# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email xiaodr98@yahoo.com.cn _publ_author_name 'Ming-Liang Tong' data_z1a _database_code_depnum_ccdc_archive 'CCDC 758887' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Co2 N4 O10 S' _chemical_formula_weight 828.56 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.5182(13) _cell_length_b 21.728(4) _cell_length_c 12.575(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.77(3) _cell_angle_gamma 90.00 _cell_volume 1755.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11645 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 28.44 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6114 _exptl_absorpt_correction_T_max 0.7758 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 11645 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.44 _reflns_number_total 6496 _reflns_number_gt 5563 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 0.014(11) _refine_ls_number_reflns 6496 _refine_ls_number_parameters 478 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 1.011 _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 -0.39326(6) 0.242672(19) -0.14328(3) 0.03042(11) Uani 1 1 d . . . Co2 Co -0.91599(6) 0.26786(2) -0.21282(3) 0.03307(11) Uani 1 1 d . . . S1 S -1.3126(2) 0.64438(5) -0.17049(7) 0.0543(3) Uani 1 1 d . . . O1 O -1.0262(4) 0.35176(12) -0.2235(2) 0.0487(7) Uani 1 1 d . . . O2 O -1.3335(4) 0.33555(12) -0.1731(2) 0.0459(6) Uani 1 1 d . . . O3 O -1.4897(4) 0.72734(14) -0.6917(2) 0.0533(8) Uani 1 1 d . . . O4 O -1.1525(4) 0.74794(15) -0.64754(19) 0.0550(7) Uani 1 1 d . . . O5 O -1.1279(6) 0.66853(15) -0.1045(2) 0.0804(11) Uani 1 1 d . . . O6 O -1.5123(6) 0.65357(14) -0.1398(2) 0.0752(11) Uani 1 1 d . . . O7 O -0.6678(3) 0.26893(12) -0.10262(16) 0.0354(5) Uani 1 1 d . . . O8 O -0.8367(5) 0.30972(17) 0.0177(3) 0.0722(10) Uani 1 1 d . . . O9 O -0.1138(3) 0.20958(11) -0.16987(19) 0.0372(5) Uani 1 1 d . . . O10 O 0.1062(4) 0.13140(13) -0.1571(2) 0.0535(7) Uani 1 1 d . . . N1 N 0.0720(7) 0.4046(2) 0.2563(5) 0.0959(17) Uani 1 1 d . . . H1B H 0.1976 0.4183 0.2654 0.115 Uiso 1 1 calc R . . N2 N -0.3024(4) 0.26160(13) 0.0269(2) 0.0376(6) Uani 1 1 d . . . H2B H -0.2779 0.2259 0.0633 0.045 Uiso 1 1 calc R . . H2C H -0.1841 0.2838 0.0377 0.045 Uiso 1 1 calc R . . N3 N -0.5998(5) -0.00023(18) -0.3709(3) 0.0596(10) Uani 1 1 d . . . H3A H -0.7185 -0.0146 -0.4011 0.072 Uiso 1 1 calc R . . N4 N -0.4273(4) 0.14608(13) -0.1189(3) 0.0392(7) Uani 1 1 d . . . H4B H -0.4936 0.1399 -0.0625 0.047 Uiso 1 1 calc R . . H4C H -0.5051 0.1294 -0.1778 0.047 Uiso 1 1 calc R . . C1 C -1.4378(6) 0.52437(19) -0.1646(3) 0.0486(10) Uani 1 1 d . . . H1A H -1.5616 0.5403 -0.1489 0.058 Uiso 1 1 calc R . . C2 C -1.4135(6) 0.46114(18) -0.1710(3) 0.0464(9) Uani 1 1 d . . . H2A H -1.5209 0.4348 -0.1608 0.056 Uiso 1 1 calc R . . C3 C -1.2276(6) 0.43785(16) -0.1928(3) 0.0365(8) Uani 1 1 d . . . C4 C -1.0699(7) 0.47805(18) -0.2088(4) 0.0529(11) Uani 1 1 d . . . H4A H -0.9447 0.4624 -0.2231 0.063 Uiso 1 1 calc R . . C5 C -1.0964(7) 0.54077(19) -0.2038(4) 0.0574(11) Uani 1 1 d . . . H5A H -0.9908 0.5674 -0.2155 0.069 Uiso 1 1 calc R . . C6 C -1.2818(6) 0.56363(17) -0.1810(3) 0.0423(9) Uani 1 1 d . . . C7 C -1.3221(6) 0.67215(17) -0.3031(3) 0.0430(9) Uani 1 1 d . . . C8 C -1.5017(7) 0.66714(19) -0.3778(3) 0.0494(10) Uani 1 1 d . . . H8A H -1.6216 0.6511 -0.3575 0.059 Uiso 1 1 calc R . . C9 C -1.5038(6) 0.68586(18) -0.4828(3) 0.0448(9) Uani 1 1 d . . . H9A H -1.6247 0.6822 -0.5336 0.054 Uiso 1 1 calc R . . C10 C -1.3254(5) 0.71003(16) -0.5119(3) 0.0355(7) Uani 1 1 d . . . C11 C -1.1477(6) 0.7169(2) -0.4352(3) 0.0494(10) Uani 1 1 d . . . H11A H -1.0296 0.7346 -0.4548 0.059 Uiso 1 1 calc R . . C12 C -1.1432(7) 0.6978(2) -0.3308(3) 0.0511(10) Uani 1 1 d . . . H12A H -1.0230 0.7021 -0.2796 0.061 Uiso 1 1 calc R . . C13 C -1.1948(6) 0.36923(17) -0.1969(3) 0.0376(8) Uani 1 1 d . . . C14 C -1.3252(5) 0.73021(16) -0.6268(3) 0.0361(8) Uani 1 1 d . . . C15 C -0.0274(11) 0.3858(2) 0.3370(5) 0.0851(19) Uani 1 1 d . . . C16 C 0.0261(13) 0.3872(4) 0.4446(6) 0.117(3) Uani 1 1 d U . . H16A H 0.1560 0.4014 0.4775 0.140 Uiso 1 1 calc R . . C17 C -0.1168(14) 0.3672(3) 0.5038(5) 0.103(2) Uani 1 1 d U . . H17A H -0.0785 0.3675 0.5785 0.123 Uiso 1 1 calc R . . C18 C -0.3191(14) 0.3458(3) 0.4610(6) 0.109(2) Uani 1 1 d U . . H18A H -0.4095 0.3327 0.5062 0.131 Uiso 1 1 calc R . . C19 C -0.3809(10) 0.3450(2) 0.3457(4) 0.0751(16) Uani 1 1 d . . . H19A H -0.5117 0.3315 0.3127 0.090 Uiso 1 1 calc R . . C20 C -0.2344(7) 0.36543(18) 0.2875(3) 0.0508(10) Uani 1 1 d . . . C21 C -0.2367(6) 0.37469(17) 0.1740(3) 0.0467(9) Uani 1 1 d . . . C22 C -0.0510(9) 0.3990(2) 0.1617(5) 0.0798(17) Uani 1 1 d . . . H22A H -0.0150 0.4102 0.0959 0.096 Uiso 1 1 calc R . . C23 C -0.4160(7) 0.36391(18) 0.0870(3) 0.0487(10) Uani 1 1 d . . . H23A H -0.3856 0.3816 0.0205 0.058 Uiso 1 1 calc R . . H23B H -0.5367 0.3851 0.1048 0.058 Uiso 1 1 calc R . . C24 C -0.4690(6) 