# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global #TrackingRef '- C1DT11622C_ccdc_795631_815020_cif.txt' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Kiran Diwan' _publ_contact_author_email rupalchembhu@gmail.com loop_ _publ_author_name N.Singh K.Diwan B.Singh S.Singh M.Drew data_Complex1 #TrackingRef '- C1DT11622C_ccdc_795631_815020_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 795631' #TrackingRef 'complex1, 2 and 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H26 Cl Cu N5 O8 S' _chemical_formula_weight 751.64 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' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 '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' _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 8.2961(19) _cell_length_b 13.477(4) _cell_length_c 15.762(5) _cell_angle_alpha 71.28(3) _cell_angle_beta 77.77(2) _cell_angle_gamma 78.14(2) _cell_volume 1613.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11479 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 30.00 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 770 _exptl_absorpt_coefficient_mu 0.886 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11479 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.1777 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9406 _reflns_number_gt 3482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; w=1/[\s^2^(Fo^2^)+(0.0376P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9015 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1540 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 0.785 _refine_ls_restrained_S_all 0.785 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.63249(5) 0.65811(3) 0.69200(3) 0.03765(14) Uani 1 1 d . . . S42 S 0.95100(12) 0.69378(8) 0.74760(6) 0.0427(3) Uani 1 1 d . . . Cl9 Cl 0.19073(14) 0.20751(8) 0.82934(7) 0.0558(3) Uani 1 1 d . . . C12 C 0.8476(4) 0.4548(3) 0.6771(3) 0.0515(11) Uani 1 1 d . . . H12 H 0.8743 0.4483 0.7332 0.062 Uiso 1 1 calc R . . C13 C 0.9191(5) 0.3762(3) 0.6337(3) 0.0583(12) Uani 1 1 d . . . H13 H 0.9894 0.3167 0.6615 0.070 Uiso 1 1 calc R . . C14 C 0.8826(5) 0.3893(3) 0.5491(3) 0.0620(13) Uani 1 1 d . . . H14 H 0.9302 0.3380 0.5196 0.074 Uiso 1 1 calc R . . C15 C 0.7772(5) 0.4765(3) 0.5066(3) 0.0473(10) Uani 1 1 d . . . C16 C 0.7060(4) 0.5504(3) 0.5558(2) 0.0372(9) Uani 1 1 d . . . C17 C 0.5916(4) 0.6411(3) 0.5183(2) 0.0389(9) Uani 1 1 d . . . C18 C 0.5588(5) 0.6605(4) 0.4292(3) 0.0491(11) Uani 1 1 d . . . C19 C 0.4486(5) 0.7517(4) 0.3964(3) 0.0609(12) Uani 1 1 d . . . H19 H 0.4289 0.7702 0.3369 0.073 Uiso 1 1 calc R . . C20 C 0.3704(5) 0.8132(4) 0.4500(3) 0.0641(13) Uani 1 1 d . . . H20 H 0.2947 0.8729 0.4281 0.077 Uiso 1 1 calc R . . C21 C 0.4038(4) 0.7868(3) 0.5392(3) 0.0453(10) Uani 1 1 d . . . H21 H 0.3473 0.8288 0.5761 0.054 Uiso 1 1 calc R . . C23 C 0.6379(5) 0.5864(4) 0.3800(3) 0.0642(13) Uani 1 1 d . . . H23 H 0.6186 0.5990 0.3211 0.077 Uiso 1 1 calc R . . C24 C 0.7400(5) 0.4983(4) 0.4173(3) 0.0644(14) Uani 1 1 d . . . H24 H 0.7874 0.4507 0.3841 0.077 Uiso 1 1 calc R . . C45 C 0.8913(4) 0.8009(3) 0.7956(2) 0.0408(9) Uani 1 1 d . . . C46 C 0.9664(5) 0.8926(3) 0.7570(3) 0.0546(11) Uani 1 1 d . . . H46 H 1.0520 0.8967 0.7078 0.066 Uiso 1 1 calc R . . C47 C 0.9120(5) 0.9771(3) 0.7930(3) 0.0631(12) Uani 1 1 d . . . H47 H 0.9618 1.0380 0.7670 0.076 Uiso 1 1 calc R . . C48 C 0.7866(5) 0.9736(4) 0.8659(3) 0.0556(11) Uani 1 1 d . . . C49 C 0.7161(5) 0.8808(4) 0.9048(3) 0.0598(12) Uani 1 1 d . . . H49 H 0.6336 0.8759 0.9555 0.072 Uiso 1 1 calc R . . C50 C 0.7658(5) 0.7963(3) 0.8697(2) 0.0499(10) Uani 1 1 d . . . H50 H 0.7149 0.7358 0.8958 0.060 Uiso 1 1 calc R . . C51 C 0.7288(6) 1.0664(4) 0.9056(3) 0.0850(16) Uani 1 1 d . . . H51A H 0.6742 1.0418 0.9670 0.128 Uiso 1 1 calc R . . H51B H 0.6523 1.1184 0.8702 0.128 Uiso 1 1 calc R . . H51C H 0.8234 1.0977 0.9048 0.128 Uiso 1 1 calc R . . C53 C 0.9008(5) 0.8027(3) 0.5854(3) 0.0396(9) Uani 1 1 d . . . O53 O 0.8034(3) 0.8155(2) 0.52268(17) 0.0560(7) Uani 1 1 d . . . C55 C 0.8338(5) 0.8975(3) 0.4384(3) 0.0737(14) Uani 1 1 d . . . H55A H 0.8217 0.9643 0.4504 0.111 Uiso 1 1 calc R . . H55B H 0.7550 0.9014 0.4003 0.111 Uiso 1 1 calc R . . H55C H 0.9449 0.8813 0.4082 0.111 Uiso 1 1 calc R . . O56 O 1.0102(3) 0.8567(2) 0.57020(18) 0.0609(8) Uani 1 1 d . . . C72 C 0.5116(4) 0.8763(3) 0.7122(3) 0.0474(10) Uani 1 1 d . . . H72 H 0.5824 0.9009 0.6583 0.057 Uiso 1 1 calc R . . C73 C 0.4177(5) 0.9486(3) 0.7572(3) 0.0539(11) Uani 1 1 d . . . H73 H 0.4266 1.0203 0.7331 0.065 Uiso 1 1 calc R . . C84 C 0.3973(4) 0.7379(3) 0.8240(2) 0.0347(9) Uani 1 1 d . . . C74 C 0.3122(5) 0.9138(3) 0.8370(3) 0.0537(11) Uani 1 1 d . . . H74 H 0.2502 0.9619 0.8671 0.064 Uiso 1 1 calc R . . C75 C 0.2985(4) 0.8061(3) 0.8729(2) 0.0426(10) Uani 1 1 d . . . C76 C 0.1893(5) 0.7606(4) 0.9553(3) 0.0571(12) Uani 1 1 d . . . H76 H 0.1238 0.8045 0.9885 0.069 Uiso 1 1 calc R . . C83 C 0.3893(4) 0.6266(3) 0.8558(2) 0.0351(9) Uani 1 1 d . . . C77 C 0.1810(5) 0.6558(4) 0.9847(3) 0.0600(12) Uani 1 1 d . . . H771 H 0.1092 0.6289 1.0375 0.072 Uiso 1 1 calc R . . C78 C 0.2810(5) 0.5851(3) 0.9358(2) 0.0497(10) Uani 1 1 d . . . C79 C 0.2748(5) 0.4760(4) 0.9622(3) 0.0674(13) Uani 1 1 d . . . H79 H 0.2041 0.4454 1.0142 0.081 Uiso 1 1 calc R . . C80 C 0.3730(6) 0.4155(3) 0.9111(3) 0.0721(14) Uani 1 1 d . . . H80 H 0.3690 0.3432 0.9276 0.087 Uiso 1 1 calc R . . C81 C 0.4815(5) 0.4630(3) 0.8327(3) 0.0517(11) Uani 1 1 d . . . H81 H 0.5500 0.4201 0.7994 0.062 Uiso 1 1 calc R . . O43 O 0.8775(3) 0.60504(19) 0.81261(16) 0.0525(7) Uani 1 1 d . . . O44 O 1.1297(3) 0.6812(2) 0.71988(16) 0.0550(7) Uani 1 1 d . . . O91 O 0.1869(4) 0.1813(2) 0.74911(18) 0.0736(9) Uani 1 1 d . . . O92 O 0.1315(4) 0.1269(2) 0.9082(2) 0.0898(10) Uani 1 1 d . . . O93 O 0.3622(4) 0.2136(3) 0.8308(2) 0.1052(12) Uani 1 1 d . . . O94 O 0.0943(4) 0.3065(2) 0.8289(2) 0.0890(10) Uani 1 1 d . . . N11 N 0.7417(4) 0.5390(2) 0.6389(2) 0.0407(8) Uani 1 1 d . . . N22 N 0.5140(3) 0.7032(2) 0.57229(19) 0.0390(7) Uani 1 1 d . . . N41 N 0.8511(3) 0.7237(2) 0.66142(18) 0.0350(7) Uani 1 1 d . . . N71 N 0.5020(3) 0.7725(2) 0.74485(19) 0.0377(7) Uani 1 1 d . . . N82 N 0.4896(3) 0.5655(2) 0.80472(18) 0.0373(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0414(3) 0.0336(3) 0.0366(3) -0.0152(2) 0.0027(2) -0.0035(2) S42 0.0456(6) 0.0469(6) 0.0355(6) -0.0137(5) -0.0049(5) -0.0054(5) Cl9 0.0709(8) 0.0462(7) 0.0466(7) -0.0211(5) -0.0013(6) 0.0033(6) C12 0.042(2) 0.038(2) 0.071(3) -0.019(2) -0.002(2) 0.000(2) C13 0.045(3) 0.045(3) 0.086(4) -0.028(3) -0.005(2) 0.001(2) C14 0.047(3) 0.046(3) 0.095(4) -0.042(3) 0.024(3) -0.015(2) C15 0.038(2) 0.052(3) 0.059(3) -0.032(2) 