# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. Yu-Peng Tian' _publ_contact_author_email lidongmei5456@126.com loop_ _publ_author_name 'Qiong Zhang' 'Yupeng Tian' 'Hongping Zhou' # Attachment '070430b_0m.cif' data_070430b_0m _database_code_depnum_ccdc_archive 'CCDC 660614' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H56 Cd2 Cl0 I4 N8 O0 S2' _chemical_formula_weight 1853.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 19.953(5) _cell_length_b 13.943(5) _cell_length_c 27.347(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 106.629(5) _cell_angle_gamma 90.000(5) _cell_volume 7290(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 2.381 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6976 _exptl_absorpt_correction_T_max 0.9150 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _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 29331 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.62 _reflns_number_total 8087 _reflns_number_gt 3641 _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^)+(0.1000P)^2^+143.1394P] 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 8087 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1858 _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.2682 _refine_ls_wR_factor_gt 0.2230 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.32590(5) -0.00113(7) 1.04756(4) 0.0601(3) Uani 1 1 d . . . I2 I 0.19450(6) -0.07432(7) 1.01063(5) 0.0817(4) Uani 1 1 d . . . I1 I 0.42015(6) -0.06587(8) 1.13520(5) 0.0815(4) Uani 1 1 d . . . S1 S 0.6483(3) 0.6559(4) 0.6792(2) 0.1020(16) Uani 1 1 d . . . N2 N 0.3716(5) 0.1190(7) 1.0072(4) 0.052(3) Uani 1 1 d . . . N3 N 0.2982(5) 0.1537(8) 1.0727(4) 0.054(3) Uani 1 1 d . . . C5 C 0.4101(6) -0.0092(8) 0.9629(5) 0.050(3) Uani 1 1 d . . . C9 C 0.3943(7) 0.2832(9) 0.9967(6) 0.061(4) Uani 1 1 d . . . H9 H 0.3881 0.3470 1.0043 0.074 Uiso 1 1 calc R . . C21 C 0.5148(10) 0.4822(13) 0.8890(8) 0.096(7) Uani 1 1 d . . . N1 N 0.3774(6) -0.0672(7) 0.9880(5) 0.060(3) Uani 1 1 d . . . C6 C 0.4069(6) 0.0965(8) 0.9735(5) 0.050(3) Uani 1 1 d . . . C32 C 0.7314(10) 0.9098(13) 0.6694(7) 0.090(5) Uani 1 1 d . . . H32 H 0.7272 0.9733 0.6784 0.108 Uiso 1 1 calc R . . C17 C 0.4630(8) 0.3390(10) 0.9393(6) 0.067(4) Uani 1 1 d . . . C18 C 0.4478(11) 0.4333(12) 0.9433(9) 0.115(8) Uani 1 1 d . . . H18 H 0.4196 0.4524 0.9634 0.138 Uiso 1 1 calc R . . N4 N 0.6460(7) 0.8637(9) 0.7116(5) 0.076(4) Uani 1 1 d . . . C10 C 0.3653(7) 0.2124(8) 1.0190(5) 0.053(3) Uani 1 1 d . . . C3 C 0.4421(8) -0.1414(11) 0.9207(6) 0.069(4) Uani 1 1 d . . . H3 H 0.4664 -0.1664 0.8992 0.083 Uiso 1 1 calc R . . C35 C 0.7840(11) 0.7970(15) 0.6264(9) 0.111(7) Uani 1 1 d . . . H35 H 0.8127 0.7818 0.6061 0.134 Uiso 1 1 calc R . . C7 C 0.4367(7) 0.1670(9) 0.9517(6) 0.058(4) Uani 1 1 d . . . H7 H 0.4606 0.1501 0.9284 0.070 Uiso 1 1 calc R . . C4 C 0.4426(7) -0.0446(9) 0.9294(6) 0.060(4) Uani 1 1 d . . . H4 H 0.4651 -0.0034 0.9125 0.072 Uiso 1 1 calc R . . C11 C 0.3232(6) 0.2296(9) 1.0550(5) 0.052(3) Uani 1 1 d . . . C29 C 0.6241(7) 0.7947(13) 0.7437(6) 0.070(4) Uani 1 1 d . . . C27 C 0.5980(9) 0.8225(16) 0.7833(7) 0.096(6) Uani 1 1 d . . . H27 H 0.5964 0.8872 0.7911 0.115 Uiso 1 1 calc R . . C14 C 0.2408(8) 0.2555(13) 1.1174(7) 0.084(5) Uani 1 1 d . . . H14 H 0.2126 0.2636 1.1388 0.100 Uiso 1 1 calc R . . C31 C 0.6922(8) 0.8393(12) 0.6861(6) 0.071(4) Uani 1 1 d . . . C13 C 0.2666(9) 0.3321(12) 1.0987(7) 0.079(5) Uani 1 1 d . . . H13 H 0.2574 0.3931 1.1088 0.095 Uiso 1 1 calc R . . C15 C 0.2572(7) 0.1634(11) 1.1038(6) 0.067(4) Uani 1 1 d . . . H15 H 0.2399 0.1096 1.1162 0.081 Uiso 1 1 calc R . . C23 C 0.5581(11) 0.5521(16) 0.8343(10) 0.111(8) Uani 1 1 d . . . H23 H 0.5660 0.4881 0.8280 0.133 Uiso 1 1 calc R . . C1 C 0.3753(8) -0.1636(9) 0.9770(6) 0.066(4) Uani 1 1 d . . . H1 H 0.3517 -0.2046 0.9933 0.079 Uiso 1 1 calc R . . C8 C 0.4321(6) 0.2623(9) 0.9635(6) 0.055(3) Uani 1 1 d . . . C12 C 0.3057(7) 0.3231(10) 1.0655(6) 0.068(4) Uani 1 1 d . . . H12 H 0.3201 0.3763 1.0505 0.081 Uiso 1 1 calc R . . C2 C 0.4062(8) -0.2006(10) 0.9433(6) 0.065(4) Uani 1 1 d . . . H2 H 0.4030 -0.2658 0.9358 0.078 Uiso 1 1 calc R . . C30 C 0.7037(9) 0.7464(12) 0.6732(7) 0.080(5) Uani 1 1 d . . . C36 C 0.6319(11) 0.9672(13) 0.7186(8) 0.101(6) Uani 1 1 d . . . H36A H 0.6292 1.0012 0.6871 0.121 Uiso 1 1 calc R . . H36B H 0.5869 0.9732 0.7252 0.121 Uiso 1 1 calc R . . C16 C 0.5079(9) 0.3199(11) 0.9108(7) 0.086(5) Uani 1 1 d . . . H16 H 0.5212 0.2565 0.9084 0.103 Uiso 1 1 calc R . . C25 C 0.6050(9) 0.6293(16) 0.7615(8) 0.105(7) Uani 1 1 d . . . H25 H 0.6081 0.5649 0.7536 0.126 Uiso 1 1 calc R . . C34 C 0.7478(10) 0.7262(14) 0.6437(7) 0.092(5) Uani 1 1 d . . . H34 H 0.7533 0.6627 0.6352 0.110 Uiso 1 1 calc R . . C26 C 0.5737(10) 0.754(2) 0.8118(7) 0.129(10) Uani 1 1 d . . . H26 H 0.5544 0.7737 0.8372 0.154 Uiso 1 1 calc R . . C28 C 0.6269(9) 0.6983(12) 0.7330(6) 0.081(5) Uani 1 1 d . . . C37 C 0.6862(12) 1.0134(15) 0.7611(9) 0.127(8) Uani 1 1 d . . . H37A H 0.6741 1.0054 0.7924 0.191 Uiso 1 1 calc R . . H37B H 0.6887 1.0805 0.7540 0.191 Uiso 1 1 calc R . . H37C H 0.7307 0.9840 0.7642 0.191 Uiso 1 1 calc R . . C22 C 0.5364(10) 0.578(2) 0.8606(11) 0.145(12) Uani 1 1 d . . . H22 H 0.5298 0.6416 0.8676 0.174 Uiso 1 1 calc R . . C19 C 0.4749(13) 0.4996(14) 0.9174(11) 0.130(9) Uani 1 1 d . . . H19 H 0.4634 0.5635 0.9206 0.156 Uiso 1 1 calc R . . C33 C 0.7765(10) 0.8887(14) 0.6399(8) 0.101(6) Uani 1 1 d . . . H33 H 0.8012 0.9376 0.6296 0.121 Uiso 1 1 calc R . . C24 C 0.5781(11) 0.654(2) 0.8023(8) 0.105(7) Uani 1 1 d . . . C20 C 0.5347(11) 0.3891(13) 0.8857(8) 0.108(7) Uani 1 1 d . . . H20 H 0.5654 0.3730 0.8671 0.129 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 Cd1 0.0641(6) 0.0441(5) 0.0825(8) 0.0041(5) 0.0379(6) -0.0031(5) I2 0.0705(7) 0.0547(6) 0.1259(11) 0.0010(6) 0.0374(7) -0.0116(5) I1 0.0825(8) 0.0845(8) 0.0866(8) 0.0139(6) 0.0389(6) 0.0096(6) S1 0.130(4) 0.072(3) 0.109(4) 0.015(3) 0.043(3) -0.004(3) N2 0.053(6) 0.035(5) 0.075(8) 0.001(5) 0.028(6) -0.004(5) N3 0.055(6) 0.052(6) 0.065(8) 0.001(6) 0.029(6) 0.002(5) C5 0.049(7) 0.036(6) 0.070(9) -0.005(6) 0.023(7) -0.001(5) C9 0.068(9) 0.034(6) 0.088(11) 0.006(7) 0.032(8) 0.004(6) C21 0.092(13) 0.077(13) 0.114(16) 0.043(11) 0.020(12) -0.035(10) N1 0.081(8) 0.036(5) 0.076(8) 0.001(5) 0.043(7) -0.004(5) C6 0.046(7) 0.038(6) 0.072(10) -0.003(6) 0.026(7) -0.007(5) C32 0.107(14) 0.073(11) 0.111(15) 0.010(10) 0.062(12) 0.003(10) C17 0.060(9) 0.051(8) 0.089(12) 0.020(8) 0.022(9) 0.000(7) C18 0.142(18) 0.052(10) 0.18(2) 0.021(12) 0.099(17) 0.007(10) N4 0.097(9) 0.057(7) 0.090(10) 0.005(7) 0.053(8) 0.014(7) C10 0.058(8) 0.031(6) 0.073(10) -0.004(6) 0.023(7) -0.004(5) C3 0.077(10) 0.067(9) 0.073(11) -0.013(8) 0.038(9) 0.016(8) C35 0.115(16) 0.090(14) 0.16(2) -0.002(14) 0.084(15) -0.005(12) C7 0.057(8) 0.052(8) 0.078(11) 0.006(7) 0.039(8) 0.000(6) C4 0.054(8) 0.047(7) 0.085(11) -0.001(7) 0.031(8) -0.002(6) C11 0.049(7) 0.044(7) 0.066(9) -0.015(7) 0.019(7) -0.008(6) C29 0.058(9) 0.103(13) 0.050(10) 0.025(9) 0.015(7) -0.016(8) C27 0.078(11) 0.134(17) 0.083(13) -0.003(12) 0.034(11) -0.026(11) C14 0.070(11) 0.096(13) 0.090(13) 0.000(11) 0.031(10) 0.014(10) C31 0.064(9) 0.092(12) 0.062(10) 0.005(9) 0.026(8) -0.003(8) C13 0.087(12) 0.060(9) 0.096(13) -0.011(9) 0.037(11) 0.015(8) C15 0.065(9) 0.076(10) 0.069(11) -0.002(8) 0.033(8) 0.008(8) C23 0.086(14) 0.100(15) 0.14(2) -0.040(14) 0.020(14) 0.027(11) C1 0.084(10) 0.038(7) 0.093(12) 0.009(7) 0.054(9) 0.001(7) C8 0.048(7) 0.042(7) 0.082(11) -0.001(7) 0.028(7) -0.001(6) C12 0.072(9) 0.054(8) 0.084(12) -0.011(8) 0.033(9) 0.008(7) C2 0.073(9) 0.044(7) 0.082(11) -0.010(7) 0.029(9) -0.003(7) C30 0.096(12) 0.067(10) 0.093(13) 0.007(9) 0.056(11) 0.010(9) C36 0.113(15) 0.073(11) 0.124(17) -0.011(11) 0.048(14) 0.005(11) C16 0.099(13) 0.053(9) 0.113(15) 0.010(9) 0.040(12) -0.012(8) C25 0.086(12) 0.123(16) 0.096(15) 0.047(13) 0.013(11) -0.042(12) C34 0.107(14) 0.087(12) 0.090(14) -0.005(10) 0.042(11) 0.024(11) C26 0.074(13) 0.25(3) 0.070(14) 0.026(18) 0.029(10) -0.057(17) C28 0.096(13) 0.073(11) 0.066(12) 0.012(9) 0.011(9) -0.016(9) C37 0.15(2) 0.111(17) 0.124(19) -0.048(15) 0.045(16) -0.020(15) C22 0.055(12) 0.18(3) 0.18(3) -0.10(2) -0.002(14) 0.019(14) C19 0.131(18) 0.066(12) 0.21(3) 0.046(15) 0.09(2) 0.002(12) C33 0.102(14) 0.077(12) 0.150(19) -0.008(12) 0.078(14) -0.002(10) C24 0.085(13) 0.15(2) 0.070(14) 0.022(14) 0.001(11) -0.052(14) C20 0.120(16) 0.074(12) 0.149(19) 0.032(12) 0.071(14) -0.011(11) _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 Cd1 N2 2.331(10) . ? Cd1 N1 2.347(11) . ? Cd1 N3 2.379(11) . ? Cd1 I2 2.7240(16) . ? Cd1 I1 2.7413(17) . ? S1 C30 1.716(17) . ? S1 C28 1.747(19) . ? N2 C6 1.346(16) . ? N2 C10 1.358(15) . ? N3 C11 1.320(16) . ? N3 C15 1.346(16) . ? C5 N1 1.345(15) . ? C5 C4 1.359(18) . ? C5 C6 1.506(16) . ? C9 C8 1.367(18) . ? C9 C10 1.373(17) . ? C9 H9 0.9300 . ? C21 C19 1.28(3) . ? C21 C20 1.37(3) . ? C21 C22 1.66(4) . ? N1 C1 1.376(16) . ? C6 C7 1.370(16) . ? C32 C33 1.40(2) . ? C32 C31 1.41(2) . ? C32 H32 0.9300 . ? C17 C18 1.36(2) . ? C17 C16 1.37(2) . ? C17 C8 1.482(18) . ? C18 C19 1.37(3) . ? C18 H18 0.9300 . ? N4 C31 1.350(19) . ? N4 C29 1.451(18) . ? N4 C36 1.49(2) . ? C10 C11 1.484(18) . ? C3 C2 1.353(19) . ? C3 C4 1.370(19) . ? C3 H3 0.9300 . ? C35 C33 1.35(2) . ? C35 C34 1.38(2) . ? C35 H35 0.9300 . ? C7 C8 1.375(17) . ? C7 H7 0.9300 . ? C4 H4 0.9300 . ? C11 C12 1.400(18) . ? C29 C28 1.38(2) . ? C29 C27 1.38(2) . ? C27 C26 1.41(3) . ? C27 H27 0.9300 . ? C14 C13 1.35(2) . ? C14 C15 1.40(2) . ? C14 H14 0.9300 . ? C31 C30 1.38(2) . ? C13 C12 1.36(2) . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C23 C22 1.00(3) . ? C23 C24 1.78(3) . ? C23 H23 0.9300 . ? C1 C2 1.349(18) . ? C1 H1 0.9300 . ? C12 H12 0.9300 . ? C2 H2 0.9300 . ? C30 C34 1.38(2) . ? C36 C37 1.49(3) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C16 C20 1.38(2) . ? C16 H16 0.9300 . ? C25 C28 1.38(2) . ? C25 C24 1.41(3) . ? C25 H25 0.9300 . ? C34 H34 0.9300 . ? C26 C24 1.42(3) . ? C26 H26 0.9300 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C22 H22 0.9300 . ? C19 H19 0.9300 . ? C33 H33 0.9300 . ? C20 H20 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 N2 Cd1 N1 69.2(3) . . ? N2 Cd1 N3 68.9(4) . . ? N1 Cd1 N3 137.8(4) . . ? N2 Cd1 I2 124.0(3) . . ? N1 Cd1 I2 99.3(3) . . ? N3 Cd1 I2 99.7(3) . . ? N2 Cd1 I1 112.8(3) . . ? N1 Cd1 I1 98.6(3) . . ? N3 Cd1 I1 101.8(3) . . ? I2 Cd1 I1 123.19(5) . . ? C30 S1 C28 98.7(8) . . ? C6 N2 C10 119.4(10) . . ? C6 N2 Cd1 120.6(7) . . ? C10 N2 Cd1 120.0(9) . . ? C11 N3 C15 120.9(12) . . ? C11 N3 Cd1 118.5(8) . . ? C15 N3 Cd1 120.5(9) . . ? N1 C5 C4 121.4(11) . . ? N1 C5 C6 115.9(11) . . ? C4 C5 C6 122.7(12) . . ? C8 C9 C10 121.7(12) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C19 C21 C20 117.4(17) . . ? C19 C21 C22 115(2) . . ? C20 C21 C22 128(2) . . ? C5 N1 C1 117.6(11) . . ? C5 N1 Cd1 119.4(8) . . ? C1 N1 Cd1 123.0(9) . . ? N2 C6 C7 120.4(11) . . ? N2 C6 C5 114.7(10) . . ? C7 C6 C5 124.8(12) . . ? C33 C32 C31 123.2(17) . . ? C33 C32 H32 118.4 . . ? C31 C32 H32 118.4 . . ? C18 C17 C16 115.6(15) . . ? C18 C17 C8 122.1(15) . . ? C16 C17 C8 122.4(13) . . ? C17 C18 C19 118.7(19) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C31 N4 C29 121.0(13) . . ? C31 N4 C36 119.3(14) . . ? C29 N4 C36 117.7(14) . . ? N2 C10 C9 120.2(12) . . ? N2 C10 C11 115.0(11) . . ? C9 C10 C11 124.7(11) . . ? C2 C3 C4 120.0(13) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C33 C35 C34 118.3(18) . . ? C33 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C6 C7 C8 121.7(13) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C5 C4 C3 119.6(13) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N3 C11 C12 121.9(12) . . ? N3 C11 C10 117.3(11) . . ? C12 C11 C10 120.5(12) . . ? C28 C29 C27 119.1(16) . . ? C28 C29 N4 118.7(15) . . ? C27 C29 N4 122.2(17) . . ? C29 C27 C26 121(2) . . ? C29 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C13 C14 C15 118.9(15) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N4 C31 C30 123.7(15) . . ? N4 C31 C32 121.1(15) . . ? C30 C31 C32 115.1(15) . . ? C14 C13 C12 122.3(15) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? N3 C15 C14 119.3(15) . . ? N3 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C22 C23 C24 106(3) . . ? C22 C23 H23 127.1 . . ? C24 C23 H23 127.1 . . ? C2 C1 N1 122.2(13) . . ? C2 C1 H1 118.9 . . ? N1 C1 H1 118.9 . . ? C9 C8 C7 116.5(12) . . ? C9 C8 C17 121.4(12) . . ? C7 C8 C17 122.0(13) . . ? C13 C12 C11 116.5(15) . . ? C13 C12 H12 121.8 . . ? C11 C12 H12 121.8 . . ? C1 C2 C3 119.0(13) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C31 C30 C34 121.3(16) . . ? C31 C30 S1 120.6(13) . . ? C34 C30 S1 116.2(14) . . ? C37 C36 N4 113.3(17) . . ? C37 C36 H36A 108.9 . . ? N4 C36 H36A 108.9 . . ? C37 C36 H36B 108.9 . . ? N4 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? C17 C16 C20 123.7(17) . . ? C17 C16 H16 118.1 . . ? C20 C16 H16 118.1 . . ? C28 C25 C24 122(2) . . ? C28 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C30 C34 C35 122.4(18) . . ? C30 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C27 C26 C24 121(2) . . ? C27 C26 H26 119.4 . . ? C24 C26 H26 119.4 . . ? C29 C28 C25 121.2(19) . . ? C29 C28 S1 122.9(13) . . ? C25 C28 S1 115.5(16) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C23 C22 C21 106(3) . . ? C23 C22 H22 127.1 . . ? C21 C22 H22 127.1 . . ? C21 C19 C18 126(2) . . ? C21 C19 H19 116.9 . . ? C18 C19 H19 116.9 . . ? C35 C33 C32 119.6(18) . . ? C35 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C25 C24 C26 116(2) . . ? C25 C24 C23 112(2) . . ? C26 C24 C23 131(2) . . ? C21 C20 C16 118.1(19) . . ? C21 C20 H20 120.9 . . ? C16 C20 H20 120.9 . . ? 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 N1 Cd1 N2 C6 -3.6(9) . . . . ? N3 Cd1 N2 C6 -178.4(11) . . . . ? I2 Cd1 N2 C6 -90.8(10) . . . . ? I1 Cd1 N2 C6 87.3(10) . . . . ? N1 Cd1 N2 C10 179.1(11) . . . . ? N3 Cd1 N2 C10 4.2(9) . . . . ? I2 Cd1 N2 C10 91.8(10) . . . . ? I1 Cd1 N2 C10 -90.1(10) . . . . ? N2 Cd1 N3 C11 -3.1(9) . . . . ? N1 Cd1 N3 C11 -10.3(13) . . . . ? I2 Cd1 N3 C11 -126.0(9) . . . . ? I1 Cd1 N3 C11 107.0(10) . . . . ? N2 Cd1 N3 C15 176.0(11) . . . . ? N1 Cd1 N3 C15 168.8(10) . . . . ? I2 Cd1 N3 C15 53.2(11) . . . . ? I1 Cd1 N3 C15 -73.9(10) . . . . ? C4 C5 N1 C1 -3(2) . . . . ? C6 C5 N1 C1 176.0(12) . . . . ? C4 C5 N1 Cd1 177.7(10) . . . . ? C6 C5 N1 Cd1 -3.4(16) . . . . ? N2 Cd1 N1 C5 3.6(10) . . . . ? N3 Cd1 N1 C5 10.8(14) . . . . ? I2 Cd1 N1 C5 126.6(10) . . . . ? I1 Cd1 N1 C5 -107.5(10) . . . . ? N2 Cd1 N1 C1 -175.7(13) . . . . ? N3 Cd1 N1 C1 -168.6(10) . . . . ? I2 Cd1 N1 C1 -52.8(12) . . . . ? I1 Cd1 N1 C1 73.1(12) . . . . ? C10 N2 C6 C7 1(2) . . . . ? Cd1 N2 C6 C7 -176.8(10) . . . . ? C10 N2 C6 C5 -179.5(11) . . . . ? Cd1 N2 C6 C5 3.1(15) . . . . ? N1 C5 C6 N2 0.2(17) . . . . ? C4 C5 C6 N2 179.1(13) . . . . ? N1 C5 C6 C7 -179.9(13) . . . . ? C4 C5 C6 C7 -1(2) . . . . ? C16 C17 C18 C19 3(3) . . . . ? C8 C17 C18 C19 -176(2) . . . . ? C6 N2 C10 C9 0(2) . . . . ? Cd1 N2 C10 C9 177.7(10) . . . . ? C6 N2 C10 C11 177.8(12) . . . . ? Cd1 N2 C10 C11 -4.8(16) . . . . ? C8 C9 C10 N2 -2(2) . . . . ? C8 C9 C10 C11 -179.5(13) . . . . ? N2 C6 C7 C8 0(2) . . . . ? C5 C6 C7 C8 -179.5(13) . . . . ? N1 C5 C4 C3 0(2) . . . . ? C6 C5 C4 C3 -178.5(13) . . . . ? C2 C3 C4 C5 3(2) . . . . ? C15 N3 C11 C12 -3(2) . . . . ? Cd1 N3 C11 C12 175.9(11) . . . . ? C15 N3 C11 C10 -177.2(12) . . . . ? Cd1 N3 C11 C10 1.9(16) . . . . ? N2 C10 C11 N3 1.8(18) . . . . ? C9 C10 C11 N3 179.2(13) . . . . ? N2 C10 C11 C12 -172.3(13) . . . . ? C9 C10 C11 C12 5(2) . . . . ? C31 N4 C29 C28 -26(2) . . . . ? C36 N4 C29 C28 170.4(16) . . . . ? C31 N4 C29 C27 156.8(16) . . . . ? C36 N4 C29 C27 -7(2) . . . . ? C28 C29 C27 C26 -1(3) . . . . ? N4 C29 C27 C26 176.5(15) . . . . ? C29 N4 C31 C30 23(3) . . . . ? C36 N4 C31 C30 -173.3(17) . . . . ? C29 N4 C31 C32 -158.3(16) . . . . ? C36 N4 C31 C32 5(2) . . . . ? C33 C32 C31 N4 -175.6(18) . . . . ? C33 C32 C31 C30 3(3) . . . . ? C15 C14 C13 C12 3(3) . . . . ? C11 N3 C15 C14 0(2) . . . . ? Cd1 N3 C15 C14 -178.9(11) . . . . ? C13 C14 C15 N3 0(2) . . . . ? C5 N1 C1 C2 2(2) . . . . ? Cd1 N1 C1 C2 -178.8(12) . . . . ? C10 C9 C8 C7 3(2) . . . . ? C10 C9 C8 C17 179.7(13) . . . . ? C6 C7 C8 C9 -2(2) . . . . ? C6 C7 C8 C17 -178.7(13) . . . . ? C18 C17 C8 C9 -9(3) . . . . ? C16 C17 C8 C9 171.9(16) . . . . ? C18 C17 C8 C7 167.6(18) . . . . ? C16 C17 C8 C7 -12(2) . . . . ? C14 C13 C12 C11 -6(3) . . . . ? N3 C11 C12 C13 6(2) . . . . ? C10 C11 C12 C13 179.6(13) . . . . ? N1 C1 C2 C3 2(2) . . . . ? C4 C3 C2 C1 -4(2) . . . . ? N4 C31 C30 C34 175.0(16) . . . . ? C32 C31 C30 C34 -3(3) . . . . ? N4 C31 C30 S1 12(3) . . . . ? C32 C31 C30 S1 -166.9(14) . . . . ? C28 S1 C30 C31 -33.8(17) . . . . ? C28 S1 C30 C34 161.9(15) . . . . ? C31 N4 C36 C37 -80(2) . . . . ? C29 N4 C36 C37 84(2) . . . . ? C18 C17 C16 C20 -3(3) . . . . ? C8 C17 C16 C20 176.6(17) . . . . ? C31 C30 C34 C35 2(3) . . . . ? S1 C30 C34 C35 165.7(17) . . . . ? C33 C35 C34 C30 1(3) . . . . ? C29 C27 C26 C24 3(3) . . . . ? C27 C29 C28 C25 -1(3) . . . . ? N4 C29 C28 C25 -178.4(15) . . . . ? C27 C29 C28 S1 171.7(13) . . . . ? N4 C29 C28 S1 -6(2) . . . . ? C24 C25 C28 C29 1(3) . . . . ? C24 C25 C28 S1 -172.3(15) . . . . ? C30 S1 C28 C29 31.0(17) . . . . ? C30 S1 C28 C25 -155.9(14) . . . . ? C24 C23 C22 C21 177.8(13) . . . . ? C19 C21 C22 C23 -168(3) . . . . ? C20 C21 C22 C23 13(3) . . . . ? C20 C21 C19 C18 -3(4) . . . . ? C22 C21 C19 C18 178(2) . . . . ? C17 C18 C19 C21 -1(4) . . . . ? C34 C35 C33 C32 -2(3) . . . . ? C31 C32 C33 C35 0(3) . . . . ? C28 C25 C24 C26 1(3) . . . . ? C28 C25 C24 C23 -177.1(16) . . . . ? C27 C26 C24 C25 -3(3) . . . . ? C27 C26 C24 C23 174.9(17) . . . . ? C22 C23 C24 C25 -176(2) . . . . ? C22 C23 C24 C26 6(3) . . . . ? C19 C21 C20 C16 3(3) . . . . ? C22 C21 C20 C16 -177.1(19) . . . . ? C17 C16 C20 C21 -1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.212 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.221 data_071121c _database_code_depnum_ccdc_archive 'CCDC 673758' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C148 H124 Cd2 Cl4 N16 O22 S4' _chemical_formula_weight 2973.