1 1 d . . . H43 H 0.2148 0.1967 0.9777 0.089 Uiso 1 1 calc R . . C44 C 0.3224(7) 0.1336(3) 0.9793(3) 0.093(3) Uani 1 1 d . . . H44 H 0.3443 0.1340 1.0209 0.111 Uiso 1 1 calc R . . C45 C 0.3655(7) 0.0962(3) 0.9442(4) 0.097(3) Uani 1 1 d . . . H45 H 0.4159 0.0706 0.9612 0.117 Uiso 1 1 calc R . . C46 C 0.3319(5) 0.0973(3) 0.8816(3) 0.0685(19) Uani 1 1 d . . . H46 H 0.3616 0.0724 0.8569 0.082 Uiso 1 1 calc R . . N51 N -0.0935(3) 0.12585(14) 0.82697(17) 0.0348(8) Uani 1 1 d . . . C52 C -0.1291(4) 0.1649(2) 0.8602(2) 0.0425(11) Uani 1 1 d . . . S53 S -0.08339(16) 0.16186(7) 0.93615(6) 0.0679(5) Uani 1 1 d . . . C54 C -0.0077(6) 0.1050(2) 0.9230(2) 0.0592(16) Uani 1 1 d . . . H54 H 0.0378 0.0862 0.9526 0.071 Uiso 1 1 calc R . . C55 C -0.0239(4) 0.09105(19) 0.8626(2) 0.0399(10) Uani 1 1 d . . . N61 N -0.2504(3) 0.19412(18) 0.7775(2) 0.0474(10) Uani 1 1 d . . . C62 C -0.2076(4) 0.2061(2) 0.8334(3) 0.0464(12) Uani 1 1 d . . . C63 C -0.2320(6) 0.2545(2) 0.8647(3) 0.0671(18) Uani 1 1 d . . . H63 H -0.1990 0.2625 0.9037 0.081 Uiso 1 1 calc R . . C64 C -0.3079(6) 0.2905(3) 0.8351(4) 0.079(2) Uani 1 1 d . . . H64 H -0.3290 0.3223 0.8552 0.094 Uiso 1 1 calc R . . C65 C -0.3514(5) 0.2793(3) 0.7768(4) 0.072(2) Uani 1 1 d . . . H65 H -0.4005 0.3039 0.7564 0.086 Uiso 1 1 calc R . . C66 C -0.3211(5) 0.2305(3) 0.7482(4) 0.0640(16) Uani 1 1 d . . . H66 H -0.3500 0.2228 0.7083 0.077 Uiso 1 1 calc R . . Cl1 Cl 0.42147(10) 0.91525(6) 0.89749(6) 0.0510(3) Uani 1 1 d DU . . O11A O 0.371(2) 0.8989(10) 0.9422(12) 0.238(17) Uani 0.50 1 d PDU . . O11B O 0.436(2) 0.8664(8) 0.9291(10) 0.188(11) Uani 0.50 1 d PU . . O12 O 0.5219(5) 0.8959(3) 0.8975(3) 0.111(2) Uani 1 1 d DU . . O13A O 0.413(2) 0.9040(7) 0.8350(5) 0.177(10) Uani 0.50 1 d PDU . . O13B O 0.3545(11) 0.8824(7) 0.8622(16) 0.210(15) Uani 0.50 1 d PU . . O14A O 0.4087(9) 0.9729(4) 0.8837(7) 0.092(4) Uani 0.50 1 d PDU . . O14B O 0.4615(12) 0.9645(6) 0.9246(9) 0.135(6) Uani 0.50 1 d PU . . Cl2 Cl 0.89175(17) 0.84358(8) 0.90103(8) 0.0785(5) Uani 1 1 d DU . . O21 O 0.8652(6) 0.7930(3) 0.9265(5) 0.176(5) Uani 1 1 d DU . . O22 O 0.8969(15) 0.8443(5) 0.8441(4) 0.380(15) Uani 1 1 d DU . . O23 O 0.9940(8) 0.8549(5) 0.9295(6) 0.243(8) Uani 1 1 d DU . . O24 O 0.8441(10) 0.8925(4) 0.9183(5) 0.224(6) Uani 1 1 d DU . . O103 O 0.8095(7) 0.0235(5) 0.9097(4) 0.170(4) Uani 1 1 d DU . . O104 O 0.8696(15) 0.0050(8) 1.0031(6) 0.408(17) Uani 1 1 d DU . . O203 O 0.0135(9) 0.6743(6) 0.8536(5) 0.133(5) Uani 0.643(11) 1 d PDU . . O204 O 0.1440(7) 0.6397(3) 0.9109(4) 0.138(3) Uani 1 1 d DU . . O205 O 0.2186(16) 0.7026(10) 0.9889(8) 0.114(8) Uani 0.357(11) 1 d PU . . C101 C 0.7028(15) 0.0197(10) 0.9774(9) 0.245(13) Uani 1 1 d DU . . C201 C 0.0571(10) 0.7101(5) 0.9497(5) 0.123(4) Uani 1 1 d DU . . N102 N 0.8050(13) 0.0132(5) 0.9627(4) 0.212(9) Uani 1 1 d DU . . N202 N 0.0700(7) 0.6692(4) 0.8998(5) 0.077(3) Uani 0.643(11) 1 d PDU . . N206 N 0.149(2) 0.6845(8) 0.9548(10) 0.093(8) Uani 0.357(11) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0418(3) 0.0304(3) 0.0425(3) -0.0066(2) 0.0017(2) 0.0020(2) N11 0.045(2) 0.0276(18) 0.038(2) 0.0004(14) 0.0014(17) 0.0090(15) C12 0.057(3) 0.030(2) 0.034(2) 0.0026(17) -0.001(2) 0.0096(19) C13 0.081(4) 0.031(2) 0.052(3) 0.006(2) 0.017(3) 0.014(2) S14 0.0884(11) 0.0272(6) 0.0695(9) 0.0074(6) 0.0228(8) 0.0184(6) C15 0.059(3) 0.027(2) 0.042(2) -0.0031(18) 0.001(2) 0.011(2) N21 0.047(2) 0.044(2) 0.053(3) -0.0108(19) 0.004(2) 0.0099(18) C22 0.051(3) 0.038(2) 0.043(3) -0.008(2) -0.004(2) 0.013(2) C23 0.068(4) 0.041(3) 0.056(3) -0.009(2) 0.006(3) 0.014(2) C24 0.072(4) 0.069(4) 0.065(4) -0.019(3) 0.010(3) 0.028(3) C25 0.059(4) 0.071(4) 0.071(4) -0.017(3) 0.017(3) 0.016(3) C26 0.048(3) 0.064(4) 0.062(3) -0.007(3) 0.008(3) 0.005(3) N31 0.042(2) 0.0268(18) 0.039(2) -0.0042(14) 0.0018(16) 0.0015(15) C32 0.060(3) 0.031(2) 0.043(3) -0.0104(19) -0.003(2) 0.005(2) S33 0.0837(11) 0.0376(7) 0.0492(7) -0.0184(5) -0.0080(7) 0.0125(6) C34 0.063(3) 0.031(2) 0.052(3) -0.004(2) 0.004(2) 0.007(2) C35 0.044(2) 0.025(2) 0.042(2) -0.0007(17) 0.007(2) 0.0005(17) N41 0.055(3) 0.037(2) 0.059(3) -0.0131(19) -0.020(2) 0.0092(19) C42 0.062(3) 0.034(2) 0.051(3) -0.012(2) -0.017(2) 0.004(2) C43 0.110(6) 0.042(3) 0.057(3) -0.017(3) -0.025(4) 0.011(3) C44 0.136(7) 0.058(4) 0.061(4) -0.018(3) -0.050(5) 0.024(4) C45 0.121(7) 0.054(4) 0.089(5) -0.019(4) -0.067(5) 0.028(4) C46 0.071(4) 0.051(3) 0.070(4) -0.015(3) -0.028(3) 0.019(3) N51 0.045(2) 0.0235(17) 0.0371(19) 0.0056(13) 0.0109(16) 0.0039(14) C52 0.062(3) 0.030(2) 0.038(2) 0.0032(18) 0.016(2) 0.008(2) S53 0.1193(15) 0.0471(8) 0.0392(7) -0.0018(6) 0.0182(8) 0.0287(8) C54 0.100(5) 0.040(3) 0.038(3) 0.005(2) 0.010(3) 0.026(3) C55 0.054(3) 0.031(2) 0.034(2) 0.0101(17) 0.006(2) 0.006(2) N61 0.042(2) 0.037(2) 0.063(3) 0.0141(19) 0.010(2) 0.0079(17) C62 0.054(3) 0.029(2) 0.060(3) 0.011(2) 0.022(3) 0.008(2) C63 0.094(5) 0.039(3) 0.077(4) 0.005(3) 0.041(4) 0.022(3) C64 0.088(5) 0.051(4) 0.107(6) 0.022(4) 0.044(5) 0.032(3) C65 0.060(4) 0.049(3) 0.111(6) 0.029(4) 0.028(4) 0.024(3) C66 0.050(3) 0.053(3) 0.088(4) 0.023(3) 0.007(3) 0.008(3) Cl1 0.0546(7) 0.0446(7) 0.0557(7) 0.0058(5) 0.0143(6) 0.0139(5) O11A 0.37(4) 0.20(2) 0.21(2) 0.066(18) 0.25(3) 0.10(2) O11B 0.31(3) 0.113(14) 0.120(14) 0.039(11) -0.041(17) -0.065(17) O12 0.098(5) 0.110(5) 0.119(5) -0.005(4) -0.003(4) 0.032(4) O13A 0.36(3) 0.108(12) 0.058(7) 0.011(7) 0.011(11) 0.136(16) O13B 0.058(8) 0.086(10) 0.44(4) 0.026(16) -0.086(15) -0.025(7) O14A 0.074(7) 0.035(5) 0.159(12) 0.002(6) -0.007(7) 0.027(4) O14B 0.118(12) 0.082(9) 0.191(17) -0.061(10) -0.014(11) 0.015(8) Cl2 0.1103(15) 0.0634(10) 0.0552(9) 0.0133(7) -0.0059(9) -0.0060(9) O21 0.139(7) 0.081(5) 0.325(14) 0.067(6) 0.090(8) 0.013(4) O22 0.86(5) 0.139(10) 0.125(9) -0.049(8) 0.030(16) 0.068(17) O23 0.248(14) 0.144(9) 0.286(16) -0.031(9) -0.111(13) 0.008(9) O24 0.307(15) 0.123(7) 0.283(14) 0.086(8) 0.171(12) 0.112(9) O103 0.165(9) 0.203(11) 0.140(8) -0.002(7) 0.022(7) -0.013(7) O104 0.65(4) 0.274(18) 0.194(14) 0.074(13) -0.26(2) -0.08(2) O203 0.102(8) 0.185(13) 0.102(8) -0.001(8) -0.015(6) 0.027(8) O204 0.174(8) 0.110(5) 0.147(7) 0.033(5) 0.078(6) 0.043(6) O205 0.124(15) 0.155(18) 0.071(10) -0.009(10) 0.044(10) -0.062(13) C101 0.33(3) 0.24(2) 0.22(2) 0.078(16) 0.19(2) 0.091(19) C201 0.157(11) 0.092(7) 0.126(9) -0.016(6) 0.041(8) 0.021(7) N102 0.48(3) 0.089(7) 0.080(6) 0.007(5) 0.076(12) 0.004(11) N202 0.066(6) 0.076(6) 0.094(8) 0.019(5) 0.030(6) 0.013(5) N206 0.14(2) 0.069(12) 0.089(14) -0.015(10) 0.069(15) -0.032(13) _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 Zn1 N21 2.150(4) . ? Zn1 N41 2.164(5) . ? Zn1 N51 2.168(4) 2_556 ? Zn1 N61 2.194(4) 2_556 ? Zn1 N11 2.195(4) . ? Zn1 N31 2.198(4) . ? N11 C15 1.332(6) . ? N11 C12 1.381(7) . ? C12 C13 1.364(7) . ? C12 C55 1.465(7) . ? C13 S14 1.726(6) . ? S14 C15 1.698(5) . ? C15 C22 1.473(8) . ? N21 C26 1.335(8) . ? N21 C22 1.350(7) . ? C22 C23 1.380(7) . ? C23 C24 1.369(9) . ? C24 C25 1.373(10) . ? C25 C26 1.384(8) . ? N31 C32 1.312(6) . ? N31 C35 1.385(6) . ? C32 C42 1.467(7) . ? C32 S33 1.720(5) . ? S33 C34 1.699(6) . ? C34 C35 1.375(7) . ? C35 C35 1.449(9) 2_556 ? N41 C42 1.336(7) . ? N41 C46 1.341(7) . ? C42 C43 1.382(8) . ? C43 C44 1.399(9) . ? C44 C45 1.358(11) . ? C45 C46 1.399(9) . ? N51 C52 1.308(6) . ? N51 C55 1.380(6) . ? N51 Zn1 2.168(4) 2_556 ? C52 C62 1.469(7) . ? C52 S53 1.712(5) . ? S53 C54 1.714(6) . ? C54 C55 1.373(7) . ? N61 C62 1.317(7) . ? N61 C66 1.352(7) . ? N61 Zn1 2.194(4) 2_556 ? C62 C63 1.388(8) . ? C63 C64 1.393(9) . ? C64 C65 1.365(11) . ? C65 C66 1.389(10) . ? Cl1 O13B 1.331(18) . ? Cl1 O11B 1.331(17) . ? Cl1 O11A 1.352(11) . ? Cl1 O14B 1.360(13) . ? Cl1 O14A 1.374(8) . ? Cl1 O13A 1.408(10) . ? Cl1 O12 1.412(6) . ? O11A O11B 1.23(3) . ? O11A O13B 1.81(4) . ? O11B O12 1.59(3) . ? O11B O13B 1.74(3) . ? O13A O13B 1.18(3) . ? O14A O14B 1.078(19) . ? Cl2 O22 1.286(10) . ? Cl2 O21 1.373(6) . ? Cl2 O24 1.384(8) . ? Cl2 O23 1.432(9) . ? O103 N102 1.221(10) . ? O104 N102 1.158(13) . ? O203 N202 1.183(11) . ? O204 N202 1.193(9) . ? O204 N206 1.42(2) . ? O205 N206 1.18(3) . ? C101 N102 1.460(18) . ? C201 N206 1.35(3) . ? C201 N202 1.494(14) . ? N202 N206 1.52(3) . ? 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 N21 Zn1 N41 95.07(17) . . ? N21 Zn1 N51 88.58(16) . 2_556 ? N41 Zn1 N51 174.25(15) . 2_556 ? N21 Zn1 N61 98.60(18) . 2_556 ? N41 Zn1 N61 98.22(19) . 2_556 ? N51 Zn1 N61 76.81(15) 2_556 2_556 ? N21 Zn1 N11 78.05(17) . . ? N41 Zn1 N11 86.18(17) . . ? N51 Zn1 N11 98.94(14) 2_556 . ? N61 Zn1 N11 174.74(15) 2_556 . ? N21 Zn1 N31 171.94(16) . . ? N41 Zn1 N31 77.08(15) . . ? N51 Zn1 N31 99.39(14) 2_556 . ? N61 Zn1 N31 84.46(16) 2_556 . ? N11 Zn1 N31 99.40(15) . . ? C15 N11 C12 111.0(4) . . ? C15 N11 Zn1 110.5(3) . . ? C12 N11 Zn1 137.5(3) . . ? C13 C12 N11 114.8(4) . . ? C13 C12 C55 123.7(5) . . ? N11 C12 C55 121.4(4) . . ? C12 C13 S14 109.6(5) . . ? C15 S14 C13 90.5(3) . . ? N11 C15 C22 121.2(4) . . ? N11 C15 S14 114.1(4) . . ? C22 C15 S14 124.6(3) . . ? C26 N21 C22 118.7(4) . . ? C26 N21 Zn1 126.2(4) . . ? C22 N21 Zn1 114.6(3) . . ? N21 C22 C23 122.1(5) . . ? N21 C22 C15 114.6(4) . . ? C23 C22 C15 123.3(5) . . ? C24 C23 C22 119.2(6) . . ? C23 C24 C25 118.8(5) . . ? C24 C25 C26 120.0(6) . . ? N21 C26 C25 121.3(6) . . ? C32 N31 C35 110.9(4) . . ? C32 N31 Zn1 110.8(3) . . ? C35 N31 Zn1 136.6(3) . . ? N31 C32 C42 121.5(4) . . ? N31 C32 S33 114.7(4) . . ? C42 C32 S33 123.6(4) . . ? C34 S33 C32 89.6(2) . . ? C35 C34 S33 111.0(4) . . ? C34 C35 N31 113.8(4) . . ? C34 C35 C35 123.0(4) . 2_556 ? N31 C35 C35 123.1(3) . 2_556 ? C42 N41 C46 118.9(5) . . ? C42 N41 Zn1 114.8(3) . . ? C46 N41 Zn1 125.0(4) . . ? N41 C42 C43 123.1(5) . . ? N41 C42 C32 114.0(5) . . ? C43 C42 C32 122.9(5) . . ? C42 C43 C44 117.0(6) . . ? C45 C44 C43 121.0(6) . . ? C44 C45 C46 118.1(6) . . ? N41 C46 C45 121.9(6) . . ? C52 N51 C55 110.4(4) . . ? C52 N51 Zn1 112.1(3) . 2_556 ? C55 N51 Zn1 136.7(3) . 2_556 ? N51 C52 C62 121.2(4) . . ? N51 C52 S53 115.6(4) . . ? C62 C52 S53 123.2(4) . . ? C52 S53 C54 89.2(2) . . ? C55 C54 S53 110.3(4) . . ? C54 C55 N51 114.5(4) . . ? C54 C55 C12 122.2(4) . . ? N51 C55 C12 123.3(4) . . ? C62 N61 C66 119.3(5) . . ? C62 N61 Zn1 114.1(3) . 2_556 ? C66 N61 Zn1 125.3(5) . 