0.011(2) -0.015(2) C16 0.037(2) 0.041(2) 0.037(2) -0.0174(19) 0.0056(17) -0.0161(19) C17 0.037(2) 0.046(2) 0.037(2) -0.0167(19) 0.0076(18) -0.019(2) C18 0.045(2) 0.069(3) 0.042(3) -0.022(2) 0.000(2) -0.024(2) C19 0.056(3) 0.092(4) 0.039(3) -0.012(3) -0.009(2) -0.028(3) C20 0.047(3) 0.075(3) 0.058(3) 0.001(3) -0.010(2) -0.013(3) C21 0.038(2) 0.051(3) 0.045(3) -0.013(2) -0.0024(19) -0.006(2) C23 0.064(3) 0.100(4) 0.044(3) -0.033(3) 0.011(2) -0.045(3) C24 0.062(3) 0.080(4) 0.072(3) -0.056(3) 0.022(3) -0.035(3) C45 0.044(2) 0.047(2) 0.032(2) -0.0115(19) -0.0050(18) -0.009(2) C46 0.057(3) 0.061(3) 0.050(3) -0.024(2) 0.001(2) -0.015(2) C47 0.082(3) 0.061(3) 0.057(3) -0.027(3) -0.007(3) -0.024(3) C48 0.060(3) 0.067(3) 0.052(3) -0.036(3) -0.016(2) 0.000(3) C49 0.055(3) 0.083(4) 0.043(3) -0.030(3) 0.000(2) -0.004(3) C50 0.052(2) 0.058(3) 0.040(2) -0.016(2) -0.002(2) -0.010(2) C51 0.090(4) 0.084(4) 0.093(4) -0.058(3) -0.014(3) 0.013(3) C53 0.038(2) 0.046(2) 0.037(2) -0.021(2) 0.0006(19) -0.002(2) O53 0.0644(18) 0.0603(19) 0.0414(17) -0.0007(15) -0.0116(15) -0.0241(16) C55 0.093(4) 0.073(3) 0.043(3) 0.011(2) -0.020(3) -0.020(3) O56 0.0606(18) 0.070(2) 0.0537(18) -0.0070(15) -0.0058(15) -0.0340(17) C72 0.049(2) 0.039(2) 0.044(2) -0.010(2) 0.0038(19) 0.002(2) C73 0.060(3) 0.035(2) 0.062(3) -0.019(2) -0.005(2) 0.008(2) C84 0.032(2) 0.040(2) 0.033(2) -0.0160(18) -0.0033(17) 0.0022(18) C74 0.052(3) 0.052(3) 0.064(3) -0.039(2) -0.012(2) 0.014(2) C75 0.033(2) 0.057(3) 0.043(2) -0.029(2) -0.0038(18) 0.002(2) C76 0.051(3) 0.077(3) 0.044(3) -0.037(3) 0.008(2) 0.003(3) C83 0.036(2) 0.042(2) 0.029(2) -0.0161(18) 0.0008(16) -0.0062(18) C77 0.055(3) 0.084(4) 0.039(3) -0.028(3) 0.015(2) -0.013(3) C78 0.052(2) 0.060(3) 0.034(2) -0.015(2) 0.0078(19) -0.015(2) C79 0.081(3) 0.075(4) 0.042(3) -0.015(3) 0.015(2) -0.029(3) C80 0.114(4) 0.048(3) 0.050(3) -0.007(2) 0.008(3) -0.035(3) C81 0.073(3) 0.042(2) 0.036(2) -0.014(2) 0.006(2) -0.010(2) O43 0.0746(18) 0.0421(16) 0.0363(15) -0.0045(13) -0.0069(13) -0.0119(15) O44 0.0402(15) 0.071(2) 0.0545(17) -0.0246(15) -0.0117(13) 0.0036(14) O91 0.110(2) 0.0618(19) 0.0518(18) -0.0324(16) -0.0127(17) 0.0075(18) O92 0.128(3) 0.067(2) 0.056(2) -0.0107(18) 0.0086(19) -0.009(2) O93 0.072(2) 0.146(3) 0.111(3) -0.059(3) -0.015(2) -0.011(2) O94 0.115(3) 0.059(2) 0.087(2) -0.0409(18) -0.008(2) 0.0262(19) N11 0.0427(19) 0.0368(19) 0.043(2) -0.0188(16) 0.0070(15) -0.0093(16) N22 0.0341(17) 0.0429(19) 0.0394(18) -0.0125(16) -0.0028(15) -0.0065(16) N41 0.0361(17) 0.0387(18) 0.0293(17) -0.0133(15) 0.0015(13) -0.0052(15) N71 0.0406(17) 0.0335(18) 0.0347(18) -0.0089(15) -0.0021(14) -0.0016(15) N82 0.0475(18) 0.0301(17) 0.0337(17) -0.0108(15) -0.0014(14) -0.0073(15) _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 N71 1.999(3) . ? Cu1 N11 2.011(3) . ? Cu1 N41 2.078(3) . ? Cu1 N82 2.101(3) . ? Cu1 N22 2.168(3) . ? S42 O44 1.445(2) . ? S42 O43 1.449(2) . ? S42 N41 1.638(3) . ? S42 C45 1.774(4) . ? Cl9 O94 1.407(3) . ? Cl9 O91 1.426(3) . ? Cl9 O92 1.435(3) . ? Cl9 O93 1.447(3) . ? C12 N11 1.341(4) . ? C12 C13 1.406(5) . ? C13 C14 1.379(6) . ? C14 C15 1.384(6) . ? C15 C16 1.416(5) . ? C15 C24 1.430(6) . ? C16 N11 1.357(4) . ? C16 C17 1.428(5) . ? C17 N22 1.359(4) . ? C17 C18 1.418(5) . ? C18 C19 1.395(5) . ? C18 C23 1.429(5) . ? C19 C20 1.349(5) . ? C20 C21 1.409(5) . ? C21 N22 1.333(4) . ? C23 C24 1.350(6) . ? C45 C50 1.384(5) . ? C45 C46 1.400(5) . ? C46 C47 1.384(5) . ? C47 C48 1.373(5) . ? C48 C49 1.392(5) . ? C48 C51 1.522(5) . ? C49 C50 1.374(5) . ? C53 O56 1.215(4) . ? C53 O53 1.354(4) . ? C53 N41 1.375(4) . ? O53 C55 1.442(4) . ? C72 N71 1.340(4) . ? C72 C73 1.398(5) . ? C73 C74 1.376(5) . ? C84 N71 1.365(4) . ? C84 C75 1.409(4) . ? C84 C83 1.432(5) . ? C74 C75 1.398(5) . ? C75 C76 1.450(5) . ? C76 C77 1.350(5) . ? C83 N82 1.371(4) . ? C83 C78 1.408(4) . ? C77 C78 1.438(5) . ? C78 C79 1.402(5) . ? C79 C80 1.359(5) . ? C80 C81 1.416(5) . ? C81 N82 1.320(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N71 Cu1 N11 174.27(12) . . ? N71 Cu1 N41 92.71(11) . . ? N11 Cu1 N41 92.86(11) . . ? N71 Cu1 N82 80.81(12) . . ? N11 Cu1 N82 95.82(11) . . ? N41 Cu1 N82 138.90(11) . . ? N71 Cu1 N22 97.00(12) . . ? N11 Cu1 N22 79.81(13) . . ? N41 Cu1 N22 110.00(11) . . ? N82 Cu1 N22 111.06(11) . . ? O44 S42 O43 118.59(16) . . ? O44 S42 N41 111.95(14) . . ? O43 S42 N41 103.79(15) . . ? O44 S42 C45 108.48(16) . . ? O43 S42 C45 106.46(16) . . ? N41 S42 C45 106.87(16) . . ? O94 Cl9 O91 110.87(19) . . ? O94 Cl9 O92 110.19(19) . . ? O91 Cl9 O92 110.16(19) . . ? O94 Cl9 O93 108.6(2) . . ? O91 Cl9 O93 107.6(2) . . ? O92 Cl9 O93 109.4(2) . . ? N11 C12 C13 121.1(4) . . ? C14 C13 C12 118.5(4) . . ? C13 C14 C15 121.9(4) . . ? C14 C15 C16 116.3(4) . . ? C14 C15 C24 125.2(4) . . ? C16 C15 C24 118.5(4) . . ? N11 C16 C15 122.4(4) . . ? N11 C16 C17 117.6(3) . . ? C15 C16 C17 120.0(4) . . ? N22 C17 C18 122.9(4) . . ? N22 C17 C16 117.3(3) . . ? C18 C17 C16 119.8(4) . . ? C19 C18 C17 116.5(4) . . ? C19 C18 C23 124.7(4) . . ? C17 C18 C23 118.7(4) . . ? C20 C19 C18 120.7(4) . . ? C19 C20 C21 119.7(4) . . ? N22 C21 C20 121.9(4) . . ? C24 C23 C18 121.2(4) . . ? C23 C24 C15 121.6(4) . . ? C50 C45 C46 119.1(4) . . ? C50 C45 S42 120.4(3) . . ? C46 C45 S42 120.4(3) . . ? C47 C46 C45 119.3(4) . . ? C48 C47 C46 121.9(4) . . ? C47 C48 C49 117.9(4) . . ? C47 C48 C51 121.6(4) . . ? C49 C48 C51 120.4(4) . . ? C50 C49 C48 121.4(4) . . ? C49 C50 C45 120.3(4) . . ? O56 C53 O53 121.2(4) . . ? O56 C53 N41 130.4(4) . . ? O53 C53 N41 108.4(3) . . ? C53 O53 C55 116.7(3) . . ? N71 C72 C73 121.6(4) . . ? C74 C73 C72 120.1(4) . . ? N71 C84 C75 123.2(3) . . ? N71 C84 C83 116.5(3) . . ? C75 C84 C83 120.3(3) . . ? C73 C74 C75 119.8(4) . . ? C74 C75 C84 116.9(3) . . ? C74 C75 C76 124.8(4) . . ? C84 C75 C76 118.4(4) . . ? C77 C76 C75 121.2(4) . . ? N82 C83 C78 123.3(3) . . ? N82 C83 C84 116.8(3) . . ? C78 C83 C84 119.9(3) . . ? C76 C77 C78 121.2(4) . . ? C79 C78 C83 117.4(4) . . ? C79 C78 C77 123.6(4) . . ? C83 C78 C77 119.0(4) . . ? C80 C79 C78 119.4(4) . . ? C79 C80 C81 119.7(4) . . ? N82 C81 C80 122.8(4) . . ? C12 N11 C16 119.7(3) . . ? C12 N11 Cu1 125.5(3) . . ? C16 N11 Cu1 114.7(3) . . ? C21 N22 C17 118.2(3) . . ? C21 N22 Cu1 131.5(3) . . ? C17 N22 Cu1 109.3(2) . . ? C53 N41 S42 117.5(2) . . ? C53 N41 Cu1 127.3(2) . . ? S42 N41 Cu1 113.87(15) . . ? C72 N71 C84 118.3(3) . . ? C72 N71 Cu1 126.9(2) . . ? C84 N71 Cu1 114.8(2) . . ? C81 N82 C83 117.4(3) . . ? C81 N82 Cu1 131.6(3) . . ? C83 N82 Cu1 111.1(2) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.418 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.068 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END data_Complex2 #TrackingRef '- C1DT11622C_ccdc_795631_815020_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 795632' #TrackingRef 'complex1, 2 and 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H66 Cl2 Cu4 N10 O25 S2 ' _chemical_formula_weight 1692.39 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' O O 0.0106 0.0060 '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' 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1797(8) _cell_length_b 18.8798(8) _cell_length_c 29.5552(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.373(6) _cell_angle_gamma 90.00 _cell_volume 6766.