# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Guang-Xiang Liu' _publ_contact_author_email LIUGX@LIVE.COM _publ_section_title ; Five 3D Metal-Organic Frameworks Constructed From V-shaped Polycarboxylate Acids and Flexible Imidazole-Based Ligands ; loop_ _publ_author_name 'Guang-Xiang Liu' 'Rong-Yi Huang' 'Sadafumi Nishihara' 'Xiao-Ming Ren' 'Huan-Min Xu' 'Kun Zhu' # Attachment 'CEC0601.cif' data_K1 _database_code_depnum_ccdc_archive 'CCDC 730708' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H20 Cd2 N4 O10 S' _chemical_formula_sum 'C30 H20 Cd2 N4 O10 S' _chemical_formula_weight 853.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.4685(12) _cell_length_b 18.677(3) _cell_length_c 21.713(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.671(4) _cell_angle_gamma 90.00 _cell_volume 2916.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3341 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 23.75 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6813 _exptl_absorpt_correction_T_max 0.8565 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 14430 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5169 _reflns_number_gt 3998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5169 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.91280(6) 0.94114(2) 0.870285(19) 0.03040(14) Uani 1 1 d . . . Cd2 Cd 1.33757(6) 1.03183(2) 0.888393(18) 0.02842(14) Uani 1 1 d . . . O1 O 1.2197(5) 0.9481(2) 0.94110(17) 0.0337(9) Uani 1 1 d . . . O2 O 1.4703(5) 0.9229(2) 1.01929(17) 0.0364(9) Uani 1 1 d . . . O3 O 1.1479(6) 0.9639(2) 1.07858(19) 0.0370(10) Uani 1 1 d . . . O4 O 0.9221(6) 0.9019(2) 1.1054(2) 0.0444(11) Uani 1 1 d . . . O5 O 1.0973(5) 0.5223(2) 1.30565(17) 0.0362(9) Uani 1 1 d . . . O6 O 1.0667(7) 0.6399(2) 1.3029(2) 0.0539(12) Uani 1 1 d . . . O7 O 1.4841(5) 0.5486(2) 1.33837(17) 0.0366(10) Uani 1 1 d . . . O8 O 1.6810(6) 0.5433(3) 1.2790(2) 0.0516(12) Uani 1 1 d . . . O9 O 0.9598(7) 0.5870(2) 0.99019(19) 0.0609(14) Uani 1 1 d . . . O10 O 0.7826(6) 0.6496(2) 1.0553(2) 0.0539(12) Uani 1 1 d . . . N1 N 0.7901(6) 0.8391(3) 0.8929(2) 0.0345(11) Uani 1 1 d . . . N2 N 0.6842(7) 0.7296(3) 0.8808(2) 0.0374(12) Uani 1 1 d . . . N3 N 0.4312(7) 0.6924(3) 0.7164(2) 0.0419(13) Uani 1 1 d . . . N4 N 0.5742(7) 0.6257(3) 0.6618(2) 0.0388(12) Uani 1 1 d . . . S1 S 0.9560(2) 0.63545(8) 1.04107(7) 0.0392(4) Uani 1 1 d . . . C1 C 1.3065(7) 0.9122(3) 0.9894(2) 0.0257(12) Uani 1 1 d . . . C2 C 1.2102(7) 0.8463(3) 1.0043(2) 0.0266(12) Uani 1 1 d . . . C3 C 1.2247(8) 0.7858(3) 0.9687(3) 0.0364(14) Uani 1 1 d . . . H3 H 1.2868 0.7888 0.9370 0.044 Uiso 1 1 calc R . . C4 C 1.1488(8) 0.7216(3) 0.9796(3) 0.0362(14) Uani 1 1 d . . . H4 H 1.1596 0.6814 0.9556 0.043 Uiso 1 1 calc R . . C5 C 1.0579(8) 0.7175(3) 1.0257(2) 0.0334(13) Uani 1 1 d . . . C6 C 1.0289(8) 0.7769(3) 1.0593(3) 0.0334(13) Uani 1 1 d . . . H6 H 0.9579 0.7735 1.0883 0.040 Uiso 1 1 calc R . . C7 C 1.1069(7) 0.8424(3) 1.0494(2) 0.0254(11) Uani 1 1 d . . . C8 C 1.0522(9) 0.9083(3) 1.0802(2) 0.0345(14) Uani 1 1 d . . . C9 C 1.1171(7) 0.5841(3) 1.2835(3) 0.0328(13) Uani 1 1 d . . . C10 C 1.1915(8) 0.5856(3) 1.2258(2) 0.0285(12) Uani 1 1 d . . . C11 C 1.0633(8) 0.6067(3) 1.1685(3) 0.0323(13) Uani 1 1 d . . . H11 H 0.9442 0.6214 1.1683 0.039 Uiso 1 1 calc R . . C12 C 1.1175(9) 0.6053(3) 1.1120(2) 0.0358(14) Uani 1 1 d . . . C13 C 1.2933(9) 0.5845(3) 1.1108(3) 0.0417(15) Uani 1 1 d . . . H13 H 1.3256 0.5823 1.0723 0.050 Uiso 1 1 calc R . . C14 C 1.4205(8) 0.5671(3) 1.1676(3) 0.0365(14) Uani 1 1 d . . . H14 H 1.5412 0.5549 1.1676 0.044 Uiso 1 1 calc R . . C15 C 1.3717(8) 0.5675(3) 1.2252(3) 0.0299(12) Uani 1 1 d . . . C16 C 1.5226(8) 0.5512(3) 1.2858(3) 0.0298(13) Uani 1 1 d . . . C17 C 0.7802(8) 0.7798(3) 0.8604(3) 0.0363(14) Uani 1 1 d . . . H17 H 0.8340 0.7735 0.8268 0.044 Uiso 1 1 calc R . . C18 C 0.6914(8) 0.8266(3) 0.9366(3) 0.0382(14) Uani 1 1 d . . . H18 H 0.6707 0.8598 0.9659 0.046 Uiso 1 1 calc R . . C19 C 0.6297(8) 0.7592(3) 0.9306(3) 0.0387(14) Uani 1 1 d . . . H19 H 0.5626 0.7366 0.9554 0.046 Uiso 1 1 calc R . . C20 C 0.6478(9) 0.6558(3) 0.8581(3) 0.0410(15) Uani 1 1 d . . . H20A H 0.7333 0.6242 0.8873 0.049 Uiso 1 1 calc R . . H20B H 0.6722 0.6517 0.8165 0.049 Uiso 1 1 calc R . . C21 C 0.4535(8) 0.6318(3) 0.8525(3) 0.0365(14) Uani 1 1 d . . . C22 C 0.4291(11) 0.5808(4) 0.8961(3) 0.0545(18) Uani 1 1 d . . . H22 H 0.5308 0.5646 0.9280 0.065 Uiso 1 1 calc R . . C23 C 0.2498(13) 0.5536(4) 0.8921(5) 0.069(2) Uani 1 1 d . . . H23 H 0.2314 0.5207 0.9219 0.082 Uiso 1 1 calc R . . C24 C 0.1074(14) 0.5761(4) 0.8446(5) 0.075(3) Uani 1 1 d . . . H24 H -0.0099 0.5569 0.8411 0.090 Uiso 1 1 calc R . . C25 C 0.1263(9) 0.6263(4) 0.8006(4) 0.058(2) Uani 1 1 d . . . H25 H 0.0236 0.6406 0.7680 0.070 Uiso 1 1 calc R . . C26 C 0.3005(9) 0.6557(3) 0.8051(3) 0.0444(16) Uani 1 1 d . . . C27 C 0.3142(10) 0.7136(4) 0.7580(3) 0.0524(18) Uani 1 1 d . . . H27A H 0.1904 0.7249 0.7316 0.063 Uiso 1 1 calc R . . H27B H 0.3655 0.7565 0.7813 0.063 Uiso 1 1 calc R . . C28 C 0.4553(8) 0.6263(3) 0.6968(3) 0.0345(13) Uani 1 1 d . . . H28 H 0.3958 0.5859 0.7067 0.041 Uiso 1 1 calc R . . C29 C 0.6202(11) 0.6954(4) 0.6581(4) 0.063(2) Uani 1 1 d . . . H29 H 0.7005 0.7121 0.6352 0.076 Uiso 1 1 calc R . . C30 C 0.5359(12) 0.7368(4) 0.6915(4) 0.069(2) Uani 1 1 d . . . H30 H 0.5468 0.7862 0.6967 0.082 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 0.0275(2) 0.0303(3) 0.0336(2) -0.00739(17) 0.00859(18) -0.00426(17) Cd2 0.0311(3) 0.0289(2) 0.0263(2) -0.00161(16) 0.00955(17) -0.00510(17) O1 0.031(2) 0.034(2) 0.032(2) 0.0101(17) 0.0026(17) -0.0076(17) O2 0.031(2) 0.041(2) 0.034(2) 0.0011(18) 0.0028(18) -0.0041(18) O3 0.036(2) 0.031(2) 0.047(2) -0.0097(18) 0.0164(19) -0.0050(18) O4 0.055(3) 0.037(3) 0.056(3) 0.002(2) 0.038(2) 0.005(2) O5 0.027(2) 0.048(3) 0.032(2) 0.0126(19) 0.0062(17) -0.0008(18) O6 0.070(3) 0.046(3) 0.055(3) 0.006(2) 0.035(3) 0.015(2) O7 0.035(2) 0.045(3) 0.028(2) 0.0073(18) 0.0056(18) -0.0031(18) O8 0.022(2) 0.091(4) 0.041(2) 0.001(2) 0.0075(19) 0.010(2) O9 0.102(4) 0.033(3) 0.033(2) 0.000(2) -0.006(2) -0.016(3) O10 0.037(3) 0.058(3) 0.059(3) 0.028(2) 0.000(2) -0.008(2) N1 0.021(2) 0.038(3) 0.045(3) -0.004(2) 0.009(2) -0.005(2) N2 0.040(3) 0.034(3) 0.040(3) -0.004(2) 0.013(2) -0.007(2) N3 0.052(3) 0.039(3) 0.040(3) -0.005(2) 0.020(3) 0.008(2) N4 0.052(3) 0.033(3) 0.036(3) -0.004(2) 0.020(2) 0.001(2) S1 0.0459(10) 0.0305(8) 0.0336(8) 0.0103(6) -0.0020(7) -0.0096(7) C1 0.025(3) 0.033(3) 0.022(3) -0.005(2) 0.009(2) -0.003(2) C2 0.030(3) 0.023(3) 0.025(3) 0.001(2) 0.005(2) 0.000(2) C3 0.046(4) 0.033(3) 0.035(3) -0.001(3) 0.019(3) 0.000(3) C4 0.047(4) 0.031(3) 0.034(3) -0.008(3) 0.016(3) 0.000(3) C5 0.047(4) 0.022(3) 0.028(3) 0.004(2) 0.003(3) -0.002(3) C6 0.041(4) 0.030(3) 0.028(3) 0.004(2) 0.007(3) -0.005(3) C7 0.022(3) 0.031(3) 0.023(3) 0.000(2) 0.005(2) 0.002(2) C8 0.048(4) 0.034(3) 0.018(3) 0.000(2) 0.003(3) 0.008(3) C9 0.021(3) 0.049(4) 0.029(3) 0.006(3) 0.007(2) 0.002(3) C10 0.035(3) 0.020(3) 0.028(3) 0.004(2) 0.006(2) 0.003(2) C11 0.025(3) 0.032(3) 0.040(3) 0.009(3) 0.008(2) -0.001(2) C12 0.053(4) 0.024(3) 0.027(3) 0.004(2) 0.005(3) -0.001(3) C13 0.056(4) 0.041(4) 0.027(3) 0.001(3) 0.008(3) 0.014(3) C14 0.033(3) 0.040(4) 0.041(3) 0.003(3) 0.017(3) 0.010(3) C15 0.032(3) 0.023(3) 0.036(3) 0.004(2) 0.010(3) -0.001(2) C16 0.026(3) 0.026(3) 0.036(3) 0.004(2) 0.007(3) 0.001(2) C17 0.032(3) 0.037(4) 0.045(3) -0.008(3) 0.019(3) -0.009(3) C18 0.037(4) 0.039(4) 0.039(3) -0.003(3) 0.011(3) 0.001(3) C19 0.030(3) 0.045(4) 0.044(4) 0.001(3) 0.015(3) 0.005(3) C20 0.044(4) 0.029(3) 0.048(4) -0.003(3) 0.010(3) 0.004(3) C21 0.037(4) 0.033(3) 0.043(3) -0.011(3) 0.018(3) -0.005(3) C22 0.071(5) 0.040(4) 0.060(4) -0.009(3) 0.032(4) -0.007(4) C23 0.077(6) 0.046(5) 0.104(7) -0.015(5) 0.061(6) -0.020(4) C24 0.074(6) 0.053(5) 0.114(8) -0.039(5) 0.056(6) -0.022(5) C25 0.033(4) 0.066(5) 0.079(5) -0.023(4) 0.021(4) -0.001(3) C26 0.051(4) 0.040(4) 0.048(4) -0.012(3) 0.022(3) 0.000(3) C27 0.054(4) 0.053(4) 0.056(4) -0.008(3) 0.024(3) 0.017(3) C28 0.042(4) 0.029(3) 0.033(3) -0.001(2) 0.010(3) 0.005(3) C29 0.077(6) 0.046(5) 0.082(5) 0.004(4) 0.048(5) 0.000(4) C30 0.102(7) 0.031(4) 0.092(6) 0.002(4) 0.060(5) 0.001(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 Cd1 O3 2.204(4) 3_777 ? Cd1 N1 2.226(5) . ? Cd1 O8 2.271(4) 4_475 ? Cd1 O5 2.319(4) 4_575 ? Cd1 O1 2.394(4) . ? Cd1 O6 2.581(4) 4_575 ? Cd2 O1 2.253(4) . ? Cd2 N4 2.255(5) 2_756 ? Cd2 O2 2.289(4) 3_877 ? Cd2 O7 2.297(4) 4_575 ? Cd2 O4 2.335(4) 3_777 ? Cd2 O5 2.394(4) 4_575 ? O1 C1 1.265(6) . ? O2 C1 1.236(6) . ? O2 Cd2 2.289(4) 3_877 ? O3 C8 1.267(7) . ? O3 Cd1 2.204(4) 3_777 ? O4 C8 1.243(7) . ? O4 Cd2 2.335(4) 3_777 ? O5 C9 1.274(7) . ? O5 Cd1 2.319(4) 4_576 ? O5 Cd2 2.394(4) 4_576 ? O6 C9 1.221(7) . ? O6 Cd1 2.581(4) 4_576 ? O7 C16 1.251(6) . ? O7 Cd2 2.297(4) 4_576 ? O8 C16 1.240(7) . ? O8 Cd1 2.271(4) 4_676 ? O9 S1 1.434(5) . ? O10 S1 1.435(5) . ? N1 C17 1.304(7) . ? N1 C18 1.370(7) . ? N2 C17 1.327(7) . ? N2 C19 1.371(7) . ? N2 C20 1.465(7) . ? N3 C28 1.333(7) . ? N3 C30 1.348(8) . ? N3 C27 1.470(7) . ? N4 C28 1.317(7) . ? N4 C29 1.353(8) . ? N4 Cd2 2.255(5) 2_746 ? S1 C12 1.772(6) . ? S1 C5 1.782(6) . ? C1 C2 1.504(7) . ? C2 C3 1.390(7) . ? C2 C7 1.401(7) . ? C3 C4 1.373(8) . ? C3 H3 0.9300 . ? C4 C5 1.356(8) . ? C4 H4 0.9300 . ? C5 C6 1.376(8) . ? C6 C7 1.397(7) . ? C6 H6 0.9300 . ? C7 C8 1.508(7) . ? C9 C10 1.502(7) . ? C10 C15 1.391(8) . ? C10 C11 1.406(7) . ? C11 C12 1.392(7) . ? C11 H11 0.9300 . ? C12 C13 1.376(8) . ? C13 C14 1.378(8) . ? C13 H13 0.9300 . ? C14 C15 1.393(8) . ? C14 H14 0.9300 . ? C15 C16 1.514(8) . ? C17 H17 0.9300 . ? C18 C19 1.334(8) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.493(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.389(9) . ? C21 C22 1.389(9) . ? C22 C23 1.412(11) . ? C22 H22 0.9300 . ? C23 C24 1.334(12) . ? C23 H23 0.9300 . ? C24 C25 1.373(11) . ? C24 H24 0.9300 . ? C25 C26 1.391(9) . ? C25 H25 0.9300 . ? C26 C27 1.511(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28 0.9300 . ? C29 C30 1.331(9) . ? C29 H29 0.9300 . ? C30 H30 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 O3 Cd1 N1 115.14(16) 3_777 . ? O3 Cd1 O8 97.14(16) 3_777 4_475 ? N1 Cd1 O8 92.32(17) . 4_475 ? O3 Cd1 O5 107.74(14) 3_777 4_575 ? N1 Cd1 O5 137.12(15) . 4_575 ? O8 Cd1 O5 82.61(14) 4_475 4_575 ? O3 Cd1 O1 85.68(15) 3_777 . ? N1 Cd1 O1 106.50(15) . . ? O8 Cd1 O1 157.76(14) 4_475 . ? O5 Cd1 O1 75.56(13) 4_575 . ? O3 Cd1 O6 160.29(15) 3_777 4_575 ? N1 Cd1 O6 84.02(15) . 4_575 ? O8 Cd1 O6 86.09(16) 4_475 4_575 ? O5 Cd1 O6 53.23(14) 4_575 4_575 ? O1 Cd1 O6 84.26(14) . 4_575 ? O1 Cd2 N4 172.18(16) . 2_756 ? O1 Cd2 O2 92.89(13) . 3_877 ? N4 Cd2 O2 86.54(16) 2_756 3_877 ? O1 Cd2 O7 95.00(15) . 4_575 ? N4 Cd2 O7 92.39(16) 2_756 4_575 ? O2 Cd2 O7 112.94(14) 3_877 4_575 ? O1 Cd2 O4 83.92(14) . 3_777 ? N4 Cd2 O4 88.36(16) 2_756 3_777 ? O2 Cd2 O4 95.05(15) 3_877 3_777 ? O7 Cd2 O4 152.00(15) 4_575 3_777 ? O1 Cd2 O5 76.78(14) . 4_575 ? N4 Cd2 O5 102.93(16) 2_756 4_575 ? O2 Cd2 O5 168.26(13) 3_877 4_575 ? O7 Cd2 O5 74.04(13) 4_575 4_575 ? O4 Cd2 O5 78.52(14) 3_777 4_575 ? C1 O1 Cd2 127.3(3) . . ? C1 O1 Cd1 133.7(3) . . ? Cd2 O1 Cd1 98.56(13) . . ? C1 O2 Cd2 144.8(3) . 3_877 ? C8 O3 Cd1 116.8(4) . 3_777 ? C8 O4 Cd2 137.3(4) . 3_777 ? C9 O5 Cd1 96.3(3) . 4_576 ? C9 O5 Cd2 121.7(3) . 4_576 ? Cd1 O5 Cd2 96.76(13) 4_576 4_576 ? C9 O6 Cd1 85.4(3) . 4_576 ? C16 O7 Cd2 135.4(4) . 4_576 ? C16 O8 Cd1 114.0(4) . 4_676 ? C17 N1 C18 105.6(5) . . ? C17 N1 Cd1 125.0(4) . . ? C18 N1 Cd1 129.0(4) . . ? C17 N2 C19 106.4(5) . . ? C17 N2 C20 128.3(5) . . ? C19 N2 C20 125.3(5) . . ? C28 N3 C30 107.4(5) . . ? C28 N3 C27 126.8(5) . . ? C30 N3 C27 125.8(5) . . ? C28 N4 C29 104.3(5) . . ? C28 N4 Cd2 128.1(4) . 2_746 ? C29 N4 Cd2 127.4(4) . 