# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Bermejo, M. R.' 'Fondo, M.' 'Garcia-Deibe, A.' 'Piro, O.' 'Sousa, A.' 'Sousa-Pedrares, A.' _publ_contact_author ; Dr A Sousa Departamento de Quimica Inorganica Universidade de Santiago de Compostela Facultade de Quimica Santiago de Compostela 15706 SPAIN ; _publ_contact_author_email ' qiansoal@uscmail.usc.es ' _publ_section_title ; Structural characterisation of metal complexes containing 1-[(4-methylphenyl)sulfonamido(-2-([1-(2-pyridylmethylidene]amino(benzene Manuel R. Bermejo*, Antonio Sousa*, Matilde Fondo, Ana Garc=EDa-Deibe, Antonio Sousa-Pedrares, Oscar Piro ; data_CuL3(p-Tos)_1 _database_code_CSD 153998 _ audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H25 Cu N3 O6 S2' _chemical_formula_weight 603.15 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' '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' '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' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' #(No. 2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.949(3) _cell_length_b 11.071(4) _cell_length_c 14.162(2) _cell_angle_alpha 77.7390(3) _cell_angle_beta 78.8870(3) _cell_angle_gamma 75.0160(5) _cell_volume 1310.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.22 _cell_measurement_theta_max 17.26 _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 622 _exptl_absorpt_coefficient_mu 1.040 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 0 9 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 12 _diffrn_standards_decay_corr_max 1.231 _diffrn_standards_decay_corr_min 0.971 _diffrn_reflns_number 6694 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.97 _reflns_number_total 6293 _reflns_number_gt 3724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _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^)+(0.1051P)^2^+4.9112P] 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 6293 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1312 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.2295 _refine_ls_wR_factor_gt 0.1749 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Cu Cu 0.00203(8) 0.20177(7) 0.06125(5) 0.0336(2) Uani 1 1 d . . . N4 N -0.1650(6) 0.3083(5) -0.0163(3) 0.0350(10) Uani 1 1 d . . . N5 N -0.1360(5) 0.0850(5) 0.0856(3) 0.0319(10) Uani 1 1 d . . . N6 N 0.1424(6) 0.0499(5) 0.1309(3) 0.0341(10) Uani 1 1 d . . . O70 O -0.1103(6) 0.2873(4) 0.1966(3) 0.0483(11) Uani 1 1 d . . . O1W O 0.1508(6) 0.3084(5) 0.0116(4) 0.0585(14) Uani 1 1 d . . . S1 S 0.30773(17) 0.04287(15) 0.16234(10) 0.0365(3) Uani 1 1 d . . . O1 O 0.3467(5) 0.1650(5) 0.1224(3) 0.0474(11) Uani 1 1 d . . . O2 O 0.4261(6) -0.0656(5) 0.1373(3) 0.0519(12) Uani 1 1 d . . . C20 C -0.2854(6) 0.2525(6) -0.0070(4) 0.0341(12) Uani 1 1 d . . . C21 C -0.4171(8) 0.3118(7) -0.0511(5) 0.0474(16) Uani 1 1 d . . . H21 H -0.4992 0.2720 -0.0443 0.057 Uiso 1 1 calc R . . C22 C -0.4230(9) 0.4327(8) -0.1059(5) 0.0550(18) Uani 1 1 d . . . H22 H -0.5103 0.4760 -0.1356 0.066 Uiso 1 1 calc R . . C23 C -0.3004(8) 0.4864(7) -0.1153(5) 0.0492(16) Uani 1 1 d . . . H23 H -0.3029 0.5667 -0.1526 0.059 Uiso 1 1 calc R . . C24 C -0.1730(8) 0.4242(6) -0.0707(5) 0.0440(15) Uani 1 1 d . . . H24 H -0.0898 0.4629 -0.0782 0.053 Uiso 1 1 calc R . . C25 C -0.2612(7) 0.1242(6) 0.0506(4) 0.0387(13) Uani 1 1 d . . . H25 H -0.3346 0.0750 0.0605 0.046 Uiso 1 1 calc R . . C26 C -0.0818(7) -0.0334(5) 0.1414(4) 0.0320(12) Uani 1 1 d . . . C27 C -0.1665(8) -0.1285(6) 0.1714(5) 0.0432(14) Uani 1 1 d . . . H27 H -0.2651 -0.1153 0.1538 0.052 Uiso 1 1 calc R . . C28 C -0.1035(9) -0.2406(6) 0.2267(5) 0.0487(16) Uani 1 1 d . . . H28 H -0.1599 -0.3036 0.2476 0.058 Uiso 1 1 calc R . . C29 C 0.0432(9) -0.2603(7) 0.2514(5) 0.0517(17) Uani 1 1 d . . . H29 H 0.0856 -0.3373 0.2883 0.062 Uiso 1 1 calc R . . C30 C 0.1284(8) -0.1684(6) 0.2226(4) 0.0423(14) Uani 1 1 d . . . H30 H 0.2267 -0.1840 0.2412 0.051 Uiso 1 1 calc R . . C31 C 0.0704(7) -0.0521(5) 0.1658(4) 0.0324(12) Uani 1 1 d . . . C32 C 0.2800(7) 0.0287(6) 0.2908(4) 0.0388(13) Uani 1 1 d . . . C33 C 0.1589(9) 0.1092(7) 0.3361(5) 0.0511(17) Uani 1 1 d . . . H33 H 0.0899 0.1697 0.2992 0.061 Uiso 1 1 calc R . . C34 C 0.1377(9) 0.1018(8) 0.4365(5) 0.0549(18) Uani 1 1 d . . . H34 H 0.0552 0.1577 0.4666 0.066 Uiso 1 1 calc R . . C35 C 0.2381(10) 0.0120(8) 0.4916(5) 0.0554(18) Uani 1 1 d . . . C38 C 0.2165(12) 0.0043(10) 0.6012(5) 0.077(3) Uani 1 1 d . . . H38A H 0.2966 -0.0629 0.6281 0.116 Uiso 1 1 calc R . . H38B H 0.1158 -0.0125 0.6293 0.116 Uiso 1 1 calc R . . H38C H 0.2233 0.0833 0.6159 0.116 Uiso 1 1 calc R . . C36 C 0.3604(10) -0.0687(8) 0.4454(5) 0.065(2) Uani 1 1 d . . . H36 H 0.4303 -0.1288 0.4819 0.078 Uiso 1 1 calc R . . C37 C 0.3802(9) -0.0612(8) 0.3455(5) 0.0572(19) Uani 1 1 d . . . H37 H 0.4620 -0.1174 0.3151 0.069 Uiso 1 1 calc R . . S7 S -0.16323(18) 0.41284(14) 0.22249(11) 0.0367(3) Uani 1 1 d . . . O71 O -0.1941(6) 0.5104(5) 0.1374(3) 0.0541(13) Uani 1 1 d . . . O72 O -0.0654(6) 0.4400(5) 0.2807(4) 0.0538(12) Uani 1 1 d . . . C71 C -0.3483(8) 0.4147(6) 0.2937(4) 0.0416(14) Uani 1 1 d . . . C72 C -0.4262(9) 0.3208(7) 0.2970(6) 0.0565(18) Uani 1 1 d . . . H72 H -0.3791 0.2536 0.2636 0.068 Uiso 1 1 calc R . . C73 C -0.5723(10) 0.3269(9) 0.3491(7) 0.071(2) Uani 1 1 d . . . H73 H -0.6231 0.2626 0.3516 0.085 Uiso 1 1 calc R . . C74 C -0.6464(10) 0.4263(11) 0.3983(6) 0.073(3) Uani 1 1 d . . . C75 C -0.5699(12) 0.5208(11) 0.3928(7) 0.084(3) Uani 1 1 d . . . H75 H -0.6188 0.5897 0.4241 0.101 Uiso 1 1 calc R . . C76 C -0.4214(10) 0.5149(9) 0.3416(6) 0.068(2) Uani 1 1 d . . . H76 H -0.3704 0.5789 0.3395 0.081 Uiso 1 1 calc R . . C77 C -0.8092(11) 0.4332(13) 0.4565(8) 0.105(4) Uani 1 1 d . . . H77A H -0.8401 0.5077 0.4864 0.158 Uiso 1 1 calc R . . H77B H -0.8083 0.3591 0.5062 0.158 Uiso 1 1 calc R . . H77C H -0.8820 0.4371 0.4136 0.158 Uiso 1 1 calc R . . H1W H 0.2291 0.2886 0.0347 0.032(17) Uiso 1 1 d R . . H2W H 0.1824 0.3774 -0.0487 0.15(5) Uiso 1 1 d 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 Cu 0.0358(4) 0.0359(4) 0.0311(4) 0.0016(3) -0.0089(3) -0.0146(3) N4 0.035(3) 0.038(3) 0.033(2) -0.002(2) -0.009(2) -0.010(2) N5 0.033(2) 0.041(3) 0.026(2) -0.0062(19) -0.0012(18) -0.016(2) N6 0.037(3) 0.037(3) 0.029(2) 0.0018(19) -0.0030(19) -0.018(2) O70 0.058(3) 0.048(3) 0.037(2) -0.007(2) -0.001(2) -0.013(2) O1W 0.044(3) 0.063(3) 0.070(3) 0.028(3) -0.027(2) -0.033(2) S1 0.0328(7) 0.0453(8) 0.0312(7) 0.0020(6) -0.0077(6) -0.0134(6) O1 0.038(2) 0.057(3) 0.049(3) 0.011(2) -0.015(2) -0.025(2) O2 0.045(3) 0.064(3) 0.040(2) -0.009(2) -0.005(2) -0.003(2) C20 0.030(3) 0.046(3) 0.029(3) -0.011(2) -0.003(2) -0.009(2) C21 0.039(3) 0.065(4) 0.042(3) -0.012(3) -0.010(3) -0.011(3) C22 0.046(4) 0.065(5) 0.047(4) -0.006(3) -0.019(3) 0.005(3) C23 0.052(4) 0.047(4) 0.043(4) 0.000(3) -0.013(3) -0.004(3) C24 0.054(4) 0.041(3) 0.037(3) 0.003(3) -0.011(3) -0.015(3) C25 0.037(3) 0.052(4) 0.033(3) -0.011(3) 0.001(2) -0.022(3) C26 0.037(3) 0.032(3) 0.028(3) -0.007(2) 0.000(2) -0.012(2) C27 0.044(3) 0.045(4) 0.045(3) -0.016(3) 0.003(3) -0.019(3) C28 0.063(4) 0.040(4) 0.047(4) -0.010(3) 0.006(3) -0.026(3) C29 0.072(5) 0.036(3) 0.044(4) -0.005(3) 0.003(3) -0.015(3) C30 0.055(4) 0.039(3) 0.032(3) -0.003(3) -0.006(3) -0.012(3) C31 0.037(3) 0.029(3) 0.029(3) -0.004(2) 0.001(2) -0.007(2) C32 0.044(3) 0.041(3) 0.033(3) -0.001(2) -0.010(3) -0.012(3) C33 0.057(4) 0.056(4) 0.039(3) -0.003(3) -0.012(3) -0.012(3) C34 0.054(4) 0.064(5) 0.047(4) -0.018(3) -0.001(3) -0.011(4) C35 0.071(5) 0.067(5) 0.033(3) -0.005(3) -0.009(3) -0.026(4) C38 0.090(7) 0.106(8) 0.034(4) -0.014(4) -0.014(4) -0.014(6) C36 0.078(6) 0.076(6) 0.033(3) -0.005(3) -0.023(4) 0.005(4) C37 0.060(5) 0.062(5) 0.043(4) -0.008(3) -0.016(3) 0.003(4) S7 0.0398(8) 0.0371(8) 0.0317(7) 0.0009(6) -0.0057(6) -0.0113(6) O71 0.058(3) 0.055(3) 0.041(3) 0.018(2) -0.003(2) -0.022(2) O72 0.046(3) 0.059(3) 0.062(3) -0.014(2) -0.017(2) -0.011(2) C71 0.047(3) 0.051(4) 0.025(3) 0.004(2) -0.005(2) -0.016(3) C72 0.058(4) 0.051(4) 0.057(4) 0.001(3) -0.002(3) -0.020(3) C73 0.055(5) 0.077(6) 0.074(6) 0.014(5) -0.003(4) -0.029(4) C74 0.056(5) 0.114(8) 0.041(4) 0.014(5) -0.006(4) -0.028(5) C75 0.076(6) 0.105(8) 0.070(6) -0.045(6) 0.019(5) -0.014(6) C76 0.062(5) 0.081(6) 0.062(5) -0.034(4) 0.016(4) -0.020(4) C77 0.060(6) 0.160(12) 0.080(7) -0.005(7) 0.014(5) -0.026(7) _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 Cu O1W 1.939(4) . ? Cu N5 1.946(5) . ? Cu N4 2.000(5) . ? Cu N6 2.015(5) . ? Cu O70 2.263(5) . ? N4 C24 1.341(8) . ? N4 C20 1.347(7) . ? N5 C25 1.250(8) . ? N5 C26 1.400(7) . ? N6 C31 1.397(7) . ? N6 S1 1.604(5) . ? O70 S7 1.449(5) . ? O1W H1W 0.7908 . ? O1W H2W 1.0653 . ? S1 O2 1.438(5) . ? S1 O1 1.453(5) . ? S1 C32 1.767(6) . ? C20 C21 1.386(9) . ? C20 C25 1.465(9) . ? C21 C22 1.391(11) . ? C21 H21 0.9300 . ? C22 C23 1.350(11) . ? C22 H22 0.9300 . ? C23 C24 1.364(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.400(8) . ? C26 C31 1.421(8) . ? C27 C28 1.367(10) . ? C27 H27 0.9300 . ? C28 C29 1.375(11) . ? C28 H28 0.9300 . ? C29 C30 1.375(9) . ? C29 H29 0.9300 . ? C30 C31 1.396(8) . ? C30 H30 0.9300 . ? C32 C33 1.362(10) . ? C32 C37 1.368(9) . ? C33 C34 1.385(10) . ? C33 H33 0.9300 . ? C34 C35 1.373(11) . ? C34 H34 0.9300 . ? C35 C36 1.375(11) . ? C35 C38 1.513(10) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C36 C37 1.379(10) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? S7 O72 1.434(5) . ? S7 O71 1.455(5) . ? S7 C71 1.763(6) . ? C71 C76 1.376(10) . ? C71 C72 1.382(10) . ? C72 C73 1.365(11) . ? C72 H72 0.9300 . ? C73 C74 1.381(14) . ? C73 H73 0.9300 . ? C74 C75 1.373(14) . ? C74 C77 1.521(12) . ? C75 C76 1.378(12) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? 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 O1W Cu N5 168.6(2) . . ? O1W Cu N4 96.0(2) . . ? N5 Cu N4 80.9(2) . . ? O1W Cu N6 99.14(19) . . ? N5 Cu N6 82.2(2) . . ? N4 Cu N6 161.5(2) . . ? O1W Cu O70 97.6(2) . . ? N5 Cu O70 93.49(18) . . ? N4 Cu O70 93.01(19) . . ? N6 Cu O70 95.44(18) . . ? C24 N4 C20 118.7(5) . . ? C24 N4 Cu 129.1(4) . . ? C20 N4 Cu 112.2(4) . . ? C25 N5 C26 128.0(5) . . ? C25 N5 Cu 116.9(4) . . ? C26 N5 Cu 115.1(4) . . ? C31 N6 S1 119.2(4) . . ? C31 N6 Cu 112.4(4) . . ? S1 N6 Cu 127.6(3) . . ? S7 O70 Cu 137.3(3) . . ? Cu O1W H1W 116.6 . . ? Cu O1W H2W 142.7 . . ? H1W O1W H2W 98.9 . . ? O2 S1 O1 115.2(3) . . ? O2 S1 N6 113.1(3) . . ? O1 S1 N6 106.8(3) . . ? O2 S1 C32 107.2(3) . . ? O1 S1 C32 106.7(3) . . ? N6 S1 C32 107.5(3) . . ? N4 C20 C21 122.0(6) . . ? N4 C20 C25 114.0(5) . . ? C21 C20 C25 124.0(6) . . ? C20 C21 C22 118.0(6) . . ? C20 C21 H21 121.0 . . ? C22 C21 H21 121.0 . . ? C23 C22 C21 119.2(6) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 120.7(7) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? N4 C24 C23 121.5(6) . . ? N4 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? N5 C25 C20 115.9(5) . . ? N5 C25 H25 122.1 . . ? C20 C25 H25 122.1 . . ? N5 C26 C27 124.2(6) . . ? N5 C26 C31 114.5(5) . . ? C27 C26 C31 121.3(6) . . ? C28 C27 C26 119.6(6) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.0(6) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 121.3(7) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 121.2(7) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C30 C31 N6 128.0(6) . . ? C30 C31 C26 116.5(5) . . ? N6 C31 C26 115.5(5) . . ? C33 C32 C37 119.5(6) . . ? C33 C32 S1 119.8(5) . . ? C37 C32 S1 120.8(5) . . ? C32 C33 C34 120.6(7) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 120.2(7) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 118.9(6) . . ? C34 C35 C38 120.4(8) . . ? C36 C35 C38 120.7(7) . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C36 C37 120.6(7) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C32 C37 C36 120.2(7) . . ? C32 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? O72 S7 O70 113.7(3) . . ? O72 S7 O71 113.3(3) . . ? O70 S7 O71 111.6(3) . . ? O72 S7 C71 107.5(3) . . ? O70 S7 C71 105.3(3) . . ? O71 S7 C71 104.5(3) . . ? C76 C71 C72 119.1(7) . . ? C76 C71 S7 119.9(6) . . ? C72 C71 S7 120.8(6) . . ? C73 C72 C71 120.0(8) . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C72 C73 C74 121.5(9) . . ? C72 C73 H73 119.3 . . ? C74 C73 H73 119.3 . . ? C75 C74 C73 118.3(8) . . ? C75 C74 C77 120.2(11) . . ? C73 C74 C77 121.6(10) . . ? C74 C75 C76 120.8(9) . . ? C74 C75 H75 119.6 . . ? C76 C75 H75 119.6 . . ? C71 C76 C75 120.3(9) . . ? C71 C76 H76 119.8 . . ? C75 C76 H76 119.8 . . ? C74 C77 H77A 109.5 . . ? C74 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C74 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Cu N4 C24 -9.2(6) . . . . ? N5 Cu N4 C24 -178.1(6) . . . . ? N6 Cu N4 C24 -154.0(6) . . . . ? O70 Cu N4 C24 88.8(6) . . . . ? O1W Cu N4 C20 173.1(4) . . . . ? N5 Cu N4 C20 4.2(4) . . . . ? N6 Cu N4 C20 28.3(8) . . . . ? O70 Cu N4 C20 -88.8(4) . . . . ? O1W Cu N5 C25 -78.3(12) . . . . ? N4 Cu N5 C25 -3.3(4) . . . . ? N6 Cu N5 C25 -175.8(5) . . . . ? O70 Cu N5 C25 89.2(4) . . . . ? O1W Cu N5 C26 102.1(10) . . . . ? N4 Cu N5 C26 177.1(4) . . . . ? N6 Cu N5 C26 4.6(4) . . . . ? O70 Cu N5 C26 -90.4(4) . . . . ? O1W Cu N6 C31 -173.0(4) . . . . ? N5 Cu N6 C31 -4.4(4) . . . . ? N4 Cu N6 C31 -28.4(8) . . . . ? O70 Cu N6 C31 88.4(4) . . . . ? O1W Cu N6 S1 16.8(4) . . . . ? N5 Cu N6 S1 -174.7(4) . . . . ? N4 Cu N6 S1 161.3(5) . . . . ? O70 Cu N6 S1 -81.9(4) . . . . ? O1W Cu O70 S7 41.9(5) . . . . ? N5 Cu O70 S7 -135.6(5) . . . . ? N4 Cu O70 S7 -54.5(5) . . . . ? N6 Cu O70 S7 142.0(4) . . . . ? C31 N6 S1 O2 57.1(5) . . . . ? Cu N6 S1 O2 -133.2(3) . . . . ? C31 N6 S1 O1 -175.2(4) . . . . ? Cu N6 S1 O1 -5.5(4) . . . . ? C31 N6 S1 C32 -61.0(5) . . . . ? Cu N6 S1 C32 108.7(4) . . . . ? C24 N4 C20 C21 -0.7(9) . . . . ? Cu N4 C20 C21 177.2(5) . . . . ? C24 N4 C20 C25 177.6(5) . . . . ? Cu N4 C20 C25 -4.5(6) . . . . ? N4 C20 C21 C22 -0.3(9) . . . . ? C25 C20 C21 C22 -178.4(6) . . . . ? C20 C21 C22 C23 1.1(10) . . . . ? C21 C22 C23 C24 -0.9(11) . . . . ? C20 N4 C24 C23 0.9(9) . . . . ? Cu N4 C24 C23 -176.6(5) . . . . ? C22 C23 C24 N4 -0.1(11) . . . . ? C26 N5 C25 C20 -178.7(5) . . . . ? Cu N5 C25 C20 1.8(7) . . . . ? N4 C20 C25 N5 2.0(8) . . . . ? C21 C20 C25 N5 -179.8(6) . . . . ? C25 N5 C26 C27 -2.9(9) . . . . ? Cu N5 C26 C27 176.6(5) . . . . ? C25 N5 C26 C31 176.5(5) . . . . ? Cu N5 C26 C31 -4.0(6) . . . . ? N5 C26 C27 C28 -179.4(6) . . . . ? C31 C26 C27 C28 1.2(9) . . . . ? C26 C27 C28 C29 -0.9(10) . . . . ? C27 C28 C29 C30 0.8(10) . . . . ? C28 C29 C30 C31 -1.0(10) . . . . ? C29 C30 C31 N6 -179.9(6) . . . . ? C29 C30 C31 C26 1.2(9) . . . . ? S1 N6 C31 C30 -4.2(8) . . . . ? Cu N6 C31 C30 -175.4(5) . . . . ? S1 N6 C31 C26 174.7(4) . . . . ? Cu N6 C31 C26 3.5(6) . . . . ? N5 C26 C31 C30 179.2(5) . . . . ? C27 C26 C31 C30 -1.3(8) . . . . ? N5 C26 C31 N6 0.2(7) . . . . ? C27 C26 C31 N6 179.6(5) . . . . ? O2 S1 C32 C33 -170.8(5) . . . . ? O1 S1 C32 C33 65.3(6) . . . . ? N6 S1 C32 C33 -49.0(6) . . . . ? O2 S1 C32 C37 10.2(7) . . . . ? O1 S1 C32 C37 -113.7(6) . . . . ? N6 S1 C32 C37 132.0(6) . . . . ? C37 C32 C33 C34 0.8(11) . . . . ? S1 C32 C33 C34 -178.3(6) . . . . ? C32 C33 C34 C35 -0.6(12) . . . . ? C33 C34 C35 C36 0.8(12) . . . . ? C33 C34 C35 C38 179.4(8) . . . . ? C34 C35 C36 C37 -1.2(13) . . . . ? C38 C35 C36 C37 -179.8(8) . . . . ? C33 C32 C37 C36 -1.1(12) . . . . ? S1 C32 C37 C36 177.9(7) . . . . ? C35 C36 C37 C32 1.4(14) . . . . ? Cu O70 S7 O72 -107.7(5) . . . . ? Cu O70 S7 O71 21.9(5) . . . . ? Cu O70 S7 C71 134.8(4) . . . . ? O72 S7 C71 C76 49.2(7) . . . . ? O70 S7 C71 C76 170.8(6) . . . . ? O71 S7 C71 C76 -71.4(7) . . . . ? O72 S7 C71 C72 -135.1(6) . . . . ? O70 S7 C71 C72 -13.5(6) . . . . ? O71 S7 C71 C72 104.3(6) . . . . ? C76 C71 C72 C73 -1.4(11) . . . . ? S7 C71 C72 C73 -177.2(6) . . . . ? C71 C72 C73 C74 0.9(13) . . . . ? C72 C73 C74 C75 0.6(14) . . . . ? C72 C73 C74 C77 -179.9(9) . . . . ? C73 C74 C75 C76 -1.6(15) . . . . ? C77 C74 C75 C76 179.0(9) . . . . ? C72 C71 C76 C75 0.5(13) . . . . ? S7 C71 C76 C75 176.2(8) . . . . ? C74 C75 C76 C71 1.0(16) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.602 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.127 #END data_znL3(p-Tos)_2 _database_code_CSD 153999 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H25 N3 O6 S2 Zn' _chemical_formula_weight 604.98 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' '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' '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' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' #(No 2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.330(2) _cell_length_b 10.721(4) _cell_length_c 14.634(3) _cell_angle_alpha 101.6840(3) _cell_angle_beta 103.9560(3) _cell_angle_gamma 105.5400(5) _cell_volume 1311.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 4.43 _cell_measurement_theta_max 13.87 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orangish yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 7 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 9 _diffrn_standards_decay_corr_max 1.239 _diffrn_standards_decay_corr_min 1.000 _diffrn_reflns_number 4925 _diffrn_reflns_number 4925 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.1933 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4613 _reflns_number_gt 1874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep for Windows (Farrugia, 1997)' _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^)+(0.0359P)^2^+4.9259P] 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 4613 _refine_ls_number_parameters 364 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.2239 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1904 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.089 _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 Zn Zn 0.18098(14) 0.22002(12) 0.43049(9) 0.0382(4) Uani 1 1 d . . . N4 N 0.2988(9) 0.1160(7) 0.5218(6) 0.037(2) Uani 1 1 d . . . N5 N 0.4159(9) 0.2950(8) 0.4402(5) 0.039(2) Uani 1 1 d . . . N6 N 0.1803(8) 0.3757(7) 0.3667(5) 0.0306(18) Uani 1 1 d . . . O70 O 0.0163(8) 0.0629(6) 0.3231(5) 0.051(2) Uani 1 1 d . . . O1W O 0.0622(8) 0.2546(6) 0.5231(5) 0.0477(18) Uiso 1 1 d . . . H1W H -0.0285 0.2794 0.5188 0.100 Uiso 1 1 d . . . H2W H 0.0537 0.2246 0.5756 0.100 Uiso 1 1 d . . . S1 S 0.0451(3) 0.4380(3) 0.35052(17) 0.0356(6) Uani 1 1 d . . . O1 O -0.0715(7) 0.3633(7) 0.3846(5) 0.0454(18) Uani 1 1 d . . . O2 O 0.1008(8) 0.5823(6) 0.3902(5) 0.0457(18) Uani 1 1 d . . . S7 S 0.0117(4) -0.0693(3) 0.2710(2) 0.0493(8) Uani 1 1 d . A . O71 O 0.1576(11) -0.0699(11) 0.2589(6) 0.102(4) Uani 1 1 d . . . O72 O -0.066(4) -0.1694(9) 0.3134(7) 0.066(7) Uani 0.87(6) 1 d PU . . O72' O 0.024(15) -0.166(7) 0.313(5) 0.05(2) Uiso 0.13(6) 1 d PU . . C20 C 0.2395(12) 0.0212(11) 0.5604(8) 0.050(3) Uani 1 1 d . . . H20 H 0.1311 -0.0143 0.5439 0.060 Uiso 1 1 calc R . . C21 C 0.3305(14) -0.0292(11) 0.6248(8) 0.057(3) Uani 1 1 d . . . H21 H 0.2836 -0.0968 0.6499 0.068 Uiso 1 1 calc R . . C22 C 0.4900(13) 0.0237(11) 0.6499(8) 0.049(3) Uani 1 1 d . . . H22 H 0.5536 -0.0067 0.6932 0.059 Uiso 1 1 calc R . . C23 C 0.5551(11) 0.1219(9) 0.6108(7) 0.042(3) Uani 1 1 d . . . H23 H 0.6633 0.1597 0.6276 0.050 Uiso 1 1 calc R . . C24 C 0.4568(11) 0.1640(9) 0.5456(6) 0.032(2) Uani 1 1 d . . . C25 C 0.5152(12) 0.2632(10) 0.4971(7) 0.043(3) Uani 1 1 d . . . H25 H 0.6220 0.3016 0.5078 0.052 Uiso 1 1 calc R . . C26 C 0.4468(11) 0.3888(9) 0.3849(7) 0.033(2) Uani 1 1 d . . . C27 C 0.5925(11) 0.4336(10) 0.3707(7) 0.040(3) Uani 1 1 d . . . H27 H 0.6734 0.4033 0.3970 0.048 Uiso 1 1 calc R . . C28 C 0.6125(13) 0.5241(11) 0.3164(8) 0.055(3) Uani 1 1 d . . . H28 H 0.7091 0.5598 0.3078 0.066 Uiso 1 1 calc R . . C29 C 0.4870(12) 0.5609(10) 0.2752(7) 0.045(3) Uani 1 1 d . . . H29 H 0.4991 0.6164 0.2344 0.054 Uiso 1 1 calc R . . C30 C 0.3437(11) 0.5196(10) 0.2912(7) 0.043(3) Uani 1 1 d . . . H30 H 0.2640 0.5509 0.2646 0.052 Uiso 1 1 calc R . . C31 C 0.3207(11) 0.4307(9) 0.3475(6) 0.030(2) Uani 1 1 d . . . C32 C -0.0422(11) 0.4050(10) 0.2230(7) 0.035(2) Uani 1 1 d . . . C33 C -0.0868(14) 0.2763(12) 0.1641(8) 0.064(3) Uani 1 1 d . . . H33 H -0.0674 0.2087 0.1911 0.077 Uiso 1 1 calc R . . C34 C -0.1614(15) 0.2454(15) 0.0638(9) 0.081(4) Uani 1 1 d . . . H34 H -0.1953 0.1564 0.0249 0.097 Uiso 1 1 calc R . . C35 C -0.1855(14) 0.3434(16) 0.0216(9) 0.067(4) Uani 1 1 d . . . C36 C -0.1419(16) 0.4704(15) 0.0820(9) 0.075(4) Uani 1 1 d . . . H36 H -0.1605 0.5380 0.0548 0.090 Uiso 1 1 calc R . . C37 C -0.0705(13) 0.5035(11) 0.1830(8) 0.055(3) Uani 1 1 d . . . H37 H -0.0427 0.5914 0.2224 0.066 Uiso 1 1 calc R . . C38 C -0.2626(18) 0.3102(18) -0.0875(8) 0.115(6) Uani 1 1 d . . . H38A H -0.3589 0.3298 -0.0993 0.172 Uiso 1 1 calc R . . H38B H -0.2841 0.2161 -0.1176 0.172 Uiso 1 1 calc R . . H38C H -0.1940 0.3637 -0.1150 0.172 Uiso 1 1 calc R . . C71 C -0.1203(12) -0.1071(10) 0.1532(8) 0.042(3) Uani 1 1 d D . . C74 C -0.3256(18) -0.1582(14) -0.0335(9) 0.076(4) Uani 1 1 d D . . C77 C -0.439(2) -0.1864(17) -0.1353(9) 0.126(7) Uani 1 1 d . . . H77A H -0.5055 -0.2793 -0.1578 0.190 Uiso 1 1 calc R . . H77B H -0.3814 -0.1686 -0.1800 0.190 Uiso 1 1 calc R . . H77C H -0.5024 -0.1292 -0.1323 0.190 Uiso 1 1 calc R . . C72 C -0.265(3) -0.090(4) 0.1405(14) 0.076(9) Uani 0.68(5) 1 d PU A 2 H72 H -0.2941 -0.0625 0.1958 0.091 Uiso 0.68(5) 1 calc PR A 2 C73 C -0.367(3) -0.111(3) 0.0494(16) 0.090(9) Uani 0.71(4) 1 d PU A 2 H73 H -0.4612 -0.0941 0.0429 0.108 Uiso 0.71(4) 1 calc PR A 2 C72' C -0.269(6) -0.167(4) 0.137(4) 0.068(13) Uiso 0.32(5) 1 d PDU A 3 H72' H -0.3104 -0.1898 0.1855 0.082 Uiso 0.32(5) 1 calc PR A 3 C73' C -0.365(7) -0.193(6) 0.035(4) 0.085(15) Uiso 0.29(4) 1 d PDU A 3 H73' H -0.4704 -0.2439 0.0195 0.102 Uiso 0.29(4) 1 calc PR A 3 C75 C -0.203(4) -0.187(4) -0.0250(13) 0.074(9) Uani 0.62(4) 1 d PU A 4 H75 H -0.1812 -0.2235 -0.0813 0.088 Uiso 0.62(4) 1 calc PR A 4 C76 C -0.094(3) -0.167(4) 0.0709(18) 0.070(9) Uani 0.58(5) 1 d PU A 4 H76 H -0.0068 -0.1941 0.0757 0.084 Uiso 0.58(5) 1 calc PR A 4 C75' C -0.151(4) -0.101(5) -0.010(3) 0.055(11) Uiso 0.38(4) 1 d PDU A 5 H75' H -0.1065 -0.0779 -0.0569 0.066 Uiso 0.38(4) 1 calc PR A 5 C76' C -0.063(4) -0.084(4) 0.080(2) 0.047(9) Uiso 0.42(5) 1 d PDU A 5 H76' H 