0.29617(17) 0.0683(3) 0.0393(8) Uani 1 1 d . . . H24A H -0.4867 0.2780 0.1374 0.047 Uiso 1 1 calc R . . C25 C -0.6760(6) 0.29144(18) -0.0086(3) 0.0432(9) Uani 1 1 d . . . C26 C -0.4433(6) 0.01643(18) -0.4244(3) 0.0495(10) Uani 1 1 d . . . C27 C -0.4290(8) 0.0114(2) -0.5312(3) 0.0627(12) Uani 1 1 d . . . H27A H -0.5375 -0.0046 -0.5813 0.075 Uiso 1 1 calc R . . C28 C -0.2462(8) 0.0311(3) -0.5610(4) 0.0702(13) Uani 1 1 d . . . H28A H -0.2312 0.0282 -0.6331 0.084 Uiso 1 1 calc R . . C29 C -0.0837(7) 0.0550(2) -0.4871(4) 0.0658(12) Uani 1 1 d . . . H29A H 0.0363 0.0684 -0.5108 0.079 Uiso 1 1 calc R . . C30 C -0.0973(6) 0.0593(2) -0.3795(3) 0.0544(10) Uani 1 1 d . . . H30A H 0.0128 0.0752 -0.3304 0.065 Uiso 1 1 calc R . . C31 C -0.2789(6) 0.03941(16) -0.3449(3) 0.0419(8) Uani 1 1 d . . . C32 C -0.3447(6) 0.03367(16) -0.2414(3) 0.0401(8) Uani 1 1 d . . . C33 C -0.5407(6) 0.00915(19) -0.2615(3) 0.0517(10) Uani 1 1 d . . . H33A H -0.6218 0.0002 -0.2094 0.062 Uiso 1 1 calc R . . C34 C -0.2276(6) 0.04784(17) -0.1305(3) 0.0440(9) Uani 1 1 d . . . H34A H -0.0854 0.0336 -0.1263 0.053 Uiso 1 1 calc R . . H34B H -0.2896 0.0245 -0.0784 0.053 Uiso 1 1 calc R . . C35 C -0.2223(5) 0.11562(16) -0.0979(3) 0.0369(8) Uani 1 1 d . . . H35A H -0.1772 0.1165 -0.0195 0.044 Uiso 1 1 calc R . . C36 C -0.0613(5) 0.15266(16) -0.1460(3) 0.0359(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0277(2) 0.0328(2) 0.0315(2) -0.00663(18) 0.00722(16) 0.00007(18) Co2 0.0296(2) 0.0361(2) 0.0352(2) -0.00309(19) 0.01032(17) 0.00346(19) S1 0.1020(9) 0.0347(5) 0.0297(5) 0.0050(4) 0.0207(5) 0.0155(5) O1 0.0508(16) 0.0395(15) 0.0609(17) 0.0063(13) 0.0245(13) 0.0119(13) O2 0.0471(15) 0.0346(14) 0.0594(16) 0.0051(11) 0.0186(13) 0.0024(12) O3 0.0452(15) 0.080(2) 0.0333(14) 0.0152(13) 0.0035(11) -0.0093(14) O4 0.0478(14) 0.084(2) 0.0338(13) 0.0072(14) 0.0105(11) -0.0201(15) O5 0.147(3) 0.0521(19) 0.0325(16) -0.0020(13) -0.0135(18) -0.008(2) O6 0.130(3) 0.0491(19) 0.0613(19) 0.0165(15) 0.058(2) 0.0352(19) O7 0.0281(10) 0.0450(13) 0.0341(12) -0.0111(11) 0.0083(9) 0.0012(11) O8 0.0529(18) 0.105(3) 0.0618(19) -0.0268(18) 0.0175(16) 0.0221(17) O9 0.0302(12) 0.0353(13) 0.0474(14) -0.0034(10) 0.0104(10) 0.0001(10) O10 0.0327(13) 0.0481(17) 0.080(2) -0.0143(14) 0.0118(13) 0.0051(12) N1 0.058(3) 0.080(4) 0.147(5) -0.034(3) 0.009(3) -0.016(2) N2 0.0422(15) 0.0332(16) 0.0359(14) -0.0063(12) 0.0028(12) -0.0026(12) N3 0.052(2) 0.059(2) 0.064(2) -0.0117(18) -0.0013(18) -0.0184(18) N4 