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 14.071(4) _cell_length_b 14.174(4) _cell_length_c 19.754(5) _cell_angle_alpha 97.391(4) _cell_angle_beta 103.966(4) _cell_angle_gamma 113.288(3) _cell_volume 3398.8(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.530 _exptl_absorpt_correction_type none _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17542 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.1170 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11636 _reflns_number_gt 5120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1320P)^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 SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11636 _refine_ls_number_parameters 759 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1809 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2603 _refine_ls_wR_factor_gt 0.1936 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 4.848 _refine_ls_shift/su_mean 0.124 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 C1 C 0.4338(6) 0.8433(6) 0.5762(4) 0.096(4) Uani 1 1 d G . . H1 H 0.4212 0.8905 0.6058 0.115 Uiso 1 1 calc R . . C2 C 0.3695(6) 0.8003(7) 0.5042(4) 0.118(5) Uani 1 1 d G . . H2 H 0.3137 0.8187 0.4857 0.141 Uiso 1 1 calc R . . C3 C 0.3883(6) 0.7297(7) 0.4600(3) 0.105(4) Uani 1 1 d G . . H3 H 0.3453 0.7009 0.4118 0.126 Uiso 1 1 calc R . . C4 C 0.4716(6) 0.7022(6) 0.4877(3) 0.082(3) Uani 1 1 d G . . H4 H 0.4842 0.6550 0.4581 0.098 Uiso 1 1 calc R . . C5 C 0.5360(5) 0.7452(5) 0.5597(3) 0.058(2) Uani 1 1 d G . . N1 N 0.5171(5) 0.8158(5) 0.6039(3) 0.068(2) Uani 1 1 d G . . C7 C 0.8740(11) 0.3555(9) 0.4411(8) 0.091(4) Uani 1 1 d . . . H7 H 0.9217 0.3374 0.4720 0.109 Uiso 1 1 calc R . . C8 C 0.6234(4) 0.7225(4) 0.5896(3) 0.052(2) Uani 1 1 d G . . N2 N 0.6806(4) 0.7729(4) 0.6620(3) 0.0468(17) Uani 1 1 d G . . C10 C 0.7693(4) 0.7569(4) 0.6971(2) 0.049(2) Uani 1 1 d G . . C11 C 0.8007(4) 0.6906(4) 0.6597(3) 0.053(2) Uani 1 1 d G . . H11 H 0.8600 0.6799 0.6831 0.064 Uiso 1 1 calc R . . C12 C 0.7435(5) 0.6403(4) 0.5872(3) 0.050(2) Uani 1 1 d G . . C13 C 0.6549(5) 0.6562(4) 0.5522(2) 0.063(3) Uani 1 1 d G . . H13 H 0.6166 0.6226 0.5037 0.075 Uiso 1 1 calc R . . C14 C 0.8463(10) 0.3135(9) 0.3739(7) 0.084(3) Uani 1 1 d . . . H14 H 0.8049 0.3369 0.3425 0.100 Uiso 1 1 calc R . . C15 C 0.8189(5) 0.8081(5) 0.7719(3) 0.058(2) Uani 1 1 d G . . N3 N 0.7678(5) 0.8606(5) 0.8018(3) 0.069(2) Uani 1 1 d G . . C17 C 0.8043(6) 0.9038(6) 0.8758(3) 0.093(4) Uani 1 1 d G . . H17 H 0.7701 0.9389 0.8958 0.112 Uiso 1 1 calc R . . C18 C 0.8918(7) 0.8945(7) 0.9199(3) 0.110(5) Uani 1 1 d G . . H18 H 0.9162 0.9233 0.9694 0.132 Uiso 1 1 calc R . . C19 C 0.9428(6) 0.8420(7) 0.8900(4) 0.104(4) Uani 1 1 d G . . H19 H 1.0014 0.8357 0.9195 0.125 Uiso 1 1 calc R . . C20 C 0.9064(5) 0.7988(6) 0.8160(4) 0.075(3) Uani 1 1 d G . . H20 H 0.9405 0.7637 0.7960 0.091 Uiso 1 1 calc R . . C84 C 0.9291(12) -0.1344(9) 0.1493(6) 0.101(4) Uani 1 1 d . . . H84A H 0.9945 -0.0824 0.1446 0.151 Uiso 1 1 calc R . . H84B H 0.8845 -0.1839 0.1035 0.151 Uiso 1 1 calc R . . H84C H 0.9481 -0.1715 0.1836 0.151 Uiso 1 1 calc R . . N7 N 0.5093(5) 0.7933(5) 0.7814(3) 0.068(2) Uani 1 1 d G . . C22 C 0.4829(6) 0.6889(4) 0.7847(4) 0.085(3) Uani 1 1 d G . . H22 H 0.5052 0.6484 0.7573 0.102 Uiso 1 1 calc R . . C23 C 0.4233(6) 0.6451(4) 0.8288(4) 0.087(4) Uani 1 1 d G . . H23 H 0.4056 0.5753 0.8310 0.105 Uiso 1 1 calc R . . C24 C 0.3899(6) 0.7056(5) 0.8697(4) 0.080(3) Uani 1 1 d G . . H24 H 0.3500 0.6763 0.8993 0.096 Uiso 1 1 calc R . . C25 C 0.4163(5) 0.8100(5) 0.8665(3) 0.069(3) Uani 1 1 d G . . H25 H 0.3940 0.8505 0.8939 0.083 Uiso 1 1 calc R . . C26 C 0.4760(5) 0.8538(3) 0.8224(3) 0.048(2) Uani 1 1 d G . . C27 C 0.3580(8) 1.4081(8) 0.9717(6) 0.064(3) Uani 1 1 d . . . H27 H 0.3537 1.4600 0.9485 0.076 Uiso 1 1 calc R . . C28 C 0.5051(4) 0.9591(3) 0.8156(3) 0.047(2) Uani 1 1 d G . . C29 C 0.4722(4) 1.0281(4) 0.8484(3) 0.050(2) Uani 1 1 d G . . H29 H 0.4244 1.0046 0.8746 0.060 Uiso 1 1 calc R . . C30 C 0.5108(4) 1.1322(4) 0.8422(3) 0.044(2) Uani 1 1 d G . . C31 C 0.5822(4) 1.1673(3) 0.8032(3) 0.048(2) Uani 1 1 d G . . H31 H 0.6080 1.2370 0.7990 0.058 Uiso 1 1 calc R . . C32 C 0.6151(4) 1.0983(4) 0.7703(3) 0.046(2) Uani 1 1 d G . . N6 N 0.5765(4) 0.9942(3) 0.7765(3) 0.0437(17) Uani 1 1 d G . . C34 C 0.8959(8) 0.2830(7) 0.8985(5) 0.063(3) Uani 1 1 d . . . H34A H 0.9103 0.2399 0.8638 0.076 Uiso 1 1 calc R . . H34B H 0.8236 0.2404 0.9005 0.076 Uiso 1 1 calc R . . C35 C 0.6913(4) 1.1264(4) 0.7316(3) 0.047(2) Uani 1 1 d G . . N5 N 0.7285(5) 1.0524(3) 0.7133(3) 0.060(2) Uani 1 1 d G . . C37 C 0.8095(5) 1.0775(5) 0.6807(4) 0.081(3) Uani 1 1 d G . . H37 H 0.8344 1.0280 0.6684 0.098 Uiso 1 1 calc R . . C38 C 0.8532(5) 1.1765(5) 0.6663(4) 0.074(3) Uani 1 1 d G . . H38 H 0.9073 1.1933 0.6445 0.089 Uiso 1 1 calc R . . C39 C 0.8159(5) 1.2505(4) 0.6846(3) 0.063(3) Uani 1 1 d G . . H39 H 0.8452 1.3168 0.6751 0.075 Uiso 1 1 calc R . . C40 C 0.7350(5) 1.2254(4) 0.7173(3) 0.061(3) Uani 1 1 d G . . H40 H 0.7101 1.2749 0.7295 0.073 Uiso 1 1 calc R . . C83 C 0.6741(8) 0.5964(8) 0.9714(6) 0.069(3) Uani 1 1 d . . . H83 H 0.6656 0.6449 0.9460 0.083 Uiso 1 1 calc R . . C41 C 0.4758(5) 1.2061(4) 0.8771(3) 0.049(2) Uani 1 1 d G . . C42 C 0.4470(5) 1.1911(4) 0.9388(3) 0.058(2) Uani 1 1 d G . . H42 H 0.4527 1.1370 0.9589 0.069 Uiso 1 1 calc R . . C43 C 0.4097(6) 1.2569(5) 0.9703(3) 0.066(3) Uani 1 1 d G . . H43 H 0.3904 1.2469 1.0116 0.079 Uiso 1 1 calc R . . C44 C 0.4011(5) 1.3378(4) 0.9402(3) 0.060(3) Uani 1 1 d G . . C45 C 0.4299(5) 1.3528(4) 0.8785(3) 0.060(2) Uani 1 1 d G . . H45 H 0.4242 1.4069 0.8583 0.072 Uiso 1 1 calc R . . C46 C 0.4673(5) 1.2870(5) 0.8469(3) 0.058(2) Uani 1 1 d G . . H46 H 0.4866 1.2970 0.8056 0.070 Uiso 1 1 calc R . . C47 C 0.9788(9) 0.3091(9) 0.9722(6) 0.085(3) Uani 1 1 d . . . H47A H 1.0478 0.3639 0.9746 0.127 Uiso 1 1 calc R . . H47B H 0.9870 0.2468 0.9796 0.127 Uiso 1 1 calc R . . H47C H 0.9536 0.3331 1.0089 0.127 Uiso 1 1 calc R . . C48 C 0.7782(6) 0.5677(5) 0.5480(3) 0.063(3) Uani 1 1 d G . . C49 C 0.7447(6) 0.5402(6) 0.4731(3) 0.078(3) Uani 1 1 d G . . H49 H 0.7021 0.5678 0.4471 0.094 Uiso 1 1 calc R . . C50 C 0.7750(7) 0.4715(6) 0.4370(3) 0.085(4) Uani 1 1 d G . . H50 H 0.7526 0.4531 0.3869 0.102 Uiso 1 1 calc R . . C51 C 0.8387(7) 0.4302(6) 0.4759(4) 0.078(3) Uani 1 1 d G . . C52 C 0.8722(6) 0.4577(6) 0.5508(4) 0.091(4) Uani 1 1 d G . . H52 H 0.9148 0.4301 0.5768 0.109 Uiso 1 1 calc R . . C53 C 0.8419(6) 0.5265(6) 0.5868(3) 0.083(3) Uani 1 1 d G . . H53 H 0.8643 0.5449 0.6369 0.099 Uiso 1 1 calc R . . N4 N 0.9094(7) -0.0341(6) 0.2520(4) 0.066(2) Uani 1 1 d . . . C55 C 0.9023(6) 0.0604(5) 0.2787(3) 0.062(3) Uani 1 1 d G . . C56 C 0.9611(5) 0.1150(5) 0.3503(3) 0.056(2) Uani 1 1 d G . . C57 C 0.9467(5) 0.2001(5) 0.3812(3) 0.062(3) Uani 1 1 d G . . H57 H 0.9860 0.2367 0.4291 0.075 Uiso 1 1 calc R . . C58 C 0.8736(6) 0.2306(5) 0.3405(3) 0.068(3) Uani 1 1 d G . . C59 C 0.8149(6) 0.1760(6) 0.2689(3) 0.077(3) Uani 1 1 d G . . H59 H 0.7660 0.1963 0.2416 0.092 Uiso 1 1 calc R . . C60 C 0.8292(6) 0.0908(5) 0.2380(3) 0.078(3) Uani 1 1 d G . . H60 H 0.7900 0.0543 0.1901 0.094 Uiso 1 1 calc R . . S1 S 1.0594(2) 0.0807(2) 0.39832(14) 0.0619(7) Uani 1 1 d . . . C62 C 0.9066(6) -0.0999(5) 0.3005(3) 0.059(3) Uani 1 1 d G . . C63 C 0.9744(5) -0.0546(4) 0.3715(4) 0.060(3) Uani 1 1 d G . . C64 C 0.9722(6) -0.1172(6) 0.4203(3) 0.077(3) Uani 1 1 d G . . H64 H 1.0177 -0.0869 0.4679 0.093 Uiso 1 1 calc R . . C65 C 0.9022(7) -0.2252(6) 0.3980(4) 0.088(4) Uani 1 1 d G . . H65 H 0.9007 -0.2671 0.4307 0.105 Uiso 1 1 calc R . . C66 C 0.8343(6) -0.2705(4) 0.3270(5) 0.094(4) Uani 1 1 d G . . H66 H 0.7874 -0.3428 0.3120 0.113 Uiso 1 1 calc R . . C67 C 0.8365(5) -0.2078(6) 0.2782(3) 0.079(3) Uani 1 1 d G . . H67 H 0.7911 -0.2382 0.2306 0.095 Uiso 1 1 calc R . . C68 C 0.8673(10) -0.0804(9) 0.1749(5) 0.081(3) Uani 1 1 d . . . H68A H 0.8701 -0.0249 0.1502 0.097 Uiso 1 1 calc R . . H68B H 0.7913 -0.1315 0.1620 0.097 Uiso 1 1 calc R . . C69 C 0.7618(5) 0.5522(4) 0.8865(3) 0.059(2) Uani 1 1 d G . . H69 H 0.7506 0.6028 0.8645 0.070 Uiso 1 1 calc R . . C70 C 0.7236(5) 0.5291(5) 0.9439(3) 0.061(3) Uani 1 1 d G . . C71 C 0.7404(5) 0.4535(5) 0.9768(3) 0.065(3) Uani 1 1 d G . . H71 H 0.7149 0.4381 1.0152 0.078 Uiso 1 1 calc R . . C72 C 0.7954(5) 0.4009(4) 0.9523(3) 0.059(3) Uani 1 1 d G . . H72 H 0.8067 0.3503 0.9742 0.071 Uiso 1 1 calc R . . C73 C 0.8336(5) 0.4240(4) 0.8948(3) 0.050(2) Uani 1 1 d G . . C74 C 0.8168(5) 0.4996(5) 0.8620(3) 0.056(2) Uani 1 1 d G . . S2 S 0.8457(2) 0.5160(2) 0.78195(14) 0.0707(8) Uani 1 1 d . . . C76 C 0.9639(5) 0.4986(5) 0.8012(4) 0.061(3) Uani 1 1 d G . . C77 C 1.0396(6) 0.5460(5) 0.7673(4) 0.086(3) Uani 1 1 d G . . H77 H 1.0317 0.5940 0.7411 0.103 Uiso 1 1 calc R . . C78 C 1.1271(6) 0.5217(6) 0.7724(4) 0.097(4) Uani 1 1 d G . . H78 H 1.1778 0.5534 0.7496 0.117 Uiso 1 1 calc R . . C79 C 1.1390(5) 0.4499(7) 0.8114(4) 0.089(4) Uani 1 1 d G . . H79 H 1.1975 0.4336 0.8148 0.106 Uiso 1 1 calc R . . C80 C 1.0632(6) 0.4024(5) 0.8454(4) 0.072(3) Uani 1 1 d G . . H80 H 1.0711 0.3544 0.8715 0.087 Uiso 1 1 calc R . . C81 C 0.9757(5) 0.4268(5) 0.8403(3) 0.059(2) Uani 1 1 d G . . N8 N 0.8953(6) 0.3746(6) 0.8723(4) 0.056(2) Uani 1 1 d . . . Cd1 Cd 0.63023(6) 0.88088(5) 0.72372(4) 0.0613(3) Uani 1 1 d . . . Cl1 Cl 0.4840(3) 0.5555(3) 0.30824(17) 0.0870(9) Uani 1 1 d D . . Cl2 Cl 0.2686(3) 0.9178(3) 0.98895(18) 0.0858(9) Uani 1 1 d D . . O1 O 0.5375(14) 0.5469(10) 0.2611(8) 0.198(7) Uani 1 1 d D . . O2 O 0.3960(14) 0.4583(12) 0.2834(13) 0.265(10) Uani 1 1 d D . . O3 O 0.534(2) 0.562(3) 0.3724(7) 0.40(2) Uani 1 1 d D . . O4 O 0.4429(10) 0.6311(9) 0.3003(6) 0.157(4) Uani 1 1 d D . . O5 O 0.2187(18) 0.8148(16) 0.9512(11) 0.285(9) Uiso 1 1 d D . . O6 O 0.2618(13) 0.9109(12) 1.0551(7) 0.186(5) Uani 1 1 d D . . O7 O 0.3759(10) 0.9694(10) 0.9922(7) 0.170(5) Uani 1 1 d D . . O8 O 0.2189(17) 0.9691(19) 0.9591(13) 0.355(16) Uani 1 1 d D . . O9 O 0.7081(6) 0.9563(5) 0.4925(3) 0.072(2) Uani 1 1 d D . . O10 O 0.799(8) 0.018(12) 0.959(10) 2.0(3) Uiso 1 1 d D . . O11 O 0.6781(18) 0.944(2) 0.3513(11) 0.071(6) Uani 0.50 1 d PD . . O12 O 0.6644(15) 0.9617(16) 0.3347(9) 0.040(4) Uani 0.50 1 d P . . H6W H 0.686(6) 0.905(5) 0.397(4) 0.080 Uiso 1 1 d D . . H5W H 0.608(3) 0.932(6) 0.340(5) 0.080 Uiso 1 1 d D . . H1W H 0.755(7) 1.015(2) 0.492(4) 0.080 Uiso 1 1 d D . . H2W H 0.703(7) 0.903(4) 0.460(3) 0.080 Uiso 1 1 d D . . H3W H 0.828(8) 0.078(6) 0.989(6) 0.080 Uiso 1 1 d D . . H4W H 0.842(7) -0.005(7) 0.955(5) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.084(9) 0.115(10) 0.089(9) 0.004(7) 0.012(7) 0.059(8) C2 0.098(10) 0.146(13) 0.107(11) 0.024(10) -0.006(9) 0.077(10) C3 0.097(10) 0.120(11) 0.095(10) 0.015(8) 0.007(8) 0.061(9) C4 0.082(8) 0.097(8) 0.064(7) 0.014(6) 0.007(6) 0.048(7) C5 0.063(6) 0.056(6) 0.058(6) 0.013(5) 0.021(5) 0.028(5) N1 0.070(5) 0.080(6) 0.065(5) 0.015(4) 0.014(4) 0.051(5) C7 0.113(10) 0.086(8) 0.102(10) 0.020(7) 0.056(8) 0.060(8) C8 0.064(6) 0.059(6) 0.048(6) 0.011(4) 0.028(5) 0.036(5) N2 0.054(4) 0.038(4) 0.060(5) 0.013(3) 0.027(4) 0.026(4) C10 0.057(6) 0.044(5) 0.056(6) 0.015(4) 0.023(5) 0.029(5) C11 0.061(6) 0.050(5) 0.057(6) 0.009(4) 0.025(5) 0.030(5) C12 0.057(6) 0.044(5) 0.058(6) 0.010(4) 0.028(5) 0.027(5) C13 0.073(7) 0.056(6) 0.059(6) 0.006(5) 0.019(5) 0.032(5) C14 0.106(9) 0.085(8) 0.095(9) 0.032(7) 0.055(8) 0.061(8) C15 0.066(6) 0.054(6) 0.056(6) 0.014(5) 0.018(5) 0.029(5) N3 0.077(6) 0.070(5) 0.062(5) -0.001(4) 0.025(5) 0.039(5) C17 0.092(9) 0.116(10) 0.056(7) -0.019(7) 0.004(7) 0.054(8) C18 0.125(12) 0.100(10) 0.064(8) -0.005(7) -0.004(8) 0.038(9) C19 0.124(11) 0.091(9) 0.072(9) 0.018(7) -0.012(8) 0.047(9) C20 0.088(8) 0.071(7) 0.075(8) 0.016(6) 0.012(6) 0.052(6) C84 0.154(12) 0.081(8) 0.091(9) 0.009(7) 0.040(8) 0.079(9) N7 0.071(6) 0.056(5) 0.082(6) 0.014(4) 0.030(5) 0.029(4) C22 0.093(9) 0.050(6) 0.126(10) 0.023(7) 0.040(8) 0.043(6) C23 0.091(9) 0.050(6) 0.126(10) 0.033(7) 0.036(8) 0.032(6) C24 0.101(9) 0.057(7) 0.093(8) 0.033(6) 0.047(7) 0.032(6) C25 0.085(8) 0.063(7) 0.072(7) 0.020(5) 0.037(6) 0.037(6) C26 0.050(5) 0.043(5) 0.059(6) 0.014(4) 0.019(5) 0.027(4) C27 0.069(7) 0.060(6) 0.075(7) 0.012(5) 0.034(6) 0.038(5) C28 0.059(6) 0.053(5) 0.043(5) 0.012(4) 0.021(4) 0.037(5) C29 0.057(6) 0.049(5) 0.052(5) 0.018(4) 0.026(5) 0.025(5) C30 0.045(5) 0.041(5) 0.048(5) 0.012(4) 0.014(4) 0.020(4) C31 0.058(6) 0.044(5) 0.051(5) 0.011(4) 0.027(5) 0.026(4) C32 0.043(5) 0.045(5) 0.047(5) 0.008(4) 0.015(4) 0.019(4) N6 0.045(4) 0.047(4) 0.042(4) 0.008(3) 0.015(3) 0.024(4) C34 0.077(7) 0.056(6) 0.065(7) 0.016(5) 0.021(6) 0.038(6) C35 0.045(5) 0.048(5) 0.053(5) 0.009(4) 0.018(4) 0.025(4) N5 0.068(5) 0.057(5) 0.068(5) 0.016(4) 0.034(4) 0.033(4) C37 0.085(8) 0.073(8) 0.104(9) 0.007(6) 0.063(7) 0.038(7) C38 0.073(7) 0.091(8) 0.080(7) 0.023(6) 0.043(6) 0.046(7) C39 0.064(6) 0.064(6) 0.070(7) 0.025(5) 0.038(6) 0.026(5) C40 0.065(6) 0.057(6) 0.067(6) 0.018(5) 0.032(5) 0.028(5) C83 0.062(7) 0.058(6) 0.092(8) 0.010(6) 0.032(6) 0.029(5) C41 0.054(5) 0.047(5) 0.054(6) 0.006(4) 0.024(5) 0.028(5) C42 0.075(7) 0.052(6) 0.054(6) 0.015(5) 0.028(5) 0.031(5) C43 0.093(8) 0.070(7) 0.058(6) 0.017(5) 0.041(6) 0.050(6) C44 0.056(6) 0.053(6) 0.071(7) 0.004(5) 0.026(5) 0.025(5) C45 0.070(6) 0.053(6) 0.069(7) 0.017(5) 0.034(5) 0.031(5) C46 0.067(6) 0.050(6) 0.073(7) 0.016(5) 0.036(5) 0.033(5) C47 0.086(8) 0.102(9) 0.067(8) 0.030(6) 0.012(6) 0.048(7) C48 0.073(7) 0.051(6) 0.075(7) 0.011(5) 0.039(6) 0.031(5) C49 0.122(10) 0.079(7) 0.074(8) 0.027(6) 0.052(7) 0.070(7) C50 0.133(11) 0.086(8) 0.065(7) 0.020(6) 0.049(7) 0.065(8) C51 0.108(9) 0.065(7) 0.091(9) 0.019(6) 0.051(7) 0.056(7) C52 0.126(10) 0.106(9) 0.075(8) 0.013(7) 0.041(8) 0.083(9) C53 0.101(9) 0.099(8) 0.085(8) 0.016(7) 0.040(7) 0.077(8) N4 0.091(6) 0.067(5) 0.053(5) 0.011(4) 0.027(5) 0.047(5) C55 0.070(7) 0.068(6) 0.063(6) 0.007(5) 0.028(5) 0.043(6) C56 0.070(6) 0.051(5) 0.054(6) 0.011(5) 0.024(5) 0.030(5) C57 0.069(7) 0.053(6) 0.069(6) 0.005(5) 0.028(5) 0.029(5) C58 0.086(7) 0.062(6) 0.079(7) 0.020(6) 0.035(6) 0.052(6) C59 0.097(8) 0.091(8) 0.056(7) 0.013(6) 0.015(6) 0.063(7) C60 0.097(8) 0.086(8) 0.061(7) 0.006(6) 0.011(6) 0.063(7) S1 0.0664(16) 0.0617(15) 0.0646(16) 0.0088(12) 0.0247(13) 0.0353(13) C62 0.065(6) 0.056(6) 0.062(7) 0.003(5) 0.022(5) 0.037(5) C63 0.068(7) 0.064(6) 0.064(7) 0.019(5) 0.028(6) 0.041(5) C64 0.098(9) 0.089(9) 0.071(7) 0.024(7) 0.043(7) 0.057(8) C65 0.106(10) 0.072(8) 0.101(10) 0.035(7) 0.057(8) 0.036(7) C66 0.092(9) 0.064(8) 0.114(11) 0.023(8) 0.047(9) 0.013(7) C67 0.086(8) 0.072(8) 0.074(8) 0.005(6) 0.028(7) 0.034(7) C68 0.109(9) 0.076(7) 0.060(7) 0.005(6) 0.014(6) 0.054(7) C69 0.079(7) 0.057(6) 0.057(6) 0.018(5) 0.028(5) 0.042(5) C70 0.071(7) 0.054(6) 0.060(6) 0.006(5) 0.017(5) 0.034(5) C71 0.081(7) 0.055(6) 0.072(7) 0.018(5) 0.047(6) 0.029(6) C72 0.081(7) 0.050(6) 0.055(6) 0.011(5) 0.024(5) 0.037(5) C73 0.060(6) 0.047(5) 0.057(6) 0.016(4) 0.022(5) 0.033(5) C74 0.063(6) 0.052(6) 0.060(6) 0.016(5) 0.024(5) 0.029(5) S2 0.090(2) 0.0820(19) 0.0683(18) 0.0302(14) 0.0369(16) 0.0560(17) C76 0.078(7) 0.061(6) 0.055(6) 0.025(5) 0.029(5) 0.036(6) C77 0.082(8) 0.094(9) 0.082(8) 0.028(7) 0.037(7) 0.032(7) C78 0.086(9) 0.127(11) 0.103(10) 0.044(8) 0.052(8) 0.055(9) C79 0.075(8) 0.130(11) 0.097(9) 0.054(8) 0.042(7) 0.064(8) C80 0.075(7) 0.077(7) 0.080(7) 0.015(6) 0.026(6) 0.051(6) C81 0.076(7) 0.050(6) 0.057(6) 0.011(5) 0.029(5) 0.030(5) N8 0.071(5) 0.051(5) 0.064(5) 0.017(4) 0.030(4) 0.037(4) Cd1 0.0693(5) 0.0568(5) 0.0690(5) 0.0038(3) 0.0282(4) 0.0389(4) Cl1 0.109(2) 0.088(2) 0.069(2) 0.0208(16) 0.0401(19) 0.042(2) Cl2 0.084(2) 0.111(2) 0.077(2) 0.0403(18) 0.0415(17) 0.043(2) O1 0.337(19) 0.175(11) 0.240(14) 0.103(10) 0.212(15) 0.184(13) O2 0.202(16) 0.129(11) 0.48(3) 0.117(15) 0.169(19) 0.036(11) O3 0.57(4) 0.79(5) 0.079(9) 0.011(17) 0.017(15) 0.61(4) O4 0.176(11) 0.158(10) 0.173(10) 0.041(8) 0.039(8) 0.121(9) O6 0.220(15) 0.225(14) 0.137(10) 0.086(10) 0.105(10) 0.081(12) O7 0.131(10) 0.183(11) 0.224(13) 0.097(10) 0.108(10) 0.053(9) O8 0.25(2) 0.41(3) 0.35(3) 0.27(3) -0.032(19) 0.11(2) O9 0.094(6) 0.077(5) 0.038(4) 0.014(3) 0.010(4) 0.039(5) O11 0.106(12) 0.156(15) 0.015(10) 0.090(9) 0.019(8) 0.099(10) O12 0.060(9) 0.093(11) 0.000(8) 0.052(7) -0.003(6) 0.061(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.3900 . ? C1 N1 1.3900 . ? C1 H1 0.9300 . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 N1 1.3900 . ? C5 C8 1.406(6) . ? N1 Cd1 2.333(5) . ? C7 C14 1.278(15) . ? C7 C51 1.495(11) . ? C7 H7 0.9300 . ? C8 N2 1.3900 . ? C8 C13 1.3900 . ? N2 C10 1.3900 . ? N2 Cd1 2.265(3) . ? C10 C11 1.3900 . ? C10 C15 1.424(6) . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 C48 1.508(5) . ? C13 H13 0.9300 . ? C14 C58 1.498(11) . ? C14 H14 0.9300 . ? C15 N3 1.3900 . ? C15 C20 1.3900 . ? N3 C17 1.3900 . ? N3 Cd1 2.307(5) . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C84 C68 1.495(14) . ? C84 H84A 0.9602 . ? C84 H84B 0.9602 . ? C84 H84C 0.9602 . ? N7 C22 1.3900 . ? N7 C26 1.3900 . ? N7 Cd1 2.317(5) . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 C28 1.417(5) . ? C27 C83 1.309(13) 2_677 ? C27 C44 1.499(9) . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 N6 1.3900 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 C41 1.482(5) . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 N6 1.3900 . ? C32 C35 1.424(5) . ? N6 Cd1 2.269(3) . ? C34 N8 1.460(11) . ? C34 C47 1.523(13) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N5 1.3900 . ? C35 C40 1.3900 . ? N5 C37 1.3900 . ? N5 Cd1 2.340(5) . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C83 C27 1.309(13) 2_677 ? C83 C70 1.504(10) . ? C83 H83 0.9300 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C42 H42 0.9300 . ? C43 C44 1.3900 . ? C43 H43 0.9300 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.3900 . ? C48 C53 1.3900 . ? C49 C50 1.3900 . ? C49 H49 0.9300 . ? C50 C51 1.3900 . ? C50 H50 0.9300 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? N4 C55 1.425(8) . ? N4 C62 1.416(9) . ? N4 C68 1.450(12) . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C56 S1 1.751(5) . ? C57 C58 1.3900 . ? C57 H57 0.9300 . ? C58 C59 1.3900 . ? C59 C60 1.3900 . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? S1 C63 1.734(6) . ? C62 C63 1.3900 . ? C62 C67 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C64 H64 0.9300 . ? C65 C66 1.3900 . ? C65 H65 0.9300 . ? C66 C67 1.3900 . ? C66 H66 0.9300 . ? C67 H67 0.9300 . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.3900 . ? C69 C74 1.3900 . ? C69 H69 0.9300 . ? C70 C71 1.3900 . ? C71 C72 1.3900 . ? C71 H71 0.9300 . ? C72 C73 1.3900 . ? C72 H72 0.9300 . ? C73 C74 1.3900 . ? C73 N8 1.426(8) . ? C74 S2 1.746(5) . ? S2 C76 1.737(6) . ? C76 C77 1.3900 . ? C76 C81 1.3900 . ? C77 C78 1.3900 . ? C77 H77 0.9300 . ? C78 C79 1.3900 . ? C78 H78 0.9300 . ? C79 C80 1.3900 . ? C79 H79 0.9300 . ? C80 C81 1.3900 . ? C80 H80 0.9300 . ? C81 N8 1.425(9) . ? Cl1 O3 1.265(13) . ? Cl1 O2 1.362(15) . ? Cl1 O1 1.352(11) . ? Cl1 O4 1.414(10) . ? Cl2 O8 1.294(16) . ? Cl2 O7 1.374(11) . ? Cl2 O5 1.36(2) . ? Cl2 O6 1.347(11) . ? Cl2 O10 1.93(12) 2_667 ? O6 O10 1.57(11) 2_667 ? O8 O10 1.7(2) 2_667 ? O9 H1W 0.84(2) . ? O10 O8 1.7(2) 2_667 ? O10 O6 1.57(11) 2_667 ? O10 Cl2 1.93(12) 2_667 ? O10 H3W 0.85(2) . ? O10 H4W 0.805(19) . ? O11 O12 0.484(13) . ? O11 H6W 1.12(4) . ? O11 H5W 0.90(2) . ? O12 H6W 1.58(4) . ? O12 H5W 0.79(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 120.0 . . ? C2 C1 H1 120.0 . . ? N1 C1 H1 120.0 . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 C8 122.1(4) . . ? N1 C5 C8 117.9(4) . . ? C5 N1 C1 120.0 . . ? C5 N1 Cd1 116.4(3) . . ? C1 N1 Cd1 123.6(3) . . ? C14 C7 C51 127.5(12) . . ? C14 C7 H7 116.2 . . ? C51 C7 H7 116.3 . . ? N2 C8 C13 120.0 . . ? N2 C8 C5 115.0(4) . . ? C13 C8 C5 125.0(4) . . ? C10 N2 C8 120.0 . . ? C10 N2 Cd1 119.6(3) . . ? C8 N2 Cd1 120.4(3) . . ? N2 C10 C11 120.0 . . ? N2 C10 C15 115.5(4) . . ? C11 C10 C15 124.4(4) . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 C48 119.1(4) . . ? C13 C12 C48 120.9(4) . . ? C12 C13 C8 120.0 . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C7 C14 C58 126.7(11) . . ? C7 C14 H14 116.7 . . ? C58 C14 H14 116.6 . . ? N3 C15 C20 120.0 . . ? N3 C15 C10 116.2(4) . . ? C20 C15 C10 123.5(4) . . ? C17 N3 C15 120.0 . . ? C17 N3 Cd1 122.4(3) . . ? C15 N3 Cd1 117.5(3) . . ? C18 C17 N3 120.0 . . ? C18 C17 H17 120.0 . . ? N3 C17 H17 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C15 120.0 . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C68 C84 H84A 109.4 . . ? C68 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C68 C84 H84C 109.5 . . ? H84A C84 H84C 109.4 . . ? H84B C84 H84C 109.4 . . ? C22 N7 C26 120.0 . . ? C22 N7 Cd1 122.3(3) . . ? C26 N7 Cd1 117.0(3) . . ? C23 C22 N7 120.0 . . ? C23 C22 H22 120.0 . . ? N7 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 N7 120.0 . . ? C25 C26 C28 123.4(4) . . ? N7 C26 C28 116.6(4) . . ? C83 C27 C44 126.5(9) 2_677 . ? C83 C27 H27 116.8 2_677 . ? C44 C27 H27 116.7 . . ? C29 C28 N6 120.0 . . ? C29 C28 C26 124.3(4) . . ? N6 C28 C26 115.5(4) . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 C41 120.2(4) . . ? C31 C30 C41 119.8(4) . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 N6 120.0 . . ? C31 C32 C35 125.0(4) . . ? N6 C32 C35 115.0(4) . . ? C32 N6 C28 120.0 . . ? C32 N6 Cd1 120.4(3) . . ? C28 N6 Cd1 119.6(3) . . ? N8 C34 C47 115.3(8) . . ? N8 C34 H34A 108.4 . . ? C47 C34 H34A 108.5 . . ? N8 C34 H34B 108.5 . . ? C47 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? N5 C35 C40 120.0 . . ? N5 C35 C32 116.7(4) . . ? C40 C35 C32 123.1(4) . . ? C37 N5 C35 120.0 . . ? C37 N5 Cd1 122.9(3) . . ? C35 N5 Cd1 116.4(3) . . ? N5 C37 C38 120.0 . . ? N5 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 H40 120.0 . . ? C35 C40 H40 120.0 . . ? C27 C83 C70 125.1(9) 2_677 . ? C27 C83 H83 117.4 2_677 . ? C70 C83 H83 117.4 . . ? C42 C41 C46 120.0 . . ? C42 C41 C30 119.3(4) . . ? C46 C41 C30 120.7(4) . . ? C43 C42 C41 120.0 . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 C27 118.7(6) . . ? C43 C44 C27 121.3(6) . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C34 C47 H47A 109.5 . . ? C34 C47 H47B 109.4 . . ? H47A C47 H47B 109.5 . . ? C34 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C53 120.0 . . ? C49 C48 C12 120.2(5) . . ? C53 C48 C12 119.8(5) . . ? C50 C49 C48 120.0 . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 120.0 . . ? C52 C51 C7 116.8(7) . . ? C50 C51 C7 123.2(7) . . ? C51 C52 C53 120.0 . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C52 C53 C48 120.0 . . ? C52 C53 H53 120.0 . . ? C48 C53 H53 120.0 . . ? C55 N4 C62 114.2(7) . . ? C55 N4 C68 118.6(7) . . ? C62 N4 C68 120.2(7) . . ? C56 C55 C60 120.0 . . ? C56 C55 N4 117.9(5) . . ? C60 C55 N4 121.6(5) . . ? C55 C56 C57 120.0 . . ? C55 C56 S1 118.9(3) . . ? C57 C56 S1 121.0(3) . . ? C58 C57 C56 120.0 . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 120.0 . . ? C57 C58 C14 121.6(6) . . ? C59 C58 C14 118.1(6) . . ? C60 C59 C58 120.0 . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? C63 S1 C56 94.7(3) . . ? C63 C62 C67 120.0 . . ? C63 C62 N4 118.9(6) . . ? C67 C62 N4 121.1(6) . . ? C62 C63 C64 120.0 . . ? C62 C63 S1 119.1(5) . . ? C64 C63 S1 120.9(5) . . ? C63 C64 C65 120.0 . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C67 C62 120.0 . . ? C66 C67 H67 120.0 . . ? C62 C67 H67 120.0 . . ? N4 C68 C84 113.2(9) . . ? N4 C68 H68A 108.9 . . ? C84 C68 H68A 109.0 . . ? N4 C68 H68B 108.9 . . ? C84 C68 H68B 108.9 . . ? H68A C68 H68B 107.8 . . ? C70 C69 C74 120.0 . . ? C70 C69 H69 120.0 . . ? C74 C69 H69 120.0 . . ? C69 C70 C71 120.0 . . ? C69 C70 C83 116.6(6) . . ? C71 C70 C83 123.2(6) . . ? C72 C71 C70 120.0 . . ? C72 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C73 C72 C71 120.0 . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 N8 119.9(5) . . ? C72 C73 N8 120.0(5) . . ? C73 C74 C69 120.0 . . ? C73 C74 S2 120.7(3) . . ? C69 C74 S2 118.6(3) . . ? C74 S2 C76 98.3(3) . . ? C77 C76 C81 120.0 . . ? C77 C76 S2 117.9(4) . . ? C81 C76 S2 121.4(4) . . ? C78 C77 C76 120.0 . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C77 C78 C79 120.0 . . ? C77 C78 H78 120.0 . . ? C79 C78 H78 120.0 . . ? C78 C79 C80 120.0 . . ? C78 C79 H79 120.0 . . ? C80 C79 H79 120.0 . . ? C81 C80 C79 120.0 . . ? C81 C80 H80 120.0 . . ? C79 C80 H80 120.0 . . ? C80 C81 C76 120.0 . . ? C80 C81 N8 120.0(5) . . ? C76 C81 N8 119.9(5) . . ? C81 N8 C73 120.9(6) . . ? C81 N8 C34 118.6(7) . . ? C73 N8 C34 118.7(7) . . ? N2 Cd1 N6 174.87(19) . . ? N2 Cd1 N3 70.45(19) . . ? N6 Cd1 N3 113.85(19) . . ? N2 Cd1 N7 112.9(2) . . ? N6 Cd1 N7 70.48(19) . . ? N3 Cd1 N7 90.3(2) . . ? N2 Cd1 N1 70.20(19) . . ? N6 Cd1 N1 105.67(19) . . ? N3 Cd1 N1 140.41(19) . . ? N7 Cd1 N1 100.9(2) . . ? N2 Cd1 N5 107.04(19) . . ? N6 Cd1 N5 69.88(18) . . ? N3 Cd1 N5 100.1(2) . . ? N7 Cd1 N5 139.91(19) . . ? N1 Cd1 N5 95.2(2) . . ? O3 Cl1 O2 107.0(18) . . ? O3 Cl1 O1 113.7(12) . . ? O2 Cl1 O1 100.0(11) . . ? O3 Cl1 O4 115.1(10) . . ? O2 Cl1 O4 106.5(10) . . ? O1 Cl1 O4 112.9(7) . . ? O8 Cl2 O7 107.0(12) . . ? O8 Cl2 O5 110.0(14) . . ? O7 Cl2 O5 113.2(12) . . ? O8 Cl2 O6 113.6(15) . . ? O7 Cl2 O6 110.3(9) . . ? O5 Cl2 O6 102.8(11) . . ? O8 Cl2 O10 60(7) . 2_667 ? O7 Cl2 O10 123(4) . 2_667 ? O5 Cl2 O10 123(5) . 2_667 ? O6 Cl2 O10 54(7) . 2_667 ? Cl2 O6 O10 82(9) . 2_667 ? Cl2 O8 O10 79(4) . 2_667 ? O8 O10 O6 85(6) 2_667 2_667 ? O8 O10 Cl2 41(3) 2_667 2_667 ? O6 O10 Cl2 44(2) 2_667 2_667 ? O8 O10 H3W 58(10) 2_667 . ? O6 O10 H3W 64(10) 2_667 . ? Cl2 O10 H3W 51(9) 2_667 . ? O8 O10 H4W 115(10) 2_667 . ? O6 O10 H4W 156(10) 2_667 . ? Cl2 O10 H4W 155(10) 2_667 . ? H3W O10 H4W 114(4) . . ? O12 O11 H6W 160(6) . . ? O12 O11 H5W 60(7) . . ? H6W O11 H5W 101(3) . . ? O11 O12 H6W 14(5) . . ? O11 O12 H5W 87(8) . . ? H6W O12 H5W 75(4) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.426 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.112 data_p1bar_1 _database_code_depnum_ccdc_archive 'CCDC 700924' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H58 Cl4 Cu N8 O8 S2' _chemical_formula_sum 'C75 H58 Cl4 Cu N8 O8 S2' _chemical_formula_weight 1468.75 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8465(4) _cell_length_b 14.0872(4) _cell_length_c 20.0791(9) _cell_angle_alpha 105.473(3) _cell_angle_beta 98.160(3) _cell_angle_gamma 112.461(2) _cell_volume 3355.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5959 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 20.04 _exptl_crystal_description flake _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1514 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7918 _exptl_absorpt_correction_T_max 0.9642 _exptl_absorpt_process_details SADBS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61783 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.70 _reflns_number_total 15439 _reflns_number_gt 7800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1175P)^2^+0.1662P] 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 15439 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1460 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2305 _refine_ls_wR_factor_gt 0.1896 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.38375(4) 0.12559(4) 0.22080(3) 0.05099(18) Uani 1 1 d . . . S1 S 0.97495(11) -0.34433(12) 0.71008(7) 0.0711(4) Uani 1 1 d . . . S2 S -0.40583(9) 0.56296(10) -0.09631(6) 0.0587(3) Uani 1 1 d . . . N1 N 0.2776(3) 0.0066(3) 0.2643(2) 0.0651(10) Uani 1 1 d . . . N2 N 0.4857(3) 0.0808(3) 0.27067(17) 0.0451(8) Uani 1 1 d . . . N3 N 0.5452(3) 0.2271(3) 0.20819(18) 0.0538(9) Uani 1 1 d . . . N4 N 0.3839(3) 0.2560(3) 0.30523(17) 0.0538(9) Uani 1 1 d . . . N5 N 0.2853(2) 0.1689(3) 0.17009(17) 0.0457(8) Uani 1 1 d . . . N6 N 0.3330(3) 0.0098(3) 0.11485(19) 0.0606(10) Uani 1 1 d . . . N7 N 1.1267(3) -0.3929(3) 0.6263(2) 0.0597(10) Uani 1 1 d . . . N8 N -0.5213(3) 0.4163(3) -0.24395(18) 0.0599(10) Uani 1 1 d . . . C1 C 0.1731(4) -0.0206(5) 0.2630(3) 0.0843(17) Uani 1 1 d . . . H1A H 0.1315 -0.0052 0.2306 0.101 Uiso 1 1 calc R . . C2 C 0.1259(4) -0.0697(6) 0.3070(3) 0.0898(18) Uani 1 1 d . . . H2A H 0.0531 -0.0881 0.3045 0.108 Uiso 1 1 calc R . . C3 C 0.1860(4) -0.0921(5) 0.3551(3) 0.0845(16) Uani 1 1 d . . . H3A H 0.1551 -0.1246 0.3864 0.101 Uiso 1 1 calc R . . C4 C 0.2930(4) -0.0659(4) 0.3569(3) 0.0655(12) Uani 1 1 d . . . H4A H 0.3353 -0.0810 0.3890 0.079 Uiso 1 1 calc R . . C5 C 0.3364(3) -0.0173(3) 0.3104(2) 0.0497(10) Uani 1 1 d . . . C6 C 0.4510(3) 0.0148(3) 0.3086(2) 0.0481(10) Uani 1 1 d . . . C7 C 0.5183(3) -0.0199(4) 0.3424(2) 0.0506(10) Uani 1 1 d . . . H7A H 0.4925 -0.0656 0.3682 0.061 Uiso 1 1 calc R . . C8 C 0.6254(3) 0.0140(3) 0.3377(2) 0.0483(10) Uani 1 1 d . . . C9 C 0.6600(3) 0.0844(3) 0.2990(2) 0.0483(10) Uani 1 1 d . . . H9A H 0.7308 0.1093 0.2950 0.058 Uiso 1 1 calc R . . C10 C 0.5891(3) 0.1164(3) 0.2670(2) 0.0443(9) Uani 1 1 d . . . C11 C 0.6211(3) 0.1948(3) 0.2279(2) 0.0453(9) Uani 1 1 d . . . C12 C 0.7217(3) 0.2372(4) 0.2162(2) 0.0555(11) Uani 1 1 d . . . H12A H 0.7722 0.2121 0.2287 0.067 Uiso 1 1 calc R . . C13 C 0.7473(4) 0.3179(4) 0.1856(2) 0.0598(11) Uani 1 1 d . . . H13A H 0.8152 0.3481 0.1777 0.072 Uiso 1 1 calc R . . C14 C 0.6712(4) 0.3522(4) 0.1675(3) 0.0666(13) Uani 1 1 d . . . H14A H 0.6872 0.4079 0.1484 0.080 Uiso 1 1 calc R . . C15 C 0.5704(4) 0.3036(4) 0.1778(3) 0.0668(13) Uani 1 1 d . . . H15A H 0.5176 0.3248 0.1630 0.080 Uiso 1 1 calc R . . C16 C 0.6983(3) -0.0218(4) 0.3729(2) 0.0512(10) Uani 1 1 d . . . C17 C 0.6855(4) -0.0489(4) 0.4333(2) 0.0599(12) Uani 1 1 d . . . H17A H 0.6305 -0.0422 0.4529 0.072 Uiso 1 1 calc R . . C18 C 0.7521(4) -0.0856(4) 0.4655(3) 0.0673(13) Uani 1 1 d . . . H18A H 0.7421 -0.1019 0.5067 0.081 Uiso 1 1 calc R . . C19 C 0.8351(3) -0.0987(4) 0.4364(2) 0.0571(11) Uani 1 1 d . . . C20 C 0.8481(3) -0.0706(4) 0.3770(2) 0.0590(12) Uani 1 1 d . . . H20A H 0.9035 -0.0770 0.3577 0.071 Uiso 1 1 calc R . . C21 C 0.7826(3) -0.0333(4) 0.3442(2) 0.0573(11) Uani 1 1 d . . . H21A H 0.7938 -0.0158 0.3036 0.069 Uiso 1 1 calc R . . C22 C 0.9049(4) -0.1409(4) 0.4673(3) 0.0670(13) Uani 1 1 d . . . H22A H 0.9588 -0.1446 0.4453 0.080 Uiso 1 1 calc R . . C23 C 0.9003(4) -0.1740(4) 0.5221(3) 0.0688(13) Uani 1 1 d . . . H23A H 0.8491 -0.1666 0.5458 0.083 Uiso 1 1 calc R . . C24 C 0.9673(4) -0.2217(4) 0.5507(3) 0.0638(12) Uani 1 1 d . . . C25 C 0.9442(4) -0.2587(4) 0.6071(2) 0.0645(12) Uani 1 1 d . . . H25A H 0.8917 -0.2474 0.6278 0.077 Uiso 1 1 calc R . . C26 C 0.9985(4) -0.3123(4) 0.6328(2) 0.0591(11) Uani 1 1 d . . . C27 C 1.0754(3) -0.3328(4) 0.6016(2) 0.0541(11) Uani 1 1 d . . . C28 C 1.1006(4) -0.2937(4) 0.5471(2) 0.0645(12) Uani 1 1 d . . . H28A H 1.1532 -0.3049 0.5264 0.077 Uiso 1 1 calc R . . C29 C 1.0481(4) -0.2377(4) 0.5228(3) 0.0670(13) Uani 1 1 d . . . H29A H 1.0677 -0.2103 0.4870 0.080 Uiso 1 1 calc R . . C30 C 0.9948(4) -0.4620(4) 0.6921(3) 0.0678(13) Uani 1 1 d . . . C31 C 0.9428(5) -0.5404(5) 0.7211(3) 0.0849(16) Uani 1 1 d . . . H31A H 0.8858 -0.5384 0.7402 0.102 Uiso 1 1 calc R . . C32 C 0.9755(5) -0.6206(5) 0.7217(3) 0.0897(17) Uani 1 1 d . . . H32A H 0.9482 -0.6664 0.7472 0.108 Uiso 1 1 calc R . . C33 C 1.0480(5) -0.6334(5) 0.6849(3) 0.0888(17) Uani 1 1 d . . . H33A H 1.0652 -0.6917 0.6824 0.107 Uiso 1 1 calc R . . C34 C 1.0961(4) -0.5610(4) 0.6515(3) 0.0722(14) Uani 1 1 d . . . H34A H 1.1446 -0.5718 0.6262 0.087 Uiso 1 1 calc R . . C35 C 1.0730(4) -0.4722(4) 0.6552(2) 0.0570(11) Uani 1 1 d . . . C36 C 1.2207(4) -0.3953(4) 0.6017(2) 0.0620(12) Uani 1 1 d . . . H36A H 1.2637 -0.4104 0.6364 0.074 Uiso 1 1 calc R . . H36B H 1.2653 -0.3228 0.6019 0.074 Uiso 1 1 calc R . . C37 C 1.1975(5) -0.4750(5) 0.5302(3) 0.0819(15) Uani 1 1 d . . . H37A H 1.2645 -0.4700 0.5199 0.123 Uiso 1 1 calc R . . H37B H 1.1578 -0.4595 0.4948 0.123 Uiso 1 1 calc R . . H37C H 1.1550 -0.5477 0.5293 0.123 Uiso 1 1 calc R . . C38 C 0.4302(4) 0.2880(4) 0.3754(3) 0.0720(14) Uani 1 1 d . . . H38A H 0.4708 0.2545 0.3907 0.086 Uiso 1 1 calc R . . C39 C 0.4200(5) 0.3681(5) 0.4254(3) 0.0844(16) Uani 1 1 d . . . H39A H 0.4511 0.3872 0.4740 0.101 Uiso 1 1 calc R . . C40 C 0.3633(4) 0.4199(5) 0.4028(3) 0.0792(15) Uani 1 1 d . . . H40A H 0.3569 0.4761 0.4359 0.095 Uiso 1 1 calc R . . C41 C 0.3155(4) 0.3879(4) 0.3301(2) 0.0668(13) Uani 1 1 d . . . H41A H 0.2777 0.4231 0.3136 0.080 Uiso 1 1 calc R . . C42 C 0.3246(3) 0.3036(4) 0.2830(2) 0.0499(10) Uani 1 1 d . . . C43 C 0.2694(3) 0.2548(3) 0.2047(2) 0.0444(9) Uani 1 1 d . . . C44 C 0.2044(3) 0.2897(4) 0.1693(2) 0.0490(10) Uani 1 1 d . . . H44A H 0.1960 0.3506 0.1942 0.059 Uiso 1 1 calc R . . C45 C 0.1509(3) 0.2338(4) 0.0959(2) 0.0485(10) Uani 1 1 d . . . C46 C 0.1681(3) 0.1441(4) 0.0612(2) 0.0514(10) Uani 1 1 d . . . H46A H 0.1335 0.1042 0.0127 0.062 Uiso 1 1 calc R . . C47 C 0.2368(3) 0.1144(4) 0.0991(2) 0.0477(10) Uani 1 1 d . . . C48 C 0.2626(3) 0.0230(4) 0.0676(2) 0.0530(10) Uani 1 1 d . . . C49 C 0.2212(4) -0.0441(4) -0.0032(3) 0.0744(14) Uani 1 1 d . . . H49A H 0.1711 -0.0359 -0.0345 0.089 Uiso 1 1 calc R . . C50 C 0.2551(5) -0.1231(5) -0.0270(3) 0.098(2) Uani 1 1 d . . . H50A H 0.2294 -0.1678 -0.0752 0.118 Uiso 1 1 calc R . . C51 C 0.3265(5) -0.1369(5) 0.0195(4) 0.101(2) Uani 1 1 d . . . H51A H 0.3499 -0.1906 0.0036 0.121 Uiso 1 1 calc R . . C52 C 0.3631(5) -0.0692(5) 0.0906(3) 0.0855(17) Uani 1 1 d . . . H52A H 0.4105 -0.0790 0.1228 0.103 Uiso 1 1 calc R . . C53 C 0.0791(3) 0.2680(4) 0.0572(2) 0.0533(11) Uani 1 1 d . . . C54 C 0.0330(4) 0.3311(4) 0.0929(2) 0.0643(13) Uani 1 1 d . . . H54A H 0.0472 0.3517 0.1426 0.077 Uiso 1 1 calc R . . C55 C -0.0318(4) 0.3631(5) 0.0572(3) 0.0710(14) Uani 1 1 d . . . H55A H -0.0615 0.4046 0.0832 0.085 Uiso 1 1 calc R . . C56 C -0.0557(4) 0.3366(4) -0.0166(3) 0.0638(12) Uani 1 1 d . . . C57 C -0.0104(4) 0.2741(4) -0.0530(3) 0.0705(14) Uani 1 1 d . . . H57A H -0.0256 0.2534 -0.1027 0.085 Uiso 1 1 calc R . . C58 C 0.0569(4) 0.2415(4) -0.0169(2) 0.0659(13) Uani 1 1 d . . . H58A H 0.0879 0.2013 -0.0427 0.079 Uiso 1 1 calc R . . C59 C -0.1309(4) 0.3713(4) -0.0520(3) 0.0713(14) Uani 1 1 d . . . H59A H -0.1502 0.4196 -0.0219 0.086 Uiso 1 1 calc R . . C60 C -0.1732(4) 0.3413(4) -0.1211(3) 0.0678(13) Uani 1 1 d . . . H60A H -0.1505 0.2973 -0.1519 0.081 Uiso 1 1 calc R . . C61 C -0.2542(4) 0.3717(4) -0.1542(2) 0.0577(11) Uani 1 1 d . . . C62 C -0.2836(3) 0.4478(4) -0.1153(2) 0.0583(11) Uani 1 1 d . . . H62A H -0.2458 0.4882 -0.0672 0.070 Uiso 1 1 calc R . . C63 C -0.3681(3) 0.4650(4) -0.1462(2) 0.0516(10) Uani 1 1 d . . . C64 C -0.4277(3) 0.4045(4) -0.2180(2) 0.0564(11) Uani 1 1 d . . . C65 C -0.3940(4) 0.3335(4) -0.2579(3) 0.0685(13) Uani 1 1 d . . . H65A H -0.4293 0.2948 -0.3065 0.082 Uiso 1 1 calc R . . C66 C -0.3077(4) 0.3197(4) -0.2259(3) 0.0668(13) Uani 1 1 d . . . H66A H -0.2848 0.2731 -0.2541 0.080 Uiso 1 1 calc R . . C67 C -0.5484(4) 0.4761(4) -0.1271(2) 0.0555(11) Uani 1 1 d . . . C68 C -0.6120(4) 0.4744(5) -0.0799(3) 0.0700(13) Uani 1 1 d . . . H68A H -0.5805 0.5176 -0.0316 0.084 Uiso 1 1 calc R . . C69 C -0.7215(5) 0.4088(5) -0.1045(3) 0.0807(16) Uani 1 1 d . . . H69A H -0.7652 0.4087 -0.0733 0.097 Uiso 1 1 calc R . . C70 C -0.7669(4) 0.3423(5) -0.1764(4) 0.0861(17) Uani 1 1 d . . . H70A H -0.8412 0.2966 -0.1932 0.103 Uiso 1 1 calc R . . C71 C -0.7035(4) 0.3436(4) -0.2230(3) 