2_556 ? N61 C62 C63 123.3(5) . . ? N61 C62 C52 114.9(4) . . ? C63 C62 C52 121.8(5) . . ? C62 C63 C64 117.1(7) . . ? C65 C64 C63 120.2(6) . . ? C64 C65 C66 119.0(6) . . ? N61 C66 C65 121.1(7) . . ? O13B Cl1 O11B 81.7(13) . . ? O13B Cl1 O11A 84.8(19) . . ? O11B Cl1 O11A 54.4(15) . . ? O13B Cl1 O14B 157.1(10) . . ? O11B Cl1 O14B 117.5(12) . . ? O11A Cl1 O14B 96.4(16) . . ? O13B Cl1 O14A 112.1(10) . . ? O11B Cl1 O14A 161.1(13) . . ? O11A Cl1 O14A 112.2(11) . . ? O14B Cl1 O14A 46.4(8) . . ? O13B Cl1 O13A 51.0(15) . . ? O11B Cl1 O13A 110.5(12) . . ? O11A Cl1 O13A 136(2) . . ? O14B Cl1 O13A 124.0(14) . . ? O14A Cl1 O13A 88.3(9) . . ? O13B Cl1 O12 111.3(11) . . ? O11B Cl1 O12 70.8(15) . . ? O11A Cl1 O12 120.1(13) . . ? O14B Cl1 O12 87.9(7) . . ? O14A Cl1 O12 113.1(6) . . ? O13A Cl1 O12 82.0(10) . . ? O11B O11A Cl1 61.9(10) . . ? O11B O11A O13B 66.8(14) . . ? Cl1 O11A O13B 47.1(8) . . ? O11A O11B Cl1 63.7(13) . . ? O11A O11B O12 115.8(16) . . ? Cl1 O11B O12 57.0(9) . . ? O11A O11B O13B 73(2) . . ? Cl1 O11B O13B 49.1(8) . . ? O12 O11B O13B 85.5(13) . . ? Cl1 O12 O11B 52.2(10) . . ? O13B O13A Cl1 61.1(14) . . ? O13A O13B Cl1 67.9(10) . . ? O13A O13B O11B 99.0(16) . . ? Cl1 O13B O11B 49.2(10) . . ? O13A O13B O11A 116.0(18) . . ? Cl1 O13B O11A 48.1(13) . . ? O11B O13B O11A 40.4(13) . . ? O14B O14A Cl1 66.1(9) . . ? O14A O14B Cl1 67.5(9) . . ? O22 Cl2 O21 118.7(7) . . ? O22 Cl2 O24 111.5(7) . . ? O21 Cl2 O24 114.9(6) . . ? O22 Cl2 O23 103.8(9) . . ? O21 Cl2 O23 105.2(6) . . ? O24 Cl2 O23 99.9(7) . . ? N202 O204 N206 70.7(13) . . ? N206 C201 N202 64.6(11) . . ? O104 N102 O103 129.9(19) . . ? O104 N102 C101 116.4(12) . . ? O103 N102 C101 113.2(13) . . ? O203 N202 O204 128.7(12) . . ? O203 N202 C201 117.2(9) . . ? O204 N202 C201 113.6(10) . . ? O203 N202 N206 160.2(14) . . ? O204 N202 N206 61.7(10) . . ? C201 N202 N206 53.1(10) . . ? O205 N206 C201 120(2) . . ? O205 N206 O204 131(3) . . ? C201 N206 O204 109(2) . . ? O205 N206 N202 166.5(17) . . ? C201 N206 N202 62.3(14) . . ? O204 N206 N202 47.6(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.918 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.133 #=END data_girlfrim _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H42 Cl4 Co2 N16 O24 S6' _chemical_formula_weight 1727.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 13.2594(7) _cell_length_b 23.1248(12) _cell_length_c 22.4373(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.8610(10) _cell_angle_gamma 90.00 _cell_volume 6778.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21778 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7757 _reflns_number_gt 4840 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7757 _refine_ls_number_parameters 469 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.1349 _refine_ls_R_factor_gt 0.1011 _refine_ls_wR_factor_ref 0.3315 _refine_ls_wR_factor_gt 0.3078 _refine_ls_goodness_of_fit_ref 1.205 _refine_ls_restrained_S_all 1.264 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.17168(6) 0.12591(3) 0.76601(4) 0.0406(3) Uani 1 1 d . . . S14 S 0.09776(17) -0.05585(7) 0.82097(9) 0.0607(5) Uani 1 1 d . . . S33 S 0.10044(17) 0.27130(8) 0.88772(9) 0.0621(6) Uani 1 1 d . . . S53 S -0.0849(2) 0.16293(9) 0.93444(9) 0.0734(7) Uani 1 1 d . . . N11 N 0.0980(4) 0.0524(2) 0.7997(2) 0.0417(12) Uani 1 1 d . . . N21 N 0.2580(4) 0.0552(2) 0.7404(3) 0.0505(14) Uani 1 1 d . . . N31 N 0.0955(4) 0.1958(2) 0.8033(2) 0.0395(11) Uani 1 1 d . . . N41 N 0.2546(5) 0.1322(2) 0.8563(3) 0.0583(16) Uani 1 1 d . . . N51 N -0.0928(4) 0.12700(19) 0.8257(2) 0.0375(11) Uani 1 1 d . . . N61 N -0.2476(4) 0.1956(2) 0.7747(3) 0.0542(15) Uani 1 1 d . . . C12 C 0.0288(5) 0.0435(2) 0.8381(3) 0.0410(14) Uani 1 1 d . . . C13 C 0.0169(6) -0.0127(3) 0.8546(3) 0.0556(18) Uani 1 1 d . . . H13 H -0.0273 -0.0256 0.8798 0.067 Uiso 1 1 calc R . . C15 C 0.1411(5) 0.0028(3) 0.7877(3) 0.0451(15) Uani 1 1 d . . . C22 C 0.2227(5) 0.0021(3) 0.7510(3) 0.0494(16) Uani 1 1 d . . . C23 C 0.2601(6) -0.0477(3) 0.7304(3) 0.0596(19) Uani 1 1 d . . . H23 H 0.2324 -0.0835 0.7375 0.071 Uiso 1 1 calc R . . C24 C 0.3417(7) -0.0433(4) 0.6980(4) 0.070(2) Uani 1 1 d . . . H24 H 0.3686 -0.0760 0.6823 0.084 Uiso 1 1 calc R . . C25 C 0.3798(7) 0.0096(4) 0.6904(4) 0.071(2) Uani 1 1 d . . . H25 H 0.4374 0.0133 0.6722 0.085 Uiso 1 1 calc R . . C26 C 0.3344(6) 0.0588(4) 0.7092(4) 0.067(2) Uani 1 1 d . . . H26 H 0.3579 0.0950 0.6999 0.080 Uiso 1 1 calc R . . C32 C 0.1384(6) 0.2078(3) 0.8594(3) 0.0493(16) Uani 1 1 d . . . C34 C 0.0220(6) 0.2836(3) 0.8204(3) 0.0502(16) Uani 1 1 d . . . H34 H -0.0193 0.3161 0.8118 0.060 Uiso 1 1 calc R . . C35 C 0.0278(5) 0.2396(2) 0.7809(3) 0.0403(13) Uani 1 1 d . . . C42 C 0.2180(6) 0.1692(3) 0.8921(3) 0.0565(18) Uani 1 1 d . . . C43 C 0.2483(8) 0.1720(3) 0.9532(4) 0.084(3) Uani 1 1 d . . . H43 H 0.2200 0.1988 0.9765 0.100 Uiso 1 1 calc R . . C44 C 0.3235(10) 0.1329(4) 0.9798(5) 0.125(6) Uani 1 1 d . . . H44 H 0.3459 0.1329 1.0214 0.150 Uiso 1 1 calc R . . C45 C 0.3635(9) 0.0948(4) 0.9435(5) 0.112(5) Uani 1 1 d . . . H45 H 0.4130 0.0683 0.9603 0.135 Uiso 1 1 calc R . . C46 C 0.3297(7) 0.0958(4) 0.8811(4) 0.078(3) Uani 1 1 d . . . H46 H 0.3594 0.0711 0.8563 0.094 Uiso 1 1 calc R . . C52 C -0.1298(5) 0.1663(3) 0.8590(3) 0.0466(15) Uani 1 1 d . . . C54 C -0.0065(7) 0.1058(3) 0.9220(3) 0.060(2) Uani 1 1 d . . . H54 H 0.0403 0.0877 0.9518 0.072 Uiso 1 1 calc R . . C55 C -0.0233(5) 0.0914(3) 0.8623(3) 0.0442(14) Uani 1 1 d . . . C62 C -0.2074(6) 0.2073(3) 0.8314(3) 0.0508(16) Uani 1 1 d . . . C63 C -0.2373(8) 0.2539(3) 0.8608(5) 0.078(3) Uani 1 1 d . . . H63 H -0.2070 0.2609 0.9007 0.093 Uiso 1 1 calc R . . C64 C -0.3118(8) 0.2909(4) 0.8324(5) 0.085(3) Uani 1 1 d . . . H64 H -0.3346 0.3222 0.8525 0.102 Uiso 1 1 calc R . . C65 C -0.3501(7) 0.2794(4) 0.7736(6) 0.088(3) Uani 1 1 d . . . H65 H -0.3992 0.3039 0.7524 0.105 Uiso 1 1 calc R . . C66 C -0.3179(6) 0.2324(4) 0.7449(5) 0.070(2) Uani 1 1 d . . . H66 H -0.3448 0.2258 0.7045 0.084 Uiso 1 1 calc R . . Cl1 Cl 0.92269(13) 0.41615(8) 0.89612(8) 0.0537(5) Uani 1 1 d D . . Cl2 Cl 0.8932(2) 0.84560(11) 0.90297(10) 0.0841(8) Uani 1 1 d D . . O102 O 0.3541(10) 0.1400(5) 0.5906(6) 0.168(5) Uani 1 1 d U . . N101 N 0.4300(11) 0.1688(6) 0.6015(7) 0.135(4) Uani 1 1 d U . . C103 C 0.4885(13) 0.1781(10) 0.6460(8) 0.173(9) Uani 1 1 d U . . O104 O 0.4254(18) 0.2053(6) 0.5433(7) 0.269(11) Uani 1 1 d U . . O21 O 0.9859(10) 0.8536(6) 0.9381(8) 0.288(12) Uani 1 1 d DU . . O22 O 0.8622(9) 0.7954(4) 0.9228(7) 0.198(6) Uani 1 1 d DU . . O23 O 0.8384(13) 0.8893(5) 0.9181(7) 0.278(11) Uani 1 1 d DU . . O24 O 0.9079(17) 0.8461(6) 0.8499(6) 0.333(14) Uani 1 1 d DU . . O11 O 1.0191(6) 0.3953(4) 0.8973(4) 0.137(4) Uani 1 1 d DU . . O12 O 0.9245(11) 0.4702(4) 0.8958(7) 0.251(9) Uani 1 1 d DU . . O13 O 0.8736(12) 0.3929(5) 0.8451(7) 0.315(14) Uani 1 1 d DU . . O14 O 0.8894(14) 0.3917(8) 0.9397(7) 0.402(18) Uani 1 1 d DU . . N201 N 0.728(2) 1.0169(10) 0.9717(13) 0.256(11) Uani 1 1 d U . . O204 O 0.863(2) 1.0070(7) 0.9843(9) 0.274(12) Uani 1 1 d U . . O202 O 0.8136(10) 1.0226(7) 0.9128(7) 0.191(5) Uani 1 1 d U . . C203 C 0.8124(18) 1.030(3) 1.0209(14) 0.40(3) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0441(5) 0.0295(5) 0.0464(5) -0.0098(3) 0.0024(4) 0.0014(3) S14 0.0917(14) 0.0271(8) 0.0647(12) 0.0054(7) 0.0177(10) 0.0198(8) S33 0.0891(14) 0.0375(9) 0.0525(10) -0.0188(7) -0.0083(9) 0.0136(9) S53 0.131(2) 0.0478(11) 0.0445(10) -0.0002(8) 0.0242(11) 0.0335(12) N11 0.049(3) 0.028(2) 0.043(3) -0.004(2) -0.006(2) 0.012(2) N21 0.048(3) 0.042(3) 0.060(3) -0.011(3) 0.003(3) 0.005(2) N31 0.046(3) 0.027(2) 0.042(3) -0.005(2) 0.000(2) 0.002(2) N41 0.063(4) 0.035(3) 0.067(4) -0.013(3) -0.017(3) 0.011(3) N51 0.047(3) 0.024(2) 0.042(3) 0.0062(19) 0.010(2) 0.005(2) N61 0.047(3) 0.037(3) 0.079(4) 0.021(3) 0.013(3) 0.012(2) C12 0.058(4) 0.028(3) 0.034(3) 0.003(2) -0.001(3) 0.008(3) C13 0.084(5) 0.030(3) 0.054(4) 0.002(3) 0.015(4) 0.013(3) C15 0.063(4) 0.027(3) 0.043(3) -0.003(2) 0.002(3) 0.014(3) C22 0.052(4) 0.046(4) 0.046(3) -0.010(3) -0.005(3) 0.015(3) C23 0.071(5) 0.041(4) 0.063(5) -0.009(3) 0.002(4) 0.016(3) C24 0.081(6) 0.069(6) 0.062(5) -0.016(4) 0.020(4) 0.029(5) C25 0.065(5) 0.067(5) 0.088(6) -0.015(5) 0.031(4) 0.011(4) C26 0.055(4) 0.071(5) 0.077(5) -0.013(4) 0.018(4) -0.003(4) C32 0.063(4) 0.038(3) 0.041(3) -0.009(3) -0.006(3) 0.004(3) C34 0.070(4) 0.028(3) 0.052(4) -0.004(3) 0.008(3) 0.006(3) C35 0.050(3) 0.025(3) 0.045(3) 0.002(2) 0.006(3) 0.002(2) C42 0.066(4) 0.039(3) 0.056(4) -0.017(3) -0.014(3) 0.006(3) C43 0.130(8) 0.039(4) 0.066(5) -0.018(4) -0.029(5) 0.013(5) C44 0.169(11) 0.064(6) 0.100(8) -0.032(5) -0.096(8) 0.041(7) C45 0.124(9) 0.060(6) 0.119(9) -0.034(6) -0.076(7) 0.039(6) C46 0.075(5) 0.059(5) 0.084(6) -0.017(4) -0.036(5) 0.023(4) C52 0.068(4) 0.035(3) 0.039(3) 0.005(3) 0.017(3) 0.010(3) C54 0.100(6) 0.042(4) 0.038(3) 0.006(3) 0.012(3) 0.027(4) C55 0.063(4) 0.030(3) 0.041(3) 0.008(2) 0.012(3) 0.008(3) C62 0.067(4) 0.032(3) 0.060(4) 0.012(3) 0.028(4) 0.011(3) C63 0.112(7) 0.040(4) 0.096(6) 0.018(4) 0.058(6) 0.028(4) C64 0.104(7) 0.053(5) 0.106(8) 0.025(5) 0.041(6) 0.034(5) C65 0.071(6) 0.058(5) 0.140(10) 0.052(6) 0.038(6) 0.034(4) C66 0.055(4) 0.056(5) 0.097(6) 0.030(4) 0.010(4) 0.016(4) Cl1 0.0581(10) 0.0464(9) 0.0577(10) 0.0026(7) 0.0134(8) 0.0153(8) Cl2 0.127(2) 0.0640(14) 0.0535(12) 0.0103(10) -0.0069(12) -0.0055(13) O102 0.172(10) 0.134(8) 0.228(14) -0.063(8) 0.116(10) -0.064(8) N101 0.122(9) 0.136(11) 0.163(12) -0.041(10) 0.066(9) -0.014(9) C103 0.129(12) 0.24(2) 0.121(12) -0.027(14) -0.050(10) -0.014(14) O104 0.54(3) 0.122(10) 0.154(12) 0.031(9) 0.077(17) 0.044(14) O21 0.30(2) 0.191(15) 0.30(2) -0.071(14) -0.157(18) 0.047(14) O22 0.157(10) 0.106(8) 0.355(19) 0.090(10) 0.105(11) -0.002(7) O23 0.45(3) 0.176(13) 0.263(17) 0.104(12) 0.219(18) 0.195(16) O24 0.67(5) 0.170(14) 0.180(15) -0.082(12) 0.11(2) 0.03(2) O11 0.128(7) 0.126(7) 0.141(8) -0.042(6) -0.021(6) 0.056(6) O12 0.322(19) 0.066(7) 0.41(3) -0.037(10) 0.200(18) 0.007(9) O13 0.39(2) 0.191(14) 0.28(2) -0.081(14) -0.165(19) 0.193(16) O14 0.44(3) 0.49(4) 0.26(2) 0.20(2) 0.04(2) -0.24(3) N201 0.33(3) 0.178(19) 0.28(3) 0.025(17) 0.10(3) -0.02(2) O204 0.53(4) 0.139(12) 0.204(17) -0.051(11) 0.20(2) -0.065(18) O202 0.190(12) 0.225(15) 0.156(12) -0.014(10) 0.028(10) -0.049(11) C203 0.124(16) 0.88(8) 0.19(2) -0.23(4) 0.030(17) -0.02(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 Co1 N21 2.130(5) . ? Co1 N41 2.138(6) . ? Co1 N51 2.143(5) 2_556 ? Co1 N31 2.150(5) . ? Co1 N11 2.161(5) . ? Co1 N61 2.182(6) 2_556 ? S14 C15 1.696(7) . ? S14 C13 1.730(7) . ? S33 C34 1.705(7) . ? S33 C32 1.710(7) . ? S53 C52 1.698(7) . ? S53 C54 1.733(7) . ? N11 C15 1.328(7) . ? N11 C12 1.377(9) . ? N21 C26 1.328(10) . ? N21 C22 1.351(9) . ? N31 C32 1.318(8) . ? N31 C35 1.389(7) . ? N41 C42 1.321(9) . ? N41 C46 1.349(9) . ? N51 C52 1.323(8) . ? N51 C55 1.392(7) . ? N51 Co1 2.143(5) 2_556 ? N61 C62 1.320(10) . ? N61 C66 1.352(9) . ? N61 Co1 2.182(6) 2_556 ? C12 C13 1.369(9) . ? C12 C55 1.459(8) . ? C15 C22 1.467(10) . ? C22 C23 1.366(9) . ? C23 C24 1.407(12) . ? C24 C25 1.346(13) . ? C25 C26 1.385(11) . ? C32 C42 1.478(9) . ? C34 C35 1.361(9) . ? C35 C35 1.455(12) 2_556 ? C42 C43 1.364(11) . ? C43 C44 1.401(12) . ? C44 C45 1.367(16) . ? C45 C46 1.395(13) . ? C52 C62 1.456(9) . ? C54 C55 1.362(9) . ? C62 C63 1.358(10) . ? C63 C64 1.378(13) . ? C64 C65 1.356(15) . ? C65 C66 1.368(14) . ? Cl1 O12 1.250(9) . ? Cl1 O14 1.273(10) . ? Cl1 O13 1.331(10) . ? Cl1 O11 1.362(7) . ? Cl2 O24 1.240(11) . ? Cl2 O23 1.322(9) . ? Cl2 O22 1.334(8) . ? Cl2 O21 1.354(10) . ? O102 N101 1.197(15) . ? N101 C103 1.173(18) . ? N101 O104 1.547(19) . ? N201 C203 1.46(3) . ? N201 O204 1.77(3) . ? O204 C203 1.26(3) . ? O204 O202 1.66(3) . ? 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 N21 Co1 N41 95.4(2) . . ? N21 Co1 N51 86.9(2) . 2_556 ? N41 Co1 N51 175.1(2) . 2_556 ? N21 Co1 N31 172.7(2) . . ? N41 Co1 N31 77.3(2) . . ? N51 Co1 N31 100.40(18) 2_556 . ? N21 Co1 N11 77.7(2) . . ? N41 Co1 N11 85.0(2) . . ? N51 Co1 N11 99.74(18) 2_556 . ? N31 Co1 N11 100.6(2) . . ? N21 Co1 N61 98.4(2) . 2_556 ? N41 Co1 N61 98.5(3) . 2_556 ? N51 Co1 N61 76.9(2) 2_556 2_556 ? N31 Co1 N61 83.6(2) . 2_556 ? N11 Co1 N61 175.1(2) . 