Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Graeme Hogarth' _publ_contact_author_address ; Department of Chemistry University College London 20 Gordon Street LONDON WC1H OAJ U.K. ; _publ_contact_author_email G.HOGARTH@UCL.AC.UK _publ_section_title ; Multiple nitrene insertions into metal-sulfur bonds of dithiocarbamate complexes: Synthesis of sulfido-amido and zwitterionic tetraamido complexes ; loop_ _publ_author_name 'Graeme Hogarth' 'K. Travis Holman' 'Andrew Pateman' 'Idris Richards' 'A. Sella' 'Jonathan Steed' data_cuamid _database_code_depnum_ccdc_archive 'CCDC 264509' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H36 Cl2 Cu N4 O4 S6' _chemical_formula_weight 783.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 12.7830(4) _cell_length_b 14.5350(4) _cell_length_c 19.6760(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.5320(10) _cell_angle_gamma 90.00 _cell_volume 3568.72(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 1.148 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 0.75A _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43653 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6115 _reflns_number_gt 5209 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+5.6790P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6115 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.22292(3) 0.85654(3) 0.21276(2) 0.04053(15) Uani 1 d . . . Cl1 Cl 0.3129(2) 0.81167(16) 0.45765(11) 0.1392(8) Uani 1 d . . . Cl2 Cl 0.3263(3) 1.00762(15) 0.44260(14) 0.1477(9) Uani 1 d . . . S1 S -0.00590(8) 0.80506(7) 0.14018(6) 0.0512(3) Uani 1 d . . . S2 S 0.05102(8) 0.76881(7) 0.28142(6) 0.0499(3) Uani 1 d . . . S3 S 0.26733(8) 0.71415(7) 0.26109(6) 0.0513(3) Uani 1 d . . . S4 S 0.37994(8) 0.87114(7) 0.11367(5) 0.0482(2) Uani 1 d . . . S5 S 0.44323(8) 0.95056(7) 0.24419(5) 0.0485(2) Uani 1 d . . . S6 S 0.21638(7) 1.01403(7) 0.23018(6) 0.0475(2) Uani 1 d . . . O1 O 0.0265(3) 0.8656(2) 0.09071(17) 0.0688(9) Uani 1 d . . . O2 O -0.1152(2) 0.8073(3) 0.1472(2) 0.0751(10) Uani 1 d . . . O3 O 0.4881(3) 0.8457(2) 0.11251(19) 0.0657(9) Uani 1 d . . . O4 O 0.2942(3) 0.8137(2) 0.07849(18) 0.0689(9) Uani 1 d . . . N1 N 0.0737(2) 0.8319(2) 0.21449(16) 0.0431(7) Uani 1 d . . . N2 N 0.1552(3) 0.6189(2) 0.33486(19) 0.0543(8) Uani 1 d . . . N3 N 0.3657(3) 0.8734(2) 0.19404(17) 0.0450(7) Uani 1 d . . . N4 N 0.3884(3) 1.1187(2) 0.27356(18) 0.0481(7) Uani 1 d . . . C1 C 0.0221(3) 0.6906(3) 0.1201(2) 0.0471(9) Uani 1 d . . . C2 C 0.1012(4) 0.6728(3) 0.0842(2) 0.0560(10) Uani 1 d . . . H2 H 0.1373 0.7208 0.0681 0.067 Uiso 1 calc R . . C3 C 0.1260(4) 0.5824(4) 0.0724(3) 0.0661(12) Uani 1 d . . . H3 H 0.1791 0.5703 0.0480 0.079 Uiso 1 calc R . . C4 C 0.0738(4) 0.5092(3) 0.0961(3) 0.0616(11) Uani 1 d . . . C5 C -0.0042(4) 0.5291(4) 0.1315(3) 0.0766(14) Uani 1 d . . . H5 H -0.0399 0.4811 0.1479 0.092 Uiso 1 calc R . . C6 C -0.0315(4) 0.6184(3) 0.1435(3) 0.0645(12) Uani 1 d . . . H6 H -0.0856 0.6301 0.1672 0.077 Uiso 1 calc R . . C7 C 0.1041(5) 0.4110(4) 0.0829(4) 0.0921(18) Uani 1 d . . . H7A H 0.0941 0.3726 0.1207 0.111 Uiso 1 calc R . . H7B H 0.1779 0.4089 0.0795 0.111 Uiso 1 calc R . . H7C H 0.0596 0.3893 0.0402 0.111 Uiso 1 calc R . . C8 C 0.1597(3) 0.6907(3) 0.2952(2) 0.0443(8) Uani 1 d . . . C9 C 0.0564(4) 0.5919(4) 0.3582(3) 0.0749(14) Uani 1 d . . . H9A H 0.0546 0.5255 0.3628 0.090 Uiso 1 calc R . . H9B H -0.0059 0.6103 0.3233 0.090 Uiso 1 calc R . . C10 C 0.0517(6) 0.6355(6) 0.4261(3) 0.113(3) Uani 1 d . . . H10A H 0.1105 0.6138 0.4615 0.135 Uiso 1 calc R . . H10B H -0.0147 0.6196 0.4384 0.135 Uiso 1 calc R . . H10C H 0.0563 0.7011 0.4221 0.135 Uiso 1 calc R . . C11 C 0.2489(4) 0.5582(3) 0.3579(3) 0.0723(14) Uani 1 d . . . H11A H 0.2447 0.5300 0.4019 0.087 Uiso 1 calc R . . H11B H 0.3138 0.5949 0.3654 0.087 Uiso 1 calc R . . C12 C 0.2552(5) 0.4843(4) 0.3059(4) 0.097(2) Uani 1 d . . . H12A H 0.1881 0.4520 0.2944 0.117 Uiso 1 calc R . . H12B H 0.3114 0.4420 0.3253 0.117 Uiso 1 calc R . . H12C H 0.2700 0.5116 0.2645 0.117 Uiso 1 calc R . . C13 C 0.3610(3) 0.9833(3) 0.0788(2) 0.0474(9) Uani 1 d . . . C14 C 0.4482(4) 1.0354(3) 0.0733(3) 0.0689(13) Uani 1 d . . . H14 H 0.5171 1.0118 0.0875 0.083 Uiso 1 calc R . . C15 C 0.4328(5) 1.1237(4) 0.0464(3) 0.0788(15) Uani 1 d . . . H15 H 0.4922 1.1593 0.0437 0.095 Uiso 1 calc R . . C16 C 0.3323(4) 1.1598(3) 0.0236(2) 0.0658(12) Uani 1 d . . . C17 C 0.2462(4) 1.1062(4) 0.0288(2) 0.0675(12) Uani 1 d . . . H17 H 0.1775 1.1295 0.0131 0.081 Uiso 1 calc R . . C18 C 0.2583(4) 1.0181(3) 0.0568(2) 0.0564(10) Uani 1 d . . . H18 H 0.1989 0.9833 0.0607 0.068 Uiso 1 calc R . . C19 C 0.3179(6) 1.2561(4) -0.0057(4) 0.100(2) Uani 1 d . . . H19A H 0.2602 1.2567 -0.0461 0.120 Uiso 1 calc R . . H19B H 0.3828 1.2755 -0.0185 0.120 Uiso 1 calc R . . H19C H 0.3017 1.2972 0.0288 0.120 Uiso 1 calc R . . C20 C 0.3498(3) 1.0385(3) 0.25005(18) 0.0411(8) Uani 1 d . . . C21 C 0.5042(3) 1.1392(3) 0.2881(3) 0.0614(11) Uani 1 d . . . H21A H 0.5142 1.2045 0.2818 0.074 Uiso 1 calc R . . H21B H 0.5366 1.1065 0.2549 0.074 Uiso 1 calc R . . C22 C 0.5597(4) 1.1124(5) 0.3601(3) 0.0877(17) Uani 1 d . . . H22A H 0.5225 1.1387 0.3930 0.105 Uiso 1 calc R . . H22B H 0.6320 1.1348 0.3695 0.105 Uiso 1 calc R . . H22C H 0.5601 1.0466 0.3643 0.105 Uiso 1 calc R . . C23 C 0.3185(4) 1.1952(3) 0.2861(3) 0.0632(12) Uani 1 d . . . H23A H 0.3573 1.2336 0.3235 0.076 Uiso 1 calc R . . H23B H 0.2564 1.1703 0.3005 0.076 Uiso 1 calc R . . C24 C 0.2823(6) 1.2527(4) 0.2222(4) 0.098(2) Uani 1 d . . . H24A H 0.3438 1.2763 0.2072 0.117 Uiso 1 calc R . . H24B H 0.2397 1.3031 0.2326 0.117 Uiso 1 calc R . . H24C H 0.2403 1.2158 0.1859 0.117 Uiso 1 calc R . . C1S C 0.3354(15) 0.8950(8) 0.4100(5) 0.265(10) Uani 1 d . . . H1S1 H 0.2852 0.8903 0.3655 0.318 Uiso 1 calc R . . H1S2 H 0.4067 0.8872 0.4014 0.318 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0419(3) 0.0355(3) 0.0465(3) 0.00084(17) 0.01468(19) -0.00318(17) Cl1 0.221(3) 0.1059(14) 0.0955(13) 0.0052(11) 0.0446(15) -0.0030(16) Cl2 0.215(3) 0.0936(14) 