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 42014 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 30.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 1.469 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.877 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; there were solvent accessible voids in the structure but no significant electron density was located therein isor was necessarily applied to several carbon atoms ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42014 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.2715 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 30.00 _reflns_number_total 19385 _reflns_number_gt 6984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0644P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19385 _refine_ls_number_parameters 912 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1965 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1723 _refine_ls_wR_factor_gt 0.1494 _refine_ls_goodness_of_fit_ref 0.811 _refine_ls_restrained_S_all 0.810 _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 Cu2 Cu 0.52677(6) 0.07261(4) 0.20109(3) 0.01391(19) Uani 1 1 d . . . Cu4 Cu 0.49362(6) 0.13373(4) 0.28923(3) 0.01168(18) Uani 1 1 d . . . Cu1 Cu 0.47144(6) 0.31831(4) 0.30048(3) 0.01121(18) Uani 1 1 d . . . Cu3 Cu 0.50343(6) 0.25523(4) 0.21328(3) 0.01079(17) Uani 1 1 d . . . O1 O 0.4199(3) 0.07116(19) 0.24517(14) 0.0161(10) Uani 1 1 d . . . H1 H 0.3530 0.0474 0.2451 0.019 Uiso 1 1 calc R . . O2 O 0.5859(3) 0.15210(18) 0.23926(13) 0.0098(9) Uani 1 1 d . . . H2 H 0.6659 0.1533 0.2470 0.012 Uiso 1 1 calc R . . O3 O 0.4130(3) 0.23693(19) 0.26358(14) 0.0123(9) Uani 1 1 d . . . H3 H 0.3330 0.2357 0.2559 0.015 Uiso 1 1 calc R . . O4 O 0.5783(3) 0.31798(19) 0.25755(14) 0.0142(10) Uani 1 1 d . . . H4 H 0.6458 0.3410 0.2578 0.017 Uiso 1 1 calc R . . N11 N 0.3780(4) 0.3019(2) 0.35154(17) 0.0124(11) Uani 1 1 d U . . C12 C 0.2789(5) 0.2714(3) 0.3483(2) 0.0158(15) Uani 1 1 d . . . H12 H 0.2461 0.2593 0.3197 0.019 Uiso 1 1 calc R . . C13 C 0.2227(6) 0.2571(3) 0.3859(2) 0.0250(18) Uani 1 1 d . . . H13 H 0.1534 0.2360 0.3827 0.030 Uiso 1 1 calc R . . C14 C 0.2716(6) 0.2747(3) 0.4278(3) 0.0302(19) Uani 1 1 d . . . H14 H 0.2367 0.2646 0.4537 0.036 Uiso 1 1 calc R . . C15 C 0.3720(6) 0.3072(3) 0.4314(2) 0.0226(16) Uani 1 1 d . . . H15 H 0.4052 0.3202 0.4599 0.027 Uiso 1 1 calc R . . C16 C 0.4242(5) 0.3209(3) 0.3930(2) 0.0143(14) Uani 1 1 d U . . C17 C 0.5331(5) 0.3552(3) 0.3927(2) 0.0159(14) Uani 1 1 d U . . C18 C 0.5943(6) 0.3824(3) 0.4307(2) 0.0291(19) Uani 1 1 d . . . H18 H 0.5678 0.3799 0.4591 0.035 Uiso 1 1 calc R . . C19 C 0.6948(6) 0.4130(4) 0.4257(3) 0.0314(19) Uani 1 1 d . . . H19 H 0.7359 0.4321 0.4509 0.038 Uiso 1 1 calc R . . C20 C 0.7343(6) 0.4157(3) 0.3844(3) 0.0299(19) Uani 1 1 d . . . H20 H 0.8033 0.4351 0.3812 0.036 Uiso 1 1 calc R . . C21 C 0.6704(5) 0.3891(3) 0.3471(2) 0.0181(15) Uani 1 1 d U . . H21 H 0.6960 0.3919 0.3185 0.022 Uiso 1 1 calc R . . N22 N 0.5725(4) 0.3594(2) 0.35165(18) 0.0154(12) Uani 1 1 d . . . N31 N 0.4261(4) 0.0298(2) 0.15146(18) 0.0159(12) Uani 1 1 d . . . C32 C 0.3291(5) -0.0002(3) 0.1561(2) 0.0214(16) Uani 1 1 d . . . H32 H 0.3040 -0.0018 0.1848 0.026 Uiso 1 1 calc R . . C33 C 0.2646(6) -0.0287(3) 0.1203(2) 0.0247(17) Uani 1 1 d . . . H33 H 0.1972 -0.0494 0.1249 0.030 Uiso 1 1 calc R . . C34 C 0.3001(6) -0.0266(3) 0.0778(3) 0.0266(17) Uani 1 1 d . . . H34 H 0.2568 -0.0451 0.0531 0.032 Uiso 1 1 calc R . . C35 C 0.4025(5) 0.0038(3) 0.0723(2) 0.0232(16) Uani 1 1 d . . . H35 H 0.4296 0.0051 0.0439 0.028 Uiso 1 1 calc R . . C36 C 0.4627(5) 0.0318(3) 0.1101(2) 0.0180(15) Uani 1 1 d . . . C37 C 0.5733(5) 0.0659(3) 0.1086(2) 0.0163(14) Uani 1 1 d . . . C38 C 0.6255(5) 0.0744(3) 0.0696(2) 0.0196(15) Uani 1 1 d . . . H38 H 0.5931 0.0582 0.0418 0.024 Uiso 1 1 calc R . . C39 C 0.7279(5) 0.1077(3) 0.0728(2) 0.0199(15) Uani 1 1 d . . . H39 H 0.7645 0.1145 0.0469 0.024 Uiso 1 1 calc R . . C40 C 0.7743(6) 0.1302(3) 0.1140(2) 0.0183(16) Uani 1 1 d . . . H40 H 0.8428 0.1524 0.1166 0.022 Uiso 1 1 calc R . . C41 C 0.7172(5) 0.1196(3) 0.1522(2) 0.0155(14) Uani 1 1 d . . . H41 H 0.7488 0.1346 0.1805 0.019 Uiso 1 1 calc R . . N42 N 0.6188(4) 0.0885(2) 0.14927(18) 0.0159(12) Uani 1 1 d . . . N51 N 0.5870(4) 0.2777(2) 0.16107(18) 0.0123(11) Uani 1 1 d . . . C52 C 0.6864(5) 0.3091(3) 0.1635(2) 0.0164(15) Uani 1 1 d . . . H52 H 0.7198 0.3219 0.1919 0.020 Uiso 1 1 calc R . . C53 C 0.7412(6) 0.3231(3) 0.1254(2) 0.0218(16) Uani 1 1 d . . . H53 H 0.8094 0.3456 0.1281 0.026 Uiso 1 1 calc R . . C54 C 0.6919(6) 0.3028(3) 0.0837(2) 0.0229(16) Uani 1 1 d . . . H54 H 0.7267 0.3114 0.0576 0.027 Uiso 1 1 calc R . . C55 C 0.5906(5) 0.2694(3) 0.0807(2) 0.0170(15) Uani 1 1 d . . . H55 H 0.5569 0.2550 0.0527 0.020 Uiso 1 1 calc R . . C56 C 0.5397(5) 0.2577(3) 0.1203(2) 0.0139(14) Uani 1 1 d . . . C57 C 0.4312(5) 0.2236(3) 0.1212(2) 0.0140(14) Uani 1 1 d U . . C58 C 0.3657(6) 0.2050(3) 0.0827(2) 0.0201(16) Uani 1 1 d . . . H58 H 0.3894 0.2117 0.0540 0.024 Uiso 1 1 calc R . . C59 C 0.2634(6) 0.1758(3) 0.0879(2) 0.0253(17) Uani 1 1 d . . . H59 H 0.2180 0.1616 0.0624 0.030 Uiso 1 1 calc R . . C60 C 0.2286(6) 0.1678(3) 0.1303(2) 0.0229(17) Uani 1 1 d . . . H60 H 0.1590 0.1497 0.1341 0.028 Uiso 1 1 calc R . . C61 C 0.2992(5) 0.1871(3) 0.1669(2) 0.0187(15) Uani 1 1 d . . . H61 H 0.2770 0.1804 0.1958 0.022 Uiso 1 1 calc R . . N62 N 0.3978(4) 0.2149(2) 0.16304(18) 0.0123(12) Uani 1 1 d . . . N71 N 0.5940(4) 0.1728(2) 0.34066(18) 0.0148(12) Uani 1 1 d . . . C72 C 0.6937(5) 0.2029(3) 0.3386(2) 0.0184(16) Uani 1 1 d . . . H72 H 0.7192 0.2096 0.3102 0.022 Uiso 1 1 calc R . . C73 C 0.7594(6) 0.2243(3) 0.3763(2) 0.0237(17) Uani 1 1 d . . . H73 H 0.8278 0.2448 0.3734 0.028 Uiso 1 1 calc R . . C74 C 0.7224(6) 0.2151(3) 0.4185(2) 0.0236(17) Uani 1 1 d . . . H74 H 0.7655 0.2293 0.4445 0.028 Uiso 1 1 calc R . . C75 C 0.6198(6) 0.1842(3) 0.4216(2) 0.0194(15) Uani 1 1 d . . . H75 H 0.5927 0.1781 0.4498 0.023 Uiso 1 1 calc R . . C76 C 0.5590(5) 0.1629(3) 0.3825(2) 0.0167(15) Uani 1 1 d . . . C77 C 0.4490(5) 0.1290(3) 0.3822(2) 