2_746 ? O9 S1 O10 119.3(3) . . ? O9 S1 C12 108.6(3) . . ? O10 S1 C12 108.3(3) . . ? O9 S1 C5 107.5(3) . . ? O10 S1 C5 109.8(3) . . ? C12 S1 C5 102.2(3) . . ? O2 C1 O1 124.2(5) . . ? O2 C1 C2 118.8(5) . . ? O1 C1 C2 116.3(5) . . ? C3 C2 C7 119.1(5) . . ? C3 C2 C1 115.6(4) . . ? C7 C2 C1 125.3(5) . . ? C4 C3 C2 121.1(5) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 119.3(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.8(5) . . ? C4 C5 S1 120.8(4) . . ? C6 C5 S1 117.3(4) . . ? C5 C6 C7 119.6(5) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 118.9(5) . . ? C6 C7 C8 118.1(5) . . ? C2 C7 C8 122.3(5) . . ? O4 C8 O3 127.2(5) . . ? O4 C8 C7 117.1(5) . . ? O3 C8 C7 115.7(5) . . ? O6 C9 O5 124.4(5) . . ? O6 C9 C10 119.3(5) . . ? O5 C9 C10 116.0(5) . . ? C15 C10 C11 119.3(5) . . ? C15 C10 C9 125.5(5) . . ? C11 C10 C9 115.2(5) . . ? C12 C11 C10 118.9(5) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 121.9(5) . . ? C13 C12 S1 120.2(4) . . ? C11 C12 S1 117.9(5) . . ? C12 C13 C14 118.7(5) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C10 C15 C14 119.9(5) . . ? C10 C15 C16 122.4(5) . . ? C14 C15 C16 117.7(5) . . ? O8 C16 O7 124.5(5) . . ? O8 C16 C15 115.5(5) . . ? O7 C16 C15 120.0(5) . . ? N1 C17 N2 112.0(5) . . ? N1 C17 H17 124.0 . . ? N2 C17 H17 124.0 . . ? C19 C18 N1 109.2(5) . . ? C19 C18 H18 125.4 . . ? N1 C18 H18 125.4 . . ? C18 C19 N2 106.8(5) . . ? C18 C19 H19 126.6 . . ? N2 C19 H19 126.6 . . ? N2 C20 C21 113.4(5) . . ? N2 C20 H20A 108.9 . . ? C21 C20 H20A 108.9 . . ? N2 C20 H20B 108.9 . . ? C21 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C26 C21 C22 119.5(6) . . ? C26 C21 C20 123.4(6) . . ? C22 C21 C20 117.1(6) . . ? C21 C22 C23 120.1(8) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 118.6(8) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 122.9(8) . . ? C23 C24 H24 118.5 . . ? C25 C24 H24 118.5 . . ? C24 C25 C26 119.4(8) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C21 C26 C25 119.5(6) . . ? C21 C26 C27 122.6(6) . . ? C25 C26 C27 117.9(7) . . ? N3 C27 C26 112.6(5) . . ? N3 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? N3 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? N4 C28 N3 111.2(5) . . ? N4 C28 H28 124.4 . . ? N3 C28 H28 124.4 . . ? C30 C29 N4 111.2(6) . . ? C30 C29 H29 124.4 . . ? N4 C29 H29 124.4 . . ? C29 C30 N3 105.7(6) . . ? C29 C30 H30 127.1 . . ? N3 C30 H30 127.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cd2 O1 C1 -124.3(11) 2_756 . . . ? O2 Cd2 O1 C1 -38.7(4) 3_877 . . . ? O7 Cd2 O1 C1 74.7(4) 4_575 . . . ? O4 Cd2 O1 C1 -133.5(4) 3_777 . . . ? O5 Cd2 O1 C1 147.0(4) 4_575 . . . ? N4 Cd2 O1 Cd1 62.7(12) 2_756 . . . ? O2 Cd2 O1 Cd1 148.28(15) 3_877 . . . ? O7 Cd2 O1 Cd1 -98.39(15) 4_575 . . . ? O4 Cd2 O1 Cd1 53.50(15) 3_777 . . . ? O5 Cd2 O1 Cd1 -26.09(13) 4_575 . . . ? O3 Cd1 O1 C1 105.2(5) 3_777 . . . ? N1 Cd1 O1 C1 -9.7(5) . . . . ? O8 Cd1 O1 C1 -156.4(5) 4_475 . . . ? O5 Cd1 O1 C1 -145.2(5) 4_575 . . . ? O6 Cd1 O1 C1 -91.7(5) 4_575 . . . ? O3 Cd1 O1 Cd2 -82.42(16) 3_777 . . . ? N1 Cd1 O1 Cd2 162.62(15) . . . . ? O8 Cd1 O1 Cd2 15.9(5) 4_475 . . . ? O5 Cd1 O1 Cd2 27.15(14) 4_575 . . . ? O6 Cd1 O1 Cd2 80.61(15) 4_575 . . . ? O3 Cd1 N1 C17 167.1(4) 3_777 . . . ? O8 Cd1 N1 C17 68.1(5) 4_475 . . . ? O5 Cd1 N1 C17 -13.6(6) 4_575 . . . ? O1 Cd1 N1 C17 -99.9(5) . . . . ? O6 Cd1 N1 C17 -17.7(5) 4_575 . . . ? O3 Cd1 N1 C18 -4.0(5) 3_777 . . . ? O8 Cd1 N1 C18 -103.0(5) 4_475 . . . ? O5 Cd1 N1 C18 175.3(4) 4_575 . . . ? O1 Cd1 N1 C18 89.0(5) . . . . ? O6 Cd1 N1 C18 171.2(5) 4_575 . . . ? Cd2 O2 C1 O1 105.9(6) 3_877 . . . ? Cd2 O2 C1 C2 -83.6(7) 3_877 . . . ? Cd2 O1 C1 O2 7.2(7) . . . . ? Cd1 O1 C1 O2 177.7(3) . . . . ? Cd2 O1 C1 C2 -163.5(3) . . . . ? Cd1 O1 C1 C2 6.9(7) . . . . ? O2 C1 C2 C3 -90.0(6) . . . . ? O1 C1 C2 C3 81.3(6) . . . . ? O2 C1 C2 C7 91.3(6) . . . . ? O1 C1 C2 C7 -97.4(6) . . . . ? C7 C2 C3 C4 -3.8(8) . . . . ? C1 C2 C3 C4 177.5(5) . . . . ? C2 C3 C4 C5 0.2(9) . . . . ? C3 C4 C5 C6 4.3(9) . . . . ? C3 C4 C5 S1 179.6(5) . . . . ? O9 S1 C5 C4 -10.9(6) . . . . ? O10 S1 C5 C4 -142.0(5) . . . . ? C12 S1 C5 C4 103.3(5) . . . . ? O9 S1 C5 C6 164.6(5) . . . . ? O10 S1 C5 C6 33.5(5) . . . . ? C12 S1 C5 C6 -81.2(5) . . . . ? C4 C5 C6 C7 -5.0(9) . . . . ? S1 C5 C6 C7 179.5(4) . . . . ? C5 C6 C7 C2 1.3(8) . . . . ? C5 C6 C7 C8 172.2(5) . . . . ? C3 C2 C7 C6 3.0(8) . . . . ? C1 C2 C7 C6 -178.4(5) . . . . ? C3 C2 C7 C8 -167.5(5) . . . . ? C1 C2 C7 C8 11.1(8) . . . . ? Cd2 O4 C8 O3 43.3(9) 3_777 . . . ? Cd2 O4 C8 C7 -138.4(5) 3_777 . . . ? Cd1 O3 C8 O4 3.0(8) 3_777 . . . ? Cd1 O3 C8 C7 -175.3(3) 3_777 . . . ? C6 C7 C8 O4 -9.5(7) . . . . ? C2 C7 C8 O4 161.1(5) . . . . ? C6 C7 C8 O3 169.0(5) . . . . ? C2 C7 C8 O3 -20.4(8) . . . . ? Cd1 O6 C9 O5 -7.6(6) 4_576 . . . ? Cd1 O6 C9 C10 166.3(5) 4_576 . . . ? Cd1 O5 C9 O6 8.5(6) 4_576 . . . ? Cd2 O5 C9 O6 -93.5(6) 4_576 . . . ? Cd1 O5 C9 C10 -165.6(4) 4_576 . . . ? Cd2 O5 C9 C10 92.4(5) 4_576 . . . ? O6 C9 C10 C15 116.3(7) . . . . ? O5 C9 C10 C15 -69.2(7) . . . . ? O6 C9 C10 C11 -64.3(7) . . . . ? O5 C9 C10 C11 110.2(6) . . . . ? C15 C10 C11 C12 3.4(8) . . . . ? C9 C10 C11 C12 -176.1(5) . . . . ? C10 C11 C12 C13 -0.6(9) . . . . ? C10 C11 C12 S1 -177.6(4) . . . . ? O9 S1 C12 C13 45.9(6) . . . . ? O10 S1 C12 C13 176.8(5) . . . . ? C5 S1 C12 C13 -67.4(5) . . . . ? O9 S1 C12 C11 -137.0(5) . . . . ? O10 S1 C12 C11 -6.1(5) . . . . ? C5 S1 C12 C11 109.7(5) . . . . ? C11 C12 C13 C14 -2.3(9) . . . . ? S1 C12 C13 C14 174.6(5) . . . . ? C12 C13 C14 C15 2.6(9) . . . . ? C11 C10 C15 C14 -3.1(8) . . . . ? C9 C10 C15 C14 176.3(5) . . . . ? C11 C10 C15 C16 174.0(5) . . . . ? C9 C10 C15 C16 -6.6(9) . . . . ? C13 C14 C15 C10 0.1(9) . . . . ? C13 C14 C15 C16 -177.1(5) . . . . ? Cd1 O8 C16 O7 -18.7(7) 4_676 . . . ? Cd1 O8 C16 C15 159.1(4) 4_676 . . . ? Cd2 O7 C16 O8 -106.7(6) 4_576 . . . ? Cd2 O7 C16 C15 75.5(7) 4_576 . . . ? C10 C15 C16 O8 -172.7(5) . . . . ? C14 C15 C16 O8 4.4(8) . . . . ? C10 C15 C16 O7 5.2(8) . . . . ? C14 C15 C16 O7 -177.7(5) . . . . ? C18 N1 C17 N2 -1.0(7) . . . . ? Cd1 N1 C17 N2 -173.8(4) . . . . ? C19 N2 C17 N1 -0.4(7) . . . . ? C20 N2 C17 N1 -177.8(5) . . . . ? C17 N1 C18 C19 2.0(7) . . . . ? Cd1 N1 C18 C19 174.5(4) . . . . ? N1 C18 C19 N2 -2.3(7) . . . . ? C17 N2 C19 C18 1.7(7) . . . . ? C20 N2 C19 C18 179.2(5) . . . . ? C17 N2 C20 C21 -138.6(6) . . . . ? C19 N2 C20 C21 44.4(8) . . . . ? N2 C20 C21 C26 72.4(7) . . . . ? N2 C20 C21 C22 -110.1(6) . . . . ? C26 C21 C22 C23 0.1(9) . . . . ? C20 C21 C22 C23 -177.5(6) . . . . ? C21 C22 C23 C24 2.2(10) . . . . ? C22 C23 C24 C25 -2.2(12) . . . . ? C23 C24 C25 C26 -0.1(11) . . . . ? C22 C21 C26 C25 -2.4(9) . . . . ? C20 C21 C26 C25 175.1(5) . . . . ? C22 C21 C26 C27 176.9(5) . . . . ? C20 C21 C26 C27 -5.6(9) . . . . ? C24 C25 C26 C21 2.4(9) . . . . ? C24 C25 C26 C27 -176.9(6) . . . . ? C28 N3 C27 C26 30.6(9) . . . . ? C30 N3 C27 C26 -148.6(7) . . . . ? C21 C26 C27 N3 63.7(8) . . . . ? C25 C26 C27 N3 -117.0(6) . . . . ? C29 N4 C28 N3 -2.0(7) . . . . ? Cd2 N4 C28 N3 -177.1(4) 2_746 . . . ? C30 N3 C28 N4 1.5(7) . . . . ? C27 N3 C28 N4 -177.8(6) . . . . ? C28 N4 C29 C30 1.8(9) . . . . ? Cd2 N4 C29 C30 176.9(5) 2_746 . . . ? N4 C29 C30 N3 -0.9(10) . . . . ? C28 N3 C30 C29 -0.4(9) . . . . ? C27 N3 C30 C29 179.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.609 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.150 #=========END data_K2 _database_code_depnum_ccdc_archive 'CCDC 730709' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H42 N8 O10 S Zn2' _chemical_formula_sum 'C56 H42 N8 O10 S Zn2' _chemical_formula_weight 1149.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.4927(13) _cell_length_b 10.6448(14) _cell_length_c 45.543(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5086.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9070 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.34 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7028 _exptl_absorpt_correction_T_max 0.8839 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 26204 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9404 _reflns_number_gt 8000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998' _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^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(8) _refine_ls_number_reflns 9404 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Zn1 Zn 0.77318(3) 0.24872(4) 0.027272(7) 0.03789(10) Uani 1 1 d . . . Zn2 Zn -0.08957(3) 0.02407(3) 0.272231(7) 0.03261(9) Uani 1 1 d . . . N1 N 0.8200(3) 0.0715(3) 0.01586(6) 0.0437(7) Uani 1 1 d . . . N2 N 0.9356(2) -0.0913(3) 0.00288(6) 0.0397(7) Uani 1 1 d . . . N3 N 1.1658(2) -0.2473(3) -0.24346(5) 0.0442(6) Uani 1 1 d . . . N4 N 1.2685(2) -0.4110(3) -0.25988(6) 0.0417(7) Uani 1 1 d . . . N5 N 0.9180(3) 0.3152(3) 0.05142(6) 0.0444(7) Uani 1 1 d . . . N6 N 1.0836(3) 0.4233(3) 0.06657(7) 0.0592(9) Uani 1 1 d . . . N7 N 0.8216(3) 1.3316(3) 0.17833(7) 0.0584(9) Uani 1 1 d . . . N8 N 0.9716(2) 1.4487(3) 0.19753(6) 0.0420(7) Uani 1 1 d . . . O1 O 0.6378(2) 0.2283(2) 0.05783(5) 0.0476(6) Uani 1 1 d . . . O2 O 0.5247(2) 0.1933(3) 0.01806(5) 0.0590(7) Uani 1 1 d . . . O3 O 0.2405(2) 0.1365(3) 0.00481(5) 0.0583(7) Uani 1 1 d . . . O4 O 0.3532(3) -0.0376(3) 0.01125(5) 0.0683(8) Uani 1 1 d . . . O5 O 0.0260(2) 0.0793(2) 0.23889(5) 0.0400(5) Uani 1 1 d . . . O6 O 0.0307(2) -0.1269(2) 0.23743(5) 0.0512(7) Uani 1 1 d . . . O7 O 0.2776(2) -0.2654(2) 0.24229(5) 0.0515(6) Uani 1 1 d . . . O8 O 0.1544(2) -0.3321(2) 0.20545(5) 0.0457(6) Uani 1 1 d . . . O9 O 0.4425(2) 0.2668(2) 0.15389(4) 0.0511(6) Uani 1 1 d . . . O10 O 0.2106(2) 0.3023(2) 0.15128(5) 0.0540(6) Uani 1 1 d . . . S1 S 0.31751(8) 0.21951(8) 0.147497(16) 0.0374(2) Uani 1 1 d . . . C1 C 0.5350(3) 0.1964(3) 0.04479(7) 0.0390(8) Uani 1 1 d . . . C2 C 0.4232(3) 0.1608(3) 0.06380(6) 0.0339(7) Uani 1 1 d . . . C3 C 0.4232(3) 0.1939(3) 0.09301(6) 0.0342(7) Uani 1 1 d . . . H3 H 0.4928 0.2360 0.1009 0.041 Uiso 1 1 calc R . . C4 C 0.3197(3) 0.1646(3) 0.11071(7) 0.0359(7) Uani 1 1 d . . . C5 C 0.2173(3) 0.1009(3) 0.09918(7) 0.0466(9) Uani 1 1 d . . . H5 H 0.1485 0.0802 0.1111 0.056 Uiso 1 1 calc R . . C6 C 0.2171(3) 0.0680(3) 0.06998(7) 0.0488(9) Uani 1 1 d . . . H6 H 0.1477 0.0247 0.0623 0.059 Uiso 1 1 calc R . . C7 C 0.3188(3) 0.0984(3) 0.05188(7) 0.0366(7) Uani 1 1 d . . . C8 C 0.3086(3) 0.0610(3) 0.01976(7) 0.0414(8) Uani 1 1 d . . . C9 C 0.0698(3) -0.0240(3) 0.22918(6) 0.0331(7) Uani 1 1 d . . . C10 C 0.1739(3) -0.0223(3) 0.20665(6) 0.0299(7) Uani 1 1 d . . . C11 C 0.1962(3) 0.0849(3) 0.18997(6) 0.0312(7) Uani 1 1 d . . . H11 H 0.1482 0.1571 0.1931 0.037 Uiso 1 1 calc R . . C12 C 0.2895(3) 0.0839(3) 0.16879(6) 0.0323(7) Uani 1 1 d . . . C13 C 0.3646(3) -0.0220(3) 0.16461(7) 0.0425(8) Uani 1 1 d . . . H13 H 0.4307 -0.0205 0.1510 0.051 Uiso 1 1 calc R . . C14 C 0.3409(3) -0.1297(3) 0.18070(7) 0.0395(8) Uani 1 1 d . . . H14 H 0.3891 -0.2017 0.1774 0.047 Uiso 1 1 calc R . . C15 C 0.2454(3) -0.1304(3) 0.20172(6) 0.0305(7) Uani 1 1 d . . . C16 C 0.2239(3) -0.2510(3) 0.21870(6) 0.0355(7) Uani 1 1 d . . . C17 C 0.9342(3) 0.0329(4) 0.00750(7) 0.0437(8) Uani 1 1 d . . . H17 H 1.0044 0.0853 0.0051 0.052 Uiso 1 1 calc R . . C18 C 0.7458(3) -0.0348(4) 0.01640(8) 0.0576(10) Uani 1 1 d . . . H18 H 0.6600 -0.0373 0.0215 0.069 Uiso 1 1 calc R . . C19 C 0.8168(3) -0.1355(4) 0.00838(9) 0.0561(10) Uani 1 1 d . . . H19 H 0.7894 -0.2184 0.0069 0.067 Uiso 1 1 calc R . . C20 C 1.0432(3) -0.1661(4) -0.00859(7) 0.0490(9) Uani 1 1 d . . . H20A H 1.0341 -0.2524 -0.0021 0.059 Uiso 1 1 calc R . . H20B H 1.1222 -0.1337 -0.0005 0.059 Uiso 1 1 calc R . . C21 C 1.0511(3) -0.1638(3) -0.04150(7) 0.0439(8) Uani 1 1 d . . . C22 C 1.0990(5) -0.0609(4) -0.05581(8) 0.0745(13) Uani 1 1 d . . . H22 H 1.1266 0.0080 -0.0450 0.089 Uiso 1 1 calc R . . C23 C 1.1066(5) -0.0582(4) -0.08599(9) 0.0763(14) Uani 1 1 d . . . H23 H 1.1389 0.0132 -0.0952 0.092 Uiso 1 1 calc R . . C24 C 1.0676(3) -0.1587(3) -0.10306(7) 0.0443(8) Uani 1 1 d . . . C25 C 1.0196(3) -0.2618(4) -0.08862(8) 0.0564(10) Uani 1 1 d . . . H25 H 0.9932 -0.3313 -0.0994 0.068 Uiso 1 1 calc R . . C26 C 1.0100(3) -0.2638(4) -0.05811(8) 0.0544(9) Uani 1 1 d . . . H26 H 0.9753 -0.3338 -0.0489 0.065 Uiso 1 1 calc R . . C27 C 1.0818(3) -0.1545(3) -0.13534(7) 0.0431(8) Uani 1 1 d . . . C28 C 1.0408(4) -0.0520(3) -0.15121(8) 0.0595(11) Uani 1 1 d . . . H28 H 0.9994 0.0133 -0.1416 0.071 Uiso 1 1 calc R . . C29 C 1.0600(3) -0.0446(3) -0.18108(7) 0.0517(10) Uani 1 1 d . . . H29 H 1.0322 0.0261 -0.1912 0.062 Uiso 1 1 calc R . . C30 C 1.1198(3) -0.1404(3) -0.19623(7) 0.0397(8) Uani 1 1 d . . . C31 C 1.1584(3) -0.2437(4) -0.18026(7) 0.0480(8) Uani 1 1 d . . . H31 H 1.1982 -0.3100 -0.1899 0.058 Uiso 1 1 calc R . . C32 C 1.1396(3) -0.2511(3) -0.15066(7) 0.0473(8) Uani 1 1 d . . . H32 H 1.1661 -0.3225 -0.1406 0.057 Uiso 