0.1412(19) -0.0046(13) 0.0535(18) -0.0237(15) S1 0.0459(5) 0.0466(5) 0.0576(6) 0.0008(4) 0.0035(4) 0.0052(4) S2 0.0442(5) 0.0536(6) 0.0574(6) 0.0053(4) 0.0229(4) 0.0056(4) S3 0.0444(5) 0.0444(5) 0.0721(7) 0.0138(5) 0.0281(5) 0.0051(4) S4 0.0547(6) 0.0391(5) 0.0569(6) -0.0011(4) 0.0258(5) -0.0008(4) S5 0.0399(5) 0.0489(5) 0.0567(6) 0.0009(4) 0.0101(4) 0.0022(4) S6 0.0380(5) 0.0392(5) 0.0651(6) -0.0055(4) 0.0109(4) -0.0018(4) O1 0.091(2) 0.0545(18) 0.0574(18) 0.0112(14) 0.0083(17) 0.0041(16) O2 0.0409(16) 0.080(2) 0.098(3) -0.0139(19) 0.0028(16) 0.0107(15) O3 0.068(2) 0.0558(18) 0.087(2) 0.0097(16) 0.0460(17) 0.0135(15) O4 0.083(2) 0.0539(18) 0.073(2) -0.0166(15) 0.0236(17) -0.0213(16) N1 0.0430(16) 0.0388(16) 0.0483(18) 0.0018(13) 0.0115(13) -0.0003(13) N2 0.052(2) 0.052(2) 0.064(2) 0.0128(16) 0.0234(16) -0.0007(16) N3 0.0486(18) 0.0381(16) 0.0528(19) 0.0013(13) 0.0210(15) -0.0014(13) N4 0.0451(17) 0.0466(18) 0.0540(19) -0.0080(14) 0.0139(14) -0.0093(14) C1 0.041(2) 0.045(2) 0.053(2) -0.0053(17) 0.0056(16) -0.0037(16) C2 0.061(3) 0.051(2) 0.059(3) -0.0057(19) 0.019(2) -0.010(2) C3 0.060(3) 0.077(3) 0.065(3) -0.017(2) 0.020(2) 0.003(2) C4 0.064(3) 0.050(2) 0.067(3) -0.008(2) 0.005(2) 0.000(2) C5 0.079(3) 0.053(3) 0.102(4) -0.001(3) 0.029(3) -0.020(2) C6 0.056(3) 0.054(3) 0.090(3) -0.008(2) 0.031(2) -0.009(2) C7 0.108(5) 0.060(3) 0.104(4) -0.010(3) 0.014(4) 0.014(3) C8 0.044(2) 0.0401(19) 0.051(2) 0.0031(16) 0.0162(16) -0.0022(16) C9 0.065(3) 0.076(3) 0.092(4) 0.022(3) 0.034(3) -0.012(3) C10 0.111(5) 0.162(7) 0.084(4) 0.044(4) 0.059(4) 0.035(5) C11 0.063(3) 0.065(3) 0.093(4) 0.035(3) 0.025(3) 0.013(2) C12 0.087(4) 0.047(3) 0.167(7) 0.003(3) 0.049(4) 0.003(3) C13 0.051(2) 0.048(2) 0.045(2) 0.0035(16) 0.0159(17) 0.0002(17) C14 0.055(3) 0.061(3) 0.094(4) 0.027(3) 0.023(2) 0.002(2) C15 0.076(3) 0.065(3) 0.099(4) 0.023(3) 0.027(3) -0.015(3) C16 0.085(3) 0.057(3) 0.056(3) 0.015(2) 0.016(2) 0.007(2) C17 0.069(3) 0.078(3) 0.054(3) 0.013(2) 0.009(2) 0.018(3) C18 0.053(2) 0.062(3) 0.053(2) 0.0073(19) 0.0104(19) -0.003(2) C19 0.128(6) 0.067(4) 0.104(5) 0.029(3) 0.022(4) 0.009(4) C20 0.0430(19) 0.0408(19) 0.0405(19) 0.0014(15) 0.0115(15) -0.0043(15) C21 0.047(2) 0.064(3) 0.075(3) -0.010(2) 0.018(2) -0.018(2) C22 0.065(3) 0.091(4) 0.095(4) -0.004(3) -0.008(3) -0.019(3) C23 0.063(3) 0.049(2) 0.082(3) -0.024(2) 0.026(2) -0.008(2) C24 0.115(5) 0.056(3) 0.116(5) 0.000(3) 0.013(4) 0.017(3) C1S 0.58(3) 0.141(9) 0.111(7) -0.021(6) 0.149(13) -0.122(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.949(3) . ? Cu1 N3 1.954(3) . ? Cu1 S3 2.2969(11) . ? Cu1 S6 2.3188(10) . ? Cl1 C1S 1.595(10) . ? Cl2 C1S 1.771(12) . ? S1 O2 1.434(3) . ? S1 O1 1.438(3) . ? S1 N1 1.637(3) . ? S1 C1 1.764(4) . ? S2 N1 1.680(3) . ? S2 C8 1.768(4) . ? S3 C8 1.691(4) . ? S4 O4 1.431(3) . ? S4 O3 1.436(3) . ? S4 N3 1.631(3) . ? S4 C13 1.764(4) . ? S5 N3 1.670(3) . ? S5 C20 1.770(4) . ? S6 C20 1.702(4) . ? N2 C8 1.313(5) . ? N2 C11 1.477(6) . ? N2 C9 1.486(5) . ? N4 C20 1.310(5) . ? N4 C21 1.476(5) . ? N4 C23 1.481(5) . ? C1 C2 1.377(6) . ? C1 C6 1.386(6) . ? C2 C3 1.383(7) . ? C3 C4 1.389(7) . ? C4 C5 1.365(7) . ? C4 C7 1.515(7) . ? C5 C6 1.377(7) . ? C9 C10 1.492(9) . ? C11 C12 1.498(8) . ? C13 C14 1.372(6) . ? C13 C18 1.386(6) . ? C14 C15 1.385(7) . ? C15 C16 1.370(7) . ? C16 C17 1.370(7) . ? C16 C19 1.510(7) . ? C17 C18 1.390(7) . ? C21 C22 1.492(7) . ? C23 C24 1.497(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 169.85(13) . . ? N1 Cu1 S3 88.97(9) . . ? N3 Cu1 S3 91.97(10) . . ? N1 Cu1 S6 96.44(10) . . ? N3 Cu1 S6 88.21(9) . . ? S3 Cu1 S6 147.34(5) . . ? O2 S1 O1 118.8(2) . . ? O2 S1 N1 109.76(19) . . ? O1 S1 N1 104.16(18) . . ? O2 S1 C1 107.0(2) . . ? O1 S1 C1 108.9(2) . . ? N1 S1 C1 107.91(17) . . ? N1 S2 C8 101.93(17) . . ? C8 S3 Cu1 101.31(14) . . ? O4 S4 O3 118.7(2) . . ? O4 S4 N3 104.24(18) . . ? O3 S4 N3 109.35(19) . . ? O4 S4 C13 109.0(2) . . ? O3 S4 C13 106.44(19) . . ? N3 S4 C13 108.84(17) . . ? N3 S5 C20 101.57(17) . . ? C20 S6 Cu1 100.01(13) . . ? S1 N1 S2 113.01(18) . . ? S1 N1 Cu1 116.68(17) . . ? S2 N1 Cu1 116.72(17) . . ? C8 N2 C11 121.3(3) . . ? C8 N2 C9 122.9(4) . . ? C11 N2 C9 115.8(4) . . ? S4 N3 S5 114.19(18) . . ? S4 N3 Cu1 119.06(19) . . ? S5 N3 Cu1 115.60(17) . . ? C20 N4 C21 122.2(3) . . ? C20 N4 C23 122.2(3) . . ? C21 N4 C23 115.6(3) . . ? C2 C1 C6 119.9(4) . . ? C2 C1 S1 120.0(3) . . ? C6 C1 S1 120.0(3) . . ? C1 C2 C3 119.0(4) . . ? C2 C3 C4 121.8(4) . . ? C5 C4 C3 117.7(4) . . ? C5 C4 C7 122.0(5) . . ? C3 C4 C7 120.3(5) . . ? C4 C5 C6 121.9(5) . . ? C5 C6 C1 119.6(4) . . ? N2 C8 S3 122.7(3) . . ? N2 C8 S2 117.8(3) . . ? S3 C8 S2 119.3(2) . . ? N2 C9 C10 111.5(5) . . ? N2 C11 C12 112.2(5) . . ? C14 C13 C18 120.3(4) . . ? C14 C13 S4 119.8(3) . . ? C18 C13 S4 120.0(3) . . ? C13 C14 C15 119.4(5) . . ? C16 C15 C14 121.7(5) . . ? C17 C16 C15 118.0(4) . . ? C17 C16 C19 121.5(5) . . ? C15 C16 C19 120.5(5) . . ? C16 C17 C18 122.1(5) . . ? C13 C18 C17 118.5(4) . . ? N4 C20 S6 123.3(3) . . ? N4 C20 S5 117.2(3) . . ? S6 C20 S5 119.4(2) . . ? N4 C21 C22 112.4(4) . . ? N4 C23 C24 111.6(4) . . ? Cl1 C1S Cl2 117.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 S3 C8 -19.45(17) . . . . ? N3 Cu1 S3 C8 170.66(17) . . . . ? S6 Cu1 S3 C8 80.91(16) . . . . ? N1 Cu1 S6 C20 166.27(16) . . . . ? N3 Cu1 S6 C20 -22.78(16) . . . . ? S3 Cu1 S6 C20 68.07(15) . . . . ? O2 S1 N1 S2 52.1(3) . . . . ? O1 S1 N1 S2 -179.8(2) . . . . ? C1 S1 N1 S2 -64.2(2) . . . . ? O2 S1 N1 Cu1 -168.4(2) . . . . ? O1 S1 N1 Cu1 -40.3(2) . . . . ? C1 S1 N1 Cu1 75.3(2) . . . . ? C8 S2 N1 S1 104.0(2) . . . . ? C8 S2 N1 Cu1 -35.5(2) . . . . ? N3 Cu1 N1 S1 -8.4(9) . . . . ? S3 Cu1 N1 S1 -103.80(17) . . . . ? S6 Cu1 N1 S1 108.49(17) . . . . ? N3 Cu1 N1 S2 129.6(7) . . . . ? S3 Cu1 N1 S2 34.17(17) . . . . ? S6 Cu1 N1 S2 -113.54(17) . . . . ? O4 S4 N3 S5 -170.0(2) . . . . ? O3 S4 N3 S5 62.0(2) . . . . ? C13 S4 N3 S5 -53.9(2) . . . . ? O4 S4 N3 Cu1 -27.7(3) . . . . ? O3 S4 N3 Cu1 -155.65(19) . . . . ? C13 S4 N3 Cu1 88.5(2) . . . . ? C20 S5 N3 S4 