0.0166(15) Uani 1 1 d . . . C78 C 0.3928(5) 0.1169(3) 0.4202(2) 0.0196(15) Uani 1 1 d . . . H78 H 0.4252 0.1283 0.4491 0.023 Uiso 1 1 calc R . . C79 C 0.2884(6) 0.0877(3) 0.4149(2) 0.0234(17) Uani 1 1 d . . . H79 H 0.2485 0.0807 0.4398 0.028 Uiso 1 1 calc R . . C80 C 0.2452(5) 0.0694(3) 0.3724(2) 0.0183(15) Uani 1 1 d . . . H80 H 0.1755 0.0490 0.3684 0.022 Uiso 1 1 calc R . . C81 C 0.3032(5) 0.0808(3) 0.3352(2) 0.0162(15) Uani 1 1 d . . . H81 H 0.2729 0.0674 0.3065 0.019 Uiso 1 1 calc R . . N82 N 0.4015(4) 0.1106(2) 0.34029(17) 0.0138(12) Uani 1 1 d . . . N91 N 0.6527(4) -0.0136(3) 0.23513(18) 0.0151(12) Uani 1 1 d . . . S92 S 0.75407(13) 0.00348(8) 0.27109(6) 0.0144(4) Uani 1 1 d . . . O93 O 0.8462(3) -0.0452(2) 0.26997(15) 0.0181(10) Uani 1 1 d . . . O94 O 0.7846(3) 0.0772(2) 0.26545(15) 0.0180(10) Uani 1 1 d . . . C95 C 0.7083(6) -0.0021(3) 0.3264(2) 0.0179(15) Uani 1 1 d . . . C96 C 0.7825(5) 0.0161(3) 0.3631(2) 0.0180(15) Uani 1 1 d . . . H96 H 0.8534 0.0306 0.3581 0.022 Uiso 1 1 calc R . . C97 C 0.7526(6) 0.0128(3) 0.4064(2) 0.0252(17) Uani 1 1 d . . . H97 H 0.8029 0.0252 0.4307 0.030 Uiso 1 1 calc R . . C98 C 0.6453(6) -0.0094(3) 0.4143(2) 0.0246(17) Uani 1 1 d . . . C99 C 0.5713(6) -0.0262(3) 0.3783(2) 0.0219(16) Uani 1 1 d . . . H99 H 0.5003 -0.0402 0.3834 0.026 Uiso 1 1 calc R . . C100 C 0.6012(5) -0.0225(3) 0.3336(2) 0.0191(15) Uani 1 1 d . . . H100 H 0.5503 -0.0335 0.3092 0.023 Uiso 1 1 calc R . . C101 C 0.6120(6) -0.0141(4) 0.4619(3) 0.041(2) Uani 1 1 d . . . H10A H 0.5375 -0.0309 0.4611 0.062 Uiso 1 1 calc R . . H10B H 0.6170 0.0320 0.4757 0.062 Uiso 1 1 calc R . . H10C H 0.6602 -0.0462 0.4793 0.062 Uiso 1 1 calc R . . C911 C 0.6210(5) -0.0815(3) 0.2314(2) 0.0201(16) Uani 1 1 d . . . O912 O 0.6480(4) -0.1317(2) 0.25510(18) 0.0360(14) Uani 1 1 d . . . O913 O 0.5455(4) -0.0875(2) 0.19500(15) 0.0218(11) Uani 1 1 d . . . C914 C 0.4922(6) -0.1553(3) 0.1889(3) 0.0299(18) Uani 1 1 d . . . H91A H 0.5471 -0.1919 0.1898 0.045 Uiso 1 1 calc R . . H91B H 0.4489 -0.1563 0.1601 0.045 Uiso 1 1 calc R . . H91C H 0.4453 -0.1629 0.2128 0.045 Uiso 1 1 calc R . . N111 N 0.3504(4) 0.4033(2) 0.26616(18) 0.0156(12) Uani 1 1 d . . . S112 S 0.25052(13) 0.38738(7) 0.22924(6) 0.0151(4) Uani 1 1 d . . . O113 O 0.2215(3) 0.31386(19) 0.23507(16) 0.0207(11) Uani 1 1 d . . . O114 O 0.1594(3) 0.4364(2) 0.23063(16) 0.0208(11) Uani 1 1 d . . . C115 C 0.2971(5) 0.3941(3) 0.1743(2) 0.0142(14) Uani 1 1 d . . . C116 C 0.4043(5) 0.4140(3) 0.1673(2) 0.0133(14) Uani 1 1 d . . . H116 H 0.4548 0.4246 0.1920 0.016 Uiso 1 1 calc R . . C117 C 0.4350(5) 0.4181(3) 0.1238(2) 0.0197(16) Uani 1 1 d . . . H117 H 0.5065 0.4320 0.1195 0.024 Uiso 1 1 calc R . . C118 C 0.3634(6) 0.4022(3) 0.0865(3) 0.0273(18) Uani 1 1 d . . . C119 C 0.2558(6) 0.3805(3) 0.0944(2) 0.0270(18) Uani 1 1 d . . . H119 H 0.2055 0.3686 0.0700 0.032 Uiso 1 1 calc R . . C120 C 0.2247(6) 0.3769(3) 0.1378(2) 0.0221(17) Uani 1 1 d . . . H120 H 0.1535 0.3625 0.1425 0.026 Uiso 1 1 calc R . . C121 C 0.3952(7) 0.4064(4) 0.0385(3) 0.046(2) Uani 1 1 d . . . H12A H 0.3399 0.3834 0.0184 0.069 Uiso 1 1 calc R . . H12B H 0.4649 0.3832 0.0368 0.069 Uiso 1 1 calc R . . H12C H 0.4011 0.4551 0.0298 0.069 Uiso 1 1 calc R . . C131 C 0.3865(5) 0.4722(3) 0.2724(2) 0.0143(14) Uani 1 1 d U . . O132 O 0.3565(4) 0.5243(2) 0.24878(15) 0.0210(11) Uani 1 1 d . . . O133 O 0.4578(4) 0.4777(2) 0.30877(15) 0.0207(11) Uani 1 1 d U . . C134 C 0.5090(6) 0.5446(3) 0.3147(3) 0.0317(19) Uani 1 1 d . . . H13A H 0.5426 0.5571 0.2877 0.048 Uiso 1 1 calc R . . H13B H 0.5645 0.5427 0.3400 0.048 Uiso 1 1 calc R . . H13C H 0.4548 0.5796 0.3205 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.98818(14) 0.26195(9) 0.04656(6) 0.0259(4) Uani 1 1 d . . . O11 O 0.9677(6) 0.1872(3) 0.0462(2) 0.075(2) Uani 1 1 d . . . O12 O 0.8984(5) 0.2959(3) 0.02076(19) 0.0579(18) Uani 1 1 d . . . O13 O 1.0873(4) 0.2753(3) 0.02549(18) 0.0554(17) Uani 1 1 d . . . O14 O 0.9996(4) 0.2866(3) 0.09225(17) 0.0432(15) Uani 1 1 d . . . Cl2 Cl 0.48667(15) 0.16501(9) 0.96352(6) 0.0259(4) Uani 1 1 d . . . O21 O 0.4712(4) 0.1583(3) 0.91516(17) 0.0442(15) Uani 1 1 d . . . O22 O 0.4511(5) 0.2350(3) 0.97644(18) 0.0508(17) Uani 1 1 d . . . O23 O 0.6000(4) 0.1559(3) 0.97967(17) 0.0363(13) Uani 1 1 d . . . O24 O 0.4218(4) 0.1124(3) 0.98478(19) 0.0503(16) Uani 1 1 d . . . O5 O 0.3687(4) 0.6702(2) 0.23767(16) 0.0269(12) Uani 1 1 d . . . O6 O 0.9944(6) 0.2215(4) 0.1847(2) 0.096(3) Uani 1 1 d . . . O7 O 0.5112(4) 0.3675(3) 0.9189(2) 0.0616(18) Uani 1 1 d . . . O8 O 0.4648(4) 0.3490(3) 0.82020(19) 0.0459(15) Uani 1 1 d . . . O9 O 0.6590(7) -0.2743(3) 0.2599(3) 0.094(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu2 0.0134(5) 0.0145(4) 0.0144(5) -0.0028(3) 0.0044(4) -0.0029(3) Cu4 0.0106(4) 0.0126(4) 0.0121(4) -0.0011(3) 0.0024(3) -0.0008(3) Cu1 0.0091(4) 0.0104(4) 0.0142(4) -0.0021(3) 0.0013(3) 0.0000(3) Cu3 0.0068(4) 0.0121(4) 0.0133(4) -0.0020(3) -0.0002(3) -0.0006(3) O1 0.012(2) 0.014(2) 0.024(3) -0.0032(18) 0.009(2) -0.0046(17) O2 0.006(2) 0.009(2) 0.015(2) 0.0003(17) 0.0085(19) 0.0006(16) O3 0.004(2) 0.018(2) 0.015(2) -0.0011(18) -0.0009(19) 0.0006(17) O4 0.007(2) 0.020(2) 0.015(3) -0.0020(18) -0.004(2) -0.0061(17) N11 0.0119(14) 0.0121(13) 0.0131(14) 0.0007(9) 0.0017(9) 0.0016(9) C12 0.016(4) 0.013(3) 0.018(4) 0.005(3) 0.000(3) 0.005(3) C13 0.019(4) 0.027(4) 0.031(5) 0.013(3) 0.012(4) 0.006(3) C14 0.038(5) 0.027(4) 0.028(5) 0.013(3) 0.017(4) 0.020(3) C15 0.034(5) 0.020(4) 0.014(4) 0.001(3) 0.005(4) 0.009(3) C16 0.018(4) 0.008(3) 0.016(3) 0.004(2) 0.000(3) 0.010(2) C17 0.022(4) 0.007(3) 0.018(4) -0.001(2) -0.001(3) 0.010(2) C18 0.045(5) 0.023(4) 0.017(4) 0.001(3) -0.008(4) 0.013(3) C19 0.028(5) 0.033(4) 0.029(5) -0.014(3) -0.017(4) -0.005(3) C20 0.031(5) 0.016(4) 0.040(5) -0.001(3) -0.012(4) 0.000(3) C21 0.010(4) 0.023(3) 0.020(4) 0.001(3) -0.005(3) -0.004(3) N22 0.014(3) 0.009(2) 0.022(3) -0.001(2) -0.003(3) 0.001(2) N31 0.017(3) 0.017(3) 0.014(3) 0.001(2) 0.004(3) -0.001(2) C32 0.021(4) 0.021(4) 0.023(4) 0.000(3) 0.005(3) -0.002(3) C33 0.014(4) 0.030(4) 0.029(5) 0.000(3) -0.001(4) -0.010(3) C34 0.030(5) 0.017(4) 0.031(5) -0.006(3) -0.008(4) -0.004(3) C35 0.022(4) 0.030(4) 0.017(4) -0.006(3) -0.001(3) -0.009(3) C36 0.016(4) 0.021(3) 0.017(4) -0.004(3) 0.004(3) -0.004(3) C37 0.014(4) 0.021(3) 0.014(4) -0.001(3) 0.001(3) 0.002(3) C38 0.013(4) 0.026(4) 0.019(4) -0.004(3) 0.000(3) 0.002(3) C39 0.022(4) 0.028(4) 0.011(4) 0.002(3) 0.008(3) 0.007(3) C40 0.016(4) 0.022(4) 0.017(4) 0.005(3) 0.003(3) 0.006(3) C41 0.013(4) 0.017(3) 0.017(4) 0.002(3) 0.005(3) 0.000(3) N42 0.013(3) 0.016(3) 0.019(3) 0.000(2) 0.005(3) 0.001(2) N51 0.008(3) 0.009(2) 0.019(3) 0.001(2) -0.004(2) 0.000(2) C52 