1 1 calc R . . C33 C 1.1469(3) -0.1269(3) -0.22859(8) 0.0525(9) Uani 1 1 d . . . H33A H 1.0763 -0.0832 -0.2378 0.063 Uiso 1 1 calc R . . H33B H 1.2227 -0.0759 -0.2311 0.063 Uiso 1 1 calc R . . C34 C 1.2790(3) -0.2970(3) -0.24942(7) 0.0426(8) Uani 1 1 d . . . H34 H 1.3561 -0.2559 -0.2465 0.051 Uiso 1 1 calc R . . C35 C 1.0763(4) -0.3345(4) -0.25001(10) 0.0811(15) Uani 1 1 d . . . H35 H 0.9885 -0.3271 -0.2478 0.097 Uiso 1 1 calc R . . C36 C 1.1415(3) -0.4348(4) -0.26052(11) 0.0819(16) Uani 1 1 d . . . H36 H 1.1046 -0.5089 -0.2672 0.098 Uiso 1 1 calc R . . C37 C 1.0102(3) 0.3916(4) 0.04378(8) 0.0607(11) Uani 1 1 d . . . H37 H 1.0229 0.4203 0.0247 0.073 Uiso 1 1 calc R . . C38 C 0.9345(5) 0.2984(4) 0.08055(9) 0.0730(13) Uani 1 1 d . . . H38 H 0.8834 0.2477 0.0923 0.088 Uiso 1 1 calc R . . C39 C 1.0343(5) 0.3648(4) 0.09029(10) 0.0754(14) Uani 1 1 d . . . H39 H 1.0637 0.3696 0.1095 0.090 Uiso 1 1 calc R . . C40 C 1.1762(4) 0.5268(5) 0.06743(10) 0.0899(16) Uani 1 1 d . . . H40A H 1.2028 0.5482 0.0477 0.108 Uiso 1 1 calc R . . H40B H 1.2510 0.5016 0.0785 0.108 Uiso 1 1 calc R . . C41 C 1.1141(4) 0.6395(5) 0.08187(10) 0.0732(13) Uani 1 1 d . . . C42 C 1.0002(5) 0.6871(5) 0.07112(10) 0.0910(17) Uani 1 1 d . . . H42 H 0.9677 0.6558 0.0536 0.109 Uiso 1 1 calc R . . C43 C 0.9344(5) 0.7797(4) 0.08576(9) 0.0778(14) Uani 1 1 d . . . H43 H 0.8574 0.8081 0.0781 0.093 Uiso 1 1 calc R . . C44 C 0.9799(4) 0.8311(4) 0.11146(9) 0.0593(11) Uani 1 1 d . . . C45 C 1.0954(5) 0.7847(4) 0.12172(10) 0.0792(14) Uani 1 1 d . . . H45 H 1.1299 0.8174 0.1389 0.095 Uiso 1 1 calc R . . C46 C 1.1598(4) 0.6917(5) 0.10705(11) 0.0853(15) Uani 1 1 d . . . H46 H 1.2371 0.6634 0.1145 0.102 Uiso 1 1 calc R . . C47 C 0.9102(4) 0.9293(3) 0.12780(8) 0.0564(10) Uani 1 1 d . . . C48 C 0.8265(4) 1.0105(4) 0.11380(9) 0.0686(12) Uani 1 1 d . . . H48 H 0.8118 1.0018 0.0938 0.082 Uiso 1 1 calc R . . C49 C 0.7648(4) 1.1036(4) 0.12915(10) 0.0698(12) Uani 1 1 d . . . H49 H 0.7090 1.1566 0.1192 0.084 Uiso 1 1 calc R . . C50 C 0.7836(4) 1.1205(4) 0.15873(10) 0.0686(12) Uani 1 1 d . . . C51 C 0.8628(4) 1.0365(5) 0.17276(10) 0.0723(13) Uani 1 1 d . . . H51 H 0.8755 1.0444 0.1929 0.087 Uiso 1 1 calc R . . C52 C 0.9237(4) 0.9418(4) 0.15791(9) 0.0680(12) Uani 1 1 d . . . H52 H 0.9745 0.8853 0.1682 0.082 Uiso 1 1 calc R . . C53 C 0.7277(4) 1.2294(4) 0.17528(11) 0.0774(13) Uani 1 1 d . . . H53A H 0.6533 1.2604 0.1649 0.093 Uiso 1 1 calc R . . H53B H 0.7009 1.2017 0.1946 0.093 Uiso 1 1 calc R . . C54 C 0.8947(3) 1.3519(3) 0.20150(8) 0.0506(9) Uani 1 1 d . . . H54 H 0.8922 1.3038 0.2185 0.061 Uiso 1 1 calc R . . C55 C 0.8557(4) 1.4201(4) 0.15795(10) 0.0722(13) Uani 1 1 d . . . H55 H 0.8217 1.4287 0.1392 0.087 Uiso 1 1 calc R . . C56 C 0.9479(4) 1.4927(4) 0.16999(8) 0.0592(10) Uani 1 1 d . . . H56 H 0.9878 1.5607 0.1611 0.071 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 Zn1 0.03645(18) 0.0393(2) 0.0380(2) 0.00084(18) 0.00444(15) -0.00092(19) Zn2 0.03406(18) 0.03057(19) 0.03319(19) -0.00207(16) 0.00494(16) -0.00034(17) N1 0.0404(16) 0.0394(17) 0.0513(18) 0.0001(13) 0.0090(13) 0.0004(14) N2 0.0392(16) 0.0360(18) 0.0439(16) -0.0035(12) 0.0028(13) 0.0030(13) N3 0.0436(15) 0.0451(17) 0.0438(15) -0.0055(15) 0.0005(12) 0.0098(16) N4 0.0309(14) 0.0407(17) 0.0537(17) -0.0127(13) -0.0058(13) 0.0063(13) N5 0.0466(16) 0.0482(18) 0.0385(16) -0.0022(13) -0.0011(14) -0.0054(15) N6 0.0456(17) 0.080(2) 0.052(2) -0.0247(17) -0.0023(16) -0.0043(19) N7 0.0497(18) 0.054(2) 0.071(2) -0.0105(18) -0.0150(17) -0.0017(17) N8 0.0467(16) 0.0431(19) 0.0362(16) -0.0022(13) -0.0030(12) -0.0035(14) O1 0.0382(12) 0.0574(17) 0.0471(14) 0.0033(12) 0.0089(10) -0.0085(12) O2 0.0558(15) 0.083(2) 0.0386(15) 0.0024(13) 0.0135(11) -0.0112(14) O3 0.0442(14) 0.083(2) 0.0472(15) 0.0241(13) -0.0028(11) 0.0069(14) O4 0.103(2) 0.0518(18) 0.0498(16) -0.0067(13) -0.0056(14) 0.0129(17) O5 0.0421(12) 0.0364(14) 0.0415(13) -0.0019(10) 0.0121(10) 0.0008(11) O6 0.0506(14) 0.0427(16) 0.0604(17) 0.0079(12) 0.0249(12) -0.0007(12) O7 0.0538(13) 0.0525(16) 0.0481(14) 0.0150(12) -0.0083(11) -0.0045(13) O8 0.0628(15) 0.0344(14) 0.0399(14) 0.0052(11) 0.0020(11) -0.0121(12) O9 0.0587(14) 0.0525(16) 0.0420(13) 0.0014(12) 0.0020(11) -0.0217(13) O10 0.0703(16) 0.0447(15) 0.0469(14) 0.0081(11) 0.0099(13) 0.0150(13) S1 0.0460(5) 0.0342(5) 0.0322(4) 0.0055(3) 0.0048(3) -0.0061(4) C1 0.0400(19) 0.040(2) 0.037(2) 0.0017(15) 0.0083(16) 0.0016(16) C2 0.0341(17) 0.0343(18) 0.0333(17) 0.0082(13) 0.0028(14) 0.0001(15) C3 0.0322(17) 0.0337(18) 0.0366(18) 0.0038(13) 0.0004(14) -0.0033(14) C4 0.0367(17) 0.0361(19) 0.0349(18) 0.0058(14) 0.0027(14) -0.0029(15) C5 0.0420(19) 0.059(2) 0.039(2) 0.0072(17) 0.0077(16) -0.0161(18) C6 0.0418(19) 0.063(3) 0.042(2) -0.0005(17) 0.0023(16) -0.0160(18) C7 0.0405(18) 0.0349(19) 0.0343(18) 0.0091(14) -0.0017(15) -0.0001(15) C8 0.0436(19) 0.045(2) 0.0353(19) 0.0122(16) -0.0040(15) -0.0035(17) C9 0.0315(15) 0.0355(17) 0.0324(16) 0.0033(16) -0.0013(14) -0.0064(15) C10 0.0288(14) 0.0363(18) 0.0245(15) 0.0002(13) -0.0023(12) -0.0043(15) C11 0.0300(16) 0.0281(17) 0.0356(17) -0.0005(13) 0.0005(13) 0.0041(14) C12 0.0390(17) 0.0310(18) 0.0268(16) 0.0030(13) 0.0011(14) -0.0053(15) C13 0.0400(17) 0.045(2) 0.0426(19) 0.0092(17) 0.0156(14) 0.0057(17) C14 0.0369(18) 0.035(2) 0.047(2) 0.0050(15) 0.0093(15) 0.0062(15) C15 0.0306(16) 0.0354(18) 0.0254(16) 0.0000(13) -0.0020(13) -0.0023(14) C16 0.0342(14) 0.0351(17) 0.0372(17) 0.0023(15) 0.0047(14) 0.0022(17) C17 0.041(2) 0.043(2) 0.0470(19) -0.0010(17) 0.0083(15) -0.0066(18) C18 0.042(2) 0.050(2) 0.081(3) -0.004(2) 0.0093(18) -0.013(2) C19 0.051(2) 0.041(2) 0.077(3) -0.009(2) 0.005(2) -0.0079(19) C20 0.050(2) 0.050(2) 0.047(2) -0.0023(17) 0.0011(17) 0.0133(18) C21 0.049(2) 0.036(2) 0.047(2) -0.0030(16) 0.0034(16) 0.0008(17) C22 0.120(4) 0.050(3) 0.053(3) -0.0199(19) 0.015(3) -0.035(3) C23 0.126(4) 0.047(3) 0.057(3) -0.0058(19) 0.017(3) -0.030(3) C24 0.053(2) 0.037(2) 0.043(2) -0.0037(16) -0.0007(17) 0.0004(18) C25 0.073(2) 0.041(2) 0.055(2) -0.002(2) -0.0037(19) -0.009(2) C26 0.066(2) 0.042(2) 0.055(2) 0.0023(19) 0.0002(18) -0.007(2) C27 0.0467(19) 0.038(2) 0.045(2) -0.0007(15) -0.0034(17) 0.0015(18) C28 0.088(3) 0.039(2) 0.052(2) -0.0055(17) 0.015(2) 0.024(2) C29 0.074(3) 0.032(2) 0.049(2) 0.0022(16) 0.0019(18) 0.0170(19) C30 0.0376(18) 0.0324(19) 0.049(2) -0.0005(15) 0.0016(15) 0.0069(15) C31 0.0530(19) 0.043(2) 0.048(2) -0.0028(18) 0.0044(16) 0.017(2) C32 0.0526(19) 0.036(2) 0.054(2) 0.0047(18) -0.0022(16) 0.0130(19) C33 0.059(2) 0.041(2) 0.058(2) 0.0032(19) 0.0067(19) 0.0181(18) C34 0.0359(17) 0.044(2) 0.048(2) -0.0029(16) 0.0021(15) 0.0035(16) C35 0.035(2) 0.087(3) 0.122(4) -0.047(3) -0.007(2) 0.007(2) C36 0.036(2) 0.079(3) 0.131(4) -0.055(3) -0.009(2) 0.001(2) C37 0.053(2) 0.089(3) 0.039(2) -0.008(2) 0.0039(18) -0.020(2) C38 0.112(4) 0.055(3) 0.052(3) 0.0142(19) -0.014(3) -0.022(3) C39 0.111(4) 0.061(3) 0.055(3) -0.005(2) -0.037(3) 0.004(3) C40 0.056(3) 0.123(4) 0.091(3) -0.047(3) 0.010(2) -0.033(3) C41 0.064(3) 0.083(3) 0.073(3) -0.018(3) 0.001(2) -0.037(3) C42 0.118(4) 0.100(4) 0.055(3) -0.011(3) -0.021(3) -0.024(4) C43 0.101(4) 0.073(3) 0.059(3) -0.005(2) -0.021(3) 0.000(3) C44 0.069(3) 0.051(3) 0.058(3) 0.001(2) -0.015(2) -0.029(2) C45 0.073(3) 0.085(4) 0.080(3) -0.030(3) -0.016(3) -0.020(3) C46 0.056(3) 0.102(4) 0.098(4) -0.027(3) -0.017(3) -0.022(3) C47 0.064(2) 0.044(2) 0.061(2) 0.0066(19) -0.019(2) -0.023(2) C48 0.090(3) 0.055(3) 0.060(3) 0.010(2) -0.012(2) -0.022(3) C49 0.073(3) 0.056(3) 0.080(3) 0.014(2) -0.018(2) -0.015(2) C50 0.052(2) 0.068(3) 0.086(3) -0.007(2) -0.025(2) -0.025(2) C51 0.068(3) 0.078(3) 0.071(3) -0.015(3) -0.029(2) -0.008(3) C52 0.068(3) 0.065(3) 0.071(3) -0.004(2) -0.032(2) -0.007(2) C53 0.047(2) 0.069(3) 0.116(4) -0.021(3) -0.021(2) -0.013(2) C54 0.055(2) 0.049(2) 0.049(2) -0.0032(17) -0.0043(19) -0.008(2) C55 0.079(3) 0.078(3) 0.060(3) -0.002(2) -0.035(2) 0.003(3) C56 0.069(3) 0.057(3) 0.051(2) 0.0078(19) -0.006(2) -0.002(2) _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 O3 1.935(2) 4 ? Zn1 O1 2.001(2) . ? Zn1 N5 2.005(3) . ? Zn1 N1 2.017(3) . ? Zn2 O8 1.960(2) 3 ? Zn2 N4 1.995(3) 4_345 ? Zn2 N8 2.018(3) 3_635 ? Zn2 O5 2.030(2) . ? N1 C17 1.322(4) . ? N1 C18 1.374(4) . ? N2 C17 1.339(4) . ? N2 C19 1.356(4) . ? N2 C20 1.478(4) . ? N3 C34 1.328(4) . ? N3 C35 1.354(5) . ? N3 C33 1.463(4) . ? N4 C34 1.308(4) . ? N4 C36 1.358(4) . ? N4 Zn2 1.995(3) 4_645 ? N5 C37 1.310(4) . ? N5 C38 1.349(4) . ? N6 C37 1.336(4) . ? N6 C39 1.350(5) . ? N6 C40 1.469(5) . ? N7 C54 1.322(4) . ? N7 C55 1.370(5) . ? N7 C53 1.473(5) . ? N8 C54 1.321(4) . ? N8 C56 1.362(4) . ? N8 Zn2 2.018(3) 3_665 ? O1 C1 1.277(4) . ? O2 C1 1.223(4) . ? O3 C8 1.274(4) . ? O3 Zn1 1.935(2) 4_455 ? O4 C8 1.212(4) . ? O5 C9 1.270(4) . ? O6 C9 1.228(4) . ? O7 C16 1.223(3) . ? O8 C16 1.280(4) . ? O8 Zn2 1.960(2) 3_545 ? O9 S1 1.434(2) . ? O10 S1 1.437(2) . ? S1 C12 1.763(3) . ? S1 C4 1.775(3) . ? C1 C2 1.507(4) . ? C2 C3 1.376(4) . ? C2 C7 1.392(4) . ? C3 C4 1.387(4) . ? C3 H3 0.9300 . ? C4 C5 1.374(4) . ? C5 C6 1.376(4) . ? C5 H5 0.9300 . ? C6 C7 1.387(4) . ? C6 H6 0.9300 . ? C7 C8 1.520(4) . ? C9 C10 1.498(4) . ? C10 C11 1.391(4) . ? C10 C15 1.392(4) . ? C11 C12 1.374(4) . ? C11 H11 0.9300 . ? C12 C13 1.389(4) . ? C13 C14 1.384(4) . ? C13 H13 0.9300 . ? C14 C15 1.386(4) . ? C14 H14 0.9300 . ? C15 C16 1.516(4) . ? C17 H17 0.9300 . ? C18 C19 1.355(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.501(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.370(5) . ? C21 C26 1.375(5) . ? C22 C23 1.377(5) . ? C22 H22 0.9300 . ? C23 C24 1.384(5) . ? C23 H23 0.9300 . ? C24 C25 1.375(5) . ? C24 C27 1.479(4) . ? C25 C26 1.393(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.377(5) . ? C27 C32 1.383(4) . ? C28 C29 1.377(4) . ? C28 H28 0.9300 . ? C29 C30 1.382(4) . ? C29 H29 0.9300 . ? C30 C31 1.379(5) . ? C30 C33 1.508(5) . ? C31 C32 1.365(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34 0.9300 . ? C35 C36 1.355(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.339(6) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.515(6) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C46 1.361(6) . ? C41 C42 1.388(7) . ? C42 C43 1.376(7) . ? C42 H42 0.9300 . ? C43 C44 1.377(5) . ? C43 H43 0.9300 . ? C44 C45 1.390(6) . ? C44 C47 1.477(6) . ? C45 C46 1.372(6) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C52 1.385(5) . ? C47 C48 1.388(5) . ? C48 C49 1.375(6) . ? C48 H48 0.9300 . ? C49 C50 1.373(6) . ? C49 H49 0.9300 . ? C50 C51 1.378(6) . ? C50 C53 1.502(6) . ? C51 C52 1.372(6) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54 0.9300 . ? C55 C56 1.354(5) . ? C55 H55 0.9300 . ? C56 H56 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 O3 Zn1 O1 117.91(10) 4 . ? O3 Zn1 N5 109.01(11) 4 . ? O1 Zn1 N5 101.25(10) . . ? O3 Zn1 N1 116.03(12) 4 . ? O1 Zn1 N1 104.51(11) . . ? N5 Zn1 N1 106.65(11) . . ? O8 Zn2 N4 111.01(10) 3 4_345 ? O8 Zn2 N8 99.78(10) 3 3_635 ? N4 Zn2 N8 114.21(11) 4_345 3_635 ? O8 Zn2 O5 111.66(9) 3 . ? N4 Zn2 O5 114.17(10) 4_345 . ? N8 Zn2 O5 105.02(10) 3_635 . ? C17 N1 C18 105.2(3) . . ? C17 N1 Zn1 125.8(2) . . ? C18 N1 Zn1 128.9(2) . . ? C17 N2 C19 107.7(3) . . ? C17 N2 C20 126.6(3) . . ? C19 N2 C20 125.5(3) . . ? C34 N3 C35 107.6(3) . . ? C34 N3 C33 124.4(3) . . ? C35 N3 C33 127.5(3) . . ? C34 N4 C36 105.2(3) . . ? C34 N4 Zn2 126.8(2) . 4_645 ? C36 N4 Zn2 127.9(3) . 4_645 ? C37 N5 C38 104.4(3) . . ? C37 N5 Zn1 129.2(2) . . ? C38 N5 Zn1 126.1(3) . . ? C37 N6 C39 106.4(3) . . ? C37 N6 C40 126.3(4) . . ? C39 N6 C40 125.3(3) . . ? C54 N7 C55 106.1(3) . . ? C54 N7 C53 125.7(4) . . ? C55 N7 C53 128.2(4) . . ? C54 N8 C56 106.4(3) . . ? C54 N8 Zn2 126.3(2) . 3_665 ? C56 N8 Zn2 127.1(2) . 3_665 ? C1 O1 Zn1 107.74(19) . . ? C8 O3 Zn1 134.7(2) . 4_455 ? C9 O5 Zn2 103.07(18) . . ? C16 O8 Zn2 118.7(2) . 3_545 ? O9 S1 O10 118.30(15) . . ? O9 S1 C12 109.15(14) . . ? O10 S1 C12 107.81(14) . . ? O9 S1 C4 107.16(14) . . ? O10 S1 C4 108.98(15) . . ? C12 S1 C4 104.60(15) . . ? O2 C1 O1 123.0(3) . . ? O2 C1 C2 119.8(3) . . ? O1 C1 C2 117.2(3) . . ? C3 C2 C7 119.9(3) . . ? C3 C2 C1 119.4(3) . . ? C7 C2 C1 120.6(3) . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 S1 120.8(2) . . ? C3 C4 S1 119.0(2) . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C2 119.0(3) . . ? C6 C7 C8 117.2(3) . . ? C2 C7 C8 123.8(3) . . ? O4 C8 O3 126.3(3) . . ? O4 C8 C7 120.5(3) . . ? O3 C8 C7 112.9(3) . . ? O6 C9 O5 123.0(3) . . ? O6 C9 C10 117.6(3) . . ? O5 C9 C10 119.4(3) . . ? C11 C10 C15 119.9(3) . . ? C11 C10 C9 120.4(3) . . ? C15 C10 C9 119.6(3) . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 S1 119.9(2) . . ? C13 C12 S1 119.6(2) . . ? C14 C13 C12 119.9(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 119.8(3) . . ? C14 C15 C16 117.7(3) . . ? C10 C15 C16 122.5(2) . . ? O7 C16 O8 126.3(3) . . ? O7 C16 C15 119.0(3) . . ? O8 C16 C15 114.5(3) . . ? N1 C17 N2 111.2(3) . . ? N1 C17 H17 124.4 . . ? N2 C17 H17 124.4 . . ? C19 C18 N1 109.6(3) . . ? C19 C18 H18 125.2 . . ? N1 C18 H18 125.2 . . ? C18 C19 N2 106.3(3) . . ? C18 C19 H19 126.8 . . ? N2 C19 H19 126.8 . . ? N2 C20 C21 112.7(3) . . ? N2 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? N2 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C26 118.2(3) . . ? C22 C21 C20 120.5(3) . . ? C26 C21 C20 121.3(3) . . ? C21 C22 C23 120.9(4) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C24 121.8(4) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 117.2(3) . . ? C25 C24 C27 122.4(3) . . ? C23 C24 C27 120.3(3) . . ? C24 C25 C26 121.1(4) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C21 C26 C25 120.9(4) . . ? C21 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C32 117.5(3) . . ? C28 C27 C24 121.0(3) . . ? C32 C27 C24 121.5(3) . . ? C27 C28 C29 121.2(3) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C28 C29 C30 121.1(3) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C31 C30 C29 117.3(3) . . ? C31 C30 C33 122.4(3) . . ? C29 C30 C33 120.2(3) . . ? C32 C31 C30 121.7(3) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C27 121.2(3) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? N3 C33 C30 113.3(3) . . ? N3 C33 H33A 108.9 . . ? C30 C33 H33A 108.9 . . ? N3 C33 H33B 108.9 . . ? C30 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? N4 C34 N3 111.7(3) . . ? N4 C34 H34 124.2 . . ? N3 C34 H34 124.2 . . ? N3 C35 C36 105.5(3) . . ? N3 C35 H35 127.2 . . ? C36 C35 H35 127.2 . . ? C35 C36 N4 109.9(4) . . ? C35 C36 H36 125.0 . . ? N4 C36 H36 125.0 . . ? N5 C37 N6 112.1(3) . . ? N5 C37 H37 123.9 . . ? N6 C37 H37 123.9 . . ? C39 C38 N5 110.9(4) . . ? C39 C38 H38 124.6 . . ? N5 C38 H38 124.6 . . ? C38 C39 N6 106.2(4) . . ? C38 C39 H39 126.9 . . ? N6 C39 H39 126.9 . . ? N6 C40 C41 108.7(3) . . ? N6 C40 H40A 110.0 . . ? C41 C40 H40A 110.0 . . ? N6 C40 H40B 110.0 . . ? C41 C40 H40B 110.0 . . ? H40A C40 H40B 108.3 . . ? C46 C41 C42 116.8(5) . . ? C46 C41 C40 122.5(5) . . ? C42 C41 C40 120.5(4) . . ? C43 C42 C41 121.6(5) . . ? C43 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C42 C43 C44 121.5(5) . . ? C42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C43 C44 C45 116.6(4) . . ? C43 C44 C47 122.5(4) . . ? C45 C44 C47 120.9(4) . . ? C46 C45 C44 121.5(4) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C41 C46 C45 122.1(5) . . ? C41 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C52 C47 C48 117.4(4) . . ? C52 C47 C44 121.1(4) . . ? C48 C47 C44 121.5(4) . . ? C49 C48 C47 120.9(4) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C50 C49 C48 121.7(4) . . ? C50 C49 H49 119.1 . . ? C48 C49 H49 119.1 . . ? C49 C50 C51 117.2(4) . . ? C49 C50 C53 122.5(4) . . ? C51 C50 C53 120.2(4) . . ? C52 C51 C50 121.9(4) . . ? C52 C51 H51 119.0 . . ? C50 C51 H51 119.0 . . ? C51 C52 C47 120.7(4) . . ? C51 C52 H52 119.6 . . ? C47 C52 H52 119.6 . . ? N7 C53 C50 110.9(3) . . ? N7 C53 H53A 109.5 . . ? C50 C53 H53A 109.5 . . ? N7 C53 H53B 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 108.1 . . ? N8 C54 N7 111.9(3) . . ? N8 C54 H54 124.1 . . ? N7 C54 H54 124.1 . . ? C56 C55 N7 107.7(4) . . ? C56 C55 H55 126.1 . . ? N7 C55 H55 126.1 . . ? C55 C56 N8 107.9(4) . . ? C55 C56 H56 126.1 . . ? N8 C56 H56 126.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 N1 C17 80.7(3) 4 . . . ? O1 Zn1 N1 C17 -147.7(3) . . . . ? N5 Zn1 N1 C17 -40.9(3) . . . . ? O3 Zn1 N1 C18 -103.0(3) 4 . . . ? O1 Zn1 N1 C18 28.6(3) . . . . ? N5 Zn1 N1 C18 135.3(3) . . . . ? O3 Zn1 N5 C37 -24.2(4) 4 . . . ? O1 Zn1 N5 C37 -149.2(3) . . . . ? N1 Zn1 N5 C37 101.8(3) . . . . ? O3 Zn1 N5 C38 149.2(3) 4 . . . ? O1 Zn1 N5 C38 24.2(3) . . . . ? N1 Zn1 N5 C38 -84.8(3) . . . . ? O3 Zn1 O1 C1 55.6(3) 4 . . . ? N5 Zn1 O1 C1 174.3(2) . . . . ? N1 Zn1 O1 C1 -75.0(2) . . . . ? O8 Zn2 O5 C9 172.93(17) 3 . . . ? N4 Zn2 O5 C9 -60.1(2) 4_345 . . . ? N8 Zn2 O5 C9 65.7(2) 3_635 . . . ? Zn1 O1 C1 O2 -6.6(4) . . . . ? Zn1 O1 C1 C2 173.0(2) . . . . ? O2 C1 C2 C3 -163.7(3) . . . . ? O1 C1 C2 C3 16.7(4) . . . . ? O2 C1 C2 C7 14.4(5) . . . . ? O1 C1 C2 C7 -165.3(3) . . . . ? C7 C2 C3 C4 0.3(5) . . . . ? C1 C2 C3 C4 178.4(3) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C2 C3 C4 S1 -175.1(2) . . . . ? O9 S1 C4 C5 172.7(3) . . . . ? O10 S1 C4 C5 -58.2(3) . . . . ? C12 S1 C4 C5 56.9(3) . . . . ? O9 S1 C4 C3 -11.4(3) . . . . ? O10 S1 C4 C3 117.7(3) . . . . ? C12 S1 C4 C3 -127.2(3) . . . . ? C3 C4 C5 C6 -1.0(5) . . . . ? S1 C4 C5 C6 174.9(3) . . . . ? C4 C5 C6 C7 -0.1(6) . . . . ? C5 C6 C7 C2 1.3(5) . . . . ? C5 C6 C7 C8 -178.5(3) . . . . ? C3 C2 C7 C6 -1.4(5) . . . . ? C1 C2 C7 C6 -179.5(3) . . . . ? C3 C2 C7 C8 178.4(3) . . . . ? C1 C2 C7 C8 0.4(5) . . . . ? Zn1 O3 C8 O4 -71.7(5) 4_455 . . . ? Zn1 O3 C8 C7 114.9(3) 4_455 . . . ? C6 C7 C8 O4 -94.0(4) . . . . ? C2 C7 C8 O4 86.2(4) . . . . ? C6 C7 C8 O3 79.8(4) . . . . ? C2 C7 C8 O3 -100.0(4) . . . . ? Zn2 O5 C9 O6 8.1(3) . . . . ? Zn2 O5 C9 C10 -171.8(2) . . . . ? O6 C9 C10 C11 160.5(3) . . . . ? O5 C9 C10 C11 -19.6(4) . . . . ? O6 C9 C10 C15 -17.2(4) . . . . ? O5 C9 C10 C15 162.8(3) . . . . ? C15 C10 C11 C12 -0.4(4) . . . . ? C9 C10 C11 C12 -178.1(3) . . . . ? C10 C11 C12 C13 -2.2(4) . . . . ? C10 C11 C12 S1 179.7(2) . . . . ? O9 S1 C12 C11 114.7(3) . . . . ? O10 S1 C12 C11 -15.0(3) . . . . ? C4 S1 C12 C11 -130.9(3) . . . . ? O9 S1 C12 C13 -63.3(3) . . . . ? O10 S1 C12 C13 167.0(3) . . . . ? C4 S1 C12 C13 51.1(3) . . . . ? C11 C12 C13 C14 3.6(5) . . . . ? S1 C12 C13 C14 -178.3(3) . . . . ? C12 C13 C14 C15 -2.4(5) . . . . ? C13 C14 C15 C10 -0.2(5) . . . . ? C13 C14 C15 C16 -180.0(3) . . . . ? C11 C10 C15 C14 1.6(4) . . . . ? C9 C10 C15 C14 179.3(3) . . . . ? C11 C10 C15 C16 -178.7(3) . . . . ? C9 C10 C15 C16 -1.0(4) . . . . ? Zn2 O8 C16 O7 16.6(4) 3_545 . . . ? Zn2 O8 C16 C15 -167.42(18) 3_545 . . . ? C14 C15 C16 O7 93.6(4) . . . . ? C10 C15 C16 O7 -86.1(4) . . . . ? C14 C15 C16 O8 -82.6(3) . . . . ? C10 C15 C16 O8 97.7(3) . . . . ? C18 N1 C17 N2 -0.2(4) . . . . ? Zn1 N1 C17 N2 176.8(2) . . . . ? C19 N2 C17 N1 0.3(4) . . . . ? C20 N2 C17 N1 175.4(3) . . . . ? C17 N1 C18 C19 0.1(4) . . . . ? Zn1 N1 C18 C19 -176.8(3) . . . . ? N1 C18 C19 N2 0.1(4) . . . . ? C17 N2 C19 C18 -0.2(4) . . . . ? C20 N2 C19 C18 -175.4(3) . . . . ? C17 N2 C20 C21 -83.1(4) . . . . ? C19 N2 C20 C21 91.2(4) . . . . ? N2 C20 C21 C22 77.0(5) . . . . ? N2 C20 C21 C26 -102.6(4) . . . . ? C26 C21 C22 C23 -0.5(7) . . . . ? C20 C21 C22 C23 179.9(4) . . . . ? C21 C22 C23 C24 -0.5(8) . . . . ? C22 C23 C24 C25 0.5(7) . . . . ? C22 C23 C24 C27 -177.7(4) . . . . ? C23 C24 C25 C26 0.5(6) . . . . ? C27 C24 C25 C26 178.6(3) . . . . ? C22 C21 C26 C25 1.5(6) . . . . ? C20 C21 C26 C25 -178.9(3) . . . . ? C24 C25 C26 C21 -1.6(6) . . . . ? C25 C24 C27 C28 132.9(4) . . . . ? C23 C24 C27 C28 -49.0(6) . . . . ? C25 C24 C27 C32 -48.9(5) . . . . ? C23 C24 C27 C32 129.1(4) . . . . ? C32 C27 C28 C29 -1.8(6) . . . . ? C24 C27 C28 C29 176.4(3) . . . . ? C27 C28 C29 C30 0.7(6) . . . . ? C28 C29 C30 C31 0.5(5) . . . . ? C28 C29 C30 C33 -176.3(4) . . . . ? C29 C30 C31 C32 -0.6(5) . . . . ? C33 C30 C31 C32 176.2(3) . . . . ? C30 C31 C32 C27 -0.5(5) . . . . ? C28 C27 C32 C31 1.7(5) . . . . ? C24 C27 C32 C31 -176.5(3) . . . . ? C34 N3 C33 C30 -98.1(4) . . . . ? C35 N3 C33 C30 72.4(5) . . . . ? C31 C30 C33 N3 24.5(5) . . . . ? C29 C30 C33 N3 -158.8(3) . . . . ? C36 N4 C34 N3 -0.1(4) . . . . ? Zn2 N4 C34 N3 179.7(2) 4_645 . . . ? C35 N3 C34 N4 0.9(4) . . . . ? C33 N3 C34 N4 173.0(3) . . . . ? C34 N3 C35 C36 -1.3(5) . . . . ? C33 N3 C35 C36 -173.1(4) . . . . ? N3 C35 C36 N4 1.3(6) . . . . ? C34 N4 C36 C35 -0.7(5) . . . . ? Zn2 N4 C36 C35 179.4(3) 4_645 . . . ? C38 N5 C37 N6 0.2(5) . . . . ? Zn1 N5 C37 N6 174.7(2) . . . . ? C39 N6 C37 N5 -0.8(5) . . . . ? C40 N6 C37 N5 -165.6(3) . . . . ? C37 N5 C38 C39 0.6(5) . . . . ? Zn1 N5 C38 C39 -174.2(3) . . . . ? N5 C38 C39 N6 -1.1(5) . . . . ? C37 N6 C39 C38 1.1(5) . . . . ? C40 N6 C39 C38 166.1(4) . . . . ? C37 N6 C40 C41 97.5(5) . . . . ? C39 N6 C40 C41 -64.5(6) . . . . ? N6 C40 C41 C46 119.1(5) . . . . ? N6 C40 C41 C42 -55.1(6) . . . . ? C46 C41 C42 C43 -2.2(7) . . . . ? C40 C41 C42 C43 172.3(5) . . . . ? C41 C42 C43 C44 1.4(8) . . . . ? C42 C43 C44 C45 0.1(7) . . . . ? C42 C43 C44 C47 -179.1(4) . . . . ? C43 C44 C45 C46 -0.6(7) . . . . ? C47 C44 C45 C46 178.6(4) . . . . ? C42 C41 C46 C45 1.7(7) . . . . ? C40 C41 C46 C45 -172.7(4) . . . . ? C44 C45 C46 C41 -0.3(8) . . . . ? C43 C44 C47 C52 152.0(4) . . . . ? C45 C44 C47 C52 -27.2(6) . . . . ? C43 C44 C47 C48 -26.5(6) . . . . ? C45 C44 C47 C48 154.4(4) . . . . ? C52 C47 C48 C49 3.3(6) . . . . ? C44 C47 C48 C49 -178.2(4) . . . . ? C47 C48 C49 C50 0.2(6) . . . . ? C48 C49 C50 C51 -2.7(6) . . . . ? C48 C49 C50 C53 173.6(4) . . . . ? C49 C50 C51 C52 1.7(6) . . . . ? C53 C50 C51 C52 -174.7(4) . . . . ? C50 C51 C52 C47 1.9(7) . . . . ? C48 C47 C52 C51 -4.3(6) . . . . ? C44 C47 C52 C51 177.2(4) . . . . ? C54 N7 C53 C50 -97.0(5) . . . . ? C55 N7 C53 C50 79.7(5) . . . . ? C49 C50 C53 N7 -96.8(5) . . . . ? C51 C50 C53 N7 79.4(5) . . . . ? C56 N8 C54 N7 -0.7(4) . . . . ? Zn2 N8 C54 N7 174.6(2) 3_665 . . . ? C55 N7 C54 N8 1.1(4) . . . . ? C53 N7 C54 N8 178.4(3) . . . . ? C54 N7 C55 C56 -1.0(5) . . . . ? C53 N7 C55 C56 -178.3(3) . . . . ? N7 C55 C56 N8 0.6(5) . . . . ? C54 N8 C56 C55 0.0(4) . . . . ? Zn2 N8 C56 C55 -175.2(3) 3_665 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.287 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.047 #=========END data_K3 _database_code_depnum_ccdc_archive 'CCDC 730710' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H32 Cd N6 O6 S, 3(H2 O)' _chemical_formula_sum 'C35 H38 Cd N6 O9 S' _chemical_formula_weight 831.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cd Cd -0.8075 1.2024 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.8544(13) _cell_length_b 14.6245(13) _cell_length_c 17.9282(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3632.