2_556 ? C15 S14 C13 90.7(3) . . ? C34 S33 C32 89.3(3) . . ? C52 S53 C54 89.6(3) . . ? C15 N11 C12 110.7(5) . . ? C15 N11 Co1 111.8(5) . . ? C12 N11 Co1 136.5(4) . . ? C26 N21 C22 117.9(6) . . ? C26 N21 Co1 126.1(5) . . ? C22 N21 Co1 115.6(5) . . ? C32 N31 C35 109.8(5) . . ? C32 N31 Co1 112.0(4) . . ? C35 N31 Co1 136.4(4) . . ? C42 N41 C46 118.4(7) . . ? C42 N41 Co1 115.9(5) . . ? C46 N41 Co1 124.9(5) . . ? C52 N51 C55 110.3(5) . . ? C52 N51 Co1 112.5(4) . 2_556 ? C55 N51 Co1 136.3(4) . 2_556 ? C62 N61 C66 118.5(7) . . ? C62 N61 Co1 114.5(4) . 2_556 ? C66 N61 Co1 126.0(6) . 2_556 ? C13 C12 N11 115.5(6) . . ? C13 C12 C55 122.4(6) . . ? N11 C12 C55 121.9(5) . . ? C12 C13 S14 108.7(6) . . ? N11 C15 C22 120.5(6) . . ? N11 C15 S14 114.3(5) . . ? C22 C15 S14 125.1(5) . . ? N21 C22 C23 123.3(7) . . ? N21 C22 C15 113.6(5) . . ? C23 C22 C15 123.1(7) . . ? C22 C23 C24 118.1(8) . . ? C25 C24 C23 118.0(7) . . ? C24 C25 C26 121.0(8) . . ? N21 C26 C25 121.4(8) . . ? N31 C32 C42 120.1(6) . . ? N31 C32 S33 115.4(5) . . ? C42 C32 S33 124.4(5) . . ? C35 C34 S33 111.0(5) . . ? C34 C35 N31 114.5(6) . . ? C34 C35 C35 123.0(5) . 2_556 ? N31 C35 C35 122.4(5) . 2_556 ? N41 C42 C43 124.5(7) . . ? N41 C42 C32 113.2(6) . . ? C43 C42 C32 122.2(7) . . ? C42 C43 C44 117.6(9) . . ? C45 C44 C43 118.9(9) . . ? C44 C45 C46 119.8(8) . . ? N41 C46 C45 120.8(8) . . ? N51 C52 C62 120.7(6) . . ? N51 C52 S53 115.4(5) . . ? C62 C52 S53 123.8(5) . . ? C55 C54 S53 110.0(5) . . ? C54 C55 N51 114.6(6) . . ? C54 C55 C12 122.9(6) . . ? N51 C55 C12 122.5(5) . . ? N61 C62 C63 121.8(7) . . ? N61 C62 C52 114.6(6) . . ? C63 C62 C52 123.6(8) . . ? C62 C63 C64 120.9(10) . . ? C63 C64 C65 116.6(9) . . ? C66 C65 C64 121.2(8) . . ? N61 C66 C65 120.8(10) . . ? O12 Cl1 O14 117.3(10) . . ? O12 Cl1 O13 114.0(9) . . ? O14 Cl1 O13 107.4(9) . . ? O12 Cl1 O11 109.6(8) . . ? O14 Cl1 O11 106.0(9) . . ? O13 Cl1 O11 101.2(7) . . ? O24 Cl2 O23 115.0(8) . . ? O24 Cl2 O22 115.9(8) . . ? O23 Cl2 O22 111.5(8) . . ? O24 Cl2 O21 106.3(10) . . ? O23 Cl2 O21 103.3(9) . . ? O22 Cl2 O21 103.1(8) . . ? C103 N101 O102 133(2) . . ? C103 N101 O104 122.8(18) . . ? O102 N101 O104 102.7(16) . . ? C203 N201 O204 44.6(15) . . ? C203 O204 O202 112(3) . . ? C203 O204 N201 54.3(16) . . ? O202 O204 N201 66.3(17) . . ? O204 C203 N201 81(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.599 _refine_diff_density_min -1.282 _refine_diff_density_rms 0.155 #=END data_zinm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H59 Cl4 N21 O16 S4 Zn2' _chemical_formula_weight 1947.24 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.430(5) _cell_length_b 15.088(6) _cell_length_c 21.650(8) _cell_angle_alpha 81.050(7) _cell_angle_beta 80.641(8) _cell_angle_gamma 78.684(8) _cell_volume 4210(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22584 _diffrn_reflns_av_R_equivalents 0.1585 _diffrn_reflns_av_sigmaI/netI 0.1893 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 20.00 _reflns_number_total 7859 _reflns_number_gt 3899 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7859 _refine_ls_number_parameters 501 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2327 _refine_ls_R_factor_gt 0.1594 _refine_ls_wR_factor_ref 0.4198 _refine_ls_wR_factor_gt 0.3834 _refine_ls_goodness_of_fit_ref 1.243 _refine_ls_restrained_S_all 1.243 _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 Zn1 Zn 0.7354(2) 0.89833(17) 0.15748(12) 0.0258(9) Uiso 1 1 d . . . Zn2 Zn 0.7635(2) 0.60158(17) 0.32694(12) 0.0260(8) Uiso 1 1 d . . . N101 N 0.8062(14) 0.8612(11) 0.2467(8) 0.027(5) Uiso 1 1 d . . . C102 C 0.9034(18) 0.8694(15) 0.2368(11) 0.031(6) Uiso 1 1 d . . . S103 S 0.9549(4) 0.8573(4) 0.3059(3) 0.0247(15) Uiso 1 1 d . . . C104 C 0.8405(17) 0.8414(14) 0.3490(11) 0.030(6) Uiso 1 1 d . . . H104 H 0.8279 0.8310 0.3938 0.036 Uiso 1 1 calc R . . C105 C 0.7659(17) 0.8462(14) 0.3073(10) 0.024(6) Uiso 1 1 d . . . N111 N 0.6823(15) 0.7663(13) 0.1667(9) 0.038(5) Uiso 1 1 d . . . C112 C 0.5799(17) 0.7755(14) 0.1649(10) 0.025(6) Uiso 1 1 d . . . S113 S 0.5377(5) 0.6790(4) 0.1572(3) 0.0360(17) Uiso 1 1 d . . . C114 C 0.6599(19) 0.6186(17) 0.1576(11) 0.038(7) Uiso 1 1 d . . . H114 H 0.6795 0.5553 0.1543 0.045 Uiso 1 1 calc R . . C115 C 0.7241(19) 0.6745(15) 0.1634(11) 0.033(6) Uiso 1 1 d . . . N121 N 0.7555(14) 0.9065(11) 0.0548(8) 0.025(5) Uiso 1 1 d . . . C122 C 0.8522(17) 0.8988(14) 0.0277(10) 0.024(6) Uiso 1 1 d . . . C123 C 0.9301(18) 0.8862(14) 0.0686(11) 0.027(6) Uiso 1 1 d . . . N124 N 0.8898(14) 0.8870(11) 0.1297(8) 0.026(5) Uiso 1 1 d . . . C125 C 0.9633(18) 0.8706(15) 0.1713(11) 0.030(6) Uiso 1 1 d . . . C126 C 1.0609(18) 0.8653(14) 0.1536(11) 0.030(6) Uiso 1 1 d . . . H126 H 1.1048 0.8634 0.1842 0.036 Uiso 1 1 calc R . . C127 C 1.1035(18) 0.8624(14) 0.0896(10) 0.029(6) Uiso 1 1 d . . . H127 H 1.1755 0.8522 0.0769 0.035 Uiso 1 1 calc R . . C128 C 1.0341(16) 0.8752(14) 0.0458(10) 0.020(5) Uiso 1 1 d . . . C129 C 1.0638(19) 0.8750(15) -0.0216(11) 0.033(6) Uiso 1 1 d . . . H129 H 1.1340 0.8666 -0.0394 0.040 Uiso 1 1 calc R . . C130 C 0.990(2) 0.8869(16) -0.0582(13) 0.045(7) Uiso 1 1 d . . . H130 H 1.0108 0.8879 -0.1023 0.053 Uiso 1 1 calc R . . C131 C 0.8852(17) 0.8979(14) -0.0384(10) 0.025(6) Uiso 1 1 d . . . C132 C 0.8043(19) 0.9091(15) -0.0752(12) 0.036(7) Uiso 1 1 d . . . H132 H 0.8197 0.9091 -0.1196 0.043 Uiso 1 1 calc R . . C133 C 0.706(2) 0.9198(16) -0.0479(12) 0.040(7) Uiso 1 1 d . . . H133 H 0.6532 0.9276 -0.0739 0.048 Uiso 1 1 calc R . . C134 C 0.6780(18) 0.9198(14) 0.0169(11) 0.028(6) Uiso 1 1 d . . . H134 H 0.6079 0.9287 0.0349 0.033 Uiso 1 1 calc R . . N141 N 0.5743(15) 0.9272(12) 0.1724(9) 0.033(5) Uiso 1 1 d . . . C142 C 0.5317(17) 1.0152(14) 0.1818(10) 0.026(6) Uiso 1 1 d . . . C143 C 0.5963(18) 1.0781(16) 0.1753(11) 0.034(6) Uiso 1 1 d . . . N144 N 0.7017(14) 1.0428(11) 0.1695(8) 0.024(5) Uiso 1 1 d . . . C145 C 0.764(2) 1.1002(16) 0.1659(11) 0.040(7) Uiso 1 1 d . . . H145 H 0.8357 1.0772 0.1605 0.049 Uiso 1 1 calc R . . C146 C 0.732(2) 1.1941(17) 0.1696(12) 0.044(7) Uiso 1 1 d . . . H146 H 0.7806 1.2329 0.1676 0.052 Uiso 1 1 calc R . . C147 C 0.630(2) 1.2279(18) 0.1762(12) 0.044(7) Uiso 1 1 d . . . H147 H 0.6066 1.2912 0.1775 0.053 Uiso 1 1 calc R . . C148 C 0.5601(18) 1.1694(15) 0.1809(11) 0.026(6) Uiso 1 1 d . . . C149 C 0.4520(19) 1.1934(16) 0.1946(11) 0.036(7) Uiso 1 1 d . . . H149 H 0.4240 1.2549 0.2003 0.044 Uiso 1 1 calc R . . C150 C 0.387(2) 1.1347(16) 0.2002(12) 0.044(7) Uiso 1 1 d . . . H150 H 0.3151 1.1552 0.2084 0.052 Uiso 1 1 calc R . . C151 C 0.4273(18) 1.0393(15) 0.1934(11) 0.031(6) Uiso 1 1 d . . . C152 C 0.3667(19) 0.9704(15) 0.1953(11) 0.033(6) Uiso 1 1 d . . . H152 H 0.2941 0.9838 0.2043 0.039 Uiso 1 1 calc R . . C153 C 0.4147(18) 0.8870(15) 0.1843(10) 0.029(6) Uiso 1 1 d . . . H153 H 0.3752 0.8412 0.1843 0.034 Uiso 1 1 calc R . . C154 C 0.5187(18) 0.8657(15) 0.1731(11) 0.032(6) Uiso 1 1 d . . . N201 N 0.8524(14) 0.6348(12) 0.2352(9) 0.029(5) Uiso 1 1 d . . . C202 C 0.9530(19) 0.6258(15) 0.2366(11) 0.033(6) Uiso 1 1 d . . . S203 S 1.0274(5) 0.6340(4) 0.1645(3) 0.0393(18) Uiso 1 1 d . . . C204 C 0.9191(19) 0.6509(16) 0.1309(13) 0.043(7) Uiso 1 1 d . . . H204 H 0.9178 0.6605 0.0866 0.051 Uiso 1 1 calc R . . C205 C 0.8364(19) 0.6493(15) 0.1732(11) 0.033(6) Uiso 1 1 d . . . N211 N 0.6550(14) 0.7358(11) 0.3227(8) 0.024(5) Uiso 1 1 d . . . C212 C 0.5603(17) 0.7257(14) 0.3305(10) 0.026(6) Uiso 1 1 d . . . S213 S 0.4741(5) 0.8236(4) 0.3447(3) 0.0328(17) Uiso 1 1 d . . . C214 C 0.5735(17) 0.8806(16) 0.3355(10) 0.029(6) Uiso 1 1 d . . . H214 H 0.5662 0.9438 0.3382 0.035 Uiso 1 1 calc R . . C215 C 0.6659(17) 0.8241(14) 0.3235(10) 0.024(6) Uiso 1 1 d . . . N221 N 0.6214(14) 0.5729(12) 0.3229(9) 0.029(5) Uiso 1 1 d . . . C222 C 0.6129(18) 0.4871(15) 0.3193(11) 0.028(6) Uiso 1 1 d . . . C223 C 0.7091(17) 0.4217(14) 0.3164(10) 0.025(6) Uiso 1 1 d . . . N224 N 0.7942(14) 0.4557(12) 0.3163(9) 0.030(5) Uiso 1 1 d . . . C225 C 0.8830(18) 0.3979(14) 0.3123(10) 0.029(6) Uiso 1 1 d . . . H225 H 0.9445 0.4190 0.3142 0.034 Uiso 1 1 calc R . . C226 C 0.8871(19) 0.3077(15) 0.3055(11) 0.033(6) Uiso 1 1 d . . . H226 H 0.9521 0.2693 0.2996 0.039 Uiso 1 1 calc R . . C227 C 0.8040(18) 0.2732(16) 0.3068(11) 0.030(6) Uiso 1 1 d . . . H227 H 0.8087 0.2099 0.3053 0.037 Uiso 1 1 calc R . . C228 C 0.7073(19) 0.3319(16) 0.3105(11) 0.037(7) Uiso 1 1 d . . . C229 C 0.6073(17) 0.3045(15) 0.3116(10) 0.027(6) Uiso 1 1 d . . . H229 H 0.6049 0.2420 0.3113 0.032 Uiso 1 1 calc R . . C230 C 0.5210(19) 0.3646(15) 0.3131(11) 0.035(7) Uiso 1 1 d . . . H230 H 0.4585 0.3450 0.3117 0.042 Uiso 1 1 calc R . . C231 C 0.5203(18) 0.4587(15) 0.3167(11) 0.032(6) Uiso 1 1 d . . . C232 C 0.4303(18) 0.5275(14) 0.3183(10) 0.030(6) Uiso 1 1 d . . . H232 H 0.3657 0.5132 0.3152 0.036 Uiso 1 1 calc R . . C233 C 0.4397(18) 0.6165(15) 0.3246(11) 0.032(6) Uiso 1 1 d . . . H233 H 0.3808 0.6631 0.3278 0.038 Uiso 1 1 calc R . . C234 C 0.5379(18) 0.6357(15) 0.3261(11) 0.030(6) Uiso 1 1 d . . . N241 N 0.7448(13) 0.5960(11) 0.4304(8) 0.020(4) Uiso 1 1 d . . . C242 C 0.8299(17) 0.6001(14) 0.4520(10) 0.021(6) Uiso 1 1 d . . . C243 C 0.9177(17) 0.6092(14) 0.4043(10) 0.025(6) Uiso 1 1 d . . . N244 N 0.9068(14) 0.6088(12) 0.3439(8) 0.026(5) Uiso 1 1 d . . . C245 C 0.9844(18) 0.6183(15) 0.2989(11) 0.029(6) Uiso 1 1 d . . . C246 C 1.0839(18) 0.6234(14) 0.3131(11) 0.027(6) Uiso 1 1 d . . . H246 H 1.1397 0.6276 0.2802 0.033 Uiso 1 1 calc R . . C247 C 1.0966(18) 0.6221(15) 0.3734(11) 0.032(6) Uiso 1 1 d . . . H247 H 1.1621 0.6259 0.3830 0.038 Uiso 1 1 calc R . . C248 C 1.0164(18) 0.6153(15) 0.4223(11) 0.030(6) Uiso 1 1 d . . . C249 C 1.020(2) 0.6156(15) 0.4901(11) 0.039(7) Uiso 1 1 d . . . H249 H 1.0823 0.6195 0.5040 0.047 Uiso 1 1 calc R . . C250 C 0.9365(18) 0.6104(15) 0.5319(12) 0.034(6) Uiso 1 1 d . . . H250 H 0.9411 0.6136 0.5748 0.041 Uiso 1 1 calc R . . C251 C 0.8414(18) 0.6005(15) 0.5166(11) 0.031(6) Uiso 1 1 d . . . C252 C 0.7525(18) 0.5952(14) 0.5571(12) 0.031(6) Uiso 1 1 d . . . H252 H 0.7542 0.5956 0.6008 0.037 Uiso 1 1 calc R . . C253 C 0.6591(18) 0.5893(14) 0.5383(11) 0.031(6) Uiso 1 1 d . . . H253 H 0.5981 0.5850 0.5669 0.038 Uiso 1 1 calc R . . C254 C 0.6651(19) 0.5904(15) 0.4709(11) 0.033(6) Uiso 1 1 d . . . H254 H 0.6041 0.5867 0.4553 0.040 Uiso 1 1 calc R . . Cl1 Cl 0.9507(5) 0.9161(4) 0.7447(3) 0.0301(16) Uiso 1 1 d . . . O1 O 0.8995(13) 1.0001(11) 0.7655(8) 0.043(5) Uiso 1 1 d . . . O2 O 0.8888(17) 0.8547(14) 0.7562(11) 0.086(7) Uiso 1 1 d . . . O3 O 0.9925(17) 0.9288(14) 0.6805(10) 0.079(7) Uiso 1 1 d . . . O4 O 1.0344(18) 0.8788(15) 0.7800(11) 0.088(7) Uiso 1 1 d . . . Cl2 Cl 0.8077(5) 0.6133(4) 0.7373(3) 0.0391(18) Uiso 1 1 d . . . O5 O 0.7727(17) 0.6877(14) 0.7734(10) 0.079(7) Uiso 1 1 d . . . O6 O 0.730(2) 0.5798(17) 0.7230(12) 0.105(8) Uiso 1 1 d . . . O7 O 0.8749(14) 0.6417(12) 0.6826(9) 0.059(5) Uiso 1 1 d . . . O8 O 0.8715(18) 0.5429(15) 0.7756(11) 0.089(7) Uiso 1 1 d . . . Cl3 Cl 0.3114(5) 0.6783(4) 0.4993(3) 0.0383(17) Uiso 1 1 d . . . O9 O 0.2445(14) 0.6279(12) 0.5412(9) 0.057(5) Uiso 1 1 d . . . O10 O 0.2946(15) 0.7694(13) 0.5131(9) 0.066(6) Uiso 1 1 d . . . O11 O 0.4126(18) 0.6395(15) 0.5025(11) 0.091(7) Uiso 1 1 d . . . O12 O 0.2885(16) 0.6782(14) 0.4351(10) 0.078(6) Uiso 1 1 d . . . Cl4 