0.0352(15) 0.0368(16) 0.0486(18) -0.0120(13) 0.0157(13) -0.0040(13) C1 0.054(2) 0.045(2) 0.050(2) 0.0098(17) 0.0186(18) 0.0180(18) C2 0.051(2) 0.043(2) 0.049(2) 0.0108(17) 0.0201(18) 0.0092(17) C3 0.046(2) 0.0318(19) 0.0333(18) 0.0051(14) 0.0100(15) 0.0072(15) C4 0.049(2) 0.039(2) 0.079(3) 0.009(2) 0.032(2) 0.0114(18) C5 0.060(3) 0.040(2) 0.078(3) 0.008(2) 0.028(2) -0.0027(19) C6 0.065(2) 0.0336(19) 0.0299(18) 0.0067(14) 0.0136(17) 0.0129(17) C7 0.069(3) 0.0311(18) 0.0293(18) 0.0031(14) 0.0105(17) 0.0080(17) C8 0.059(2) 0.050(2) 0.044(2) 0.0074(18) 0.0209(19) -0.0043(19) C9 0.044(2) 0.052(2) 0.0370(19) 0.0103(16) 0.0042(16) -0.0047(17) C10 0.0416(19) 0.0341(18) 0.0318(17) 0.0034(14) 0.0096(14) 0.0000(14) C11 0.048(2) 0.060(3) 0.040(2) 0.0120(18) 0.0060(17) -0.0073(18) C12 0.054(2) 0.059(3) 0.037(2) 0.0073(18) -0.0023(17) -0.006(2) C13 0.048(2) 0.037(2) 0.0292(17) 0.0044(14) 0.0092(15) 0.0094(16) C14 0.0430(19) 0.035(2) 0.0310(17) 0.0034(13) 0.0081(15) -0.0002(15) C15 0.122(5) 0.046(3) 0.067(3) -0.027(2) -0.041(3) 0.011(3) C16 0.129(5) 0.093(5) 0.107(5) -0.029(4) -0.045(4) 0.016(4) C17 0.167(6) 0.067(4) 0.057(3) -0.002(3) -0.029(4) 0.013(4) C18 0.182(6) 0.060(3) 0.091(4) 0.007(3) 0.040(4) 0.001(4) C19 0.135(5) 0.047(3) 0.046(3) -0.004(2) 0.024(3) -0.007(3) C20 0.069(3) 0.0300(19) 0.046(2) -0.0081(16) -0.009(2) -0.0033(18) C21 0.054(2) 0.031(2) 0.059(3) -0.0156(17) 0.0209(19) -0.0091(17) C22 0.084(4) 0.054(3) 0.111(5) -0.032(3) 0.043(3) -0.025(3) C23 0.077(3) 0.035(2) 0.035(2) -0.0043(15) 0.0125(19) 0.0012(19) C24 0.050(2) 0.0389(19) 0.0295(18) -0.0076(14) 0.0082(15) 0.0022(16) C25 0.043(2) 0.043(2) 0.046(2) -0.0085(16) 0.0151(17) 0.0050(17) C26 0.051(2) 0.038(2) 0.056(3) -0.0073(18) 0.0021(19) 0.0032(18) C27 0.076(3) 0.060(3) 0.047(2) -0.014(2) -0.003(2) 0.004(2) C28 0.084(4) 0.083(4) 0.043(3) -0.005(2) 0.009(2) 0.009(3) C29 0.064(3) 0.080(3) 0.057(3) 0.001(2) 0.020(2) 0.001(3) C30 0.050(2) 0.057(3) 0.056(3) -0.006(2) 0.008(2) -0.002(2) C31 0.043(2) 0.0296(18) 0.053(2) -0.0050(15) 0.0070(17) 0.0027(15) C32 0.043(2) 0.0276(18) 0.049(2) -0.0052(15) 0.0088(17) 0.0033(15) C33 0.052(2) 0.042(2) 0.064(3) -0.0050(19) 0.019(2) -0.0099(18) C34 0.047(2) 0.033(2) 0.052(2) 0.0025(17) 0.0089(18) 0.0025(16) C35 0.0403(19) 0.0334(18) 0.0368(19) -0.0050(14) 0.0065(15) -0.0007(15) C36 0.0341(18) 0.0349(19) 0.0377(19) -0.0131(14) 0.0038(15) 0.0001(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 Co1 O7 2.025(2) . ? Co1 O9 2.038(2) . ? Co1 