103.9(2) . . . . ? C20 S5 N3 Cu1 -39.8(2) . . . . ? N1 Cu1 N3 S4 14.7(9) . . . . ? S3 Cu1 N3 S4 109.85(18) . . . . ? S6 Cu1 N3 S4 -102.83(18) . . . . ? N1 Cu1 N3 S5 156.5(6) . . . . ? S3 Cu1 N3 S5 -108.34(17) . . . . ? S6 Cu1 N3 S5 38.98(17) . . . . ? O2 S1 C1 C2 154.3(3) . . . . ? O1 S1 C1 C2 24.8(4) . . . . ? N1 S1 C1 C2 -87.7(4) . . . . ? O2 S1 C1 C6 -29.0(4) . . . . ? O1 S1 C1 C6 -158.5(4) . . . . ? N1 S1 C1 C6 89.0(4) . . . . ? C6 C1 C2 C3 -0.3(7) . . . . ? S1 C1 C2 C3 176.4(3) . . . . ? C1 C2 C3 C4 -0.3(7) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? C2 C3 C4 C7 -179.3(5) . . . . ? C3 C4 C5 C6 0.3(8) . . . . ? C7 C4 C5 C6 179.9(5) . . . . ? C4 C5 C6 C1 -0.9(9) . . . . ? C2 C1 C6 C5 0.9(7) . . . . ? S1 C1 C6 C5 -175.8(4) . . . . ? C11 N2 C8 S3 5.9(6) . . . . ? C9 N2 C8 S3 -172.7(4) . . . . ? C11 N2 C8 S2 -170.4(4) . . . . ? C9 N2 C8 S2 11.0(6) . . . . ? Cu1 S3 C8 N2 -172.7(3) . . . . ? Cu1 S3 C8 S2 3.6(3) . . . . ? N1 S2 C8 N2 -166.4(3) . . . . ? N1 S2 C8 S3 17.1(3) . . . . ? C8 N2 C9 C10 -90.9(6) . . . . ? C11 N2 C9 C10 90.5(6) . . . . ? C8 N2 C11 C12 -86.5(6) . . . . ? C9 N2 C11 C12 92.2(5) . . . . ? O4 S4 C13 C14 -145.0(4) . . . . ? O3 S4 C13 C14 -15.9(4) . . . . ? N3 S4 C13 C14 101.9(4) . . . . ? O4 S4 C13 C18 34.6(4) . . . . ? O3 S4 C13 C18 163.7(3) . . . . ? N3 S4 C13 C18 -78.5(4) . . . . ? C18 C13 C14 C15 0.9(8) . . . . ? S4 C13 C14 C15 -179.5(4) . . . . ? C13 C14 C15 C16 -1.4(9) . . . . ? C14 C15 C16 C17 0.6(9) . . . . ? C14 C15 C16 C19 -179.7(6) . . . . ? C15 C16 C17 C18 0.7(8) . . . . ? C19 C16 C17 C18 -178.9(5) . . . . ? C14 C13 C18 C17 0.4(7) . . . . ? S4 C13 C18 C17 -179.2(3) . . . . ? C16 C17 C18 C13 -1.3(7) . . . . ? C21 N4 C20 S6 -177.9(3) . . . . ? C23 N4 C20 S6 1.0(6) . . . . ? C21 N4 C20 S5 6.0(5) . . . . ? C23 N4 C20 S5 -175.1(3) . . . . ? Cu1 S6 C20 N4 -170.5(3) . . . . ? Cu1 S6 C20 S5 5.5(2) . . . . ? N3 S5 C20 N4 -165.6(3) . . . . ? N3 S5 C20 S6 18.2(3) . . . . ? C20 N4 C21 C22 -87.4(5) . . . . ? C23 N4 C21 C22 93.6(5) . . . . ? C20 N4 C23 C24 -88.6(5) . . . . ? C21 N4 C23 C24 90.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.750 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.072 data_niamid _database_code_depnum_ccdc_archive 'CCDC 264510' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H35 Cl3 N4 Ni O4 S6' _chemical_formula_weight 812.99 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 12.8318(4) _cell_length_b 14.6975(4) _cell_length_c 19.5611(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.5790(10) _cell_angle_gamma 90.00 _cell_volume 3637.70(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6216 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6216 _reflns_number_gt 5166 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'RES2INS (Barbour, 1995)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+11.5858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0028(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6216 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1820 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.22959(5) 0.11977(4) 0.21805(3) 0.0397(2) Uani 1 d . . . S1 S 0.39001(12) 0.11075(10) 0.11911(8) 0.0514(4) Uani 1 d . . . S2 S 0.43934(11) 0.02063(10) 0.24469(8) 0.0500(4) Uani 1 d . . . S3 S 0.21171(11) -0.03022(9) 0.22112(8) 0.0482(4) Uani 1 d . . . S4 S 0.00468(11) 0.16524(10) 0.15464(8) 0.0524(4) Uani 1 d . . . S5 S 0.06569(12) 0.20858(10) 0.29333(8) 0.0530(4) Uani 1 d . . . S6 S 0.26919(11) 0.26014(9) 0.25142(8) 0.0479(4) Uani 1 d . . . O1 O 0.3165(4) 0.1790(3) 0.0872(2) 0.0649(12) Uani 1 d . . . O2 O 0.5008(4) 0.1247(3) 0.1208(3) 0.0717(13) Uani 1 d . . . O3 O 0.0341(4) 0.1044(3) 0.1035(2) 0.0669(12) Uani 1 d . . . O4 O -0.1016(3) 0.1626(3) 0.1681(3) 0.0727(13) Uani 1 d . . . N1 N 0.3689(3) 0.1039(3) 0.1995(2) 0.0450(10) Uani 1 d . . . N2 N 0.3713(4) -0.1458(3) 0.2625(3) 0.0516(12) Uani 1 d . . . N3 N 0.0861(4) 0.1416(3) 0.2267(2) 0.0466(10) Uani 1 d . . . N4 N 0.1659(4) 0.3637(3) 0.3292(3) 0.0587(13) Uani 1 d . . . C1 C 0.3576(5) 0.0070(4) 0.0766(3) 0.0499(13) Uani 1 d . . . C2 C 0.4353(6) -0.0549(5) 0.0678(4) 0.0670(18) Uani 1 d . . . H2 H 0.5059 -0.0413 0.0843 0.080 Uiso 1 calc R . . C3 C 0.4089(6) -0.1369(5) 0.0346(4) 0.0732(19) Uani 1 d . . . H3 H 0.4619 -0.1780 0.0290 0.088 Uiso 1 calc R . . C4 C 0.3042(6) -0.1587(5) 0.0097(3) 0.0679(18) Uani 1 d . . . C5 C 0.2278(6) -0.0961(5) 0.0180(3) 0.0673(17) Uani 1 d . . . H5 H 0.1576 -0.1095 0.0004 0.081 Uiso 1 calc R . . C6 C 0.2514(5) -0.0137(5) 0.0519(3) 0.0600(16) Uani 1 d . . . H6 H 0.1980 0.0268 0.0580 0.072 Uiso 1 calc R . . C7 C 0.2755(9) -0.2490(6) -0.0258(5) 0.109(3) Uani 1 d . . . H7A H 0.2002 -0.2568 -0.0330 0.131 Uiso 1 calc R . . H7B H 0.3086 -0.2975 0.0028 0.131 Uiso 1 calc R . . H7C H 0.2997 -0.2500 -0.0697 0.131 Uiso 1 calc R . . C8 C 0.3403(4) -0.0629(4) 0.2431(3) 0.0436(12) Uani 1 d . . . C9 C 0.2948(6) -0.2198(4) 0.2677(4) 0.0683(18) Uani 1 d . . . H9A H 0.2308 -0.1942 0.2802 0.082 Uiso 1 calc R . . H9B H 0.3246 -0.2617 0.3041 0.082 Uiso 1 calc R . . C10 C 0.2679(9) -0.2704(6) 0.2010(6) 0.112(3) Uani 1 d . . . H10A H 0.2233 -0.2333 0.1678 0.134 Uiso 1 calc R . . H10B H 0.2315 -0.3256 0.2086 0.134 Uiso 1 calc R . . H10C H 0.3316 -0.2848 0.1836 0.134 Uiso 1 calc R . . C11 C 0.4851(5) -0.1688(5) 0.2810(4) 0.0660(17) Uani 1 d . . . H11A H 0.5244 -0.1360 0.2506 0.079 Uiso 1 calc R . . H11B H 0.4944 -0.2334 0.2738 0.079 Uiso 1 calc R . . C12 C 0.5289(7) -0.1454(6) 0.3554(4) 0.086(2) Uani 1 d . . . H12A H 0.5074 -0.0849 0.3653 0.103 Uiso 1 calc R . . H12B H 0.6046 -0.1485 0.3624 0.103 Uiso 1 calc R . . H12C H 0.5024 -0.1878 0.3856 0.103 Uiso 1 calc R . . C13 C 0.0289(4) 0.2787(4) 0.1303(3) 0.0498(13) Uani 1 d . . . C14 C 0.1061(5) 0.2964(4) 0.0902(3) 0.0600(16) Uani 1 d . . . H14 H 0.1435 0.2491 0.0740 0.072 Uiso 1 calc R . . C15 C 0.1256(6) 0.3842(5) 0.0750(4) 0.0730(19) Uani 1 d . . . H15 H 0.1768 0.3962 0.0477 0.088 Uiso 1 calc R . . C16 C 0.0723(6) 0.4571(5) 0.0985(4) 0.0684(18) Uani 1 d . . . C17 C -0.0028(6) 