0.0751(14) Uani 1 1 d . . . H71A H -0.7352 0.2982 -0.2709 0.090 Uiso 1 1 calc R . . C72 C -0.5910(4) 0.4127(4) -0.1993(2) 0.0574(11) Uani 1 1 d . . . C73 C -0.5700(4) 0.3710(5) -0.3230(2) 0.0746(15) Uani 1 1 d . . . H73A H -0.6226 0.2950 -0.3370 0.090 Uiso 1 1 calc R . . H73B H -0.5135 0.3729 -0.3470 0.090 Uiso 1 1 calc R . . C74 C -0.6252(5) 0.4351(6) -0.3470(3) 0.0933(19) Uani 1 1 d . . . H74A H -0.6562 0.4033 -0.3981 0.140 Uiso 1 1 calc R . . H74B H -0.5729 0.5099 -0.3343 0.140 Uiso 1 1 calc R . . H74C H -0.6817 0.4327 -0.3238 0.140 Uiso 1 1 calc R . . Cl1 Cl 0.93140(11) 0.02681(13) 0.18534(7) 0.0746(4) Uani 1 1 d . . . Cl2 Cl 0.60532(15) 0.23789(15) 0.52898(8) 0.0928(5) Uani 1 1 d . . . O1 O 0.9482(6) 0.0046(7) 0.1198(3) 0.193(3) Uani 1 1 d . . . O2 O 0.8474(3) 0.0604(4) 0.1887(3) 0.1193(16) Uani 1 1 d . . . O3 O 0.9106(5) -0.0617(6) 0.2073(5) 0.194(3) Uani 1 1 d . . . O4 O 1.0313(5) 0.1092(5) 0.2325(3) 0.160(2) Uani 1 1 d . . . O5 O 0.6179(5) 0.2280(5) 0.4616(3) 0.1393(19) Uani 1 1 d . . . O6 O 0.7093(8) 0.2765(13) 0.5715(5) 0.333(7) Uani 1 1 d . . . O7 O 0.5658(7) 0.1556(9) 0.5488(6) 0.281(6) Uani 1 1 d . . . O8 O 0.5643(11) 0.3084(9) 0.5477(5) 0.297(7) Uani 1 1 d . . . C1S C 0.6267(6) 0.8162(8) 0.0981(5) 0.149(3) Uani 1 1 d . . . H1S1 H 0.6898 0.8871 0.1168 0.179 Uiso 1 1 calc R . . H1S2 H 0.6523 0.7609 0.0975 0.179 Uiso 1 1 calc R . . Cl1S Cl 0.5654(2) 0.7942(2) 0.01298(14) 0.1653(10) Uani 1 1 d . . . Cl2S Cl 0.5449(2) 0.8136(2) 0.15609(12) 0.1391(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0503(3) 0.0561(4) 0.0554(3) 0.0233(3) 0.0097(2) 0.0314(3) S1 0.0783(8) 0.0953(10) 0.0688(7) 0.0399(7) 0.0302(6) 0.0566(8) S2 0.0586(7) 0.0630(8) 0.0609(7) 0.0232(6) 0.0113(5) 0.0341(6) N1 0.047(2) 0.083(3) 0.089(3) 0.048(2) 0.0228(19) 0.038(2) N2 0.0429(18) 0.049(2) 0.0513(18) 0.0234(16) 0.0131(15) 0.0247(16) N3 0.054(2) 0.063(2) 0.063(2) 0.0339(19) 0.0155(17) 0.0355(19) N4 0.055(2) 0.069(2) 0.0502(19) 0.0251(18) 0.0097(16) 0.0389(19) N5 0.0411(18) 0.050(2) 0.0494(18) 0.0179(16) 0.0098(14) 0.0245(16) N6 0.065(2) 0.062(2) 0.062(2) 0.0180(19) 0.0089(18) 0.041(2) N7 0.055(2) 0.073(3) 0.068(2) 0.034(2) 0.0149(18) 0.040(2) N8 0.059(2) 0.076(3) 0.054(2) 0.0257(19) 0.0083(17) 0.040(2) C1 0.057(3) 0.108(5) 0.111(4) 0.055(4) 0.023(3) 0.049(3) C2 0.051(3) 0.120(5) 0.119(5) 0.054(4) 0.037(3) 0.046(3) C3 0.072(4) 0.092(4) 0.107(4) 0.048(4) 0.047(3) 0.037(3) C4 0.063(3) 0.079(4) 0.071(3) 0.038(3) 0.028(2) 0.036(3) C5 0.045(2) 0.050(3) 0.063(3) 0.024(2) 0.0160(19) 0.027(2) C6 0.046(2) 0.046(2) 0.058(2) 0.022(2) 0.0127(19) 0.025(2) C7 0.049(2) 0.055(3) 0.061(2) 0.031(2) 0.0159(19) 0.030(2) C8 0.045(2) 0.050(3) 0.052(2) 0.020(2) 0.0047(18) 0.025(2) C9 0.040(2) 0.059(3) 0.055(2) 0.027(2) 0.0101(18) 0.027(2) C10 0.043(2) 0.043(2) 0.052(2) 0.0191(19) 0.0113(17) 0.0230(19) C11 0.046(2) 0.047(2) 0.047(2) 0.0193(19) 0.0088(17) 0.024(2) C12 0.049(2) 0.063(3) 0.064(3) 0.029(2) 0.015(2) 0.029(2) C13 0.057(3) 0.059(3) 0.069(3) 0.031(2) 0.022(2) 0.024(2) C14 0.078(3) 0.068(3) 0.076(3) 0.046(3) 0.027(3) 0.039(3) C15 0.072(3) 0.077(3) 0.082(3) 0.048(3) 0.023(3) 0.048(3) C16 0.050(2) 0.057(3) 0.055(2) 0.025(2) 0.0084(19) 0.030(2) C17 0.056(3) 0.072(3) 0.069(3) 0.036(2) 0.018(2) 0.039(2) C18 0.070(3) 0.088(4) 0.064(3) 0.044(3) 0.016(2) 0.044(3) C19 0.050(2) 0.062(3) 0.062(3) 0.029(2) 0.003(2) 0.027(2) C20 0.052(3) 0.078(3) 0.068(3) 0.035(3) 0.021(2) 0.042(2) C21 0.054(3) 0.065(3) 0.066(3) 0.033(2) 0.016(2) 0.034(2) C22 0.058(3) 0.079(4) 0.073(3) 0.034(3) 0.006(2) 0.039(3) C23 0.069(3) 0.067(3) 0.072(3) 0.030(3) 0.003(2) 0.034(3) C24 0.058(3) 0.064(3) 0.069(3) 0.028(2) 0.003(2) 0.029(2) C25 0.061(3) 0.076(3) 0.066(3) 0.028(3) 0.009(2) 0.040(3) C26 0.055(3) 0.070(3) 0.062(3) 0.027(2) 0.014(2) 0.036(2) C27 0.050(2) 0.058(3) 0.055(2) 0.026(2) 0.0042(19) 0.023(2) C28 0.056(3) 0.082(4) 0.066(3) 0.032(3) 0.014(2) 0.037(3) C29 0.063(3) 0.077(3) 0.077(3) 0.047(3) 0.016(2) 0.034(3) C30 0.066(3) 0.079(4) 0.062(3) 0.034(3) 0.012(2) 0.032(3) C31 0.085(4) 0.089(4) 0.087(4) 0.045(3) 0.039(3) 0.030(3) C32 0.115(5) 0.077(4) 0.105(4) 0.054(4) 0.055(4) 0.047(4) C33 0.115(5) 0.075(4) 0.095(4) 0.047(3) 0.023(4) 0.050(4) C34 0.080(3) 0.077(4) 0.075(3) 0.033(3) 0.022(3) 0.045(3) C35 0.059(3) 0.065(3) 0.056(2) 0.028(2) 0.012(2) 0.032(2) C36 0.059(3) 0.072(3) 0.069(3) 0.028(3) 0.020(2) 0.038(3) C37 0.088(4) 0.078(4) 0.090(4) 0.033(3) 0.039(3) 0.040(3) C38 0.074(3) 0.081(4) 0.065(3) 0.027(3) 0.001(2) 0.044(3) C39 0.088(4) 0.099(4) 0.058(3) 0.021(3) -0.001(3) 0.044(4) C40 0.077(3) 0.095(4) 0.062(3) 0.009(3) 0.014(3) 0.047(3) C41 0.063(3) 0.082(4) 0.063(3) 0.019(3) 0.009(2) 0.047(3) C42 0.045(2) 0.057(3) 0.053(2) 0.021(2) 0.0088(18) 0.029(2) C43 0.041(2) 0.050(3) 0.051(2) 0.0237(19) 0.0167(17) 0.0238(19) C44 0.047(2) 0.054(3) 0.056(2) 0.021(2) 0.0148(19) 0.029(2) C45 0.039(2) 0.057(3) 0.057(2) 0.030(2) 0.0114(18) 0.025(2) C46 0.052(2) 0.060(3) 0.047(2) 0.020(2) 0.0093(18) 0.030(2) C47 0.041(2) 0.058(3) 0.048(2) 0.020(2) 0.0106(17) 0.026(2) C48 0.055(3) 0.050(3) 0.057(2) 0.019(2) 0.010(2) 0.028(2) C49 0.089(4) 0.079(4) 0.054(3) 0.015(3) 0.005(3) 0.046(3) C50 0.111(5) 0.092(5) 0.079(4) -0.003(3) 0.012(3) 0.060(4) C51 0.118(5) 0.096(5) 0.102(5) 0.010(4) 0.019(4) 0.081(4) C52 0.090(4) 0.084(4) 0.092(4) 0.020(3) 0.005(3) 0.063(3) C53 0.051(2) 0.060(3) 0.061(3) 0.031(2) 0.012(2) 0.031(2) C54 0.071(3) 0.082(4) 0.061(3) 0.032(3) 0.017(2) 0.052(3) C55 0.080(3) 0.099(4) 0.064(3) 0.032(3) 0.020(2) 0.066(3) C56 0.061(3) 0.079(3) 0.078(3) 0.041(3) 0.021(2) 0.047(3) C57 0.077(3) 0.095(4) 0.064(3) 0.041(3) 0.017(2) 0.055(3) C58 0.071(3) 0.096(4) 0.061(3) 0.038(3) 0.023(2) 0.058(3) C59 0.080(3) 0.083(4) 0.072(3) 0.034(3) 0.012(3) 0.056(3) C60 0.069(3) 0.084(4) 0.074(3) 0.038(3) 0.018(2) 0.051(3) C61 0.059(3) 0.069(3) 0.062(3) 0.032(2) 0.017(2) 0.040(2) C62 0.056(3) 0.072(3) 0.057(2) 0.030(2) 0.008(2) 0.035(2) C63 0.052(2) 0.052(3) 0.058(2) 0.025(2) 0.013(2) 0.028(2) C64 0.055(3) 0.061(3) 0.062(3) 0.028(2) 0.008(2) 0.032(2) C65 0.076(3) 0.078(4) 0.056(3) 0.018(2) 0.007(2) 0.047(3) C66 0.070(3) 0.072(3) 0.074(3) 0.027(3) 0.019(3) 0.045(3) C67 0.059(3) 0.061(3) 0.065(3) 0.035(2) 0.017(2) 0.036(2) C68 0.075(3) 0.080(4) 0.081(3) 0.047(3) 0.024(3) 0.047(3) C69 0.075(4) 0.104(5) 0.101(4) 0.070(4) 0.043(3) 0.047(4) C70 0.052(3) 0.092(4) 0.118(5) 0.058(4) 0.019(3) 0.023(3) C71 0.061(3) 0.074(4) 0.086(4) 0.030(3) 0.008(3) 0.029(3) C72 0.059(3) 0.060(3) 0.065(3) 0.030(2) 0.007(2) 0.035(2) C73 0.073(3) 0.100(4) 0.054(3) 0.025(3) 0.003(2) 0.047(3) C74 0.086(4) 0.137(5) 0.079(4) 0.056(4) 0.008(3) 0.064(4) Cl1 0.0671(8) 0.0986(11) 0.0681(8) 0.0340(7) 0.0164(6) 0.0441(8) Cl2 0.1271(13) 0.1110(13) 0.0829(9) 0.0631(9) 0.0491(9) 0.0686(11) O1 0.265(8) 0.313(9) 0.099(4) 0.072(5) 0.073(5) 0.218(8) O2 0.091(3) 0.126(4) 0.156(4) 0.038(3) 0.024(3) 0.074(3) O3 0.144(5) 0.201(6) 0.363(10) 0.216(7) 0.120(6) 0.105(5) O4 0.127(4) 0.137(5) 0.166(5) -0.009(4) -0.024(4) 0.073(4) O5 0.156(5) 0.169(5) 0.102(3) 0.061(3) 0.063(3) 0.063(4) O6 0.205(9) 0.491(19) 0.199(8) 0.160(11) -0.039(7) 0.056(10) O7 0.213(8) 0.379(13) 0.487(15) 0.391(13) 0.205(9) 0.171(9) O8 0.58(2) 0.367(13) 0.196(7) 0.145(8) 0.184(10) 0.410(15) C1S 0.086(5) 0.165(8) 0.198(9) 0.081(7) 0.009(5) 0.057(5) Cl1S 0.189(2) 0.189(3) 0.1371(19) 0.0513(18) 0.0712(18) 0.097(2) Cl2S 0.177(2) 0.1559(19) 0.1447(17) 0.0840(16) 0.0664(16) 0.1050(17) _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 1.959(3) . ? Cu1 N2 2.002(3) . ? Cu1 N6 2.128(4) . ? Cu1 N4 2.141(3) . ? Cu1 N1 2.234(4) . ? Cu1 N3 2.240(4) . ? S1 C30 1.736(5) . ? S1 C26 1.767(5) . ? S2 C63 1.773(4) . ? S2 C67 1.783(5) . ? N1 C5 1.339(5) . ? N1 C1 1.343(6) . ? N2 C10 1.345(5) . ? N2 C6 1.349(5) . ? N3 C15 1.334(5) . ? N3 C11 1.346(5) . ? N4 C38 1.336(5) . ? N4 C42 1.341(5) . ? N5 C43 1.339(5) . ? N5 C47 1.350(5) . ? N6 C52 1.331(6) . ? N6 C48 1.362(5) . ? N7 C35 1.403(6) . ? N7 C27 1.432(5) . ? N7 C36 1.465(6) . ? N8 C72 1.404(6) . ? N8 C64 1.413(5) . ? N8 C73 1.486(5) . ? C1 C2 1.354(8) . ? C2 C3 1.364(8) . ? C3 C4 1.375(7) . ? C4 C5 1.374(6) . ? C5 C6 1.484(5) . ? C6 C7 1.383(5) . ? C7 C8 1.400(6) . ? C8 C9 1.403(6) . ? C8 C16 1.466(5) . ? C9 C10 1.376(5) . ? C10 C11 1.490(5) . ? C11 C12 1.373(6) . ? C12 C13 1.386(6) . ? C13 C14 1.361(6) . ? C14 C15 1.373(7) . ? C16 C17 1.379(6) . ? C16 C21 1.417(6) . ? C17 C18 1.382(6) . ? C18 C19 1.410(6) . ? C19 C20 1.368(6) . ? C19 C22 1.462(5) . ? C20 C21 1.383(5) . ? C22 C23 1.306(6) . ? C23 C24 1.473(6) . ? C24 C29 1.385(7) . ? C24 C25 1.397(7) . ? C25 C26 1.389(6) . ? C26 C27 1.393(6) . ? C27 C28 1.382(6) . ? C28 C29 1.390(6) . ? C30 C31 1.391(7) . ? C30 C35 1.425(7) . ? C31 C32 1.371(8) . ? C32 C33 1.365(8) . ? C33 C34 1.381(7) . ? C34 C35 1.392(6) . ? C36 C37 1.469(7) . ? C38 C39 1.363(7) . ? C39 C40 1.366(7) . ? C40 C41 1.385(6) . ? C41 C42 1.368(6) . ? C42 C43 1.486(5) . ? C43 C44 1.378(5) . ? C44 C45 1.402(6) . ? C45 C46 1.394(6) . ? C45 C53 1.473(5) . ? C46 C47 1.389(5) . ? C47 C48 1.473(6) . ? C48 C49 1.372(6) . ? C49 C50 1.366(7) . ? C50 C51 1.368(8) . ? C51 C52 1.380(8) . ? C53 C54 1.391(6) . ? C53 C58 1.391(6) . ? C54 C55 1.351(6) . ? C55 C56 1.383(6) . ? C56 C57 1.383(6) . ? C56 C59 1.480(6) . ? C57 C58 1.384(6) . ? C59 C60 1.309(6) . ? C60 C61 1.482(6) . ? C61 C66 1.369(6) . ? C61 C62 1.379(6) . ? C62 C63 1.380(5) . ? C63 C64 1.397(6) . ? C64 C65 1.378(6) . ? C65 C66 1.380(6) . ? C67 C68 1.382(7) . ? C67 C72 1.382(6) . ? C68 C69 1.367(7) . ? C69 C70 1.389(8) . ? C70 C71 1.369(8) . ? C71 C72 1.409(6) . ? C73 C74 1.512(7) . ? Cl1 O1 1.344(5) . ? Cl1 O3 1.373(5) . ? Cl1 O4 1.404(5) . ? Cl1 O2 1.416(4) . ? Cl2 O7 1.275(6) . ? Cl2 O8 1.321(7) . ? Cl2 O5 1.365(5) . ? Cl2 O6 1.379(9) . ? C1S Cl1S 1.687(9) . ? C1S Cl2S 1.733(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 N2 178.68(13) . . ? N5 Cu1 N6 78.47(13) . . ? N2 Cu1 N6 100.54(13) . . ? N5 Cu1 N4 77.62(12) . . ? N2 Cu1 N4 103.41(12) . . ? N6 Cu1 N4 155.93(12) . . ? N5 Cu1 N1 104.28(13) . . ? N2 Cu1 N1 76.62(13) . . ? N6 Cu1 N1 94.63(16) . . ? N4 Cu1 N1 88.62(15) . . ? N5 Cu1 N3 103.02(13) . . ? N2 Cu1 N3 76.11(12) . . ? N6 Cu1 N3 92.86(14) . . ? N4 Cu1 N3 95.14(14) . . ? N1 Cu1 N3 152.61(12) . . ? C30 S1 C26 99.5(2) . . ? C63 S2 C67 95.6(2) . . ? C5 N1 C1 118.3(4) . . ? C5 N1 Cu1 111.5(3) . . ? C1 N1 Cu1 128.2(3) . . ? C10 N2 C6 119.4(3) . . ? C10 N2 Cu1 120.6(3) . . ? C6 N2 Cu1 120.0(2) . . ? C15 N3 C11 118.4(4) . . ? C15 N3 Cu1 128.9(3) . . ? C11 N3 Cu1 112.3(3) . . ? C38 N4 C42 119.0(4) . . ? C38 N4 Cu1 127.0(3) . . ? C42 N4 Cu1 113.9(3) . . ? C43 N5 C47 119.9(3) . . ? C43 N5 Cu1 120.5(3) . . ? C47 N5 Cu1 119.6(3) . . ? C52 N6 C48 118.4(4) . . ? C52 N6 Cu1 128.2(3) . . ? C48 N6 Cu1 113.3(3) . . ? C35 N7 C27 121.2(3) . . ? C35 N7 C36 118.2(4) . . ? C27 N7 C36 118.1(4) . . ? C72 N8 C64 115.6(3) . . ? C72 N8 C73 118.3(4) . . ? C64 N8 C73 117.3(4) . . ? N1 C1 C2 122.4(5) . . ? C1 C2 C3 119.4(5) . . ? C2 C3 C4 119.1(5) . . ? C5 C4 C3 119.0(5) . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 115.4(4) . . ? C4 C5 C6 122.9(4) . . ? N2 C6 C7 121.7(4) . . ? N2 C6 C5 114.7(3) . . ? C7 C6 C5 123.6(4) . . ? C6 C7 C8 119.8(4) . . ? C7 C8 C9 117.4(3) . . ? C7 C8 C16 120.8(4) . . ? C9 C8 C16 121.8(4) . . ? C10 C9 C8 120.0(4) . . ? N2 C10 C9 121.8(4) . . ? N2 C10 C11 115.0(3) . . ? C9 C10 C11 123.2(3) . . ? N3 C11 C12 121.5(4) . . ? N3 C11 C10 114.6(3) . . ? C12 C11 C10 123.8(3) . . ? C11 C12 C13 119.4(4) . . ? C14 C13 C12 118.8(4) . . ? C13 C14 C15 119.2(4) . . ? N3 C15 C14 122.6(4) . . ? C17 C16 C21 117.6(4) . . ? C17 C16 C8 121.7(4) . . ? C21 C16 C8 120.6(4) . . ? C16 C17 C18 121.9(4) . . ? C17 C18 C19 120.6(4) . . ? C20 C19 C18 117.2(4) . . ? C20 C19 C22 120.4(4) . . ? C18 C19 C22 122.4(4) . . ? C19 C20 C21 123.0(4) . . ? C20 C21 C16 119.6(4) . . ? C23 C22 C19 127.5(5) . . ? C22 C23 C24 127.2(5) . . ? C29 C24 C25 117.5(4) . . ? C29 C24 C23 124.4(5) . . ? C25 C24 C23 118.0(4) . . ? C26 C25 C24 120.9(4) . . ? C25 C26 C27 120.8(4) . . ? C25 C26 S1 118.3(3) . . ? C27 C26 S1 120.8(3) . . ? C28 C27 C26 118.4(4) . . ? C28 C27 N7 121.5(4) . . ? C26 C27 N7 120.1(4) . . ? C27 C28 C29 120.5(4) . . ? C24 C29 C28 121.7(4) . . ? C31 C30 C35 120.3(5) . . ? C31 C30 S1 119.1(4) . . ? C35 C30 S1 120.3(4) . . ? C32 C31 C30 119.9(5) . . ? C33 C32 C31 120.1(5) . . ? C32 C33 C34 121.0(5) . . ? C33 C34 C35 120.8(5) . . ? C34 C35 N7 122.0(4) . . ? C34 C35 C30 117.3(5) . . ? N7 C35 C30 120.6(4) . . ? N7 C36 C37 116.6(4) . . ? N4 C38 C39 122.2(4) . . ? C38 C39 C40 119.0(5) . . ? C39 C40 C41 119.3(5) . . ? C42 C41 C40 118.9(4) . . ? N4 C42 C41 121.5(4) . . ? N4 C42 C43 114.2(3) . . ? C41 C42 C43 124.3(4) . . ? N5 C43 C44 121.4(4) . . ? N5 C43 C42 113.7(3) . . ? C44 C43 C42 124.9(4) . . ? C43 C44 C45 120.4(4) . . ? C46 C45 C44 117.1(3) . . ? C46 C45 C53 121.5(4) . . ? C44 C45 C53 121.4(4) . . ? C47 C46 C45 120.1(4) . . ? N5 C47 C46 121.1(4) . . ? N5 C47 C48 114.3(3) . . ? C46 C47 C48 124.6(4) . . ? N6 C48 C49 121.6(4) . . ? N6 C48 C47 114.3(4) . . ? C49 C48 C47 124.1(4) . . ? C50 C49 C48 118.7(5) . . ? C49 C50 C51 120.5(5) . . ? C50 C51 C52 118.3(5) . . ? N6 C52 C51 122.4(5) . . ? C54 C53 C58 116.7(4) . . ? C54 C53 C45 121.9(4) . . ? C58 C53 C45 121.4(4) . . ? C55 C54 C53 121.6(4) . . ? C54 C55 C56 122.5(4) . . ? C57 C56 C55 116.6(4) . . ? C57 C56 C59 124.1(4) . . ? C55 C56 C59 119.2(4) . . ? C56 C57 C58 121.4(4) . . ? C57 C58 C53 121.1(4) . . ? C60 C59 C56 127.0(5) . . ? C59 C60 C61 125.3(5) . . ? C66 C61 C62 117.0(4) . . ? C66 C61 C60 120.1(4) . . ? C62 C61 C60 122.8(4) . . ? C61 C62 C63 121.2(4) . . ? C62 C63 C64 120.9(4) . . ? C62 C63 S2 121.3(3) . . ? C64 C63 S2 117.8(3) . . ? C65 C64 C63 117.7(4) . . ? C65 C64 N8 124.2(4) . . ? C63 C64 N8 118.1(4) . . ? C64 C65 C66 120.0(4) . . ? C61 C66 C65 122.8(4) . . ? C68 C67 C72 122.4(4) . . ? C68 C67 S2 120.4(4) . . ? C72 C67 S2 117.2(3) . . ? C69 C68 C67 119.8(5) . . ? C68 C69 C70 119.4(5) . . ? C71 C70 C69 120.6(5) . . ? C70 C71 C72 120.9(5) . . ? C67 C72 N8 119.4(4) . . ? C67 C72 C71 116.8(5) . . ? N8 C72 C71 123.7(4) . . ? N8 C73 C74 111.7(4) . . ? O1 Cl1 O3 110.6(5) . . ? O1 Cl1 O4 105.8(5) . . ? O3 Cl1 O4 105.4(4) . . ? O1 Cl1 O2 112.8(3) . . ? O3 Cl1 O2 110.6(3) . . ? O4 Cl1 O2 111.4(3) . . ? O7 Cl2 O8 113.2(7) . . ? O7 Cl2 O5 122.8(6) . . ? O8 Cl2 O5 109.1(4) . . ? O7 Cl2 O6 94.4(7) . . ? O8 Cl2 O6 111.7(9) . . ? O5 Cl2 O6 103.9(6) . . ? Cl1S C1S Cl2S 114.6(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.819 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.075 # Attachment 'ldm2.cif' data_p1bar_2 _database_code_depnum_ccdc_archive 'CCDC 700925' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H58 Cl2 Co N8 O8 S2' _chemical_formula_sum 'C74 H58 Cl2 Co N8 O8 S2' _chemical_formula_weight 1381.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 11.0672(7) _cell_length_b 15.9039(9) _cell_length_c 19.6022(12) _cell_angle_alpha 105.422(4) _cell_angle_beta 100.550(4) _cell_angle_gamma 94.827(4) _cell_volume 3237.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4741 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description flake _exptl_crystal_colour red _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1430 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8173 _exptl_absorpt_correction_T_max 0.9765 _exptl_absorpt_process_details SADBS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59464 _diffrn_reflns_av_R_equivalents 0.1004 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.55 _reflns_number_total 14843 _reflns_number_gt 6186 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1068P)^2^+0.9281P] 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 14843 _refine_ls_number_parameters 856 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1990 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.2446 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.05472(6) 0.25132(4) 0.25886(3) 0.0547(2) Uani 1 1 d . . . N1 N 1.2394(4) 0.3031(3) 0.2842(2) 0.0622(11) Uani 1 1 d . . . N2 N 1.0954(3) 0.2099(2) 0.16728(19) 0.0521(9) Uani 1 1 d . . . N3 N 0.8856(3) 0.1827(2) 0.19919(19) 0.0543(10) Uani 1 1 d . . . N4 N 1.1126(3) 0.1566(2) 0.31017(19) 0.0580(10) Uani 1 1 d . . . N5 N 1.0060(3) 0.2927(2) 0.3491(2) 0.0544(10) Uani 1 1 d . . . N6 N 0.9785(4) 0.3643(3) 0.2451(2) 0.0609(10) Uani 1 1 d . . . N7 N 1.3251(4) -0.1783(3) -0.5815(2) 0.0681(12) Uani 1 1 d . . . N8 N 0.5375(6) 0.6553(5) 1.0270(3) 0.129(2) Uani 1 1 d . . . S1 S 1.05534(15) -0.13160(11) -0.58321(8) 0.0844(5) Uani 1 1 d . . . S2 S 0.8162(2) 0.64361(17) 1.04491(12) 0.1404(9) Uani 1 1 d . . . C1 C 1.3094(5) 0.3454(4) 0.3497(3) 0.0766(16) Uani 1 1 d . . . H1A H 1.2706 0.3624 0.3885 0.092 Uiso 1 1 calc R . . C2 C 1.4346(6) 0.3647(4) 0.3619(3) 0.100(2) Uani 1 1 d . . . H2A H 1.4801 0.3944 0.4082 0.120 Uiso 1 1 calc R . . C3 C 1.4934(6) 0.3403(5) 0.3058(4) 0.107(2) Uani 1 1 d . . . H3A H 1.5793 0.3531 0.3135 0.129 Uiso 1 1 calc R . . C4 C 1.4231(5) 0.2959(4) 0.2369(3) 0.0832(17) Uani 1 1 d . . . H4A H 1.4610 0.2785 0.1978 0.100 Uiso 1 1 calc R . . C5 C 1.2970(4) 0.2785(3) 0.2281(2) 0.0587(12) Uani 1 1 d . . . C6 C 1.2112(4) 0.2292(3) 0.1589(2) 0.0528(12) Uani 1 1 d . . . C7 C 1.2418(4) 0.2032(3) 0.0921(2) 0.0582(12) Uani 1 1 d . . . H7A H 1.3223 0.2186 0.0876 0.070 Uiso 1 1 calc R . . C8 C 1.1531(4) 0.1538(3) 0.0310(2) 0.0525(11) Uani 1 1 d . . . C9 C 1.0338(4) 0.1352(3) 0.0418(2) 0.0577(12) Uani 1 1 d . . . H9A H 0.9715 0.1027 0.0028 0.069 Uiso 1 1 calc R . . C10 C 1.0069(4) 0.1643(3) 0.1093(2) 0.0551(12) Uani 1 1 d . . . C11 C 0.8835(4) 0.1516(3) 0.1277(2) 0.0551(12) Uani 1 1 d . . . C12 C 0.7759(5) 0.1132(4) 0.0770(3) 0.0711(15) Uani 1 1 d . . . H12A H 0.7775 0.0925 0.0282 0.085 Uiso 1 1 calc R . . C13 C 0.6670(5) 0.1060(4) 0.0996(3) 0.0749(15) Uani 1 1 d . . . H13A H 0.5932 0.0808 0.0663 0.090 Uiso 1 1 calc R . . C14 C 0.6679(5) 0.1369(3) 0.1727(3) 0.0738(15) Uani 