0.0451 -0.0533 0.0941 0.056 Uiso 0.42(5) 1 calc PR A 5 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 Zn 0.0318(7) 0.0396(8) 0.0408(7) 0.0144(6) 0.0060(6) 0.0106(6) N4 0.024(5) 0.028(5) 0.045(5) 0.008(4) -0.002(4) -0.001(4) N5 0.030(5) 0.055(6) 0.032(5) 0.008(4) 0.008(4) 0.022(4) N6 0.026(4) 0.039(5) 0.032(5) 0.015(4) 0.010(4) 0.013(4) O70 0.044(4) 0.037(4) 0.047(4) -0.004(3) -0.014(4) 0.011(3) S1 0.0359(15) 0.0417(17) 0.0301(14) 0.0120(12) 0.0072(12) 0.0162(13) O1 0.035(4) 0.073(5) 0.040(4) 0.028(4) 0.017(3) 0.023(4) O2 0.059(5) 0.035(4) 0.040(4) 0.002(3) 0.009(4) 0.024(4) S7 0.055(2) 0.0524(19) 0.0398(17) 0.0136(14) 0.0040(14) 0.0261(16) O71 0.080(7) 0.184(10) 0.058(6) 0.021(6) 0.011(5) 0.091(7) O72 0.100(17) 0.053(6) 0.046(6) 0.032(5) 0.022(6) 0.017(6) C20 0.034(6) 0.057(7) 0.064(8) 0.025(6) 0.016(6) 0.017(6) C21 0.060(8) 0.063(8) 0.058(8) 0.032(7) 0.021(7) 0.026(7) C22 0.048(7) 0.053(7) 0.050(7) 0.020(6) 0.003(6) 0.029(6) C23 0.030(6) 0.033(6) 0.051(7) 0.008(5) -0.001(5) 0.008(5) C24 0.037(6) 0.033(6) 0.024(5) 0.011(4) 0.004(4) 0.010(5) C25 0.034(6) 0.038(6) 0.053(7) 0.007(5) 0.005(5) 0.016(5) C26 0.039(6) 0.022(5) 0.035(6) 0.005(4) 0.010(5) 0.010(5) C27 0.029(6) 0.047(7) 0.041(6) 0.012(5) 0.010(5) 0.007(5) C28 0.041(7) 0.059(8) 0.071(8) 0.025(7) 0.030(6) 0.009(6) C29 0.043(7) 0.043(7) 0.048(7) 0.017(5) 0.013(6) 0.011(6) C30 0.030(6) 0.053(7) 0.045(6) 0.026(6) 0.007(5) 0.008(5) C31 0.039(6) 0.028(5) 0.017(5) 0.004(4) -0.001(4) 0.009(5) C32 0.036(6) 0.041(6) 0.032(6) 0.011(5) 0.007(5) 0.021(5) C33 0.075(9) 0.065(9) 0.047(8) 0.020(7) 0.000(7) 0.029(7) C34 0.073(10) 0.095(11) 0.051(8) 0.008(8) -0.009(7) 0.024(8) C35 0.058(8) 0.100(11) 0.038(7) 0.028(8) 0.004(6) 0.024(8) C36 0.089(11) 0.089(11) 0.053(9) 0.041(8) 0.011(8) 0.033(9) C37 0.071(8) 0.051(7) 0.049(7) 0.030(6) 0.009(6) 0.024(6) C38 0.106(13) 0.193(18) 0.032(8) 0.041(9) 0.002(8) 0.040(12) C71 0.039(7) 0.039(7) 0.047(7) 0.018(6) 0.009(5) 0.010(6) C74 0.079(11) 0.083(10) 0.041(8) 0.004(8) -0.007(7) 0.025(9) C77 0.142(16) 0.149(16) 0.045(9) 0.006(10) -0.016(9) 0.037(13) C72 0.079(14) 0.11(2) 0.038(11) 0.011(12) 0.014(10) 0.041(14) C73 0.079(14) 0.12(2) 0.055(13) 0.011(13) -0.006(11) 0.053(14) C75 0.114(19) 0.08(2) 0.014(10) -0.009(10) -0.010(11) 0.047(16) C76 0.068(15) 0.08(2) 0.077(16) 0.013(14) 0.020(12) 0.053(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 Zn O1W 1.985(7) . ? Zn O70 2.011(6) . ? Zn N6 2.072(7) . ? Zn N5 2.081(8) . ? Zn N4 2.188(8) . ? N4 C20 1.319(12) . ? N4 C24 1.354(11) . ? N5 C25 1.258(11) . ? N5 C26 1.427(11) . ? N6 C31 1.405(11) . ? N6 S1 1.570(7) . ? O70 S7 1.451(7) . ? O1W H1W 0.9446 . ? O1W H2W 0.9036 . ? S1 O1 1.426(7) . ? S1 O2 1.436(6) . ? S1 C32 1.765(9) . ? S7 O72' 1.32(7) . ? S7 O71 1.416(9) . ? S7 O72 1.459(16) . ? S7 C71 1.755(10) . ? C20 C21 1.403(13) . ? C20 H20 0.9300 . ? C21 C22 1.368(14) . ? C21 H21 0.9300 . ? C22 C23 1.369(14) . ? C22 H22 0.9300 . ? C23 C24 1.389(12) . ? C23 H23 0.9300 . ? C24 C25 1.454(13) . ? C25 H25 0.9300 . ? C26 C27 1.396(13) . ? C26 C31 1.400(12) . ? C27 C28 1.376(14) . ? C27 H27 0.9300 . ? C28 C29 1.376(14) . ? C28 H28 0.9300 . ? C29 C30 1.383(13) . ? C29 H29 0.9300 . ? C30 C31 1.388(12) . ? C30 H30 0.9300 . ? C32 C37 1.362(12) . ? C32 C33 1.363(14) . ? C33 C34 1.392(15) . ? C33 H33 0.9300 . ? C34 C35 1.364(17) . ? C34 H34 0.9300 . ? C35 C36 1.357(17) . ? C35 C38 1.507(15) . ? C36 C37 1.393(15) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C71 C72' 1.30(5) . ? C71 C76' 1.34(3) . ? C71 C76 1.35(2) . ? C71 C72 1.39(3) . ? C74 C73' 1.24(6) . ? C74 C75 1.25(2) . ? C74 C73 1.40(3) . ? C74 C75' 1.50(4) . ? C74 C77 1.523(17) . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C72 C73 1.37(3) . ? C72 H72 0.9300 . ? C73 H73 0.9300 . ? C72' C73' 1.47(7) . ? C72' H72' 0.9300 . ? C73' H73' 0.9300 . ? C75 C76 1.46(3) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C75' C76' 1.32(4) . ? C75' H75' 0.9300 . ? C76' H76' 0.9300 . ? 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 O1W Zn O70 100.6(3) . . ? O1W Zn N6 100.9(3) . . ? O70 Zn N6 100.9(3) . . ? O1W Zn N5 133.2(3) . . ? O70 Zn N5 125.6(3) . . ? N6 Zn N5 79.1(3) . . ? O1W Zn N4 90.8(3) . . ? O70 Zn N4 101.3(3) . . ? N6 Zn N4 152.5(3) . . ? N5 Zn N4 74.9(3) . . ? C20 N4 C24 116.8(8) . . ? C20 N4 Zn 129.7(7) . . ? C24 N4 Zn 113.3(6) . . ? C25 N5 C26 126.8(9) . . ? C25 N5 Zn 119.2(7) . . ? C26 N5 Zn 113.7(6) . . ? C31 N6 S1 122.1(6) . . ? C31 N6 Zn 113.4(5) . . ? S1 N6 Zn 124.3(4) . . ? S7 O70 Zn 134.3(4) . . ? Zn O1W H1W 134.1 . . ? Zn O1W H2W 131.3 . . ? H1W O1W H2W 91.6 . . ? O1 S1 O2 116.8(4) . . ? O1 S1 N6 106.3(4) . . ? O2 S1 N6 112.8(4) . . ? O1 S1 C32 106.1(4) . . ? O2 S1 C32 105.9(4) . . ? N6 S1 C32 108.5(4) . . ? O72' S7 O71 84(6) . . ? O72' S7 O70 124(3) . . ? O71 S7 O70 112.9(6) . . ? O72' S7 O72 34(5) . . ? O71 S7 O72 117.9(12) . . ? O70 S7 O72 108.8(8) . . ? O72' S7 C71 121(4) . . ? O71 S7 C71 107.0(5) . . ? O70 S7 C71 105.2(5) . . ? O72 S7 C71 104.0(8) . . ? N4 C20 C21 123.8(10) . . ? N4 C20 H20 118.1 . . ? C21 C20 H20 118.1 . . ? C22 C21 C20 118.2(11) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C21 C22 C23 119.4(9) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 118.8(9) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? N4 C24 C23 122.9(9) . . ? N4 C24 C25 114.4(8) . . ? C23 C24 C25 122.7(9) . . ? N5 C25 C24 117.4(9) . . ? N5 C25 H25 121.3 . . ? C24 C25 H25 121.3 . . ? C27 C26 C31 123.9(9) . . ? C27 C26 N5 121.5(8) . . ? C31 C26 N5 114.6(8) . . ? C28 C27 C26 117.8(9) . . ? C28 C27 H27 121.1 . . ? C26 C27 H27 121.1 . . ? C27 C28 C29 118.8(10) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C28 C29 C30 123.5(10) . . ? C28 C29 H29 118.2 . . ? C30 C29 H29 118.2 . . ? C29 C30 C31 119.0(9) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C30 C31 C26 116.8(9) . . ? C30 C31 N6 125.6(8) . . ? C26 C31 N6 117.6(8) . . ? C37 C32 C33 119.6(10) . . ? C37 C32 S1 121.7(8) . . ? C33 C32 S1 118.7(8) . . ? C32 C33 C34 120.3(11) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C35 C34 C33 121.1(13) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C34 117.4(12) . . ? C36 C35 C38 121.6(13) . . ? C34 C35 C38 120.9(14) . . ? C35 C36 C37 122.7(12) . . ? C35 C36 H36 118.6 . . ? C37 C36 H36 118.6 . . ? C32 C37 C36 118.9(11) . . ? C32 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C72' C71 C76' 122(3) . . ? C72' C71 C76 104(2) . . ? C76' C71 C76 35.9(12) . . ? C72' C71 C72 34.7(15) . . ? C76' C71 C72 111.6(17) . . ? C76 C71 C72 116.3(15) . . ? C72' C71 S7 119(2) . . ? C76' C71 S7 118.6(15) . . ? C76 C71 S7 122.4(12) . . ? C72 C71 S7 121.0(11) . . ? C73' C74 C75 101(3) . . ? C73' C74 C73 38.0(19) . . ? C75 C74 C73 120.8(16) . . ? C73' C74 C75' 113(3) . . ? C75 C74 C75' 35.8(14) . . ? C73 C74 C75' 108.9(19) . . ? C73' C74 C77 124(3) . . ? C75 C74 C77 119.7(16) . . ? C73 C74 C77 119.2(15) . . ? C75' C74 C77 123.0(18) . . ? C74 C77 H77A 109.5 . . ? C74 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C74 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C73 C72 C71 122(2) . . ? C73 C72 H72 118.8 . . ? C71 C72 H72 118.8 . . ? C72 C73 C74 118(2) . . ? C72 C73 H73 120.8 . . ? C74 C73 H73 120.8 . . ? C71 C72' C73' 113(5) . . ? C71 C72' H72' 123.3 . . ? C73' C72' H72' 123.3 . . ? C74 C73' C72' 129(6) . . ? C74 C73' H73' 115.5 . . ? C72' C73' H73' 115.5 . . ? C74 C75 C76 122(2) . . ? C74 C75 H75 119.2 . . ? C76 C75 H75 119.2 . . ? C71 C76 C75 119.7(19) . . ? C71 C76 H76 120.2 . . ? C75 C76 H76 120.2 . . ? C76' C75' C74 118(3) . . ? C76' C75' H75' 121.0 . . ? C74 C75' H75' 121.0 . . ? C75' C76' C71 124(3) . . ? C75' C76' H76' 118.1 . . ? C71 C76' H76' 118.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Zn N4 C20 48.1(9) . . . . ? O70 Zn N4 C20 -52.9(9) . . . . ? N6 Zn N4 C20 163.9(8) . . . . ? N5 Zn N4 C20 -177.0(9) . . . . ? O1W Zn N4 C24 -127.6(6) . . . . ? O70 Zn N4 C24 131.4(6) . . . . ? N6 Zn N4 C24 -11.8(10) . . . . ? N5 Zn N4 C24 7.3(6) . . . . ? O1W Zn N5 C25 69.1(9) . . . . ? O70 Zn N5 C25 -100.5(8) . . . . ? N6 Zn N5 C25 163.9(8) . . . . ? N4 Zn N5 C25 -7.3(7) . . . . ? O1W Zn N5 C26 -105.9(6) . . . . ? O70 Zn N5 C26 84.5(7) . . . . ? N6 Zn N5 C26 -11.1(6) . . . . ? N4 Zn N5 C26 177.7(6) . . . . ? O1W Zn N6 C31 142.9(6) . . . . ? O70 Zn N6 C31 -113.9(6) . . . . ? N5 Zn N6 C31 10.6(6) . . . . ? N4 Zn N6 C31 29.3(10) . . . . ? O1W Zn N6 S1 -31.2(5) . . . . ? O70 Zn N6 S1 72.0(5) . . . . ? N5 Zn N6 S1 -163.5(5) . . . . ? N4 Zn N6 S1 -144.8(5) . . . . ? O1W Zn O70 S7 -129.9(6) . . . . ? N6 Zn O70 S7 126.7(7) . . . . ? N5 Zn O70 S7 42.4(8) . . . . ? N4 Zn O70 S7 -36.9(7) . . . . ? C31 N6 S1 O1 -175.5(7) . . . . ? Zn N6 S1 O1 -1.9(6) . . . . ? C31 N6 S1 O2 -46.3(8) . . . . ? Zn N6 S1 O2 127.3(5) . . . . ? C31 N6 S1 C32 70.7(8) . . . . ? Zn N6 S1 C32 -115.7(5) . . . . ? Zn O70 S7 O72' 65(7) . . . . ? Zn O70 S7 O71 -32.9(8) . . . . ? Zn O70 S7 O72 99.8(12) . . . . ? Zn O70 S7 C71 -149.2(6) . . . . ? C24 N4 C20 C21 1.2(15) . . . . ? Zn N4 C20 C21 -174.4(8) . . . . ? N4 C20 C21 C22 0.6(17) . . . . ? C20 C21 C22 C23 -0.8(16) . . . . ? C21 C22 C23 C24 -0.7(15) . . . . ? C20 N4 C24 C23 -2.8(14) . . . . ? Zn N4 C24 C23 173.5(7) . . . . ? C20 N4 C24 C25 177.0(9) . . . . ? Zn N4 C24 C25 -6.7(10) . . . . ? C22 C23 C24 N4 2.6(15) . . . . ? C22 C23 C24 C25 -177.2(9) . . . . ? C26 N5 C25 C24 -179.6(8) . . . . ? Zn N5 C25 C24 6.1(12) . . . . ? N4 C24 C25 N5 0.8(13) . . . . ? C23 C24 C25 N5 -179.3(9) . . . . ? C25 N5 C26 C27 15.3(15) . . . . ? Zn N5 C26 C27 -170.1(7) . . . . ? C25 N5 C26 C31 -164.6(9) . . . . ? Zn N5 C26 C31 9.9(9) . . . . ? C31 C26 C27 C28 -0.1(15) . . . . ? N5 C26 C27 C28 180.0(9) . . . . ? C26 C27 C28 C29 -3.0(15) . . . . ? C27 C28 C29 C30 5.0(17) . . . . ? C28 C29 C30 C31 -3.5(16) . . . . ? C29 C30 C31 C26 0.2(14) . . . . ? C29 C30 C31 N6 -177.3(9) . . . . ? C27 C26 C31 C30 1.6(14) . . . . ? N5 C26 C31 C30 -178.5(8) . . . . ? C27 C26 C31 N6 179.2(8) . . . . ? N5 C26 C31 N6 -0.8(12) . . . . ? S1 N6 C31 C30 -17.0(13) . . . . ? Zn N6 C31 C30 168.8(8) . . . . ? S1 N6 C31 C26 165.6(6) . . . . ? Zn N6 C31 C26 -8.7(10) . . . . ? O1 S1 C32 C37 113.8(9) . . . . ? O2 S1 C32 C37 -11.0(10) . . . . ? N6 S1 C32 C37 -132.3(9) . . . . ? O1 S1 C32 C33 -64.0(10) . . . . ? O2 S1 C32 C33 171.2(9) . . . . ? N6 S1 C32 C33 49.9(10) . . . . ? C37 C32 C33 C34 -0.2(18) . . . . ? S1 C32 C33 C34 177.6(10) . . . . ? C32 C33 C34 C35 3(2) . . . . ? C33 C34 C35 C36 -4(2) . . . . ? C33 C34 C35 C38 178.5(13) . . . . ? C34 C35 C36 C37 2(2) . . . . ? C38 C35 C36 C37 180.0(12) . . . . ? C33 C32 C37 C36 -1.3(17) . . . . ? S1 C32 C37 C36 -179.0(9) . . . . ? C35 C36 C37 C32 0(2) . . . . ? O72' S7 C71 C72' 59(7) . . . . ? O71 S7 C71 C72' 152(2) . . . . ? O70 S7 C71 C72' -88(2) . . . . ? O72 S7 C71 C72' 26(2) . . . . ? O72' S7 C71 C76' -116(7) . . . . ? O71 S7 C71 C76' -23(2) . . . . ? O70 S7 C71 C76' 97(2) . . . . ? O72 S7 C71 C76' -148(2) . . . . ? O72' S7 C71 C76 -74(7) . . . . ? O71 S7 C71 C76 19(2) . . . . ? O70 S7 C71 C76 139(2) . . . . ? O72 S7 C71 C76 -107(2) . . . . ? O72' S7 C71 C72 99(7) . . . . ? O71 S7 C71 C72 -167.8(18) . . . . ? O70 S7 C71 C72 -47.5(18) . . . . ? O72 S7 C71 C72 67(2) . . . . ? C72' C71 C72 C73 -86(6) . . . . ? C76' C71 C72 C73 29(4) . . . . ? C76 C71 C72 C73 -10(4) . . . . ? S7 C71 C72 C73 176(2) . . . . ? C71 C72 C73 C74 3(4) . . . . ? C73' C74 C73 C72 69(6) . . . . ? C75 C74 C73 C72 4(4) . . . . ? C75' C74 C73 C72 -34(3) . . . . ? C77 C74 C73 C72 178(2) . . . . ? C76' C71 C72' C73' -5(2) . . . . ? C76 C71 C72' C73' -38.8(18) . . . . ? C72 C71 C72' C73' 78(4) . . . . ? S7 C71 C72' C73' -179.3(13) . . . . ? C75 C74 C73' C72' 46(4) . . . . ? C73 C74 C73' C72' -81(5) . . . . ? C75' C74 C73' C72' 11(4) . . . . ? C77 C74 C73' C72' -176.6(19) . . . . ? C71 C72' C73' C74 -6(3) . . . . ? C73' C74 C75 C76 -38(5) . . . . ? C73 C74 C75 C76 -4(5) . . . . ? C75' C74 C75 C76 76(4) . . . . ? C77 C74 C75 C76 -178(3) . . . . ? C72' C71 C76 C75 45(4) . . . . ? C76' C71 C76 C75 -81(4) . . . . ? C72 C71 C76 C75 10(4) . . . . ? S7 C71 C76 C75 -176(2) . . . . ? C74 C75 C76 C71 -4(5) . . . . ? C73' C74 C75' C76' -6(5) . . . . ? C75 C74 C75' C76' -82(4) . . . . ? C73 C74 C75' C76' 35(4) . . . . ? C77 C74 C75' C76' -178(3) . . . . ? C74 C75' C76' C71 -4(5) . . . . ? C72' C71 C76' C75' 9(5) . . . . ? C76 C71 C76' C75' 77(4) . . . . ? C72 C71 C76' C75' -28(4) . . . . ? S7 C71 C76' C75' -176(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.585 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.126 #END data_Co(L3)2_3 _database_code_CSD 154000 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 Co N6 O4 S2' _chemical_formula_weight 759.