Cl 0.4024(6) 0.8183(5) 0.0072(3) 0.0478(19) Uiso 1 1 d . . . O13 O 0.438(2) 0.7297(18) -0.0008(13) 0.115(9) Uiso 1 1 d . . . O14 O 0.3138(15) 0.8530(13) -0.0255(9) 0.067(6) Uiso 1 1 d . . . O15 O 0.469(2) 0.865(2) -0.0196(15) 0.142(11) Uiso 1 1 d . . . O16 O 0.360(2) 0.810(2) 0.0733(15) 0.138(11) Uiso 1 1 d . . . N1 N 0.6681(19) 0.0679(16) 0.3368(12) 0.064(7) Uiso 1 1 d . . . C2 C 0.715(2) 0.0559(17) 0.3764(13) 0.046(7) Uiso 1 1 d . . . C3 C 0.785(2) 0.0393(19) 0.4232(14) 0.058(8) Uiso 1 1 d . . . N4 N 0.7660(15) 0.2240(13) 0.7249(10) 0.040(6) Uiso 1 1 d . . . C5 C 0.7827(19) 0.1744(16) 0.6888(12) 0.035(7) Uiso 1 1 d . . . C6 C 0.801(2) 0.1137(18) 0.6410(13) 0.056(8) Uiso 1 1 d . . . N7 N 0.491(2) 0.4616(17) 0.1502(12) 0.069(7) Uiso 1 1 d . . . C8 C 0.414(3) 0.515(2) 0.1492(15) 0.072(10) Uiso 1 1 d . . . C9 C 0.315(2) 0.588(2) 0.1468(14) 0.062(9) Uiso 1 1 d . . . N10 N 0.382(2) 0.0181(19) 0.3891(13) 0.085(9) Uiso 1 1 d . . . C11 C 0.326(2) 0.084(2) 0.3781(14) 0.061(9) Uiso 1 1 d . . . C12 C 0.251(2) 0.172(2) 0.3654(15) 0.070(9) Uiso 1 1 d . . . N13 N 0.191(3) 0.322(2) -0.0042(17) 0.115(11) Uiso 1 1 d . . . C14 C 0.253(3) 0.330(2) 0.0259(18) 0.081(11) Uiso 1 1 d . . . C15 C 0.323(3) 0.330(3) 0.070(2) 0.110(13) Uiso 1 1 d . . . N16 N 0.6907(19) 0.8275(14) 0.4826(11) 0.054(6) Uiso 1 1 d . . . C17 C 0.609(2) 0.8347(17) 0.4985(13) 0.043(7) Uiso 1 1 d . . . C18 C 0.498(3) 0.848(2) 0.5211(17) 0.089(11) Uiso 1 1 d . . . N19 N 0.8195(19) 0.4192(15) 0.1592(11) 0.060(7) Uiso 1 1 d . . . C20 C 0.905(3) 0.3920(19) 0.1472(14) 0.061(9) Uiso 1 1 d . . . C21 C 1.014(3) 0.351(2) 0.1319(18) 0.095(12) Uiso 1 1 d . . . N22 N 0.976(2) 0.8597(17) 0.4489(14) 0.079(8) Uiso 1 1 d . . . C23 C 0.996(2) 0.836(2) 0.5016(16) 0.065(9) Uiso 1 1 d . . . C24 C 1.028(2) 0.806(2) 0.5646(15) 0.066(9) Uiso 1 1 d . . . N25 N 0.123(3) 0.622(2) 1.0231(16) 0.112(11) Uiso 1 1 d . . . C26 C 0.211(3) 0.609(3) 0.9977(19) 0.100(13) Uiso 1 1 d . . . C27 C 0.307(3) 0.594(2) 0.9607(16) 0.079(10) Uiso 1 1 d . . . _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 Zn1 N124 2.043(18) . ? Zn1 N141 2.103(19) . ? Zn1 N121 2.182(18) . ? Zn1 N144 2.185(17) . ? Zn1 N111 2.215(19) . ? Zn1 N101 2.236(19) . ? Zn2 N244 2.043(19) . ? Zn2 N221 2.056(19) . ? Zn2 N201 2.184(17) . ? Zn2 N224 2.199(18) . ? Zn2 N241 2.204(17) . ? Zn2 N211 2.249(17) . ? N101 C102 1.31(3) . ? N101 C105 1.34(3) . ? C102 C125 1.51(3) . ? C102 S103 1.72(3) . ? S103 C104 1.70(2) . ? C104 C105 1.44(3) . ? C105 C215 1.42(3) . ? N111 C112 1.36(3) . ? N111 C115 1.40(3) . ? C112 C154 1.47(3) . ? C112 S113 1.70(2) . ? S113 C114 1.71(3) . ? C114 C115 1.35(3) . ? C115 C205 1.52(3) . ? N121 C122 1.33(3) . ? N121 C134 1.39(3) . ? C122 C131 1.43(3) . ? C122 C123 1.44(3) . ? C123 N124 1.35(3) . ? C123 C128 1.39(3) . ? N124 C125 1.40(3) . ? C125 C126 1.29(3) . ? C126 C127 1.42(3) . ? C127 C128 1.40(3) . ? C128 C129 1.45(3) . ? C129 C130 1.34(3) . ? C130 C131 1.38(3) . ? C131 C132 1.42(3) . ? C132 C133 1.35(3) . ? C133 C134 1.39(3) . ? N141 C154 1.30(3) . ? N141 C142 1.37(3) . ? C142 C151 1.37(3) . ? C142 C143 1.38(3) . ? C143 C148 1.38(3) . ? C143 N144 1.40(3) . ? N144 C145 1.30(3) . ? C145 C146 1.41(3) . ? C146 C147 1.36(3) . ? C147 C148 1.39(3) . ? C148 C149 1.42(3) . ? C149 C150 1.34(3) . ? C150 C151 1.46(3) . ? C151 C152 1.43(3) . ? C152 C153 1.34(3) . ? C153 C154 1.36(3) . ? N201 C202 1.34(3) . ? N201 C205 1.37(3) . ? C202 C245 1.46(3) . ? C202 S203 1.71(2) . ? S203 C204 1.69(3) . ? C204 C205 1.32(3) . ? N211 C212 1.29(3) . ? N211 C215 1.37(3) . ? C212 C234 1.47(3) . ? C212 S213 1.72(2) . ? S213 C214 1.69(2) . ? C214 C215 1.37(3) . ? N221 C234 1.32(3) . ? N221 C222 1.34(3) . ? C222 C231 1.40(3) . ? C222 C223 1.46(3) . ? C223 N224 1.34(3) . ? C223 C228 1.39(3) . ? N224 C225 1.33(3) . ? C225 C226 1.38(3) . ? C226 C227 1.31(3) . ? C227 C228 1.42(3) . ? C228 C229 1.48(3) . ? C229 C230 1.32(3) . ? C230 C231 1.43(3) . ? C231 C232 1.43(3) . ? C232 C233 1.40(3) . ? C233 C234 1.41(3) . ? N241 C254 1.28(3) . ? N241 C242 1.32(3) . ? C242 C251 1.43(3) . ? C242 C243 1.45(3) . ? C243 N244 1.34(3) . ? C243 C248 1.46(3) . ? N244 C245 1.32(3) . ? C245 C246 1.44(3) . ? C246 C247 1.34(3) . ? C247 C248 1.39(3) . ? C248 C249 1.48(3) . ? C249 C250 1.33(3) . ? C250 C251 1.41(3) . ? C251 C252 1.37(3) . ? C252 C253 1.40(3) . ? C253 C254 1.45(3) . ? Cl1 O2 1.33(2) . ? Cl1 O3 1.41(2) . ? Cl1 O1 1.420(17) . ? Cl1 O4 1.44(2) . ? Cl2 O6 1.34(3) . ? Cl2 O5 1.43(2) . ? Cl2 O7 1.431(18) . ? Cl2 O8 1.47(2) . ? Cl3 O11 1.38(2) . ? Cl3 O9 1.413(18) . ? Cl3 O10 1.418(19) . ? Cl3 O12 1.47(2) . ? Cl4 O15 1.25(3) . ? Cl4 O13 1.36(3) . ? Cl4 O16 1.44(3) . ? Cl4 O14 1.45(2) . ? N1 C2 1.12(3) . ? C2 C3 1.45(4) . ? N4 C5 1.13(3) . ? C5 C6 1.45(4) . ? N7 C8 1.18(3) . ? C8 C9 1.55(4) . ? N10 C11 1.14(3) . ? C11 C12 1.52(4) . ? N13 C14 1.18(4) . ? C14 C15 1.45(5) . ? N16 C17 1.08(3) . ? C17 C18 1.48(4) . ? N19 C20 1.14(3) . ? C20 C21 1.49(4) . ? N22 C23 1.20(4) . ? C23 C24 1.47(4) . ? N25 C26 1.21(4) . ? C26 C27 1.41(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 N124 Zn1 N141 170.1(7) . . ? N124 Zn1 N121 74.6(7) . . ? N141 Zn1 N121 97.8(7) . . ? N124 Zn1 N144 98.3(7) . . ? N141 Zn1 N144 76.6(7) . . ? N121 Zn1 N144 100.9(6) . . ? N124 Zn1 N111 112.5(7) . . ? N141 Zn1 N111 73.4(7) . . ? N121 Zn1 N111 90.5(7) . . ? N144 Zn1 N111 149.1(7) . . ? N124 Zn1 N101 74.7(7) . . ? N141 Zn1 N101 113.6(7) . . ? N121 Zn1 N101 148.1(7) . . ? N144 Zn1 N101 91.9(7) . . ? N111 Zn1 N101 93.2(7) . . ? N244 Zn2 N221 169.0(7) . . ? N244 Zn2 N201 73.3(7) . . ? N221 Zn2 N201 114.8(7) . . ? N244 Zn2 N224 96.8(7) . . ? N221 Zn2 N224 76.1(7) . . ? N201 Zn2 N224 91.7(7) . . ? N244 Zn2 N241 77.0(7) . . ? N221 Zn2 N241 95.9(7) . . ? N201 Zn2 N241 148.8(7) . . ? N224 Zn2 N241 101.1(6) . . ? N244 Zn2 N211 114.2(7) . . ? N221 Zn2 N211 73.6(7) . . ? N201 Zn2 N211 94.6(6) . . ? N224 Zn2 N211 148.9(7) . . ? N241 Zn2 N211 88.9(6) . . ? C102 N101 C105 115(2) . . ? C102 N101 Zn1 111.4(15) . . ? C105 N101 Zn1 132.3(15) . . ? N101 C102 C125 121(2) . . ? N101 C102 S103 112.4(17) . . ? C125 C102 S103 125.6(18) . . ? C104 S103 C102 90.9(12) . . ? C105 C104 S103 109.6(17) . . ? N101 C105 C215 120(2) . . ? N101 C105 C104 112(2) . . ? C215 C105 C104 127(2) . . ? C112 N111 C115 107.0(19) . . ? C112 N111 Zn1 113.2(14) . . ? C115 N111 Zn1 138.7(16) . . ? N111 C112 C154 116(2) . . ? N111 C112 S113 115.7(16) . . ? C154 C112 S113 127.9(18) . . ? C112 S113 C114 90.1(12) . . ? C115 C114 S113 109.7(19) . . ? C114 C115 N111 117(2) . . ? C114 C115 C205 128(2) . . ? N111 C115 C205 114(2) . . ? C122 N121 C134 119.0(19) . . ? C122 N121 Zn1 114.5(15) . . ? C134 N121 Zn1 126.5(14) . . ? N121 C122 C131 125(2) . . ? N121 C122 C123 117(2) . . ? C131 C122 C123 118(2) . . ? N124 C123 C128 125(2) . . ? N124 C123 C122 112.2(19) . . ? C128 C123 C122 122(2) . . ? C123 N124 C125 113.9(18) . . ? C123 N124 Zn1 121.4(16) . . ? C125 N124 Zn1 124.4(14) . . ? C126 C125 N124 124(2) . . ? C126 C125 C102 130(2) . . ? N124 C125 C102 105.7(19) . . ? C125 C126 C127 121(2) . . ? C128 C127 C126 117(2) . . ? C123 C128 C127 118(2) . . ? C123 C128 C129 118(2) . . ? C127 C128 C129 124(2) . . ? C130 C129 C128 118(2) . . ? C129 C130 C131 127(3) . . ? C130 C131 C132 129(2) . . ? C130 C131 C122 117(2) . . ? C132 C131 C122 114(2) . . ? C133 C132 C131 121(2) . . ? C132 C133 C134 122(3) . . ? C133 C134 N121 118(2) . . ? C154 N141 C142 122(2) . . ? C154 N141 Zn1 122.2(16) . . ? C142 N141 Zn1 115.7(15) . . ? C151 C142 N141 119(2) . . ? C151 C142 C143 122(2) . . ? N141 C142 C143 118(2) . . ? C142 C143 C148 122(2) . . ? C142 C143 N144 116(2) . . ? C148 C143 N144 121(2) . . ? C145 N144 C143 117(2) . . ? C145 N144 Zn1 129.7(16) . . ? C143 N144 Zn1 112.6(14) . . ? N144 C145 C146 124(2) . . ? C147 C146 C145 118(3) . . ? C146 C147 C148 120(2) . . ? C143 C148 C147 119(2) . . ? C143 C148 C149 115(2) . . ? C147 C148 C149 126(2) . . ? C150 C149 C148 124(2) . . ? C149 C150 C151 119(2) . . ? C142 C151 C152 118(2) . . ? C142 C151 C150 117(2) . . ? C152 C151 C150 125(2) . . ? C153 C152 C151 118(2) . . ? C152 C153 C154 122(2) . . ? N141 C154 C153 120(2) . . ? N141 C154 C112 113(2) . . ? C153 C154 C112 127(2) . . ? C202 N201 C205 107.9(19) . . ? C202 N201 Zn2 114.3(15) . . ? C205 N201 Zn2 136.8(16) . . ? N201 C202 C245 116(2) . . ? N201 C202 S203 115.5(18) . . ? C245 C202 S203 128.3(19) . . ? C204 S203 C202 88.1(13) . . ? C205 C204 S203 112(2) . . ? C204 C205 N201 116(2) . . ? C204 C205 C115 129(2) . . ? N201 C205 C115 114(2) . . ? C212 N211 C215 112.8(18) . . ? C212 N211 Zn2 112.4(14) . . ? C215 N211 Zn2 133.9(14) . . ? N211 C212 C234 118.2(19) . . ? N211 C212 S213 113.9(16) . . ? C234 C212 S213 127.8(17) . . ? C214 S213 C212 89.1(11) . . ? C215 C214 S213 111.7(18) . . ? C214 C215 N211 112(2) . . ? C214 C215 C105 129(2) . . ? N211 C215 C105 118.1(19) . . ? C234 N221 C222 119(2) . . ? C234 N221 Zn2 122.1(16) . . ? C222 N221 Zn2 118.9(15) . . ? N221 C222 C231 124(2) . . ? N221 C222 C223 115(2) . . ? C231 C222 C223 120(2) . . ? N224 C223 C228 125(2) . . ? N224 C223 C222 116.1(19) . . ? C228 C223 C222 119(2) . . ? C225 N224 C223 117.2(19) . . ? C225 N224 Zn2 129.4(16) . . ? C223 N224 Zn2 113.4(14) . . ? N224 C225 C226 121(2) . . ? C227 C226 C225 122(2) . . ? C226 C227 C228 119(2) . . ? C223 C228 C227 115(2) . . ? C223 C228 C229 119(2) . . ? C227 C228 C229 126(2) . . ? C230 C229 C228 122(2) . . ? C229 C230 C231 121(2) . . ? C222 C231 C232 117(2) . . ? C222 C231 C230 119(2) . . ? C232 C231 C230 124(2) . . ? C233 C232 C231 119(2) . . ? C232 C233 C234 119(2) . . ? N221 C234 C233 123(2) . . ? N221 C234 C212 112(2) . . ? C233 C234 C212 125(2) . . ? C254 N241 C242 117(2) . . ? C254 N241 Zn2 129.6(17) . . ? C242 N241 Zn2 113.2(13) . . ? N241 C242 C251 126(2) . . ? N241 C242 C243 115.4(19) . . ? C251 C242 C243 118(2) . . ? N244 C243 C242 118(2) . . ? N244 C243 C248 121.2(19) . . ? C242 C243 C248 121(2) . . ? C245 N244 C243 120(2) . . ? C245 N244 Zn2 123.6(16) . . ? C243 N244 Zn2 116.2(14) . . ? N244 C245 C246 122(2) . . ? N244 C245 C202 111(2) . . ? C246 C245 C202 127(2) . . ? C247 C246 C245 119(2) . . ? C246 C247 C248 122(2) . . ? C247 C248 C243 116(2) . . ? C247 C248 C249 127(2) . . ? C243 C248 C249 117(2) . . ? C250 C249 C248 121(2) . . ? C249 C250 C251 124(2) . . ? C252 C251 C250 127(2) . . ? C252 C251 C242 113(2) . . ? C250 C251 C242 120(2) . . ? C251 C252 C253 124(2) . . ? C252 C253 C254 113(2) . . ? N241 C254 C253 126(2) . . ? O2 Cl1 O3 112.0(14) . . ? O2 Cl1 O1 111.0(12) . . ? O3 Cl1 O1 111.1(11) . . ? O2 Cl1 O4 105.9(13) . . ? O3 Cl1 O4 107.2(13) . . ? O1 Cl1 O4 109.5(12) . . ? O6 Cl2 O5 112.3(15) . . ? O6 Cl2 O7 112.7(14) . . ? O5 Cl2 O7 108.8(12) . . ? O6 Cl2 O8 110.2(15) . . ? O5 Cl2 O8 106.7(13) . . ? O7 Cl2 O8 105.8(12) . . ? O11 Cl3 O9 111.5(12) . . ? O11 Cl3 O10 109.3(14) . . ? O9 Cl3 O10 110.5(11) . . ? O11 Cl3 O12 109.0(14) . . ? O9 Cl3 O12 107.1(12) . . ? O10 Cl3 O12 109.4(12) . . ? O15 Cl4 O13 108.9(19) . . ? O15 Cl4 O16 127(2) . . ? O13 Cl4 O16 101.0(16) . . ? O15 Cl4 O14 104.9(17) . . ? O13 Cl4 O14 109.9(15) . . ? O16 Cl4 O14 104.4(15) . . ? N1 C2 C3 175(3) . . ? N4 C5 C6 177(3) . . ? N7 C8 C9 178(3) . . ? N10 C11 C12 178(4) . . ? N13 C14 C15 171(4) . . ? N16 C17 C18 178(3) . . ? N19 C20 C21 177(3) . . ? N22 C23 C24 177(3) . . ? N25 C26 C27 172(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.375 _refine_diff_density_min -3.407 _refine_diff_density_rms 0.254 #=END data_trialm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 Cl4 Cu2 N14 O24 S4' _chemical_formula_weight 1568.02 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' 'Cl' 'Cl' 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0704(17) _cell_length_b 13.675(2) _cell_length_c 19.688(3) _cell_angle_alpha 94.440(3) _cell_angle_beta 104.884(3) _cell_angle_gamma 106.271(3) _cell_volume 2975.