0.013(4) 0.013(3) 0.022(4) -0.001(3) 0.000(3) 0.007(3) C53 0.016(4) 0.023(4) 0.029(5) -0.001(3) 0.010(3) 0.003(3) C54 0.023(4) 0.030(4) 0.016(4) 0.000(3) 0.009(3) 0.007(3) C55 0.011(4) 0.021(3) 0.019(4) -0.001(3) 0.001(3) -0.001(3) C56 0.013(4) 0.010(3) 0.021(4) 0.005(3) 0.010(3) 0.006(2) C57 0.004(3) 0.018(3) 0.019(4) -0.002(3) -0.003(3) 0.005(2) C58 0.021(4) 0.024(4) 0.015(4) -0.004(3) 0.000(3) -0.004(3) C59 0.024(4) 0.031(4) 0.020(4) -0.009(3) -0.008(4) -0.004(3) C60 0.022(4) 0.018(4) 0.030(4) -0.006(3) 0.006(4) -0.008(3) C61 0.013(4) 0.020(3) 0.024(4) -0.001(3) 0.008(3) -0.002(3) N62 0.006(3) 0.014(3) 0.017(3) -0.004(2) 0.003(2) 0.001(2) N71 0.016(3) 0.010(3) 0.018(3) 0.002(2) 0.001(3) -0.001(2) C72 0.011(4) 0.013(3) 0.031(4) -0.002(3) 0.001(3) -0.002(3) C73 0.011(4) 0.028(4) 0.030(5) -0.006(3) -0.005(3) 0.001(3) C74 0.026(5) 0.020(4) 0.023(4) -0.001(3) -0.008(4) 0.006(3) C75 0.021(4) 0.018(3) 0.017(4) -0.001(3) -0.007(3) 0.004(3) C76 0.024(4) 0.007(3) 0.020(4) 0.000(3) 0.005(3) 0.004(3) C77 0.016(4) 0.016(3) 0.017(4) 0.005(3) -0.007(3) 0.003(3) C78 0.022(4) 0.028(4) 0.009(4) 0.001(3) 0.006(3) 0.004(3) C79 0.025(4) 0.021(4) 0.027(4) 0.004(3) 0.014(4) -0.001(3) C80 0.011(4) 0.013(3) 0.032(4) 0.004(3) 0.004(3) -0.006(2) C81 0.014(4) 0.010(3) 0.025(4) 0.000(3) 0.003(3) 0.000(2) N82 0.016(3) 0.016(3) 0.012(3) 0.001(2) 0.009(3) 0.002(2) N91 0.007(3) 0.021(3) 0.017(3) -0.006(2) -0.003(2) 0.006(2) S92 0.0120(9) 0.0155(8) 0.0157(9) -0.0019(6) 0.0006(7) 0.0049(6) O93 0.008(2) 0.020(2) 0.025(3) -0.0034(19) -0.006(2) 0.0076(18) O94 0.022(3) 0.016(2) 0.018(3) 0.0015(18) 0.009(2) 0.0010(18) C95 0.021(4) 0.010(3) 0.024(4) -0.003(3) 0.008(3) 0.006(3) C96 0.011(4) 0.019(3) 0.024(4) 0.000(3) 0.002(3) 0.001(3) C97 0.021(4) 0.034(4) 0.020(4) 0.000(3) -0.001(4) 0.008(3) C98 0.034(5) 0.022(4) 0.019(4) 0.002(3) 0.005(4) 0.017(3) C99 0.024(4) 0.018(3) 0.025(4) 0.001(3) 0.009(4) 0.005(3) C100 0.016(4) 0.019(3) 0.022(4) -0.003(3) 0.003(3) 0.004(3) C101 0.037(5) 0.060(5) 0.030(5) 0.005(4) 0.018(4) 0.015(4) C911 0.016(4) 0.016(3) 0.028(4) -0.009(3) 0.001(3) 0.008(3) O912 0.044(4) 0.014(2) 0.045(4) -0.006(2) -0.022(3) 0.004(2) O913 0.030(3) 0.016(2) 0.019(3) -0.0030(18) 0.002(2) -0.0090(19) C914 0.029(5) 0.027(4) 0.034(5) -0.011(3) 0.004(4) 0.005(3) N111 0.015(3) 0.012(3) 0.019(3) 0.005(2) 0.000(3) 0.005(2) S112 0.0098(9) 0.0120(8) 0.0232(10) 0.0015(6) 0.0007(8) 0.0002(6) O113 0.014(3) 0.011(2) 0.036(3) 0.0054(19) 0.001(2) -0.0044(17) O114 0.010(2) 0.018(2) 0.035(3) 0.002(2) 0.004(2) 0.0070(18) C115 0.016(4) 0.010(3) 0.015(4) 0.001(3) -0.006(3) 0.002(3) C116 0.010(4) 0.006(3) 0.023(4) 0.002(3) 0.002(3) 0.001(2) C117 0.009(4) 0.020(4) 0.030(4) -0.001(3) 0.005(3) 0.003(3) C118 0.036(5) 0.023(4) 0.024(4) 0.001(3) 0.011(4) 0.002(3) C119 0.037(5) 0.026(4) 0.014(4) -0.004(3) -0.013(4) 0.002(3) C120 0.018(4) 0.022(4) 0.026(4) -0.002(3) -0.005(4) -0.003(3) C121 0.050(6) 0.062(6) 0.026(5) 0.004(4) 0.006(5) 0.016(4) C131 0.009(3) 0.022(3) 0.013(3) 0.001(3) 0.007(3) 0.003(2) O132 0.020(3) 0.016(2) 0.025(3) 0.004(2) -0.008(2) 0.0011(19) O133 0.0190(13) 0.0225(13) 0.0201(13) -0.0013(9) -0.0005(9) 0.0001(9) C134 0.018(4) 0.032(4) 0.046(5) -0.008(4) 0.012(4) -0.015(3) Cl1 0.0204(10) 0.0365(10) 0.0212(10) 0.0009(7) 0.0046(8) -0.0055(7) O11 0.120(6) 0.044(4) 0.063(5) 0.002(3) 0.029(5) -0.032(4) O12 0.043(4) 0.099(5) 0.030(4) 0.004(3) -0.005(3) 0.034(3) O13 0.032(4) 0.113(5) 0.023(3) 0.008(3) 0.010(3) -0.016(3) O14 0.028(3) 0.084(4) 0.017(3) -0.007(3) -0.002(3) -0.008(3) Cl2 0.0233(11) 0.0372(10) 0.0167(9) 0.0016(7) -0.0007(8) -0.0012(7) O21 0.047(4) 0.065(4) 0.019(3) 0.004(3) -0.002(3) 0.004(3) O22 0.080(5) 0.036(3) 0.035(4) -0.006(2) 0.000(3) 0.025(3) O23 0.020(3) 0.057(3) 0.033(3) 0.013(3) 0.008(3) 0.002(2) O24 0.042(4) 0.062(4) 0.048(4) 0.016(3) 0.008(3) -0.019(3) O5 0.027(3) 0.017(2) 0.035(3) -0.001(2) -0.002(3) 0.0059(19) O6 0.083(6) 0.108(6) 0.088(6) 0.070(5) -0.048(5) -0.056(4) O7 0.027(4) 0.073(4) 0.085(5) -0.010(4) 0.003(4) -0.010(3) O8 0.038(4) 0.049(3) 0.053(4) -0.002(3) 0.019(3) -0.009(3) O9 0.123(7) 0.069(5) 0.088(6) 0.001(4) -0.005(5) 0.003(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 Cu2 O1 1.926(4) . ? Cu2 O2 1.973(4) . ? Cu2 N31 1.993(5) . ? Cu2 N42 2.003(5) . ? Cu2 N91 2.393(5) . ? Cu2 Cu4 2.9115(11) . ? Cu4 O1 1.918(4) . ? Cu4 O2 1.969(4) . ? Cu4 N71 2.000(5) . ? Cu4 N82 2.011(5) . ? Cu4 O3 2.279(4) . ? Cu1 O4 1.900(4) . ? Cu1 O3 1.977(4) . ? Cu1 N11 1.997(5) . ? Cu1 N22 2.014(5) . ? Cu1 N111 2.344(5) . ? Cu1 Cu3 2.8983(10) . ? Cu3 O4 1.929(4) . ? Cu3 O3 1.962(4) . ? Cu3 N51 1.972(5) . ? Cu3 N62 2.021(5) . ? Cu3 O2 2.290(4) . ? N11 C12 1.333(7) . ? N11 C16 1.349(8) . ? C12 C13 1.386(8) . ? C13 C14 1.362(10) . ? C14 C15 1.364(9) . ? C15 C16 1.376(8) . ? C16 C17 1.476(9) . ? C17 N22 1.349(8) . ? C17 C18 1.386(9) . ? C18 C19 1.374(10) . ? C19 C20 1.352(10) . ? C20 C21 1.382(9) . ? C21 N22 1.335(7) . ? N31 C32 1.329(7) . ? N31 C36 1.341(8) . ? C32 C33 1.367(9) . ? C33 C34 1.366(9) . ? C34 C35 1.397(9) . ? C35 C36 1.381(8) . ? C36 C37 1.498(8) . ? C37 N42 1.346(8) . ? C37 C38 1.375(8) . ? C38 C39 1.392(9) . ? C39 C40 1.361(9) . ? C40 C41 1.395(8) . ? C41 N42 1.330(7) . ? N51 C56 1.341(8) . ? N51 C52 1.343(7) . ? C52 C53 1.387(8) . ? C53 C54 1.375(9) . ? C54 C55 1.380(9) . ? C55 C56 1.392(8) . ? C56 C57 1.473(8) . ? C57 N62 1.348(8) . ? C57 C58 1.372(8) . ? C58 C59 1.385(9) . ? C59 C60 1.369(9) . ? C60 C61 1.366(9) . ? C61 N62 1.325(7) . ? N71 C72 1.348(7) . ? N71 C76 1.358(8) . ? C72 C73 1.369(9) . ? C73 C74 1.376(9) . ? C74 C75 1.390(9) . ? C75 C76 1.374(9) . ? C76 C77 1.483(9) . ? C77 N82 1.361(8) . ? C77 C78 1.391(8) . ? C78 C79 1.381(9) . ? C79 C80 1.360(9) . ? C80 C81 1.378(8) . ? C81 N82 1.318(7) . ? N91 C911 1.339(7) . ? N91 S92 1.585(5) . ? S92 O93 1.453(4) . ? S92 O94 1.454(4) . ? S92 C95 1.779(7) . ? C95 C96 1.388(9) . ? C95 C100 1.395(8) . ? C96 C97 1.365(9) . ? C97 C98 1.412(9) . ? C98 C99 1.367(9) . ? C98 C101 1.502(9) . ? C99 C100 1.404(9) . ? C911 O912 1.206(7) . ? C911 O913 1.353(8) . ? O913 C914 1.439(7) . ? N111 C131 1.381(7) . ? N111 S112 1.585(6) . ? S112 O113 1.447(4) . ? S112 O114 1.448(4) . ? S112 C115 1.773(7) . ? C115 C120 1.367(9) . ? C115 C116 1.393(8) . ? C116 C117 1.376(8) . ? C117 C118 1.373(9) . ? C118 C119 1.413(10) . ? C118 C121 1.506(10) . ? C119 C120 1.373(9) . ? C131 O132 1.241(7) . ? C131 O133 1.321(7) . ? O133 C134 1.413(7) . ? Cl1 O14 1.423(5) . ? Cl1 O12 1.425(5) . ? Cl1 O13 1.431(5) . ? Cl1 O11 1.434(5) . ? Cl2 O23 1.429(5) . ? Cl2 O21 1.430(5) . ? Cl2 O24 1.448(5) . ? Cl2 O22 1.453(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu2 O2 81.83(16) . . ? O1 Cu2 N31 94.82(19) . . ? O2 Cu2 N31 153.65(18) . . ? O1 