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)' #(No. 5) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.780(2) _cell_length_b 15.226(3) _cell_length_c 11.158(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.235(4) _cell_angle_gamma 90.00 _cell_volume 1782.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 976 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 21.78 _exptl_crystal_description 'plate' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.875909 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _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_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '117 first frames' _diffrn_standards_interval_count 'end of measurement' _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.26 _diffrn_reflns_number 9356 _diffrn_reflns_av_R_equivalents 0.1117 _diffrn_reflns_av_sigmaI/netI 0.3312 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.49 _reflns_number_total 5573 _reflns_number_gt 1930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _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^)+(0.0105P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(3) _refine_ls_number_reflns 5573 _refine_ls_number_parameters 460 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2280 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.843 _refine_ls_shift/su_max 0.012 _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 0.60380(12) 0.58068(9) 0.60495(13) 0.0341(4) Uani 1 1 d . . . N1 N 0.5950(8) 0.6516(6) 0.7754(9) 0.042(3) Uani 1 1 d . . . N2 N 0.6768(8) 0.7036(5) 0.5835(9) 0.032(2) Uani 1 1 d . . . N3 N 0.6148(6) 0.5777(6) 0.4201(6) 0.0288(19) Uani 1 1 d . . . N4 N 0.4027(8) 0.6205(7) 0.5574(8) 0.041(3) Uani 1 1 d . . . N5 N 0.5100(8) 0.4711(6) 0.6516(8) 0.035(3) Uani 1 1 d . . . N6 N 0.7569(7) 0.4998(5) 0.6892(8) 0.033(2) Uani 1 1 d . . . C1 C 0.5544(11) 0.6211(9) 0.8748(12) 0.065(4) Uani 1 1 d . . . H1 H 0.5331 0.5621 0.8781 0.077 Uiso 1 1 calc R . . C2 C 0.5447(15) 0.6741(10) 0.9672(14) 0.080(5) Uani 1 1 d . . . H2 H 0.5119 0.6529 1.0318 0.096 Uiso 1 1 calc R . . C3 C 0.5833(16) 0.7606(12) 0.9669(13) 0.097(6) Uani 1 1 d . . . H3 H 0.5815 0.7963 1.0341 0.116 Uiso 1 1 calc R . . C4 C 0.6257(13) 0.7957(9) 0.8657(15) 0.086(5) Uani 1 1 d . . . H4 H 0.6480 0.8545 0.8619 0.104 Uiso 1 1 calc R . . C5 C 0.6318(12) 0.7358(9) 0.7716(13) 0.053(4) Uani 1 1 d . . . C6 C 0.6765(12) 0.7636(8) 0.6630(12) 0.046(4) Uani 1 1 d . . . H6 H 0.7026 0.8208 0.6528 0.055 Uiso 1 1 calc R . . C7 C 0.7252(9) 0.7133(7) 0.4734(11) 0.033(3) Uani 1 1 d . . . C8 C 0.7996(10) 0.7829(8) 0.4546(12) 0.047(4) Uani 1 1 d . . . H8 H 0.8209 0.8264 0.5144 0.056 Uiso 1 1 calc R . . C9 C 0.8421(12) 0.7889(8) 0.3503(15) 0.055(4) Uani 1 1 d . . . H9 H 0.8932 0.8355 0.3375 0.067 Uiso 1 1 calc R . . C10 C 0.8076(12) 0.7235(8) 0.2630(12) 0.055(4) Uani 1 1 d . . . H10 H 0.8370 0.7274 0.1910 0.066 Uiso 1 1 calc R . . C11 C 0.7321(10) 0.6533(8) 0.2767(11) 0.050(4) Uani 1 1 d . . . H11 H 0.7093 0.6112 0.2152 0.059 Uiso 1 1 calc R . . C12 C 0.6907(10) 0.6472(7) 0.3870(11) 0.034(3) Uani 1 1 d . . . S1 S 0.5515(3) 0.50675(19) 0.3196(3) 0.0400(8) Uani 1 1 d . . . O1 O 0.4840(7) 0.4457(5) 0.3828(7) 0.054(2) Uani 1 1 d . . . O2 O 0.4789(6) 0.5484(4) 0.2066(6) 0.050(2) Uani 1 1 d . . . C13 C 0.6743(10) 0.4481(7) 0.2766(11) 0.030(3) Uani 1 1 d . . . C14 C 0.7826(13) 0.4253(8) 0.3623(13) 0.064(4) Uani 1 1 d . . . H14 H 0.7944 0.4434 0.4438 0.076 Uiso 1 1 calc R . . C15 C 0.8747(14) 0.3745(10) 0.3247(15) 0.076(5) Uani 1 1 d . . . H15 H 0.9470 0.3580 0.3833 0.092 Uiso 1 1 calc R . . C16 C 0.8632(14) 0.3476(8) 0.2041(14) 0.062(4) Uani 1 1 d . . . C17 C 0.7505(12) 0.3727(9) 0.1173(13) 0.064(4) Uani 1 1 d . . . H17 H 0.7379 0.3567 0.0350 0.077 Uiso 1 1 calc R . . C18 C 0.6606(11) 0.4213(8) 0.1581(11) 0.055(4) Uani 1 1 d . . . H18 H 0.5864 0.4366 0.1013 0.066 Uiso 1 1 calc R . . C19 C 0.9641(12) 0.2914(9) 0.1610(13) 0.109(6) Uani 1 1 d . . . H19A H 0.9361 0.2798 0.0744 0.164 Uiso 1 1 calc R . . H19B H 0.9754 0.2369 0.2054 0.164 Uiso 1 1 calc R . . H19C H 1.0436 0.3226 0.1764 0.164 Uiso 1 1 calc R . . C20 C 0.3531(11) 0.6985(8) 0.5155(12) 0.056(4) Uani 1 1 d . . . H20 H 0.4040 0.7437 0.4977 0.068 Uiso 1 1 calc R . . C21 C 0.2186(12) 0.7090(9) 0.4995(12) 0.063(4) Uani 1 1 d . . . H21 H 0.1800 0.7610 0.4666 0.076 Uiso 1 1 calc R . . C22 C 0.1492(12) 0.6462(11) 0.5305(13) 0.071(5) Uani 1 1 d . . . H22 H 0.0625 0.6558 0.5222 0.085 Uiso 1 1 calc R . . C23 C 0.1987(10) 0.5691(10) 0.5735(10) 0.058(4) Uani 1 1 d . . . H23 H 0.1481 0.5246 0.5940 0.070 Uiso 1 1 calc R . . C24 C 0.3248(11) 0.5584(9) 0.5859(11) 0.051(4) Uani 1 1 d . . . C25 C 0.3922(11) 0.4784(7) 0.6397(11) 0.047(4) Uani 1 1 d . . . H25 H 0.3467 0.4329 0.6651 0.056 Uiso 1 1 calc R . . C26 C 0.5882(11) 0.4001(7) 0.7043(11) 0.038(3) Uani 1 1 d . . . C27 C 0.5404(13) 0.3197(8) 0.7335(11) 0.058(4) Uani 1 1 d . . . H27 H 0.4530 0.3102 0.7192 0.069 Uiso 1 1 calc R . . C28 C 0.6243(13) 0.2551(9) 0.7834(11) 0.058(4) Uani 1 1 d . . . H28 H 0.5932 0.2014 0.8032 0.069 Uiso 1 1 calc R . . C29 C 0.7487(14) 0.2673(8) 0.8043(11) 0.055(4) Uani 1 1 d . . . H29 H 0.8029 0.2217 0.8383 0.066 Uiso 1 1 calc R . . C30 C 0.8017(11) 0.3469(7) 0.7766(10) 0.044(3) Uani 1 1 d . . . H30 H 0.8897 0.3534 0.7917 0.053 Uiso 1 1 calc R . . C31 C 0.7212(12) 0.4171(8) 0.7260(11) 0.038(3) Uani 1 1 d . . . S2 S 0.9036(3) 0.5234(2) 0.7069(3) 0.0409(9) Uani 1 1 d . . . O3 O 0.9731(6) 0.4578(4) 0.6538(7) 0.048(2) Uani 1 1 d . . . O4 O 0.9125(6) 0.6120(4) 0.6632(7) 0.046(2) Uani 1 1 d . . . C33 C 0.9067(11) 0.5470(8) 0.9496(12) 0.070(5) Uani 1 1 d . . . H33 H 0.8205 0.5602 0.9230 0.084 Uiso 1 1 calc R . . C34 C 0.9647(13) 0.5511(11) 1.0749(12) 0.088(6) Uani 1 1 d . . . H34 H 0.9183 0.5677 1.1319 0.106 Uiso 1 1 calc R . . C35 C 1.0904(14) 0.5303(8) 1.1120(13) 0.066(4) Uani 1 1 d . . . C36 C 1.1582(13) 0.5156(10) 1.0233(16) 0.099(6) Uani 1 1 d . . . H36 H 1.2464 0.5109 1.0478 0.118 Uiso 1 1 calc R . . C37 C 1.1030(15) 0.5076(12) 0.9033(14) 0.130(8) Uani 1 1 d . . . H37 H 1.1500 0.4914 0.8465 0.156 Uiso 1 1 calc R . . C32 C 0.9745(10) 0.5242(7) 0.8672(9) 0.036(3) Uani 1 1 d . . . C38 C 1.1488(12) 0.5295(9) 1.2512(11) 0.091(5) Uani 1 1 d . . . H38A H 1.2377 0.5151 1.2656 0.136 Uiso 1 1 calc R . . H38B H 1.1060 0.4865 1.2900 0.136 Uiso 1 1 calc R . . H38C H 1.1392 0.5865 1.2849 0.136 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0333(8) 0.0317(9) 0.0384(10) 0.0002(10) 0.0108(7) -0.0016(10) N1 0.040(6) 0.040(6) 0.042(7) -0.010(6) 0.001(5) 0.009(5) N2 0.029(6) 0.027(6) 0.034(7) 0.006(5) -0.002(5) 0.000(5) N3 0.037(5) 0.026(4) 0.024(5) -0.012(5) 0.008(4) -0.019(6) N4 0.029(6) 0.067(8) 0.027(6) 0.009(5) 0.007(5) -0.014(6) N5 0.034(6) 0.034(6) 0.041(7) 0.003(5) 0.017(5) -0.009(5) N6 0.019(5) 0.032(6) 0.053(7) 0.006(5) 0.017(5) 0.002(5) C1 0.084(10) 0.085(13) 0.026(9) -0.001(8) 0.016(8) 0.004(9) C2 0.132(15) 0.066(12) 0.049(12) 0.006(9) 0.032(11) 0.000(11) C3 0.137(17) 0.127(16) 0.023(10) -0.018(11) 0.011(11) 0.048(13) C4 0.106(13) 0.074(12) 0.065(12) -0.030(10) -0.011(11) 0.033(10) C5 0.048(9) 0.048(9) 0.056(10) -0.022(9) -0.004(8) 0.013(8) C6 0.053(9) 0.033(8) 0.050(10) -0.026(8) 0.011(8) -0.011(7) C7 0.020(6) 0.031(7) 0.047(9) 0.026(7) 0.007(6) 0.004(6) C8 0.038(8) 0.047(8) 0.050(10) -0.002(7) 0.001(7) -0.014(7) C9 0.043(9) 0.037(9) 0.087(13) 0.011(9) 0.017(9) -0.011(7) C10 0.064(10) 0.050(9) 0.057(10) 0.013(8) 0.026(9) -0.004(8) C11 0.043(8) 0.049(9) 0.059(10) 0.015(8) 0.017(8) -0.009(7) C12 0.026(7) 0.032(7) 0.041(8) 0.009(7) 0.004(6) 0.004(6) S1 0.0390(18) 0.040(2) 0.041(2) -0.0079(17) 0.0096(17) -0.0038(17) O1 0.058(5) 0.063(6) 0.049(6) -0.016(5) 0.028(5) -0.030(5) O2 0.047(5) 0.056(6) 0.039(5) -0.005(4) -0.009(4) 0.010(4) C13 0.038(7) 0.026(7) 0.032(8) -0.007(6) 0.019(6) 0.009(6) C14 0.079(11) 0.069(11) 0.046(10) 0.006(8) 0.019(9) 0.023(9) C15 0.065(11) 0.101(14) 0.062(13) 0.025(11) 0.013(10) 0.021(10) C16 0.082(11) 0.045(9) 0.065(11) -0.001(8) 0.032(10) 0.019(8) C17 0.051(9) 0.069(11) 0.068(12) -0.037(9) 0.004(9) -0.011(8) C18 0.041(8) 0.074(10) 0.047(10) -0.013(8) 0.005(7) 0.020(8) C19 0.098(13) 0.129(16) 0.103(15) -0.003(12) 0.029(12) 0.059(12) C20 0.045(9) 0.038(8) 0.084(12) 0.012(8) 0.010(8) -0.001(7) C21 0.047(9) 0.071(11) 0.071(11) 0.013(9) 0.014(9) 0.018(9) C22 0.028(8) 0.112(14) 0.077(12) 0.018(11) 0.022(9) 0.013(9) C23 0.032(7) 0.088(13) 0.057(9) 0.002(9) 0.016(6) -0.020(9) C24 0.034(7) 0.076(13) 0.044(9) 0.001(8) 0.008(7) 0.001(8) C25 0.041(8) 0.047(9) 0.062(10) 0.010(7) 0.032(7) -0.014(7) C26 0.042(8) 0.027(7) 0.046(9) -0.007(7) 0.010(7) -0.002(6) C27 0.078(10) 0.047(9) 0.047(10) 0.007(7) 0.015(8) -0.024(8) C28 0.079(11) 0.044(9) 0.045(9) 0.011(7) 0.002(9) -0.008(9) C29 0.088(12) 0.034(9) 0.043(9) 0.002(7) 0.015(9) 0.009(8) C30 0.042(8) 0.035(8) 0.055(10) 0.014(7) 0.011(7) 0.009(7) C31 0.050(9) 0.037(8) 0.027(8) -0.007(6) 0.012(7) -0.003(7) S2 0.0291(18) 0.047(2) 0.045(2) 0.0029(19) 0.0060(16) 0.0006(18) O3 0.046(5) 0.049(5) 0.055(6) -0.006(4) 0.022(5) 0.021(4) O4 0.034(5) 0.034(6) 0.070(6) 0.022(4) 0.012(4) -0.008(4) C33 0.049(8) 0.102(14) 0.051(10) -0.023(8) -0.006(8) 0.025(8) C34 0.072(10) 0.150(18) 0.044(10) -0.034(10) 0.016(8) 0.015(11) C35 0.067(9) 0.070(10) 0.051(10) -0.020(9) -0.011(9) 0.003(10) C36 0.072(11) 0.120(14) 0.107(15) -0.025(13) 0.027(12) 0.024(11) C37 0.111(14) 0.200(19) 0.057(12) -0.034(14) -0.025(11) 0.104(14) C32 0.047(7) 0.041(7) 0.018(7) 0.004(6) 0.004(6) 0.012(7) C38 0.100(11) 0.088(11) 0.072(12) -0.002(9) -0.003(10) -0.032(10) _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 