0.4374(5) 0.1383(4) 0.075(2) Uani 1 d . . . H17 H -0.0388 0.4851 0.1553 0.090 Uiso 1 calc R . . C18 C -0.0268(5) 0.3499(5) 0.1541(4) 0.0659(17) Uani 1 d . . . H18 H -0.0795 0.3383 0.1802 0.079 Uiso 1 calc R . . C19 C 0.0985(9) 0.5548(6) 0.0813(5) 0.108(3) Uani 1 d . . . H19A H 0.0386 0.5931 0.0836 0.129 Uiso 1 calc R . . H19B H 0.1156 0.5571 0.0354 0.129 Uiso 1 calc R . . H19C H 0.1579 0.5757 0.1140 0.129 Uiso 1 calc R . . C20 C 0.1686(4) 0.2887(4) 0.2940(3) 0.0464(12) Uani 1 d . . . C21 C 0.2601(6) 0.4248(5) 0.3426(5) 0.080(2) Uani 1 d . . . H21A H 0.3240 0.3885 0.3467 0.096 Uiso 1 calc R . . H21B H 0.2607 0.4565 0.3862 0.096 Uiso 1 calc R . . C22 C 0.2594(7) 0.4932(5) 0.2854(6) 0.105(3) Uani 1 d . . . H22A H 0.2529 0.4621 0.2417 0.126 Uiso 1 calc R . . H22B H 0.3242 0.5272 0.2932 0.126 Uiso 1 calc R . . H22C H 0.2008 0.5339 0.2848 0.126 Uiso 1 calc R . . C23 C 0.0720(6) 0.3932(5) 0.3586(4) 0.076(2) Uani 1 d . . . H23A H 0.0085 0.3738 0.3280 0.091 Uiso 1 calc R . . H23B H 0.0710 0.4591 0.3608 0.091 Uiso 1 calc R . . C24 C 0.0705(8) 0.3558(8) 0.4290(5) 0.109(3) Uani 1 d . . . H24A H 0.0589 0.2913 0.4260 0.131 Uiso 1 calc R . . H24B H 0.0145 0.3840 0.4485 0.131 Uiso 1 calc R . . H24C H 0.1369 0.3680 0.4581 0.131 Uiso 1 calc R . . Cl1S Cl 0.6768(2) 0.70432(17) 0.04102(14) 0.1063(8) Uani 1 d . . . Cl2S Cl 0.5000(2) 0.6045(2) 0.0717(2) 0.1422(13) Uani 1 d . . . Cl3S Cl 0.6971(3) 0.5134(2) 0.07577(18) 0.1349(11) Uani 1 d . . . C1S C 0.6354(8) 0.6163(6) 0.0905(4) 0.087(2) Uani 1 d . . . H1S H 0.6549 0.6320 0.1396 0.104 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0370(4) 0.0343(4) 0.0494(4) -0.0008(3) 0.0116(3) 0.0013(2) S1 0.0541(8) 0.0421(7) 0.0635(9) 0.0051(6) 0.0260(7) 0.0004(6) S2 0.0390(7) 0.0486(8) 0.0619(9) 0.0007(6) 0.0068(6) 0.0025(6) S3 0.0397(7) 0.0378(7) 0.0681(9) 0.0030(6) 0.0117(6) 0.0010(5) S4 0.0405(7) 0.0437(8) 0.0709(10) -0.0035(7) 0.0028(6) -0.0021(6) S5 0.0485(8) 0.0516(8) 0.0636(9) -0.0047(7) 0.0229(7) -0.0020(6) S6 0.0422(7) 0.0404(7) 0.0641(9) -0.0067(6) 0.0178(6) -0.0028(5) O1 0.081(3) 0.045(2) 0.074(3) 0.018(2) 0.028(2) 0.013(2) O2 0.062(3) 0.065(3) 0.098(4) -0.004(3) 0.043(3) -0.016(2) O3 0.075(3) 0.051(2) 0.069(3) -0.015(2) -0.002(2) 0.001(2) O4 0.036(2) 0.069(3) 0.111(4) 0.004(3) 0.005(2) -0.008(2) N1 0.043(2) 0.038(2) 0.056(3) -0.001(2) 0.014(2) 0.0028(18) N2 0.051(3) 0.041(2) 0.068(3) 0.006(2) 0.021(2) 0.011(2) N3 0.044(2) 0.040(2) 0.057(3) -0.004(2) 0.011(2) 0.0016(19) N4 0.054(3) 0.052(3) 0.072(3) -0.013(3) 0.017(2) 0.003(2) C1 0.058(3) 0.045(3) 0.050(3) 0.001(2) 0.018(3) 0.009(3) C2 0.056(4) 0.069(4) 0.077(4) -0.007(4) 0.016(3) 0.013(3) C3 0.072(5) 0.066(4) 0.082(5) -0.011(4) 0.015(4) 0.021(4) C4 0.084(5) 0.064(4) 0.054(4) -0.010(3) 0.008(3) 0.012(4) C5 0.059(4) 0.080(5) 0.060(4) -0.009(3) 0.001(3) 0.005(3) C6 0.061(4) 0.065(4) 0.054(3) 0.001(3) 0.009(3) 0.016(3) C7 0.139(9) 0.080(6) 0.095(6) -0.027(5) -0.020(6) 0.017(6) C8 0.044(3) 0.042(3) 0.047(3) -0.002(2) 0.014(2) 0.007(2) C9 0.067(4) 0.046(3) 0.098(5) 0.015(3) 0.029(4) 0.004(3) C10 0.125(8) 0.073(6) 0.138(9) -0.009(6) 0.021(7) -0.031(6) C11 0.059(4) 0.058(4) 0.083(5) 0.008(3) 0.017(3) 0.021(3) C12 0.080(5) 0.077(5) 0.095(6) 0.003(4) -0.002(4) 0.027(4) C13 0.043(3) 0.044(3) 0.060(3) -0.002(3) 0.003(2) 0.005(2) C14 0.066(4) 0.052(4) 0.065(4) 0.003(3) 0.018(3) 0.016(3) C15 0.081(5) 0.071(5) 0.069(4) 0.012(4) 0.017(4) 0.000(4) C16 0.080(5) 0.049(4) 0.072(4) 0.007(3) 0.001(4) 0.004(3) C17 0.079(5) 0.053(4) 0.093(5) -0.004(4) 0.017(4) 0.014(3) C18 0.059(4) 0.057(4) 0.085(5) 0.002(3) 0.022(3) 0.009(3) C19 0.154(10) 0.059(5) 0.105(7) 0.007(5) 0.009(6) -0.007(5) C20 0.042(3) 0.039(3) 0.060(3) 0.001(2) 0.014(2) 0.006(2) C21 0.068(4) 0.063(4) 0.113(6) -0.038(4) 0.028(4) -0.010(3) C22 0.090(6) 0.050(4) 0.183(11) -0.008(5) 0.047(6) 0.000(4) C23 0.064(4) 0.071(5) 0.097(5) -0.025(4) 0.028(4) 0.016(3) C24 0.117(8) 0.137(9) 0.084(6) -0.036(6) 0.049(6) -0.015(6) Cl1S 0.138(2) 0.0873(15) 0.0994(16) 0.0130(12) 0.0369(15) -0.0219(14) Cl2S 0.1018(19) 0.146(3) 0.169(3) 0.071(2) -0.0053(19) -0.0135(18) Cl3S 0.161(3) 0.105(2) 0.140(2) 0.0284(18) 0.029(2) 0.0232(19) C1S 0.112(7) 0.082(5) 0.060(4) 0.011(4) 0.001(4) -0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.897(4) . ? Ni1 N3 1.904(4) . ? Ni1 S6 2.1977(15) . ? Ni1 S3 2.2183(15) . ? S1 O2 1.431(5) . ? S1 O1 1.446(4) . ? S1 N1 1.643(5) . ? S1 C1 1.754(6) . ? S2 N1 1.683(5) . ? S2 C8 1.764(6) . ? S3 C8 1.703(5) . ? S4 O4 1.432(5) . ? S4 O3 1.437(5) . ? S4 N3 1.647(5) . ? S4 C13 1.776(6) . ? S5 N3 1.688(5) . ? S5 C20 1.767(6) . ? S6 C20 1.701(5) . ? N2 C8 1.318(7) . ? N2 C9 1.481(8) . ? N2 C11 1.483(8) . ? N4 C20 1.303(7) . ? N4 C23 1.485(8) . ? N4 C21 1.494(8) . ? C1 C2 1.381(8) . ? C1 C6 1.401(9) . ? C2 C3 1.385(10) . ? C3 C4 1.388(10) . ? C4 C5 1.374(10) . ? C4 C7 1.515(10) . ? C5 C6 1.390(10) . ? C9 C10 1.492(13) . ? C11 C12 1.509(11) . ? C13 C14 1.387(9) . ? C13 C18 1.390(9) . ? C14 C15 1.357(10) . ? C15 C16 1.391(10) . ? C16 C17 1.366(11) . ? C16 C19 1.525(10) . ? C17 C18 1.369(10) . ? C21 C22 1.502(13) . ? C23 C24 1.486(13) . ? Cl1S C1S 1.750(8) . ? Cl2S C1S 1.724(10) . ? Cl3S C1S 1.752(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N3 173.6(2) . . ? N1 Ni1 S6 89.62(14) . . ? N3 Ni1 S6 89.68(14) . . ? N1 Ni1 S3 89.33(14) . . ? N3 Ni1 S3 93.39(14) . . ? S6 Ni1 S3 160.86(7) . . ? O2 S1 O1 119.1(3) . . ? O2 S1 N1 107.9(3) . . ? O1 S1 N1 104.8(2) . . ? O2 S1 C1 107.0(3) . . ? O1 S1 C1 108.2(3) . . ? N1 S1 C1 109.7(3) . . ? N1 S2 C8 100.1(2) . . ? C8 S3 Ni1 100.77(19) . . ? O4 S4 O3 118.6(3) . . ? O4 S4 N3 109.0(3) . . ? O3 S4 N3 105.2(3) . . ? O4 S4 C13 106.8(3) . . ? O3 S4 C13 108.6(3) . . ? N3 S4 C13 108.2(3) . . ? N3 S5 C20 100.5(2) . . ? C20 S6 Ni1 102.7(2) . . ? S1 N1 S2 112.8(3) . . ? S1 N1 Ni1 119.1(3) . . ? S2 N1 Ni1 115.4(3) . . ? C8 N2 C9 121.8(5) . . ? C8 N2 C11 121.3(5) . . ? C9 N2 C11 116.9(5) . . ? S4 N3 S5 112.3(3) . . ? S4 N3 Ni1 116.4(3) . . ? S5 N3 Ni1 116.4(3) . . ? C20 N4 C23 123.1(6) . . ? C20 N4 C21 120.7(5) . . ? C23 N4 C21 116.2(5) . . ? C2 