1 1 d . . . H14A H 0.5948 0.1322 0.1892 0.089 Uiso 1 1 calc R . . C15 C 0.7776(5) 0.1743(3) 0.2203(3) 0.0665(14) Uani 1 1 d . . . H15A H 0.7774 0.1948 0.2694 0.080 Uiso 1 1 calc R . . C16 C 1.1836(4) 0.1228(3) -0.0406(2) 0.0564(12) Uani 1 1 d . . . C17 C 1.3049(5) 0.1292(4) -0.0503(3) 0.0758(16) Uani 1 1 d . . . H17A H 1.3690 0.1532 -0.0098 0.091 Uiso 1 1 calc R . . C18 C 1.3342(5) 0.1020(4) -0.1164(3) 0.0793(16) Uani 1 1 d . . . H18A H 1.4168 0.1091 -0.1200 0.095 Uiso 1 1 calc R . . C19 C 1.2435(5) 0.0639(3) -0.1782(3) 0.0666(14) Uani 1 1 d . . . C20 C 1.1219(5) 0.0552(4) -0.1705(3) 0.0752(15) Uani 1 1 d . . . H20A H 1.0587 0.0297 -0.2111 0.090 Uiso 1 1 calc R . . C21 C 1.0927(5) 0.0844(3) -0.1023(3) 0.0698(15) Uani 1 1 d . . . H21A H 1.0101 0.0778 -0.0985 0.084 Uiso 1 1 calc R . . C22 C 1.2810(6) 0.0299(4) -0.2484(3) 0.0781(16) Uani 1 1 d . . . H22A H 1.3656 0.0324 -0.2472 0.094 Uiso 1 1 calc R . . C23 C 1.2083(6) -0.0022(4) -0.3099(3) 0.0842(17) Uani 1 1 d . . . H23A H 1.1240 -0.0004 -0.3119 0.101 Uiso 1 1 calc R . . C24 C 1.2463(6) -0.0432(3) -0.3802(3) 0.0766(16) Uani 1 1 d . . . C25 C 1.3616(6) -0.0716(4) -0.3836(3) 0.0863(18) Uani 1 1 d . . . H25A H 1.4209 -0.0623 -0.3411 0.104 Uiso 1 1 calc R . . C26 C 1.3889(6) -0.1138(4) -0.4501(3) 0.0797(16) Uani 1 1 d . . . H26A H 1.4679 -0.1291 -0.4514 0.096 Uiso 1 1 calc R . . C27 C 1.2991(5) -0.1334(3) -0.5150(3) 0.0648(14) Uani 1 1 d . . . C28 C 1.1828(5) -0.1058(3) -0.5099(3) 0.0681(14) Uani 1 1 d . . . C29 C 1.1598(6) -0.0613(3) -0.4436(3) 0.0760(15) Uani 1 1 d . . . H29A H 1.0825 -0.0428 -0.4422 0.091 Uiso 1 1 calc R . . C30 C 1.1293(6) -0.1612(3) -0.6560(3) 0.0723(15) Uani 1 1 d . . . C31 C 1.0590(6) -0.1662(4) -0.7238(3) 0.097(2) Uani 1 1 d . . . H31A H 0.9786 -0.1523 -0.7282 0.116 Uiso 1 1 calc R . . C32 C 1.1087(8) -0.1919(5) -0.7846(4) 0.118(3) Uani 1 1 d . . . H32A H 1.0613 -0.1958 -0.8300 0.141 Uiso 1 1 calc R . . C33 C 1.2241(8) -0.2111(5) -0.7784(3) 0.105(2) Uani 1 1 d . . . H33A H 1.2562 -0.2291 -0.8198 0.126 Uiso 1 1 calc R . . C34 C 1.2971(6) -0.2048(4) -0.7118(3) 0.0872(18) Uani 1 1 d . . . H34A H 1.3783 -0.2170 -0.7089 0.105 Uiso 1 1 calc R . . C35 C 1.2509(5) -0.1804(3) -0.6483(3) 0.0654(14) Uani 1 1 d . . . C36 C 1.4439(5) -0.2112(4) -0.5809(3) 0.0790(16) Uani 1 1 d . . . H36A H 1.4351 -0.2621 -0.6228 0.095 Uiso 1 1 calc R . . H36B H 1.4661 -0.2307 -0.5379 0.095 Uiso 1 1 calc R . . C37 C 1.5482(6) -0.1440(5) -0.5818(3) 0.102(2) Uani 1 1 d . . . H37A H 1.6236 -0.1698 -0.5812 0.153 Uiso 1 1 calc R . . H37B H 1.5589 -0.0939 -0.5400 0.153 Uiso 1 1 calc R . . H37C H 1.5281 -0.1256 -0.6249 0.153 Uiso 1 1 calc R . . C38 C 1.1773(5) 0.0911(3) 0.2867(3) 0.0668(14) Uani 1 1 d . . . H38A H 1.1846 0.0764 0.2386 0.080 Uiso 1 1 calc R . . C39 C 1.2327(5) 0.0455(4) 0.3304(3) 0.0742(15) Uani 1 1 d . . . H39A H 1.2760 0.0000 0.3122 0.089 Uiso 1 1 calc R . . C40 C 1.2238(5) 0.0674(3) 0.4020(3) 0.0736(15) Uani 1 1 d . . . H40A H 1.2616 0.0374 0.4329 0.088 Uiso 1 1 calc R . . C41 C 1.1580(5) 0.1345(3) 0.4272(3) 0.0642(13) Uani 1 1 d . . . H41A H 1.1508 0.1504 0.4753 0.077 Uiso 1 1 calc R . . C42 C 1.1033(4) 0.1777(3) 0.3805(2) 0.0517(11) Uani 1 1 d . . . C43 C 1.0314(4) 0.2511(3) 0.4007(2) 0.0531(12) Uani 1 1 d . . . C44 C 0.9892(4) 0.2766(3) 0.4636(2) 0.0572(12) Uani 1 1 d . . . H44A H 1.0076 0.2472 0.4985 0.069 Uiso 1 1 calc R . . C45 C 0.9195(4) 0.3453(3) 0.4760(3) 0.0611(13) Uani 1 1 d . . . C46 C 0.8961(5) 0.3891(3) 0.4230(3) 0.0635(13) Uani 1 1 d . . . H46A H 0.8516 0.4367 0.4298 0.076 Uiso 1 1 calc R . . C47 C 0.9400(4) 0.3609(3) 0.3602(3) 0.0566(12) Uani 1 1 d . . . C48 C 0.9179(5) 0.3982(3) 0.2981(3) 0.0602(13) Uani 1 1 d . . . C49 C 0.8380(5) 0.4592(4) 0.2916(3) 0.0760(15) Uani 1 1 d . . . H49A H 0.7965 0.4812 0.3282 0.091 Uiso 1 1 calc R . . C50 C 0.8206(6) 0.4869(4) 0.2304(4) 0.0944(19) Uani 1 1 d . . . H50A H 0.7655 0.5267 0.2244 0.113 Uiso 1 1 calc R . . C51 C 0.8857(7) 0.4551(4) 0.1781(4) 0.0925(19) Uani 1 1 d . . . H51A H 0.8784 0.4752 0.1373 0.111 Uiso 1 1 calc R . . C52 C 0.9610(6) 0.3939(4) 0.1868(3) 0.0787(16) Uani 1 1 d . . . H52A H 1.0026 0.3713 0.1502 0.094 Uiso 1 1 calc R . . C53 C 0.8710(5) 0.3727(3) 0.5431(3) 0.0666(14) Uani 1 1 d . . . C54 C 0.9360(5) 0.3653(3) 0.6085(3) 0.0736(15) Uani 1 1 d . . . H54A H 1.0114 0.3433 0.6106 0.088 Uiso 1 1 calc R . . C55 C 0.8892(7) 0.3906(4) 0.6705(3) 0.0872(18) Uani 1 1 d . . . H55A H 0.9341 0.3858 0.7140 0.105 Uiso 1 1 calc R . . C56 C 0.7788(8) 0.4223(4) 0.6689(4) 0.099(2) Uani 1 1 d . . . C57 C 0.7135(7) 0.4283(4) 0.6052(4) 0.101(2) Uani 1 1 d . . . H57A H 0.6371 0.4487 0.6036 0.121 Uiso 1 1 calc R . . C58 C 0.7581(6) 0.4047(4) 0.5431(3) 0.0881(18) Uani 1 1 d . . . H58A H 0.7121 0.4103 0.5002 0.106 Uiso 1 1 calc R . . C59 C 0.7565(9) 0.4602(6) 0.7619(8) 0.161(5) Uani 1 1 d . . . H59A H 0.7590 0.4145 0.7863 0.194 Uiso 1 1 calc R . . H59B H 0.8133 0.5125 0.7911 0.194 Uiso 1 1 calc R . . C60 C 0.6683(12) 0.4731(8) 0.7456(9) 0.225(8) Uani 1 1 d . . . H60A H 0.6098 0.4204 0.7197 0.270 Uiso 1 1 calc R . . H60B H 0.6649 0.5156 0.7180 0.270 Uiso 1 1 calc R . . C61 C 0.6527(14) 0.5202(5) 0.8404(5) 0.155(5) Uani 1 1 d . . . C62 C 0.7369(9) 0.5504(4) 0.9052(5) 0.127(3) Uani 1 1 d . . . H62A H 0.8192 0.5409 0.9079 0.152 Uiso 1 1 calc R . . C63 C 0.6979(8) 0.5957(4) 0.9672(3) 0.100(2) Uani 1 1 d . . . C64 C 0.5776(8) 0.6083(5) 0.9658(4) 0.109(2) Uani 1 1 d . . . C65 C 0.4938(9) 0.5765(6) 0.8998(4) 0.141(3) Uani 1 1 d . . . H65A H 0.4111 0.5849 0.8971 0.169 Uiso 1 1 calc R . . C66 C 0.5312(12) 0.5331(7) 0.8385(5) 0.177(5) Uani 1 1 d . . . H66A H 0.4731 0.5119 0.7950 0.213 Uiso 1 1 calc R . . C67 C 0.7281(7) 0.6639(4) 1.1119(4) 0.0877(18) Uani 1 1 d . . . C68 C 0.7945(8) 0.6819(4) 1.1820(4) 0.109(2) Uani 1 1 d . . . H68A H 0.8787 0.6771 1.1905 0.131 Uiso 1 1 calc R . . C69 C 0.7375(10) 0.7070(6) 1.2396(4) 0.129(3) Uani 1 1 d . . . H69A H 0.7823 0.7192 1.2870 0.155 Uiso 1 1 calc R . . C70 C 0.6156(11) 0.7134(6) 1.2258(4) 0.139(3) Uani 1 1 d . . . H70A H 0.5763 0.7302 1.2644 0.167 Uiso 1 1 calc R . . C71 C 0.5478(8) 0.6960(5) 1.1566(4) 0.121(3) Uani 1 1 d . . . H71A H 0.4637 0.7014 1.1488 0.145 Uiso 1 1 calc R . . C72 C 0.6039(7) 0.6701(4) 1.0980(3) 0.0913(19) Uani 1 1 d . . . C73 C 0.4126(11) 0.6989(7) 1.0122(6) 0.175(4) Uani 1 1 d . . . H73A H 0.4170 0.7544 1.0489 0.210 Uiso 1 1 calc R . . H73B H 0.3990 0.7091 0.9650 0.210 Uiso 1 1 calc R . . C74 C 0.3195(13) 0.6377(8) 1.0155(5) 0.227(7) Uani 1 1 d . . . H74A H 0.2409 0.6586 1.0061 0.340 Uiso 1 1 calc R . . H74B H 0.3341 0.6292 1.0628 0.340 Uiso 1 1 calc R . . H74C H 0.3185 0.5829 0.9798 0.340 Uiso 1 1 calc R . . Cl1 Cl 0.68022(15) 0.61342(11) 0.43217(9) 0.0877(5) Uani 1 1 d . . . Cl2 Cl 0.66415(13) 0.01423(11) 0.87035(8) 0.0787(4) Uani 1 1 d . . . O1 O 0.7745(6) 0.5753(4) 0.4649(4) 0.160(2) Uani 1 1 d . . . O2 O 0.6159(7) 0.6552(5) 0.4802(3) 0.194(3) Uani 1 1 d . . . O3 O 0.6121(6) 0.5635(6) 0.3679(4) 0.229(4) Uani 1 1 d . . . O4 O 0.7503(7) 0.6821(5) 0.4145(4) 0.189(3) Uani 1 1 d . . . O5 O 0.7928(4) 0.0097(3) 0.8837(2) 0.1079(15) Uani 1 1 d . . . O6 O 0.6478(7) 0.1003(5) 0.8829(6) 0.244(5) Uani 1 1 d . . . O7 O 0.6081(4) -0.0301(6) 0.8024(3) 0.206(4) Uani 1 1 d . . . O8 O 0.6088(4) -0.0134(5) 0.9196(3) 0.159(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0573(4) 0.0574(4) 0.0443(4) 0.0035(3) 0.0157(3) 0.0055(3) N1 0.068(3) 0.064(2) 0.048(2) 0.0056(19) 0.016(2) 0.004(2) N2 0.049(2) 0.055(2) 0.046(2) 0.0044(17) 0.0121(18) 0.0030(18) N3 0.057(2) 0.056(2) 0.044(2) 0.0031(17) 0.0177(18) 0.0035(18) N4 0.057(2) 0.065(2) 0.046(2) 0.0013(18) 0.0173(18) 0.010(2) N5 0.059(2) 0.048(2) 0.054(2) 0.0067(19) 0.0175(19) 0.0117(19) N6 0.065(3) 0.063(2) 0.050(2) 0.007(2) 0.016(2) 0.007(2) N7 0.080(3) 0.076(3) 0.053(2) 0.013(2) 0.024(2) 0.026(2) N8 0.130(5) 0.185(6) 0.068(4) 0.006(4) 0.042(4) 0.058(5) S1 0.0852(11) 0.0986(11) 0.0718(9) 0.0180(8) 0.0280(8) 0.0223(9) S2 0.1375(18) 0.164(2) 0.1191(17) 0.0098(15) 0.0660(15) 0.0330(16) C1 0.077(4) 0.085(4) 0.050(3) -0.003(3) 0.010(3) -0.001(3) C2 0.088(5) 0.110(5) 0.067(4) -0.019(3) 0.005(4) -0.007(4) C3 0.062(4) 0.131(6) 0.095(5) -0.004(4) 0.001(4) -0.017(4) C4 0.062(4) 0.104(4) 0.064(3) -0.004(3) 0.016(3) -0.006(3) C5 0.056(3) 0.064(3) 0.047(3) 0.002(2) 0.010(2) 0.003(2) C6 0.058(3) 0.051(3) 0.044(3) 0.003(2) 0.014(2) 0.005(2) C7 0.045(3) 0.070(3) 0.053(3) 0.004(2) 0.015(2) 0.004(2) C8 0.050(3) 0.060(3) 0.047(3) 0.012(2) 0.015(2) 0.011(2) C9 0.053(3) 0.062(3) 0.049(3) 0.006(2) 0.007(2) 0.005(2) C10 0.057(3) 0.054(3) 0.046(3) 0.002(2) 0.011(2) 0.004(2) C11 0.055(3) 0.057(3) 0.050(3) 0.009(2) 0.015(2) 0.006(2) C12 0.061(3) 0.085(4) 0.055(3) 0.005(3) 0.008(3) 0.000(3) C13 0.051(3) 0.084(4) 0.077(4) 0.009(3) 0.007(3) -0.002(3) C14 0.057(3) 0.080(4) 0.082(4) 0.013(3) 0.028(3) 0.004(3) C15 0.075(4) 0.063(3) 0.064(3) 0.010(3) 0.033(3) 0.010(3) C16 0.059(3) 0.062(3) 0.047(3) 0.011(2) 0.014(2) 0.010(2) C17 0.061(3) 0.098(4) 0.056(3) -0.001(3) 0.013(3) 0.012(3) C18 0.073(4) 0.097(4) 0.063(3) 0.001(3) 0.033(3) 0.018(3) C19 0.080(4) 0.066(3) 0.055(3) 0.009(2) 0.029(3) 0.013(3) C20 0.076(4) 0.091(4) 0.051(3) 0.012(3) 0.012(3) 0.002(3) C21 0.065(3) 0.091(4) 0.048(3) 0.008(3) 0.019(3) 0.005(3) C22 0.093(4) 0.076(4) 0.065(4) 0.016(3) 0.024(3) 0.013(3) C23 0.099(5) 0.084(4) 0.063(4) 0.011(3) 0.019(3) 0.012(3) C24 0.106(5) 0.066(3) 0.060(3) 0.009(3) 0.035(3) 0.014(3) C25 0.112(5) 0.094(4) 0.053(3) 0.019(3) 0.019(3) 0.020(4) C26 0.092(4) 0.094(4) 0.053(3) 0.015(3) 0.020(3) 0.024(3) C27 0.091(4) 0.059(3) 0.051(3) 0.012(2) 0.034(3) 0.017(3) C28 0.095(4) 0.059(3) 0.057(3) 0.013(2) 0.038(3) 0.016(3) C29 0.098(4) 0.075(4) 0.057(3) 0.013(3) 0.027(3) 0.020(3) C30 0.087(4) 0.074(4) 0.058(3) 0.014(3) 0.025(3) 0.019(3) C31 0.098(5) 0.117(5) 0.067(4) 0.010(4) 0.007(4) 0.038(4) C32 0.145(7) 0.140(6) 0.058(4) 0.013(4) 0.008(4) 0.045(6) C33 0.127(6) 0.137(6) 0.061(4) 0.022(4) 0.037(4) 0.050(5) C34 0.102(5) 0.107(5) 0.058(3) 0.018(3) 0.030(3) 0.033(4) C35 0.078(4) 0.066(3) 0.053(3) 0.011(2) 0.019(3) 0.018(3) C36 0.086(4) 0.077(4) 0.072(4) 0.010(3) 0.022(3) 0.028(3) C37 0.085(5) 0.122(5) 0.087(4) 0.008(4) 0.020(4) 0.020(4) C38 0.071(3) 0.068(3) 0.056(3) 0.002(3) 0.023(3) 0.017(3) C39 0.078(4) 0.068(3) 0.076(4) 0.009(3) 0.025(3) 0.023(3) C40 0.074(4) 0.072(4) 0.074(4) 0.018(3) 0.013(3) 0.021(3) C41 0.065(3) 0.075(3) 0.053(3) 0.015(3) 0.016(3) 0.014(3) C42 0.050(3) 0.056(3) 0.046(3) 0.007(2) 0.012(2) 0.007(2) C43 0.051(3) 0.053(3) 0.049(3) 0.004(2) 0.010(2) 0.003(2) C44 0.060(3) 0.062(3) 0.046(3) 0.008(2) 0.015(2) 0.007(2) C45 0.056(3) 0.058(3) 0.060(3) -0.002(3) 0.020(2) 0.001(2) C46 0.065(3) 0.055(3) 0.064(3) 0.002(3) 0.020(3) 0.012(2) C47 0.058(3) 0.048(3) 0.058(3) 0.004(2) 0.017(2) 0.005(2) C48 0.068(3) 0.048(3) 0.057(3) 0.003(2) 0.014(3) 0.003(2) C49 0.082(4) 0.063(3) 0.082(4) 0.015(3) 0.021(3) 0.020(3) C50 0.098(5) 0.076(4) 0.111(5) 0.033(4) 0.013(4) 0.026(4) C51 0.116(5) 0.087(4) 0.077(4) 0.033(4) 0.012(4) 0.013(4) C52 0.093(4) 0.079(4) 0.059(3) 0.016(3) 0.012(3) 0.003(3) C53 0.069(4) 0.061(3) 0.059(3) -0.005(2) 0.026(3) 0.002(3) C54 0.082(4) 0.077(4) 0.053(3) -0.002(3) 0.027(3) 0.007(3) C55 0.117(5) 0.077(4) 0.060(3) -0.005(3) 0.042(3) -0.002(4) C56 0.139(7) 0.066(4) 0.094(5) -0.015(4) 0.085(5) 0.000(4) C57 0.102(5) 0.097(5) 0.112(6) 0.009(4) 0.070(5) 0.024(4) C58 0.083(4) 0.095(4) 0.091(4) 0.015(3) 0.040(4) 0.025(3) C59 0.097(7) 0.095(6) 0.300(16) 0.088(8) 0.030(9) -0.016(6) C60 0.156(11) 0.149(10) 0.34(2) 0.142(12) -0.074(14) -0.067(9) C61 0.299(15) 0.083(5) 0.083(6) -0.015(4) 0.122(8) -0.018(7) C62 0.212(9) 0.066(4) 0.125(6) 0.010(4) 0.117(7) 0.018(5) C63 0.144(6) 0.086(4) 0.072(4) 0.005(3) 0.056(4) 0.017(4) C64 0.151(7) 0.110(5) 0.070(4) 0.008(4) 0.061(5) 0.013(5) C65 0.183(8) 0.165(7) 0.056(4) -0.005(4) 0.049(5) -0.014(6) C66 0.241(13) 0.187(10) 0.082(6) -0.011(6) 0.082(8) -0.038(9) C67 0.119(6) 0.074(4) 0.076(4) 0.012(3) 0.045(4) 0.026(4) C68 0.129(6) 0.098(5) 0.101(6) 0.020(4) 0.035(5) 0.026(4) C69 0.164(9) 0.138(7) 0.085(5) 0.026(5) 0.030(6) 0.040(6) C70 0.170(9) 0.171(8) 0.081(6) 0.016(5) 0.057(6) 0.049(7) C71 0.135(6) 0.154(7) 0.068(4) 0.002(4) 0.045(4) 0.033(5) C72 0.116(6) 0.093(4) 0.065(4) 0.008(3) 0.038(4) 0.023(4) C73 0.194(11) 0.146(8) 0.156(9) -0.021(7) 0.067(8) 0.007(8) C74 0.268(15) 0.237(13) 0.107(7) -0.026(8) 0.047(8) -0.107(12) Cl1 0.0815(10) 0.0906(11) 0.0781(10) -0.0025(8) 0.0179(9) 0.0255(9) Cl2 0.0603(9) 0.1027(11) 0.0673(9) 0.0088(8) 0.0217(7) 0.0121(8) O1 0.145(5) 0.134(5) 0.197(6) 0.040(4) 0.014(4) 0.072(4) O2 0.219(7) 0.293(8) 0.115(4) 0.057(5) 0.082(4) 0.179(7) O3 0.129(5) 0.304(9) 0.146(5) -0.084(6) 0.011(4) -0.042(6) O4 0.195(7) 0.188(6) 0.181(6) 0.077(5) 0.016(5) -0.007(5) O5 0.057(3) 0.157(4) 0.092(3) 0.010(3) 0.014(2) 0.002(2) O6 0.202(8) 0.149(6) 0.444(15) 0.121(8) 0.149(9) 0.081(5) O7 0.073(3) 0.411(11) 0.070(3) -0.023(5) 0.015(3) -0.014(5) O8 0.077(3) 0.294(8) 0.101(4) 0.064(4) 0.022(3) -0.033(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.891(4) . ? Co1 N5 1.908(4) . ? Co1 N1 2.057(4) . ? Co1 N3 2.059(4) . ? Co1 N4 2.103(4) . ? Co1 N6 2.108(4) . ? N1 C1 1.338(6) . ? N1 C5 1.355(6) . ? N2 C6 1.342(6) . ? N2 C10 1.346(5) . ? N3 C15 1.342(6) . ? N3 C11 1.351(5) . ? N4 C38 1.341(6) . ? N4 C42 1.355(5) . ? N5 C47 1.350(6) . ? N5 C43 1.350(6) . ? N6 C52 1.336(7) . ? N6 C48 1.356(6) . ? N7 C35 1.403(6) . ? N7 C27 1.404(6) . ? N7 C36 1.455(6) . ? N8 C72 1.397(8) . ? N8 C64 1.404(8) . ? N8 C73 1.612(12) . ? S1 C30 1.749(5) . ? S1 C28 1.752(6) . ? S2 C67 1.754(6) . ? S2 C63 1.761(8) . ? C1 C2 1.356(8) . ? C2 C3 1.364(8) . ? C3 C4 1.395(7) . ? C4 C5 1.370(7) . ? C5 C6 1.481(6) . ? C6 C7 1.378(6) . ? C7 C8 1.397(6) . ? C8 C9 1.394(6) . ? C8 C16 1.470(6) . ? C9 C10 1.377(6) . ? C10 C11 1.486(6) . ? C11 C12 1.379(6) . ? C12 C13 1.364(7) . ? C13 C14 1.383(7) . ? C14 C15 1.367(7) . ? C16 C21 1.381(6) . ? C16 C17 1.390(7) . ? C17 C18 1.360(7) . ? C18 C19 1.379(7) . ? C19 C20 1.381(7) . ? C19 C22 1.487(7) . ? C20 C21 1.400(7) . ? C22 C23 1.268(7) . ? C23 C24 1.510(7) . ? C24 C29 1.370(7) . ? C24 C25 1.395(8) . ? C25 C26 1.398(7) . ? C26 C27 1.406(7) . ? C27 C28 1.406(7) . ? C28 C29 1.384(7) . ? C30 C31 1.391(7) . ? C30 C35 1.395(7) . ? C31 C32 1.381(9) . ? C32 C33 1.330(9) . ? C33 C34 1.378(8) . ? C34 C35 1.404(7) . ? C36 C37 1.512(8) . ? C38 C39 1.361(7) . ? C39 C40 1.377(7) . ? C40 C41 1.376(7) . ? C41 C42 1.369(7) . ? C42 C43 1.477(6) . ? C43 C44 1.371(6) . ? C44 C45 1.385(6) . ? C45 C46 1.396(7) . ? C45 C53 1.484(6) . ? C46 C47 1.385(6) . ? C47 C48 1.480(7) . ? C48 C49 1.380(7) . ? C49 C50 1.372(8) . ? C50 C51 1.371(9) . ? C51 C52 1.358(8) . ? C53 C58 1.388(7) . ? C53 C54 1.389(7) . ? C54 C55 1.383(7) . ? C55 C56 1.360(9) . ? C56 C57 1.354(10) . ? C56 C59 1.831(15) . ? C57 C58 1.369(8) . ? C59 C60 1.026(12) . ? C60 C61 1.856(19) . ? C61 C62 1.371(13) . ? C61 C66 1.373(15) . ? C62 C63 1.400(8) . ? C63 C64 1.360(10) . ? C64 C65 1.386(10) . ? C65 C66 1.371(11) . ? C67 C72 1.368(9) . ? C67 C68 1.377(9) . ? C68 C69 1.377(10) . ? C69 C70 1.344(11) . ? C70 C71 1.369(10) . ? C71 C72 1.389(8) . ? C73 C74 1.379(12) . ? Cl1 O3 1.344(6) . ? Cl1 O2 1.352(5) . ? Cl1 O1 1.392(5) . ? Cl1 O4 1.439(7) . ? Cl2 O7 1.334(5) . ? Cl2 O6 1.358(7) . ? Cl2 O8 1.376(5) . ? Cl2 O5 1.411(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N5 177.40(16) . . ? N2 Co1 N1 79.92(15) . . ? N5 Co1 N1 102.44(15) . . ? N2 Co1 N3 80.12(15) . . ? N5 Co1 N3 97.53(15) . . ? N1 Co1 N3 160.03(15) . . ? N2 Co1 N4 102.30(15) . . ? N5 Co1 N4 79.06(16) . . ? N1 Co1 N4 85.67(15) . . ? N3 Co1 N4 98.03(15) . . ? N2 Co1 N6 99.23(16) . . ? N5 Co1 N6 79.41(16) . . ? N1 Co1 N6 98.38(16) . . ? N3 Co1 N6 85.39(15) . . ? N4 Co1 N6 158.47(15) . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Co1 127.7(4) . . ? C5 N1 Co1 113.3(3) . . ? C6 N2 C10 119.5(4) . . ? C6 N2 Co1 120.3(3) . . ? C10 N2 Co1 120.1(3) . . ? C15 N3 C11 117.5(4) . . ? C15 N3 Co1 128.8(3) . . ? C11 N3 Co1 113.2(3) . . ? C38 N4 C42 118.0(4) . . ? C38 N4 Co1 127.7(3) . . ? C42 N4 Co1 112.8(3) . . ? C47 N5 C43 119.5(4) . . ? C47 N5 Co1 120.1(3) . . ? C43 N5 Co1 120.3(3) . . ? C52 N6 C48 117.6(5) . . ? C52 N6 Co1 129.0(4) . . ? C48 N6 Co1 111.9(3) . . ? C35 N7 C27 122.6(4) . . ? C35 N7 C36 118.6(4) . . ? C27 N7 C36 118.1(4) . . ? C72 N8 C64 123.5(7) . . ? C72 N8 C73 119.7(6) . . ? C64 N8 C73 116.6(6) . . ? C30 S1 C28 100.8(3) . . ? C67 S2 C63 100.4(4) . . ? N1 C1 C2 122.7(5) . . ? C1 C2 C3 119.6(5) . . ? C2 C3 C4 119.1(6) . . ? C5 C4 C3 118.5(5) . . ? N1 C5 C4 122.0(4) . . ? N1 C5 C6 113.5(4) . . ? C4 C5 C6 124.5(4) . . ? N2 C6 C7 121.4(4) . . ? N2 C6 C5 112.4(4) . . ? C7 C6 C5 126.1(4) . . ? C6 C7 C8 120.7(4) . . ? C9 C8 C7 116.2(4) . . ? C9 C8 C16 121.8(4) . . ? C7 C8 C16 122.0(4) . . ? C10 C9 C8 121.1(4) . . ? N2 C10 C9 121.0(4) . . ? N2 C10 C11 112.5(4) . . ? C9 C10 C11 126.5(4) . . ? N3 C11 C12 122.6(4) . . ? N3 C11 C10 113.7(4) . . ? C12 C11 C10 123.7(4) . . ? C13 C12 C11 119.0(5) . . ? C12 C13 C14 119.1(5) . . ? C15 C14 C13 119.3(5) . . ? N3 C15 C14 122.6(5) . . ? C21 C16 C17 116.0(4) . . ? C21 C16 C8 121.6(4) . . ? C17 C16 C8 122.4(4) . . ? C18 C17 C16 122.9(5) . . ? C17 C18 C19 121.2(5) . . ? C18 C19 C20 117.5(5) . . ? C18 C19 C22 119.1(5) . . ? C20 C19 C22 123.3(5) . . ? C19 C20 C21 120.9(5) . . ? C16 C21 C20 121.5(5) . . ? C23 C22 C19 126.1(6) . . ? C22 C23 C24 125.9(6) . . ? C29 C24 C25 117.8(5) . . ? C29 C24 C23 118.6(6) . . ? C25 C24 C23 123.4(6) . . ? C24 C25 C26 120.8(5) . . ? C25 C26 C27 121.2(5) . . ? N7 C27 C26 121.3(5) . . ? N7 C27 C28 121.9(5) . . ? C26 C27 C28 116.8(4) . . ? C29 C28 C27 120.8(5) . . ? C29 C28 S1 115.4(4) . . ? C27 C28 S1 123.6(4) . . ? C24 C29 C28 122.6(6) . . ? C31 C30 C35 120.6(5) . . ? C31 C30 S1 116.1(5) . . ? C35 C30 S1 123.3(4) . . ? C32 C31 C30 120.0(6) . . ? C33 C32 C31 120.2(6) . . ? C32 C33 C34 121.2(6) . . ? C33 C34 C35 121.1(6) . . ? C30 C35 N7 123.0(5) . . ? C30 C35 C34 116.9(5) . . ? N7 C35 C34 120.1(5) . . ? N7 C36 C37 113.7(5) . . ? N4 C38 C39 122.7(5) . . ? C38 C39 C40 119.2(5) . . ? C41 C40 C39 119.0(5) . . ? C42 C41 C40 119.3(5) . . ? N4 C42 C41 121.9(4) . . ? N4 C42 C43 113.4(4) . . ? C41 C42 C43 124.7(4) . . ? N5 C43 C44 120.6(4) . . ? N5 C43 C42 113.2(4) . . ? C44 C43 C42 126.1(5) . . ? C43 C44 C45 121.2(5) . . ? C44 C45 C46 117.7(4) . . ? C44 C45 C53 121.9(5) . . ? C46 C45 C53 120.4(5) . . ? C47 C46 C45 119.1(5) . . ? N5 C47 C46 121.8(5) . . ? N5 C47 C48 113.0(4) . . ? C46 C47 C48 125.2(5) . . ? N6 C48 C49 121.6(5) . . ? N6 C48 C47 114.3(4) . . ? C49 C48 C47 124.1(5) . . ? C50 C49 C48 119.3(6) . . ? C51 C50 C49 119.0(6) . . ? C52 C51 C50 119.1(6) . . ? N6 C52 C51 123.4(6) . . ? C58 C53 C54 117.3(5) . . ? C58 C53 C45 121.7(5) . . ? C54 C53 C45 121.0(5) . . ? C55 C54 C53 120.3(6) . . ? C56 C55 C54 121.0(6) . . ? C57 C56 C55 119.1(6) . . ? C57 C56 C59 132.2(7) . . ? C55 C56 C59 108.4(7) . . ? C56 C57 C58 121.2(6) . . ? C57 C58 C53 121.0(6) . . ? C60 C59 C56 93.0(17) . . ? C59 C60 C61 92.3(16) . . ? C62 C61 C66 118.9(7) . . ? C62 C61 C60 133.2(10) . . ? C66 C61 C60 107.5(10) . . ? C61 C62 C63 119.4(9) . . ? C64 C63 C62 121.9(8) . . ? C64 C63 S2 122.0(5) . . ? C62 C63 S2 115.8(7) . . ? C63 C64 C65 117.6(7) . . ? C63 C64 N8 122.6(7) . . ? C65 C64 N8 119.6(8) . . ? C66 C65 C64 121.0(9) . . ? C65 C66 C61 121.1(10) . . ? C72 C67 C68 120.7(6) . . ? C72 C67 S2 123.7(5) . . ? C68 C67 S2 115.3(6) . . ? C69 C68 C67 120.7(8) . . ? C70 C69 C68 118.5(8) . . ? C69 C70 C71 121.8(8) . . ? C70 C71 C72 120.3(8) . . ? C67 C72 C71 118.0(7) . . ? C67 C72 N8 120.7(6) . . ? C71 C72 N8 121.2(7) . . ? C74 C73 N8 104.4(11) . . ? O3 Cl1 O2 115.9(5) . . ? O3 Cl1 O1 116.1(5) . . ? O2 Cl1 O1 111.6(4) . . ? O3 Cl1 O4 104.1(5) . . ? O2 Cl1 O4 105.6(5) . . ? O1 Cl1 O4 101.5(4) . . ? O7 Cl2 O6 109.5(6) . . ? O7 Cl2 O8 111.4(4) . . ? O6 Cl2 O8 103.9(5) . . ? O7 Cl2 O5 111.8(3) . . ? O6 Cl2 O5 108.3(4) . . ? O8 Cl2 O5 111.5(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.680 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.061 # Attachment 'ldm3.cif' data_p1bar_3 _database_code_depnum_ccdc_archive 'CCDC 700926' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H58 Cl4 N8 O8 S2 Zn' _chemical_formula_sum 'C75 H58 Cl4 N8 O8 S2 Zn' _chemical_formula_weight 1470.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9221(3) _cell_length_b 14.1176(3) _cell_length_c 20.0140(4) _cell_angle_alpha 105.3220(10) _cell_angle_beta 97.9320(10) _cell_angle_gamma 112.5160(10) _cell_volume 3376.01(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9093 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 21.02 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8096 _exptl_absorpt_correction_T_max 0.9380 _exptl_absorpt_process_details SADBS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61814 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.58 _reflns_number_total 15371 _reflns_number_gt 9068 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1165P)^2^+1.1668P] 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 15371 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.2181 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.61487(3) 0.37435(4) 0.27791(2) 0.05044(15) Uani 1 1 d . . . S1 S 1.40872(8) -0.06299(9) 0.59738(6) 0.0582(3) Uani 1 1 d . . . S2 S 0.02319(10) 0.84580(11) -0.21243(6) 0.0678(3) Uani 1 1 d . . . N1 N 0.7173(2) 0.3272(2) 0.33205(15) 0.0454(7) Uani 1 1 d . . . N2 N 0.6185(3) 0.2393(3) 0.19586(16) 0.0541(8) Uani 1 1 d . . . N3 N 0.6728(3) 0.4897(3) 0.38820(18) 0.0594(8) Uani 1 1 d . . . N4 N 0.4554(2) 0.2781(3) 0.29174(17) 0.0508(7) Uani 1 1 d . . . N5 N 0.5098(2) 0.4214(2) 0.22699(15) 0.0445(7) Uani 1 1 d . . . N6 N 0.7144(2) 0.4878(3) 0.23064(19) 0.0574(8) Uani 1 1 d . . . N7 N 1.5244(3) 0.0853(3) 0.74461(17) 0.0599(9) Uani 1 1 d . . . N8 N -0.1264(3) 0.8954(3) -0.12695(18) 0.0591(8) Uani 1 1 d . . . C1 C 0.5740(4) 0.2063(4) 0.1250(2) 0.0718(12) Uani 1 1 d . . . H1A H 0.5347 0.2402 0.1088 0.086 Uiso 1 1 calc R . . C2 C 0.5836(4) 0.1263(5) 0.0760(2) 0.0819(14) Uani 1 1 d . . . H2A H 0.5535 0.1072 0.0271 0.098 Uiso 1 1 calc R . . C3 C 0.6392(4) 0.0730(5) 0.0999(3) 0.0824(15) Uani 1 1 d . . . H3A H 0.6446 0.0156 0.0675 0.099 Uiso 1 1 calc R . . C4 C 0.6862(3) 0.1069(4) 0.1725(2) 0.0651(11) Uani 1 1 d . . . H4A H 0.7237 0.0724 0.1899 0.078 Uiso 1 1 calc R . . C5 C 0.6769(3) 0.1921(3) 0.21904(19) 0.0484(8) Uani 1 1 d . . . C6 C 0.7322(3) 0.2411(3) 0.29755(19) 0.0447(8) Uani 1 1 d . . . C7 C 0.7978(3) 0.2068(3) 0.33255(19) 0.0479(8) Uani 1 1 d . . . H7A H 0.8065 0.1463 0.3076 0.057 Uiso 1 1 calc R . . C8 C 0.8512(3) 0.2632(3) 0.4057(2) 0.0481(8) Uani 1 1 d . . . C9 C 0.8347(3) 0.3529(3) 0.4401(2) 0.0520(9) Uani 1 1 d . . . H9A H 0.8694 0.3930 0.4885 0.062 Uiso 1 1 calc R . . C10 C 0.7667(3) 0.3827(3) 0.40225(19) 0.0471(8) Uani 1 1 d . . . C11 C 0.7419(3) 0.4753(3) 0.4340(2) 0.0527(9) Uani 1 1 d . . . C12 C 0.7853(4) 0.5417(4) 0.5056(2) 0.0716(12) Uani 1 1 d . . . H12A H 0.8354 0.5323 0.5358 0.086 Uiso 1 1 calc R . . C13 C 0.7530(5) 0.6222(5) 0.5314(3) 0.0906(16) Uani 1 1 d . . . H13A H 0.7787 0.6658 0.5797 0.109 Uiso 1 1 calc R . . C14 C 0.6834(5) 0.6372(5) 0.4853(3) 0.0985(18) Uani 1 1 d . . . H14A H 0.6618 0.6919 0.5019 0.118 Uiso 1 1 calc R . . C15 C 0.6443(4) 0.5702(4) 0.4132(3) 0.0837(15) Uani 1 1 d . . . H15A H 0.5976 0.5815 0.3817 0.100 Uiso 1 1 calc R . . C16 C 0.9234(3) 0.2289(3) 0.4446(2) 0.0533(9) Uani 1 1 d . . . C17 C 0.9676(3) 0.1655(4) 0.4079(2) 0.0662(11) Uani 1 1 d . . . H17A H 0.9526 0.1445 0.3581 0.079 Uiso 1 1 calc R . . C18 C 1.0332(4) 0.1331(4) 0.4443(2) 0.0725(13) Uani 1 1 d . . . H18A H 1.0613 0.0901 0.4182 0.087 Uiso 1 1 calc R . . C19 C 1.0592(3) 0.1623(4) 0.5185(2) 0.0643(11) Uani 1 1 d . . . C20 C 1.0139(4) 0.2235(4) 0.5542(2) 0.0741(13) Uani 1 1 d . . . H20A H 1.0284 0.2431 0.6040 0.089 Uiso 1 1 calc R . . C21 C 0.9470(4) 0.2574(4) 0.5190(2) 0.0659(11) Uani 1 1 d . . . H21A H 0.9180 0.2993 0.5453 0.079 Uiso 1 1 calc R . . C22 C 1.1334(4) 0.1270(4) 0.5530(2) 0.0709(12) Uani 1 1 d . . . H22A H 1.1516 0.0781 0.5226 0.085 Uiso 1 1 calc R . . C23 C 1.1765(3) 0.1574(4) 0.6222(2) 0.0659(11) Uani 1 1 d . . . H23A H 1.1539 0.2012 0.6531 0.079 Uiso 1 1 calc R . . C24 C 1.2580(3) 0.1284(4) 0.6554(2) 0.0579(10) Uani 1 1 d . . . C25 C 1.2876(3) 0.0517(4) 0.6156(2) 0.0562(10) Uani 1 1 d . . . H25A H 1.2504 0.0114 0.5675 0.067 Uiso 1 1 calc R . . C26 C 1.3716(3) 0.0353(3) 0.6472(2) 0.0526(9) Uani 1 1 d . . . C27 C 1.5492(3) 0.0228(3) 0.6267(2) 0.0540(9) Uani 1 1 d . . . C28 C 1.6135(4) 0.0254(4) 0.5794(3) 0.0669(11) Uani 1 1 d . . . H28A H 1.5824 -0.0179 0.5311 0.080 Uiso 1 1 calc R . . C29 C 1.7221(4) 0.0912(5) 0.6030(3) 0.0810(14) Uani 1 1 d . . . H29A H 1.7649 0.0915 0.5712 0.097 Uiso 1 1 calc R . . C30 C 1.7675(4) 0.1564(5) 0.6736(3) 0.0860(15) Uani 1 1 d . . . H30A H 1.8414 0.2014 0.6897 0.103 Uiso 1 1 calc R . . C31 C 1.7038(4) 0.1560(4) 0.7220(3) 0.0758(13) Uani 1 1 d . . . H31A H 1.7353 0.2016 0.7699 0.091 Uiso 1 1 calc R . . C32 C 1.5940(3) 0.0882(3) 0.6990(2) 0.0575(10) Uani 1 1 d . . . C33 C 1.4310(3) 0.0958(3) 0.7185(2) 0.0540(9) Uani 1 1 d . . . C34 C 1.3971(4) 0.1676(4) 0.7587(2) 0.0667(11) Uani 1 1 d . . . H34A H 1.4328 0.2067 0.8071 0.080 Uiso 1 1 calc R . . C35 C 1.3110(4) 0.1809(4) 0.7271(2) 0.0676(11) Uani 1 1 d . . . H35A H 1.2879 0.2272 0.7554 0.081 Uiso 1 1 calc R . . C36 C 1.5716(4) 0.1307(4) 0.8234(2) 0.0735(13) Uani 1 1 d . . . H36A H 1.5151 0.1287 0.8472 0.088 Uiso 1 1 calc R . . H36B H 1.6238 0.2064 0.8372 0.088 Uiso 1 1 calc R . . C37 C 1.6267(4) 0.0662(5) 0.8478(3) 0.0907(16) Uani 1 1 d . . . H37A H 1.6566 0.0974 0.8991 0.136 Uiso 1 1 calc R . . H37B H 1.6834 0.0690 0.8249 0.136 Uiso 1 1 calc R . . H37C H 1.5749 -0.0085 0.8350 0.136 Uiso 1 1 calc R . . C38 C 0.4322(3) 0.2013(4) 0.3224(2) 0.0640(11) Uani 1 1 d . . . H38A H 0.4857 0.1811 0.3368 0.077 Uiso 1 1 calc R . . C39 C 0.3338(4) 0.1518(4) 0.3333(2) 0.0670(11) Uani 1 1 d . . . H39A H 0.3199 0.0973 0.3535 0.080 Uiso 1 1 calc R . . C40 C 0.2551(3) 0.1831(3) 0.3144(2) 0.0587(10) Uani 1 1 d . . . H40A H 0.1876 0.1508 0.3222 0.070 Uiso 1 1 calc R . . C41 C 0.2779(3) 0.2636(3) 0.2835(2) 0.0523(9) Uani 1 1 d . . . H41A H 0.2266 0.2875 0.2713 0.063 Uiso 1 1 calc R . . C42 C 0.3783(3) 0.3077(3) 0.27118(18) 0.0443(8) Uani 1 1 d . . . C43 C 0.4074(3) 0.3854(3) 0.23148(18) 0.0443(8) Uani 1 1 d . . . C44 C 0.3367(3) 0.4179(3) 0.19987(19) 0.0468(8) Uani 1 1 d . . . H44A H 0.2668 0.3938 0.2049 0.056 Uiso 1 1 calc R . . C45 C 0.3702(3) 0.4869(3) 0.1604(2) 0.0482(8) Uani 1 1 d . . . C46 C 0.4777(3) 0.5213(3) 0.15530(19) 0.0494(9) Uani 1 1 d . . . H46A H 0.5036 0.5670 0.1295 0.059 Uiso 1 1 calc R . . C47 C 0.5434(3) 0.4864(3) 0.18894(19) 0.0449(8) Uani 1 1 d . . . C48 C 0.6588(3) 0.5174(3) 0.1868(2) 0.0495(8) Uani 1 1 d . . . C49 C 0.7040(3) 0.5707(4) 0.1425(2) 0.0618(10) Uani 1 1 d . . . H49A H 0.6640 0.5901 0.1122 0.074 Uiso 1 1 calc R . . C50 C 0.8097(4) 0.5944(5) 0.1444(3) 0.0802(14) Uani 1 1 d . . . H50A H 0.8426 0.6303 0.1151 0.096 Uiso 1 1 calc R . . C51 C 0.8669(4) 0.5649(5) 0.1899(3) 0.0883(16) Uani 1 1 d . . . H51A H 0.9388 0.5810 0.1920 0.106 Uiso 1 1 calc R . . C52 C 0.8166(3) 0.5119(4) 0.2317(3) 0.0768(14) Uani 1 1 d . . . H52A H 0.8553 0.4917 0.2623 0.092 Uiso 1 1 calc R . . C53 C 0.2984(3) 0.5241(3) 0.1259(2) 0.0501(9) Uani 1 1 d . . . C54 C 0.3112(3) 0.5501(4) 0.0640(2) 0.0608(10) Uani 1 1 d . . . H54A H 0.3649 0.5420 0.0436 0.073 Uiso 1 1 calc R . . C55 C 0.2452(3) 0.5877(4) 0.0328(2) 0.0642(11) Uani 1 1 d . . . H55A H 0.2558 0.6048 -0.0082 0.077 Uiso 1 1 calc R . . C56 C 0.1633(3) 0.6006(3) 0.0612(2) 0.0570(10) Uani 1 1 d . . . C57 C 0.1500(3) 0.5719(4) 0.1218(2) 0.0596(10) Uani 1 1 d . . . H57A H 0.0946 0.5778 0.1412 0.072 Uiso 1 1 calc R . . C58 C 0.2151(3) 0.5353(3) 0.1544(2) 0.0568(10) Uani 1 1 d . . . H58A H 0.2040 0.5179 0.1952 0.068 Uiso 1 1 calc R . . C59 C 0.0929(3) 0.6422(4) 0.0313(2) 0.0647(11) Uani 1 1 d . . . H59A H 0.0395 0.6456 0.0537 0.078 Uiso 1 1 calc R . . C60 C 0.0976(4) 0.6755(4) -0.0245(2) 0.0676(11) Uani 1 1 d . . . H60A H 0.1480 0.6674 -0.0486 0.081 Uiso 1 1 calc R . . C61 C 0.0322(3) 0.7240(4) -0.0526(2) 0.0616(10) Uani 1 1 d . . . C62 C 0.0536(3) 0.7602(4) -0.1092(2) 0.0619(10) Uani 1 1 d . . . H62A H 0.1051 0.7484 -0.1307 0.074 Uiso 1 1 calc R . . C63 C 0.0000(3) 0.8136(4) -0.1346(2) 0.0569(10) Uani 1 1 d . . . C64 C 0.0036(3) 0.9644(4) -0.1941(2) 0.0629(11) Uani 1 1 d . . . C65 C 0.0537(4) 1.0414(5) -0.2243(3) 0.0826(14) Uani 1 1 d . . . H65A H 0.1078 1.0370 -0.2456 0.099 Uiso 1 1 calc R . . C66 C 0.0243(5) 1.1241(5) -0.2230(3) 0.0907(16) Uani 1 1 d . . . H66A H 0.0534 1.1716 -0.2472 0.109 Uiso 1 1 calc R . . C67 C -0.0469(5) 1.1360(4) -0.1864(3) 0.0844(15) Uani 1 1 d . . . H67A H -0.0638 1.1943 -0.1836 0.101 Uiso 1 1 calc R . . C68 C -0.0960(4) 1.0628(4) -0.1527(2) 0.0688(12) Uani 1 1 d . . . H68A H -0.1445 1.0734 -0.1274 0.083 Uiso 1 1 calc R . . C69 C -0.0730(3) 0.9740(3) -0.1567(2) 0.0543(9) Uani 1 1 d . . . C70 C -0.0761(3) 0.8352(3) -0.1026(2) 0.0530(9) Uani 1 1 d . . . C71 C -0.1011(3) 0.7952(4) -0.0483(2) 0.0616(10) Uani 1 1 d . . . H71A H -0.1537 0.8057 -0.0275 0.074 Uiso 1 1 calc R . . C72 C -0.0486(4) 0.7392(4) -0.0243(2) 0.0662(11) Uani 1 1 d . . . H72A H -0.0681 0.7113 0.0115 0.079 Uiso 1 1 calc R . . C73 C -0.2199(3) 0.8976(4) -0.1029(2) 0.0589(10) Uani 1 1 d . . . H73A H -0.2647 0.8249 -0.1036 0.071 Uiso 1 1 calc R . . H73B H -0.2616 0.9135 -0.1375 0.071 Uiso 1 1 calc R . . C74 C -0.1980(4) 0.9765(4) -0.0304(3) 0.0794(13) Uani 1 1 d . . . H74A H -0.2650 0.9711 -0.0205 0.119 Uiso 1 1 calc R . . H74B H -0.1553 1.0493 -0.0289 0.119 Uiso 1 1 calc R . . H74C H -0.1594 0.9601 0.0050 0.119 Uiso 1 1 calc R . . Cl1 Cl 0.39797(14) 0.26324(13) 0.97450(8) 0.0905(4) Uani 1 1 d . . . Cl2 Cl 0.06666(9) 0.47611(11) 0.31264(6) 0.0735(3) Uani 1 1 d . . . O1 O 0.3865(4) 0.2687(5) 1.0417(3) 0.1375(18) Uani 1 1 d . . . O2 O 0.2965(7) 0.2134(12) 0.9299(5) 0.342(8) Uani 1 1 d . . . O3 O 0.4409(6) 0.3527(8) 0.9612(6) 0.260(5) Uani 1 1 d . . . O4 O 0.4450(11) 0.1976(9) 0.9569(5) 0.281(6) Uani 1 1 d . . . O5 O 0.1488(3) 0.4409(4) 0.3083(3) 0.1156(14) Uani 1 1 d . . . O6 O 0.0800(5) 0.5562(6) 0.2848(5) 0.209(4) Uani 1 1 d . . . O7 O 0.0558(8) 0.5059(8) 0.3781(3) 0.240(5) Uani 1 1 d . . . O8 O -0.0323(5) 0.3916(5) 0.2683(4) 0.181(3) Uani 1 1 d . . . C1S C 0.6237(6) 0.3179(8) 0.5978(5) 0.155(3) Uani 1 1 d . . . H1SA H 0.6868 0.3881 0.6157 0.187 Uiso 1 1 calc R . . H1SB H 0.6485 0.2622 0.5966 0.187 Uiso 1 1 calc R . . Cl1S Cl 0.5597(2) 0.2960(2) 0.51220(13) 0.1631(9) Uani 1 1 d . . . Cl2S Cl 0.5452(2) 0.31653(19) 0.65672(12) 0.1411(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0461(2) 0.0583(3) 0.0571(3) 0.0250(2) 0.00774(19) 0.0320(2) S1 0.0583(6) 0.0630(7) 0.0604(6) 0.0227(5) 0.0110(5) 0.0346(5) S2 0.0740(7) 0.0889(8) 0.0678(7) 0.0368(6) 0.0295(6) 0.0533(7) N1 0.0390(15) 0.0538(18) 0.0472(17) 0.0171(14) 0.0080(12) 0.0257(14) N2 0.0554(18) 0.063(2) 0.0467(17) 0.0170(15) 0.0041(14) 0.0328(16) N3 0.0600(19) 0.058(2) 0.065(2) 0.0160(17) 0.0065(16) 0.0377(17) N4 0.0488(17) 0.0573(19) 0.0595(18) 0.0300(16) 0.0124(14) 0.0309(15) N5 0.0400(15) 0.0501(18) 0.0514(17) 0.0231(14) 0.0118(13) 0.0242(14) N6 0.0416(16) 0.067(2) 0.079(2) 0.0385(18) 0.0200(15) 0.0304(16) N7 0.0588(19) 0.077(2) 0.0509(18) 0.0216(17) 0.0050(15) 0.0405(18) N8 0.0546(18) 0.073(2) 0.064(2) 0.0320(18) 0.0156(16) 0.0371(18) C1 0.077(3) 0.080(3) 0.059(3) 0.022(2) -0.002(2) 0.042(3) C2 0.091(3) 0.098(4) 0.049(3) 0.014(3) 0.000(2) 0.047(3) C3 0.077(3) 0.099(4) 0.062(3) 0.004(3) 0.009(2) 0.048(3) C4 0.061(2) 0.077(3) 0.060(2) 0.014(2) 0.0072(19) 0.043(2) C5 0.0444(18) 0.057(2) 0.049(2) 0.0186(18) 0.0096(15) 0.0283(18) C6 0.0391(17) 0.055(2) 0.0482(19) 0.0215(17) 0.0115(14) 0.0263(17) C7 0.0448(19) 0.056(2) 0.052(2) 0.0201(18) 0.0131(16) 0.0304(18) C8 0.0402(18) 0.059(2) 0.054(2) 0.0275(18) 0.0119(15) 0.0256(17) C9 0.049(2) 0.063(2) 0.047(2) 0.0213(18) 0.0079(16) 0.0277(19) C10 0.0440(18) 0.056(2) 0.046(2) 0.0186(17) 0.0106(15) 0.0265(17) C11 0.049(2) 0.053(2) 0.056(2) 0.0162(19) 0.0083(17) 0.0253(18) C12 0.086(3) 0.074(3) 0.057(3) 0.016(2) 0.008(2) 0.045(3) C13 0.110(4) 0.081(4) 0.077(3) 0.004(3) 0.018(3) 0.056(3) C14 0.116(5) 0.090(4) 0.095(4) 0.004(3) 0.017(3) 0.072(4) C15 0.088(3) 0.075(3) 0.092(4) 0.014(3) 0.005(3) 0.057(3) C16 0.0458(19) 0.064(3) 0.058(2) 0.028(2) 0.0098(17) 0.0292(19) C17 0.067(3) 0.091(3) 0.061(2) 0.030(2) 0.013(2) 0.054(3) C18 0.075(3) 0.098(4) 0.069(3) 0.031(3) 0.017(2) 0.062(3) C19 0.061(2) 0.081(3) 0.072(3) 0.035(2) 0.017(2) 0.047(2) C20 0.082(3) 0.105(4) 0.060(3) 0.039(3) 0.017(2) 0.060(3) C21 0.073(3) 0.095(3) 0.059(2) 0.036(2) 0.022(2) 0.058(3) C22 0.078(3) 0.089(3) 0.068(3) 0.034(2) 0.016(2) 0.055(3) C23 0.067(3) 0.087(3) 0.070(3) 0.040(2) 0.021(2) 0.050(3) C24 0.059(2) 0.068(3) 0.064(2) 0.031(2) 0.0158(19) 0.040(2) C25 0.055(2) 0.069(3) 0.053(2) 0.027(2) 0.0083(17) 0.034(2) C26 0.053(2) 0.059(2) 0.057(2) 0.0271(19) 0.0139(17) 0.0324(19) C27 0.055(2) 0.062(2) 0.059(2) 0.031(2) 0.0117(18) 0.034(2) C28 0.070(3) 0.083(3) 0.069(3) 0.043(2) 0.021(2) 0.043(3) C29 0.074(3) 0.106(4) 0.094(4) 0.063(3) 0.040(3) 0.047(3) C30 0.057(3) 0.094(4) 0.113(4) 0.057(4) 0.021(3) 0.026(3) C31 0.059(3) 0.075(3) 0.086(3) 0.029(3) 0.005(2) 0.027(2) C32 0.056(2) 0.058(2) 0.069(3) 0.031(2) 0.0112(19) 0.032(2) C33 0.054(2) 0.062(2) 0.056(2) 0.0265(19) 0.0086(17) 0.034(2) C34 0.072(3) 0.079(3) 0.055(2) 0.020(2) 0.006(2) 0.046(2) C35 0.073(3) 0.079(3) 0.068(3) 0.024(2) 0.016(2) 0.052(3) C36 0.065(3) 0.098(4) 0.057(3) 0.021(2) 0.001(2) 0.046(3) C37 0.083(3) 0.134(5) 0.080(3) 0.053(3) 0.013(3) 0.065(4) C38 0.064(3) 0.072(3) 0.082(3) 0.047(2) 0.021(2) 0.042(2) C39 0.071(3) 0.068(3) 0.080(3) 0.046(2) 0.021(2) 0.035(2) C40 0.058(2) 0.063(3) 0.063(2) 0.031(2) 0.0226(19) 0.027(2) C41 0.047(2) 0.059(2) 0.062(2) 0.028(2) 0.0169(17) 0.0289(19) C42 0.0445(18) 0.047(2) 0.0467(19) 0.0184(16) 0.0092(15) 0.0250(17) C43 0.0430(18) 0.047(2) 0.0466(19) 0.0172(16) 0.0089(15) 0.0245(16) C44 0.0406(18) 0.053(2) 0.057(2) 0.0257(18) 0.0125(15) 0.0274(17) C45 0.0465(19) 0.053(2) 0.054(2) 0.0227(18) 0.0092(16) 0.0294(18) C46 0.051(2) 0.056(2) 0.053(2) 0.0272(18) 0.0159(16) 0.0295(18) C47 0.0419(18) 0.047(2) 0.052(2) 0.0209(17) 0.0104(15) 0.0245(16) C48 0.0431(19) 0.049(2) 0.063(2) 0.0231(18) 0.0153(16) 0.0240(17) C49 0.056(2) 0.070(3) 0.072(3) 0.035(2) 0.023(2) 0.031(2) C50 0.067(3) 0.095(4) 0.097(4) 0.046(3) 0.044(3) 0.038(3) C51 0.052(3) 0.105(4) 0.131(5) 0.058(4) 0.040(3) 0.041(3) C52 0.045(2) 0.088(4) 0.112(4) 0.050(3) 0.023(2) 0.034(2) C53 0.049(2) 0.056(2) 0.053(2) 0.0238(18) 0.0095(16) 0.0303(18) C54 0.062(2) 0.077(3) 0.066(3) 0.036(2) 0.021(2) 0.044(2) C55 0.071(3) 0.084(3) 0.058(2) 0.038(2) 0.015(2) 0.047(2) C56 0.050(2) 0.058(2) 0.066(2) 0.025(2) 0.0033(18) 0.0284(19) C57 0.047(2) 0.076(3) 0.072(3) 0.035(2) 0.0178(19) 0.037(2) C58 0.049(2) 0.072(3) 0.067(2) 0.038(2) 0.0178(18) 0.035(2) C59 0.056(2) 0.076(3) 0.071(3) 0.032(2) 0.004(2) 0.037(2) C60 0.065(3) 0.072(3) 0.076(3) 0.034(2) 0.012(2) 0.038(2) C61 0.058(2) 0.063(3) 0.067(3) 0.026(2) 0.005(2) 0.032(2) C62 0.059(2) 0.072(3) 0.064(3) 0.026(2) 0.0098(19) 0.039(2) C63 0.054(2) 0.069(3) 0.058(2) 0.026(2) 0.0128(18) 0.035(2) C64 0.061(2) 0.074(3) 0.062(2) 0.030(2) 0.015(2) 0.034(2) C65 0.084(3) 0.087(4) 0.083(3) 0.038(3) 0.039(3) 0.032(3) C66 0.120(5) 0.076(4) 0.103(4) 0.053(3) 0.056(4) 0.048(3) C67 0.111(4) 0.069(3) 0.091(4) 0.041(3) 0.025(3) 0.049(3) C68 0.074(3) 0.075(3) 0.073(3) 0.032(2) 0.022(2) 0.044(3) C69 0.056(2) 0.060(2) 0.052(2) 0.0233(19) 0.0088(17) 0.031(2) C70 0.049(2) 0.059(2) 0.054(2) 0.0242(19) 0.0055(16) 0.0256(19) C71 0.051(2) 0.077(3) 0.065(3) 0.033(2) 0.0151(19) 0.032(2) C72 0.068(3) 0.070(3) 0.066(3) 0.037(2) 0.010(2) 