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3852 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.38 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8347 _exptl_absorpt_correction_T_max 0.8692 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 18935 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.49 _reflns_number_total 6733 _reflns_number_gt 5563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 6733 _refine_ls_number_parameters 472 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.034 _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 0.18198(2) 0.83990(2) 0.612676(19) 0.03436(11) Uani 1 1 d . . . N1 N 0.3040(3) 0.9479(3) 0.6150(3) 0.0447(10) Uani 1 1 d . . . N2 N 0.4379(3) 1.0206(3) 0.6403(2) 0.0410(11) Uani 1 1 d . . . N3 N 0.8949(3) 0.9570(3) 0.5780(3) 0.0482(12) Uani 1 1 d . . . N4 N 1.0378(3) 0.9115(3) 0.6157(3) 0.0408(10) Uani 1 1 d . . . N5 N 0.7590(3) 1.3434(3) 0.6397(2) 0.0436(11) Uani 1 1 d . . . N6 N 0.8122(3) 1.3617(3) 0.7549(2) 0.0430(10) Uani 1 1 d . . . O1 O 0.0893(3) 0.6954(3) 0.5870(3) 0.0608(12) Uani 1 1 d . . . O2 O 0.2237(3) 0.6891(3) 0.6502(2) 0.0532(11) Uani 1 1 d . . . O3 O 0.2330(3) 0.2084(3) 1.0058(2) 0.0623(12) Uani 1 1 d . . . O4 O 0.3409(3) 0.1126(3) 0.9610(3) 0.0748(15) Uani 1 1 d . . . O5 O 0.0139(3) 0.2183(3) 0.6432(3) 0.0724(15) Uani 1 1 d . . . O6 O 0.1787(4) 0.2015(3) 0.5915(2) 0.0838(15) Uani 1 1 d . . . O1W O 0.4253(4) 0.6615(5) 0.6557(3) 0.111(2) Uani 1 1 d D . . H1WB H 0.3642 0.6664 0.6563 0.111 Uiso 1 1 d RD . . O2W O 0.0321(3) 0.2106(4) 0.0484(3) 0.0940(17) Uani 1 1 d D . . O3W O 0.4827(5) 0.9940(5) 0.8736(4) 0.146(3) Uani 1 1 d D . . H3WB H 0.5033 1.0483 0.8679 0.146 Uiso 1 1 d RD . . S1 S 0.11499(13) 0.24064(10) 0.64525(8) 0.0534(4) Uani 1 1 d . . . C1 C 0.1519(4) 0.6518(4) 0.6205(3) 0.0433(12) Uani 1 1 d . . . C2 C 0.1441(4) 0.5492(4) 0.6273(3) 0.0399(13) Uani 1 1 d . . . C3 C 0.0591(4) 0.5062(4) 0.6071(4) 0.0582(16) Uani 1 1 d . . . H3 H 0.0078 0.5408 0.5894 0.070 Uiso 1 1 calc R . . C4 C 0.0494(4) 0.4120(4) 0.6130(4) 0.0560(15) Uani 1 1 d . . . H4 H -0.0079 0.3834 0.5993 0.067 Uiso 1 1 calc R . . C5 C 0.1263(4) 0.3617(4) 0.6397(3) 0.0424(14) Uani 1 1 d . . . C6 C 0.2119(4) 0.4046(4) 0.6591(3) 0.0512(15) Uani 1 1 d . . . H6 H 0.2639 0.3700 0.6758 0.061 Uiso 1 1 calc R . . C7 C 0.2202(4) 0.4974(4) 0.6538(3) 0.0498(15) Uani 1 1 d . . . H7 H 0.2773 0.5259 0.6681 0.060 Uiso 1 1 calc R . . C8 C 0.2734(4) 0.1673(5) 0.9527(3) 0.0480(15) Uani 1 1 d . . . C9 C 0.2344(4) 0.1841(3) 0.8759(3) 0.0389(13) Uani 1 1 d . . . C10 C 0.1402(4) 0.2112(4) 0.8659(3) 0.0481(15) Uani 1 1 d . . . H10 H 0.1008 0.2199 0.9073 0.058 Uiso 1 1 calc R . . C11 C 0.1035(4) 0.2257(4) 0.7957(3) 0.0459(14) Uani 1 1 d . . . H11 H 0.0394 0.2430 0.7897 0.055 Uiso 1 1 calc R . . C12 C 0.1622(4) 0.2144(3) 0.7340(3) 0.0372(13) Uani 1 1 d . . . C13 C 0.2555(4) 0.1876(4) 0.7425(3) 0.0517(16) Uani 1 1 d . . . H13 H 0.2950 0.1808 0.7009 0.062 Uiso 1 1 calc R . . C14 C 0.2920(4) 0.1703(4) 0.8130(3) 0.0496(15) Uani 1 1 d . . . H14 H 0.3551 0.1495 0.8185 0.059 Uiso 1 1 calc R . . C15 C 0.3755(4) 0.9562(4) 0.6617(3) 0.0501(15) Uani 1 1 d . . . H15 H 0.3822 0.9214 0.7048 0.060 Uiso 1 1 calc R . . C16 C 0.3223(5) 1.0096(4) 0.5603(3) 0.0581(16) Uani 1 1 d . . . H16 H 0.2841 1.0190 0.5183 0.070 Uiso 1 1 calc R . . C17 C 0.4037(5) 1.0549(5) 0.5761(4) 0.0615(18) Uani 1 1 d . . . H17 H 0.4313 1.1014 0.5479 0.074 Uiso 1 1 calc R . . C18 C 0.5222(4) 1.0518(5) 0.6833(3) 0.0566(17) Uani 1 1 d . . . H18A H 0.5436 1.0027 0.7157 0.068 Uiso 1 1 calc R . . H18B H 0.5032 1.1028 0.7146 0.068 Uiso 1 1 calc R . . C19 C 0.9779(4) 0.9172(4) 0.5590(3) 0.0452(14) Uani 1 1 d . . . H19 H 0.9918 0.8960 0.5113 0.054 Uiso 1 1 calc R . . C20 C 0.9904(4) 0.9508(5) 0.6739(3) 0.0563(17) Uani 1 1 d . . . H20 H 1.0151 0.9578 0.7218 0.068 Uiso 1 1 calc R . . C21 C 0.9024(5) 0.9779(5) 0.6514(4) 0.064(2) Uani 1 1 d . . . H21 H 0.8554 1.0057 0.6807 0.076 Uiso 1 1 calc R . . C22 C 0.8122(4) 0.9734(5) 0.5277(3) 0.0620(17) Uani 1 1 d . . . H22A H 0.7775 0.9166 0.5198 0.074 Uiso 1 1 calc R . . H22B H 0.8356 0.9945 0.4797 0.074 Uiso 1 1 calc R . . C23 C 0.7860(4) 1.3024(4) 0.7043(3) 0.0449(14) Uani 1 1 d . . . H23 H 0.7859 1.2395 0.7117 0.054 Uiso 1 1 calc R . . C24 C 0.8017(4) 1.4454(4) 0.7205(3) 0.0478(14) Uani 1 1 d . . . H24 H 0.8148 1.5014 0.7428 0.057 Uiso 1 1 calc R . . C25 C 0.7701(4) 1.4349(4) 0.6506(3) 0.0474(14) Uani 1 1 d . . . H25 H 0.7581 1.4810 0.6162 0.057 Uiso 1 1 calc R . . C26 C 0.7231(6) 1.3018(4) 0.5707(3) 0.065(2) Uani 1 1 d . . . H26A H 0.7710 1.3095 0.5317 0.077 Uiso 1 1 calc R . . H26B H 0.6648 1.3331 0.5551 0.077 Uiso 1 1 calc R . . C27 C 0.6050(4) 1.0810(4) 0.6342(3) 0.0407(13) Uani 1 1 d . . . C28 C 0.6669(4) 1.0152(4) 0.6029(3) 0.0439(13) Uani 1 1 d . . . C29 C 0.7446(4) 1.0437(4) 0.5601(3) 0.0481(16) Uani 1 1 d . . . C30 C 0.7642(4) 1.1363(4) 0.5505(3) 0.0453(15) Uani 1 1 d . . . C31 C 0.7016(4) 1.2007(4) 0.5803(3) 0.0473(15) Uani 1 1 d . . . C32 C 0.6210(4) 1.1735(4) 0.6210(3) 0.0442(13) Uani 1 1 d . . . C33 C 0.6491(5) 0.9155(4) 0.6188(5) 0.080(2) Uani 1 1 d . . . H33A H 0.5945 0.8949 0.5903 0.121 Uiso 1 1 calc R . . H33B H 0.6363 0.9074 0.6710 0.121 Uiso 1 1 calc R . . H33C H 0.7050 0.8806 0.6050 0.121 Uiso 1 1 calc R . . C34 C 0.8559(4) 1.1651(6) 0.5084(4) 0.078(2) Uani 1 1 d . . . H34A H 0.8873 1.1118 0.4887 0.117 Uiso 1 1 calc R . . H34B H 0.8987 1.1962 0.5420 0.117 Uiso 1 1 calc R . . H34C H 0.8388 1.2053 0.4682 0.117 Uiso 1 1 calc R . . C35 C 0.5509(4) 1.2478(4) 0.6519(4) 0.077(2) Uani 1 1 d . . . H35A H 0.4858 1.2324 0.6385 0.116 Uiso 1 1 calc R . . H35B H 0.5673 1.3062 0.6309 0.116 Uiso 1 1 calc R . . H35C H 0.5564 1.2506 0.7052 0.116 Uiso 1 1 calc R . . H2WB H -0.0166 0.1839 0.0264 0.077 Uiso 1 1 d RD . . H1WA H 0.4490 0.7054 0.6249 0.077 Uiso 1 1 d RD . . H3WA H 0.5301 0.9568 0.8527 0.077 Uiso 1 1 d RD . . H2WA H 0.0887 0.1957 0.0285 0.077 Uiso 1 1 d RD . . 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 0.03235(17) 0.03724(19) 0.03349(18) 0.00280(17) -0.00085(17) 0.00119(18) N1 0.041(3) 0.049(3) 0.044(2) 0.003(2) -0.005(3) -0.008(2) N2 0.034(2) 0.051(3) 0.038(3) 0.003(2) 0.0025(19) -0.001(2) N3 0.036(3) 0.065(3) 0.043(3) -0.013(2) -0.003(2) 0.011(2) N4 0.039(2) 0.050(3) 0.033(2) -0.002(2) -0.001(2) 0.009(2) N5 0.061(3) 0.042(3) 0.027(2) 0.000(2) -0.0099(19) -0.012(3) N6 0.051(3) 0.043(3) 0.035(2) -0.0076(18) -0.005(2) 0.002(2) O1 0.049(2) 0.041(2) 0.093(4) 0.018(2) 0.001(2) 0.0074(19) O2 0.071(3) 0.039(2) 0.050(2) 0.0015(18) 0.000(2) -0.001(2) O3 0.079(3) 0.071(3) 0.037(2) 0.001(2) -0.011(2) -0.009(2) O4 0.056(3) 0.095(4) 0.074(3) 0.028(3) -0.019(2) 0.004(3) O5 0.087(3) 0.057(3) 0.073(3) 0.014(2) -0.043(3) -0.028(3) O6 0.161(5) 0.057(3) 0.034(2) -0.0003(18) 0.013(3) 0.027(3) O1W 0.079(4) 0.134(5) 0.120(5) 0.044(4) 0.004(3) 0.023(4) O2W 0.066(3) 0.136(5) 0.079(4) 0.003(3) 0.005(3) -0.001(3) O3W 0.176(7) 0.098(5) 0.163(7) 0.006(5) -0.017(6) 0.015(5) S1 0.0920(13) 0.0368(8) 0.0314(7) 0.0013(6) -0.0073(8) -0.0026(8) C1 0.052(3) 0.037(3) 0.041(3) 0.003(3) 0.009(3) 0.000(3) C2 0.045(3) 0.037(3) 0.037(3) -0.002(2) 0.005(2) 0.004(2) C3 0.055(4) 0.044(4) 0.076(4) 0.013(3) -0.002(4) -0.001(3) C4 0.054(3) 0.047(3) 0.066(4) 0.001(4) -0.022(4) -0.006(3) C5 0.063(4) 0.037(3) 0.027(3) 0.002(2) 0.003(2) -0.002(3) C6 0.051(4) 0.046(4) 0.056(4) 0.004(3) -0.006(3) 0.008(3) C7 0.058(4) 0.044(4) 0.048(4) 0.005(3) -0.009(3) -0.001(3) C8 0.048(3) 0.052(4) 0.043(3) 0.014(3) -0.009(3) -0.015(3) C9 0.046(3) 0.033(3) 0.039(3) 0.005(2) -0.004(3) -0.004(2) C10 0.055(3) 0.059(4) 0.030(3) 0.004(2) 0.008(2) 0.007(3) C11 0.047(3) 0.052(4) 0.039(3) 0.003(3) -0.004(3) 0.004(3) C12 0.053(4) 0.029(3) 0.030(3) 0.001(2) -0.002(2) 0.002(2) C13 0.060(4) 0.049(4) 0.045(3) 0.008(3) 0.017(3) 0.006(3) C14 0.041(3) 0.054(4) 0.053(3) 0.010(3) 0.004(2) 0.008(3) C15 0.042(3) 0.057(4) 0.051(4) 0.014(3) -0.002(3) -0.006(3) C16 0.059(4) 0.066(4) 0.049(3) 0.021(3) -0.017(3) -0.031(4) C17 0.061(4) 0.067(4) 0.057(4) 0.025(3) -0.010(3) -0.022(3) C18 0.045(4) 0.076(5) 0.049(4) -0.001(3) -0.007(3) -0.015(3) C19 0.037(3) 0.064(4) 0.034(3) -0.008(3) -0.001(2) 0.008(3) C20 0.053(4) 0.076(5) 0.040(4) -0.006(3) -0.003(3) 0.017(3) C21 0.055(4) 0.098(6) 0.038(4) -0.012(3) 0.001(3) 0.026(4) C22 0.045(3) 0.085(5) 0.056(4) -0.020(3) -0.017(3) 0.024(4) C23 0.058(4) 0.035(3) 0.041(3) 0.002(2) -0.004(3) -0.008(3) C24 0.062(4) 0.036(3) 0.046(3) -0.002(2) -0.008(3) -0.002(3) C25 0.068(4) 0.040(3) 0.035(3) 0.002(2) -0.003(3) -0.006(3) C26 0.107(6) 0.054(4) 0.033(3) 0.000(3) -0.020(3) -0.023(4) C27 0.032(3) 0.048(3) 0.042(3) 0.000(2) -0.005(2) -0.007(3) C28 0.035(3) 0.037(3) 0.059(4) -0.001(3) -0.013(3) 0.003(2) C29 0.036(3) 0.065(4) 0.044(3) -0.007(3) -0.015(3) 0.007(3) C30 0.041(3) 0.062(4) 0.033(3) 0.002(3) -0.010(2) -0.009(3) C31 0.061(4) 0.042(3) 0.039(3) 0.002(2) -0.015(3) -0.014(3) C32 0.042(3) 0.046(3) 0.045(3) -0.008(3) -0.007(3) 0.005(3) C33 0.062(4) 0.048(4) 0.131(7) -0.004(5) -0.003(5) -0.006(3) C34 0.051(3) 0.123(6) 0.061(4) 0.014(5) -0.002(3) -0.025(4) C35 0.066(5) 0.064(5) 0.102(6) -0.024(4) -0.016(4) 0.015(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 Cd1 N4 2.256(4) 1_455 ? Cd1 N1 2.314(4) . ? Cd1 O3 2.358(4) 2_564 ? Cd1 O2 2.377(4) . ? Cd1 N6 2.397(4) 4_646 ? Cd1 O1 2.516(4) . ? N1 C15 1.302(7) . ? N1 C16 1.357(7) . ? N2 C15 1.335(7) . ? N2 C17 1.342(7) . ? N2 C18 1.472(7) . ? N3 C19 1.333(7) . ? N3 C21 1.354(7) . ? N3 C22 1.478(7) . ? N4 C19 1.315(7) . ? N4 C20 1.359(7) . ? N4 Cd1 2.256(4) 1_655 ? N5 C23 1.356(7) . ? N5 C25 1.360(7) . ? N5 C26 1.465(6) . ? N6 C23 1.307(6) . ? N6 C24 1.378(6) . ? N6 Cd1 2.397(4) 4_656 ? O1 C1 1.233(6) . ? O2 C1 1.254(6) . ? O3 C8 1.257(7) . ? O3 Cd1 2.358(4) 2_565 ? O4 C8 1.241(7) . ? O5 S1 1.439(5) . ? O6 S1 1.427(5) . ? O1W H1WB 0.8500 . ? O1W H1WA 0.9089 . ? O2W H2WB 0.8734 . ? O2W H2WA 0.8887 . ? O3W H3WB 0.8500 . ? O3W H3WA 0.9318 . ? S1 C12 1.763(5) . ? S1 C5 1.780(5) . ? C1 C2 1.510(7) . ? C2 C3 1.382(7) . ? C2 C7 1.383(7) . ? C3 C4 1.387(8) . ? C3 H3 0.9300 . ? C4 C5 1.382(8) . ? C4 H4 0.9300 . ? C5 C6 1.385(8) . ? C6 C7 1.366(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.499(7) . ? C9 C10 1.375(7) . ? C9 C14 1.396(7) . ? C10 C11 1.374(7) . ? C10 H10 0.9300 . ? C11 C12 1.383(7) . ? C11 H11 0.9300 . ? C12 C13 1.360(8) . ? C13 C14 1.384(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.339(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C27 1.507(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19 0.9300 . ? C20 C21 1.344(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C29 1.507(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23 0.9300 . ? C24 C25 1.335(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C31 1.518(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C32 1.391(8) . ? C27 C28 1.406(7) . ? C28 C29 1.387(8) . ? C28 C33 1.506(8) . ? C29 C30 1.391(8) . ? C30 C31 1.387(8) . ? C30 C34 1.537(8) . ? C31 C32 1.391(8) . ? C32 C35 1.559(8) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cd1 N1 109.23(16) 1_455 . ? N4 Cd1 O3 126.94(17) 1_455 2_564 ? N1 Cd1 O3 81.63(16) . 2_564 ? N4 Cd1 O2 129.74(16) 1_455 . ? N1 Cd1 O2 116.77(15) . . ? O3 Cd1 O2 80.26(15) 2_564 . ? N4 Cd1 N6 86.78(17) 1_455 4_646 ? N1 Cd1 N6 82.34(16) . 4_646 ? O3 Cd1 N6 145.94(16) 2_564 4_646 ? O2 Cd1 N6 80.49(14) . 4_646 ? N4 Cd1 O1 86.70(14) 1_455 . ? N1 Cd1 O1 161.76(14) . . ? O3 Cd1 O1 81.61(14) 2_564 . ? O2 Cd1 O1 52.91(14) . . ? N6 Cd1 O1 108.09(15) 4_646 . ? C15 N1 C16 105.1(5) . . ? C15 N1 Cd1 129.1(4) . . ? C16 N1 Cd1 125.3(4) . . ? C15 N2 C17 106.4(5) . . ? C15 N2 C18 125.6(5) . . ? C17 N2 C18 127.8(5) . . ? C19 N3 C21 106.3(5) . . ? C19 N3 C22 125.7(5) . . ? C21 N3 C22 128.0(5) . . ? C19 N4 C20 105.2(4) . . ? C19 N4 Cd1 124.7(4) . 1_655 ? C20 N4 Cd1 130.0(4) . 1_655 ? C23 N5 C25 106.3(4) . . ? C23 N5 C26 129.1(5) . . ? C25 N5 C26 124.6(4) . . ? C23 N6 C24 104.4(4) . . ? C23 N6 Cd1 127.5(4) . 4_656 ? C24 N6 Cd1 124.4(3) . 4_656 ? C1 O1 Cd1 89.2(4) . . ? C1 O2 Cd1 95.2(4) . . ? C8 O3 Cd1 104.5(4) . 2_565 ? H1WB O1W H1WA 107.9 . . ? H2WB O2W H2WA 113.1 . . ? H3WB O3W H3WA 105.1 . . ? O6 S1 O5 119.6(3) . . ? O6 S1 C12 107.0(3) . . ? O5 S1 C12 109.5(3) . . ? O6 S1 C5 107.9(3) . . ? O5 S1 C5 108.1(3) . . ? C12 S1 C5 103.6(2) . . ? O1 C1 O2 122.8(5) . . ? O1 C1 C2 120.1(5) . . ? O2 C1 C2 117.1(5) . . ? C3 C2 C7 119.3(5) . . ? C3 C2 C1 119.5(5) . . ? C7 C2 C1 121.2(5) . . ? C2 C3 C4 121.0(5) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 118.7(5) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 120.3(5) . . ? C4 C5 S1 118.8(4) . . ? C6 C5 S1 120.8(4) . . ? C7 C6 C5 120.4(5) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C2 120.2(6) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? O4 C8 O3 123.6(5) . . ? O4 C8 C9 119.2(6) . . ? O3 C8 C9 117.2(6) . . ? C10 C9 C14 118.6(5) . . ? C10 C9 C8 120.6(5) . . ? C14 C9 C8 120.8(5) . . ? C11 C10 C9 121.0(5) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.8(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 120.2(5) . . ? C13 C12 S1 121.2(4) . . ? C11 C12 S1 118.5(4) . . ? C12 C13 C14 120.2(5) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C9 120.1(5) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? N1 C15 N2 111.9(5) . . ? N1 C15 H15 124.0 . . ? N2 C15 H15 124.0 . . ? C17 C16 N1 109.5(5) . . ? C17 C16 H16 125.3 . . ? N1 C16 H16 125.3 . . ? C16 C17 N2 107.1(5) . . ? C16 C17 H17 126.4 . . ? N2 C17 H17 126.4 . . ? N2 C18 C27 112.7(5) . . ? N2 C18 H18A 109.1 . . ? C27 C18 H18A 109.1 . . ? N2 C18 H18B 109.1 . . ? C27 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? N4 C19 N3 112.0(5) . . ? N4 C19 H19 124.0 . . ? N3 C19 H19 124.0 . . ? C21 C20 N4 109.4(6) . . ? C21 C20 H20 125.3 . . ? N4 C20 H20 125.3 . . ? C20 C21 N3 107.1(6) . . ? C20 C21 H21 126.4 . . ? N3 C21 H21 126.4 . . ? N3 C22 C29 110.9(4) . . ? N3 C22 H22A 109.5 . . ? C29 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? C29 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? N6 C23 N5 112.1(5) . . ? N6 C23 H23 124.0 . . ? N5 C23 H23 124.0 . . ? C25 C24 N6 110.6(5) . . ? C25 C24 H24 124.7 . . ? N6 C24 H24 124.7 . . ? C24 C25 N5 106.6(5) . . ? C24 C25 H25 126.7 . . ? N5 C25 H25 126.7 . . ? N5 C26 C31 112.0(5) . . ? N5 C26 H26A 109.2 . . ? C31 C26 H26A 109.2 . . ? N5 C26 H26B 109.2 . . ? C31 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C32 C27 C28 120.0(5) . . ? C32 C27 C18 119.8(5) . . ? C28 C27 C18 120.2(5) . . ? C29 C28 C27 119.3(5) . . ? C29 C28 C33 121.5(5) . . ? C27 C28 C33 119.2(5) . . ? C28 C29 C30 120.8(5) . . ? C28 C29 C22 119.4(6) . . ? C30 C29 C22 119.7(6) . . ? C31 C30 C29 119.4(5) . . ? C31 C30 C34 121.3(6) . . ? C29 C30 C34 119.2(6) . . ? C30 C31 C32 120.6(5) . . ? C30 C31 C26 119.6(6) . . ? C32 C31 C26 119.7(6) . . ? C27 C32 C31 119.7(5) . . ? C27 C32 C35 121.2(5) . . ? C31 C32 C35 119.1(5) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cd1 N1 C15 123.7(5) 1_455 . . . ? O3 Cd1 N1 C15 -110.0(5) 2_564 . . . ? O2 Cd1 N1 C15 -35.4(5) . . . . ? N6 Cd1 N1 C15 39.8(5) 4_646 . . . ? O1 Cd1 N1 C15 -86.5(7) . . . . ? N4 Cd1 N1 C16 -65.8(5) 1_455 . . . ? O3 Cd1 N1 C16 60.5(5) 2_564 . . . ? O2 Cd1 N1 C16 135.1(5) . . . . ? N6 Cd1 N1 C16 -149.6(5) 4_646 . . . ? O1 Cd1 N1 C16 84.0(7) . . . . ? N4 Cd1 O1 C1 -148.4(4) 1_455 . . . ? N1 Cd1 O1 C1 60.1(7) . . . . ? O3 Cd1 O1 C1 83.5(3) 2_564 . . . ? O2 Cd1 O1 C1 -0.6(3) . . . . ? N6 Cd1 O1 C1 -62.9(4) 4_646 . . . ? N4 Cd1 O2 C1 44.3(4) 1_455 . . . ? N1 Cd1 O2 C1 -161.6(3) . . . . ? O3 Cd1 O2 C1 -86.2(3) 2_564 . . . ? N6 Cd1 O2 C1 122.0(3) 4_646 . . . ? O1 Cd1 O2 C1 0.6(3) . . . . ? Cd1 O1 C1 O2 1.0(5) . . . . ? Cd1 O1 C1 C2 -179.0(4) . . . . ? Cd1 O2 C1 O1 -1.1(6) . . . . ? Cd1 O2 C1 C2 179.0(4) . . . . ? O1 C1 C2 C3 -11.0(8) . . . . ? O2 C1 C2 C3 168.9(5) . . . . ? O1 C1 C2 C7 169.5(5) . . . . ? O2 C1 C2 C7 -10.6(7) . . . . ? C7 C2 C3 C4 -0.2(10) . . . . ? C1 C2 C3 C4 -179.7(6) . . . . ? C2 C3 C4 C5 0.2(11) . . . . ? C3 C4 C5 C6 -0.9(10) . . . . ? C3 C4 C5 S1 -178.5(5) . . . . ? O6 S1 C5 C4 111.8(5) . . . . ? O5 S1 C5 C4 -18.8(6) . . . . ? C12 S1 C5 C4 -135.0(5) . . . . ? O6 S1 C5 C6 -65.8(5) . . . . ? O5 S1 C5 C6 163.5(4) . . . . ? C12 S1 C5 C6 47.4(5) . . . . ? C4 C5 C6 C7 1.6(9) . . . . ? S1 C5 C6 C7 179.2(4) . . . . ? C5 C6 C7 C2 -1.6(8) . . . . ? C3 C2 C7 C6 0.9(9) . . . . ? C1 C2 C7 C6 -179.6(5) . . . . ? Cd1 O3 C8 O4 1.8(7) 2_565 . . . ? Cd1 O3 C8 C9 179.7(4) 2_565 . . . ? O4 C8 C9 C10 152.9(6) . . . . ? O3 C8 C9 C10 -25.1(8) . . . . ? O4 C8 C9 C14 -25.4(8) . . . . ? O3 C8 C9 C14 156.6(6) . . . . ? C14 C9 C10 C11 -0.8(8) . . . . ? C8 C9 C10 C11 -179.2(5) . . . . ? C9 C10 C11 C12 -1.1(9) . . . . ? C10 C11 C12 C13 1.1(8) . . . . ? C10 C11 C12 S1 -175.9(4) . . . . ? O6 S1 C12 C13 17.8(5) . . . . ? O5 S1 C12 C13 148.8(5) . . . . ? C5 S1 C12 C13 -96.0(5) . . . . ? O6 S1 C12 C11 -165.2(5) . . . . ? O5 S1 C12 C11 -34.2(5) . . . . ? C5 S1 C12 C11 81.0(5) . . . . ? C11 C12 C13 C14 0.8(8) . . . . ? S1 C12 C13 C14 177.8(4) . . . . ? C12 C13 C14 C9 -2.8(9) . . . . ? C10 C9 C14 C13 2.7(8) . . . . ? C8 C9 C14 C13 -178.9(6) . . . . ? C16 N1 C15 N2 0.7(7) . . . . ? Cd1 N1 C15 N2 172.7(4) . . . . ? C17 N2 C15 N1 -0.1(7) . . . . ? C18 N2 C15 N1 175.1(5) . . . . ? C15 N1 C16 C17 -1.1(8) . . . . ? Cd1 N1 C16 C17 -173.5(4) . . . . ? N1 C16 C17 N2 1.1(8) . . . . ? C15 N2 C17 C16 -0.6(7) . . . . ? C18 N2 C17 C16 -175.6(6) . . . . ? C15 N2 C18 C27 148.0(6) . . . . ? C17 N2 C18 C27 -37.9(9) . . . . ? C20 N4 C19 N3 -0.6(7) . . . . ? Cd1 N4 C19 N3 175.0(4) 1_655 . . . ? C21 N3 C19 N4 -0.1(7) . . . . ? C22 N3 C19 N4 -179.6(6) . . . . ? C19 N4 C20 C21 1.1(8) . . . . ? Cd1 N4 C20 C21 -174.3(5) 1_655 . . . ? N4 C20 C21 N3 -1.1(9) . . . . ? C19 N3 C21 C20 0.7(8) . . . . ? C22 N3 C21 C20 -179.8(6) . . . . ? C19 N3 C22 C29 -162.6(6) . . . . ? C21 N3 C22 C29 17.9(10) . . . . ? C24 N6 C23 N5 -0.2(7) . . . . ? Cd1 N6 C23 N5 158.6(4) 4_656 . . . ? C25 N5 C23 N6 0.6(7) . . . . ? C26 N5 C23 N6 -178.5(6) . . . . ? C23 N6 C24 C25 -0.3(7) . . . . ? Cd1 N6 C24 C25 -160.0(4) 4_656 . . . ? N6 C24 C25 N5 0.6(7) . . . . ? C23 N5 C25 C24 -0.8(6) . . . . ? C26 N5 C25 C24 178.4(6) . . . . ? C23 N5 C26 C31 9.5(10) . . . . ? C25 N5 C26 C31 -169.6(6) . . . . ? N2 C18 C27 C32 100.6(6) . . . . ? N2 C18 C27 C28 -80.6(7) . . . . ? C32 C27 C28 C29 1.1(8) . . . . ? C18 C27 C28 C29 -177.7(5) . . . . ? C32 C27 C28 C33 179.2(6) . . . . ? C18 C27 C28 C33 0.4(8) . . . . ? C27 C28 C29 C30 2.7(8) . . . . ? C33 C28 C29 C30 -175.3(6) . . . . ? C27 C28 C29 C22 178.9(5) . . . . ? C33 C28 C29 C22 0.9(8) . . . . ? N3 C22 C29 C28 -92.9(7) . . . . ? N3 C22 C29 C30 83.4(7) . . . . ? C28 C29 C30 C31 -4.0(8) . . . . ? C22 C29 C30 C31 179.9(5) . . . . ? C28 C29 C30 C34 174.7(5) . . . . ? C22 C29 C30 C34 -1.4(8) . . . . ? C29 C30 C31 C32 1.4(8) . . . . ? C34 C30 C31 C32 -177.3(5) . . . . ? C29 C30 C31 C26 179.4(5) . . . . ? C34 C30 C31 C26 0.7(8) . . . . ? N5 C26 C31 C30 -105.1(7) . . . . ? N5 C26 C31 C32 72.8(7) . . . . ? C28 C27 C32 C31 -3.6(8) . . . . ? C18 C27 C32 C31 175.2(5) . . . . ? C28 C27 C32 C35 177.2(5) . . . . ? C18 C27 C32 C35 -4.0(8) . . . . ? C30 C31 C32 C27 2.4(8) . . . . ? C26 C31 C32 C27 -175.6(5) . . . . ? C30 C31 C32 C35 -178.4(5) . . . . ? C26 C31 C32 C35 3.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.587 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.115 #=======END data_K4 _database_code_depnum_ccdc_archive 'CCDC 730711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H26 Co N4 O6 S' _chemical_formula_sum 'C34 H26 Co N4 O6 S' _chemical_formula_weight 677.58 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' 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' _cell_length_a 6.039(3) _cell_length_b 29.302(15) _cell_length_c 17.045(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.896(7) _cell_angle_gamma 90.00 _cell_volume 2980(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1425 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 20.47 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8387 _exptl_absorpt_correction_T_max 0.9460 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 7364 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.09 _reflns_number_total 4912 _reflns_number_gt 3634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(18) _refine_ls_number_reflns 4912 _refine_ls_number_parameters 415 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.991 _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 Co1 Co 0.52170(10) 0.05326(2) 1.00708(5) 0.0407(2) Uani 1 1 d . . . N1 N 0.2726(7) 0.03312(15) 0.9214(2) 0.0394(11) Uani 1 1 d . . . N2 N -0.0244(7) 0.03109(15) 0.8278(3) 0.0419(11) Uani 1 1 d . . . N3 N -0.3337(7) 0.40162(14) 0.6776(3) 0.0407(11) Uani 1 1 d . . . N4 N -0.1140(7) 0.43752(15) 0.6067(2) 0.0443(11) Uani 1 1 d . . . O1 O 0.7053(6) 0.10812(12) 0.9907(2) 0.0459(10) Uani 1 1 d . . . O2 O 0.3628(6) 0.13694(13) 0.9802(2) 0.0542(11) Uani 1 1 d . . . O3 O 0.2140(6) 0.50006(12) 0.9953(2) 0.0522(11) Uani 1 1 d . . . O4 O 0.3937(7) 0.50287(14) 1.1190(2) 0.0615(12) Uani 1 1 d . . . O5 O 0.9776(7) 0.34069(13) 0.8865(2) 0.0591(11) Uani 1 1 d . . . O6 O 1.1542(6) 0.33187(13) 1.0267(2) 0.0543(11) Uani 1 1 d . . . S1 S 0.9543(2) 0.33211(5) 0.96802(9) 0.0426(4) Uani 1 1 d . . . C1 C 0.5703(10) 0.14235(18) 0.9834(3) 0.0396(13) Uani 1 1 d . . . C2 C 0.6619(8) 0.18912(17) 0.9797(3) 0.0352(12) Uani 1 1 d . . . C3 C 0.8575(9) 0.19722(19) 0.9483(3) 0.0504(15) Uani 1 1 d . . . H3 H 0.9362 0.1729 0.9307 0.060 Uiso 1 1 calc R . . C4 C 0.9356(9) 0.24178(19) 0.9430(3) 0.0496(15) Uani 1 1 d . . . H4 H 1.0628 0.2472 0.9198 0.060 Uiso 1 1 calc R . . C5 C 0.8250(9) 0.27794(18) 0.9721(3) 0.0399(13) Uani 1 1 d . . . C6 C 0.6351(9) 0.27011(18) 1.0042(3) 0.0500(15) Uani 1 1 d . . . H6 H 0.5624 0.2942 1.0250 0.060 Uiso 1 1 calc R . . C7 C 0.5508(11) 0.22610(17) 1.0059(4) 0.0511(14) Uani 1 1 d . . . H7 H 0.4165 0.2214 1.0250 0.061 Uiso 1 1 calc R . . C8 C 0.3612(9) 0.48619(19) 1.0531(4) 0.0435(14) Uani 1 1 d . . . C9 C 0.5027(8) 0.44609(17) 1.0324(3) 0.0347(12) Uani 1 1 d . . . C10 C 0.6997(9) 0.4351(2) 1.0818(3) 0.0500(15) Uani 1 1 d . . . H10 H 0.7435 0.4519 1.1278 0.060 Uiso 1 1 calc R . . C11 C 0.8326(9) 0.39916(19) 1.0632(3) 0.0511(15) Uani 1 1 d . . . H11 H 0.9651 0.3923 1.0967 0.061 Uiso 1 1 calc R . . C12 C 0.7698(8) 0.37387(17) 0.9959(3) 0.0349(12) Uani 1 1 d . . . C13 C 0.5730(9) 0.38431(19) 0.9459(3) 0.0451(14) Uani 1 1 d . . . H13 H 0.5289 0.3671 0.9003 0.054 Uiso 1 1 calc R . . C14 C 0.4420(10) 0.42060(19) 0.9644(4) 0.0499(15) Uani 1 1 d . . . H14 H 0.3112 0.4278 0.9303 0.060 Uiso 1 1 calc R . . C15 C 0.0802(8) 0.05343(18) 0.8913(3) 0.0410(13) Uani 1 1 d . . . H15 H 0.0258 0.0798 0.9119 0.049 Uiso 1 1 calc R . . C16 C 0.2864(9) -0.00361(19) 0.8721(3) 0.0498(15) Uani 1 1 d . . . H16 H 0.4036 -0.0245 0.8781 0.060 Uiso 1 1 calc R . . C17 C 0.1075(9) -0.0053(2) 0.8137(3) 0.0521(16) Uani 1 1 d . . . H17 H 0.0797 -0.0265 0.7728 0.062 Uiso 1 1 calc R . . C18 C -0.2473(9) 0.04014(18) 0.7815(4) 0.0485(15) Uani 1 1 d . . . H18A H -0.3614 0.0275 0.8094 0.058 Uiso 1 1 calc R . . H18B H -0.2584 0.0249 0.7305 0.058 Uiso 1 1 calc R . . C19 C -0.2911(9) 0.0903(2) 0.7681(3) 0.0423(14) Uani 1 1 d . . . C20 C -0.1454(9) 0.1171(2) 0.7343(3) 0.0544(16) Uani 1 1 d . . . H20 H -0.0162 0.1042 0.7205 0.065 Uiso 1 1 calc R . . C21 C -0.1873(9) 0.1630(2) 0.7205(3) 0.0540(16) Uani 1 1 d . . . H21 H -0.0843 0.1806 0.6985 0.065 Uiso 1 1 calc R . . C22 C -0.3793(8) 0.18336(19) 0.7389(3) 0.0436(14) Uani 1 1 d . . . C23 C -0.5263(9) 0.1559(2) 0.7736(3) 0.0524(15) Uani 1 1 d . . . H23 H -0.6554 0.1686 0.7881 0.063 Uiso 1 1 calc R . . C24 C -0.4811(9) 0.10997(19) 0.7867(3) 0.0475(14) Uani 1 1 d . . . H24 H -0.5829 0.0921 0.8087 0.057 Uiso 1 1 calc R . . C25 C -0.3101(9) 0.41734(19) 0.6071(3) 0.0475(14) Uani 1 1 d . . . H25 H -0.4191 0.4146 0.5624 0.057 Uiso 1 1 calc R . . C26 C -0.0088(10) 0.43469(18) 0.6850(3) 0.0491(15) Uani 1 1 d . . . H26 H 0.1320 0.4466 0.7041 0.059 Uiso 1 1 calc R . . C27 C -0.1409(9) 0.4121(2) 0.7295(3) 0.0484(16) Uani 1 1 d . . . H27 H -0.1088 0.4052 0.7833 0.058 Uiso 1 1 calc R . . C28 C -0.5278(10) 0.37687(19) 0.6959(3) 0.0532(16) Uani 1 1 d . . . H28A H -0.6520 0.3817 0.6533 0.064 Uiso 1 1 calc R . . H28B H -0.5703 0.3893 0.7442 0.064 Uiso 1 1 calc R . . C29 C -0.4892(9) 0.32661(19) 0.7065(3) 0.0446(14) Uani 1 1 d . . . C30 C -0.3564(12) 0.3031(2) 0.6639(4) 0.082(2) Uani 1 1 d . . . H30 H -0.2826 0.3186 0.6280 0.098 Uiso 1 1 calc R . . C31 C -0.3277(13) 0.2564(2) 0.6727(5) 0.088(2) Uani 1 1 d . . . H31 H -0.2400 0.2411 0.6409 0.106 Uiso 1 1 calc R . . C32 C -0.4239(9) 0.23237(19) 0.7264(3) 0.0449(14) Uani 1 1 d . . . C33 C -0.5647(11) 0.2564(2) 0.7683(4) 0.072(2) Uani 1 1 d . . . H33 H -0.6391 0.2408 0.8040 0.086 Uiso 1 1 calc R . . C34 C -0.5983(10) 0.3030(2) 0.7588(4) 0.0682(19) Uani 1 1 d . . . H34 H -0.6942 0.3182 0.7877 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0426(4) 0.0325(4) 0.0472(4) -0.0012(4) 0.0074(3) 0.0038(4) N1 0.041(3) 0.034(3) 0.043(3) -0.002(2) 0.007(2) 0.000(2) N2 0.040(3) 0.036(3) 0.050(3) -0.002(2) 0.006(2) 0.000(2) N3 0.045(3) 0.030(3) 0.048(3) 0.005(2) 0.010(2) 0.001(2) N4 0.043(3) 0.043(3) 0.046(3) -0.002(2) 0.004(2) 0.000(2) O1 0.050(2) 0.029(2) 0.059(2) -0.0010(19) 0.0083(19) 0.0040(19) O2 0.040(2) 0.043(2) 0.080(3) 0.004(2) 0.012(2) -0.0008(19) O3 0.052(2) 0.039(2) 0.065(3) 0.004(2) 0.007(2) 0.013(2) O4 0.074(3) 0.053(3) 0.056(3) -0.014(2) 0.006(2) 0.011(2) O5 0.084(3) 0.045(2) 0.054(2) 0.011(2) 0.030(2) 0.004(2) O6 0.036(2) 0.047(3) 0.077(3) -0.003(2) 0.002(2) 0.006(2) S1 0.0435(8) 0.0335(8) 0.0533(8) 0.0042(8) 0.0150(7) 0.0017(7) C1 0.046(3) 0.035(3) 0.040(3) 0.002(3) 0.011(3) 0.002(3) C2 0.040(3) 0.025(3) 0.040(3) 0.000(2) 0.005(3) -0.001(2) C3 0.049(3) 0.039(4) 0.068(4) -0.009(3) 0.023(3) 0.008(3) C4 0.041(3) 0.042(4) 0.071(4) -0.004(3) 0.028(3) -0.001(3) C5 0.042(3) 0.031(3) 0.049(3) -0.001(3) 0.012(3) 0.002(3) C6 0.052(4) 0.029(3) 0.074(4) -0.004(3) 0.027(3) 0.002(3) C7 0.050(3) 0.034(3) 0.076(4) 0.000(4) 0.031(3) 0.000(3) C8 0.041(3) 0.030(3) 0.061(4) 0.008(3) 0.011(3) -0.001(3) C9 0.040(3) 0.025(3) 0.039(3) 0.002(3) 0.006(3) 0.002(3) C10 0.056(3) 0.050(4) 0.042(3) -0.009(3) 0.000(3) 0.004(3) C11 0.046(3) 0.049(4) 0.056(4) -0.002(3) 0.000(3) 0.016(3) C12 0.041(3) 0.027(3) 0.037(3) 0.002(3) 0.007(2) 0.002(2) C13 0.052(3) 0.036(3) 0.046(3) -0.004(3) 0.003(3) 