C1 C6 119.7(6) . . ? C2 C1 S1 120.8(5) . . ? C6 C1 S1 119.5(4) . . ? C1 C2 C3 120.4(7) . . ? C2 C3 C4 120.8(6) . . ? C5 C4 C3 118.2(7) . . ? C5 C4 C7 121.1(7) . . ? C3 C4 C7 120.7(7) . . ? C4 C5 C6 122.4(7) . . ? C5 C6 C1 118.4(6) . . ? N2 C8 S3 124.5(4) . . ? N2 C8 S2 117.1(4) . . ? S3 C8 S2 118.2(3) . . ? N2 C9 C10 111.4(7) . . ? N2 C11 C12 112.1(6) . . ? C14 C13 C18 120.2(6) . . ? C14 C13 S4 120.0(4) . . ? C18 C13 S4 119.7(5) . . ? C15 C14 C13 118.5(6) . . ? C14 C15 C16 122.8(7) . . ? C17 C16 C15 117.2(7) . . ? C17 C16 C19 121.9(7) . . ? C15 C16 C19 120.9(8) . . ? C16 C17 C18 122.3(7) . . ? C17 C18 C13 119.0(7) . . ? N4 C20 S6 123.8(4) . . ? N4 C20 S5 118.9(4) . . ? S6 C20 S5 117.3(3) . . ? N4 C21 C22 111.5(7) . . ? N4 C23 C24 112.9(7) . . ? Cl2S C1S Cl1S 110.1(5) . . ? Cl2S C1S Cl3S 110.2(5) . . ? Cl1S C1S Cl3S 111.2(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 N1 Ni1 S3 C8 25.2(2) . . . . ? N3 Ni1 S3 C8 -160.5(2) . . . . ? S6 Ni1 S3 C8 -61.7(3) . . . . ? N1 Ni1 S6 C20 -164.8(2) . . . . ? N3 Ni1 S6 C20 21.5(3) . . . . ? S3 Ni1 S6 C20 -78.0(3) . . . . ? O2 S1 N1 S2 -57.4(3) . . . . ? O1 S1 N1 S2 174.7(3) . . . . ? C1 S1 N1 S2 58.8(3) . . . . ? O2 S1 N1 Ni1 162.4(3) . . . . ? O1 S1 N1 Ni1 34.6(3) . . . . ? C1 S1 N1 Ni1 -81.4(3) . . . . ? C8 S2 N1 S1 -102.1(3) . . . . ? C8 S2 N1 Ni1 39.6(3) . . . . ? N3 Ni1 N1 S1 -17.1(19) . . . . ? S6 Ni1 N1 S1 -100.8(3) . . . . ? S3 Ni1 N1 S1 98.3(3) . . . . ? N3 Ni1 N1 S2 -156.3(16) . . . . ? S6 Ni1 N1 S2 120.1(2) . . . . ? S3 Ni1 N1 S2 -40.8(2) . . . . ? O4 S4 N3 S5 -53.1(4) . . . . ? O3 S4 N3 S5 178.7(3) . . . . ? C13 S4 N3 S5 62.7(3) . . . . ? O4 S4 N3 Ni1 169.1(3) . . . . ? O3 S4 N3 Ni1 41.0(3) . . . . ? C13 S4 N3 Ni1 -75.0(3) . . . . ? C20 S5 N3 S4 -100.4(3) . . . . ? C20 S5 N3 Ni1 37.4(3) . . . . ? N1 Ni1 N3 S4 15.4(19) . . . . ? S6 Ni1 N3 S4 99.1(2) . . . . ? S3 Ni1 N3 S4 -99.8(2) . . . . ? N1 Ni1 N3 S5 -120.6(16) . . . . ? S6 Ni1 N3 S5 -36.9(3) . . . . ? S3 Ni1 N3 S5 124.2(3) . . . . ? O2 S1 C1 C2 16.6(6) . . . . ? O1 S1 C1 C2 146.0(5) . . . . ? N1 S1 C1 C2 -100.2(6) . . . . ? O2 S1 C1 C6 -164.1(5) . . . . ? O1 S1 C1 C6 -34.7(6) . . . . ? N1 S1 C1 C6 79.1(5) . . . . ? C6 C1 C2 C3 0.1(10) . . . . ? S1 C1 C2 C3 179.5(6) . . . . ? C1 C2 C3 C4 -0.1(11) . . . . ? C2 C3 C4 C5 0.8(11) . . . . ? C2 C3 C4 C7 -179.3(8) . . . . ? C3 C4 C5 C6 -1.7(11) . . . . ? C7 C4 C5 C6 178.4(7) . . . . ? C4 C5 C6 C1 1.8(10) . . . . ? C2 C1 C6 C5 -1.0(9) . . . . ? S1 C1 C6 C5 179.7(5) . . . . ? C9 N2 C8 S3 -0.6(8) . . . . ? C11 N2 C8 S3 -179.8(5) . . . . ? C9 N2 C8 S2 175.8(5) . . . . ? C11 N2 C8 S2 -3.4(7) . . . . ? Ni1 S3 C8 N2 168.5(5) . . . . ? Ni1 S3 C8 S2 -7.9(3) . . . . ? N1 S2 C8 N2 167.2(4) . . . . ? N1 S2 C8 S3 -16.2(4) . . . . ? C8 N2 C9 C10 90.1(8) . . . . ? C11 N2 C9 C10 -90.7(8) . . . . ? C8 N2 C11 C12 84.0(8) . . . . ? C9 N2 C11 C12 -95.2(7) . . . . ? O4 S4 C13 C14 -155.8(5) . . . . ? O3 S4 C13 C14 -26.7(6) . . . . ? N3 S4 C13 C14 87.0(5) . . . . ? O4 S4 C13 C18 26.8(6) . . . . ? O3 S4 C13 C18 155.8(5) . . . . ? N3 S4 C13 C18 -90.5(5) . . . . ? C18 C13 C14 C15 0.2(10) . . . . ? S4 C13 C14 C15 -177.3(5) . . . . ? C13 C14 C15 C16 0.6(11) . . . . ? C14 C15 C16 C17 -0.2(11) . . . . ? C14 C15 C16 C19 178.8(7) . . . . ? C15 C16 C17 C18 -1.0(12) . . . . ? C19 C16 C17 C18 -180.0(8) . . . . ? C16 C17 C18 C13 1.7(12) . . . . ? C14 C13 C18 C17 -1.3(10) . . . . ? S4 C13 C18 C17 176.2(6) . . . . ? C23 N4 C20 S6 172.1(5) . . . . ? C21 N4 C20 S6 -8.6(9) . . . . ? C23 N4 C20 S5 -11.1(9) . . . . ? C21 N4 C20 S5 168.2(5) . . . . ? Ni1 S6 C20 N4 172.4(5) . . . . ? Ni1 S6 C20 S5 -4.5(4) . . . . ? N3 S5 C20 N4 165.6(5) . . . . ? N3 S5 C20 S6 -17.4(4) . . . . ? C20 N4 C21 C22 88.8(8) . . . . ? C23 N4 C21 C22 -91.8(8) . . . . ? C20 N4 C23 C24 87.8(9) . . . . ? C21 N4 C23 C24 -91.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.323 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.109 data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 264511' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common cobisamid _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H48.5 Co N6 O8.25 S8' _chemical_formula_weight 1036.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 P21/c 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 15.4966(13) _cell_length_b 12.7398(7) _cell_length_c 24.914(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.2140(10) _cell_angle_gamma 90.00 _cell_volume 4917.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2158 _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8400 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8400 _reflns_number_gt 5284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed interface to POVRay' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0464P)^2^+7.7906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8400 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1516 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.25828(4) 0.76753(5) 0.15319(3) 0.0472(2) Uani 1 1 d . . . S1 S 0.26676(9) 0.97887(10) 0.22325(6) 0.0561(4) Uani 1 1 d . . . S2 S 0.09566(10) 0.62623(12) 0.11362(7) 0.0712(5) Uani 1 1 d . . . S3 S 0.11837(8) 0.95197(10) 0.16062(6) 0.0553(4) Uani 1 1 d . . . S4 S 0.07813(10) 0.73929(12) 0.20727(7) 0.0735(5) Uani 1 1 d . . . S5 S 0.33092(9) 0.60725(10) 0.24579(6) 0.0551(4) Uani 1 1 d . . . S6 S 0.34031(9) 0.82305(12) 0.03907(6) 0.0582(4) Uani 1 1 d . . . S7 S 0.45039(8) 0.72293(11) 0.18982(5) 0.0530(4) Uani 1 1 d . . . S8 S 0.38707(9) 0.63204(11) 0.08392(6) 0.0564(4) Uani 1 1 d . . . O1 O 0.3570(2) 0.9541(3) 0.21854(16) 0.0679(11) Uani 1 1 d . . . O2 O 0.2404(3) 1.0869(3) 0.22025(17) 0.0752(12) Uani 1 1 d . . . O3 O 0.1645(3) 0.5912(3) 0.07996(19) 0.0894(14) Uani 1 1 d . . . O4 O 0.0453(3) 0.5493(3) 0.1407(2) 0.0969(15) Uani 1 1 d . . . O5 O 0.2396(2) 0.6089(3) 0.25569(16) 0.0710(11) Uani 1 1 d . . . O6 O 0.3902(3) 0.6192(3) 0.29062(14) 0.0703(11) Uani 1 1 d . . . O7 O 0.2771(2) 0.9032(3) 0.04786(16) 0.0754(12) Uani 1 1 d . . . O8 O 0.3408(2) 0.7705(3) -0.01222(14) 