Cu2 N42 168.87(19) . . ? O2 Cu2 N42 97.06(18) . . ? N31 Cu2 N42 81.2(2) . . ? O1 Cu2 N91 98.80(17) . . ? O2 Cu2 N91 95.27(17) . . ? N31 Cu2 N91 111.05(18) . . ? N42 Cu2 N91 92.33(19) . . ? O1 Cu2 Cu4 40.66(12) . . ? O2 Cu2 Cu4 42.33(10) . . ? N31 Cu2 Cu4 133.80(15) . . ? N42 Cu2 Cu4 139.39(15) . . ? N91 Cu2 Cu4 91.75(12) . . ? O1 Cu4 O2 82.14(16) . . ? O1 Cu4 N71 163.14(18) . . ? O2 Cu4 N71 98.85(19) . . ? O1 Cu4 N82 96.72(19) . . ? O2 Cu4 N82 177.53(17) . . ? N71 Cu4 N82 81.6(2) . . ? O1 Cu4 O3 98.11(16) . . ? O2 Cu4 O3 81.85(14) . . ? N71 Cu4 O3 98.69(17) . . ? N82 Cu4 O3 100.49(17) . . ? O1 Cu4 Cu2 40.87(11) . . ? O2 Cu4 Cu2 42.43(11) . . ? N71 Cu4 Cu2 134.42(15) . . ? N82 Cu4 Cu2 135.99(15) . . ? O3 Cu4 Cu2 97.63(10) . . ? O4 Cu1 O3 82.11(16) . . ? O4 Cu1 N11 167.94(18) . . ? O3 Cu1 N11 95.46(18) . . ? O4 Cu1 N22 95.40(19) . . ? O3 Cu1 N22 151.20(18) . . ? N11 Cu1 N22 81.0(2) . . ? O4 Cu1 N111 98.95(17) . . ? O3 Cu1 N111 96.54(17) . . ? N11 Cu1 N111 93.06(19) . . ? N22 Cu1 N111 112.15(18) . . ? O4 Cu1 Cu3 41.20(12) . . ? O3 Cu1 Cu3 42.42(11) . . ? N11 Cu1 Cu3 137.87(15) . . ? N22 Cu1 Cu3 134.62(15) . . ? N111 Cu1 Cu3 91.60(13) . . ? O4 Cu3 O3 81.79(17) . . ? O4 Cu3 N51 98.78(19) . . ? O3 Cu3 N51 176.38(18) . . ? O4 Cu3 N62 163.28(18) . . ? O3 Cu3 N62 97.28(18) . . ? N51 Cu3 N62 81.1(2) . . ? O4 Cu3 O2 97.48(16) . . ? O3 Cu3 O2 81.71(14) . . ? N51 Cu3 O2 101.72(16) . . ? N62 Cu3 O2 98.90(17) . . ? O4 Cu3 Cu1 40.44(12) . . ? O3 Cu3 Cu1 42.84(11) . . ? N51 Cu3 Cu1 136.82(14) . . ? N62 Cu3 Cu1 132.78(14) . . ? O2 Cu3 Cu1 98.19(10) . . ? Cu4 O1 Cu2 98.47(18) . . ? Cu4 O2 Cu2 95.24(15) . . ? Cu4 O2 Cu3 97.92(15) . . ? Cu2 O2 Cu3 109.26(18) . . ? Cu3 O3 Cu1 94.74(16) . . ? Cu3 O3 Cu4 98.51(15) . . ? Cu1 O3 Cu4 111.06(18) . . ? Cu1 O4 Cu3 98.36(18) . . ? C12 N11 C16 118.5(6) . . ? C12 N11 Cu1 126.1(4) . . ? C16 N11 Cu1 115.3(4) . . ? N11 C12 C13 122.6(7) . . ? C14 C13 C12 118.3(7) . . ? C13 C14 C15 119.7(7) . . ? C14 C15 C16 119.9(7) . . ? N11 C16 C15 120.9(6) . . ? N11 C16 C17 114.2(6) . . ? C15 C16 C17 124.9(6) . . ? N22 C17 C18 119.8(6) . . ? N22 C17 C16 115.3(6) . . ? C18 C17 C16 124.9(6) . . ? C19 C18 C17 119.1(7) . . ? C20 C19 C18 120.5(7) . . ? C19 C20 C21 119.0(7) . . ? N22 C21 C20 120.9(7) . . ? C21 N22 C17 120.7(6) . . ? C21 N22 Cu1 125.1(5) . . ? C17 N22 Cu1 114.1(4) . . ? C32 N31 C36 118.7(6) . . ? C32 N31 Cu2 126.1(5) . . ? C36 N31 Cu2 115.2(4) . . ? N31 C32 C33 122.7(6) . . ? C34 C33 C32 119.4(6) . . ? C33 C34 C35 118.9(7) . . ? C36 C35 C34 118.3(6) . . ? N31 C36 C35 122.0(6) . . ? N31 C36 C37 114.5(6) . . ? C35 C36 C37 123.4(6) . . ? N42 C37 C38 121.8(6) . . ? N42 C37 C36 114.0(6) . . ? C38 C37 C36 124.2(6) . . ? C37 C38 C39 118.5(6) . . ? C40 C39 C38 119.7(6) . . ? C39 C40 C41 118.8(6) . . ? N42 C41 C40 121.7(6) . . ? C41 N42 C37 119.4(6) . . ? C41 N42 Cu2 125.5(5) . . ? C37 N42 Cu2 115.0(4) . . ? C56 N51 C52 118.8(6) . . ? C56 N51 Cu3 115.7(4) . . ? C52 N51 Cu3 125.6(5) . . ? N51 C52 C53 122.8(7) . . ? C54 C53 C52 118.1(6) . . ? C53 C54 C55 119.9(6) . . ? C54 C55 C56 118.9(6) . . ? N51 C56 C55 121.6(6) . . ? N51 C56 C57 114.7(5) . . ? C55 C56 C57 123.7(6) . . ? N62 C57 C58 121.8(6) . . ? N62 C57 C56 114.7(6) . . ? C58 C57 C56 123.4(6) . . ? C57 C58 C59 118.0(6) . . ? C60 C59 C58 120.3(7) . . ? C61 C60 C59 118.0(6) . . ? N62 C61 C60 123.2(6) . . ? C61 N62 C57 118.7(6) . . ? C61 N62 Cu3 127.3(5) . . ? C57 N62 Cu3 113.7(4) . . ? C72 N71 C76 117.4(6) . . ? C72 N71 Cu4 127.6(5) . . ? C76 N71 Cu4 114.8(4) . . ? N71 C72 C73 123.2(7) . . ? C72 C73 C74 118.9(7) . . ? C73 C74 C75 119.1(7) . . ? C76 C75 C74 118.9(7) . . ? N71 C76 C75 122.4(6) . . ? N71 C76 C77 114.4(6) . . ? C75 C76 C77 123.2(6) . . ? N82 C77 C78 119.6(6) . . ? N82 C77 C76 115.1(6) . . ? C78 C77 C76 125.3(6) . . ? C79 C78 C77 119.4(6) . . ? C80 C79 C78 118.7(6) . . ? C79 C80 C81 120.9(6) . . ? N82 C81 C80 120.3(6) . . ? C81 N82 C77 121.1(6) . . ? C81 N82 Cu4 124.9(5) . . ? C77 N82 Cu4 114.0(4) . . ? C911 N91 S92 116.8(5) . . ? C911 N91 Cu2 116.6(4) . . ? S92 N91 Cu2 124.9(3) . . ? O93 S92 O94 113.3(3) . . ? O93 S92 N91 114.3(3) . . ? O94 S92 N91 108.0(3) . . ? O93 S92 C95 107.0(3) . . ? O94 S92 C95 105.5(3) . . ? N91 S92 C95 108.2(3) . . ? C96 C95 C100 119.9(6) . . ? C96 C95 S92 117.7(5) . . ? C100 C95 S92 122.4(6) . . ? C97 C96 C95 120.6(6) . . ? C96 C97 C98 120.2(7) . . ? C99 C98 C97 119.5(7) . . ? C99 C98 C101 119.9(7) . . ? C97 C98 C101 120.6(7) . . ? C98 C99 C100 120.7(6) . . ? C95 C100 C99 119.1(7) . . ? O912 C911 N91 130.0(7) . . ? O912 C911 O913 121.6(6) . . ? N91 C911 O913 108.3(5) . . ? C911 O913 C914 116.1(5) . . ? C131 N111 S112 119.0(4) . . ? C131 N111 Cu1 114.1(4) . . ? S112 N111 Cu1 125.4(3) . . ? O113 S112 O114 114.4(3) . . ? O113 S112 N111 106.3(3) . . ? O114 S112 N111 113.6(3) . . ? O113 S112 C115 106.3(3) . . ? O114 S112 C115 107.0(3) . . ? N111 S112 C115 109.0(3) . . ? C120 C115 C116 119.5(6) . . ? C120 C115 S112 117.9(5) . . ? C116 C115 S112 122.7(5) . . ? C117 C116 C115 119.6(6) . . ? C118 C117 C116 122.1(6) . . ? C117 C118 C119 117.3(6) . . ? C117 C118 C121 123.0(7) . . ? C119 C118 C121 119.7(7) . . ? C120 C119 C118 120.8(7) . . ? C115 C120 C119 120.7(7) . . ? O132 C131 O133 122.1(6) . . ? O132 C131 N111 126.8(6) . . ? O133 C131 N111 111.1(5) . . ? C131 O133 C134 114.9(5) . . ? O14 Cl1 O12 111.2(3) . . ? O14 Cl1 O13 110.1(3) . . ? O12 Cl1 O13 108.9(3) . . ? O14 Cl1 O11 109.4(4) . . ? O12 Cl1 O11 108.4(4) . . ? O13 Cl1 O11 108.9(4) . . ? O23 Cl2 O21 110.9(3) . . ? O23 Cl2 O24 108.7(3) . . ? O21 Cl2 O24 110.3(3) . . ? O23 Cl2 O22 108.9(3) . . ? O21 Cl2 O22 109.2(3) . . ? O24 Cl2 O22 108.8(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.372 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.150 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END data_Complex3 #TrackingRef '- C1DT11622C_ccdc_795631_815020_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 815020' #TrackingRef 'complex1, 2 and 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H40 Cu N O3 P2 S2' _chemical_formula_weight 832.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 13.1335(11) _cell_length_b 13.5099(12) _cell_length_c 14.0175(13) _cell_angle_alpha 91.287(7) _cell_angle_beta 107.473(8) _cell_angle_gamma 116.536(9) _cell_volume 2086.