N2 2.065(8) . ? Co1 N5 2.078(8) . ? Co1 N3 2.093(7) . ? Co1 N6 2.101(8) . ? Co1 N4 2.196(9) . ? Co1 N1 2.208(9) . ? N1 C5 1.346(14) . ? N1 C1 1.362(12) . ? N2 C6 1.275(12) . ? N2 C7 1.448(12) . ? N3 C12 1.437(12) . ? N3 S1 1.593(8) . ? N4 C24 1.350(12) . ? N4 C20 1.341(12) . ? N5 C25 1.251(12) . ? N5 C26 1.414(13) . ? N6 C31 1.406(13) . ? N6 S2 1.590(7) . ? C1 C2 1.333(15) . ? C2 C3 1.382(19) . ? C3 C4 1.416(18) . ? C4 C5 1.404(16) . ? C5 C6 1.466(16) . ? C7 C12 1.384(14) . ? C7 C8 1.374(13) . ? C8 C9 1.347(15) . ? C9 C10 1.383(15) . ? C10 C11 1.374(14) . ? C11 C12 1.405(13) . ? S1 O1 1.459(7) . ? S1 O2 1.468(7) . ? S1 C13 1.752(10) . ? C13 C18 1.360(13) . ? C13 C14 1.374(15) . ? C14 C15 1.396(16) . ? C15 C16 1.386(18) . ? C16 C17 1.421(17) . ? C16 C19 1.545(15) . ? C17 C18 1.376(14) . ? C20 C21 1.428(15) . ? C21 C22 1.308(15) . ? C22 C23 1.333(18) . ? C23 C24 1.345(13) . ? C24 C25 1.474(14) . ? C26 C27 1.395(13) . ? C26 C31 1.422(14) . ? C27 C28 1.365(15) . ? C28 C29 1.321(15) . ? C29 C30 1.404(14) . ? C30 C31 1.410(13) . ? S2 O4 1.445(7) . ? S2 O3 1.454(7) . ? S2 C32 1.776(10) . ? C33 C32 1.345(12) . ? C33 C34 1.396(15) . ? C34 C35 1.360(16) . ? C35 C36 1.377(16) . ? C35 C38 1.537(16) . ? C36 C37 1.341(17) . ? C37 C32 1.375(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N5 167.7(4) . . ? N2 Co1 N3 78.3(4) . . ? N5 Co1 N3 111.7(3) . . ? N2 Co1 N6 107.6(3) . . ? N5 Co1 N6 78.2(3) . . ? N3 Co1 N6 102.2(3) . . ? N2 Co1 N4 95.9(3) . . ? N5 Co1 N4 76.8(4) . . ? N3 Co1 N4 92.5(3) . . ? N6 Co1 N4 154.3(3) . . ? N2 Co1 N1 75.5(4) . . ? N5 Co1 N1 93.3(4) . . ? N3 Co1 N1 152.0(4) . . ? N6 Co1 N1 94.9(3) . . ? N4 Co1 N1 80.7(3) . . ? C5 N1 C1 120.1(11) . . ? C5 N1 Co1 111.5(9) . . ? C1 N1 Co1 128.3(8) . . ? C6 N2 C7 125.1(11) . . ? C6 N2 Co1 120.5(9) . . ? C7 N2 Co1 114.4(7) . . ? C12 N3 S1 119.7(7) . . ? C12 N3 Co1 113.6(7) . . ? S1 N3 Co1 126.6(5) . . ? C24 N4 C20 118.8(10) . . ? C24 N4 Co1 112.5(8) . . ? C20 N4 Co1 128.5(8) . . ? C25 N5 C26 127.3(10) . . ? C25 N5 Co1 116.3(8) . . ? C26 N5 Co1 116.1(7) . . ? C31 N6 S2 119.9(8) . . ? C31 N6 Co1 114.6(7) . . ? S2 N6 Co1 125.5(5) . . ? C2 C1 N1 121.4(13) . . ? C1 C2 C3 119.9(14) . . ? C2 C3 C4 120.9(14) . . ? C5 C4 C3 115.5(15) . . ? N1 C5 C4 122.1(14) . . ? N1 C5 C6 117.2(12) . . ? C4 C5 C6 120.7(14) . . ? N2 C6 C5 114.9(12) . . ? C12 C7 C8 121.9(12) . . ? C12 C7 N2 115.1(10) . . ? C8 C7 N2 123.0(12) . . ? C9 C8 C7 120.6(13) . . ? C8 C9 C10 118.1(12) . . ? C11 C10 C9 123.5(13) . . ? C10 C11 C12 117.6(12) . . ? C7 C12 C11 118.3(11) . . ? C7 C12 N3 115.8(10) . . ? C11 C12 N3 125.9(11) . . ? O1 S1 O2 117.7(4) . . ? O1 S1 N3 105.8(5) . . ? O2 S1 N3 111.7(5) . . ? O1 S1 C13 107.4(5) . . ? O2 S1 C13 105.8(5) . . ? N3 S1 C13 108.0(5) . . ? C18 C13 C14 119.1(11) . . ? C18 C13 S1 119.9(10) . . ? C14 C13 S1 120.9(10) . . ? C13 C14 C15 118.7(13) . . ? C16 C15 C14 123.0(14) . . ? C15 C16 C17 117.1(13) . . ? C15 C16 C19 123.6(14) . . ? C17 C16 C19 119.3(13) . . ? C18 C17 C16 118.4(13) . . ? C13 C18 C17 123.7(12) . . ? N4 C20 C21 117.1(11) . . ? C22 C21 C20 120.7(13) . . ? C21 C22 C23 122.2(13) . . ? C22 C23 C24 117.0(13) . . ? N4 C24 C23 124.1(13) . . ? N4 C24 C25 113.5(10) . . ? C23 C24 C25 122.3(13) . . ? N5 C25 C24 120.7(11) . . ? C27 C26 C31 122.1(12) . . ? C27 C26 N5 123.4(11) . . ? C31 C26 N5 114.5(10) . . ? C28 C27 C26 118.7(13) . . ? C29 C28 C27 121.5(13) . . ? C28 C29 C30 122.0(13) . . ? C29 C30 C31 119.9(11) . . ? N6 C31 C26 116.5(11) . . ? N6 C31 C30 127.7(11) . . ? C26 C31 C30 115.8(11) . . ? O4 S2 O3 115.0(5) . . ? O4 S2 N6 108.1(5) . . ? O3 S2 N6 112.6(5) . . ? O4 S2 C32 106.7(5) . . ? O3 S2 C32 105.8(5) . . ? N6 S2 C32 108.3(5) . . ? C32 C33 C34 120.5(12) . . ? C35 C34 C33 118.7(13) . . ? C34 C35 C36 118.4(14) . . ? C34 C35 C38 117.3(14) . . ? C36 C35 C38 124.3(14) . . ? C37 C36 C35 123.0(15) . . ? C36 C37 C32 117.6(15) . . ? C33 C32 C37 121.1(11) . . ? C33 C32 S2 120.9(9) . . ? C37 C32 S2 117.8(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Co1 N1 C5 4.2(8) . . . . ? N5 Co1 N1 C5 -170.5(8) . . . . ? N3 Co1 N1 C5 -16.8(12) . . . . ? N6 Co1 N1 C5 111.1(8) . . . . ? N4 Co1 N1 C5 -94.4(8) . . . . ? N2 Co1 N1 C1 -178.2(10) . . . . ? N5 Co1 N1 C1 7.1(10) . . . . ? N3 Co1 N1 C1 160.8(8) . . . . ? N6 Co1 N1 C1 -71.3(10) . . . . ? N4 Co1 N1 C1 83.2(10) . . . . ? N5 Co1 N2 C6 20(2) . . . . ? N3 Co1 N2 C6 164.9(9) . . . . ? N6 Co1 N2 C6 -95.8(9) . . . . ? N4 Co1 N2 C6 73.6(9) . . . . ? N1 Co1 N2 C6 -5.2(9) . . . . ? N5 Co1 N2 C7 -159.4(15) . . . . ? N3 Co1 N2 C7 -14.8(6) . . . . ? N6 Co1 N2 C7 84.5(7) . . . . ? N4 Co1 N2 C7 -106.1(7) . . . . ? N1 Co1 N2 C7 175.1(7) . . . . ? N2 Co1 N3 C12 14.0(6) . . . . ? N5 Co1 N3 C12 -173.7(6) . . . . ? N6 Co1 N3 C12 -91.7(7) . . . . ? N4 Co1 N3 C12 109.5(7) . . . . ? N1 Co1 N3 C12 34.7(10) . . . . ? N2 Co1 N3 S1 -167.5(6) . . . . ? N5 Co1 N3 S1 4.9(7) . . . . ? N6 Co1 N3 S1 86.9(6) . . . . ? N4 Co1 N3 S1 -71.9(6) . . . . ? N1 Co1 N3 S1 -146.7(6) . . . . ? N2 Co1 N4 C24 -167.4(8) . . . . ? N5 Co1 N4 C24 2.5(8) . . . . ? N3 Co1 N4 C24 114.2(8) . . . . ? N6 Co1 N4 C24 -11.2(12) . . . . ? N1 Co1 N4 C24 -93.1(8) . . . . ? N2 Co1 N4 C20 6.5(11) . . . . ? N5 Co1 N4 C20 176.4(11) . . . . ? N3 Co1 N4 C20 -71.9(11) . . . . ? N6 Co1 N4 C20 162.7(10) . . . . ? N1 Co1 N4 C20 80.8(11) . . . . ? N2 Co1 N5 C25 51(2) . . . . ? N3 Co1 N5 C25 -91.3(9) . . . . ? N6 Co1 N5 C25 170.1(9) . . . . ? N4 Co1 N5 C25 -3.9(9) . . . . ? N1 Co1 N5 C25 75.7(9) . . . . ? N2 Co1 N5 C26 -123.0(16) . . . . ? N3 Co1 N5 C26 94.6(8) . . . . ? N6 Co1 N5 C26 -4.0(7) . . . . ? N4 Co1 N5 C26 -177.9(8) . . . . ? N1 Co1 N5 C26 -98.3(8) . . . . ? N2 Co1 N6 C31 171.5(7) . . . . ? N5 Co1 N6 C31 2.9(7) . . . . ? N3 Co1 N6 C31 -107.1(8) . . . . ? N4 Co1 N6 C31 16.5(12) . . . . ? N1 Co1 N6 C31 95.2(8) . . . . ? N2 Co1 N6 S2 -11.6(7) . . . . ? N5 Co1 N6 S2 179.8(7) . . . . ? N3 Co1 N6 S2 69.8(6) . . . . ? N4 Co1 N6 S2 -166.6(6) . . . . ? N1 Co1 N6 S2 -87.9(6) . . . . ? C5 N1 C1 C2 3.1(19) . . . . ? Co1 N1 C1 C2 -174.3(10) . . . . ? N1 C1 C2 C3 -4(2) . . . . ? C1 C2 C3 C4 4(3) . . . . ? C2 C3 C4 C5 -3(2) . . . . ? C1 N1 C5 C4 -2.4(19) . . . . ? Co1 N1 C5 C4 175.4(10) . . . . ? C1 N1 C5 C6 178.9(11) . . . . ? Co1 N1 C5 C6 -3.3(14) . . . . ? C3 C4 C5 N1 3(2) . . . . ? C3 C4 C5 C6 -178.9(13) . . . . ? C7 N2 C6 C5 -175.3(10) . . . . ? Co1 N2 C6 C5 5.0(15) . . . . ? N1 C5 C6 N2 -0.8(17) . . . . ? C4 C5 C6 N2 -179.5(12) . . . . ? C6 N2 C7 C12 -166.1(11) . . . . ? Co1 N2 C7 C12 13.6(11) . . . . ? C6 N2 C7 C8 13.6(16) . . . . ? Co1 N2 C7 C8 -166.7(8) . . . . ? C12 C7 C8 C9 -0.2(17) . . . . ? N2 C7 C8 C9 -180.0(10) . . . . ? C7 C8 C9 C10 0.6(18) . . . . ? C8 C9 C10 C11 0.2(19) . . . . ? C9 C10 C11 C12 -1.4(18) . . . . ? C8 C7 C12 C11 -1.0(16) . . . . ? N2 C7 C12 C11 178.7(9) . . . . ? C8 C7 C12 N3 178.8(9) . . . . ? N2 C7 C12 N3 -1.4(13) . . . . ? C10 C11 C12 C7 1.8(16) . . . . ? C10 C11 C12 N3 -178.0(10) . . . . ? S1 N3 C12 C7 170.2(8) . . . . ? Co1 N3 C12 C7 -11.1(11) . . . . ? S1 N3 C12 C11 -10.0(14) . . . . ? Co1 N3 C12 C11 168.7(9) . . . . ? C12 N3 S1 O1 179.1(7) . . . . ? Co1 N3 S1 O1 0.6(7) . . . . ? C12 N3 S1 O2 -51.7(8) . . . . ? Co1 N3 S1 O2 129.8(5) . . . . ? C12 N3 S1 C13 64.3(9) . . . . ? Co1 N3 S1 C13 -114.2(6) . . . . ? O1 S1 C13 C18 102.2(10) . . . . ? O2 S1 C13 C18 -24.2(11) . . . . ? N3 S1 C13 C18 -144.0(9) . . . . ? O1 S1 C13 C14 -75.0(11) . . . . ? O2 S1 C13 C14 158.5(10) . . . . ? N3 S1 C13 C14 38.7(11) . . . . ? C18 C13 C14 C15 -0.6(19) . . . . ? S1 C13 C14 C15 176.6(10) . . . . ? C13 C14 C15 C16 2(2) . . . . ? C14 C15 C16 C17 -1(2) . . . . ? C14 C15 C16 C19 -180.0(13) . . . . ? C15 C16 C17 C18 0(2) . . . . ? C19 C16 C17 C18 178.7(12) . . . . ? C14 C13 C18 C17 -1(2) . . . . ? S1 C13 C18 C17 -178.0(10) . . . . ? C16 C17 C18 C13 1(2) . . . . ? C24 N4 C20 C21 -2.3(18) . . . . ? Co1 N4 C20 C21 -175.9(9) . . . . ? N4 C20 C21 C22 3(2) . . . . ? C20 C21 C22 C23 -3(2) . . . . ? C21 C22 C23 C24 1(2) . . . . ? C20 N4 C24 C23 0.9(18) . . . . ? Co1 N4 C24 C23 175.4(10) . . . . ? C20 N4 C24 C25 -175.6(11) . . . . ? Co1 N4 C24 C25 -1.0(12) . . . . ? C22 C23 C24 N4 0(2) . . . . ? C22 C23 C24 C25 176.1(12) . . . . ? C26 N5 C25 C24 178.0(11) . . . . ? Co1 N5 C25 C24 4.8(15) . . . . ? N4 C24 C25 N5 -2.4(16) . . . . ? C23 C24 C25 N5 -178.9(12) . . . . ? C25 N5 C26 C27 11.0(19) . . . . ? Co1 N5 C26 C27 -175.7(9) . . . . ? C25 N5 C26 C31 -168.8(12) . . . . ? Co1 N5 C26 C31 4.4(13) . . . . ? C31 C26 C27 C28 -0.6(19) . . . . ? N5 C26 C27 C28 179.6(11) . . . . ? C26 C27 C28 C29 0(2) . . . . ? C27 C28 C29 C30 0(2) . . . . ? C28 C29 C30 C31 0.5(19) . . . . ? S2 N6 C31 C26 -178.5(8) . . . . ? Co1 N6 C31 C26 -1.4(13) . . . . ? S2 N6 C31 C30 -1.9(16) . . . . ? Co1 N6 C31 C30 175.2(9) . . . . ? C27 C26 C31 N6 178.2(11) . . . . ? N5 C26 C31 N6 -1.9(15) . . . . ? C27 C26 C31 C30 1.2(17) . . . . ? N5 C26 C31 C30 -179.0(10) . . . . ? C29 C30 C31 N6 -177.8(11) . . . . ? C29 C30 C31 C26 -1.1(16) . . . . ? C31 N6 S2 O4 -179.3(8) . . . . ? Co1 N6 S2 O4 4.0(8) . . . . ? C31 N6 S2 O3 52.6(10) . . . . ? Co1 N6 S2 O3 -124.2(6) . . . . ? C31 N6 S2 C32 -64.0(9) . . . . ? Co1 N6 S2 C32 119.2(6) . . . . ? C32 C33 C34 C35 -1(2) . . . . ? C33 C34 C35 C36 7(2) . . . . ? C33 C34 C35 C38 -176.0(12) . . . . ? C34 C35 C36 C37 -10(3) . . . . ? C38 C35 C36 C37 172.9(16) . . . . ? C35 C36 C37 C32 7(3) . . . . ? C34 C33 C32 C37 -2(2) . . . . ? C34 C33 C32 S2 -177.2(11) . . . . ? C36 C37 C32 C33 0(3) . . . . ? C36 C37 C32 S2 174.5(14) . . . . ? O4 S2 C32 C33 85.1(11) . . . . ? O3 S2 C32 C33 -151.9(10) . . . . ? N6 S2 C32 C33 -31.0(12) . . . . ? O4 S2 C32 C37 -89.8(13) . . . . ? O3 S2 C32 C37 33.2(13) . . . . ? N6 S2 C32 C37 154.1(12) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.498 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.087 #END data_cu(L3)2_4 _database_code_CSD 154001 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H48 Cu1.50 N9 O6 S3' _chemical_formula_weight 1146.