0.0738(11) Uani 1 1 d . . . N1 N 0.2179(2) 0.9095(3) 0.17637(16) 0.0474(10) Uani 1 1 d . . . N2 N 0.1405(3) 0.7066(3) 0.15581(19) 0.0575(12) Uani 1 1 d . . . N3 N -0.0268(3) 0.9032(4) 0.2092(2) 0.0677(13) Uani 1 1 d . . . N4 N 0.3457(2) 0.6990(3) 0.20132(16) 0.0463(10) Uani 1 1 d . . . N5 N 0.3259(2) 0.7403(3) 0.08817(16) 0.0489(10) Uani 1 1 d . . . N6 N 0.5484(3) 0.6189(4) 0.12254(19) 0.0635(12) Uani 1 1 d . . . C1 C 0.2324(3) 0.9298(4) 0.2850(2) 0.0525(13) Uani 1 1 d . . . C2 C 0.1575(4) 0.9665(5) 0.3082(3) 0.0754(18) Uani 1 1 d . . . H2 H 0.1257 1.0219 0.2918 0.090 Uiso 1 1 calc R . . C3 C 0.1295(4) 0.9223(6) 0.3553(3) 0.090(2) Uani 1 1 d . . . H3 H 0.0774 0.9469 0.3703 0.108 Uiso 1 1 calc R . . C4 C 0.1750(4) 0.8434(6) 0.3813(3) 0.0772(18) Uani 1 1 d . . . C5 C 0.2503(4) 0.8088(5) 0.3588(2) 0.0672(16) Uani 1 1 d . . . H5 H 0.2835 0.7559 0.3765 0.081 Uiso 1 1 calc R . . C6 C 0.2779(4) 0.8502(4) 0.3109(2) 0.0613(15) Uani 1 1 d . . . H6 H 0.3290 0.8238 0.2955 0.074 Uiso 1 1 calc R . . C7 C 0.1437(5) 0.7954(8) 0.4327(3) 0.129(3) Uani 1 1 d . . . H7A H 0.1802 0.7353 0.4425 0.155 Uiso 1 1 calc R . . H7B H 0.0839 0.7719 0.4276 0.155 Uiso 1 1 calc R . . H7C H 0.1467 0.8478 0.4615 0.155 Uiso 1 1 calc R . . C8 C 0.0234(4) 0.7017(6) 0.0732(3) 0.0821(19) Uani 1 1 d . . . C9 C 0.0521(5) 0.7875(5) 0.0471(3) 0.0845(19) Uani 1 1 d . . . H9 H 0.1101 0.8101 0.0522 0.101 Uiso 1 1 calc R . . C10 C -0.0032(6) 0.8425(6) 0.0129(3) 0.101(2) Uani 1 1 d . . . H10 H 0.0188 0.9002 -0.0068 0.122 Uiso 1 1 calc R . . C11 C -0.0854(6) 0.8176(9) 0.0066(4) 0.143(4) Uani 1 1 d . . . C12 C -0.1142(6) 0.7367(12) 0.0342(6) 0.244(9) Uani 1 1 d . . . H12 H -0.1734 0.7181 0.0304 0.292 Uiso 1 1 calc R . . C13 C -0.0612(6) 0.6769(10) 0.0690(5) 0.205(7) Uani 1 1 d . . . H13 H -0.0842 0.6204 0.0890 0.246 Uiso 1 1 calc R . . C14 C -0.1456(6) 0.8737(11) -0.0350(5) 0.225(7) Uani 1 1 d . . . H14A H -0.1697 0.9371 -0.0189 0.270 Uiso 1 1 calc R . . H14B H -0.1926 0.8263 -0.0459 0.270 Uiso 1 1 calc R . . H14C H -0.1124 0.8931 -0.0666 0.270 Uiso 1 1 calc R . . C15 C 0.0485(3) 0.8678(4) 0.1943(2) 0.0574(14) Uani 1 1 d . . . C16 C -0.0484(4) 1.0150(5) 0.2099(3) 0.0772(18) Uani 1 1 d . . . H16A H 0.0045 1.0561 0.2179 0.093 Uiso 1 1 calc R . . H16B H -0.0896 1.0284 0.2390 0.093 Uiso 1 1 calc R . . C17 C -0.0873(5) 1.0514(7) 0.1578(4) 0.120(3) Uani 1 1 d . . . H17A H -0.0423 1.0556 0.1308 0.144 Uiso 1 1 calc R . . H17B H -0.1132 1.1208 0.1626 0.144 Uiso 1 1 calc R . . H17C H -0.1319 1.0016 0.1458 0.144 Uiso 1 1 calc R . . C18 C -0.0958(4) 0.8302(6) 0.2286(4) 0.100(3) Uani 1 1 d . . . H18A H -0.0927 0.7634 0.2084 0.120 Uiso 1 1 calc R . . H18B H -0.1531 0.8619 0.2210 0.120 Uiso 1 1 calc R . . C19 C -0.0868(5) 0.8076(6) 0.2879(4) 0.119(3) Uani 1 1 d . . . H19A H -0.0354 0.7643 0.2946 0.143 Uiso 1 1 calc R . . H19B H -0.1381 0.7700 0.2999 0.143 Uiso 1 1 calc R . . H19C H -0.0810 0.8738 0.3076 0.143 Uiso 1 1 calc R . . C20 C 0.3549(3) 0.4877(4) 0.2143(2) 0.0549(13) Uani 1 1 d . . . C21 C 0.2949(4) 0.4441(5) 0.1797(3) 0.0782(18) Uani 1 1 d . . . H21 H 0.2410 0.4779 0.1734 0.094 Uiso 1 1 calc R . . C22 C 0.3133(5) 0.3503(5) 0.1539(3) 0.088(2) Uani 1 1 d . . . H22 H 0.2713 0.3202 0.1302 0.105 Uiso 1 1 calc R . . C23 C 0.3905(5) 0.3003(5) 0.1617(3) 0.0765(18) Uani 1 1 d . . . C24 C 0.4510(4) 0.3461(5) 0.1959(3) 0.0756(18) Uani 1 1 d . . . H24 H 0.5055 0.3130 0.2011 0.091 Uiso 1 1 calc R . . C25 C 0.4343(4) 0.4390(5) 0.2229(2) 0.0656(16) Uani 1 1 d . . . H25 H 0.4763 0.4688 0.2467 0.079 Uiso 1 1 calc R . . C26 C 0.4120(6) 0.1975(5) 0.1339(3) 0.117(3) Uani 1 1 d . . . H26A H 0.3598 0.1693 0.1163 0.140 Uiso 1 1 calc R . . H26B H 0.4340 0.1470 0.1605 0.140 Uiso 1 1 calc R . . H26C H 0.4560 0.2101 0.1070 0.140 Uiso 1 1 calc R . . C27 C 0.4452(3) 0.8742(4) 0.0502(2) 0.0520(13) Uani 1 1 d . . . C28 C 0.5097(4) 0.8528(4) 0.0149(2) 0.0627(15) Uani 1 1 d . . . H28 H 0.4980 0.8136 -0.0169 0.075 Uiso 1 1 calc R . . C29 C 0.5924(4) 0.8897(5) 0.0266(3) 0.0737(17) Uani 1 1 d . . . H29 H 0.6374 0.8754 0.0023 0.088 Uiso 1 1 calc R . . C30 C 0.6110(4) 0.9470(4) 0.0730(2) 0.0646(15) Uani 1 1 d . . . C31 C 0.5440(4) 0.9683(4) 0.1068(2) 0.0655(15) Uani 1 1 d . . . H31 H 0.5549 1.0087 0.1382 0.079 Uiso 1 1 calc R . . C32 C 0.4613(4) 0.9324(4) 0.0960(2) 0.0615(15) Uani 1 1 d . . . H32 H 0.4161 0.9477 0.1200 0.074 Uiso 1 1 calc R . . C33 C 0.7018(4) 0.9855(6) 0.0853(3) 0.091(2) Uani 1 1 d . . . H33A H 0.7036 1.0190 0.1207 0.110 Uiso 1 1 calc R . . H33B H 0.7185 1.0365 0.0580 0.110 Uiso 1 1 calc R . . H33C H 0.7418 0.9260 0.0851 0.110 Uiso 1 1 calc R . . C34 C 0.4706(3) 0.6545(4) 0.1312(2) 0.0503(13) Uani 1 1 d . . . C35 C 0.6173(4) 0.6196(5) 0.1652(3) 0.0730(17) Uani 1 1 d . . . H35A H 0.6569 0.5598 0.1593 0.088 Uiso 1 1 calc R . . H35B H 0.5907 0.6099 0.2006 0.088 Uiso 1 1 calc R . . C36 C 0.6683(4) 0.7196(6) 0.1657(3) 0.109(3) Uani 1 1 d . . . H36A H 0.6964 0.7283 0.1311 0.131 Uiso 1 1 calc R . . H36B H 0.7121 0.7168 0.1945 0.131 Uiso 1 1 calc R . . H36C H 0.6295 0.7790 0.1717 0.131 Uiso 1 1 calc R . . C37 C 0.5728(4) 0.5728(6) 0.0706(3) 0.091(2) Uani 1 1 d . . . H37A H 0.6350 0.5848 0.0650 0.109 Uiso 1 1 calc R . . H37B H 0.5402 0.6082 0.0412 0.109 Uiso 1 1 calc R . . C38 C 0.5543(6) 0.4554(6) 0.0687(3) 0.121(3) Uani 1 1 d . . . H38A H 0.5835 0.4208 0.0992 0.145 Uiso 1 1 calc R . . H38B H 0.5755 0.4262 0.0351 0.145 Uiso 1 1 calc R . . H38C H 0.4919 0.4437 0.0706 0.145 Uiso 1 1 calc R . . O1S O 0.2511(13) 0.9954(16) 0.4915(8) 0.104(6) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0366(4) 0.0472(4) 0.0580(4) -0.0013(3) 0.0029(3) 0.0032(3) S1 0.0487(8) 0.0493(8) 0.0702(9) -0.0086(7) 0.0005(7) -0.0037(6) S2 0.0518(9) 0.0545(9) 0.1065(13) -0.0031(9) -0.0159(9) -0.0052(7) S3 0.0451(8) 0.0512(8) 0.0694(9) 0.0047(7) -0.0017(7) 0.0078(6) S4 0.0608(10) 0.0566(9) 0.1042(13) 0.0089(8) 0.0317(9) 0.0035(7) S5 0.0525(9) 0.0549(8) 0.0583(9) 0.0081(7) 0.0098(7) 0.0063(6) S6 0.0501(8) 0.0728(9) 0.0517(8) 0.0064(7) -0.0015(6) 0.0098(7) S7 0.0420(7) 0.0604(8) 0.0565(8) -0.0013(7) 