O2 2.101(3) 1_655 ? Co1 O3 2.112(3) 2_344 ? Co1 N4 2.138(3) . ? Co1 N2 2.161(3) . ? Co2 O4 1.933(2) 2_344 ? Co2 O7 1.943(2) . ? Co2 O1 1.956(3) . ? Co2 O9 1.948(2) 1_455 ? S1 O5 1.440(4) . ? S1 O6 1.433(4) . ? S1 C7 1.765(3) . ? S1 C6 1.774(4) . ? O1 C13 1.260(4) . ? O2 C13 1.238(4) . ? O2 Co1 2.101(3) 1_455 ? O3 C14 1.234(4) . ? O3 Co1 2.112(3) 2_354 ? O4 C14 1.258(4) . ? O4 Co2 1.933(2) 2_354 ? O7 C25 1.289(4) . ? O8 C25 1.218(4) . ? O9 C36 1.305(4) . ? O9 Co2 1.948(2) 1_655 ? O10 C36 1.215(4) . ? N1 C15 1.356(8) . ? N1 C22 1.323(7) . ? N1 H1B 0.8600 . ? N2 C24 1.485(4) . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? N3 C26 1.363(5) . ? N3 C33 1.379(5) . ? N3 H3A 0.8600 . ? N4 C35 1.474(4) . ? N4 H4B 0.9000 . ? N4 H4C 0.9000 . ? C1 C6 1.370(6) . ? C1 C2 1.387(5) . ? C1 H1A 0.9300 . ? C2 C3 1.383(5) . ? C2 H2A 0.9300 . ? C3 C4 1.390(5) . ? C3 C13 1.508(5) . ? C4 C5 1.376(6) . ? C4 H4A 0.9300 . ? C5 C6 1.380(6) . ? C5 H5A 0.9300 . ? C7 C12 1.389(5) . ? C7 C8 1.375(5) . ? C8 C9 1.379(5) . ? C8 H8A 0.9300 . ? C9 C10 1.381(5) . ? C9 H9A 0.9300 . ? C10 C11 1.383(5) . ? C10 C14 1.510(5) . ? C11 C12 1.373(5) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C15 C16 1.339(8) . ? C15 C20 1.455(7) . ? C16 C17 1.359(10) . ? C16 H16A 0.9300 . ? C17 C18 1.415(10) . ? C17 H17A 0.9300 . ? C18 C19 1.437(8) . ? C18 H18A 0.9300 . ? C19 C20 1.372(7) . ? C19 H19A 0.9300 . ? C20 C21 1.439(6) . ? C21 C22 1.353(6) . ? C21 C23 1.478(5) . ? C22 H22A 0.9300 . ? C23 C24 1.521(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.524(5) . ? C24 H24A 0.9800 . ? C26 C27 1.366(6) . ? C26 C31 1.426(5) . ? C27 C28 1.377(7) . ? C27 H27A 0.9300 . ? C28 C29 1.386(7) . ? C28 H28A 0.9300 . ? C29 C30 1.374(6) . ? C29 H29A 0.9300 . ? C30 C31 1.397(5) . ? C30 H30A 0.9300 . ? C31 C32 1.443(5) . ? C32 C33 1.368(5) . ? C32 C34 1.504(5) . ? C33 H33A 0.9300 . ? C34 C35 1.528(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.527(5) . ? C35 H35A 0.9800 . ? 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 O7 Co1 O9 173.55(10) . . ? O7 Co1 O2 88.47(10) . 1_655 ? O9 Co1 O2 96.40(10) . 1_655 ? O7 Co1 O3 96.04(10) . 2_344 ? O9 Co1 O3 88.11(10) . 2_344 ? O2 Co1 O3 91.31(11) 1_655 2_344 ? O7 Co1 N4 97.05(11) . . ? O9 Co1 N4 78.15(10) . . ? O2 Co1 N4 174.45(11) 1_655 . ? O3 Co1 N4 87.55(12) 2_344 . ? O7 Co1 N2 78.56(10) . . ? O9 Co1 N2 97.31(10) . . ? O2 Co1 N2 88.07(11) 1_655 . ? O3 Co1 N2 174.58(11) 2_344 . ? N4 Co1 N2 93.57(11) . . ? O4 Co2 O7 110.97(10) 2_344 . ? O4 Co2 O1 106.58(12) 2_344 . ? O7 Co2 O1 106.82(12) . . ? O4 Co2 O9 111.84(12) 2_344 1_455 ? O7 Co2 O9 108.67(10) . 