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 1.130 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31484 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.1599 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.68 _reflns_number_total 13557 _reflns_number_gt 5997 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1042P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13557 _refine_ls_number_parameters 847 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1749 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2080 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 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 0.66228(7) 0.20148(6) 0.25108(3) 0.0324(2) Uani 1 1 d . . . Cu2 Cu 0.40527(9) 0.36882(8) 0.24509(4) 0.0631(3) Uani 1 1 d . . . N111 N 0.6483(5) 0.1038(4) 0.3222(2) 0.0321(12) Uani 1 1 d . . . C112 C 0.5994(6) 0.0024(5) 0.3077(3) 0.0418(17) Uani 1 1 d . . . H146 H 0.5637 -0.0297 0.2594 0.050 Uiso 1 1 calc R . . C113 C 0.5985(7) -0.0590(6) 0.3608(4) 0.0506(19) Uani 1 1 d . . . H145 H 0.5616 -0.1317 0.3492 0.061 Uiso 1 1 calc R . . C114 C 0.6531(7) -0.0113(6) 0.4311(4) 0.052(2) Uani 1 1 d . . . H144 H 0.6546 -0.0512 0.4686 0.063 Uiso 1 1 calc R . . C115 C 0.7038(6) 0.0920(6) 0.4458(3) 0.0412(17) Uani 1 1 d . . . H143 H 0.7401 0.1250 0.4939 0.049 Uiso 1 1 calc R . . C116 C 0.7034(5) 0.1505(5) 0.3913(3) 0.0334(15) Uani 1 1 d . . . N121 N 0.7461(4) 0.3022(4) 0.3382(2) 0.0308(12) Uani 1 1 d . . . C122 C 0.7572(5) 0.2610(5) 0.4006(3) 0.0306(14) Uani 1 1 d . . . C123 C 0.8163(5) 0.3339(5) 0.4599(3) 0.0380(16) Uani 1 1 d . . . H124 H 0.8326 0.3192 0.5072 0.046 Uiso 1 1 calc R . . S124 S 0.85691(15) 0.45358(14) 0.43868(8) 0.0389(4) Uani 1 1 d . . . C125 C 0.7941(5) 0.4031(5) 0.3500(3) 0.0304(14) Uani 1 1 d . . . N131 N 0.6792(4) 0.4159(4) 0.2390(2) 0.0313(12) Uani 1 1 d . . . C132 C 0.7826(5) 0.4623(5) 0.2908(3) 0.0302(14) Uani 1 1 d . . . C133 C 0.8662(6) 0.5524(5) 0.2864(3) 0.0402(16) Uani 1 1 d . . . H253 H 0.9357 0.5852 0.3256 0.048 Uiso 1 1 calc R . . C134 C 0.8480(6) 0.5938(5) 0.2251(4) 0.0448(18) Uani 1 1 d . . . H254 H 0.9065 0.6537 0.2202 0.054 Uiso 1 1 calc R . . C135 C 0.7423(6) 0.5468(5) 0.1701(3) 0.0449(18) Uani 1 1 d . . . H255 H 0.7272 0.5737 0.1268 0.054 Uiso 1 1 calc R . . C136 C 0.6592(5) 0.4595(5) 0.1800(3) 0.0309(14) Uani 1 1 d . . . N141 N 0.4502(4) 0.3577(4) 0.1507(2) 0.0301(12) Uani 1 1 d . . . C142 C 0.5413(6) 0.4039(5) 0.1286(3) 0.0340(15) Uani 1 1 d . . . S143 S 0.51215(16) 0.38020(14) 0.03767(8) 0.0415(4) Uani 1 1 d . . . C144 C 0.3688(6) 0.3033(5) 0.0295(3) 0.0401(16) Uani 1 1 d . . . H214 H 0.3104 0.2688 -0.0144 0.048 Uiso 1 1 calc R . . C145 C 0.3502(6) 0.2985(5) 0.0947(3) 0.0333(15) Uani 1 1 d . . . N151 N 0.2568(5) 0.2604(4) 0.1862(3) 0.0371(13) Uani 1 1 d . . . C152 C 0.2468(6) 0.2415(5) 0.1155(3) 0.0359(15) Uani 1 1 d . . . C153 C 0.1433(6) 0.1699(6) 0.0691(4) 0.0460(18) Uani 1 1 d . . . H233 H 0.1359 0.1574 0.0197 0.055 Uiso 1 1 calc R . . C154 C 0.0532(7) 0.1182(6) 0.0947(4) 0.055(2) Uani 1 1 d . . . H234 H -0.0165 0.0678 0.0636 0.065 Uiso 1 1 calc R . . C155 C 0.0635(6) 0.1392(6) 0.1662(4) 0.057(2) Uani 1 1 d . . . H235 H 0.0004 0.1053 0.1849 0.069 Uiso 1 1 calc R . . C156 C 0.1664(6) 0.2096(6) 0.2092(4) 0.0455(18) Uani 1 1 d . . . H236 H 0.1738 0.2232 0.2585 0.055 Uiso 1 1 calc R . . N211 N 0.7579(5) 0.2496(4) 0.1836(2) 0.0350(13) Uani 1 1 d . . . C212 C 0.8729(6) 0.3072(6) 0.2014(4) 0.0422(17) Uani 1 1 d . . . H136 H 0.9152 0.3313 0.2503 0.051 Uiso 1 1 calc R . . C213 C 0.9329(7) 0.3332(6) 0.1517(4) 0.057(2) Uani 1 1 d . . . H135 H 1.0150 0.3751 0.1662 0.068 Uiso 1 1 calc R . . C214 C 0.8731(8) 0.2980(7) 0.0809(4) 0.067(2) Uani 1 1 d . . . H134 H 0.9135 0.3149 0.0458 0.080 Uiso 1 1 calc R . . C215 C 0.7544(7) 0.2383(6) 0.0613(3) 0.0495(19) Uani 1 1 d . . . H133 H 0.7114 0.2153 0.0123 0.059 Uiso 1 1 calc R . . C216 C 0.6967(6) 0.2114(5) 0.1133(3) 0.0368(16) Uani 1 1 d . . . N221 N 0.5382(5) 0.1289(4) 0.1615(2) 0.0320(12) Uani 1 1 d . . . C222 C 0.5754(6) 0.1470(5) 0.1011(3) 0.0364(16) Uani 1 1 d . . . C223 C 0.4832(6) 0.1014(5) 0.0395(3) 0.0410(17) Uani 1 1 d . . . H114 H 0.4900 0.1075 -0.0071 0.049 Uiso 1 1 calc R . . S224 S 0.35622(17) 0.03316(14) 0.05740(8) 0.0451(5) Uani 1 1 d . . . C225 C 0.4265(6) 0.0698(5) 0.1468(3) 0.0345(15) Uani 1 1 d . . . N231 N 0.4104(4) 0.1366(4) 0.2545(2) 0.0305(12) Uani 1 1 d . . . C232 C 0.3674(6) 0.0521(5) 0.2037(3) 0.0333(15) Uani 1 1 d . . . C233 C 0.2826(6) -0.0370(5) 0.2055(4) 0.0465(18) Uani 1 1 d . . . H153 H 0.2540 -0.0936 0.1677 0.056 Uiso 1 1 calc R . . C234 C 0.2398(7) -0.0421(6) 0.2642(4) 0.0487(19) Uani 1 1 d . . . H154 H 0.1815 -0.1034 0.2674 0.058 Uiso 1 1 calc R . . C235 C 0.2816(6) 0.0420(5) 0.3186(4) 0.0446(18) Uani 1 1 d . . . H155 H 0.2539 0.0394 0.3596 0.054 Uiso 1 1 calc R . . C236 C 0.3654(6) 0.1299(5) 0.3104(3) 0.0332(15) Uani 1 1 d . . . N241 N 0.4430(5) 0.3178(4) 0.3391(2) 0.0350(13) Uani 1 1 d . . . C242 C 0.4156(6) 0.2280(5) 0.3613(3) 0.0350(15) Uani 1 1 d . . . S243 S 0.46636(17) 0.23726(15) 0.45172(8) 0.0430(4) Uani 1 1 d . . . C244 C 0.5290(6) 0.3661(5) 0.4600(3) 0.0417(17) Uani 1 1 d . . . H224 H 0.5713 0.4107 0.5041 0.050 Uiso 1 1 calc R . . C245 C 0.5110(6) 0.3979(5) 0.3953(3) 0.0340(15) Uani 1 1 d . . . N251 N 0.5152(5) 0.4998(4) 0.3045(3) 0.0365(13) Uani 1 1 d . . . C252 C 0.5545(6) 0.4991(5) 0.3748(3) 0.0340(15) Uani 1 1 d . . . C253 C 0.6368(6) 0.5843(5) 0.4223(3) 0.0394(16) Uani 1 1 d . . . H243 H 0.6610 0.5822 0.4719 0.047 Uiso 1 1 calc R . . C254 C 0.6826(7) 0.6725(6) 0.3955(4) 0.052(2) Uani 1 1 d . . . H244 H 0.7422 0.7310 0.4262 0.063 Uiso 1 1 calc R . . C255 C 0.6409(7) 0.6746(6) 0.3234(4) 0.0492(19) Uani 1 1 d . . . H245 H 0.6705 0.7349 0.3043 0.059 Uiso 1 1 calc R . . C256 C 0.5555(6) 0.5877(5) 0.2797(4) 0.0446(17) Uani 1 1 d . . . H246 H 0.5244 0.5904 0.2306 0.053 Uiso 1 1 calc R . . Cl1 Cl 0.00736(15) 0.84267(13) 0.38214(8) 0.0405(4) Uani 1 1 d . . . O11 O 0.1107(4) 0.9306(4) 0.4178(2) 0.0518(13) Uani 1 1 d . . . O12 O 0.0098(5) 0.7563(4) 0.4198(2) 0.0548(14) Uani 1 1 d . . . O13 O -0.1014(4) 0.8676(4) 0.3804(3) 0.0566(14) Uani 1 1 d . . . O14 O 0.0078(5) 0.8152(4) 0.3102(2) 0.0585(15) Uani 1 1 d . . . Cl2 Cl 0.47095(17) 0.76940(16) 0.14087(9) 0.0536(5) Uani 1 1 d . . . O21 O 0.5430(8) 0.7146(7) 0.1270(4) 0.126(3) Uani 1 1 d . . . O22 O 0.4704(8) 0.7737(6) 0.2113(3) 0.119(3) Uani 1 1 d . . . O23 O 0.3541(8) 0.7330(10) 0.0971(5) 0.200(5) Uani 1 1 d . . . O24 O 0.5091(9) 0.8727(6) 0.1275(4) 0.124(3) Uani 1 1 d . . . Cl3 Cl -0.00173(17) 0.74230(19) 0.09097(9) 0.0590(6) Uani 1 1 d . . . O31 O 0.0662(5) 0.7275(5) 0.1582(3) 0.0746(18) Uani 1 1 d . . . O32 O -0.1135(6) 0.7446(8) 0.0953(4) 0.136(4) Uani 1 1 d . . . O33 O -0.0364(8) 0.6542(7) 0.0362(4) 0.138(3) Uani 1 1 d . . . O34 O 0.0654(7) 0.8197(8) 0.0663(4) 0.180(5) Uani 1 1 d . . . Cl4 Cl 0.16192(19) 0.43103(16) 0.37294(9) 0.0596(6) Uani 1 1 d . . . O41 O 0.2584(9) 0.4114(15) 0.4050(5) 0.282(10) Uani 1 1 d . . . O42 O 0.1627(10) 0.5311(6) 0.4022(4) 0.141(4) Uani 1 1 d . . . O43 O 0.0571(6) 0.3646(6) 0.3812(4) 0.101(2) Uani 1 1 d . . . O44 O 0.1511(8) 0.4251(6) 0.2996(3) 0.134(4) Uani 1 1 d . . . N51 N 0.6736(6) 0.2780(6) 0.6359(3) 0.0545(17) Uani 1 1 d U . . O52 O 0.6905(8) 0.2196(7) 0.5954(4) 0.125(3) Uani 1 1 d U . . O53 O 0.5889(6) 0.3077(6) 0.6199(3) 0.083(2) Uani 1 1 d U . . C54 C 0.7602(8) 0.3163(7) 0.7093(4) 0.069(3) Uani 1 1 d U . . N61 N 0.2502(13) 0.5068(9) 0.1183(13) 0.240(13) Uani 1 1 d U . . O62 O 0.2826(9) 0.4761(6) 0.1798(7) 0.142(4) Uani 1 1 d U . . C63 C 0.3359(17) 0.5099(14) 0.0688(11) 0.180(9) Uani 1 1 d U . . O64 O 0.1530(10) 0.5374(10) 0.0806(7) 0.215(6) Uani 1 1 d U . . N71 N 0.7746(5) 0.9578(6) 0.1533(4) 0.0557(17) Uani 1 1 d U . . O72 O 0.7487(8) 1.0276(6) 0.1767(5) 0.120(3) Uani 1 1 d U . . O73 O 0.7653(6) 0.9368(6) 0.0915(3) 0.096(2) Uani 1 1 d U . . C74 C 0.8228(7) 0.8967(6) 0.2057(4) 0.057(2) Uani 1 1 d U . . O82 O 0.0617(10) 0.1183(7) 0.3297(4) 0.126(3) Uani 1 1 d U . . N81 N 0.125(3) 0.1592(13) 0.4031(12) 0.317(14) Uani 1 1 d U . . O83 O -0.0450(17) 0.1362(7) 0.3404(7) 0.246(9) Uani 1 1 d U . . C84 C 0.0109(8) 0.1312(7) 0.4369(4) 0.064(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0370(5) 0.0371(5) 0.0184(3) 0.0020(3) 0.0068(3) 0.0059(4) Cu2 0.0637(6) 0.0670(7) 0.0264(4) 0.0120(4) 0.0008(4) -0.0199(5) N111 0.038(3) 0.031(3) 0.027(3) 0.006(2) 0.007(2) 0.011(2) C112 0.051(4) 0.038(4) 0.040(4) 0.009(3) 0.018(3) 0.014(3) C113 0.059(5) 0.041(4) 0.054(4) 0.013(3) 0.018(4) 0.014(4) C114 0.069(5) 0.053(5) 0.035(4) 0.019(3) 0.015(4) 0.018(4) C115 0.048(4) 0.051(5) 0.027(3) 0.011(3) 0.010(3) 0.017(4) C116 0.030(3) 0.048(4) 0.023(3) 0.010(3) 0.002(3) 0.018(3) N121 0.030(3) 0.037(3) 0.022(2) 0.004(2) 0.004(2) 0.010(2) C122 0.032(3) 0.045(4) 0.021(3) 0.007(3) 0.011(3) 0.019(3) C123 0.032(4) 0.053(4) 0.022(3) 0.000(3) -0.001(3) 0.013(3) S124 0.0362(9) 0.0466(11) 0.0261(8) -0.0059(7) 0.0009(7) 0.0113(8) C125 0.027(3) 0.037(4) 0.024(3) -0.001(3) 0.003(2) 0.011(3) N131 0.030(3) 0.036(3) 0.026(3) 0.004(2) 0.004(2) 0.012(2) C132 0.029(3) 0.030(4) 0.031(3) 0.001(3) 0.009(3) 0.009(3) C133 0.038(4) 0.042(4) 0.040(4) 0.009(3) 0.015(3) 0.008(3) C134 0.044(4) 0.035(4) 0.052(4) 0.009(3) 0.021(3) 0.000(3) C135 0.052(4) 0.044(4) 0.036(4) 0.014(3) 0.011(3) 0.009(4) C136 0.031(3) 0.034(4) 0.031(3) 0.010(3) 0.013(3) 0.011(3) N141 0.032(3) 0.031(3) 0.023(2) 0.004(2) 0.001(2) 0.009(2) C142 0.042(4) 0.033(4) 0.027(3) 0.009(3) 0.008(3) 0.011(3) S143 0.0516(11) 0.0449(11) 0.0281(8) 0.0123(7) 0.0112(7) 0.0138(9) C144 0.044(4) 0.037(4) 0.035(4) 0.011(3) 0.003(3) 0.013(3) C145 0.040(4) 0.031(4) 0.025(3) 0.003(3) 0.003(3) 0.012(3) N151 0.033(3) 0.041(3) 0.034(3) 0.011(2) 0.004(2) 0.010(3) C152 0.032(4) 0.038(4) 0.032(3) 0.009(3) 0.003(3) 0.008(3) C153 0.040(4) 0.049(5) 0.037(4) 0.009(3) -0.001(3) 0.005(4) C154 0.036(4) 0.066(6) 0.048(4) 0.005(4) 0.003(3) 0.005(4) C155 0.031(4) 0.065(6) 0.068(5) 0.017(4) 0.012(4) 0.000(4) C156 0.039(4) 0.054(5) 0.046(4) 0.015(3) 0.013(3) 0.016(4) N211 0.046(3) 0.038(3) 0.029(3) 0.007(2) 0.016(2) 0.019(3) C212 0.040(4) 0.052(5) 0.040(4) 0.010(3) 0.020(3) 0.014(4) C213 0.048(5) 0.075(6) 0.056(5) 0.010(4) 0.032(4) 0.017(4) C214 0.085(7) 0.078(6) 0.048(5) 0.015(4) 0.045(5) 0.018(5) C215 0.073(6) 0.052(5) 0.029(3) 0.006(3) 0.025(4) 0.019(4) C216 0.048(4) 0.045(4) 0.023(3) 0.009(3) 0.013(3) 0.021(3) N221 0.038(3) 0.037(3) 0.018(2) 0.000(2) 0.006(2) 0.010(3) C222 0.052(4) 0.035(4) 0.028(3) 0.003(3) 0.013(3) 0.022(3) C223 0.062(5) 0.039(4) 0.019(3) -0.002(3) 0.002(3) 0.022(4) S224 0.0544(11) 0.0425(11) 0.0270(8) -0.0059(7) -0.0055(7) 0.0163(9) C225 0.037(4) 0.034(4) 0.027(3) -0.003(3) -0.001(3) 