0.030(2) C73 0.054(2) 0.067(3) 0.066(3) 0.027(2) 0.0192(19) 0.033(2) C74 0.085(3) 0.079(3) 0.086(3) 0.031(3) 0.038(3) 0.042(3) Cl1 0.1251(12) 0.1026(10) 0.0813(8) 0.0584(8) 0.0486(8) 0.0632(9) Cl2 0.0664(7) 0.0957(9) 0.0661(7) 0.0314(6) 0.0159(5) 0.0417(7) O1 0.157(4) 0.162(5) 0.108(3) 0.069(3) 0.067(3) 0.059(4) O2 0.172(7) 0.485(18) 0.234(9) 0.212(11) -0.054(6) -0.013(9) O3 0.183(6) 0.347(11) 0.459(14) 0.360(11) 0.176(8) 0.152(7) O4 0.519(17) 0.324(11) 0.203(7) 0.113(8) 0.157(10) 0.356(13) O5 0.089(3) 0.118(3) 0.158(4) 0.046(3) 0.030(3) 0.066(3) O6 0.174(6) 0.235(7) 0.383(11) 0.241(8) 0.157(7) 0.140(6) O7 0.374(11) 0.399(12) 0.094(4) 0.076(5) 0.080(5) 0.318(11) O8 0.121(4) 0.141(5) 0.228(7) -0.002(5) -0.023(4) 0.073(4) C1S 0.087(5) 0.172(8) 0.203(9) 0.086(7) 0.010(5) 0.048(5) Cl1S 0.175(2) 0.194(2) 0.1257(16) 0.0453(16) 0.0580(16) 0.0881(19) Cl2S 0.185(2) 0.1526(18) 0.1371(16) 0.0752(14) 0.0666(15) 0.1020(17) _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 N5 2.076(3) . ? Zn1 N1 2.082(3) . ? Zn1 N2 2.185(3) . ? Zn1 N3 2.186(3) . ? Zn1 N6 2.201(3) . ? Zn1 N4 2.216(3) . ? S1 C27 1.769(4) . ? S1 C26 1.773(4) . ? S2 C64 1.751(5) . ? S2 C63 1.771(4) . ? N1 C6 1.337(5) . ? N1 C10 1.342(4) . ? N2 C5 1.340(4) . ? N2 C1 1.342(5) . ? N3 C15 1.342(5) . ? N3 C11 1.345(5) . ? N4 C38 1.339(5) . ? N4 C42 1.345(4) . ? N5 C47 1.334(4) . ? N5 C43 1.343(4) . ? N6 C52 1.326(5) . ? N6 C48 1.340(5) . ? N7 C33 1.411(5) . ? N7 C32 1.416(5) . ? N7 C36 1.479(5) . ? N8 C69 1.407(5) . ? N8 C70 1.425(5) . ? N8 C73 1.457(5) . ? C1 C2 1.350(7) . ? C1 H1A 0.9300 . ? C2 C3 1.389(7) . ? C2 H2A 0.9300 . ? C3 C4 1.379(6) . ? C3 H3A 0.9300 . ? C4 C5 1.376(6) . ? C4 H4A 0.9300 . ? C5 C6 1.491(5) . ? C6 C7 1.377(5) . ? C7 C8 1.400(5) . ? C7 H7A 0.9300 . ? C8 C9 1.391(5) . ? C8 C16 1.486(5) . ? C9 C10 1.386(5) . ? C9 H9A 0.9300 . ? C10 C11 1.482(5) . ? C11 C12 1.384(6) . ? C12 C13 1.381(7) . ? C12 H12A 0.9300 . ? C13 C14 1.359(8) . ? C13 H13A 0.9300 . ? C14 C15 1.394(7) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.385(6) . ? C16 C21 1.391(6) . ? C17 C18 1.373(6) . ? C17 H17A 0.9300 . ? C18 C19 1.385(6) . ? C18 H18A 0.9300 . ? C19 C20 1.368(6) . ? C19 C22 1.474(5) . ? C20 C21 1.390(6) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.312(6) . ? C22 H22A 0.9300 . ? C23 C24 1.479(5) . ? C23 H23A 0.9300 . ? C24 C35 1.372(6) . ? C24 C25 1.398(6) . ? C25 C26 1.379(5) . ? C25 H25A 0.9300 . ? C26 C33 1.393(5) . ? C27 C28 1.389(6) . ? C27 C32 1.393(6) . ? C28 C29 1.366(7) . ? C28 H28A 0.9300 . ? C29 C30 1.366(8) . ? C29 H29A 0.9300 . ? C30 C31 1.401(7) . ? C30 H30A 0.9300 . ? C31 C32 1.384(6) . ? C31 H31A 0.9300 . ? C33 C34 1.390(6) . ? C34 C35 1.379(6) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 C37 1.524(6) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.358(6) . ? C38 H38A 0.9300 . ? C39 C40 1.371(6) . ? C39 H39A 0.9300 . ? C40 C41 1.387(5) . ? C40 H40A 0.9300 . ? C41 C42 1.382(5) . ? C41 H41A 0.9300 . ? C42 C43 1.487(5) . ? C43 C44 1.380(4) . ? C44 C45 1.397(5) . ? C44 H44A 0.9300 . ? C45 C46 1.413(5) . ? C45 C53 1.468(5) . ? C46 C47 1.373(5) . ? C46 H46A 0.9300 . ? C47 C48 1.505(5) . ? C48 C49 1.376(5) . ? C49 C50 1.371(6) . ? C49 H49A 0.9300 . ? C50 C51 1.375(7) . ? C50 H50A 0.9300 . ? C51 C52 1.357(7) . ? C51 H51A 0.9300 . ? C52 H52A 0.9300 . ? C53 C54 1.397(5) . ? C53 C58 1.403(5) . ? C54 C55 1.380(5) . ? C54 H54A 0.9300 . ? C55 C56 1.393(6) . ? C55 H55A 0.9300 . ? C56 C57 1.392(6) . ? C56 C59 1.458(5) . ? C57 C58 1.374(5) . ? C57 H57A 0.9300 . ? C58 H58A 0.9300 . ? C59 C60 1.322(6) . ? C59 H59A 0.9300 . ? C60 C61 1.468(5) . ? C60 H60A 0.9300 . ? C61 C62 1.385(6) . ? C61 C72 1.388(6) . ? C62 C63 1.382(5) . ? C62 H62A 0.9300 . ? C63 C70 1.399(5) . ? C64 C65 1.383(6) . ? C64 C69 1.411(6) . ? C65 C66 1.373(7) . ? C65 H65A 0.9300 . ? C66 C67 1.345(8) . ? C66 H66A 0.9300 . ? C67 C68 1.394(7) . ? C67 H67A 0.9300 . ? C68 C69 1.394(6) . ? C68 H68A 0.9300 . ? C70 C71 1.378(5) . ? C71 C72 1.391(6) . ? C71 H71A 0.9300 . ? C72 H72A 0.9300 . ? C73 C74 1.483(6) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? Cl1 O3 1.292(6) . ? Cl1 O4 1.329(7) . ? Cl1 O2 1.358(8) . ? Cl1 O1 1.361(4) . ? Cl2 O7 1.315(5) . ? Cl2 O6 1.351(5) . ? Cl2 O8 1.398(6) . ? Cl2 O5 1.415(4) . ? C1S Cl1S 1.707(9) . ? C1S Cl2S 1.714(9) . ? C1S H1SA 0.9700 . ? C1S H1SB 0.9700 . ? 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 Zn1 N1 177.83(11) . . ? N5 Zn1 N2 106.61(11) . . ? N1 Zn1 N2 74.85(11) . . ? N5 Zn1 N3 103.15(12) . . ? N1 Zn1 N3 75.45(12) . . ? N2 Zn1 N3 150.18(11) . . ? N5 Zn1 N6 75.47(11) . . ? N1 Zn1 N6 106.28(11) . . ? N2 Zn1 N6 88.93(13) . . ? N3 Zn1 N6 96.75(14) . . ? N5 Zn1 N4 74.94(11) . . ? N1 Zn1 N4 103.39(11) . . ? N2 Zn1 N4 96.23(12) . . ? N3 Zn1 N4 93.20(13) . . ? N6 Zn1 N4 150.21(11) . . ? C27 S1 C26 95.59(19) . . ? C64 S2 C63 99.5(2) . . ? C6 N1 C10 120.2(3) . . ? C6 N1 Zn1 120.4(2) . . ? C10 N1 Zn1 119.4(2) . . ? C5 N2 C1 118.5(4) . . ? C5 N2 Zn1 116.0(2) . . ? C1 N2 Zn1 125.3(3) . . ? C15 N3 C11 118.8(4) . . ? C15 N3 Zn1 125.8(3) . . ? C11 N3 Zn1 115.4(2) . . ? C38 N4 C42 118.7(3) . . ? C38 N4 Zn1 126.6(3) . . ? C42 N4 Zn1 114.5(2) . . ? C47 N5 C43 119.8(3) . . ? C47 N5 Zn1 120.1(2) . . ? C43 N5 Zn1 120.2(2) . . ? C52 N6 C48 118.7(4) . . ? C52 N6 Zn1 125.6(3) . . ? C48 N6 Zn1 114.5(2) . . ? C33 N7 C32 115.7(3) . . ? C33 N7 C36 116.9(3) . . ? C32 N7 C36 119.0(3) . . ? C69 N8 C70 121.2(3) . . ? C69 N8 C73 118.2(3) . . ? C70 N8 C73 118.4(3) . . ? N2 C1 C2 123.0(4) . . ? N2 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 118.8(4) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 118.7(5) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? N2 C5 C4 121.5(3) . . ? N2 C5 C6 114.9(3) . . ? C4 C5 C6 123.5(3) . . ? N1 C6 C7 121.4(3) . . ? N1 C6 C5 113.7(3) . . ? C7 C6 C5 124.8(3) . . ? C6 C7 C8 119.9(3) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 117.3(3) . . ? C9 C8 C16 121.6(3) . . ? C7 C8 C16 121.1(3) . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? N1 C10 C9 120.9(3) . . ? N1 C10 C11 114.6(3) . . ? C9 C10 C11 124.5(3) . . ? N3 C11 C12 122.1(4) . . ? N3 C11 C10 115.1(3) . . ? C12 C11 C10 122.8(3) . . ? C13 C12 C11 118.8(4) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C14 C13 C12 119.3(5) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C13 C14 C15 119.7(5) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? N3 C15 C14 121.3(5) . . ? N3 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? C17 C16 C21 117.7(3) . . ? C17 C16 C8 121.2(3) . . ? C21 C16 C8 121.1(4) . . ? C18 C17 C16 120.7(4) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C17 C18 C19 122.4(4) . . ? C17 C18 H18A 118.8 . . ? C19 C18 H18A 118.8 . . ? C20 C19 C18 116.6(4) . . ? C20 C19 C22 125.0(4) . . ? C18 C19 C22 118.5(4) . . ? C19 C20 C21 122.5(4) . . ? C19 C20 H20A 118.8 . . ? C21 C20 H20A 118.8 . . ? C20 C21 C16 120.1(4) . . ? C20 C21 H21A 119.9 . . ? C16 C21 H21A 119.9 . . ? C23 C22 C19 126.7(4) . . ? C23 C22 H22A 116.7 . . ? C19 C22 H22A 116.7 . . ? C22 C23 C24 125.8(4) . . ? C22 C23 H23A 117.1 . . ? C24 C23 H23A 117.1 . . ? C35 C24 C25 117.6(3) . . ? C35 C24 C23 119.9(4) . . ? C25 C24 C23 122.4(4) . . ? C26 C25 C24 120.4(4) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C26 C33 121.5(4) . . ? C25 C26 S1 120.7(3) . . ? C33 C26 S1 117.8(3) . . ? C28 C27 C32 120.6(4) . . ? C28 C27 S1 121.3(3) . . ? C32 C27 S1 118.1(3) . . ? C29 C28 C27 120.6(5) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C30 C29 C28 119.7(5) . . ? C30 C29 H29A 120.2 . . ? C28 C29 H29A 120.2 . . ? C29 C30 C31 120.5(5) . . ? C29 C30 H30A 119.7 . . ? C31 C30 H30A 119.7 . . ? C32 C31 C30 120.3(5) . . ? C32 C31 H31A 119.8 . . ? C30 C31 H31A 119.8 . . ? C31 C32 C27 118.2(4) . . ? C31 C32 N7 123.3(4) . . ? C27 C32 N7 118.4(4) . . ? C34 C33 C26 117.5(3) . . ? C34 C33 N7 123.9(4) . . ? C26 C33 N7 118.5(3) . . ? C35 C34 C33 120.4(4) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C24 C35 C34 122.3(4) . . ? C24 C35 H35A 118.9 . . ? C34 C35 H35A 118.9 . . ? N7 C36 C37 111.3(4) . . ? N7 C36 H36A 109.4 . . ? C37 C36 H36A 109.4 . . ? N7 C36 H36B 109.4 . . ? C37 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 C39 122.6(4) . . ? N4 C38 H38A 118.7 . . ? C39 C38 H38A 118.7 . . ? C38 C39 C40 119.4(4) . . ? C38 C39 H39A 120.3 . . ? C40 C39 H39A 120.3 . . ? C39 C40 C41 118.9(4) . . ? C39 C40 H40A 120.5 . . ? C41 C40 H40A 120.5 . . ? C42 C41 C40 118.8(3) . . ? C42 C41 H41A 120.6 . . ? C40 C41 H41A 120.6 . . ? N4 C42 C41 121.4(3) . . ? N4 C42 C43 115.2(3) . . ? C41 C42 C43 123.4(3) . . ? N5 C43 C44 121.4(3) . . ? N5 C43 C42 114.3(3) . . ? C44 C43 C42 124.3(3) . . ? C43 C44 C45 120.0(3) . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C44 C45 C46 117.2(3) . . ? C44 C45 C53 122.2(3) . . ? C46 C45 C53 120.6(3) . . ? C47 C46 C45 119.3(3) . . ? C47 C46 H46A 120.4 . . ? C45 C46 H46A 120.4 . . ? N5 C47 C46 122.3(3) . . ? N5 C47 C48 113.9(3) . . ? C46 C47 C48 123.8(3) . . ? N6 C48 C49 122.2(3) . . ? N6 C48 C47 115.1(3) . . ? C49 C48 C47 122.7(3) . . ? C50 C49 C48 118.0(4) . . ? C50 C49 H49A 121.0 . . ? C48 C49 H49A 121.0 . . ? C49 C50 C51 119.7(4) . . ? C49 C50 H50A 120.1 . . ? C51 C50 H50A 120.1 . . ? C52 C51 C50 118.9(4) . . ? C52 C51 H51A 120.6 . . ? C50 C51 H51A 120.6 . . ? N6 C52 C51 122.5(4) . . ? N6 C52 H52A 118.7 . . ? C51 C52 H52A 118.7 . . ? C54 C53 C58 117.9(3) . . ? C54 C53 C45 121.1(3) . . ? C58 C53 C45 121.0(3) . . ? C55 C54 C53 120.9(4) . . ? C55 C54 H54A 119.6 . . ? C53 C54 H54A 119.6 . . ? C54 C55 C56 121.7(4) . . ? C54 C55 H55A 119.1 . . ? C56 C55 H55A 119.1 . . ? C57 C56 C55 116.7(3) . . ? C57 C56 C59 119.4(4) . . ? C55 C56 C59 124.0(4) . . ? C58 C57 C56 122.8(4) . . ? C58 C57 H57A 118.6 . . ? C56 C57 H57A 118.6 . . ? C57 C58 C53 120.0(4) . . ? C57 C58 H58A 120.0 . . ? C53 C58 H58A 120.0 . . ? C60 C59 C56 126.4(4) . . ? C60 C59 H59A 116.8 . . ? C56 C59 H59A 116.8 . . ? C59 C60 C61 127.3(4) . . ? C59 C60 H60A 116.4 . . ? C61 C60 H60A 116.4 . . ? C62 C61 C72 117.3(4) . . ? C62 C61 C60 118.8(4) . . ? C72 C61 C60 123.9(4) . . ? C63 C62 C61 121.4(4) . . ? C63 C62 H62A 119.3 . . ? C61 C62 H62A 119.3 . . ? C62 C63 C70 120.8(4) . . ? C62 C63 S2 118.4(3) . . ? C70 C63 S2 120.7(3) . . ? C65 C64 C69 120.7(4) . . ? C65 C64 S2 119.1(4) . . ? C69 C64 S2 119.8(3) . . ? C66 C65 C64 120.7(5) . . ? C66 C65 H65A 119.7 . . ? C64 C65 H65A 119.7 . . ? C67 C66 C65 119.4(5) . . ? C67 C66 H66A 120.3 . . ? C65 C66 H66A 120.3 . . ? C66 C67 C68 121.6(5) . . ? C66 C67 H67A 119.2 . . ? C68 C67 H67A 119.2 . . ? C69 C68 C67 120.4(4) . . ? C69 C68 H68A 119.8 . . ? C67 C68 H68A 119.8 . . ? C68 C69 N8 121.5(4) . . ? C68 C69 C64 117.0(4) . . ? N8 C69 C64 121.5(4) . . ? C71 C70 C63 118.0(4) . . ? C71 C70 N8 121.9(4) . . ? C63 C70 N8 120.1(3) . . ? C70 C71 C72 120.6(4) . . ? C70 C71 H71A 119.7 . . ? C72 C71 H71A 119.7 . . ? C61 C72 C71 121.7(4) . . ? C61 C72 H72A 119.2 . . ? C71 C72 H72A 119.2 . . ? N8 C73 C74 116.8(4) . . ? N8 C73 H73A 108.1 . . ? C74 C73 H73A 108.1 . . ? N8 C73 H73B 108.1 . . ? C74 C73 H73B 108.1 . . ? H73A C73 H73B 107.3 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O3 Cl1 O4 113.6(6) . . ? O3 Cl1 O2 102.5(6) . . ? O4 Cl1 O2 107.9(9) . . ? O3 Cl1 O1 119.2(6) . . ? O4 Cl1 O1 106.6(4) . . ? O2 Cl1 O1 106.3(5) . . ? O7 Cl2 O6 110.5(6) . . ? O7 Cl2 O8 107.8(6) . . ? O6 Cl2 O8 102.9(5) . . ? O7 Cl2 O5 113.3(4) . . ? O6 Cl2 O5 112.1(3) . . ? O8 Cl2 O5 109.7(3) . . ? Cl1S C1S Cl2S 114.3(4) . . ? Cl1S C1S H1SA 108.7 . . ? Cl2S C1S H1SA 108.7 . . ? Cl1S C1S H1SB 108.7 . . ? Cl2S C1S H1SB 108.7 . . ? H1SA C1S H1SB 107.6 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.800 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.072 # Attachment 'ldm6.cif' data_p1bar_6 _database_code_depnum_ccdc_archive 'CCDC 700929' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37.50 H29 Cl2 Mn0.50 N4 O4 S' _chemical_formula_sum 'C37.50 H29 Cl2 Mn0.50 N4 O4 S' _chemical_formula_weight 730.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 14.0610(3) _cell_length_b 14.1018(3) _cell_length_c 19.9266(7) _cell_angle_alpha 104.860(2) _cell_angle_beta 97.678(2) _cell_angle_gamma 112.8040(10) _cell_volume 3397.99(16) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9952 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 23.54 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1506 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADBS;Bruker,2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63393 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.52 _reflns_number_total 15562 _reflns_number_gt 10091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1308P)^2^+2.1056P] 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 15562 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2412 _refine_ls_wR_factor_gt 0.2106 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.38351(4) 0.62768(4) 0.22235(3) 0.04911(17) Uani 1 1 d . . . S1 S 0.97946(9) 0.15400(9) 0.71518(6) 0.0629(3) Uani 1 1 d . . . S2 S -0.41391(8) 1.06227(8) -0.09953(5) 0.0543(2) Uani 1 1 d . . . N1 N 0.5490(2) 0.7235(2) 0.21092(17) 0.0512(7) Uani 1 1 d . . . N2 N 0.4935(2) 0.5771(2) 0.27460(14) 0.0422(6) Uani 1 1 d . . . N3 N 0.2916(2) 0.5112(3) 0.27471(18) 0.0568(8) Uani 1 1 d . . . N4 N 1.1257(2) 0.1043(3) 0.62819(16) 0.0517(7) Uani 1 1 d . . . N5 N 0.3193(3) 0.5135(3) 0.10743(18) 0.0609(8) Uani 1 1 d . . . N6 N 0.2774(2) 0.6780(2) 0.16502(15) 0.0439(6) Uani 1 1 d . . . N7 N 0.3712(3) 0.7643(3) 0.30271(16) 0.0567(8) Uani 1 1 d . . . N8 N -0.5292(2) 0.9139(3) -0.24606(17) 0.0566(8) Uani 1 1 d . . . C1 C 0.5728(3) 0.8013(4) 0.1800(2) 0.0644(10) Uani 1 1 d . . . H1A H 0.5207 0.8228 0.1664 0.077 Uiso 1 1 calc R . . C2 C 0.6713(4) 0.8500(3) 0.1676(2) 0.0673(11) Uani 1 1 d . . . H2A H 0.6863 0.9056 0.1478 0.081 Uiso 1 1 calc R . . C3 C 0.7474(3) 0.8151(3) 0.1849(2) 0.0564(9) Uani 1 1 d . . . H3A H 0.8139 0.8454 0.1759 0.068 Uiso 1 1 calc R . . C4 C 0.7231(3) 0.7342(3) 0.21606(19) 0.0506(8) Uani 1 1 d . . . H4A H 0.7728 0.7088 0.2277 0.061 Uiso 1 1 calc R . . C5 C 0.6241(3) 0.6917(3) 0.22960(17) 0.0434(7) Uani 1 1 d . . . C6 C 0.5946(2) 0.6130(3) 0.26938(17) 0.0419(7) Uani 1 1 d . . . C7 C 0.6653(3) 0.5812(3) 0.30149(18) 0.0452(7) Uani 1 1 d . . . H7A H 0.7347 0.6062 0.2966 0.054 Uiso 1 1 calc R . . C8 C 0.6323(3) 0.5120(3) 0.34107(18) 0.0436(7) Uani 1 1 d . . . C9 C 0.5270(3) 0.4768(3) 0.34668(18) 0.0467(7) Uani 1 1 d . . . H9A H 0.5019 0.4304 0.3727 0.056 Uiso 1 1 calc R . . C10 C 0.4600(3) 0.5116(3) 0.31319(18) 0.0439(7) Uani 1 1 d . . . C11 C 0.3472(3) 0.4802(3) 0.3168(2) 0.0484(8) Uani 1 1 d . . . C12 C 0.3036(3) 0.4255(3) 0.3615(2) 0.0601(9) Uani 1 1 d . . . H12A H 0.3437 0.4049 0.3905 0.072 Uiso 1 1 calc R . . C13 C 0.1985(4) 0.4019(4) 0.3623(3) 0.0757(12) Uani 1 1 d . . . H13A H 0.1673 0.3659 0.3924 0.091 Uiso 1 1 calc R . . C14 C 0.1419(4) 0.4317(4) 0.3190(3) 0.0817(14) Uani 1 1 d . . . H14A H 0.0709 0.4150 0.3183 0.098 Uiso 1 1 calc R . . C15 C 0.1894(3) 0.4870(4) 0.2757(3) 0.0775(13) Uani 1 1 d . . . H15A H 0.1500 0.5080 0.2465 0.093 Uiso 1 1 calc R . . C16 C 0.7042(3) 0.4750(3) 0.37582(19) 0.0472(7) Uani 1 1 d . . . C17 C 0.7872(3) 0.4648(3) 0.3467(2) 0.0531(8) Uani 1 1 d . . . H17A H 0.7980 0.4830 0.3058 0.064 Uiso 1 1 calc R . . C18 C 0.8518(3) 0.4281(3) 0.3783(2) 0.0547(9) Uani 1 1 d . . . H18A H 0.9064 0.4225 0.3585 0.066 Uiso 1 1 calc R . . C19 C 0.8381(3) 0.3988(3) 0.4397(2) 0.0529(8) Uani 1 1 d . . . C20 C 0.7571(3) 0.4108(4) 0.4685(2) 0.0595(9) Uani 1 1 d . . . H20A H 0.7471 0.3937 0.5099 0.071 Uiso 1 1 calc R . . C21 C 0.6911(3) 0.4476(3) 0.4373(2) 0.0542(9) Uani 1 1 d . . . H21A H 0.6371 0.4541 0.4576 0.065 Uiso 1 1 calc R . . C22 C 0.9078(3) 0.3568(3) 0.4695(2) 0.0581(9) Uani 1 1 d . . . H22A H 0.9600 0.3528 0.4464 0.070 Uiso 1 1 calc R . . C23 C 0.9042(3) 0.3240(3) 0.5259(2) 0.0625(10) Uani 1 1 d . . . H23A H 0.8547 0.3324 0.5505 0.075 Uiso 1 1 calc R . . C24 C 0.9687(3) 0.2762(3) 0.5542(2) 0.0561(9) Uani 1 1 d . . . C25 C 1.0482(3) 0.2606(3) 0.5254(2) 0.0620(10) Uani 1 1 d . . . H25A H 1.0670 0.2885 0.4892 0.074 Uiso 1 1 calc R . . C26 C 1.1003(3) 0.2050(3) 0.5487(2) 0.0565(9) Uani 1 1 d . . . H26A H 1.1520 0.1948 0.5273 0.068 Uiso 1 1 calc R . . C27 C 1.0758(3) 0.1640(3) 0.60436(19) 0.0497(8) Uani 1 1 d . . . C28 C 1.0017(3) 0.1869(3) 0.63716(19) 0.0517(8) Uani 1 1 d . . . C29 C 0.9473(3) 0.2393(3) 0.6120(2) 0.0574(9) Uani 1 1 d . . . H29A H 0.8960 0.2503 0.6336 0.069 Uiso 1 1 calc R . . C30 C 0.9981(3) 0.0346(3) 0.6963(2) 0.0573(9) Uani 1 1 d . . . C31 C 0.9481(4) -0.0422(4) 0.7267(2) 0.0753(12) Uani 1 1 d . . . H31A H 0.8950 -0.0373 0.7487 0.090 Uiso 1 1 calc R . . C32 C 0.9759(5) -0.1264(4) 0.7250(3) 0.0848(15) Uani 1 1 d . . . H32A H 0.9466 -0.1742 0.7494 0.102 Uiso 1 1 calc R . . C33 C 1.0462(5) -0.1386(4) 0.6874(3) 0.0812(13) Uani 1 1 d . . . H33A H 1.0623 -0.1974 0.6842 0.097 Uiso 1 1 calc R . . C34 C 1.0951(3) -0.0646(3) 0.6535(2) 0.0643(10) Uani 1 1 d . . . H34A H 1.1430 -0.0747 0.6278 0.077 Uiso 1 1 calc R . . C35 C 1.0726(3) 0.0246(3) 0.65789(19) 0.0503(8) Uani 1 1 d . . . C36 C 1.2183(3) 0.1023(3) 0.6028(2) 0.0542(8) Uani 1 1 d . . . H36A H 1.2601 0.0859 0.6370 0.065 Uiso 1 1 calc R . . H36B H 1.2627 0.1749 0.6030 0.065 Uiso 1 1 calc R . . C37 C 1.1936(4) 0.0223(4) 0.5293(3) 0.0730(12) Uani 1 1 d . . . H37A H 1.2592 0.0271 0.5178 0.109 Uiso 1 1 calc R . . H37B H 1.1545 0.0390 0.4945 0.109 Uiso 1 1 calc R . . H37C H 1.1515 -0.0504 0.5286 0.109 Uiso 1 1 calc R . . C38 C 0.3452(4) 0.4322(4) 0.0802(3) 0.0863(15) Uani 1 1 d . . . H38A H 0.3915 0.4196 0.1107 0.104 Uiso 1 1 calc R . . C39 C 0.3065(5) 0.3670(4) 0.0094(3) 0.0962(17) Uani 1 1 d . . . H39A H 0.3277 0.3126 -0.0079 0.115 Uiso 1 1 calc R . . C40 C 0.2365(5) 0.3830(4) -0.0353(3) 0.0901(15) Uani 1 1 d . . . H40A H 0.2090 0.3393 -0.0835 0.108 Uiso 1 1 calc R . . C41 C 0.2068(4) 0.4642(4) -0.0087(2) 0.0686(11) Uani 