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C 2/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 42.6482(4) _cell_length_b 14.7187(2) _cell_length_c 17.70550(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.8850(10) _cell_angle_gamma 90.00 _cell_volume 10239.37(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Blocklike' _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4740 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23365 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.1288 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.28 _reflns_number_total 11708 _reflns_number_gt 4823 _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 w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+28.2120P] 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 11708 _refine_ls_number_parameters 690 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2150 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2143 _refine_ls_wR_factor_gt 0.1590 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.19717(2) 0.48290(6) -0.36593(5) 0.0686(3) Uani 1 d . . . S1 S 0.24494(4) 0.64707(12) -0.37833(12) 0.0661(5) Uani 1 d . . . S2 S 0.13441(4) 0.61045(12) -0.37174(12) 0.0656(5) Uani 1 d . . . O1 O 0.24694(12) 0.7357(3) -0.3427(3) 0.0848(16) Uani 1 d . . . O2 O 0.22064(12) 0.6367(3) -0.4616(3) 0.0858(16) Uani 1 d . . . O3 O 0.10077(11) 0.5709(3) -0.4002(3) 0.0870(16) Uani 1 d . . . O4 O 0.15557(13) 0.5945(3) -0.2865(3) 0.0821(15) Uani 1 d . . . N1 N 0.23748(19) 0.3642(5) -0.3780(5) 0.088(2) Uani 1 d . . . N2 N 0.18731(15) 0.4706(4) -0.4895(4) 0.0651(15) Uani 1 d . . . N3 N 0.15596(12) 0.5787(4) -0.4222(3) 0.0576(14) Uani 1 d . . . N4 N 0.16298(15) 0.3842(4) -0.3659(4) 0.0726(16) Uani 1 d . . . N5 N 0.21579(13) 0.4506(3) -0.2499(3) 0.0573(14) Uani 1 d . . . N6 N 0.23739(13) 0.5690(3) -0.3249(3) 0.0611(14) Uani 1 d . . . C1 C 0.2372(3) 0.3744(7) -0.4518(7) 0.106(3) Uani 1 d . . . C2 C 0.2626(4) 0.3420(12) -0.4785(9) 0.205(7) Uani 1 d . . . H2 H 0.2628 0.3547 -0.5297 0.246 Uiso 1 calc R . . C3 C 0.2879(3) 0.2874(12) -0.4178(10) 0.211(8) Uani 1 d . . . H3 H 0.3048 0.2611 -0.4313 0.254 Uiso 1 calc R . . C4 C 0.2884(3) 0.2719(9) -0.3398(9) 0.143(5) Uani 1 d . . . H4 H 0.3047 0.2359 -0.3009 0.172 Uiso 1 calc R . . C5 C 0.2627(2) 0.3144(6) -0.3259(6) 0.098(3) Uani 1 d . . . H5 H 0.2628 0.3077 -0.2735 0.118 Uiso 1 calc R . . C6 C 0.2082(3) 0.4279(7) -0.5117(6) 0.112(3) Uani 1 d . . . H6 H 0.2055 0.4299 -0.5665 0.134 Uiso 1 calc R . . C7 C 0.1595(2) 0.5195(5) -0.5439(4) 0.0654(19) Uani 1 d . . . C8 C 0.1482(2) 0.5123(6) -0.6282(5) 0.084(2) Uani 1 d . . . H8 H 0.1594 0.4739 -0.6511 0.101 Uiso 1 calc R . . C9 C 0.1211(3) 0.5603(7) -0.6773(5) 0.095(3) Uani 1 d . . . H9 H 0.1145 0.5563 -0.7339 0.114 Uiso 1 calc R . . C10 C 0.1033(2) 0.6146(6) -0.6460(5) 0.092(3) Uani 1 d . . . H10 H 0.0845 0.6463 -0.6813 0.111 Uiso 1 calc R . . C11 C 0.11344(18) 0.6234(5) -0.5590(5) 0.075(2) Uani 1 d . . . H11 H 0.1013 0.6600 -0.5372 0.090 Uiso 1 calc R . . C12 C 0.14206(16) 0.5754(5) -0.5082(4) 0.0622(18) Uani 1 d . . . C13 C 0.12822(17) 0.7298(5) -0.3819(4) 0.0659(19) Uani 1 d . . . C14 C 0.15609(18) 0.7862(5) -0.3687(5) 0.079(2) Uani 1 d . . . H14 H 0.1772 0.7615 -0.3608 0.095 Uiso 1 calc R . . C15 C 0.15194(19) 0.8790(6) -0.3675(5) 0.087(2) Uani 1 d . . . H15 H 0.1706 0.9168 -0.3577 0.105 Uiso 1 calc R . . C16 C 0.1206(2) 0.9170(5) -0.3803(5) 0.076(2) Uani 1 d . . . C17 C 0.09323(19) 0.8593(6) -0.3948(4) 0.077(2) Uani 1 d . . . H17 H 0.0719 0.8839 -0.4047 0.092 Uiso 1 calc R . . C18 C 0.09691(17) 0.7668(5) -0.3947(5) 0.075(2) Uani 1 d . . . H18 H 0.0783 0.7292 -0.4032 0.089 Uiso 1 calc R . . C19 C 0.1156(2) 1.0180(5) -0.3792(5) 0.108(3) Uani 1 d . . . H19A H 0.1368 1.0483 -0.3688 0.162 Uiso 1 calc R . . H19B H 0.1077 1.0330 -0.3368 0.162 Uiso 1 calc R . . H19C H 0.0991 1.0372 -0.4313 0.162 Uiso 1 calc R . . C20 C 0.16955(17) 0.3501(5) -0.2911(5) 0.0651(19) Uani 1 d . . . C21 C 0.1491(2) 0.2863(5) -0.2764(6) 0.087(2) Uani 1 d . . . H21 H 0.1548 0.2609 -0.2246 0.105 Uiso 1 calc R . . C22 C 0.1195(2) 0.2613(5) -0.3415(7) 0.099(3) Uani 1 d . . . H22 H 0.1049 0.2193 -0.3334 0.119 Uiso 1 calc R . . C23 C 0.1121(2) 0.2972(6) -0.4155(7) 0.102(3) Uani 1 d . . . H23 H 0.0919 0.2821 -0.4588 0.122 Uiso 1 calc R . . C24 C 0.1346(2) 0.3567(6) -0.4268(5) 0.094(3) Uani 1 d . . . H24 H 0.1299 0.3789 -0.4793 0.113 Uiso 1 calc R . . C25 C 0.20025(18) 0.3877(5) -0.2278(5) 0.0683(19) Uani 1 d . . . H25 H 0.2082 0.3670 -0.1739 0.082 Uiso 1 calc R . . C26 C 0.24537(17) 0.4966(5) -0.1991(4) 0.0647(18) Uani 1 d . . . C27 C 0.2635(2) 0.4774(6) -0.1162(5) 0.100(3) Uani 1 d . . . H27 H 0.2566 0.4306 -0.0907 0.120 Uiso 1 calc R . . C28 C 0.2914(3) 0.5286(8) -0.0732(6) 0.126(4) Uani 1 d . . . H28 H 0.3040 0.5160 -0.0182 0.151 Uiso 1 calc R . . C29 C 0.3012(2) 0.6003(7) -0.1120(6) 0.103(3) Uani 1 d . . . H29 H 0.3195 0.6370 -0.0817 0.124 Uiso 1 calc R . . C30 C 0.28393(18) 0.6165(5) -0.1934(5) 0.073(2) Uani 1 d . . . H30 H 0.2909 0.6637 -0.2182 0.088 Uiso 1 calc R . . C31 C 0.25621(16) 0.5639(4) -0.2399(4) 0.0597(17) Uani 1 d . . . C32 C 0.28563(16) 0.6283(4) -0.3809(4) 0.0561(17) Uani 1 d . . . C33 C 0.29595(17) 0.6918(5) -0.4249(4) 0.0683(19) Uani 1 d . . . H33 H 0.2816 0.7395 -0.4513 0.082 Uiso 1 calc R . . C34 C 0.32697(19) 0.6841(5) -0.4294(4) 0.077(2) Uani 1 d . . . H34 H 0.3337 0.7277 -0.4581 0.093 Uiso 1 calc R . . C35 C 0.34878(19) 0.6125(5) -0.3921(5) 0.0704(19) Uani 1 d . . . C36 C 0.3382(2) 0.5505(6) -0.3500(4) 0.078(2) Uani 1 d . . . H36 H 0.3527 0.5028 -0.3237 0.094 Uiso 1 calc R . . C37 C 0.30648(18) 0.5560(5) -0.3452(4) 0.0684(19) Uani 1 d . . . H37 H 0.2995 0.5113 -0.3180 0.082 Uiso 1 calc R . . C38 C 0.3837(2) 0.6072(7) -0.3961(6) 0.112(3) Uani 1 d . . . H38A H 0.3864 0.6570 -0.4281 0.168 Uiso 1 calc R . . H38B H 0.3858 0.5509 -0.4210 0.168 Uiso 1 calc R . . H38C H 0.4010 0.6106 -0.3416 0.168 Uiso 1 calc R . . Cu2 Cu 0.0000 0.34405(7) -0.7500 0.0505(3) Uani 1 d S . . S3 S 0.01308(4) 0.20552(10) -0.58645(10) 0.0487(4) Uani 1 d . . . O5 O 0.03846(10) 0.2030(3) -0.5042(2) 0.0589(11) Uani 1 d . . . O6 O -0.01814(10) 0.2507(3) -0.5970(3) 0.0588(11) Uani 1 d . . . N7 N -0.00319(13) 0.4577(3) -0.8389(4) 0.0597(14) Uani 1 d . . . N8 N 0.04689(12) 0.3522(3) -0.7448(3) 0.0477(12) Uani 1 d . . . N9 N 0.02654(11) 0.2507(3) -0.6500(3) 0.0433(11) Uani 1 d . . . C50 C 0.02778(16) 0.4734(4) -0.8385(4) 0.0493(15) Uani 1 d . . . C51 C 0.03437(18) 0.5410(4) -0.8849(4) 0.0591(17) Uani 1 d . . . H51 H 0.0562 0.5500 -0.8836 0.071 Uiso 1 calc R . . C52 C 0.0077(2) 0.5939(5) -0.9325(5) 0.079(2) Uani 1 d . . . H52 H 0.0113 0.6410 -0.9632 0.095 Uiso 1 calc R . . C53 C -0.0238(2) 0.5780(6) -0.9352(5) 0.092(3) Uani 1 d . . . H53 H -0.0422 0.6125 -0.9688 0.110 Uiso 1 calc R . . C54 C -0.0284(2) 0.5087(6) -0.8864(6) 0.086(2) Uani 1 d . . . H54 H -0.0501 0.4984 -0.8877 0.103 Uiso 1 calc R . . C55 C 0.05430(15) 0.4120(4) -0.7873(4) 0.0517(15) Uani 1 d . . . H55 H 0.0763 0.4163 -0.7856 0.062 Uiso 1 calc R . . C56 C 0.00247(14) 0.0902(4) -0.6162(4) 0.0471(15) Uani 1 d . . . C57 C 0.01944(19) 0.0195(5) -0.5677(4) 0.074(2) Uani 1 d . . . H57 H 0.0375 0.0307 -0.5181 0.089 Uiso 1 calc R . . C58 C 0.0097(2) -0.0690(5) -0.5925(5) 0.083(2) Uani 1 d . . . H58 H 0.0220 -0.1168 -0.5601 0.099 Uiso 1 calc R . . C59 C -0.0170(2) -0.0871(5) -0.6622(5) 0.077(2) Uani 1 d . . . C60 C -0.0338(2) -0.0161(6) -0.7104(5) 0.093(3) Uani 1 d . . . H60 H -0.0522 -0.0276 -0.7592 0.112 Uiso 1 calc R . . C61 C -0.02415(19) 0.0718(5) -0.6881(4) 0.076(2) Uani 1 d . . . H61 H -0.0358 0.1192 -0.7221 0.091 Uiso 1 calc R . . C62 C -0.0282(2) -0.1861(5) -0.6876(6) 0.110(3) Uani 1 d . . . H62A H -0.0476 -0.1863 -0.7387 0.165 Uiso 1 calc R . . H62B H -0.0341 -0.2146 -0.6462 0.165 Uiso 1 calc R . . H62C H -0.0099 -0.2188 -0.6938 0.165 Uiso 1 calc R . . C63 C 0.05929(14) 0.2329(4) -0.6460(4) 0.0443(14) Uani 1 d . . . C64 C 0.07069(15) 0.2882(4) -0.6955(4) 0.0495(15) Uani 1 d . . . C65 C 0.10256(18) 0.2755(5) -0.6970(5) 0.079(2) Uani 1 d . . . H65 H 0.1099 0.3133 -0.7289 0.095 Uiso 1 calc R . . C66 C 0.12349(19) 0.2074(6) -0.6513(6) 0.101(3) Uani 1 d . . . H66 H 0.1445 0.1972 -0.6544 0.121 Uiso 1 calc R . . C67 C 0.11306(18) 0.1540(5) -0.6008(5) 0.082(2) Uani 1 d . . . H67 H 0.1276 0.1099 -0.5680 0.098 Uiso 1 calc R . . C68 C 0.08194(15) 0.1653(4) -0.5987(4) 0.0595(17) Uani 1 d . . . H68 H 0.0753 0.1277 -0.5654 0.071 Uiso 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 0.0664(6) 0.0707(6) 0.0661(6) 0.0051(5) 0.0229(5) -0.0185(4) S1 0.0537(10) 0.0600(12) 0.0777(13) 0.0126(10) 0.0180(10) -0.0064(8) S2 0.0590(10) 0.0715(12) 0.0752(13) 0.0077(10) 0.0360(10) 0.0000(9) O1 0.076(3) 0.054(3) 0.129(4) 0.007(3) 0.045(3) 0.001(2) O2 0.065(3) 0.103(4) 0.071(3) 0.032(3) 0.007(3) -0.017(3) O3 0.064(3) 0.087(3) 0.126(5) 0.005(3) 0.055(3) -0.012(3) O4 0.107(4) 0.087(4) 0.064(3) 0.016(3) 0.046(3) 0.025(3) N1 0.096(5) 0.089(5) 0.100(5) -0.006(4) 0.061(5) -0.001(4) N2 0.070(4) 0.067(4) 0.065(4) -0.011(3) 0.034(3) -0.008(3) N3 0.046(3) 0.076(4) 0.052(3) -0.005(3) 0.020(3) -0.007(3) N4 0.067(4) 0.073(4) 0.079(4) -0.004(4) 0.029(4) -0.017(3) N5 0.057(3) 0.051(3) 0.068(4) 0.008(3) 0.029(3) 0.002(3) N6 0.059(3) 0.056(3) 0.058(3) 0.008(3) 0.011(3) -0.003(3) C1 0.120(8) 0.111(7) 0.111(8) -0.003(6) 0.070(7) 0.018(6) C2 0.167(13) 0.33(2) 0.145(11) -0.010(13) 0.092(11) 0.099(14) C3 0.126(11) 0.32(2) 0.171(14) -0.068(15) 0.034(11) 0.100(12) C4 0.121(9) 0.176(11) 0.133(10) -0.046(9) 0.049(9) 0.020(8) C5 0.089(6) 0.095(7) 0.113(8) -0.008(6) 0.042(6) 0.005(5) C6 0.151(9) 0.118(8) 0.093(7) 0.002(6) 0.076(7) 0.014(7) C7 0.081(5) 0.063(5) 0.058(4) -0.009(4) 0.034(4) -0.027(4) C8 0.116(7) 0.089(6) 0.051(5) -0.004(4) 0.035(5) -0.030(5) C9 0.123(8) 0.105(7) 0.055(5) -0.011(5) 0.032(6) -0.049(6) C10 0.079(6) 0.106(7) 0.069(6) 0.022(5) 0.004(5) -0.040(5) C11 0.060(4) 0.082(5) 0.071(5) 0.012(4) 0.012(4) -0.012(4) C12 0.050(4) 0.067(5) 0.056(4) -0.003(4) 0.007(4) -0.027(3) C13 0.054(4) 0.082(5) 0.066(5) 0.006(4) 0.028(4) 0.002(4) C14 0.055(4) 0.083(6) 0.104(6) 0.008(5) 0.036(4) 0.007(4) C15 0.061(5) 0.082(6) 0.107(7) 0.004(5) 0.019(5) -0.004(4) C16 0.080(5) 0.070(5) 0.070(5) 0.012(4) 0.020(5) 0.016(4) C17 0.059(5) 0.093(6) 0.076(5) 0.009(5) 0.023(4) 0.015(4) C18 0.054(4) 0.082(6) 0.089(6) 0.007(4) 0.029(4) 0.000(4) C19 0.109(7) 0.091(7) 0.100(7) 0.000(5) 0.015(6) 0.018(5) C20 0.058(4) 0.058(4) 0.087(5) 0.006(4) 0.037(4) 0.008(4) C21 0.086(6) 0.070(5) 0.125(7) 0.017(5) 0.062(6) -0.005(5) C22 0.091(7) 0.063(5) 0.166(10) -0.018(6) 0.073(7) -0.027(5) C23 0.088(6) 0.103(7) 0.117(8) -0.030(6) 0.044(6) -0.052(5) C24 0.083(6) 0.106(7) 0.087(6) -0.013(5) 0.027(5) -0.033(5) C25 0.069(5) 0.068(5) 0.077(5) 0.017(4) 0.037(4) 0.013(4) C26 0.061(4) 0.069(5) 0.061(4) 0.003(4) 0.020(4) 0.001(4) C27 0.099(7) 0.115(7) 0.070(6) 0.026(5) 0.016(5) -0.013(6) C28 0.111(8) 0.173(11) 0.062(6) 0.017(7) 0.000(6) -0.022(8) C29 0.077(6) 0.131(8) 0.082(7) -0.010(6) 0.010(6) -0.015(5) C30 0.058(4) 0.088(5) 0.064(5) -0.003(4) 0.015(4) -0.007(4) C31 0.048(4) 0.062(4) 0.067(5) -0.004(4) 0.020(4) -0.005(3) C32 0.053(4) 0.057(4) 0.054(4) 0.002(3) 0.016(3) -0.008(3) C33 0.059(4) 0.078(5) 0.065(5) 0.015(4) 0.020(4) -0.001(4) C34 0.072(5) 0.087(6) 0.069(5) 0.018(4) 0.023(4) -0.012(4) C35 0.071(5) 0.082(5) 0.062(5) -0.005(4) 0.029(4) -0.004(4) C36 0.080(5) 0.094(6) 0.062(5) 0.009(4) 0.029(4) 0.020(4) C37 0.079(5) 0.066(5) 0.068(5) 0.006(4) 0.038(4) -0.003(4) C38 0.087(6) 0.142(8) 0.119(8) 0.001(6) 0.051(6) 0.003(6) Cu2 0.0575(7) 0.0413(6) 0.0575(7) 0.000 0.0277(6) 0.000 S3 0.0471(9) 0.0505(9) 0.0517(10) 0.0012(8) 0.0227(8) -0.0018(7) O5 0.061(3) 0.066(3) 0.047(3) -0.002(2) 0.019(2) -0.009(2) O6 0.053(2) 0.061(3) 0.074(3) 0.006(2) 0.037(2) 0.004(2) N7 0.053(3) 0.056(3) 0.076(4) -0.011(3) 0.031(3) -0.007(3) N8 0.054(3) 0.043(3) 0.047(3) 0.003(2) 0.021(3) -0.006(2) N9 0.039(3) 0.039(3) 0.052(3) 0.008(2) 0.018(2) 0.002(2) C50 0.061(4) 0.039(3) 0.052(4) -0.006(3) 0.027(3) -0.007(3) C51 0.068(4) 0.053(4) 0.060(4) 0.007(3) 0.028(4) -0.007(3) C52 0.112(7) 0.056(5) 0.067(5) 0.010(4) 0.033(5) 0.013(5) C53 0.077(6) 0.099(7) 0.079(6) 0.000(5) 0.007(5) 0.030(5) C54 0.065(5) 0.087(6) 0.103(7) -0.017(5) 0.030(5) 0.004(5) C55 0.056(4) 0.045(4) 0.060(4) -0.003(3) 0.029(3) -0.009(3) C56 