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17347 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.96929 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffraction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17347 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0926 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8957 _reflns_number_gt 5493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystalis Oxford Diffraction' _computing_cell_refinement 'Crystalis Oxford Diffraction' _computing_data_reduction 'Crystalis Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 ; _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0472P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8957 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1274 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.27290(3) 0.17395(4) 0.24393(3) 0.03884(14) Uani 1 1 d . . . P1 P 0.16551(7) 0.10677(8) 0.34583(6) 0.0354(2) Uani 1 1 d . . . C11 C 0.0189(3) 0.1053(3) 0.3056(2) 0.0343(8) Uani 1 1 d . . . C12 C -0.0213(3) 0.1443(3) 0.3708(3) 0.0457(9) Uani 1 1 d . . . H12 H 0.0289 0.1763 0.4381 0.055 Uiso 1 1 calc R . . C13 C -0.1357(3) 0.1361(4) 0.3367(3) 0.0596(12) Uani 1 1 d . . . H13 H -0.1617 0.1634 0.3808 0.072 Uiso 1 1 calc R . . C14 C -0.2108(4) 0.0877(4) 0.2380(3) 0.0639(12) Uani 1 1 d . . . H14 H -0.2881 0.0812 0.2156 0.077 Uiso 1 1 calc R . . C15 C -0.1725(3) 0.0488(4) 0.1722(3) 0.0609(12) Uani 1 1 d . . . H15 H -0.2236 0.0159 0.1052 0.073 Uiso 1 1 calc R . . C16 C -0.0573(3) 0.0588(3) 0.2057(3) 0.0475(10) Uani 1 1 d . . . H16 H -0.0307 0.0339 0.1605 0.057 Uiso 1 1 calc R . . C21 C 0.1243(3) -0.0384(3) 0.3611(2) 0.0363(8) Uani 1 1 d . . . C22 C 0.2120(3) -0.0735(3) 0.3779(3) 0.0512(10) Uani 1 1 d . . . H22 H 0.2901 -0.0228 0.3813 0.061 Uiso 1 1 calc R . . C23 C 0.1845(4) -0.1827(4) 0.3897(3) 0.0626(12) Uani 1 1 d . . . H23 H 0.2444 -0.2047 0.4012 0.075 Uiso 1 1 calc R . . C24 C 0.0696(4) -0.2594(4) 0.3844(3) 0.0591(11) Uani 1 1 d . . . H24 H 0.0514 -0.3330 0.3919 0.071 Uiso 1 1 calc R . . C25 C -0.0174(4) -0.2264(3) 0.3679(3) 0.0537(10) Uani 1 1 d . . . H25 H -0.0954 -0.2780 0.3641 0.064 Uiso 1 1 calc R . . C26 C 0.0094(3) -0.1173(3) 0.3570(2) 0.0433(9) Uani 1 1 d . . . H26 H -0.0509 -0.0961 0.3467 0.052 Uiso 1 1 calc R . . C31 C 0.2408(3) 0.1857(3) 0.4760(2) 0.0353(8) Uani 1 1 d . . . C32 C 0.3063(3) 0.3019(3) 0.4907(3) 0.0512(10) Uani 1 1 d . . . H32 H 0.3093 0.3368 0.4344 0.061 Uiso 1 1 calc R . . C33 C 0.3670(3) 0.3669(4) 0.5870(3) 0.0607(11) Uani 1 1 d . . . H33 H 0.4094 0.4449 0.5955 0.073 Uiso 1 1 calc R . . C34 C 0.3643(3) 0.3156(4) 0.6698(3) 0.0610(12) Uani 1 1 d . . . H34 H 0.4063 0.3590 0.7349 0.073 Uiso 1 1 calc R . . C35 C 0.3002(3) 0.2009(4) 0.6581(3) 0.0538(11) Uani 1 1 d . . . H35 H 0.2982 0.1666 0.7148 0.065 Uiso 1 1 calc R . . C36 C 0.2384(3) 0.1361(3) 0.5610(2) 0.0451(9) Uani 1 1 d . . . H36 H 0.1946 0.0583 0.5531 0.054 Uiso 1 1 calc R . . P2 P 0.45200(8) 0.18710(8) 0.25187(6) 0.0377(2) Uani 1 1 d . . . C41 C 0.4862(3) 0.2187(3) 0.1357(2) 0.0390(8) Uani 1 1 d . . . C42 C 0.5120(3) 0.1523(3) 0.0804(3) 0.0546(10) Uani 1 1 d . . . H42 H 0.5165 0.0900 0.1037 0.066 Uiso 1 1 calc R . . C43 C 0.5312(4) 0.1788(4) -0.0100(3) 0.0697(13) Uani 1 1 d . . . H43 H 0.5479 0.1335 -0.0470 0.084 Uiso 1 1 calc R . . C44 C 0.5259(4) 0.2695(4) -0.0450(3) 0.0647(12) Uani 1 1 d . . . H44 H 0.5388 0.2864 -0.1057 0.078 Uiso 1 1 calc R . . C45 C 0.5017(4) 0.3360(4) 0.0091(3) 0.0690(12) Uani 1 1 d . . . H45 H 0.4986 0.3988 -0.0144 0.083 Uiso 1 1 calc R . . C46 C 0.4816(3) 0.3107(3) 0.0985(3) 0.0562(11) Uani 1 1 d . . . H46 H 0.4647 0.3566 0.1345 0.067 Uiso 1 1 calc R . . C51 C 0.4486(3) 0.0519(3) 0.2644(3) 0.0417(9) Uani 1 1 d . . . C52 C 0.5275(3) 0.0357(4) 0.3454(3) 0.0593(11) Uani 1 1 d . . . H52 H 0.5912 0.0971 0.3939 0.071 Uiso 1 1 calc R . . C53 C 0.5116(5) -0.0721(5) 0.3543(4) 0.0840(15) Uani 1 1 d . . . H53 H 0.5634 -0.0824 0.4102 0.101 Uiso 1 1 calc R . . C54 C 0.4215(5) -0.1625(4) 0.2825(4) 0.0794(15) Uani 1 1 d . . . H54 H 0.4140 -0.2338 0.2876 0.095 Uiso 1 1 calc R . . C55 C 0.3415(4) -0.1483(4) 0.2023(4) 0.0712(13) Uani 1 1 d . . . H55 H 0.2789 -0.2103 0.1537 0.085 Uiso 1 1 calc R . . C56 C 0.3538(4) -0.0425(3) 0.1937(3) 0.0562(11) Uani 1 1 d . . . H56 H 0.2981 -0.0339 0.1399 0.067 Uiso 1 1 calc R . . C61 C 0.5907(3) 0.2881(3) 0.3530(3) 0.0426(9) Uani 1 1 d . . . C62 C 0.5827(4) 0.3224(4) 0.4424(3) 0.0617(12) Uani 1 1 d . . . H62 H 0.5075 0.2924 0.4505 0.074 Uiso 1 1 calc R . . C63 C 0.6845(5) 0.4005(4) 0.5202(3) 0.0836(16) Uani 1 1 d . . . H63 H 0.6774 0.4224 0.5802 0.100 Uiso 1 1 calc R . . C64 C 0.7953(5) 0.4458(4) 0.5094(4) 0.0840(16) Uani 1 1 d . . . H64 H 0.8637 0.4999 0.5611 0.101 Uiso 1 1 calc R . . C65 C 0.8047(4) 0.4109(4) 0.4222(4) 0.0919(17) Uani 1 1 d . . . H65 H 0.8805 0.4401 0.4152 0.110 Uiso 1 1 calc R . . C66 C 0.7040(3) 0.3333(4) 0.3442(3) 0.0675(13) Uani 1 1 d . . . H66 H 0.7122 0.3110 0.2849 0.081 Uiso 1 1 calc R . . S71 S 0.15606(8) 0.10248(8) 0.05741(7) 0.0463(2) Uani 1 1 d . . . C72 C 0.1785(3) 0.2344(3) 0.0740(2) 0.0452(9) Uani 1 1 d . . . O721 O 0.1362(3) 0.2813(3) 0.00083(19) 0.0864(10) Uani 1 1 d . . . C722 C 0.0707(6) 0.2145(5) -0.1010(3) 0.152(3) Uani 1 1 d . . . H72A H 0.1257 0.2033 -0.1265 0.182 Uiso 1 1 calc R . . H72B H 0.0355 0.2531 -0.1447 0.182 Uiso 1 1 calc R . . H72C H 0.0076 0.1429 -0.0991 0.182 Uiso 1 1 calc R . . N73 N 0.2388(2) 0.2949(2) 0.16775(19) 0.0392(7) Uani 1 1 d . . . S74 S 0.28199(8) 0.42830(8) 0.19580(7) 0.0434(2) Uani 1 1 d . . . O75 O 0.3448(2) 0.4937(2) 0.1325(2) 0.0620(7) Uani 1 1 d . . . O76 O 0.3468(2) 0.4572(2) 0.30346(17) 0.0553(7) Uani 1 1 d . . . C77 C 0.1497(3) 0.4419(3) 0.1756(3) 0.0450(9) Uani 1 1 d . . . C78 C 0.0574(4) 0.3690(4) 0.2012(4) 0.0911(17) Uani 1 1 d . . . H78 H 0.0611 0.3079 0.2282 0.109 Uiso 1 1 calc R . . C79 C -0.0445(4) 0.3833(4) 0.1878(4) 0.0951(18) Uani 1 1 d . . . H79 H -0.1087 0.3298 0.2042 0.114 Uiso 1 1 calc R . . C80 C -0.0528(4) 0.4707(4) 0.1526(3) 0.0690(12) Uani 1 1 d . . . C81 C 0.0425(5) 0.5447(5) 0.1275(6) 0.137(3) Uani 1 1 d . . . H81 H 0.0403 0.6072 0.1026 0.164 Uiso 1 1 calc R . . C82 C 0.1429(4) 0.5296(4) 0.1380(5) 0.119(2) Uani 1 1 d . . . H82 H 0.2057 0.5808 0.1188 0.142 Uiso 1 1 calc R . . C83 C -0.1642(4) 0.4849(4) 0.1390(4) 0.0960(17) Uani 1 1 d . . . H83A H -0.2326 0.4128 0.1312 0.115 Uiso 1 1 calc R . . H83B H -0.1805 0.5170 0.0795 0.115 Uiso 1 1 calc R . . H83C H -0.1501 0.5338 0.1976 0.115 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 Cu1 0.0390(2) 0.0476(3) 0.0390(2) 0.0150(2) 0.02039(19) 0.0235(2) P1 0.0346(5) 0.0425(6) 0.0342(5) 0.0107(4) 0.0162(4) 0.0197(4) C11 0.0356(18) 0.037(2) 0.0363(18) 0.0118(16) 0.0172(15) 0.0187(16) C12 0.047(2) 0.060(3) 0.040(2) 0.0133(18) 0.0192(17) 0.030(2) C13 0.059(3) 0.083(3) 0.065(3) 0.022(2) 0.037(2) 0.047(3) C14 0.048(2) 0.088(4) 0.070(3) 0.025(3) 0.022(2) 0.043(3) C15 0.048(2) 0.079(3) 0.050(2) 0.007(2) 0.0084(19) 0.032(2) C16 0.042(2) 0.056(3) 0.045(2) 0.0044(19) 0.0156(17) 0.024(2) C21 0.0396(19) 0.043(2) 0.0297(17) 0.0078(16) 0.0157(15) 0.0202(17) C22 0.054(2) 0.058(3) 0.065(2) 