0.0002(6) -0.0011(6) S8 0.0535(8) 0.0579(8) 0.0579(8) -0.0081(7) 0.0003(6) 0.0095(7) O1 0.041(2) 0.080(3) 0.083(3) -0.007(2) 0.0025(19) -0.0097(19) O2 0.086(3) 0.045(2) 0.094(3) -0.010(2) -0.003(2) -0.002(2) O3 0.072(3) 0.079(3) 0.117(4) -0.044(3) -0.017(3) 0.014(2) O4 0.080(3) 0.071(3) 0.139(4) 0.022(3) -0.024(3) -0.032(2) O5 0.054(2) 0.071(3) 0.090(3) 0.014(2) 0.029(2) 0.0109(19) O6 0.080(3) 0.078(3) 0.053(2) 0.0072(19) -0.006(2) 0.007(2) O7 0.061(3) 0.087(3) 0.079(3) 0.020(2) 0.002(2) 0.031(2) O8 0.069(3) 0.106(3) 0.046(2) -0.008(2) -0.0085(19) 0.000(2) N1 0.035(2) 0.050(2) 0.057(3) -0.004(2) -0.0059(19) 0.0010(18) N2 0.035(2) 0.054(3) 0.084(3) -0.011(2) 0.007(2) -0.0027(19) N3 0.037(3) 0.067(3) 0.099(4) -0.018(3) 0.007(2) 0.007(2) N4 0.036(2) 0.049(2) 0.055(3) 0.0036(19) 0.0071(19) 0.0020(18) N5 0.041(2) 0.055(3) 0.051(2) 0.002(2) 0.0035(19) 0.0060(19) N6 0.050(3) 0.071(3) 0.070(3) 0.016(2) 0.010(2) 0.023(2) C1 0.042(3) 0.058(3) 0.057(3) -0.009(3) -0.003(2) 0.005(3) C2 0.062(4) 0.098(5) 0.067(4) -0.008(4) -0.001(3) 0.030(3) C3 0.062(4) 0.136(6) 0.072(5) -0.008(4) 0.012(4) 0.029(4) C4 0.061(4) 0.104(5) 0.067(4) -0.007(4) 0.000(3) 0.007(4) C5 0.061(4) 0.080(4) 0.061(4) -0.002(3) 0.004(3) 0.010(3) C6 0.049(3) 0.063(4) 0.071(4) -0.014(3) 0.003(3) 0.005(3) C7 0.109(7) 0.197(10) 0.082(6) 0.020(6) 0.033(5) 0.018(6) C8 0.047(4) 0.095(5) 0.104(5) 0.017(4) -0.008(3) -0.002(3) C9 0.089(5) 0.082(5) 0.082(5) 0.001(4) 0.004(4) 0.007(4) C10 0.122(7) 0.108(6) 0.075(5) 0.006(4) 0.017(5) 0.025(5) C11 0.081(7) 0.184(10) 0.164(9) 0.081(8) 0.020(6) 0.037(7) C12 0.070(6) 0.313(17) 0.345(19) 0.223(16) -0.056(9) -0.024(8) C13 0.077(6) 0.248(13) 0.287(15) 0.172(12) -0.077(8) -0.051(7) C14 0.120(8) 0.353(19) 0.201(12) 0.162(13) 0.009(8) 0.094(10) C15 0.047(3) 0.057(3) 0.068(4) -0.005(3) 0.001(3) 0.002(3) C16 0.061(4) 0.076(4) 0.094(5) -0.011(4) 0.008(3) 0.024(3) C17 0.073(5) 0.132(7) 0.155(8) 0.008(6) -0.015(5) 0.041(5) C18 0.049(4) 0.093(5) 0.160(8) -0.032(5) 0.033(4) -0.007(4) C19 0.100(6) 0.104(6) 0.156(8) -0.004(6) 0.063(6) -0.013(5) C20 0.050(3) 0.048(3) 0.067(4) 0.011(3) 0.009(3) 0.002(3) C21 0.051(4) 0.069(4) 0.115(5) -0.006(4) -0.002(4) 0.005(3) C22 0.077(5) 0.069(4) 0.116(6) -0.016(4) -0.002(4) -0.002(4) C23 0.091(5) 0.053(4) 0.087(5) 0.001(3) 0.023(4) 0.011(4) C24 0.080(5) 0.072(4) 0.076(4) 0.014(4) 0.017(4) 0.029(4) C25 0.062(4) 0.071(4) 0.064(4) 0.009(3) 0.000(3) 0.012(3) C26 0.168(8) 0.067(4) 0.117(6) -0.010(4) 0.034(6) 0.017(5) C27 0.058(3) 0.050(3) 0.048(3) 0.008(2) -0.001(3) 0.001(3) C28 0.060(4) 0.075(4) 0.053(3) -0.006(3) 0.011(3) -0.004(3) C29 0.062(4) 0.087(5) 0.073(4) 0.006(4) 0.015(3) -0.002(3) C30 0.070(4) 0.055(3) 0.068(4) 0.010(3) -0.008(3) -0.007(3) C31 0.076(4) 0.057(3) 0.064(4) -0.010(3) 0.001(3) -0.009(3) C32 0.076(4) 0.052(3) 0.057(4) 0.003(3) 0.009(3) 0.007(3) C33 0.081(5) 0.098(5) 0.094(5) 0.015(4) -0.016(4) -0.027(4) C34 0.040(3) 0.044(3) 0.067(3) 0.013(2) 0.004(2) 0.008(2) C35 0.048(4) 0.086(4) 0.085(4) 0.026(4) 0.002(3) 0.019(3) C36 0.065(5) 0.126(6) 0.136(7) 0.046(5) -0.018(4) -0.012(4) C37 0.072(4) 0.120(6) 0.082(5) 0.005(4) 0.021(4) 0.035(4) C38 0.151(8) 0.120(7) 0.091(6) -0.020(5) 0.004(5) 0.067(6) _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 N5 1.979(4) . ? Co1 N2 1.985(4) . ? Co1 N4 1.992(4) . ? Co1 N1 2.003(4) . ? S1 O2 1.437(4) . ? S1 O1 1.440(4) . ? S1 N1 1.637(4) . ? S1 C1 1.753(6) . ? S2 O4 1.431(4) . ? S2 O3 1.441(4) . ? S2 N2 1.615(4) . ? S2 C8 1.773(7) . ? S3 N1 1.673(4) . ? S3 C15 1.751(6) . ? S4 N2 1.674(4) . ? S4 C15 1.729(5) . ? S5 O6 1.440(4) . ? S5 O5 1.442(4) . ? S5 N4 1.630(4) . ? S5 C20 1.756(5) . ? S6 O7 1.435(4) . ? S6 O8 1.443(4) . ? S6 N5 1.633(4) . ? S6 C27 1.767(5) . ? S7 N4 1.681(4) . ? S7 C34 1.735(5) . ? S8 N5 1.678(4) . ? S8 C34 1.755(5) . ? N3 C15 1.311(6) . ? N3 C16 1.464(7) . ? N3 C18 1.504(8) . ? N6 C34 1.309(6) . ? N6 C37 1.477(7) . ? N6 C35 1.490(7) . ? C1 C6 1.387(7) . ? C1 C2 1.389(7) . ? C2 C3 1.379(9) . ? C3 C4 1.381(9) . ? C4 C5 1.376(8) . ? C4 C7 1.511(9) . ? C5 C6 1.381(8) . ? C8 C13 1.350(10) . ? C8 C9 1.353(9) . ? C9 C10 1.387(9) . ? C10 C11 1.319(11) . ? C11 C12 1.323(13) . ? C11 C14 1.554(11) . ? C12 C13 1.406(12) . ? C16 C17 1.493(9) . ? C18 C19 1.509(11) . ? C20 C21 1.372(8) . ? C20 C25 1.391(7) . ? C21 C22 1.390(8) . ? C22 C23 1.366(9) . ? C23 C24 1.382(9) . ? C23 C26 1.522(8) . ? C24 C25 1.388(8) . ? C27 C28 1.373(7) . ? C27 C32 1.380(7) . ? C28 C29 1.390(8) . ? C29 C30 1.392(8) . ? C30 C31 1.378(8) . ? C30 C33 1.515(8) . ? C31 C32 1.380(8) . ? C35 C36 1.498(9) . ? C37 C38 1.524(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Co1 N2 117.51(17) . . ? N5 Co1 N4 92.90(16) . . ? N2 Co1 N4 115.02(17) . . ? N5 Co1 N1 124.63(17) . . ? N2 Co1 N1 92.89(16) . . ? N4 Co1 N1 115.78(16) . . ? O2 S1 O1 118.7(2) . . ? O2 S1 N1 110.7(2) . . ? O1 S1 N1 105.0(2) . . ? O2 S1 C1 107.2(3) . . ? O1 S1 C1 107.9(2) . . ? N1 S1 C1 106.8(2) . . ? O4 S2 O3 118.7(3) . . ? O4 S2 N2 111.0(3) . . ? O3 S2 N2 105.2(2) . . ? O4 S2 C8 107.2(3) . . ? O3 S2 C8 107.7(3) . . ? N2 S2 C8 106.5(3) . . ? N1 S3 C15 105.4(2) . . ? N2 S4 C15 104.4(2) . . ? O6 S5 O5 118.6(2) . . ? O6 S5 N4 110.8(2) . . ? O5 S5 N4 105.0(2) . . ? O6 S5 C20 107.5(3) . . ? O5 S5 C20 107.8(3) . . ? N4 S5 C20 106.5(2) . . ? O7 S6 O8 118.8(2) . . ? O7 S6 N5 103.9(2) . . ? O8 S6 N5 111.6(2) . . ? O7 S6 C27 110.0(3) . . ? O8 S6 C27 106.7(2) . . ? N5 S6 C27 105.0(2) . . ? N4 S7 C34 104.1(2) . . ? N5 S8 C34 103.5(2) . . ? S1 N1 S3 113.8(2) . . ? S1 N1 Co1 123.4(2) . . ? S3 N1 Co1 121.1(2) . . ? S2 N2 S4 114.1(2) . . ? S2 N2 Co1 127.6(3) . . ? S4 N2 Co1 118.3(2) . . ? C15 N3 C16 122.9(5) . . ? C15 N3 C18 121.4(5) . . ? C16 N3 C18 115.7(5) . . ? S5 N4 S7 113.3(2) . . ? S5 N4 Co1 128.3(2) . . ? S7 N4 Co1 117.7(2) . . ? S6 N5 S8 113.4(2) . . ? S6 N5 Co1 125.7(2) . . ? S8 N5 Co1 120.3(2) . . ? C34 N6 C37 122.4(5) . . ? C34 N6 C35 121.9(5) . . ? C37 N6 C35 115.7(5) . . ? C6 C1 C2 118.1(5) . . ? C6 C1 S1 120.6(4) . . ? C2 C1 S1 121.2(4) . . ? C3 C2 C1 119.9(6) . . ? C2 C3 C4 