0.046(3) 0.050(4) 0.045(3) 0.008(3) 0.018(3) -0.007(3) C57 0.078(5) 0.063(5) 0.065(5) 0.010(4) 0.010(4) 0.002(4) C58 0.102(6) 0.048(5) 0.086(6) 0.022(4) 0.023(5) -0.004(4) C59 0.099(6) 0.058(5) 0.086(6) -0.002(5) 0.050(5) -0.018(5) C60 0.100(6) 0.073(6) 0.080(6) -0.009(5) 0.006(5) -0.033(5) C61 0.079(5) 0.063(5) 0.063(5) 0.008(4) 0.004(4) -0.011(4) C62 0.155(9) 0.068(5) 0.122(7) -0.005(5) 0.070(7) -0.031(6) C63 0.042(3) 0.047(3) 0.044(3) -0.003(3) 0.017(3) -0.003(3) C64 0.047(3) 0.052(4) 0.051(4) 0.001(3) 0.020(3) -0.001(3) C65 0.067(5) 0.083(5) 0.104(6) 0.030(5) 0.050(5) 0.008(4) C66 0.059(5) 0.129(8) 0.128(8) 0.034(6) 0.052(5) 0.032(5) C67 0.063(5) 0.098(6) 0.091(6) 0.027(5) 0.037(5) 0.032(4) C68 0.052(4) 0.060(4) 0.066(4) 0.013(4) 0.022(4) 0.009(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 N5 1.952(5) . ? Cu1 N6 2.026(5) . ? Cu1 N4 2.058(6) . ? Cu1 N2 2.068(6) . ? Cu1 N3 2.170(5) . ? Cu1 N1 2.518(7) . ? S1 O1 1.437(5) . ? S1 O2 1.442(5) . ? S1 N6 1.600(5) . ? S1 C32 1.775(7) . ? S2 O3 1.445(5) . ? S2 O4 1.446(5) . ? S2 N3 1.581(5) . ? S2 C13 1.776(7) . ? N1 C1 1.312(11) . ? N1 C5 1.333(10) . ? N2 C6 1.273(10) . ? N2 C7 1.402(9) . ? N3 C12 1.403(8) . ? N4 C24 1.332(8) . ? N4 C20 1.340(9) . ? N5 C25 1.285(8) . ? N5 C26 1.405(8) . ? N6 C31 1.404(8) . ? C1 C2 1.420(14) . ? C1 C6 1.501(12) . ? C2 C3 1.436(18) . ? C3 C4 1.390(18) . ? C4 C5 1.365(13) . ? C7 C8 1.382(9) . ? C7 C12 1.413(10) . ? C8 C9 1.343(11) . ? C9 C10 1.360(12) . ? C10 C11 1.435(11) . ? C11 C12 1.394(9) . ? C13 C18 1.377(9) . ? C13 C14 1.393(9) . ? C14 C15 1.379(10) . ? C15 C16 1.382(10) . ? C16 C17 1.386(10) . ? C16 C19 1.503(10) . ? C17 C18 1.371(9) . ? C20 C21 1.375(9) . ? C20 C25 1.461(9) . ? C21 C22 1.386(11) . ? C22 C23 1.331(12) . ? C23 C24 1.372(11) . ? C26 C27 1.396(10) . ? C26 C31 1.407(9) . ? C27 C28 1.363(11) . ? C28 C29 1.409(12) . ? C29 C30 1.360(10) . ? C30 C31 1.385(9) . ? C32 C37 1.373(8) . ? C32 C33 1.393(9) . ? C33 C34 1.361(10) . ? C34 C35 1.390(9) . ? C35 C36 1.362(10) . ? C35 C38 1.520(10) . ? C36 C37 1.392(10) . ? Cu2 N8 1.970(5) . ? Cu2 N8 1.970(5) 2_553 ? Cu2 N9 2.178(4) 2_553 ? Cu2 N9 2.178(4) . ? Cu2 N7 2.264(6) 2_553 ? Cu2 N7 2.264(6) . ? S3 O6 1.434(4) . ? S3 O5 1.438(4) . ? S3 N9 1.594(5) . ? S3 C56 1.783(6) . ? N7 C54 1.314(9) . ? N7 C50 1.338(8) . ? N8 C55 1.274(7) . ? N8 C64 1.411(7) . ? N9 C63 1.395(7) . ? C50 C51 1.387(8) . ? C50 C55 1.456(8) . ? C51 C52 1.364(9) . ? C52 C53 1.347(11) . ? C53 C54 1.398(11) . ? C56 C61 1.362(8) . ? C56 C57 1.364(8) . ? C57 C58 1.385(9) . ? C58 C59 1.342(10) . ? C59 C60 1.362(10) . ? C59 C62 1.545(10) . ? C60 C61 1.369(9) . ? C63 C68 1.412(8) . ? C63 C64 1.414(8) . ? C64 C65 1.382(9) . ? C65 C66 1.376(10) . ? C66 C67 1.389(10) . ? C67 C68 1.352(9) . ? 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 N5 Cu1 N6 80.4(2) . . ? N5 Cu1 N4 80.0(2) . . ? N6 Cu1 N4 160.4(2) . . ? N5 Cu1 N2 157.5(2) . . ? N6 Cu1 N2 103.3(2) . . ? N4 Cu1 N2 94.9(2) . . ? N5 Cu1 N3 124.5(2) . . ? N6 Cu1 N3 100.38(19) . . ? N4 Cu1 N3 90.6(2) . . ? N2 Cu1 N3 77.1(2) . . ? N5 Cu1 N1 84.8(2) . . ? N6 Cu1 N1 87.4(2) . . ? N4 Cu1 N1 91.0(2) . . ? N2 Cu1 N1 73.4(3) . . ? N3 Cu1 N1 150.4(2) . . ? O1 S1 O2 116.1(3) . . ? O1 S1 N6 112.6(3) . . ? O2 S1 N6 107.4(3) . . ? O1 S1 C32 105.1(3) . . ? O2 S1 C32 106.2(3) . . ? N6 S1 C32 109.1(3) . . ? O3 S2 O4 115.5(3) . . ? O3 S2 N3 113.6(3) . . ? O4 S2 N3 106.2(3) . . ? O3 S2 C13 106.0(3) . . ? O4 S2 C13 105.9(3) . . ? N3 S2 C13 109.4(3) . . ? C1 N1 C5 116.5(8) . . ? C1 N1 Cu1 105.3(6) . . ? C5 N1 Cu1 135.8(6) . . ? C6 N2 C7 123.2(7) . . ? C6 N2 Cu1 119.5(6) . . ? C7 N2 Cu1 116.9(5) . . ? C12 N3 S2 122.0(5) . . ? C12 N3 Cu1 113.7(4) . . ? S2 N3 Cu1 118.5(3) . . ? C24 N4 C20 117.4(6) . . ? C24 N4 Cu1 129.4(6) . . ? C20 N4 Cu1 112.9(5) . . ? C25 N5 C26 126.3(6) . . ? C25 N5 Cu1 116.7(5) . . ? C26 N5 Cu1 116.9(4) . . ? C31 N6 S1 120.6(4) . . ? C31 N6 Cu1 113.8(4) . . ? S1 N6 Cu1 125.0(3) . . ? N1 C1 C2 125.4(11) . . ? N1 C1 C6 116.7(9) . . ? C2 C1 C6 117.8(11) . . ? C1 C2 C3 112.8(13) . . ? C4 C3 C2 123.5(12) . . ? C5 C4 C3 113.6(13) . . ? N1 C5 C4 128.0(11) . . ? N2 C6 C1 121.6(8) . . ? C8 C7 N2 123.4(8) . . ? C8 C7 C12 120.2(8) . . ? N2 C7 C12 116.3(6) . . ? C9 C8 C7 120.8(9) . . ? C8 C9 C10 121.3(8) . . ? C9 C10 C11 120.5(8) . . ? C12 C11 C10 118.0(8) . . ? C11 C12 N3 125.3(7) . . ? C11 C12 C7 119.1(7) . . ? N3 C12 C7 115.6(6) . . ? C18 C13 C14 120.1(7) . . ? C18 C13 S2 120.3(6) . . ? C14 C13 S2 119.3(5) . . ? C15 C14 C13 119.1(7) . . ? C14 C15 C16 121.4(7) . . ? C15 C16 C17 118.3(7) . . ? C15 C16 C19 122.1(8) . . ? C17 C16 C19 119.6(8) . . ? C18 C17 C16 121.4(7) . . ? C17 C18 C13 119.8(7) . . ? N4 C20 C21 122.6(7) . . ? N4 C20 C25 113.4(6) . . ? C21 C20 C25 124.0(8) . . ? C20 C21 C22 117.5(8) . . ? C23 C22 C21 120.4(8) . . ? C22 C23 C24 118.9(9) . . ? N4 C24 C23 122.9(9) . . ? N5 C25 C20 117.0(7) . . ? C27 C26 N5 124.6(7) . . ? C27 C26 C31 121.7(7) . . ? N5 C26 C31 113.7(6) . . ? C28 C27 C26 118.8(8) . . ? C27 C28 C29 120.1(8) . . ? C30 C29 C28 120.5(8) . . ? C29 C30 C31 121.2(8) . . ? C30 C31 N6 127.5(6) . . ? C30 C31 C26 117.6(7) . . ? N6 C31 C26 115.0(6) . . ? C37 C32 C33 119.2(6) . . ? C37 C32 S1 125.0(5) . . ? C33 C32 S1 115.8(5) . . ? C34 C33 C32 120.2(7) . . ? C33 C34 C35 121.4(7) . . ? C36 C35 C34 117.8(7) . . ? C36 C35 C38 122.0(8) . . ? C34 C35 C38 120.2(7) . . ? C35 C36 C37 122.1(7) . . ? C32 C37 C36 119.2(7) . . ? N8 Cu2 N8 173.0(3) . 2_553 ? N8 Cu2 N9 105.87(18) . 2_553 ? N8 Cu2 N9 78.66(18) 2_553 2_553 ? N8 Cu2 N9 78.66(18) . . ? N8 Cu2 N9 105.87(18) 2_553 . ? N9 Cu2 N9 101.8(2) 2_553 . ? N8 Cu2 N7 97.90(19) . 2_553 ? N8 Cu2 N7 76.86(19) 2_553 2_553 ? N9 Cu2 N7 154.51(18) 2_553 2_553 ? N9 Cu2 N7 91.68(18) . 2_553 ? N8 Cu2 N7 76.86(19) . . ? N8 Cu2 N7 97.90(19) 2_553 . ? N9 Cu2 N7 91.68(18) 2_553 . ? N9 Cu2 N7 154.51(18) . . ? N7 Cu2 N7 84.8(3) 2_553 . ? O6 S3 O5 116.0(3) . . ? O6 S3 N9 106.6(2) . . ? O5 S3 N9 112.9(2) . . ? O6 S3 C56 106.7(3) . . ? O5 S3 C56 106.2(3) . . ? N9 S3 C56 107.9(3) . . ? C54 N7 C50 117.7(6) . . ? C54 N7 Cu2 132.9(5) . . ? C50 N7 Cu2 109.4(4) . . ? C55 N8 C64 122.9(5) . . ? C55 N8 Cu2 119.7(4) . . ? C64 N8 Cu2 117.4(4) . . ? C63 N9 S3 120.9(4) . . ? C63 N9 Cu2 110.7(4) . . ? S3 N9 Cu2 128.4(2) . . ? N7 C50 C51 123.2(6) . . ? N7 C50 C55 115.0(5) . . ? C51 C50 C55 121.8(6) . . ? C52 C51 C50 117.6(7) . . ? C53 C52 C51 120.2(8) . . ? C52 C53 C54 118.9(8) . . ? N7 C54 C53 122.4(8) . . ? N8 C55 C50 119.0(6) . . ? C61 C56 C57 118.8(6) . . ? C61 C56 S3 119.2(5) . . ? C57 C56 S3 121.9(5) . . ? C56 C57 C58 119.9(7) . . ? C59 C58 C57 121.3(7) . . ? C58 C59 C60 118.4(7) . . ? C58 C59 C62 120.7(8) . . ? C60 C59 C62 120.9(8) . . ? C59 C60 C61 121.2(7) . . ? C56 C61 C60 120.3(7) . . ? N9 C63 C68 127.1(5) . . ? N9 C63 C64 116.0(5) . . ? C68 C63 C64 116.8(5) . . ? C65 C64 N8 123.6(6) . . ? C65 C64 C63 120.8(6) . . ? N8 C64 C63 115.5(5) . . ? C66 C65 C64 120.4(7) . . ? C65 C66 C67 119.6(7) . . ? C68 C67 C66 120.7(7) . . ? C67 C68 C63 121.6(7) . . ? _diffrn_measured_fraction_theta_max 0.443 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.443 _refine_diff_density_max 0.381 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.069 #END data_Zn(L3)2.2CH3CN_5 _database_code_CSD 154002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H38 N8 O4 S2 Zn' _chemical_formula_weight 848.29 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' '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 11.372(2) _cell_length_b 11.7922(13) _cell_length_c 14.668(6) _cell_angle_alpha 98.446(18) _cell_angle_beta 92.76(2) _cell_angle_gamma 95.033(12) _cell_volume 1934.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13600 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.1107 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6800 _reflns_number_gt 4415 _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^)+(0.0898P)^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 6800 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1775 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.007 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.97131(6) 0.48209(5) 0.24852(4) 0.0263(2) Uani 1 1 d . . . S1 S 0.94506(13) 0.22079(11) 0.28491(9) 0.0273(3) Uani 1 1 d . . . S2 S 0.70712(12) 0.46060(12) 0.15132(9) 0.0289(3) Uani 1 1 d . . . O1 O 1.0419(4) 0.1598(3) 0.3101(3) 0.0360(9) Uani 1 1 d . . . O2 O 0.8942(3) 0.2892(3) 0.3599(2) 0.0332(9) Uani 1 1 d . . . O3 O 0.7756(3) 0.3932(3) 0.0881(2) 0.0339(9) Uani 1 1 d . . . O4 O 0.6436(3) 0.5439(3) 0.1119(3) 0.0376(10) Uani 1 1 d . . . N1 N 1.0298(4) 0.6790(4) 0.2167(3) 0.0295(10) Uani 1 1 d . . . N2 N 1.0605(4) 0.4699(4) 0.1255(3) 0.0259(10) Uani 1 1 d . . . N3 N 0.9749(4) 0.3044(3) 0.2132(3) 0.0249(10) Uani 1 1 d . . . N4 N 1.1475(4) 0.4920(4) 0.3320(3) 0.0303(11) Uani 1 1 d . . . N5 N 0.9461(4) 0.5781(3) 0.3777(3) 0.0243(10) Uani 1 1 d . . . N6 N 0.7930(4) 0.5128(4) 0.2375(3) 0.0256(10) Uani 1 1 d . . . C1 C 1.0218(6) 0.7837(5) 0.2624(4) 0.0393(15) Uani 1 1 d . . . H1 H 0.9822 0.7904 0.3166 0.047 Uiso 1 1 calc R . . C2 C 1.0695(6) 0.8832(5) 0.2332(4) 0.0389(15) Uani 1 1 d . . . H2 H 1.0637 0.9547 0.2683 0.047 Uiso 1 1 calc R . . C3 C 1.1246(6) 0.8754(5) 0.1532(4) 0.0421(15) Uani 1 1 d . . . H3 H 1.1574 0.9410 0.1321 0.051 Uiso 1 1 calc R . . C4 C 1.1309(6) 0.7673(5) 0.1038(4) 0.0446(17) Uani 1 1 d . . . H4 H 1.1659 0.7588 0.0475 0.054 Uiso 1 1 calc R . . C5 C 1.0849(5) 0.6732(4) 0.1387(4) 0.0315(13) Uani 1 1 d . . . C6 C 1.0959(6) 0.5575(5) 0.0908(4) 0.0391(15) Uani 1 1 d . . . H6 H 1.1296 0.5483 0.0340 0.047 Uiso 1 1 calc R . . C7 C 1.0784(5) 0.3567(4) 0.0871(3) 0.0266(12) Uani 1 1 d . . . C8 C 1.1421(6) 0.3308(5) 0.0083(4) 0.0345(14) Uani 1 1 d . . . H8 H 1.1731 0.3898 -0.0217 0.041 Uiso 1 1 calc R . . C9 C 1.1586(5) 0.2186(5) -0.0246(4) 0.0371(14) Uani 1 1 d . . . H9 H 1.2005 0.2014 -0.0770 0.045 Uiso 1 1 calc R . . C10 C 1.1134(5) 0.1323(5) 0.0200(4) 0.0367(14) Uani 1 1 d . . . H10 H 1.1235 0.0563 -0.0032 0.044 Uiso 1 1 calc R . . C11 C 1.0527(5) 0.1560(4) 0.0993(4) 0.0294(12) Uani 1 1 d . . . H11 H 1.0232 0.0961 0.1290 0.035 Uiso 1 1 calc R . . C12 C 1.0356(5) 0.2701(4) 0.1350(3) 0.0257(12) Uani 1 1 d . . . C13 C 0.8324(5) 0.1156(5) 0.2335(4) 0.0314(13) Uani 1 1 d . . . C14 C 0.8040(6) 0.0205(5) 0.2765(4) 0.0470(17) Uani 1 1 d . . . H14 H 0.8471 0.0103 0.3297 0.056 Uiso 1 1 calc R . . C15 C 0.7114(7) -0.0588(6) 0.2397(5) 0.056(2) Uani 1 1 d . . . H15 H 0.6922 -0.1224 0.2687 0.067 Uiso 1 1 calc R . . C16 C 0.6465(7) -0.0453(6) 0.1606(6) 0.057(2) Uani 1 1 d . . . C17 C 0.6772(6) 0.0486(6) 0.1200(5) 0.0502(18) Uani 1 1 d . . . H17 H 0.6344 0.0578 0.0663 0.060 Uiso 1 1 calc R . . C18 C 0.7676(5) 0.1303(5) 0.1538(4) 0.0362(14) Uani 1 1 d . . . H18 H 0.7855 0.1938 0.1244 0.043 Uiso 1 1 calc R . . C19 C 0.5454(8) -0.1324(8) 0.1208(7) 0.095(3) Uani 1 1 d . . . H19A H 0.5141 -0.1709 0.1690 0.143 Uiso 1 1 calc R . . H19B H 0.5732 -0.1879 0.0742 0.143 Uiso 1 1 calc R . . H19C H 0.4844 -0.0940 0.0940 0.143 Uiso 1 1 calc R . . C20 C 1.2463(5) 0.4492(5) 0.3100(4) 0.0390(15) Uani 1 1 d . . . H20 H 1.2474 0.4021 0.2534 0.047 Uiso 