0.014(3) N231 0.026(3) 0.032(3) 0.032(3) 0.004(2) 0.007(2) 0.008(2) C232 0.035(4) 0.034(4) 0.033(3) 0.005(3) 0.007(3) 0.016(3) C233 0.038(4) 0.034(4) 0.056(4) 0.001(3) 0.006(3) 0.002(3) C234 0.046(4) 0.037(4) 0.069(5) 0.009(4) 0.028(4) 0.011(4) C235 0.040(4) 0.041(4) 0.061(5) 0.021(4) 0.026(4) 0.011(3) C236 0.033(4) 0.039(4) 0.034(3) 0.007(3) 0.014(3) 0.017(3) N241 0.041(3) 0.040(3) 0.027(3) 0.006(2) 0.015(2) 0.013(3) C242 0.042(4) 0.039(4) 0.032(3) 0.010(3) 0.018(3) 0.016(3) S243 0.0540(11) 0.0494(11) 0.0326(8) 0.0155(8) 0.0196(8) 0.0185(9) C244 0.042(4) 0.052(5) 0.032(3) 0.005(3) 0.018(3) 0.011(3) C245 0.037(4) 0.043(4) 0.029(3) 0.006(3) 0.014(3) 0.019(3) N251 0.039(3) 0.037(3) 0.036(3) 0.010(2) 0.011(2) 0.015(3) C252 0.037(4) 0.036(4) 0.036(3) 0.004(3) 0.017(3) 0.016(3) C253 0.040(4) 0.041(4) 0.038(4) 0.000(3) 0.013(3) 0.013(3) C254 0.052(5) 0.042(5) 0.062(5) -0.011(4) 0.024(4) 0.010(4) C255 0.056(5) 0.036(4) 0.068(5) 0.016(4) 0.036(4) 0.015(4) C256 0.049(4) 0.041(4) 0.053(4) 0.015(3) 0.022(4) 0.020(4) Cl1 0.0459(10) 0.0440(10) 0.0292(8) 0.0086(7) 0.0081(7) 0.0122(8) O11 0.047(3) 0.049(3) 0.047(3) 0.003(2) 0.003(2) 0.005(2) O12 0.081(4) 0.043(3) 0.042(3) 0.015(2) 0.012(3) 0.024(3) O13 0.043(3) 0.067(4) 0.064(3) 0.016(3) 0.013(2) 0.026(3) O14 0.075(4) 0.074(4) 0.023(2) 0.006(2) 0.012(2) 0.021(3) Cl2 0.0525(11) 0.0678(14) 0.0297(9) 0.0108(8) 0.0041(8) 0.0083(10) O21 0.179(8) 0.158(8) 0.077(5) 0.002(5) 0.036(5) 0.114(7) O22 0.236(10) 0.098(6) 0.047(4) 0.030(3) 0.051(5) 0.077(6) O23 0.094(7) 0.290(15) 0.142(8) 0.026(8) -0.044(6) 0.020(8) O24 0.201(9) 0.108(6) 0.130(6) 0.073(5) 0.110(6) 0.084(6) Cl3 0.0454(11) 0.0974(17) 0.0316(9) 0.0165(10) 0.0071(8) 0.0202(11) O31 0.057(3) 0.117(5) 0.039(3) 0.029(3) -0.002(2) 0.020(3) O32 0.078(5) 0.291(12) 0.087(5) 0.071(6) 0.030(4) 0.115(7) O33 0.161(8) 0.171(9) 0.077(5) -0.018(5) 0.024(5) 0.062(7) O34 0.103(6) 0.228(11) 0.100(6) 0.104(7) -0.048(5) -0.068(6) Cl4 0.0696(14) 0.0529(12) 0.0341(9) -0.0036(8) 0.0131(9) -0.0109(10) O41 0.129(8) 0.70(3) 0.089(6) 0.042(11) 0.014(6) 0.262(14) O42 0.248(11) 0.074(5) 0.088(5) -0.011(4) 0.085(6) 0.000(6) O43 0.077(5) 0.116(6) 0.105(5) 0.005(4) 0.050(4) 0.004(4) O44 0.202(9) 0.100(6) 0.038(3) -0.024(3) 0.039(4) -0.041(6) N51 0.058(4) 0.073(5) 0.044(4) 0.017(3) 0.019(3) 0.032(4) O52 0.141(7) 0.168(8) 0.072(5) -0.027(5) 0.010(5) 0.089(7) O53 0.066(4) 0.137(6) 0.065(4) 0.039(4) 0.023(3) 0.052(4) C54 0.064(5) 0.084(7) 0.040(4) 0.010(4) -0.002(4) 0.009(5) N61 0.107(10) 0.043(7) 0.46(3) -0.018(12) -0.092(15) 0.032(7) O62 0.131(8) 0.063(6) 0.268(13) 0.012(7) 0.126(9) 0.029(5) C63 0.184(16) 0.177(17) 0.30(2) 0.118(16) 0.162(17) 0.135(15) O64 0.124(8) 0.220(13) 0.259(14) 0.081(10) -0.035(8) 0.059(9) N71 0.039(4) 0.056(5) 0.066(5) 0.021(4) 0.003(3) 0.013(3) O72 0.145(7) 0.080(6) 0.150(7) 0.018(5) 0.028(6) 0.072(6) O73 0.073(4) 0.183(8) 0.045(4) 0.043(4) 0.017(3) 0.053(5) C74 0.072(6) 0.061(5) 0.040(4) 0.021(4) 0.000(4) 0.035(5) O82 0.210(10) 0.121(7) 0.100(6) 0.052(5) 0.090(7) 0.084(7) N81 0.67(5) 0.109(13) 0.32(3) 0.034(14) 0.28(3) 0.22(2) O83 0.47(2) 0.076(6) 0.230(13) -0.016(7) 0.300(16) -0.024(11) C84 0.078(6) 0.080(6) 0.046(4) 0.008(4) 0.030(4) 0.035(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 Cu1 N121 1.956(5) . ? Cu1 N221 1.969(5) . ? Cu1 N211 2.007(5) . ? Cu1 N111 2.014(5) . ? Cu2 N251 1.971(5) . ? Cu2 N151 1.983(5) . ? Cu2 N241 2.016(5) . ? Cu2 N141 2.071(5) . ? N111 C112 1.321(8) . ? N111 C116 1.366(7) . ? C112 C113 1.390(9) . ? C113 C114 1.388(10) . ? C114 C115 1.347(10) . ? C115 C116 1.386(8) . ? C116 C122 1.444(9) . ? N121 C125 1.315(8) . ? N121 C122 1.382(7) . ? C122 C123 1.364(8) . ? C123 S124 1.690(7) . ? S124 C125 1.715(6) . ? C125 C132 1.468(8) . ? N131 C132 1.343(7) . ? N131 C136 1.345(7) . ? C132 C133 1.382(8) . ? C133 C134 1.365(9) . ? C134 C135 1.392(9) . ? C135 C136 1.391(9) . ? C136 C142 1.470(8) . ? N141 C142 1.302(8) . ? N141 C145 1.401(7) . ? C142 S143 1.720(6) . ? S143 C144 1.714(7) . ? C144 C145 1.362(8) . ? C145 C152 1.449(9) . ? N151 C156 1.326(8) . ? N151 C152 1.364(8) . ? C152 C153 1.394(9) . ? C153 C154 1.358(10) . ? C154 C155 1.382(10) . ? C155 C156 1.360(10) . ? N211 C212 1.328(8) . ? N211 C216 1.371(7) . ? C212 C213 1.371(9) . ? C213 C214 1.371(10) . ? C214 C215 1.371(11) . ? C215 C216 1.397(9) . ? C216 C222 1.429(9) . ? N221 C225 1.307(8) . ? N221 C222 1.391(7) . ? C222 C223 1.378(8) . ? C223 S224 1.694(7) . ? S224 C225 1.711(6) . ? C225 C232 1.477(9) . ? N231 C236 1.344(7) . ? N231 C232 1.351(8) . ? C232 C233 1.363(9) . ? C233 C234 1.380(10) . ? C234 C235 1.389(10) . ? C235 C236 1.388(9) . ? C236 C242 1.482(9) . ? N241 C242 1.319(8) . ? N241 C245 1.393(8) . ? C242 S243 1.709(6) . ? S243 C244 1.687(7) . ? C244 C245 1.361(8) . ? C245 C252 1.465(9) . ? N251 C256 1.344(8) . ? N251 C252 1.345(7) . ? C252 C253 1.388(9) . ? C253 C254 1.383(10) . ? C254 C255 1.384(10) . ? C255 C256 1.384(10) . ? Cl1 O14 1.438(4) . ? Cl1 O13 1.439(5) . ? Cl1 O11 1.440(5) . ? Cl1 O12 1.445(5) . ? Cl2 O21 1.360(7) . ? Cl2 O23 1.377(8) . ? Cl2 O22 1.385(6) . ? Cl2 O24 1.425(7) . ? Cl3 O34 1.347(7) . ? Cl3 O32 1.382(6) . ? Cl3 O31 1.428(5) . ? Cl3 O33 1.439(8) . ? Cl4 O41 1.284(8) . ? Cl4 O43 1.391(6) . ? Cl4 O44 1.409(6) . ? Cl4 O42 1.439(8) . ? N51 O52 1.181(8) . ? N51 O53 1.181(8) . ? N51 C54 1.502(9) . ? N61 O62 1.31(2) . ? N61 O64 1.407(14) . ? N61 C63 1.59(3) . ? N71 O72 1.181(9) . ? N71 O73 1.198(8) . ? N71 C74 1.483(9) . ? O82 N81 1.43(3) . ? O82 O83 1.438(18) . ? N81 C84 1.65(3) . ? O83 C84 1.858(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 N121 Cu1 N221 159.6(2) . . ? N121 Cu1 N211 104.0(2) . . ? N221 Cu1 N211 81.9(2) . . ? N121 Cu1 N111 81.6(2) . . ? N221 Cu1 N111 106.3(2) . . ? N211 Cu1 N111 141.2(2) . . ? N251 Cu2 N151 161.7(2) . . ? N251 Cu2 N241 81.5(2) . . ? N151 Cu2 N241 103.8(2) . . ? N251 Cu2 N141 107.0(2) . . ? N151 Cu2 N141 81.1(2) . . ? N241 Cu2 N141 137.5(2) . . ? C112 N111 C116 119.4(5) . . ? C112 N111 Cu1 126.6(4) . . ? C116 N111 Cu1 113.8(4) . . ? N111 C112 C113 122.3(6) . . ? C114 C113 C112 118.2(7) . . ? C115 C114 C113 119.5(6) . . ? C114 C115 C116 120.6(6) . . ? N111 C116 C115 120.0(6) . . ? N111 C116 C122 114.6(5) . . ? C115 C116 C122 125.4(6) . . ? C125 N121 C122 112.3(5) . . ? C125 N121 Cu1 132.8(4) . . ? C122 N121 Cu1 115.0(4) . . ? C123 C122 N121 113.0(6) . . ? C123 C122 C116 132.1(5) . . ? N121 C122 C116 114.9(5) . . ? C122 C123 S124 111.4(5) . . ? C123 S124 C125 90.2(3) . . ? N121 C125 C132 120.6(5) . . ? N121 C125 S124 113.1(4) . . ? C132 C125 S124 126.1(5) . . ? C132 N131 C136 117.3(5) . . ? N131 C132 C133 123.1(6) . . ? N131 C132 C125 110.9(5) . . ? C133 C132 C125 126.0(5) . . ? C134 C133 C132 119.3(6) . . ? C133 C134 C135 118.9(6) . . ? C136 C135 C134 118.5(6) . . ? N131 C136 C135 122.8(5) . . ? N131 C136 C142 112.1(5) . . ? C135 C136 C142 125.1(5) . . ? C142 N141 C145 112.3(5) . . ? C142 N141 Cu2 135.7(4) . . ? C145 N141 Cu2 111.0(4) . . ? N141 C142 C136 120.4(5) . . ? N141 C142 S143 113.5(4) . . ? C136 C142 S143 125.7(5) . . ? C144 S143 C142 90.3(3) . . ? C145 C144 S143 110.5(5) . . ? C144 C145 N141 113.4(6) . . ? C144 C145 C152 131.2(6) . . ? N141 C145 C152 115.5(5) . . ? C156 N151 C152 118.5(6) . . ? C156 N151 Cu2 125.6(5) . . ? C152 N151 Cu2 115.8(4) . . ? N151 C152 C153 120.1(6) . . ? N151 C152 C145 115.3(5) . . ? C153 C152 C145 124.6(6) . . ? C154 C153 C152 119.8(7) . . ? C153 C154 C155 119.6(7) . . ? C156 C155 C154 118.3(7) . . ? N151 C156 C155 123.7(7) . . ? C212 N211 C216 119.5(5) . . ? C212 N211 Cu1 126.3(4) . . ? C216 N211 Cu1 114.0(4) . . ? N211 C212 C213 122.5(7) . . ? C212 C213 C214 119.3(8) . . ? C215 C214 C213 119.3(7) . . ? C214 C215 C216 120.0(7) . . ? N211 C216 C215 119.4(6) . . ? N211 C216 C222 114.4(5) . . ? C215 C216 C222 126.2(6) . . ? C225 N221 C222 113.1(5) . . ? C225 N221 Cu1 133.2(4) . . ? C222 N221 Cu1 113.6(4) . . ? C223 C222 N221 111.7(6) . . ? C223 C222 C216 132.2(6) . . ? N221 C222 C216 116.1(5) . . ? C222 C223 S224 111.5(5) . . ? C223 S224 C225 90.3(3) . . ? N221 C225 C232 120.6(5) . . ? N221 C225 S224 113.3(5) . . ? C232 C225 S224 125.6(5) . . ? C236 N231 C232 116.2(5) . . ? N231 C232 C233 124.6(6) . . ? N231 C232 C225 110.2(6) . . ? C233 C232 C225 125.2(6) . . ? C232 C233 C234 117.7(6) . . ? C233 C234 C235 120.3(7) . . ? C236 C235 C234 117.2(7) . . ? N231 C236 C235 123.9(6) . . ? N231 C236 C242 111.5(5) . . ? C235 C236 C242 124.6(6) . . ? C242 N241 C245 111.6(5) . . ? C242 N241 Cu2 136.1(4) . . ? C245 N241 Cu2 112.2(4) . . ? N241 C242 C236 121.1(5) . . ? N241 C242 S243 113.3(5) . . ? C236 C242 S243 124.8(5) . . ? C244 S243 C242 90.6(3) . . ? C245 C244 S243 111.3(5) . . ? C244 C245 N241 113.1(6) . . ? C244 C245 C252 131.6(6) . . ? N241 C245 C252 115.3(5) . . ? C256 N251 C252 118.3(6) . . ? C256 N251 Cu2 124.9(5) . . ? C252 N251 Cu2 116.7(4) . . ? N251 C252 C253 122.9(6) . . ? N251 C252 C245 113.7(5) . . ? C253 C252 C245 123.2(6) . . ? C254 C253 C252 118.1(6) . . ? C253 C254 C255 119.4(7) . . ? C254 C255 C256 119.1(7) . . ? N251 C256 C255 122.0(7) . . ? O14 Cl1 O13 108.8(3) . . ? O14 Cl1 O11 109.9(3) . . ? O13 Cl1 O11 109.6(3) . . ? O14 Cl1 O12 109.6(3) . . ? O13 Cl1 O12 109.0(3) . . ? O11 Cl1 O12 109.9(3) . . ? O21 Cl2 O23 114.0(7) . . ? O21 Cl2 O22 110.9(5) . . ? O23 Cl2 O22 109.4(7) . . ? O21 Cl2 O24 112.1(5) . . ? O23 Cl2 O24 102.2(7) . . ? O22 Cl2 O24 107.8(5) . . ? O34 Cl3 O32 119.0(7) . . ? O34 Cl3 O31 110.7(4) . . ? O32 Cl3 O31 109.0(4) . . ? O34 Cl3 O33 104.3(6) . . ? O32 Cl3 O33 100.7(6) . . ? O31 Cl3 O33 112.8(5) . . ? O41 Cl4 O43 113.8(9) . . ? O41 Cl4 O44 109.3(6) . . ? O43 Cl4 O44 108.4(4) . . ? O41 Cl4 O42 111.2(8) . . ? O43 Cl4 O42 103.4(5) . . ? O44 Cl4 O42 110.6(5) . . ? O52 N51 O53 121.2(8) . . ? O52 N51 C54 120.2(8) . . ? O53 N51 C54 118.6(7) . . ? O62 N61 O64 137(2) . . ? O62 N61 C63 116.7(12) . . ? O64 N61 C63 107(2) . . ? O72 N71 O73 123.4(8) . . ? O72 N71 C74 116.0(8) . . ? O73 N71 C74 120.5(8) . . ? N81 O82 O83 90.0(12) . . ? O82 N81 C84 99(2) . . ? O82 O83 C84 90.0(12) . . ? N81 C84 O83 70.5(10) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.181 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.111 #=END data_lyricalm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H38 Cl4 Cu2 N14 O20 S4' _chemical_formula_weight 1600.10 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' 'Cl' 'Cl' 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4345(6) _cell_length_b 12.5367(6) _cell_length_c 20.9227(11) _cell_angle_alpha 89.8910(10) _cell_angle_beta 76.8420(10) _cell_angle_gamma 79.2060(10) _cell_volume 3116.