0.030(2) 0.035(2) 0.036(2) C23 0.080(3) 0.075(3) 0.068(3) 0.031(2) 0.039(2) 0.055(3) C24 0.083(3) 0.044(3) 0.062(3) 0.020(2) 0.033(2) 0.035(3) C25 0.057(2) 0.048(3) 0.052(2) 0.016(2) 0.0221(19) 0.019(2) C26 0.046(2) 0.047(2) 0.044(2) 0.0124(18) 0.0218(17) 0.0235(19) C31 0.0308(17) 0.042(2) 0.0350(18) 0.0078(16) 0.0154(14) 0.0169(17) C32 0.049(2) 0.051(3) 0.045(2) 0.011(2) 0.0091(18) 0.021(2) C33 0.053(2) 0.043(3) 0.060(3) -0.003(2) 0.006(2) 0.011(2) C34 0.051(2) 0.072(3) 0.041(2) -0.007(2) -0.0005(18) 0.025(2) C35 0.052(2) 0.072(3) 0.033(2) 0.011(2) 0.0128(17) 0.027(2) C36 0.040(2) 0.053(3) 0.043(2) 0.0102(19) 0.0161(16) 0.0212(19) P2 0.0367(5) 0.0451(6) 0.0381(5) 0.0096(4) 0.0183(4) 0.0217(5) C41 0.0323(18) 0.045(2) 0.0407(19) 0.0105(17) 0.0176(15) 0.0158(17) C42 0.070(3) 0.054(3) 0.062(3) 0.020(2) 0.041(2) 0.036(2) C43 0.094(3) 0.062(3) 0.065(3) 0.010(2) 0.055(3) 0.030(3) C44 0.076(3) 0.069(3) 0.052(3) 0.017(2) 0.037(2) 0.027(3) C45 0.071(3) 0.076(3) 0.082(3) 0.046(3) 0.045(3) 0.041(3) C46 0.067(3) 0.057(3) 0.066(3) 0.023(2) 0.043(2) 0.033(2) C51 0.044(2) 0.050(2) 0.045(2) 0.0148(18) 0.0279(17) 0.0252(19) C52 0.055(2) 0.065(3) 0.069(3) 0.021(2) 0.020(2) 0.039(2) C53 0.096(4) 0.092(4) 0.101(4) 0.045(3) 0.044(3) 0.068(4) C54 0.111(4) 0.068(4) 0.110(4) 0.041(3) 0.067(4) 0.065(3) C55 0.089(3) 0.051(3) 0.092(4) 0.015(3) 0.051(3) 0.037(3) C56 0.064(3) 0.052(3) 0.063(3) 0.015(2) 0.030(2) 0.032(2) C61 0.045(2) 0.042(2) 0.044(2) 0.0073(17) 0.0155(17) 0.0242(18) C62 0.060(3) 0.078(3) 0.049(2) -0.001(2) 0.014(2) 0.038(2) C63 0.098(4) 0.105(4) 0.055(3) -0.017(3) 0.002(3) 0.071(4) C64 0.079(4) 0.064(3) 0.076(3) -0.015(3) -0.014(3) 0.034(3) C65 0.051(3) 0.091(4) 0.091(4) -0.003(3) 0.006(3) 0.010(3) C66 0.048(2) 0.077(3) 0.063(3) 0.003(2) 0.020(2) 0.018(2) S71 0.0526(6) 0.0361(6) 0.0395(5) -0.0011(4) 0.0107(4) 0.0159(5) C72 0.052(2) 0.042(2) 0.0346(19) 0.0079(17) 0.0106(17) 0.0199(19) O721 0.145(3) 0.057(2) 0.0351(15) 0.0049(14) -0.0053(16) 0.054(2) C722 0.263(8) 0.091(5) 0.042(3) -0.008(3) -0.036(4) 0.091(5) N73 0.0423(16) 0.0346(17) 0.0343(15) 0.0002(13) 0.0071(12) 0.0171(14) S74 0.0486(5) 0.0330(5) 0.0420(5) 0.0040(4) 0.0140(4) 0.0151(4) O75 0.0707(18) 0.0469(18) 0.0738(19) 0.0236(15) 0.0388(15) 0.0232(15) O76 0.0581(16) 0.0463(17) 0.0413(14) -0.0099(12) 0.0033(12) 0.0178(13) C77 0.054(2) 0.031(2) 0.048(2) 0.0073(18) 0.0166(18) 0.0202(19) C78 0.106(4) 0.082(4) 0.151(5) 0.084(4) 0.089(4) 0.067(3) C79 0.086(4) 0.085(4) 0.167(5) 0.074(4) 0.085(4) 0.056(3) C80 0.060(3) 0.060(3) 0.090(3) 0.021(3) 0.024(2) 0.032(3) C81 0.091(4) 0.085(4) 0.285(9) 0.105(5) 0.090(5) 0.065(4) C82 0.071(3) 0.059(3) 0.248(7) 0.075(4) 0.073(4) 0.035(3) C83 0.073(3) 0.097(4) 0.135(5) 0.039(4) 0.039(3) 0.053(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 Cu1 N73 2.111(3) . ? Cu1 P1 2.2310(9) . ? Cu1 P2 2.2464(9) . ? Cu1 S71 2.5053(10) . ? P1 C21 1.824(4) . ? P1 C31 1.826(3) . ? P1 C11 1.827(3) . ? C11 C12 1.381(4) . ? C11 C16 1.383(4) . ? C12 C13 1.384(4) . ? C13 C14 1.371(5) . ? C14 C15 1.368(5) . ? C15 C16 1.385(5) . ? C21 C26 1.388(4) . ? C21 C22 1.391(4) . ? C22 C23 1.380(5) . ? C23 C24 1.375(5) . ? C24 C25 1.363(5) . ? C25 C26 1.378(5) . ? C31 C36 1.382(4) . ? C31 C32 1.385(5) . ? C32 C33 1.380(5) . ? C33 C34 1.367(5) . ? C34 C35 1.370(6) . ? C35 C36 1.386(4) . ? P2 C51 1.820(4) . ? P2 C61 1.825(3) . ? P2 C41 1.826(3) . ? C41 C46 1.378(5) . ? C41 C42 1.385(5) . ? C42 C43 1.387(5) . ? C43 C44 1.353(6) . ? C44 C45 1.362(6) . ? C45 C46 1.376(5) . ? C51 C52 1.384(5) . ? C51 C56 1.394(5) . ? C52 C53 1.390(6) . ? C53 C54 1.358(6) . ? C54 C55 1.373(6) . ? C55 C56 1.377(5) . ? C61 C62 1.376(5) . ? C61 C66 1.379(5) . ? C62 C63 1.379(5) . ? C63 C64 1.362(6) . ? C64 C65 1.360(6) . ? C65 C66 1.373(5) . ? S71 C72 1.669(4) . ? C72 O721 1.329(4) . ? C72 N73 1.331(4) . ? O721 C722 1.450(5) . ? N73 S74 1.627(3) . ? S74 O76 1.435(2) . ? S74 O75 1.439(3) . ? S74 C77 1.768(4) . ? C77 C78 1.333(5) . ? C77 C82 1.336(6) . ? C78 C79 1.396(6) . ? C79 C80 1.326(6) . ? C80 C81 1.361(6) . ? C80 C83 1.515(6) . ? C81 C82 1.388(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 N73 Cu1 P1 113.32(8) . . ? N73 Cu1 P2 112.22(8) . . ? P1 Cu1 P2 129.97(4) . . ? N73 Cu1 S71 67.10(7) . . ? P1 Cu1 S71 115.38(4) . . ? P2 Cu1 S71 100.49(3) . . ? C21 P1 C31 103.97(15) . . ? C21 P1 C11 102.57(15) . . ? C31 P1 C11 103.71(14) . . ? C21 P1 Cu1 115.99(10) . . ? C31 P1 Cu1 114.18(11) . . ? C11 P1 Cu1 114.83(11) . . ? C12 C11 C16 118.6(3) . . ? C12 C11 P1 123.3(2) . . ? C16 C11 P1 118.1(2) . . ? C11 C12 C13 120.4(3) . . ? C14 C13 C12 120.2(3) . . ? C15 C14 C13 120.3(3) . . ? C14 C15 C16 119.6(4) . . ? C11 C16 C15 120.9(3) . . ? C26 C21 C22 117.4(3) . . ? C26 C21 P1 123.7(3) . . ? C22 C21 P1 119.0(3) . . ? C23 C22 C21 120.8(4) . . ? C24 C23 C22 120.6(4) . . ? C25 C24 C23 119.3(4) . . ? C24 C25 C26 120.5(4) . . ? C25 C26 C21 121.4(3) . . ? C36 C31 C32 118.0(3) . . ? C36 C31 P1 123.8(3) . . ? C32 C31 P1 118.2(3) . . ? C33 C32 C31 121.4(4) . . ? C34 C33 C32 119.4(4) . . ? C33 C34 C35 120.7(4) . . ? C34 C35 C36 119.6(4) . . ? C31 C36 C35 120.9(4) . . ? C51 P2 C61 104.55(16) . . ? C51 P2 C41 104.34(16) . . ? C61 P2 C41 103.75(16) . . ? C51 P2 Cu1 109.95(11) . . ? C61 P2 Cu1 119.78(12) . . ? C41 P2 Cu1 113.09(11) . . ? C46 C41 C42 117.9(3) . . ? C46 C41 P2 118.6(3) . . ? C42 C41 P2 123.4(3) . . ? C41 C42 C43 120.0(4) . . ? C44 C43 C42 120.9(4) . . ? C43 C44 C45 119.6(4) . . ? C44 C45 C46 120.3(4) . . ? C45 C46 C41 121.2(4) . . ? C52 C51 C56 118.0(4) . . ? C52 C51 P2 123.8(3) . . ? C56 C51 P2 117.9(3) . . ? C51 C52 C53 120.2(4) . . ? C54 C53 C52 120.8(4) . . ? C53 C54 C55 119.7(5) . . ? C54 C55 C56 120.2(5) . . ? C55 C56 C51 120.9(4) . . ? C62 C61 C66 117.8(3) . . ? C62 C61 P2 118.8(3) . . ? C66 C61 P2 123.3(3) . . ? C61 C62 C63 121.0(4) . . ? C64 C63 C62 120.3(4) . . ? C65 C64 C63 119.2(4) . . ? C64 C65 C66 121.0(5) . . ? C65 C66 C61 120.6(4) . . ? C72 S71 Cu1 76.40(12) . . ? O721 C72 N73 117.9(3) . . ? O721 C72 S71 124.4(3) . . ? N73 C72 S71 117.6(3) . . ? C72 O721 C722 117.3(3) . . ? C72 N73 S74 124.2(3) . . ? C72 N73 Cu1 98.9(2) . . ? S74 N73 Cu1 136.28(15) . . ? O76 S74 O75 117.10(16) . . ? O76 S74 N73 104.22(15) . . ? O75 S74 N73 112.73(15) . . ? O76 S74 C77 107.09(15) . . ? O75 S74 C77 107.97(17) . . ? N73 S74 C77 107.20(16) . . ? C78 C77 C82 118.5(4) . . ? C78 C77 S74 121.5(3) . . ? C82 C77 S74 119.9(3) . . ? C77 C78 C79 120.7(4) . . ? C80 C79 C78 122.2(4) . . ? C79 C80 C81 116.3(4) . . ? C79 C80 C83 121.3(4) . . ? C81 C80 C83 122.3(5) . . ? C80 C81 C82 122.0(5) . . ? C77 C82 C81 120.3(5) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.408 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.068 #===END