0.004(3) C14 0.045(3) 0.046(4) 0.054(3) 0.007(3) -0.008(3) 0.008(3) C15 0.040(3) 0.037(3) 0.047(3) -0.003(3) 0.011(3) -0.002(3) C16 0.055(4) 0.037(3) 0.058(4) -0.003(3) 0.008(3) 0.008(3) C17 0.053(4) 0.040(4) 0.060(4) -0.015(3) 0.001(3) 0.008(3) C18 0.042(3) 0.038(3) 0.062(4) -0.001(3) -0.002(3) -0.004(3) C19 0.044(3) 0.041(4) 0.040(3) 0.003(3) 0.002(3) -0.001(3) C20 0.046(3) 0.056(4) 0.061(4) 0.006(3) 0.009(3) 0.007(3) C21 0.044(3) 0.054(4) 0.067(4) 0.015(3) 0.015(3) -0.001(3) C22 0.036(3) 0.036(3) 0.059(4) 0.001(3) 0.009(3) 0.000(3) C23 0.048(3) 0.051(4) 0.060(4) 0.007(3) 0.014(3) 0.005(3) C24 0.041(3) 0.043(4) 0.060(4) 0.005(3) 0.015(3) -0.005(3) C25 0.050(4) 0.049(4) 0.043(3) 0.007(3) 0.005(3) 0.000(3) C26 0.053(3) 0.034(4) 0.057(4) -0.009(3) -0.002(3) -0.001(3) C27 0.056(4) 0.055(4) 0.034(3) -0.001(3) 0.008(3) -0.001(3) C28 0.063(4) 0.041(4) 0.059(4) 0.007(3) 0.021(3) -0.001(3) C29 0.055(3) 0.039(3) 0.042(3) 0.005(3) 0.013(3) 0.007(3) C30 0.121(6) 0.049(4) 0.093(5) 0.014(4) 0.075(5) 0.004(4) C31 0.122(6) 0.049(4) 0.113(6) 0.005(4) 0.079(5) 0.023(4) C32 0.049(3) 0.040(4) 0.048(3) 0.004(3) 0.016(3) -0.005(3) C33 0.078(4) 0.048(4) 0.100(5) 0.023(4) 0.046(4) 0.000(4) C34 0.070(4) 0.048(4) 0.096(5) 0.013(4) 0.044(4) 0.007(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 O3 1.972(4) 3_545 ? Co1 O1 1.997(4) . ? Co1 N4 2.014(5) 4 ? Co1 N1 2.016(4) . ? N1 C15 1.335(6) . ? N1 C16 1.377(7) . ? N2 C15 1.337(6) . ? N2 C17 1.373(6) . ? N2 C18 1.475(6) . ? N3 C25 1.316(6) . ? N3 C27 1.383(6) . ? N3 C28 1.452(7) . ? N4 C25 1.324(6) . ? N4 C26 1.389(6) . ? N4 Co1 2.014(4) 4_454 ? O1 C1 1.287(6) . ? O2 C1 1.256(6) . ? O3 C8 1.287(6) . ? O3 Co1 1.972(4) 3_455 ? O4 C8 1.213(6) . ? O5 S1 1.440(4) . ? O6 S1 1.443(3) . ? S1 C12 1.769(5) . ? S1 C5 1.775(6) . ? C1 C2 1.483(7) . ? C2 C7 1.384(7) . ? C2 C3 1.391(7) . ? C3 C4 1.396(7) . ? C3 H3 0.9300 . ? C4 C5 1.384(7) . ? C4 H4 0.9300 . ? C5 C6 1.365(7) . ? C6 C7 1.388(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.526(7) . ? C9 C14 1.381(7) . ? C9 C10 1.385(7) . ? C10 C11 1.389(7) . ? C10 H10 0.9300 . ? C11 C12 1.369(7) . ? C11 H11 0.9300 . ? C12 C13 1.385(6) . ? C13 C14 1.390(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.351(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.504(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.365(7) . ? C19 C20 1.371(8) . ? C20 C21 1.383(7) . ? C20 H20 0.9300 . ? C21 C22 1.382(7) . ? C21 H21 0.9300 . ? C22 C23 1.395(7) . ? C22 C32 1.471(7) . ? C23 C24 1.385(7) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.355(7) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.498(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.351(8) . ? C29 C34 1.374(8) . ? C30 C31 1.384(9) . ? C30 H30 0.9300 . ? C31 C32 1.354(8) . ? C31 H31 0.9300 . ? C32 C33 1.385(8) . ? C33 C34 1.386(8) . ? C33 H33 0.9300 . ? C34 H34 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 O3 Co1 O1 105.87(16) 3_545 . ? O3 Co1 N4 120.95(17) 3_545 4 ? O1 Co1 N4 108.49(16) . 4 ? O3 Co1 N1 94.61(17) 3_545 . ? O1 Co1 N1 120.18(16) . . ? N4 Co1 N1 107.11(18) 4 . ? C15 N1 C16 104.2(4) . . ? C15 N1 Co1 131.0(4) . . ? C16 N1 Co1 124.2(4) . . ? C15 N2 C17 107.9(4) . . ? C15 N2 C18 128.5(4) . . ? C17 N2 C18 123.5(4) . . ? C25 N3 C27 107.9(5) . . ? C25 N3 C28 125.1(5) . . ? C27 N3 C28 127.0(5) . . ? C25 N4 C26 104.2(5) . . ? C25 N4 Co1 123.0(4) . 4_454 ? C26 N4 Co1 129.2(4) . 4_454 ? C1 O1 Co1 106.5(3) . . ? C8 O3 Co1 121.3(4) . 3_455 ? O5 S1 O6 118.2(3) . . ? O5 S1 C12 107.4(2) . . ? O6 S1 C12 108.1(2) . . ? O5 S1 C5 107.6(2) . . ? O6 S1 C5 107.1(2) . . ? C12 S1 C5 108.0(3) . . ? O2 C1 O1 121.3(5) . . ? O2 C1 C2 119.4(5) . . ? O1 C1 C2 119.3(5) . . ? C7 C2 C3 118.3(5) . . ? C7 C2 C1 120.5(5) . . ? C3 C2 C1 121.2(5) . . ? C2 C3 C4 120.0(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.4(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.8(5) . . ? C6 C5 S1 124.6(4) . . ? C4 C5 S1 115.5(4) . . ? C5 C6 C7 119.9(5) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C2 C7 C6 121.5(5) . . ? C2 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? O4 C8 O3 125.2(5) . . ? O4 C8 C9 120.5(5) . . ? O3 C8 C9 114.3(5) . . ? C14 C9 C10 118.4(5) . . ? C14 C9 C8 121.7(5) . . ? C10 C9 C8 119.9(5) . . ? C9 C10 C11 120.7(5) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 120.4(5) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.8(5) . . ? C11 C12 S1 119.7(4) . . ? C13 C12 S1 120.2(4) . . ? C12 C13 C14 119.6(5) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C9 C14 C13 121.1(5) . . ? C9 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? N1 C15 N2 111.6(5) . . ? N1 C15 H15 124.2 . . ? N2 C15 H15 124.2 . . ? C17 C16 N1 111.1(5) . . ? C17 C16 H16 124.4 . . ? N1 C16 H16 124.4 . . ? C16 C17 N2 105.2(5) . . ? C16 C17 H17 127.4 . . ? N2 C17 H17 127.4 . . ? N2 C18 C19 112.4(4) . . ? N2 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? N2 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C24 C19 C20 118.2(6) . . ? C24 C19 C18 120.8(5) . . ? C20 C19 C18 121.0(5) . . ? C19 C20 C21 121.1(6) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 121.2(6) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 117.3(5) . . ? C21 C22 C32 121.9(5) . . ? C23 C22 C32 120.6(5) . . ? C24 C23 C22 120.4(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C19 C24 C23 121.7(6) . . ? C19 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? N3 C25 N4 112.6(5) . . ? N3 C25 H25 123.7 . . ? N4 C25 H25 123.7 . . ? C27 C26 N4 110.2(5) . . ? C27 C26 H26 124.9 . . ? N4 C26 H26 124.9 . . ? C26 C27 N3 105.1(5) . . ? C26 C27 H27 127.4 . . ? N3 C27 H27 127.4 . . ? N3 C28 C29 113.7(5) . . ? N3 C28 H28A 108.8 . . ? C29 C28 H28A 108.8 . . ? N3 C28 H28B 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C30 C29 C34 118.4(6) . . ? C30 C29 C28 122.1(6) . . ? C34 C29 C28 119.5(5) . . ? C29 C30 C31 121.4(6) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C32 C31 C30 121.8(6) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C31 C32 C33 116.5(6) . . ? C31 C32 C22 121.2(6) . . ? C33 C32 C22 122.3(5) . . ? C32 C33 C34 122.1(6) . . ? C32 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? C29 C34 C33 119.7(6) . . ? C29 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? 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 O3 Co1 N1 C15 -176.6(4) 3_545 . . . ? O1 Co1 N1 C15 -65.2(5) . . . . ? N4 Co1 N1 C15 59.0(5) 4 . . . ? O3 Co1 N1 C16 -7.3(4) 3_545 . . . ? O1 Co1 N1 C16 104.0(4) . . . . ? N4 Co1 N1 C16 -131.7(4) 4 . . . ? O3 Co1 O1 C1 168.3(3) 3_545 . . . ? N4 Co1 O1 C1 -60.5(4) 4 . . . ? N1 Co1 O1 C1 63.1(4) . . . . ? Co1 O1 C1 O2 -6.3(6) . . . . ? Co1 O1 C1 C2 173.0(4) . . . . ? O2 C1 C2 C7 27.4(8) . . . . ? O1 C1 C2 C7 -151.9(5) . . . . ? O2 C1 C2 C3 -151.0(5) . . . . ? O1 C1 C2 C3 29.8(8) . . . . ? C7 C2 C3 C4 -0.6(8) . . . . ? C1 C2 C3 C4 177.8(5) . . . . ? C2 C3 C4 C5 2.8(8) . . . . ? C3 C4 C5 C6 -1.7(8) . . . . ? C3 C4 C5 S1 175.6(4) . . . . ? O5 S1 C5 C6 -125.7(5) . . . . ? O6 S1 C5 C6 106.2(5) . . . . ? C12 S1 C5 C6 -10.1(5) . . . . ? O5 S1 C5 C4 57.1(5) . . . . ? O6 S1 C5 C4 -71.0(5) . . . . ? C12 S1 C5 C4 172.7(4) . . . . ? C4 C5 C6 C7 -1.5(8) . . . . ? S1 C5 C6 C7 -178.6(4) . . . . ? C3 C2 C7 C6 -2.7(9) . . . . ? C1 C2 C7 C6 178.9(5) . . . . ? C5 C6 C7 C2 3.8(9) . . . . ? Co1 O3 C8 O4 1.6(7) 3_455 . . . ? Co1 O3 C8 C9 -177.2(3) 3_455 . . . ? O4 C8 C9 C14 166.7(5) . . . . ? O3 C8 C9 C14 -14.5(7) . . . . ? O4 C8 C9 C10 -14.6(8) . . . . ? O3 C8 C9 C10 164.3(5) . . . . ? C14 C9 C10 C11 -0.1(8) . . . . ? C8 C9 C10 C11 -178.9(5) . . . . ? C9 C10 C11 C12 -0.5(9) . . . . ? C10 C11 C12 C13 0.3(8) . . . . ? C10 C11 C12 S1 173.6(5) . . . . ? O5 S1 C12 C11 -128.0(4) . . . . ? O6 S1 C12 C11 0.6(5) . . . . ? C5 S1 C12 C11 116.2(5) . . . . ? O5 S1 C12 C13 45.3(5) . . . . ? O6 S1 C12 C13 173.9(4) . . . . ? C5 S1 C12 C13 -70.5(5) . . . . ? C11 C12 C13 C14 0.4(8) . . . . ? S1 C12 C13 C14 -172.9(4) . . . . ? C10 C9 C14 C13 0.8(8) . . . . ? C8 C9 C14 C13 179.6(5) . . . . ? C12 C13 C14 C9 -1.0(9) . . . . ? C16 N1 C15 N2 0.9(6) . . . . ? Co1 N1 C15 N2 171.8(3) . . . . ? C17 N2 C15 N1 -1.6(6) . . . . ? C18 N2 C15 N1 174.8(5) . . . . ? C15 N1 C16 C17 0.1(6) . . . . ? Co1 N1 C16 C17 -171.5(4) . . . . ? N1 C16 C17 N2 -1.1(6) . . . . ? C15 N2 C17 C16 1.6(6) . . . . ? C18 N2 C17 C16 -175.0(5) . . . . ? C15 N2 C18 C19 41.4(7) . . . . ? C17 N2 C18 C19 -142.8(6) . . . . ? N2 C18 C19 C24 -127.8(5) . . . . ? N2 C18 C19 C20 54.5(7) . . . . ? C24 C19 C20 C21 1.0(9) . . . . ? C18 C19 C20 C21 178.8(5) . . . . ? C19 C20 C21 C22 -1.2(9) . . . . ? C20 C21 C22 C23 1.5(9) . . . . ? C20 C21 C22 C32 178.5(5) . . . . ? C21 C22 C23 C24 -1.7(8) . . . . ? C32 C22 C23 C24 -178.8(5) . . . . ? C20 C19 C24 C23 -1.2(8) . . . . ? C18 C19 C24 C23 -179.0(5) . . . . ? C22 C23 C24 C19 1.6(9) . . . . ? C27 N3 C25 N4 0.5(6) . . . . ? C28 N3 C25 N4 -178.3(5) . . . . ? C26 N4 C25 N3 -1.2(6) . . . . ? Co1 N4 C25 N3 159.2(4) 4_454 . . . ? C25 N4 C26 C27 1.5(6) . . . . ? Co1 N4 C26 C27 -157.2(4) 4_454 . . . ? N4 C26 C27 N3 -1.2(6) . . . . ? C25 N3 C27 C26 0.4(6) . . . . ? C28 N3 C27 C26 179.2(5) . . . . ? C25 N3 C28 C29 104.5(6) . . . . ? C27 N3 C28 C29 -74.1(7) . . . . ? N3 C28 C29 C30 -34.6(8) . . . . ? N3 C28 C29 C34 148.0(5) . . . . ? C34 C29 C30 C31 -0.6(11) . . . . ? C28 C29 C30 C31 -178.0(7) . . . . ? C29 C30 C31 C32 -2.6(13) . . . . ? C30 C31 C32 C33 4.2(11) . . . . ? C30 C31 C32 C22 -175.7(7) . . . . ? C21 C22 C32 C31 23.5(9) . . . . ? C23 C22 C32 C31 -159.5(6) . . . . ? C21 C22 C32 C33 -156.4(6) . . . . ? C23 C22 C32 C33 20.6(8) . . . . ? C31 C32 C33 C34 -2.9(10) . . . . ? C22 C32 C33 C34 177.0(6) . . . . ? C30 C29 C34 C33 1.9(10) . . . . ? C28 C29 C34 C33 179.4(6) . . . . ? C32 C33 C34 C29 -0.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.264 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.053 #========END data_K5 _database_code_depnum_ccdc_archive 'CCDC 730712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 Co N4 O6 S' _chemical_formula_sum 'C28 H22 Co N4 O6 S' _chemical_formula_weight 601.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.7329(2) _cell_length_b 11.2712(3) _cell_length_c 27.1832(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2675.65(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2933 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 21.18 _exptl_crystal_description pillar _exptl_crystal_colour purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8367 _exptl_absorpt_correction_T_max 0.9133 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 10926 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4506 _reflns_number_gt 3730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998' _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^)+(0.0408P)^2^+0.9312P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 4506 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Co1 Co 0.56714(6) 0.50343(5) 0.131536(18) 0.03368(16) Uani 1 1 d . . . N1 N 0.7119(4) 0.3703(3) 0.11768(13) 0.0419(10) Uani 1 1 d . . . N2 N 0.8056(5) 0.1898(3) 0.12365(15) 0.0504(11) Uani 1 1 d . . . N3 N 0.8816(4) -0.2190(3) 0.13431(16) 0.0432(10) Uani 1 1 d . . . N4 N 0.7030(4) -0.3516(3) 0.12091(13) 0.0374(9) Uani 1 1 d . . . O1 O 0.4015(4) 0.5367(3) 0.08676(12) 0.0520(9) Uani 1 1 d . . . O2 O 0.3572(4) 0.3427(3) 0.08728(13) 0.0634(10) Uani 1 1 d . . . O3 O -0.0537(3) 0.4771(3) -0.29773(10) 0.0458(8) Uani 1 1 d . . . O4 O 0.0168(4) 0.6647(3) -0.28687(11) 0.0575(10) Uani 1 1 d . . . O5 O -0.2786(4) 0.6358(3) -0.04581(10) 0.0426(8) Uani 1 1 d . . . O6 O -0.3132(3) 0.4202(3) -0.05502(11) 0.0437(8) Uani 1 1 d . . . S1 S -0.21600(12) 0.52243(10) -0.05877(4) 0.0337(3) Uani 1 1 d . . . C1 C 0.3298(5) 0.4436(5) 0.07266(17) 0.0437(12) Uani 1 1 d . . . C2 C 0.2013(5) 0.4633(4) 0.03584(14) 0.0355(11) Uani 1 1 d . . . C3 C 0.1321(5) 0.3678(4) 0.01267(15) 0.0359(11) Uani 1 1 d . . . H3 H 0.1711 0.2917 0.0170 0.043 Uiso 1 1 calc R . . C4 C 0.0061(5) 0.3852(4) -0.01663(15) 0.0350(11) Uani 1 1 d . . . H4 H -0.0415 0.3212 -0.0319 0.042 Uiso 1 1 calc R . . C5 C -0.0490(4) 0.4987(4) -0.02316(12) 0.0303(8) Uani 1 1 d . . . C6 C 0.0212(5) 0.5949(4) -0.00178(16) 0.0392(12) Uani 1 1 d . . . H6 H -0.0159 0.6711 -0.0073 0.047 Uiso 1 1 calc R . . C7 C 0.1472(5) 0.5773(4) 0.02793(17) 0.0400(12) Uani 1 1 d . . . H7 H 0.1956 