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32873 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14162 _reflns_number_gt 8153 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14162 _refine_ls_number_parameters 901 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.011 _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 0.69502(4) 0.87453(4) 0.35122(3) 0.03295(15) Uani 1 1 d . . . Cu2 Cu 0.74709(4) 0.66886(4) 0.15264(3) 0.03148(15) Uani 1 1 d . . . Cl1 Cl 0.68207(9) 0.32918(9) 0.09441(6) 0.0398(3) Uani 1 1 d . . . Cl2 Cl 0.24074(11) 0.46645(11) 0.36112(7) 0.0486(3) Uani 1 1 d . . . Cl3 Cl 0.73693(13) 0.22011(14) 0.44502(8) 0.0649(4) Uani 1 1 d . . . Cl4 Cl 0.20645(14) 0.05537(12) 0.09167(7) 0.0600(4) Uani 1 1 d D . . S113 S 0.82585(10) 1.11649(9) 0.21595(6) 0.0393(3) Uani 1 1 d . . . S203 S 0.91899(10) 0.93203(11) 0.06353(6) 0.0427(3) Uani 1 1 d . . . S213 S 0.54880(10) 0.46593(9) 0.28686(6) 0.0399(3) Uani 1 1 d . . . S103 S 0.55589(12) 0.59599(11) 0.44359(7) 0.0488(3) Uani 1 1 d . . . O2 O 0.0982(5) 0.0125(4) 0.3236(3) 0.1023(18) Uani 1 1 d . . . O3 O 0.2346(6) 0.0986(5) 0.3031(3) 0.120(2) Uani 1 1 d . . . O6 O 0.1271(3) 0.4003(4) 0.2125(2) 0.0710(12) Uani 1 1 d . . . O7 O 0.2587(4) 0.4829(4) 0.1646(2) 0.0693(12) Uani 1 1 d . . . O11 O 0.6924(3) 0.4331(3) 0.06787(17) 0.0500(9) Uani 1 1 d . . . O12 O 0.7164(3) 0.3240(3) 0.15570(18) 0.0610(10) Uani 1 1 d . . . O13 O 0.5681(3) 0.3148(3) 0.1049(2) 0.0779(14) Uani 1 1 d . . . O14 O 0.7533(3) 0.2447(3) 0.04981(19) 0.0581(10) Uani 1 1 d . . . O21 O 0.2136(3) 0.5576(3) 0.32386(19) 0.0584(10) Uani 1 1 d . . . O22 O 0.1529(4) 0.4153(5) 0.3862(3) 0.118(2) Uani 1 1 d . . . O23 O 0.3193(5) 0.4753(6) 0.3962(3) 0.139(3) Uani 1 1 d . . . O24 O 0.3149(5) 0.3866(4) 0.3107(3) 0.121(2) Uani 1 1 d . . . O31 O 0.8106(4) 0.1866(4) 0.3860(2) 0.0943(16) Uani 1 1 d . . . O32 O 0.7563(6) 0.3129(5) 0.4724(3) 0.119(2) Uani 1 1 d . . . O41 O 0.2321(4) 0.0332(5) 0.1521(2) 0.0990(18) Uani 1 1 d D . . O42 O 0.0859(5) 0.1079(4) 0.1128(3) 0.129(2) Uani 1 1 d D . . O43 O 0.2601(9) 0.1219(7) 0.0568(3) 0.276(7) Uani 1 1 d D . . O44 O 0.1977(4) -0.0392(3) 0.0588(2) 0.0786(13) Uani 1 1 d D . . O33A O 0.7963(9) 0.1432(8) 0.4935(5) 0.093(3) Uani 0.50 1 d P . . O34A O 0.6442(7) 0.2934(7) 0.4114(4) 0.071(2) Uani 0.50 1 d P . . O33B O 0.6857(11) 0.1495(13) 0.4753(9) 0.157(8) Uani 0.50 1 d P . . O34B O 0.6317(8) 0.1959(12) 0.4626(6) 0.089(4) Uani 0.50 1 d P . . N1 N 0.1277(6) 0.0946(6) 0.3205(5) 0.117(3) Uani 1 1 d . . . N5 N 0.2238(4) 0.4017(4) 0.1850(2) 0.0543(12) Uani 1 1 d . . . N101 N 0.6514(3) 0.7491(3) 0.39571(17) 0.0325(8) Uani 1 1 d . . . N111 N 0.7356(3) 0.9931(3) 0.29858(17) 0.0309(8) Uani 1 1 d . . . N121 N 0.5489(3) 0.9930(3) 0.38349(17) 0.0321(8) Uani 1 1 d . . . N131 N 0.8205(3) 0.8372(3) 0.40676(18) 0.0384(9) Uani 1 1 d . . . N141 N 0.8791(3) 0.8076(3) 0.26262(17) 0.0303(8) Uani 1 1 d . . . N151 N 0.8120(3) 0.6096(3) 0.25885(17) 0.0300(8) Uani 1 1 d . . . N201 N 0.8384(3) 0.7689(3) 0.11000(17) 0.0314(8) Uani 1 1 d . . . N211 N 0.6486(3) 0.5820(3) 0.20304(18) 0.0318(8) Uani 1 1 d . . . N221 N 0.6138(3) 0.6953(3) 0.10451(18) 0.0344(9) Uani 1 1 d . . . N231 N 0.9032(3) 0.5606(3) 0.11417(18) 0.0343(9) Uani 1 1 d . . . N251 N 0.6417(3) 0.8762(3) 0.18394(17) 0.0297(8) Uani 1 1 d . . . N252 N 0.5391(3) 0.8050(3) 0.30243(17) 0.0308(8) Uani 1 1 d . . . C4 C 0.0654(7) 0.1948(6) 0.3013(5) 0.105(3) Uani 1 1 d . . . C8 C 0.3057(6) 0.2963(5) 0.1746(5) 0.093(3) Uani 1 1 d . . . C102 C 0.5643(4) 0.7037(3) 0.3935(2) 0.0353(11) Uani 1 1 d . . . C104 C 0.6756(4) 0.6111(4) 0.4662(2) 0.0466(13) Uani 1 1 d . . . H104 H 0.7092 0.5661 0.4957 0.056 Uiso 1 1 calc R . . C105 C 0.7165(4) 0.6964(4) 0.4360(2) 0.0396(11) Uani 1 1 d . . . C112 C 0.8288(4) 0.9958(3) 0.2545(2) 0.0321(10) Uani 1 1 d . . . C114 C 0.6912(4) 1.1627(4) 0.2608(2) 0.0387(11) Uani 1 1 d . . . H114 H 0.6471 1.2318 0.2567 0.046 Uiso 1 1 calc R . . C115 C 0.6565(4) 1.0875(3) 0.3027(2) 0.0320(10) Uani 1 1 d . . . C122 C 0.5508(4) 1.0865(3) 0.3505(2) 0.0303(9) Uani 1 1 d . . . C123 C 0.4580(4) 1.1704(4) 0.3607(2) 0.0398(11) Uani 1 1 d . . . H123 H 0.4611 1.2350 0.3371 0.048 Uiso 1 1 calc R . . C124 C 0.3616(4) 1.1591(4) 0.4051(3) 0.0472(13) Uani 1 1 d . . . H124 H 0.2974 1.2161 0.4126 0.057 Uiso 1 1 calc R . . C125 C 0.3581(4) 1.0647(4) 0.4391(2) 0.0418(12) Uani 1 1 d . . . H125 H 0.2915 1.0551 0.4695 0.050 Uiso 1 1 calc R . . C126 C 0.4546(4) 0.9843(4) 0.4276(2) 0.0366(11) Uani 1 1 d . . . H126 H 0.4537 0.9205 0.4521 0.044 Uiso 1 1 calc R . . C132 C 0.8153(4) 0.7436(4) 0.4394(2) 0.0391(11) Uani 1 1 d . . . C133 C 0.8959(5) 0.6993(5) 0.4721(3) 0.0521(14) Uani 1 1 d . . . H133 H 0.8915 0.6335 0.4943 0.063 Uiso 1 1 calc R . . C134 C 0.9843(5) 0.7529(5) 0.4720(3) 0.0653(17) Uani 1 1 d . . . H134 H 1.0411 0.7243 0.4943 0.078 Uiso 1 1 calc R . . C135 C 0.9887(5) 0.8470(5) 0.4395(3) 0.0582(15) Uani 1 1 d . . . H135 H 1.0489 0.8841 0.4385 0.070 Uiso 1 1 calc R . . C136 C 0.9041(4) 0.8876(4) 0.4080(2) 0.0445(12) Uani 1 1 d . . . H136 H 0.9064 0.9542 0.3864 0.053 Uiso 1 1 calc R . . C142 C 0.9538(4) 0.7145(4) 0.2561(2) 0.0320(10) Uani 1 1 d . . . C143 C 1.0691(4) 0.7080(4) 0.2270(2) 0.0377(11) Uani 1 1 d . . . H143 H 1.1206 0.6408 0.2236 0.045 Uiso 1 1 calc R . . C144 C 1.1054(4) 0.8003(4) 0.2038(2) 0.0413(12) Uani 1 1 d . . . H144 H 1.1823 0.7974 0.1831 0.050 Uiso 1 1 calc R . . C145 C 1.0294(4) 0.8980(4) 0.2105(2) 0.0373(11) Uani 1 1 d . . . H145 H 1.0529 0.9631 0.1949 0.045 Uiso 1 1 calc R . . C146 C 0.9174(3) 0.8978(4) 0.2409(2) 0.0315(10) Uani 1 1 d . . . C152 C 0.9055(4) 0.6180(4) 0.2790(2) 0.0323(10) Uani 1 1 d . . . C153 C 0.9514(4) 0.5443(4) 0.3200(2) 0.0411(11) Uani 1 1 d . . . H153 H 1.0186 0.5516 0.3324 0.049 Uiso 1 1 calc R . . C154 C 0.8968(4) 0.4603(4) 0.3420(3) 0.0460(13) Uani 1 1 d . . . H154 H 0.9254 0.4095 0.3707 0.055 Uiso 1 1 calc R . . C155 C 0.7994(4) 0.4504(4) 0.3220(2) 0.0408(11) Uani 1 1 d . . . H155 H 0.7603 0.3933 0.3367 0.049 Uiso 1 1 calc R . . C156 C 0.7616(4) 0.5258(3) 0.2804(2) 0.0330(10) Uani 1 1 d . . . C202 C 0.8110(4) 0.8756(4) 0.1059(2) 0.0332(10) Uani 1 1 d . . . C204 C 1.0051(4) 0.8063(4) 0.0506(2) 0.0412(11) Uani 1 1 d . . . H204 H 1.0817 0.7929 0.0273 0.049 Uiso 1 1 calc R . . C205 C 0.9492(4) 0.7288(4) 0.0782(2) 0.0342(10) Uani 1 1 d . . . C212 C 0.6618(4) 0.5253(3) 0.2546(2) 0.0311(10) Uani 1 1 d . . . C214 C 0.4815(4) 0.5208(4) 0.2283(2) 0.0410(11) Uani 1 1 d . . . H214 H 0.4090 0.5112 0.2249 0.049 Uiso 1 1 calc R . . C215 C 0.5475(4) 0.5806(4) 0.1870(2) 0.0346(10) Uani 1 1 d . . . C222 C 0.5279(4) 0.6462(4) 0.1315(2) 0.0348(10) Uani 1 1 d . . . C223 C 0.4275(4) 0.6621(5) 0.1098(3) 0.0516(14) Uani 1 1 d . . . H223 H 0.3682 0.6262 0.1296 0.062 Uiso 1 1 calc R . . C224 C 0.4164(5) 0.7305(5) 0.0594(3) 0.0611(16) Uani 1 1 d . . . H224 H 0.3493 0.7429 0.0439 0.073 Uiso 1 1 calc R . . C225 C 0.5043(5) 0.7809(5) 0.0318(3) 0.0547(15) Uani 1 1 d . . . H225 H 0.4977 0.8293 -0.0027 0.066 Uiso 1 1 calc R . . C226 C 0.6021(4) 0.7608(4) 0.0542(2) 0.0434(12) Uani 1 1 d . . . H226 H 0.6630 0.7942 0.0337 0.052 Uiso 1 1 calc R . . C232 C 0.9846(4) 0.6108(4) 0.0806(2) 0.0352(10) Uani 1 1 d . . . C233 C 1.0908(4) 0.5543(4) 0.0503(2) 0.0443(12) Uani 1 1 d . . . H233 H 1.1472 0.5913 0.0276 0.053 Uiso 1 1 calc R . . C234 C 1.1128(4) 0.4422(5) 0.0541(3) 0.0499(14) Uani 1 1 d . . . H234 H 1.1844 0.4011 0.0331 0.060 Uiso 1 1 calc R . . C235 C 1.0304(5) 0.3909(4) 0.0884(3) 0.0487(13) Uani 1 1 d . . . H235 H 1.0449 0.3142 0.0917 0.058 Uiso 1 1 calc R . . C236 C 0.9261(4) 0.4522(4) 0.1182(2) 0.0391(11) Uani 1 1 d . . . H236 H 0.8694 0.4166 0.1421 0.047 Uiso 1 1 calc R . . C242 C 0.6960(4) 0.9317(4) 0.1362(2) 0.0323(10) Uani 1 1 d . . . C243 C 0.6474(4) 1.0287(4) 0.1138(2) 0.0429(12) Uani 1 1 d . . . H243 H 0.6898 1.0658 0.0805 0.051 Uiso 1 1 calc R . . C244 C 0.5350(4) 1.0698(4) 0.1414(2) 0.0444(12) Uani 1 1 d . . . H244 H 0.4985 1.1362 0.1274 0.053 Uiso 1 1 calc R . . C245 C 0.4765(4) 1.0131(4) 0.1895(2) 0.0420(12) Uani 1 1 d . . . H245 H 0.3990 1.0394 0.2084 0.050 Uiso 1 1 calc R . . C246 C 0.5326(3) 0.9164(4) 0.2103(2) 0.0332(10) Uani 1 1 d . . . C253 C 0.4894(4) 0.7459(3) 0.3507(2) 0.0337(10) Uani 1 1 d . . . C254 C 0.3795(4) 0.7300(4) 0.3594(2) 0.0410(11) Uani 1 1 d . . . H254 H 0.3490 0.6852 0.3927 0.049 Uiso 1 1 calc R . . C255 C 0.3159(4) 0.7811(4) 0.3182(3) 0.0464(13) Uani 1 1 d . . . H255 H 0.2400 0.7731 0.3233 0.056 Uiso 1 1 calc R . . C256 C 0.3633(4) 0.8443(4) 0.2693(2) 0.0397(11) Uani 1 1 d . . . H256 H 0.3202 0.8808 0.2409 0.048 Uiso 1 1 calc R . . C257 C 0.4762(3) 0.8535(3) 0.2624(2) 0.0310(10) 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 0.0339(3) 0.0302(3) 0.0334(3) 0.0099(2) -0.0053(2) -0.0060(2) Cu2 0.0275(3) 0.0317(3) 0.0333(3) 0.0059(2) -0.0024(2) -0.0065(2) Cl1 0.0393(6) 0.0393(6) 0.0367(7) -0.0045(5) 0.0035(5) -0.0121(5) Cl2 0.0458(7) 0.0478(7) 0.0581(8) 0.0206(6) -0.0224(6) -0.0113(6) Cl3 0.0643(9) 0.0783(11) 0.0527(9) -0.0101(8) 0.0063(7) -0.0390(8) Cl4 0.0839(11) 0.0596(9) 0.0487(8) 0.0138(7) -0.0258(8) -0.0315(8) S113 0.0453(7) 0.0322(6) 0.0368(7) 0.0082(5) -0.0002(5) -0.0100(5) S203 0.0437(7) 0.0487(7) 0.0369(7) 0.0140(6) -0.0031(5) -0.0195(6) S213 0.0425(7) 0.0299(6) 0.0436(7) 0.0050(5) 0.0010(5) -0.0111(5) S103 0.0604(8) 0.0433(7) 0.0401(8) 0.0163(6) -0.0003(6) -0.0179(6) O2 0.101(4) 0.068(3) 0.129(5) 0.009(3) 0.005(3) -0.032(3) O3 0.136(5) 0.116(5) 0.114(5) -0.016(4) -0.035(4) -0.034(4) O6 0.047(2) 0.100(3) 0.063(3) -0.005(2) -0.006(2) -0.011(2) O7 0.073(3) 0.061(3) 0.076(3) 0.000(2) -0.019(2) -0.018(2) O11 0.058(2) 0.045(2) 0.043(2) 0.0104(16) -0.0044(17) -0.0082(17) O12 0.092(3) 0.052(2) 0.041(2) 0.0097(18) -0.013(2) -0.020(2) O13 0.042(2) 0.076(3) 0.106(4) -0.020(3) 0.011(2) -0.024(2) O14 0.055(2) 0.053(2) 0.052(2) -0.0152(18) 0.0094(18) -0.0022(18) O21 0.054(2) 0.059(2) 0.070(3) 0.034(2) -0.024(2) -0.0181(18) O22 0.062(3) 0.153(5) 0.151(5) 0.114(4) -0.029(3) -0.042(3) O23 0.157(5) 0.201(7) 0.123(5) 0.112(5) -0.099(4) -0.115(5) O24 0.111(4) 0.073(3) 0.156(6) 0.021(4) 0.003(4) 0.005(3) O31 0.090(4) 0.117(4) 0.061(3) -0.002(3) 0.010(3) -0.016(3) O32 0.170(6) 0.107(4) 0.102(5) 0.000(4) -0.044(4) -0.067(4) O41 0.097(4) 0.165(5) 0.063(3) 0.025(3) -0.031(3) -0.079(4) O42 0.121(5) 0.084(4) 0.162(6) 0.005(4) -0.023(4) 0.020(4) O43 0.517(17) 0.321(11) 0.067(4) 0.031(6) 0.005(7) -0.359(13) O44 0.112(4) 0.062(3) 0.070(3) -0.001(2) -0.032(3) -0.022(3) O33A 0.104(8) 0.111(8) 0.070(6) 0.031(6) -0.048(6) -0.007(6) O34A 0.060(5) 0.080(6) 0.077(6) 0.002(5) -0.022(4) -0.015(4) O33B 0.079(10) 0.171(14) 0.213(17) 0.144(13) -0.002(10) -0.046(10) O34B 0.048(6) 0.153(12) 0.075(7) 0.011(8) -0.008(5) -0.045(7) N1 0.076(5) 0.074(5) 0.219(9) -0.010(5) -0.059(5) -0.028(4) N5 0.047(3) 0.066(3) 0.052(3) -0.007(2) -0.013(2) -0.016(2) N101 0.036(2) 0.032(2) 0.028(2) 0.0048(16) -0.0052(16) -0.0057(16) N111 0.034(2) 0.0294(19) 0.029(2) 0.0024(15) -0.0051(16) -0.0075(16) N121 0.038(2) 0.0285(19) 0.027(2) -0.0002(15) -0.0048(16) -0.0043(16) N131 0.043(2) 0.041(2) 0.029(2) 0.0061(17) -0.0069(17) -0.0040(18) N141 0.035(2) 0.032(2) 0.025(2) 0.0037(15) -0.0077(15) -0.0076(16) N151 0.0315(19) 0.0268(19) 0.029(2) 0.0024(15) -0.0018(15) -0.0044(15) N201 0.0315(19) 0.036(2) 0.028(2) 0.0057(16) -0.0070(16) -0.0086(16) N211 0.034(2) 0.0263(19) 0.032(2) -0.0002(16) -0.0013(16) -0.0072(16) N221 0.037(2) 0.033(2) 0.031(2) 0.0004(16) -0.0064(16) -0.0022(16) N231 0.037(2) 0.039(2) 0.026(2) -0.0014(16) -0.0075(16) -0.0037(17) N251 0.0318(19) 0.0312(19) 0.027(2) 0.0038(15) -0.0068(15) -0.0081(15) N252 0.0309(19) 0.0288(19) 0.029(2) 0.0003(15) -0.0006(16) -0.0047(15) C4 0.083(5) 0.059(4) 0.152(8) 0.018(5) 0.005(5) 0.003(4) C8 0.057(4) 0.043(4) 0.161(8) -0.018(4) 0.001(4) 0.006(3) C102 0.043(3) 0.027(2) 0.030(3) 0.0050(19) 0.005(2) -0.007(2) C104 0.060(3) 0.049(3) 0.028(3) 0.015(2) -0.007(2) -0.007(3) C105 0.049(3) 0.038(3) 0.024(2) 0.008(2) 