121.9(6) . . ? C5 C4 C3 118.2(6) . . ? C5 C4 C7 120.3(7) . . ? C3 C4 C7 121.4(6) . . ? C4 C5 C6 120.5(6) . . ? C5 C6 C1 121.3(5) . . ? C13 C8 C9 118.7(7) . . ? C13 C8 S2 121.2(6) . . ? C9 C8 S2 120.1(5) . . ? C8 C9 C10 119.9(7) . . ? C11 C10 C9 122.3(8) . . ? C10 C11 C12 117.5(9) . . ? C10 C11 C14 122.2(10) . . ? C12 C11 C14 120.1(10) . . ? C11 C12 C13 122.9(9) . . ? C8 C13 C12 118.4(9) . . ? N3 C15 S4 120.5(4) . . ? N3 C15 S3 119.2(4) . . ? S4 C15 S3 120.3(3) . . ? N3 C16 C17 112.3(6) . . ? N3 C18 C19 112.4(6) . . ? C21 C20 C25 120.1(5) . . ? C21 C20 S5 119.0(4) . . ? C25 C20 S5 120.9(5) . . ? C20 C21 C22 119.8(6) . . ? C23 C22 C21 121.4(7) . . ? C22 C23 C24 118.2(6) . . ? C22 C23 C26 122.3(7) . . ? C24 C23 C26 119.5(7) . . ? C23 C24 C25 121.8(6) . . ? C24 C25 C20 118.6(6) . . ? C28 C27 C32 121.0(5) . . ? C28 C27 S6 120.4(4) . . ? C32 C27 S6 118.6(4) . . ? C27 C28 C29 118.6(5) . . ? C28 C29 C30 121.7(6) . . ? C31 C30 C29 117.7(5) . . ? C31 C30 C33 121.4(6) . . ? C29 C30 C33 120.9(6) . . ? C30 C31 C32 121.7(5) . . ? C27 C32 C31 119.3(5) . . ? N6 C34 S7 119.7(4) . . ? N6 C34 S8 120.1(4) . . ? S7 C34 S8 120.2(3) . . ? N6 C35 C36 112.4(5) . . ? N6 C37 C38 111.5(6) . . ? 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 O2 S1 N1 S3 -32.3(3) . . . . ? O1 S1 N1 S3 -161.6(3) . . . . ? C1 S1 N1 S3 84.0(3) . . . . ? O2 S1 N1 Co1 162.7(3) . . . . ? O1 S1 N1 Co1 33.4(3) . . . . ? C1 S1 N1 Co1 -81.0(3) . . . . ? C15 S3 N1 S1 -100.6(3) . . . . ? C15 S3 N1 Co1 64.8(3) . . . . ? N5 Co1 N1 S1 -100.1(3) . . . . ? N2 Co1 N1 S1 133.2(3) . . . . ? N4 Co1 N1 S1 13.6(3) . . . . ? N5 Co1 N1 S3 95.9(3) . . . . ? N2 Co1 N1 S3 -30.7(3) . . . . ? N4 Co1 N1 S3 -150.4(2) . . . . ? O4 S2 N2 S4 -38.4(4) . . . . ? O3 S2 N2 S4 -168.0(3) . . . . ? C8 S2 N2 S4 77.9(4) . . . . ? O4 S2 N2 Co1 141.0(3) . . . . ? O3 S2 N2 Co1 11.4(4) . . . . ? C8 S2 N2 Co1 -102.7(4) . . . . ? C15 S4 N2 S2 -107.7(3) . . . . ? C15 S4 N2 Co1 72.7(3) . . . . ? N5 Co1 N2 S2 7.1(4) . . . . ? N4 Co1 N2 S2 -100.7(3) . . . . ? N1 Co1 N2 S2 139.0(3) . . . . ? N5 Co1 N2 S4 -173.5(2) . . . . ? N4 Co1 N2 S4 78.7(3) . . . . ? N1 Co1 N2 S4 -41.6(3) . . . . ? O6 S5 N4 S7 42.8(3) . . . . ? O5 S5 N4 S7 171.9(2) . . . . ? C20 S5 N4 S7 -73.8(3) . . . . ? O6 S5 N4 Co1 -147.1(3) . . . . ? O5 S5 N4 Co1 -17.9(4) . . . . ? C20 S5 N4 Co1 96.3(3) . . . . ? C34 S7 N4 S5 99.4(3) . . . . ? C34 S7 N4 Co1 -71.9(3) . . . . ? N5 Co1 N4 S5 -128.2(3) . . . . ? N2 Co1 N4 S5 -5.9(4) . . . . ? N1 Co1 N4 S5 100.8(3) . . . . ? N5 Co1 N4 S7 41.6(2) . . . . ? N2 Co1 N4 S7 163.9(2) . . . . ? N1 Co1 N4 S7 -89.4(3) . . . . ? O7 S6 N5 S8 174.8(3) . . . . ? O8 S6 N5 S8 45.6(3) . . . . ? C27 S6 N5 S8 -69.6(3) . . . . ? O7 S6 N5 Co1 -14.1(3) . . . . ? O8 S6 N5 Co1 -143.2(3) . . . . ? C27 S6 N5 Co1 101.5(3) . . . . ? C34 S8 N5 S6 102.6(3) . . . . ? C34 S8 N5 Co1 -69.1(3) . . . . ? N2 Co1 N5 S6 101.8(3) . . . . ? N4 Co1 N5 S6 -137.9(3) . . . . ? N1 Co1 N5 S6 -13.6(4) . . . . ? N2 Co1 N5 S8 -87.6(3) . . . . ? N4 Co1 N5 S8 32.6(3) . . . . ? N1 Co1 N5 S8 157.0(2) . . . . ? O2 S1 C1 C6 -150.4(4) . . . . ? O1 S1 C1 C6 -21.4(5) . . . . ? N1 S1 C1 C6 91.0(5) . . . . ? O2 S1 C1 C2 32.0(5) . . . . ? O1 S1 C1 C2 161.0(5) . . . . ? N1 S1 C1 C2 -86.6(5) . . . . ? C6 C1 C2 C3 -1.3(9) . . . . ? S1 C1 C2 C3 176.4(5) . . . . ? C1 C2 C3 C4 1.6(10) . . . . ? C2 C3 C4 C5 -0.1(10) . . . . ? C2 C3 C4 C7 -179.9(7) . . . . ? C3 C4 C5 C6 -1.7(9) . . . . ? C7 C4 C5 C6 178.1(7) . . . . ? C4 C5 C6 C1 2.0(9) . . . . ? C2 C1 C6 C5 -0.5(8) . . . . ? S1 C1 C6 C5 -178.2(4) . . . . ? O4 S2 C8 C13 -4.9(10) . . . . ? O3 S2 C8 C13 123.8(9) . . . . ? N2 S2 C8 C13 -123.8(9) . . . . ? O4 S2 C8 C9 173.2(6) . . . . ? O3 S2 C8 C9 -58.0(7) . . . . ? N2 S2 C8 C9 54.4(7) . . . . ? C13 C8 C9 C10 -5.8(13) . . . . ? S2 C8 C9 C10 175.9(5) . . . . ? C8 C9 C10 C11 3.6(12) . . . . ? C9 C10 C11 C12 -0.3(18) . . . . ? C9 C10 C11 C14 -175.1(9) . . . . ? C10 C11 C12 C13 -1(2) . . . . ? C14 C11 C12 C13 174.3(14) . . . . ? C9 C8 C13 C12 4.9(18) . . . . ? S2 C8 C13 C12 -176.9(11) . . . . ? C11 C12 C13 C8 -2(3) . . . . ? C16 N3 C15 S4 166.7(5) . . . . ? C18 N3 C15 S4 -11.2(8) . . . . ? C16 N3 C15 S3 -14.0(8) . . . . ? C18 N3 C15 S3 168.2(5) . . . . ? N2 S4 C15 N3 147.9(4) . . . . ? N2 S4 C15 S3 -31.5(4) . . . . ? N1 S3 C15 N3 151.0(4) . . . . ? N1 S3 C15 S4 -29.6(4) . . . . ? C15 N3 C16 C17 90.0(7) . . . . ? C18 N3 C16 C17 -92.1(7) . . . . ? C15 N3 C18 C19 86.3(7) . . . . ? C16 N3 C18 C19 -91.8(7) . . . . ? O6 S5 C20 C21 163.1(5) . . . . ? O5 S5 C20 C21 34.1(5) . . . . ? N4 S5 C20 C21 -78.1(5) . . . . ? O6 S5 C20 C25 -18.9(5) . . . . ? O5 S5 C20 C25 -147.9(4) . . . . ? N4 S5 C20 C25 99.8(5) . . . . ? C25 C20 C21 C22 1.0(9) . . . . ? S5 C20 C21 C22 179.0(5) . . . . ? C20 C21 C22 C23 -0.6(10) . . . . ? C21 C22 C23 C24 -0.6(10) . . . . ? C21 C22 C23 C26 179.9(7) . . . . ? C22 C23 C24 C25 1.4(10) . . . . ? C26 C23 C24 C25 -179.1(6) . . . . ? C23 C24 C25 C20 -1.0(9) . . . . ? C21 C20 C25 C24 -0.3(8) . . . . ? S5 C20 C25 C24 -178.2(4) . . . . ? O7 S6 C27 C28 -135.1(4) . . . . ? O8 S6 C27 C28 -4.9(5) . . . . ? N5 S6 C27 C28 113.6(4) . . . . ? O7 S6 C27 C32 47.2(5) . . . . ? O8 S6 C27 C32 177.4(4) . . . . ? N5 S6 C27 C32 -64.0(4) . . . . ? C32 C27 C28 C29 1.0(8) . . . . ? S6 C27 C28 C29 -176.6(4) . . . . ? C27 C28 C29 C30 0.2(9) . . . . ? C28 C29 C30 C31 -1.4(9) . . . . ? C28 C29 C30 C33 179.4(6) . . . . ? C29 C30 C31 C32 1.5(8) . . . . ? C33 C30 C31 C32 -179.3(5) . . . . ? C28 C27 C32 C31 -1.0(8) . . . . ? S6 C27 C32 C31 176.7(4) . . . . ? C30 C31 C32 C27 -0.3(8) . . . . ? C37 N6 C34 S7 -171.6(5) . . . . ? C35 N6 C34 S7 10.3(7) . . . . ? C37 N6 C34 S8 8.9(7) . . . . ? C35 N6 C34 S8 -169.2(4) . . . . ? N4 S7 C34 N6 -151.3(4) . . . . ? N4 S7 C34 S8 28.2(3) . . . . ? N5 S8 C34 N6 -146.4(4) . . . . ? N5 S8 C34 S7 34.1(3) . . . . ? C34 N6 C35 C36 -89.2(7) . . . . ? C37 N6 C35 C36 92.5(7) . . . . ? C34 N6 C37 C38 -88.2(7) . . . . ? C35 N6 C37 C38 90.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.602 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.065