0.6417 0.0426 0.048 Uiso 1 1 calc R . . C8 C -0.0285(5) 0.5690(4) -0.27136(15) 0.0402(11) Uani 1 1 d . . . C9 C -0.0647(5) 0.5529(4) -0.21770(15) 0.0362(10) Uani 1 1 d . . . C10 C -0.1136(5) 0.4431(4) -0.19913(16) 0.0399(12) Uani 1 1 d . . . H10 H -0.1173 0.3769 -0.2195 0.048 Uiso 1 1 calc R . . C11 C -0.1567(5) 0.4341(4) -0.14990(15) 0.0370(11) Uani 1 1 d . . . H11 H -0.1893 0.3618 -0.1373 0.044 Uiso 1 1 calc R . . C12 C -0.1506(4) 0.5332(4) -0.11988(13) 0.0304(10) Uani 1 1 d . . . C13 C -0.0987(5) 0.6415(4) -0.13672(15) 0.0356(10) Uani 1 1 d . . . H13 H -0.0925 0.7066 -0.1158 0.043 Uiso 1 1 calc R . . C14 C -0.0560(5) 0.6504(4) -0.18589(15) 0.0372(10) Uani 1 1 d . . . H14 H -0.0208 0.7227 -0.1979 0.045 Uiso 1 1 calc R . . C15 C 0.8668(6) 0.3757(5) 0.10902(18) 0.0535(14) Uani 1 1 d . . . H15 H 0.9225 0.4440 0.1020 0.064 Uiso 1 1 calc R . . C16 C 0.9249(7) 0.2633(5) 0.11260(19) 0.0634(15) Uani 1 1 d . . . H16 H 1.0267 0.2412 0.1083 0.076 Uiso 1 1 calc R . . C17 C 0.6814(5) 0.2576(4) 0.12692(19) 0.0488(12) Uani 1 1 d . . . H17 H 0.5845 0.2292 0.1348 0.059 Uiso 1 1 calc R . . C18 C 0.8151(7) 0.0630(4) 0.1337(2) 0.0627(15) Uani 1 1 d . . . H18A H 0.8955 0.0287 0.1136 0.075 Uiso 1 1 calc R . . H18B H 0.7193 0.0258 0.1244 0.075 Uiso 1 1 calc R . . C19 C 0.8475(5) 0.0363(4) 0.18698(19) 0.0451(12) Uani 1 1 d . . . C20 C 0.7890(6) 0.1086(4) 0.22384(19) 0.0553(14) Uani 1 1 d . . . H20 H 0.7363 0.1778 0.2161 0.066 Uiso 1 1 calc R . . C21 C 0.8107(7) 0.0753(6) 0.2722(2) 0.0672(16) Uani 1 1 d . . . H21 H 0.7693 0.1226 0.2969 0.081 Uiso 1 1 calc R . . C22 C 0.8897(7) -0.0234(6) 0.2853(2) 0.0761(18) Uani 1 1 d . . . H22 H 0.9028 -0.0426 0.3183 0.091 Uiso 1 1 calc R . . C23 C 0.9479(7) -0.0921(5) 0.2505(2) 0.0712(18) Uani 1 1 d . . . H23 H 1.0023 -0.1596 0.2595 0.085 Uiso 1 1 calc R . . C24 C 0.9297(5) -0.0659(4) 0.2000(2) 0.0504(13) Uani 1 1 d . . . C25 C 0.9968(5) -0.1464(4) 0.1603(2) 0.0610(16) Uani 1 1 d . . . H25A H 1.0503 -0.0978 0.1364 0.073 Uiso 1 1 calc R . . H25B H 1.0713 -0.1989 0.1753 0.073 Uiso 1 1 calc R . . C26 C 0.7908(5) -0.3020(4) 0.15421(17) 0.0437(12) Uani 1 1 d . . . H26 H 0.7902 -0.3219 0.1874 0.052 Uiso 1 1 calc R . . C27 C 0.7416(6) -0.2978(4) 0.07799(17) 0.0528(14) Uani 1 1 d . . . H27 H 0.6983 -0.3148 0.0475 0.063 Uiso 1 1 calc R . . C28 C 0.8512(7) -0.2166(4) 0.08580(19) 0.0585(15) Uani 1 1 d . . . H28 H 0.8971 -0.1682 0.0623 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0338(3) 0.0339(3) 0.0334(3) -0.0002(3) -0.0053(2) 0.0012(3) N1 0.038(2) 0.040(3) 0.048(3) -0.0011(18) -0.0020(19) 0.003(2) N2 0.053(3) 0.036(2) 0.062(3) 0.000(2) 0.002(2) 0.011(2) N3 0.034(2) 0.027(2) 0.069(3) -0.005(2) 0.012(2) 0.0002(16) N4 0.038(2) 0.034(2) 0.039(2) 0.0030(18) -0.0014(18) 0.0016(19) O1 0.051(2) 0.045(2) 0.061(2) -0.0085(16) -0.0228(17) 0.0025(17) O2 0.064(2) 0.052(2) 0.074(2) 0.014(2) -0.031(2) 0.007(2) O3 0.0612(19) 0.045(2) 0.0314(15) -0.0043(15) 0.0045(15) 0.0013(18) O4 0.083(3) 0.048(2) 0.0420(19) 0.0026(16) 0.0073(17) -0.013(2) O5 0.0447(18) 0.0413(19) 0.0419(18) -0.0058(14) -0.0028(15) 0.0148(17) O6 0.0345(17) 0.049(2) 0.0475(18) 0.0048(16) -0.0039(15) -0.0103(15) S1 0.0310(5) 0.0390(7) 0.0312(5) -0.0005(5) -0.0039(4) 0.0024(5) C1 0.038(3) 0.051(3) 0.042(3) 0.002(2) -0.008(2) 0.008(3) C2 0.035(2) 0.041(3) 0.031(2) 0.0063(19) -0.0051(19) -0.002(2) C3 0.045(3) 0.026(3) 0.037(3) -0.005(2) -0.007(2) 0.007(2) C4 0.044(3) 0.034(3) 0.028(2) -0.0020(19) -0.009(2) -0.003(2) C5 0.035(2) 0.030(2) 0.0260(18) 0.001(2) -0.0038(16) 0.001(2) C6 0.043(3) 0.031(3) 0.044(3) 0.005(2) -0.010(2) 0.002(2) C7 0.046(3) 0.026(3) 0.049(3) 0.001(2) -0.010(2) -0.001(2) C8 0.046(3) 0.045(3) 0.030(2) -0.001(2) -0.002(2) 0.002(2) C9 0.038(2) 0.038(3) 0.033(2) -0.0049(19) -0.007(2) 0.003(2) C10 0.050(3) 0.031(3) 0.038(3) -0.004(2) -0.004(2) 0.005(2) C11 0.044(3) 0.032(3) 0.036(3) 0.008(2) -0.003(2) 0.002(2) C12 0.032(2) 0.033(3) 0.026(2) 0.0007(17) -0.0089(17) 0.0026(18) C13 0.035(2) 0.037(3) 0.034(2) -0.003(2) -0.005(2) -0.003(2) C14 0.039(2) 0.029(3) 0.043(3) 0.004(2) -0.005(2) -0.004(2) C15 0.043(3) 0.054(4) 0.063(3) 0.016(3) 0.014(3) 0.004(3) C16 0.048(3) 0.061(4) 0.082(4) 0.012(3) 0.022(3) 0.022(3) C17 0.039(3) 0.036(3) 0.071(4) 0.000(3) -0.002(3) 0.001(2) C18 0.085(4) 0.034(3) 0.069(4) -0.007(3) 0.000(3) 0.019(3) C19 0.041(3) 0.029(3) 0.065(3) 0.000(2) -0.003(2) -0.006(2) C20 0.058(3) 0.044(3) 0.064(4) -0.012(3) -0.009(3) 0.001(3) C21 0.068(4) 0.068(4) 0.066(4) -0.017(3) 0.000(3) -0.015(4) C22 0.101(5) 0.063(4) 0.065(4) 0.002(3) -0.025(3) -0.007(4) C23 0.075(4) 0.052(4) 0.087(5) 0.012(3) -0.032(4) -0.003(3) C24 0.035(3) 0.031(3) 0.085(4) -0.006(3) -0.012(3) -0.008(2) C25 0.031(2) 0.035(3) 0.116(5) -0.002(3) -0.004(3) -0.001(2) C26 0.041(3) 0.038(3) 0.052(3) 0.008(2) 0.001(2) -0.004(2) C27 0.075(4) 0.046(3) 0.037(3) 0.000(2) 0.004(3) -0.001(3) C28 0.090(4) 0.041(3) 0.044(3) 0.007(2) 0.027(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.927(3) . ? Co1 O3 1.939(3) 2_565 ? Co1 N1 1.998(4) . ? Co1 N4 2.040(4) 1_565 ? N1 C17 1.322(5) . ? N1 C15 1.374(6) . ? N2 C17 1.331(5) . ? N2 C16 1.365(6) . ? N2 C18 1.457(6) . ? N3 C26 1.341(5) . ? N3 C28 1.345(6) . ? N3 C25 1.476(5) . ? N4 C26 1.311(5) . ? N4 C27 1.358(5) . ? N4 Co1 2.040(4) 1_545 ? O1 C1 1.280(5) . ? O2 C1 1.228(5) . ? O3 C8 1.279(5) . ? O3 Co1 1.939(3) 2_564 ? O4 C8 1.225(5) . ? O5 S1 1.434(3) . ? O6 S1 1.435(3) . ? S1 C12 1.761(4) . ? S1 C5 1.771(4) . ? C1 C2 1.519(6) . ? C2 C7 1.386(6) . ? C2 C3 1.387(5) . ? C3 C4 1.373(6) . ? C3 H3 0.9300 . ? C4 C5 1.378(5) . ? C4 H4 0.9300 . ? C5 C6 1.375(5) . ? C6 C7 1.379(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.503(6) . ? C9 C14 1.401(5) . ? C9 C10 1.402(6) . ? C10 C11 1.394(6) . ? C10 H10 0.9300 . ? C11 C12 1.384(5) . ? C11 H11 0.9300 . ? C12 C13 1.380(5) . ? C13 C14 1.391(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.368(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.506(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.389(7) . ? C19 C24 1.403(6) . ? C20 C21 1.380(8) . ? C20 H20 0.9300 . ? C21 C22 1.357(8) . ? C21 H21 0.9300 . ? C22 C23 1.324(8) . ? C22 H22 0.9300 . ? C23 C24 1.412(7) . ? C23 H23 0.9300 . ? C24 C25 1.528(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26 0.9300 . ? C27 C28 1.341(7) . ? C27 H27 0.9300 . ? C28 H28 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 O1 Co1 O3 123.98(14) . 2_565 ? O1 Co1 N1 120.13(14) . . ? O3 Co1 N1 108.08(13) 2_565 . ? O1 Co1 N4 101.04(14) . 1_565 ? O3 Co1 N4 94.85(13) 2_565 1_565 ? N1 Co1 N4 101.95(14) . 1_565 ? C17 N1 C15 105.9(4) . . ? C17 N1 Co1 123.9(3) . . ? C15 N1 Co1 128.4(3) . . ? C17 N2 C16 106.7(4) . . ? C17 N2 C18 126.7(5) . . ? C16 N2 C18 126.4(5) . . ? C26 N3 C28 107.0(4) . . ? C26 N3 C25 126.6(4) . . ? C28 N3 C25 126.3(4) . . ? C26 N4 C27 104.9(4) . . ? C26 N4 Co1 125.7(3) . 1_545 ? C27 N4 Co1 128.6(3) . 1_545 ? C1 O1 Co1 113.4(3) . . ? C8 O3 Co1 118.3(3) . 2_564 ? O5 S1 O6 118.19(18) . . ? O5 S1 C12 107.09(19) . . ? O6 S1 C12 108.33(19) . . ? O5 S1 C5 108.34(19) . . ? O6 S1 C5 109.08(19) . . ? C12 S1 C5 105.03(17) . . ? O2 C1 O1 124.5(4) . . ? O2 C1 C2 119.5(4) . . ? O1 C1 C2 116.0(4) . . ? C7 C2 C3 120.1(4) . . ? C7 C2 C1 119.3(4) . . ? C3 C2 C1 120.5(4) . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 121.5(4) . . ? C6 C5 S1 118.6(3) . . ? C4 C5 S1 119.9(3) . . ? C5 C6 C7 119.3(4) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C7 C2 119.8(4) . . ? C6 C7 H7 120.1 . . ? C2 C7 H7 120.1 . . ? O4 C8 O3 125.2(4) . . ? O4 C8 C9 120.6(4) . . ? O3 C8 C9 114.2(4) . . ? C14 C9 C10 119.1(4) . . ? C14 C9 C8 119.5(4) . . ? C10 C9 C8 121.3(4) . . ? C11 C10 C9 119.5(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 119.8(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 122.0(4) . . ? C13 C12 S1 118.7(3) . . ? C11 C12 S1 119.2(3) . . ? C12 C13 C14 118.1(4) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? C13 C14 C9 121.4(4) . . ? C13 C14 H14 119.3 . . ? C9 C14 H14 119.3 . . ? C16 C15 N1 108.2(5) . . ? C16 C15 H15 125.9 . . ? N1 C15 H15 125.9 . . ? N2 C16 C15 107.1(4) . . ? N2 C16 H16 126.4 . . ? C15 C16 H16 126.4 . . ? N1 C17 N2 112.0(4) . . ? N1 C17 H17 124.0 . . ? N2 C17 H17 124.0 . . ? N2 C18 C19 112.8(4) . . ? N2 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? N2 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C24 119.2(5) . . ? C20 C19 C18 120.5(4) . . ? C24 C19 C18 120.2(4) . . ? C21 C20 C19 118.5(5) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C22 C21 C20 122.8(6) . . ? C22 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? C23 C22 C21 119.2(6) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 121.9(6) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C19 C24 C23 118.3(5) . . ? C19 C24 C25 120.4(5) . . ? C23 C24 C25 121.3(5) . . ? N3 C25 C24 113.9(4) . . ? N3 C25 H25A 108.8 . . ? C24 C25 H25A 108.8 . . ? N3 C25 H25B 108.8 . . ? C24 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N4 C26 N3 111.4(4) . . ? N4 C26 H26 124.3 . . ? N3 C26 H26 124.3 . . ? C28 C27 N4 110.2(4) . . ? C28 C27 H27 124.9 . . ? N4 C27 H27 124.9 . . ? C27 C28 N3 106.4(4) . . ? C27 C28 H28 126.8 . . ? N3 C28 H28 126.8 . . ? 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 O1 Co1 N1 C17 -80.0(4) . . . . ? O3 Co1 N1 C17 70.4(4) 2_565 . . . ? N4 Co1 N1 C17 169.6(4) 1_565 . . . ? O1 Co1 N1 C15 117.2(4) . . . . ? O3 Co1 N1 C15 -92.4(4) 2_565 . . . ? N4 Co1 N1 C15 6.8(4) 1_565 . . . ? O3 Co1 O1 C1 -100.5(3) 2_565 . . . ? N1 Co1 O1 C1 45.0(4) . . . . ? N4 Co1 O1 C1 155.9(3) 1_565 . . . ? Co1 O1 C1 O2 3.0(6) . . . . ? Co1 O1 C1 C2 -177.9(3) . . . . ? O2 C1 C2 C7 165.3(4) . . . . ? O1 C1 C2 C7 -13.9(6) . . . . ? O2 C1 C2 C3 -10.6(6) . . . . ? O1 C1 C2 C3 170.2(4) . . . . ? C7 C2 C3 C4 -2.6(6) . . . . ? C1 C2 C3 C4 173.3(4) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C3 C4 C5 C6 1.3(6) . . . . ? C3 C4 C5 S1 -177.4(3) . . . . ? O5 S1 C5 C6 -19.1(4) . . . . ? O6 S1 C5 C6 -148.9(3) . . . . ? C12 S1 C5 C6 95.1(3) . . . . ? O5 S1 C5 C4 159.7(3) . . . . ? O6 S1 C5 C4 29.8(4) . . . . ? C12 S1 C5 C4 -86.1(3) . . . . ? C4 C5 C6 C7 -1.7(6) . . . . ? S1 C5 C6 C7 177.0(3) . . . . ? C5 C6 C7 C2 0.0(7) . . . . ? C3 C2 C7 C6 2.1(6) . . . . ? C1 C2 C7 C6 -173.8(4) . . . . ? Co1 O3 C8 O4 -14.7(6) 2_564 . . . ? Co1 O3 C8 C9 163.2(3) 2_564 . . . ? O4 C8 C9 C14 4.2(7) . . . . ? O3 C8 C9 C14 -173.9(4) . . . . ? O4 C8 C9 C10 -178.6(4) . . . . ? O3 C8 C9 C10 3.3(6) . . . . ? C14 C9 C10 C11 1.9(7) . . . . ? C8 C9 C10 C11 -175.4(4) . . . . ? C9 C10 C11 C12 -0.1(7) . . . . ? C10 C11 C12 C13 -1.9(6) . . . . ? C10 C11 C12 S1 176.3(3) . . . . ? O5 S1 C12 C13 30.5(4) . . . . ? O6 S1 C12 C13 159.0(3) . . . . ? C5 S1 C12 C13 -84.6(3) . . . . ? O5 S1 C12 C11 -147.8(3) . . . . ? O6 S1 C12 C11 -19.3(4) . . . . ? C5 S1 C12 C11 97.1(3) . . . . ? C11 C12 C13 C14 2.0(6) . . . . ? S1 C12 C13 C14 -176.3(3) . . . . ? C12 C13 C14 C9 -0.1(6) . . . . ? C10 C9 C14 C13 -1.8(7) . . . . ? C8 C9 C14 C13 175.5(4) . . . . ? C17 N1 C15 C16 1.0(6) . . . . ? Co1 N1 C15 C16 166.3(3) . . . . ? C17 N2 C16 C15 -0.6(6) . . . . ? C18 N2 C16 C15 -176.2(5) . . . . ? N1 C15 C16 N2 -0.3(6) . . . . ? C15 N1 C17 N2 -1.5(6) . . . . ? Co1 N1 C17 N2 -167.5(3) . . . . ? C16 N2 C17 N1 1.3(6) . . . . ? C18 N2 C17 N1 176.9(4) . . . . ? C17 N2 C18 C19 -87.8(6) . . . . ? C16 N2 C18 C19 86.9(6) . . . . ? N2 C18 C19 C20 34.2(7) . . . . ? N2 C18 C19 C24 -149.6(4) . . . . ? C24 C19 C20 C21 -1.6(7) . . . . ? C18 C19 C20 C21 174.6(5) . . . . ? C19 C20 C21 C22 1.6(8) . . . . ? C20 C21 C22 C23 -0.6(9) . . . . ? C21 C22 C23 C24 -0.3(9) . . . . ? C20 C19 C24 C23 0.8(7) . . . . ? C18 C19 C24 C23 -175.5(5) . . . . ? C20 C19 C24 C25 -179.4(4) . . . . ? C18 C19 C24 C25 4.3(6) . . . . ? C22 C23 C24 C19 0.1(8) . . . . ? C22 C23 C24 C25 -179.6(5) . . . . ? C26 N3 C25 C24 -62.4(6) . . . . ? C28 N3 C25 C24 119.7(5) . . . . ? C19 C24 C25 N3 -73.8(6) . . . . ? C23 C24 C25 N3 106.0(5) . . . . ? C27 N4 C26 N3 0.6(5) . . . . ? Co1 N4 C26 N3 171.4(3) 1_545 . . . ? C28 N3 C26 N4 -0.7(5) . . . . ? C25 N3 C26 N4 -178.9(4) . . . . ? C26 N4 C27 C28 -0.2(5) . . . . ? Co1 N4 C27 C28 -170.6(3) 1_545 . . . ? N4 C27 C28 N3 -0.2(6) . . . . ? C26 N3 C28 C27 0.6(5) . . . . ? C25 N3 C28 C27 178.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.223 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.061 #========END