1 1 d . . . H41A H 0.1576 0.4750 -0.0381 0.082 Uiso 1 1 calc R . . C42 C 0.2515(3) 0.5298(3) 0.06283(19) 0.0500(8) Uani 1 1 d . . . C43 C 0.2278(3) 0.6230(3) 0.09468(18) 0.0456(7) Uani 1 1 d . . . C44 C 0.1606(3) 0.6528(3) 0.05724(19) 0.0496(8) Uani 1 1 d . . . H44A H 0.1262 0.6129 0.0089 0.060 Uiso 1 1 calc R . . C45 C 0.1442(3) 0.7423(3) 0.09152(19) 0.0465(7) Uani 1 1 d . . . C46 C 0.1974(3) 0.7981(3) 0.16379(19) 0.0468(7) Uani 1 1 d . . . H46A H 0.1894 0.8590 0.1885 0.056 Uiso 1 1 calc R . . C47 C 0.2621(3) 0.7637(3) 0.19924(18) 0.0434(7) Uani 1 1 d . . . C48 C 0.3165(3) 0.8135(3) 0.27805(18) 0.0474(8) Uani 1 1 d . . . C49 C 0.3083(3) 0.9001(4) 0.3234(2) 0.0649(10) Uani 1 1 d . . . H49A H 0.2726 0.9353 0.3053 0.078 Uiso 1 1 calc R . . C50 C 0.3543(4) 0.9343(5) 0.3968(3) 0.0850(15) Uani 1 1 d . . . H50A H 0.3493 0.9922 0.4287 0.102 Uiso 1 1 calc R . . C51 C 0.4070(4) 0.8808(5) 0.4214(2) 0.0837(14) Uani 1 1 d . . . H51A H 0.4373 0.9014 0.4704 0.100 Uiso 1 1 calc R . . C52 C 0.4146(4) 0.7980(4) 0.3739(2) 0.0748(12) Uani 1 1 d . . . H52A H 0.4512 0.7629 0.3911 0.090 Uiso 1 1 calc R . . C53 C 0.0725(3) 0.7762(3) 0.0530(2) 0.0513(8) Uani 1 1 d . . . C54 C 0.0463(4) 0.7461(4) -0.0223(2) 0.0663(11) Uani 1 1 d . . . H54A H 0.0746 0.7042 -0.0489 0.080 Uiso 1 1 calc R . . C55 C -0.0211(4) 0.7784(4) -0.0574(2) 0.0716(12) Uani 1 1 d . . . H55A H -0.0372 0.7575 -0.1073 0.086 Uiso 1 1 calc R . . C56 C -0.0651(3) 0.8402(4) -0.0209(2) 0.0611(10) Uani 1 1 d . . . C57 C -0.0376(4) 0.8717(4) 0.0544(2) 0.0700(11) Uani 1 1 d . . . H57A H -0.0653 0.9144 0.0808 0.084 Uiso 1 1 calc R . . C58 C 0.0296(3) 0.8404(4) 0.0898(2) 0.0627(10) Uani 1 1 d . . . H58A H 0.0467 0.8629 0.1398 0.075 Uiso 1 1 calc R . . C59 C -0.1402(4) 0.8735(4) -0.0555(2) 0.0690(11) Uani 1 1 d . . . H59A H -0.1592 0.9211 -0.0249 0.083 Uiso 1 1 calc R . . C60 C -0.1832(3) 0.8439(4) -0.1242(2) 0.0653(10) Uani 1 1 d . . . H60A H -0.1604 0.8010 -0.1553 0.078 Uiso 1 1 calc R . . C61 C -0.2639(3) 0.8717(3) -0.1569(2) 0.0555(9) Uani 1 1 d . . . C62 C -0.3175(3) 0.8191(4) -0.2296(2) 0.0650(10) Uani 1 1 d . . . H62A H -0.2949 0.7731 -0.2582 0.078 Uiso 1 1 calc R . . C63 C -0.4025(3) 0.8327(4) -0.2608(2) 0.0638(10) Uani 1 1 d . . . H63A H -0.4373 0.7946 -0.3093 0.077 Uiso 1 1 calc R . . C64 C -0.4365(3) 0.9030(3) -0.22014(19) 0.0517(8) Uani 1 1 d . . . C65 C -0.3779(3) 0.9638(3) -0.14926(19) 0.0489(8) Uani 1 1 d . . . C66 C -0.2937(3) 0.9476(3) -0.1174(2) 0.0539(8) Uani 1 1 d . . . H66A H -0.2571 0.9878 -0.0694 0.065 Uiso 1 1 calc R . . C67 C -0.5529(3) 0.9763(3) -0.1275(2) 0.0513(8) Uani 1 1 d . . . C68 C -0.6157(3) 0.9738(4) -0.0793(2) 0.0643(10) Uani 1 1 d . . . H68A H -0.5844 1.0176 -0.0313 0.077 Uiso 1 1 calc R . . C69 C -0.7231(4) 0.9076(4) -0.1018(3) 0.0792(13) Uani 1 1 d . . . H69A H -0.7653 0.9075 -0.0696 0.095 Uiso 1 1 calc R . . C70 C -0.7686(4) 0.8405(4) -0.1730(3) 0.0833(14) Uani 1 1 d . . . H70A H -0.8415 0.7944 -0.1883 0.100 Uiso 1 1 calc R . . C71 C -0.7063(4) 0.8415(4) -0.2219(3) 0.0746(12) Uani 1 1 d . . . H71A H -0.7378 0.7960 -0.2696 0.090 Uiso 1 1 calc R . . C72 C -0.5974(3) 0.9102(3) -0.1996(2) 0.0548(9) Uani 1 1 d . . . C73 C -0.5768(4) 0.8680(4) -0.3246(2) 0.0707(12) Uani 1 1 d . . . H73A H -0.6289 0.7925 -0.3375 0.085 Uiso 1 1 calc R . . H73B H -0.5213 0.8693 -0.3491 0.085 Uiso 1 1 calc R . . C74 C -0.6307(4) 0.9326(5) -0.3491(3) 0.0890(16) Uani 1 1 d . . . H74A H -0.6601 0.9016 -0.4003 0.133 Uiso 1 1 calc R . . H74B H -0.5791 1.0073 -0.3366 0.133 Uiso 1 1 calc R . . H74C H -0.6869 0.9297 -0.3260 0.133 Uiso 1 1 calc R . . Cl1 Cl 0.40627(12) 0.26578(11) 0.48091(7) 0.0815(4) Uani 1 1 d . . . Cl2 Cl 0.93842(9) 0.51888(11) 0.18962(6) 0.0729(3) Uani 1 1 d . . . O1 O 0.4692(10) 0.2135(8) 0.4644(5) 0.254(5) Uani 1 1 d . . . O2 O 0.4532(5) 0.3671(6) 0.4766(5) 0.203(4) Uani 1 1 d . . . O3 O 0.3971(4) 0.2621(5) 0.5470(3) 0.1356(18) Uani 1 1 d . . . O4 O 0.3078(7) 0.2141(10) 0.4357(5) 0.303(7) Uani 1 1 d . . . O5 O 0.9382(5) 0.4542(7) 0.2297(5) 0.197(3) Uani 1 1 d . . . O6 O 0.9363(11) 0.4753(11) 0.1234(3) 0.324(8) Uani 1 1 d . . . O7 O 1.0386(5) 0.6067(5) 0.2249(5) 0.205(3) Uani 1 1 d . . . O8 O 0.8589(3) 0.5565(4) 0.1952(3) 0.1146(14) Uani 1 1 d . . . C1S C 0.6187(6) 0.3164(8) 0.0943(5) 0.153(3) Uani 1 1 d . . . H1SA H 0.6840 0.3839 0.1103 0.184 Uiso 1 1 calc R . . H1SB H 0.6384 0.2572 0.0923 0.184 Uiso 1 1 calc R . . Cl1S Cl 0.5442(2) 0.3226(2) 0.15671(12) 0.1478(8) Uani 1 1 d . . . Cl2S Cl 0.5521(2) 0.2966(2) 0.01010(12) 0.1565(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0448(3) 0.0566(3) 0.0558(3) 0.0244(3) 0.0059(2) 0.0311(2) S1 0.0722(6) 0.0812(7) 0.0615(6) 0.0341(5) 0.0292(5) 0.0498(6) S2 0.0557(5) 0.0578(5) 0.0545(5) 0.0191(4) 0.0092(4) 0.0317(4) N1 0.0516(16) 0.0567(17) 0.0591(17) 0.0299(14) 0.0132(13) 0.0314(14) N2 0.0400(13) 0.0475(14) 0.0461(15) 0.0189(12) 0.0091(11) 0.0249(12) N3 0.0412(15) 0.0664(19) 0.077(2) 0.0362(17) 0.0165(14) 0.0303(14) N4 0.0481(15) 0.0633(18) 0.0573(17) 0.0284(15) 0.0147(13) 0.0327(14) N5 0.066(2) 0.0594(18) 0.063(2) 0.0132(15) 0.0073(16) 0.0418(16) N6 0.0391(13) 0.0531(15) 0.0465(15) 0.0208(13) 0.0102(11) 0.0251(12) N7 0.0621(18) 0.0635(19) 0.0465(16) 0.0153(14) 0.0017(14) 0.0358(16) N8 0.0546(17) 0.072(2) 0.0504(17) 0.0206(15) 0.0051(14) 0.0375(16) C1 0.067(2) 0.072(3) 0.077(3) 0.044(2) 0.017(2) 0.042(2) C2 0.078(3) 0.064(2) 0.075(3) 0.044(2) 0.023(2) 0.033(2) C3 0.057(2) 0.060(2) 0.058(2) 0.0286(18) 0.0197(17) 0.0248(18) C4 0.0492(18) 0.059(2) 0.053(2) 0.0253(17) 0.0161(15) 0.0287(16) C5 0.0452(17) 0.0448(17) 0.0430(17) 0.0170(14) 0.0053(13) 0.0232(14) C6 0.0415(16) 0.0452(16) 0.0429(16) 0.0177(14) 0.0078(13) 0.0223(14) C7 0.0380(16) 0.0520(18) 0.0529(19) 0.0222(15) 0.0089(14) 0.0251(14) C8 0.0436(16) 0.0470(17) 0.0464(17) 0.0180(14) 0.0075(14) 0.0262(14) C9 0.0476(18) 0.0524(18) 0.0493(18) 0.0242(15) 0.0127(14) 0.0267(15) C10 0.0425(16) 0.0468(17) 0.0494(18) 0.0201(15) 0.0106(14) 0.0245(14) C11 0.0429(17) 0.0496(18) 0.059(2) 0.0201(16) 0.0139(15) 0.0254(15) C12 0.051(2) 0.072(2) 0.067(2) 0.034(2) 0.0216(18) 0.0285(19) C13 0.061(2) 0.087(3) 0.090(3) 0.041(3) 0.035(2) 0.032(2) C14 0.048(2) 0.100(4) 0.114(4) 0.049(3) 0.035(2) 0.037(2) C15 0.045(2) 0.092(3) 0.115(4) 0.052(3) 0.020(2) 0.039(2) C16 0.0434(17) 0.0535(19) 0.0520(19) 0.0224(16) 0.0076(14) 0.0272(15) C17 0.0497(19) 0.065(2) 0.060(2) 0.0335(18) 0.0162(16) 0.0317(17) C18 0.0466(18) 0.066(2) 0.066(2) 0.0304(19) 0.0171(17) 0.0336(17) C19 0.0482(18) 0.0536(19) 0.060(2) 0.0244(17) 0.0023(16) 0.0262(16) C20 0.065(2) 0.078(3) 0.054(2) 0.0331(19) 0.0144(18) 0.042(2) C21 0.057(2) 0.071(2) 0.055(2) 0.0300(18) 0.0177(17) 0.0411(19) C22 0.052(2) 0.064(2) 0.065(2) 0.0261(19) 0.0021(17) 0.0329(18) C23 0.059(2) 0.069(2) 0.068(2) 0.031(2) 0.0084(19) 0.034(2) C24 0.0493(19) 0.058(2) 0.063(2) 0.0243(18) 0.0026(17) 0.0269(17) C25 0.062(2) 0.071(2) 0.065(2) 0.039(2) 0.0157(19) 0.031(2) C26 0.0482(19) 0.076(2) 0.057(2) 0.0307(19) 0.0157(16) 0.0341(18) C27 0.0447(17) 0.056(2) 0.0512(19) 0.0225(16) 0.0062(15) 0.0248(16) C28 0.0497(19) 0.060(2) 0.0511(19) 0.0210(17) 0.0093(15) 0.0298(17) C29 0.057(2) 0.067(2) 0.060(2) 0.0252(19) 0.0120(17) 0.0376(19) C30 0.062(2) 0.063(2) 0.051(2) 0.0219(18) 0.0118(17) 0.0310(19) C31 0.083(3) 0.079(3) 0.070(3) 0.032(2) 0.036(2) 0.033(2) C32 0.119(4) 0.069(3) 0.091(3) 0.045(3) 0.053(3) 0.046(3) C33 0.107(4) 0.068(3) 0.088(3) 0.042(3) 0.029(3) 0.048(3) C34 0.068(2) 0.067(2) 0.070(3) 0.029(2) 0.019(2) 0.038(2) C35 0.0517(19) 0.0556(19) 0.0470(18) 0.0189(16) 0.0073(15) 0.0277(16) C36 0.0499(19) 0.059(2) 0.066(2) 0.0243(18) 0.0195(17) 0.0323(17) C37 0.082(3) 0.067(3) 0.077(3) 0.023(2) 0.037(2) 0.036(2) C38 0.097(4) 0.085(3) 0.092(4) 0.017(3) 0.010(3) 0.068(3) C39 0.119(4) 0.080(3) 0.096(4) 0.004(3) 0.018(3) 0.069(3) C40 0.116(4) 0.079(3) 0.069(3) 0.005(3) 0.014(3) 0.053(3) C41 0.083(3) 0.071(3) 0.052(2) 0.0096(19) 0.007(2) 0.044(2) C42 0.0502(18) 0.0477(18) 0.054(2) 0.0151(16) 0.0088(15) 0.0264(16) C43 0.0429(16) 0.0523(18) 0.0467(18) 0.0190(15) 0.0111(14) 0.0247(15) C44 0.0475(18) 0.060(2) 0.0464(18) 0.0195(16) 0.0075(15) 0.0289(16) C45 0.0387(16) 0.060(2) 0.0520(19) 0.0277(16) 0.0127(14) 0.0270(15) C46 0.0448(17) 0.0558(19) 0.0510(19) 0.0198(16) 0.0153(14) 0.0312(15) C47 0.0408(16) 0.0528(18) 0.0465(17) 0.0204(15) 0.0138(13) 0.0274(14) C48 0.0426(17) 0.0548(19) 0.0473(18) 0.0158(15) 0.0097(14) 0.0255(15) C49 0.065(2) 0.077(3) 0.058(2) 0.014(2) 0.0132(19) 0.042(2) C50 0.084(3) 0.099(4) 0.057(3) 0.000(2) 0.013(2) 0.043(3) C51 0.092(3) 0.097(4) 0.049(2) 0.012(2) -0.001(2) 0.042(3) C52 0.084(3) 0.080(3) 0.055(2) 0.018(2) -0.005(2) 0.041(2) C53 0.0466(18) 0.062(2) 0.056(2) 0.0288(17) 0.0104(15) 0.0305(17) C54 0.077(3) 0.096(3) 0.058(2) 0.036(2) 0.023(2) 0.061(3) C55 0.082(3) 0.103(3) 0.055(2) 0.036(2) 0.017(2) 0.060(3) C56 0.060(2) 0.078(3) 0.067(2) 0.036(2) 0.0175(19) 0.045(2) C57 0.078(3) 0.095(3) 0.068(3) 0.034(2) 0.020(2) 0.064(3) C58 0.069(2) 0.084(3) 0.054(2) 0.025(2) 0.0126(18) 0.053(2) C59 0.075(3) 0.088(3) 0.068(3) 0.034(2) 0.015(2) 0.057(2) C60 0.068(2) 0.086(3) 0.072(3) 0.041(2) 0.025(2) 0.054(2) C61 0.056(2) 0.068(2) 0.060(2) 0.0305(19) 0.0166(17) 0.0403(19) C62 0.071(3) 0.073(3) 0.066(2) 0.022(2) 0.018(2) 0.048(2) C63 0.066(2) 0.077(3) 0.053(2) 0.0161(19) 0.0068(18) 0.043(2) C64 0.055(2) 0.059(2) 0.052(2) 0.0253(17) 0.0092(16) 0.0340(17) C65 0.0508(18) 0.0543(19) 0.0514(19) 0.0231(16) 0.0093(15) 0.0307(16) C66 0.054(2) 0.065(2) 0.051(2) 0.0260(17) 0.0080(16) 0.0314(18) C67 0.0531(19) 0.057(2) 0.057(2) 0.0293(17) 0.0115(16) 0.0319(17) C68 0.068(2) 0.077(3) 0.068(2) 0.040(2) 0.024(2) 0.040(2) C69 0.073(3) 0.103(4) 0.088(3) 0.056(3) 0.039(3) 0.044(3) C70 0.056(2) 0.090(3) 0.107(4) 0.053(3) 0.023(3) 0.022(2) C71 0.059(2) 0.076(3) 0.084(3) 0.030(2) 0.004(2) 0.026(2) C72 0.053(2) 0.057(2) 0.063(2) 0.0278(18) 0.0082(17) 0.0304(17) C73 0.070(3) 0.094(3) 0.050(2) 0.018(2) -0.0010(19) 0.047(2) C74 0.083(3) 0.136(5) 0.072(3) 0.050(3) 0.012(2) 0.065(3) Cl1 0.1111(10) 0.0860(8) 0.0727(7) 0.0466(6) 0.0427(7) 0.0502(7) Cl2 0.0715(7) 0.0940(8) 0.0622(6) 0.0317(6) 0.0182(5) 0.0420(6) O1 0.405(14) 0.290(10) 0.203(7) 0.078(7) 0.125(9) 0.278(11) O2 0.152(5) 0.241(7) 0.335(10) 0.242(8) 0.118(6) 0.094(5) O3 0.149(4) 0.160(4) 0.107(3) 0.077(3) 0.053(3) 0.051(3) O4 0.160(7) 0.383(14) 0.254(9) 0.207(10) -0.058(6) -0.017(7) O5 0.166(5) 0.294(9) 0.302(9) 0.240(8) 0.135(6) 0.159(6) O6 0.564(18) 0.540(18) 0.078(4) 0.052(6) 0.061(6) 0.493(17) O7 0.113(4) 0.131(5) 0.342(11) 0.054(6) 0.034(5) 0.048(4) O8 0.102(3) 0.131(3) 0.140(4) 0.051(3) 0.030(3) 0.078(3) C1S 0.099(5) 0.167(8) 0.195(9) 0.076(7) 0.018(5) 0.056(5) Cl1S 0.200(2) 0.1531(18) 0.1253(15) 0.0634(14) 0.0676(15) 0.0944(17) Cl2S 0.168(2) 0.188(2) 0.1147(15) 0.0406(15) 0.0474(14) 0.0825(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N2 2.188(3) . ? Mn1 N6 2.194(3) . ? Mn1 N3 2.247(3) . ? Mn1 N7 2.248(3) . ? Mn1 N5 2.254(3) . ? Mn1 N1 2.271(3) . ? S1 C30 1.756(4) . ? S1 C28 1.766(4) . ? S2 C67 1.768(4) . ? S2 C65 1.773(4) . ? N1 C5 1.342(4) . ? N1 C1 1.346(5) . ? N2 C10 1.338(4) . ? N2 C6 1.341(4) . ? N3 C11 1.336(5) . ? N3 C15 1.346(5) . ? N4 C35 1.408(5) . ? N4 C27 1.414(4) . ? N4 C36 1.466(4) . ? N5 C38 1.340(5) . ? N5 C42 1.342(5) . ? N6 C47 1.337(4) . ? N6 C43 1.347(4) . ? N7 C48 1.343(5) . ? N7 C52 1.344(5) . ? N8 C64 1.415(4) . ? N8 C72 1.416(5) . ? N8 C73 1.477(5) . ? C1 C2 1.375(6) . ? C2 C3 1.380(6) . ? C3 C4 1.386(5) . ? C4 C5 1.380(5) . ? C5 C6 1.488(4) . ? C6 C7 1.386(4) . ? C7 C8 1.390(5) . ? C8 C9 1.398(5) . ? C8 C16 1.476(4) . ? C9 C10 1.391(5) . ? C10 C11 1.489(4) . ? C11 C12 1.377(5) . ? C12 C13 1.386(6) . ? C13 C14 1.348(7) . ? C14 C15 1.375(7) . ? C16 C21 1.390(5) . ? C16 C17 1.409(5) . ? C17 C18 1.367(5) . ? C18 C19 1.401(5) . ? C19 C20 1.390(5) . ? C19 C22 1.463(5) . ? C20 C21 1.378(5) . ? C22 C23 1.320(6) . ? C23 C24 1.459(5) . ? C24 C25 1.387(6) . ? C24 C29 1.401(6) . ? C25 C26 1.381(5) . ? C26 C27 1.399(5) . ? C27 C28 1.398(5) . ? C28 C29 1.382(5) . ? C30 C31 1.377(6) . ? C30 C35 1.407(5) . ? C31 C32 1.381(7) . ? C32 C33 1.354(7) . ? C33 C34 1.396(6) . ? C34 C35 1.396(5) . ? C36 C37 1.500(6) . ? C38 C39 1.368(7) . ? C39 C40 1.362(8) . ? C40 C41 1.373(7) . ? C41 C42 1.384(5) . ? C42 C43 1.486(5) . ? C43 C44 1.380(5) . ? C44 C45 1.392(5) . ? C45 C46 1.388(5) . ? C45 C53 1.480(5) . ? C46 C47 1.383(5) . ? C47 C48 1.497(5) . ? C48 C49 1.376(5) . ? C49 C50 1.390(6) . ? C50 C51 1.372(7) . ? C51 C52 1.353(7) . ? C53 C58 1.388(5) . ? C53 C54 1.404(5) . ? C54 C55 1.383(6) . ? C55 C56 1.372(6) . ? C56 C57 1.403(6) . ? C56 C59 1.474(5) . ? C57 C58 1.374(5) . ? C59 C60 1.305(6) . ? C60 C61 1.464(5) . ? C61 C62 1.394(6) . ? C61 C66 1.395(5) . ? C62 C63 1.375(6) . ? C63 C64 1.389(5) . ? C64 C65 1.389(5) . ? C65 C66 1.391(5) . ? C67 C68 1.385(5) . ? C67 C72 1.395(5) . ? C68 C69 1.366(6) . ? C69 C70 1.384(7) . ? C70 C71 1.393(7) . ? C71 C72 1.389(6) . ? C73 C74 1.520(6) . ? Cl1 O4 1.344(7) . ? Cl1 O3 1.352(4) . ? Cl1 O2 1.353(6) . ? Cl1 O1 1.376(7) . ? Cl2 O6 1.296(6) . ? Cl2 O5 1.358(5) . ? Cl2 O7 1.396(6) . ? Cl2 O8 1.417(4) . ? C1S Cl2S 1.705(9) . ? C1S Cl1S 1.736(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 N2 Mn1 N6 176.84(10) . . ? N2 Mn1 N3 72.50(10) . . ? N6 Mn1 N3 109.95(10) . . ? N2 Mn1 N7 110.25(10) . . ? N6 Mn1 N7 72.04(11) . . ? N3 Mn1 N7 89.48(12) . . ? N2 Mn1 N5 105.36(11) . . ? N6 Mn1 N5 72.50(11) . . ? N3 Mn1 N5 98.66(13) . . ? N7 Mn1 N5 144.28(11) . . ? N2 Mn1 N1 71.80(10) . . ? N6 Mn1 N1 105.89(10) . . ? N3 Mn1 N1 144.00(10) . . ? N7 Mn1 N1 98.52(12) . . ? N5 Mn1 N1 94.99(12) . . ? C30 S1 C28 99.55(18) . . ? C67 S2 C65 95.42(17) . . ? C5 N1 C1 118.6(3) . . ? C5 N1 Mn1 116.9(2) . . ? C1 N1 Mn1 124.2(2) . . ? C10 N2 C6 119.8(3) . . ? C10 N2 Mn1 119.6(2) . . ? C6 N2 Mn1 120.5(2) . . ? C11 N3 C15 118.7(3) . . ? C11 N3 Mn1 117.1(2) . . ? C15 N3 Mn1 123.2(3) . . ? C35 N4 C27 120.9(3) . . ? C35 N4 C36 118.2(3) . . ? C27 N4 C36 118.5(3) . . ? C38 N5 C42 117.8(4) . . ? C38 N5 Mn1 125.1(3) . . ? C42 N5 Mn1 117.1(2) . . ? C47 N6 C43 119.5(3) . . ? C47 N6 Mn1 120.5(2) . . ? C43 N6 Mn1 120.0(2) . . ? C48 N7 C52 118.6(3) . . ? C48 N7 Mn1 117.9(2) . . ? C52 N7 Mn1 123.4(3) . . ? C64 N8 C72 115.0(3) . . ? C64 N8 C73 117.1(3) . . ? C72 N8 C73 119.0(3) . . ? N1 C1 C2 122.5(4) . . ? C1 C2 C3 118.9(4) . . ? C2 C3 C4 118.9(4) . . ? C5 C4 C3 119.2(3) . . ? N1 C5 C4 121.9(3) . . ? N1 C5 C6 115.0(3) . . ? C4 C5 C6 123.1(3) . . ? N2 C6 C7 121.4(3) . . ? N2 C6 C5 114.6(3) . . ? C7 C6 C5 123.9(3) . . ? C6 C7 C8 120.0(3) . . ? C7 C8 C9 117.6(3) . . ? C7 C8 C16 122.1(3) . . ? C9 C8 C16 120.3(3) . . ? C10 C9 C8 119.7(3) . . ? N2 C10 C9 121.4(3) . . ? N2 C10 C11 114.8(3) . . ? C9 C10 C11 123.8(3) . . ? N3 C11 C12 122.0(3) . . ? N3 C11 C10 115.2(3) . . ? C12 C11 C10 122.7(3) . . ? C11 C12 C13 118.6(4) . . ? C14 C13 C12 119.4(4) . . ? C13 C14 C15 119.9(4) . . ? N3 C15 C14 121.5(4) . . ? C21 C16 C17 118.1(3) . . ? C21 C16 C8 121.1(3) . . ? C17 C16 C8 120.7(3) . . ? C18 C17 C16 120.3(3) . . ? C17 C18 C19 121.9(3) . . ? C20 C19 C18 117.2(3) . . ? C20 C19 C22 123.6(4) . . ? C18 C19 C22 119.2(4) . . ? C21 C20 C19 121.6(3) . . ? C20 C21 C16 120.8(3) . . ? C23 C22 C19 126.7(4) . . ? C22 C23 C24 127.7(4) . . ? C25 C24 C29 117.2(3) . . ? C25 C24 C23 123.8(4) . . ? C29 C24 C23 118.9(4) . . ? C26 C25 C24 122.4(4) . . ? C25 C26 C27 120.4(3) . . ? C28 C27 C26 117.2(3) . . ? C28 C27 N4 120.9(3) . . ? C26 C27 N4 121.9(3) . . ? C29 C28 C27 121.8(3) . . ? C29 C28 S1 118.1(3) . . ? C27 C28 S1 120.1(3) . . ? C28 C29 C24 120.7(4) . . ? C31 C30 C35 120.9(4) . . ? C31 C30 S1 118.8(3) . . ? C35 C30 S1 119.9(3) . . ? C30 C31 C32 120.8(4) . . ? C33 C32 C31 119.2(4) . . ? C32 C33 C34 121.3(4) . . ? C35 C34 C33 120.4(4) . . ? C34 C35 C30 117.3(4) . . ? C34 C35 N4 121.7(3) . . ? C30 C35 N4 121.0(3) . . ? N4 C36 C37 115.9(3) . . ? N5 C38 C39 122.9(5) . . ? C40 C39 C38 118.9(5) . . ? C39 C40 C41 119.5(5) . . ? C40 C41 C42 118.8(4) . . ? N5 C42 C41 122.0(3) . . ? N5 C42 C43 116.0(3) . . ? C41 C42 C43 122.0(3) . . ? N6 C43 C44 121.2(3) . . ? N6 C43 C42 114.4(3) . . ? C44 C43 C42 124.4(3) . . ? C43 C44 C45 120.3(3) . . ? C46 C45 C44 117.2(3) . . ? C46 C45 C53 121.2(3) . . ? C44 C45 C53 121.6(3) . . ? C47 C46 C45 120.3(3) . . ? N6 C47 C46 121.4(3) . . ? N6 C47 C48 114.2(3) . . ? C46 C47 C48 124.3(3) . . ? N7 C48 C49 121.5(3) . . ? N7 C48 C47 115.0(3) . . ? C49 C48 C47 123.5(3) . . ? C48 C49 C50 119.0(4) . . ? C51 C50 C49 118.7(4) . . ? C52 C51 C50 119.4(4) . . ? N7 C52 C51 122.7(4) . . ? C58 C53 C54 117.2(3) . . ? C58 C53 C45 121.4(3) . . ? C54 C53 C45 121.5(3) . . ? C55 C54 C53 120.6(4) . . ? C56 C55 C54 122.1(4) . . ? C55 C56 C57 117.4(4) . . ? C55 C56 C59 124.4(4) . . ? C57 C56 C59 118.2(4) . . ? C58 C57 C56 121.1(4) . . ? C57 C58 C53 121.7(4) . . ? C60 C59 C56 127.4(4) . . ? C59 C60 C61 126.2(4) . . ? C62 C61 C66 116.9(3) . . ? C62 C61 C60 120.5(4) . . ? C66 C61 C60 122.6(4) . . ? C63 C62 C61 122.6(4) . . ? C62 C63 C64 120.2(4) . . ? C65 C64 C63 117.9(3) . . ? C65 C64 N8 118.2(3) . . ? C63 C64 N8 123.8(3) . . ? C64 C65 C66 121.4(3) . . ? C64 C65 S2 118.1(3) . . ? C66 C65 S2 120.5(3) . . ? C65 C66 C61 120.6(3) . . ? C68 C67 C72 120.9(4) . . ? C68 C67 S2 121.2(3) . . ? C72 C67 S2 117.8(3) . . ? C69 C68 C67 120.6(4) . . ? C68 C69 C70 119.3(4) . . ? C69 C70 C71 120.7(4) . . ? C72 C71 C70 120.1(5) . . ? C71 C72 C67 118.2(4) . . ? C71 C72 N8 123.1(4) . . ? C67 C72 N8 118.6(3) . . ? N8 C73 C74 111.2(4) . . ? O4 Cl1 O3 108.3(5) . . ? O4 Cl1 O2 107.5(6) . . ? O3 Cl1 O2 115.5(5) . . ? O4 Cl1 O1 113.0(8) . . ? O3 Cl1 O1 103.9(5) . . ? O2 Cl1 O1 108.8(6) . . ? O6 Cl2 O5 112.9(6) . . ? O6 Cl2 O7 109.4(8) . . ? O5 Cl2 O7 99.5(5) . . ? O6 Cl2 O8 112.4(4) . . ? O5 Cl2 O8 112.9(3) . . ? O7 Cl2 O8 108.9(3) . . ? Cl2S C1S Cl1S 113.2(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.884 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.076