1 1 calc R . . C21 C 1.3489(6) 0.4700(6) 0.3662(5) 0.0456(16) Uani 1 1 d . . . H21 H 1.4173 0.4378 0.3477 0.055 Uiso 1 1 calc R . . C22 C 1.3482(5) 0.5390(5) 0.4495(4) 0.0406(15) Uani 1 1 d . . . H22 H 1.4166 0.5559 0.4882 0.049 Uiso 1 1 calc R . . C23 C 1.2450(5) 0.5827(5) 0.4750(4) 0.0339(13) Uani 1 1 d . . . H23 H 1.2419 0.6286 0.5319 0.041 Uiso 1 1 calc R . . C24 C 1.1463(5) 0.5580(4) 0.4156(3) 0.0253(12) Uani 1 1 d . . . C25 C 1.0335(5) 0.6033(5) 0.4369(4) 0.0295(13) Uani 1 1 d . . . H25 H 1.0258 0.6498 0.4928 0.035 Uiso 1 1 calc R . . C26 C 0.8375(5) 0.6213(4) 0.3876(3) 0.0250(11) Uani 1 1 d . . . C27 C 0.8069(5) 0.6949(5) 0.4633(4) 0.0339(14) Uani 1 1 d . . . H27 H 0.8617 0.7175 0.5132 0.041 Uiso 1 1 calc R . . C28 C 0.6990(5) 0.7344(5) 0.4665(4) 0.0398(15) Uani 1 1 d . . . H28 H 0.6806 0.7843 0.5179 0.048 Uiso 1 1 calc R . . C29 C 0.6172(5) 0.7012(5) 0.3945(4) 0.0392(15) Uani 1 1 d . . . H29 H 0.5428 0.7283 0.3972 0.047 Uiso 1 1 calc R . . C30 C 0.6438(5) 0.6274(5) 0.3171(4) 0.0353(14) Uani 1 1 d . . . H30 H 0.5872 0.6058 0.2683 0.042 Uiso 1 1 calc R . . C31 C 0.7533(5) 0.5860(4) 0.3118(4) 0.0258(12) Uani 1 1 d . . . C32 C 0.5995(5) 0.3647(5) 0.1888(4) 0.0318(13) Uani 1 1 d . . . C33 C 0.4945(5) 0.3306(5) 0.1364(4) 0.0367(14) Uani 1 1 d . . . H33 H 0.4785 0.3624 0.0832 0.044 Uiso 1 1 calc R . . C34 C 0.4146(6) 0.2506(6) 0.1626(5) 0.0485(17) Uani 1 1 d . . . H34 H 0.3443 0.2292 0.1266 0.058 Uiso 1 1 calc R . . C35 C 0.4340(5) 0.1990(5) 0.2419(4) 0.0419(16) Uani 1 1 d . . . C36 C 0.5405(5) 0.2354(5) 0.2936(4) 0.0392(15) Uani 1 1 d . . . H36 H 0.5574 0.2037 0.3467 0.047 Uiso 1 1 calc R . . C37 C 0.6206(5) 0.3167(5) 0.2679(4) 0.0333(13) Uani 1 1 d . . . H37 H 0.6903 0.3401 0.3043 0.040 Uiso 1 1 calc R . . C38 C 0.3468(7) 0.1119(7) 0.2684(6) 0.066(2) Uani 1 1 d . . . H38A H 0.3708 0.0942 0.3280 0.098 Uiso 1 1 calc R . . H38B H 0.3420 0.0433 0.2236 0.098 Uiso 1 1 calc R . . H38C H 0.2708 0.1413 0.2709 0.098 Uiso 1 1 calc R . . N80 N 0.3413(9) 0.7360(10) 0.2789(7) 0.122(3) Uani 1 1 d . . . C80 C 0.3759(9) 0.5993(8) 0.1212(7) 0.087(3) Uani 1 1 d . . . H80A H 0.3567 0.6379 0.0700 0.131 Uiso 1 1 calc R . . H80B H 0.3271 0.5276 0.1159 0.131 Uiso 1 1 calc R . . H80C H 0.4576 0.5845 0.1211 0.131 Uiso 1 1 calc R . . C81 C 0.3544(9) 0.6744(10) 0.2103(8) 0.091(3) Uani 1 1 d . . . C90A C 0.2460(16) 0.9096(11) 0.4681(8) 0.143(6) Uani 0.50 1 d P A 1 H90A H 0.2435 0.8337 0.4334 0.215 Uiso 0.50 1 calc PR A 1 H90B H 0.2851 0.9107 0.5277 0.215 Uiso 0.50 1 calc PR A 1 H90C H 0.2886 0.9637 0.4358 0.215 Uiso 0.50 1 calc PR A 1 C91A C 0.105(3) 0.946(3) 0.4811(15) 0.131(11) Uani 0.50 1 d P A 1 N90A N 0.0000 1.0000 0.5000 0.221(13) Uani 1 2 d S . 1 C90B C 0.2460(16) 0.9096(11) 0.4681(8) 0.143(6) Uani 0.50 1 d P B 2 H90D H 0.2032 0.9762 0.4805 0.215 Uiso 0.50 1 calc PR B 2 H90E H 0.2199 0.8541 0.5064 0.215 Uiso 0.50 1 calc PR B 2 H90F H 0.2318 0.8764 0.4043 0.215 Uiso 0.50 1 calc PR B 2 C91B C 0.376(2) 0.944(2) 0.4886(15) 0.093(6) Uani 0.50 1 d P B 2 N90B N 0.5000 1.0000 0.5000 0.266(16) Uani 1 2 d S . 2 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 0.0334(4) 0.0263(4) 0.0166(3) -0.0061(2) 0.0019(2) 0.0037(3) S1 0.0405(8) 0.0250(7) 0.0155(6) -0.0006(5) 0.0052(5) 0.0025(6) S2 0.0296(8) 0.0357(8) 0.0191(7) -0.0001(6) -0.0001(5) -0.0011(6) O1 0.050(3) 0.034(2) 0.025(2) 0.0036(17) 0.0033(18) 0.0096(19) O2 0.049(3) 0.035(2) 0.0137(18) -0.0033(16) 0.0075(17) 0.0056(18) O3 0.038(2) 0.045(2) 0.0154(18) -0.0026(16) 0.0044(16) 0.0003(18) O4 0.040(2) 0.045(2) 0.029(2) 0.0094(18) -0.0001(18) 0.0062(19) N1 0.034(3) 0.027(2) 0.026(2) -0.0006(19) 0.001(2) 0.003(2) N2 0.037(3) 0.022(2) 0.016(2) -0.0042(18) -0.0051(18) 0.0001(19) N3 0.038(3) 0.018(2) 0.017(2) -0.0038(17) 0.0051(19) 0.0025(19) N4 0.039(3) 0.035(3) 0.015(2) -0.0046(19) -0.0019(19) 0.008(2) N5 0.029(2) 0.022(2) 0.021(2) -0.0003(18) 0.0049(19) 0.0015(18) N6 0.023(2) 0.032(2) 0.018(2) -0.0080(18) -0.0017(18) 0.0024(19) C1 0.049(4) 0.034(3) 0.033(3) -0.002(3) 0.004(3) 0.005(3) C2 0.053(4) 0.020(3) 0.041(4) -0.001(3) -0.002(3) 0.006(3) C3 0.063(4) 0.027(3) 0.036(3) 0.008(3) -0.002(3) -0.003(3) C4 0.078(5) 0.029(3) 0.026(3) 0.004(3) 0.012(3) -0.003(3) C5 0.052(4) 0.022(3) 0.019(3) 0.000(2) -0.004(2) -0.004(3) C6 0.070(4) 0.026(3) 0.017(3) -0.003(2) 0.010(3) -0.006(3) C7 0.034(3) 0.027(3) 0.017(3) -0.003(2) 0.002(2) 0.001(2) C8 0.055(4) 0.029(3) 0.019(3) 0.003(2) 0.006(3) 0.000(3) C9 0.052(4) 0.043(4) 0.014(3) -0.006(2) 0.011(3) 0.005(3) C10 0.055(4) 0.029(3) 0.024(3) -0.008(2) 0.005(3) 0.011(3) C11 0.041(3) 0.023(3) 0.023(3) -0.001(2) 0.007(2) 0.001(2) C12 0.033(3) 0.029(3) 0.013(2) -0.005(2) 0.001(2) 0.004(2) C13 0.044(4) 0.028(3) 0.020(3) -0.005(2) 0.009(2) 0.003(3) C14 0.067(5) 0.038(4) 0.036(4) 0.004(3) 0.018(3) -0.002(3) C15 0.066(5) 0.037(4) 0.063(5) 0.004(3) 0.028(4) -0.009(3) C16 0.056(5) 0.042(4) 0.066(5) -0.019(4) 0.022(4) -0.012(3) C17 0.040(4) 0.059(4) 0.042(4) -0.020(3) 0.002(3) 0.000(3) C18 0.044(4) 0.035(3) 0.024(3) -0.009(2) 0.006(3) -0.004(3) C19 0.080(6) 0.073(6) 0.111(8) -0.035(6) 0.016(6) -0.036(5) C20 0.041(4) 0.048(4) 0.024(3) -0.009(3) -0.003(3) 0.010(3) C21 0.037(4) 0.055(4) 0.045(4) 0.000(3) 0.011(3) 0.010(3) C22 0.038(4) 0.055(4) 0.026(3) -0.001(3) -0.004(3) 0.007(3) C23 0.034(3) 0.039(3) 0.025(3) -0.005(2) -0.005(2) 0.005(3) C24 0.028(3) 0.028(3) 0.019(3) 0.001(2) 0.002(2) 0.003(2) C25 0.033(3) 0.037(3) 0.017(3) -0.001(2) 0.002(2) 0.000(2) C26 0.029(3) 0.022(3) 0.023(3) -0.001(2) 0.001(2) 0.003(2) C27 0.040(3) 0.039(3) 0.021(3) -0.007(2) 0.007(2) 0.007(3) C28 0.046(4) 0.043(4) 0.028(3) -0.009(3) 0.012(3) 0.011(3) C29 0.036(3) 0.043(4) 0.039(3) 0.001(3) 0.006(3) 0.010(3) C30 0.036(3) 0.035(3) 0.033(3) -0.003(3) 0.000(3) 0.006(3) C31 0.028(3) 0.023(3) 0.026(3) -0.001(2) 0.007(2) 0.001(2) C32 0.032(3) 0.031(3) 0.028(3) -0.004(2) 0.003(2) -0.001(2) C33 0.037(3) 0.043(4) 0.024(3) -0.007(3) -0.005(2) -0.004(3) C34 0.041(4) 0.053(4) 0.043(4) -0.013(3) -0.001(3) -0.004(3) C35 0.039(4) 0.036(3) 0.046(4) -0.006(3) 0.010(3) -0.008(3) C36 0.042(4) 0.044(4) 0.030(3) -0.001(3) 0.009(3) 0.003(3) C37 0.037(3) 0.038(3) 0.020(3) -0.006(2) 0.000(2) -0.004(3) C38 0.059(5) 0.067(5) 0.065(5) -0.003(4) 0.018(4) -0.012(4) N80 0.134(9) 0.161(10) 0.070(6) 0.004(6) -0.016(6) 0.036(7) C80 0.088(7) 0.087(7) 0.084(7) 0.012(5) -0.019(5) 0.011(5) C81 0.087(7) 0.102(8) 0.081(7) 0.008(6) -0.006(6) 0.015(6) C90A 0.224(19) 0.122(10) 0.068(8) 0.001(7) -0.008(9) -0.035(11) C91A 0.13(2) 0.21(3) 0.040(11) -0.007(14) 0.001(14) -0.03(2) N90A 0.17(2) 0.38(4) 0.124(17) 0.12(2) -0.028(16) -0.05(2) C90B 0.224(19) 0.122(10) 0.068(8) 0.001(7) -0.008(9) -0.035(11) C91B 0.108(18) 0.101(16) 0.073(14) 0.008(12) 0.008(13) 0.038(15) N90B 0.26(3) 0.38(4) 0.142(18) -0.09(2) -0.059(19) 0.19(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 Zn1 N3 2.087(4) . ? Zn1 N6 2.094(4) . ? Zn1 N2 2.105(4) . ? Zn1 N5 2.106(4) . ? Zn1 N4 2.282(5) . ? Zn1 N1 2.476(4) . ? S1 O1 1.430(4) . ? S1 O2 1.441(3) . ? S1 N3 1.573(4) . ? S1 C13 1.762(6) . ? S2 O3 1.435(4) . ? S2 O4 1.439(4) . ? S2 N6 1.574(4) . ? S2 C32 1.756(6) . ? N1 C5 1.327(7) . ? N1 C1 1.327(7) . ? N2 C6 1.261(7) . ? N2 C7 1.407(6) . ? N3 C12 1.395(6) . ? N4 C20 1.307(7) . ? N4 C24 1.353(6) . ? N5 C25 1.273(7) . ? N5 C26 1.383(6) . ? N6 C31 1.405(6) . ? C1 C2 1.382(8) . ? C2 C3 1.352(8) . ? C3 C4 1.380(8) . ? C4 C5 1.363(8) . ? C5 C6 1.458(7) . ? C7 C12 1.389(8) . ? C7 C8 1.403(7) . ? C8 C9 1.372(8) . ? C9 C10 1.365(8) . ? C10 C11 1.387(7) . ? C11 C12 1.403(7) . ? C13 C14 1.386(8) . ? C13 C18 1.392(8) . ? C14 C15 1.378(9) . ? C15 C16 1.382(11) . ? C16 C17 1.360(10) . ? C16 C19 1.507(10) . ? C17 C18 1.367(8) . ? C20 C21 1.378(9) . ? C21 C22 1.365(8) . ? C22 C23 1.369(8) . ? C23 C24 1.370(8) . ? C24 C25 1.462(7) . ? C26 C27 1.384(7) . ? C26 C31 1.421(7) . ? C27 C28 1.350(8) . ? C28 C29 1.362(9) . ? C29 C30 1.388(8) . ? C30 C31 1.379(7) . ? C32 C37 1.384(8) . ? C32 C33 1.384(8) . ? C33 C34 1.361(9) . ? C34 C35 1.407(10) . ? C35 C36 1.397(9) . ? C35 C38 1.472(9) . ? C36 C37 1.371(8) . ? N80 C81 1.175(12) . ? C80 C81 1.510(14) . ? C90A C91A 1.71(3) . ? C91A N90A 1.42(4) . ? N90A C91A 1.42(4) 2_576 ? C91B N90B 1.49(3) . ? N90B C91B 1.49(3) 2_676 ? 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 N3 Zn1 N6 106.01(17) . . ? N3 Zn1 N2 77.81(16) . . ? N6 Zn1 N2 116.23(17) . . ? N3 Zn1 N5 128.94(16) . . ? N6 Zn1 N5 76.83(16) . . ? N2 Zn1 N5 147.93(16) . . ? N3 Zn1 N4 89.94(17) . . ? N6 Zn1 N4 151.25(15) . . ? N2 Zn1 N4 90.12(16) . . ? N5 Zn1 N4 74.56(16) . . ? N3 Zn1 N1 149.04(15) . . ? N6 Zn1 N1 89.98(16) . . ? N2 Zn1 N1 71.32(15) . . ? N5 Zn1 N1 79.96(15) . . ? N4 Zn1 N1 87.85(16) . . ? O1 S1 O2 115.9(2) . . ? O1 S1 N3 113.9(2) . . ? O2 S1 N3 105.7(2) . . ? O1 S1 C13 106.3(3) . . ? O2 S1 C13 106.6(2) . . ? N3 S1 C13 107.9(2) . . ? O3 S2 O4 114.9(2) . . ? O3 S2 N6 106.6(2) . . ? O4 S2 N6 114.4(2) . . ? O3 S2 C32 107.0(2) . . ? O4 S2 C32 106.1(3) . . ? N6 S2 C32 107.4(3) . . ? C5 N1 C1 116.6(5) . . ? C5 N1 Zn1 109.6(3) . . ? C1 N1 Zn1 133.7(4) . . ? C6 N2 C7 123.6(5) . . ? C6 N2 Zn1 122.2(4) . . ? C7 N2 Zn1 114.2(3) . . ? C12 N3 S1 121.7(4) . . ? C12 N3 Zn1 115.1(3) . . ? S1 N3 Zn1 120.9(2) . . ? C20 N4 C24 117.6(5) . . ? C20 N4 Zn1 130.5(4) . . ? C24 N4 Zn1 111.8(3) . . ? C25 N5 C26 124.2(4) . . ? C25 N5 Zn1 119.0(4) . . ? C26 N5 Zn1 116.3(3) . . ? C31 N6 S2 120.9(4) . . ? C31 N6 Zn1 115.9(3) . . ? S2 N6 Zn1 123.2(2) . . ? N1 C1 C2 123.3(6) . . ? C3 C2 C1 119.2(5) . . ? C2 C3 C4 118.2(6) . . ? C5 C4 C3 119.0(6) . . ? N1 C5 C4 123.7(5) . . ? N1 C5 C6 115.9(5) . . ? C4 C5 C6 120.4(5) . . ? N2 C6 C5 120.9(5) . . ? C12 C7 C8 120.7(5) . . ? C12 C7 N2 116.2(4) . . ? C8 C7 N2 123.0(5) . . ? C9 C8 C7 120.2(5) . . ? C10 C9 C8 119.7(5) . . ? C9 C10 C11 121.2(5) . . ? C10 C11 C12 120.3(5) . . ? C7 C12 N3 116.5(4) . . ? C7 C12 C11 117.9(5) . . ? N3 C12 C11 125.5(5) . . ? C14 C13 C18 120.0(6) . . ? C14 C13 S1 119.1(5) . . ? C18 C13 S1 120.8(4) . . ? C15 C14 C13 119.5(7) . . ? C14 C15 C16 121.1(7) . . ? C17 C16 C15 117.9(6) . . ? C17 C16 C19 121.4(9) . . ? C15 C16 C19 120.7(8) . . ? C16 C17 C18 123.5(7) . . ? C17 C18 C13 118.1(6) . . ? N4 C20 C21 123.5(5) . . ? C22 C21 C20 118.7(6) . . ? C21 C22 C23 118.8(6) . . ? C22 C23 C24 119.2(5) . . ? N4 C24 C23 122.1(5) . . ? N4 C24 C25 115.4(5) . . ? C23 C24 C25 122.5(5) . . ? N5 C25 C24 119.0(5) . . ? N5 C26 C27 125.4(5) . . ? N5 C26 C31 115.3(4) . . ? C27 C26 C31 119.3(5) . . ? C28 C27 C26 121.4(5) . . ? C27 C28 C29 120.1(5) . . ? C28 C29 C30 120.5(6) . . ? C31 C30 C29 120.7(5) . . ? C30 C31 N6 126.8(5) . . ? C30 C31 C26 118.0(5) . . ? N6 C31 C26 115.2(4) . . ? C37 C32 C33 118.8(5) . . ? C37 C32 S2 120.9(4) . . ? C33 C32 S2 120.2(5) . . ? C34 C33 C32 120.1(6) . . ? C33 C34 C35 122.6(6) . . ? C36 C35 C34 116.1(6) . . ? C36 C35 C38 122.2(7) . . ? C34 C35 C38 121.7(6) . . ? C37 C36 C35 121.4(6) . . ? C36 C37 C32 121.0(6) . . ? N80 C81 C80 177.3(13) . . ? N90A C91A C90A 168(2) . . ? C91A N90A C91A 180.0(17) 2_576 . ? C91B N90B C91B 180(2) 2_676 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.053 _refine_diff_density_min -1.382 _refine_diff_density_rms 0.120 #END