0.000(2) -0.001(2) C112 0.037(2) 0.031(2) 0.030(2) 0.0062(18) -0.0051(19) -0.0119(19) C114 0.041(3) 0.029(2) 0.042(3) 0.005(2) -0.004(2) -0.005(2) C115 0.034(2) 0.029(2) 0.032(3) 0.0016(19) -0.0072(19) -0.0051(19) C122 0.039(2) 0.028(2) 0.024(2) 0.0005(17) -0.0061(18) -0.0089(19) C123 0.045(3) 0.031(2) 0.040(3) 0.004(2) -0.009(2) 0.001(2) C124 0.044(3) 0.042(3) 0.047(3) -0.001(2) -0.002(2) 0.003(2) C125 0.038(3) 0.044(3) 0.037(3) -0.005(2) 0.005(2) -0.008(2) C126 0.044(3) 0.035(3) 0.028(3) 0.0031(19) -0.002(2) -0.008(2) C132 0.042(3) 0.046(3) 0.025(2) 0.003(2) -0.002(2) -0.002(2) C133 0.060(3) 0.055(3) 0.038(3) 0.011(2) -0.013(3) -0.002(3) C134 0.058(4) 0.087(5) 0.051(4) 0.008(3) -0.027(3) 0.003(3) C135 0.050(3) 0.075(4) 0.053(4) 0.006(3) -0.016(3) -0.014(3) C136 0.044(3) 0.055(3) 0.037(3) 0.005(2) -0.012(2) -0.013(2) C142 0.031(2) 0.034(2) 0.032(3) 0.0027(19) -0.0087(19) -0.0064(19) C143 0.030(2) 0.039(3) 0.040(3) 0.002(2) -0.005(2) 0.000(2) C144 0.027(2) 0.053(3) 0.044(3) 0.007(2) -0.004(2) -0.012(2) C145 0.035(2) 0.040(3) 0.039(3) 0.009(2) -0.007(2) -0.015(2) C146 0.029(2) 0.040(3) 0.027(2) 0.0079(19) -0.0084(18) -0.0098(19) C152 0.032(2) 0.032(2) 0.027(2) 0.0034(18) -0.0016(18) -0.0008(19) C153 0.040(3) 0.040(3) 0.041(3) 0.008(2) -0.010(2) 0.000(2) C154 0.045(3) 0.046(3) 0.043(3) 0.017(2) -0.009(2) -0.001(2) C155 0.050(3) 0.031(2) 0.040(3) 0.007(2) -0.007(2) -0.009(2) C156 0.032(2) 0.031(2) 0.029(2) 0.0024(19) 0.0015(19) -0.0002(19) C202 0.042(3) 0.035(2) 0.025(2) 0.0071(19) -0.0082(19) -0.014(2) C204 0.035(2) 0.053(3) 0.033(3) 0.002(2) 0.000(2) -0.010(2) C205 0.032(2) 0.043(3) 0.026(2) 0.0023(19) -0.0035(19) -0.007(2) C212 0.033(2) 0.022(2) 0.035(3) 0.0006(18) -0.0016(19) -0.0068(18) C214 0.037(3) 0.033(3) 0.051(3) -0.003(2) -0.002(2) -0.011(2) C215 0.029(2) 0.033(2) 0.040(3) -0.003(2) -0.006(2) -0.0051(19) C222 0.035(2) 0.034(2) 0.033(3) -0.006(2) -0.004(2) -0.006(2) C223 0.042(3) 0.063(4) 0.052(3) 0.003(3) -0.012(2) -0.016(3) C224 0.051(3) 0.082(4) 0.053(4) 0.011(3) -0.022(3) -0.010(3) C225 0.056(3) 0.066(4) 0.044(3) 0.013(3) -0.024(3) -0.001(3) C226 0.052(3) 0.043(3) 0.034(3) 0.004(2) -0.007(2) -0.009(2) C232 0.031(2) 0.050(3) 0.024(2) 0.001(2) -0.0058(19) -0.005(2) C233 0.035(3) 0.064(3) 0.029(3) -0.004(2) -0.002(2) -0.004(2) C234 0.040(3) 0.059(4) 0.041(3) -0.011(3) -0.009(2) 0.013(3) C235 0.060(3) 0.038(3) 0.049(3) -0.006(2) -0.022(3) 0.000(3) C236 0.047(3) 0.037(3) 0.033(3) 0.000(2) -0.010(2) -0.004(2) C242 0.034(2) 0.034(2) 0.031(2) 0.0033(19) -0.0081(19) -0.0089(19) C243 0.047(3) 0.042(3) 0.040(3) 0.015(2) -0.009(2) -0.009(2) C244 0.049(3) 0.036(3) 0.042(3) 0.009(2) -0.009(2) 0.005(2) C245 0.038(3) 0.039(3) 0.044(3) 0.003(2) -0.009(2) 0.004(2) C246 0.028(2) 0.038(3) 0.032(3) 0.0028(19) -0.0042(18) -0.0061(19) C253 0.036(2) 0.030(2) 0.033(3) 0.0026(19) -0.0026(19) -0.0065(19) C254 0.042(3) 0.037(3) 0.039(3) 0.000(2) 0.004(2) -0.011(2) C255 0.033(3) 0.051(3) 0.054(3) -0.002(3) -0.002(2) -0.015(2) C256 0.035(2) 0.042(3) 0.040(3) -0.004(2) -0.005(2) -0.005(2) C257 0.031(2) 0.027(2) 0.033(3) -0.0012(18) -0.0023(19) -0.0049(18) _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 N111 1.923(4) . ? Cu1 N101 1.928(4) . ? Cu1 N121 2.097(3) . ? Cu1 N131 2.134(4) . ? Cu2 N211 1.925(4) . ? Cu2 N201 1.930(4) . ? Cu2 N221 2.103(4) . ? Cu2 N231 2.136(4) . ? Cl1 O13 1.430(4) . ? Cl1 O11 1.431(3) . ? Cl1 O14 1.432(3) . ? Cl1 O12 1.438(4) . ? Cl2 O23 1.368(5) . ? Cl2 O22 1.371(5) . ? Cl2 O21 1.414(3) . ? Cl2 O24 1.477(6) . ? Cl3 O33B 1.271(12) . ? Cl3 O34B 1.366(10) . ? Cl3 O31 1.372(5) . ? Cl3 O32 1.382(5) . ? Cl3 O33A 1.605(8) . ? Cl3 O34A 1.625(8) . ? Cl4 O43 1.287(5) . ? Cl4 O41 1.389(4) . ? Cl4 O44 1.406(4) . ? Cl4 O42 1.485(5) . ? S113 C112 1.712(4) . ? S113 C114 1.715(5) . ? S203 C202 1.704(4) . ? S203 C204 1.715(5) . ? S213 C214 1.709(5) . ? S213 C212 1.715(4) . ? S103 C104 1.703(6) . ? S103 C102 1.712(4) . ? O2 N1 1.152(7) . ? O3 N1 1.306(8) . ? O6 N5 1.212(6) . ? O7 N5 1.218(6) . ? O33A O33B 1.497(18) . ? O34A O34B 1.631(15) . ? O33B O34B 0.891(14) . ? N1 C4 1.453(10) . ? N5 C8 1.492(7) . ? N101 C102 1.324(6) . ? N101 C105 1.384(6) . ? N111 C112 1.313(5) . ? N111 C115 1.379(5) . ? N121 C126 1.340(5) . ? N121 C122 1.361(5) . ? N131 C136 1.319(6) . ? N131 C132 1.361(6) . ? N141 C142 1.334(5) . ? N141 C146 1.347(5) . ? N151 C152 1.345(6) . ? N151 C156 1.347(5) . ? N201 C202 1.324(5) . ? N201 C205 1.386(5) . ? N211 C212 1.316(5) . ? N211 C215 1.376(6) . ? N221 C222 1.345(6) . ? N221 C226 1.351(6) . ? N231 C236 1.342(6) . ? N231 C232 1.352(6) . ? N251 C246 1.342(5) . ? N251 C242 1.343(5) . ? N252 C257 1.342(5) . ? N252 C253 1.355(5) . ? C102 C253 1.462(6) . ? C104 C105 1.363(7) . ? C105 C132 1.474(7) . ? C112 C146 1.469(6) . ? C114 C115 1.349(6) . ? C115 C122 1.462(6) . ? C122 C123 1.384(6) . ? C123 C124 1.369(7) . ? C124 C125 1.383(7) . ? C125 C126 1.390(6) . ? C132 C133 1.372(7) . ? C133 C134 1.391(8) . ? C134 C135 1.363(8) . ? C135 C136 1.383(7) . ? C142 C143 1.411(6) . ? C142 C152 1.482(6) . ? C143 C144 1.369(6) . ? C144 C145 1.385(6) . ? C145 C146 1.394(6) . ? C152 C153 1.391(6) . ? C153 C154 1.381(7) . ? C154 C155 1.395(7) . ? C155 C156 1.375(6) . ? C156 C212 1.463(6) . ? C202 C242 1.467(6) . ? C204 C205 1.352(6) . ? C205 C232 1.466(6) . ? C214 C215 1.374(6) . ? C215 C222 1.460(6) . ? C222 C223 1.404(7) . ? C223 C224 1.371(8) . ? C224 C225 1.378(8) . ? C225 C226 1.381(7) . ? C232 C233 1.385(6) . ? C233 C234 1.386(7) . ? C234 C235 1.374(8) . ? C235 C236 1.387(7) . ? C242 C243 1.385(6) . ? C243 C244 1.385(6) . ? C244 C245 1.380(7) . ? C245 C246 1.402(6) . ? C246 C257 1.469(6) . ? C253 C254 1.390(6) . ? C254 C255 1.378(7) . ? C255 C256 1.384(7) . ? C256 C257 1.404(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 N111 Cu1 N101 173.87(16) . . ? N111 Cu1 N121 79.81(14) . . ? N101 Cu1 N121 101.47(15) . . ? N111 Cu1 N131 104.86(15) . . ? N101 Cu1 N131 79.62(15) . . ? N121 Cu1 N131 122.29(14) . . ? N211 Cu2 N201 173.36(15) . . ? N211 Cu2 N221 79.24(15) . . ? N201 Cu2 N221 101.55(15) . . ? N211 Cu2 N231 106.15(15) . . ? N201 Cu2 N231 79.05(15) . . ? N221 Cu2 N231 123.09(14) . . ? O13 Cl1 O11 110.1(2) . . ? O13 Cl1 O14 109.2(2) . . ? O11 Cl1 O14 109.9(2) . . ? O13 Cl1 O12 109.9(3) . . ? O11 Cl1 O12 108.5(2) . . ? O14 Cl1 O12 109.3(2) . . ? O23 Cl2 O22 120.8(3) . . ? O23 Cl2 O21 114.4(3) . . ? O22 Cl2 O21 114.7(2) . . ? O23 Cl2 O24 96.5(4) . . ? O22 Cl2 O24 102.9(4) . . ? O21 Cl2 O24 102.6(3) . . ? O33B Cl3 O34B 39.3(6) . . ? O33B Cl3 O31 116.6(10) . . ? O34B Cl3 O31 123.3(6) . . ? O33B Cl3 O32 126.6(10) . . ? O34B Cl3 O32 118.6(6) . . ? O31 Cl3 O32 113.2(4) . . ? O33B Cl3 O33A 61.5(8) . . ? O34B Cl3 O33A 99.1(7) . . ? O31 Cl3 O33A 100.2(5) . . ? O32 Cl3 O33A 92.4(5) . . ? O33B Cl3 O34A 104.2(7) . . ? O34B Cl3 O34A 65.4(6) . . ? O31 Cl3 O34A 93.8(4) . . ? O32 Cl3 O34A 90.3(4) . . ? O33A Cl3 O34A 163.4(5) . . ? O43 Cl4 O41 116.1(4) . . ? O43 Cl4 O44 116.6(4) . . ? O41 Cl4 O44 111.8(3) . . ? O43 Cl4 O42 108.6(6) . . ? O41 Cl4 O42 100.7(3) . . ? O44 Cl4 O42 100.5(3) . . ? C112 S113 C114 90.1(2) . . ? C202 S203 C204 90.2(2) . . ? C214 S213 C212 90.8(2) . . ? C104 S103 C102 90.9(2) . . ? O33B O33A Cl3 48.2(5) . . ? Cl3 O34A O34B 49.6(4) . . ? O34B O33B Cl3 76.2(12) . . ? O34B O33B O33A 142(2) . . ? Cl3 O33B O33A 70.3(8) . . ? O33B O34B Cl3 64.6(11) . . ? O33B O34B O34A 128.7(14) . . ? Cl3 O34B O34A 64.9(6) . . ? O2 N1 O3 120.8(7) . . ? O2 N1 C4 124.6(7) . . ? O3 N1 C4 107.6(7) . . ? O6 N5 O7 124.7(5) . . ? O6 N5 C8 117.7(5) . . ? O7 N5 C8 117.6(5) . . ? C102 N101 C105 112.8(4) . . ? C102 N101 Cu1 128.6(3) . . ? C105 N101 Cu1 118.6(3) . . ? C112 N111 C115 112.8(4) . . ? C112 N111 Cu1 128.7(3) . . ? C115 N111 Cu1 118.4(3) . . ? C126 N121 C122 118.1(4) . . ? C126 N121 Cu1 128.4(3) . . ? C122 N121 Cu1 113.3(3) . . ? C136 N131 C132 118.8(4) . . ? C136 N131 Cu1 128.1(3) . . ? C132 N131 Cu1 112.8(3) . . ? C142 N141 C146 117.6(4) . . ? C152 N151 C156 117.3(4) . . ? C202 N201 C205 111.9(4) . . ? C202 N201 Cu2 129.2(3) . . ? C205 N201 Cu2 118.9(3) . . ? C212 N211 C215 113.1(4) . . ? C212 N211 Cu2 128.5(3) . . ? C215 N211 Cu2 118.3(3) . . ? C222 N221 C226 118.0(4) . . ? C222 N221 Cu2 114.1(3) . . ? C226 N221 Cu2 127.7(3) . . ? C236 N231 C232 118.8(4) . . ? C236 N231 Cu2 127.6(3) . . ? C232 N231 Cu2 113.5(3) . . ? C246 N251 C242 117.6(4) . . ? C257 N252 C253 117.4(4) . . ? N101 C102 C253 120.1(4) . . ? N101 C102 S103 112.3(3) . . ? C253 C102 S103 127.6(4) . . ? C105 C104 S103 110.7(4) . . ? C104 C105 N101 113.2(5) . . ? C104 C105 C132 132.1(4) . . ? N101 C105 C132 114.7(4) . . ? N111 C112 C146 119.0(4) . . ? N111 C112 S113 112.9(3) . . ? C146 C112 S113 128.0(3) . . ? C115 C114 S113 110.7(3) . . ? C114 C115 N111 113.5(4) . . ? C114 C115 C122 132.3(4) . . ? N111 C115 C122 114.2(4) . . ? N121 C122 C123 121.7(4) . . ? N121 C122 C115 114.0(4) . . ? C123 C122 C115 124.2(4) . . ? C124 C123 C122 119.3(4) . . ? C123 C124 C125 119.8(4) . . ? C124 C125 C126 118.2(4) . . ? N121 C126 C125 122.8(4) . . ? N131 C132 C133 121.8(5) . . ? N131 C132 C105 113.9(4) . . ? C133 C132 C105 124.4(5) . . ? C132 C133 C134 118.5(5) . . ? C135 C134 C133 119.4(5) . . ? C134 C135 C136 119.1(6) . . ? N131 C136 C135 122.3(5) . . ? N141 C142 C143 122.5(4) . . ? N141 C142 C152 114.8(4) . . ? C143 C142 C152 122.7(4) . . ? C144 C143 C142 118.8(4) . . ? C143 C144 C145 119.7(4) . . ? C144 C145 C146 117.9(4) . . ? N141 C146 C145 123.5(4) . . ? N141 C146 C112 112.5(4) . . ? C145 C146 C112 124.0(4) . . ? N151 C152 C153 123.0(4) . . ? N151 C152 C142 114.7(4) . . ? C153 C152 C142 122.3(4) . . ? C154 C153 C152 118.3(5) . . ? C153 C154 C155 119.7(4) . . ? C156 C155 C154 117.9(4) . . ? N151 C156 C155 123.9(4) . . ? N151 C156 C212 112.0(4) . . ? C155 C156 C212 124.2(4) . . ? N201 C202 C242 119.3(4) . . ? N201 C202 S203 113.4(3) . . ? C242 C202 S203 127.3(3) . . ? C205 C204 S203 110.8(3) . . ? C204 C205 N201 113.7(4) . . ? C204 C205 C232 131.8(4) . . ? N201 C205 C232 114.6(4) . . ? N211 C212 C156 119.3(4) . . ? N211 C212 S213 112.6(3) . . ? C156 C212 S213 127.9(3) . . ? C215 C214 S213 110.2(4) . . ? C214 C215 N211 113.3(4) . . ? C214 C215 C222 132.0(4) . . ? N211 C215 C222 114.7(4) . . ? N221 C222 C223 122.3(5) . . ? N221 C222 C215 113.6(4) . . ? C223 C222 C215 124.1(4) . . ? C224 C223 C222 118.8(5) . . ? C223 C224 C225 119.0(5) . . ? C224 C225 C226 119.9(5) . . ? N221 C226 C225 122.1(5) . . ? N231 C232 C233 122.3(5) . . ? N231 C232 C205 114.0(4) . . ? C233 C232 C205 123.7(4) . . ? C232 C233 C234 118.3(5) . . ? C235 C234 C233 119.6(5) . . ? C234 C235 C236 119.3(5) . . ? N231 C236 C235 121.7(5) . . ? N251 C242 C243 124.2(4) . . ? N251 C242 C202 113.5(4) . . ? C243 C242 C202 122.2(4) . . ? C242 C243 C244 117.8(4) . . ? C245 C244 C243 119.1(4) . . ? C244 C245 C246 119.4(4) . . ? N251 C246 C245 121.8(4) . . ? N251 C246 C257 116.0(4) . . ? C245 C246 C257 122.2(4) . . ? N252 C253 C254 123.8(4) . . ? N252 C253 C102 111.9(4) . . ? C254 C253 C102 124.3(4) . . ? C255 C254 C253 118.0(4) . . ? C254 C255 C256 119.6(4) . . ? C255 C256 C257 119.0(4) . . ? N252 C257 C256 122.2(4) . . ? N252 C257 C246 116.1(4) . . ? C256 C257 C246 121.7(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.511 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.093 #=END