1_455 ? O1 Co2 O9 111.85(10) . 1_455 ? O5 S1 O6 120.2(2) . . ? O5 S1 C7 108.1(2) . . ? O6 S1 C7 108.6(2) . . ? O5 S1 C6 108.0(2) . . ? O6 S1 C6 106.13(19) . . ? C7 S1 C6 104.70(16) . . ? C13 O1 Co2 126.1(2) . . ? C13 O2 Co1 140.9(2) . 1_455 ? C14 O3 Co1 140.3(2) . 2_354 ? C14 O4 Co2 127.5(2) . 2_354 ? C25 O7 Co2 120.0(2) . . ? C25 O7 Co1 121.0(2) . . ? Co2 O7 Co1 118.75(10) . . ? C36 O9 Co2 121.3(2) . 1_655 ? C36 O9 Co1 120.2(2) . . ? Co2 O9 Co1 117.93(12) 1_655 . ? C15 N1 C22 110.6(4) . . ? C15 N1 H1B 124.7 . . ? C22 N1 H1B 124.7 . . ? C24 N2 Co1 110.4(2) . . ? C24 N2 H2B 109.6 . . ? Co1 N2 H2B 109.6 . . ? C24 N2 H2C 109.6 . . ? Co1 N2 H2C 109.6 . . ? H2B N2 H2C 108.1 . . ? C26 N3 C33 110.3(3) . . ? C26 N3 H3A 124.8 . . ? C33 N3 H3A 124.8 . . ? C35 N4 Co1 110.7(2) . . ? C35 N4 H4B 109.5 . . ? Co1 N4 H4B 109.5 . . ? C35 N4 H4C 109.5 . . ? Co1 N4 H4C 109.5 . . ? H4B N4 H4C 108.1 . . ? C6 C1 C2 120.9(4) . . ? C6 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? C1 C2 C3 119.1(4) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 C13 120.2(3) . . ? C4 C3 C13 120.2(3) . . ? C5 C4 C3 121.0(4) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 119.1(4) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C1 C6 C5 120.4(4) . . ? C1 C6 S1 120.6(3) . . ? C5 C6 S1 119.1(3) . . ? C12 C7 C8 121.0(3) . . ? C12 C7 S1 118.5(3) . . ? C8 C7 S1 120.5(3) . . ? C9 C8 C7 120.0(4) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 119.6(4) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C9 C10 C11 119.9(3) . . ? C9 C10 C14 120.1(3) . . ? C11 C10 C14 119.9(3) . . ? C12 C11 C10 120.9(4) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C7 C12 C11 118.6(4) . . ? C7 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? O2 C13 O1 126.2(3) . . ? O2 C13 C3 117.5(3) . . ? O1 C13 C3 116.2(3) . . ? O3 C14 O4 125.9(3) . . ? O3 C14 C10 118.4(3) . . ? O4 C14 C10 115.7(3) . . ? N1 C15 C16 132.3(7) . . ? N1 C15 C20 107.3(4) . . ? C16 C15 C20 120.2(7) . . ? C17 C16 C15 117.4(7) . . ? C17 C16 H16A 121.3 . . ? C15 C16 H16A 121.3 . . ? C16 C17 C18 125.3(6) . . ? C16 C17 H17A 117.3 . . ? C18 C17 H17A 117.3 . . ? C17 C18 C19 118.1(6) . . ? C17 C18 H18A 121.0 . . ? C19 C18 H18A 121.0 . . ? C20 C19 C18 115.7(6) . . ? C20 C19 H19A 122.2 . . ? C18 C19 H19A 122.2 . . ? C19 C20 C21 133.1(4) . . ? C19 C20 C15 123.3(5) . . ? C21 C20 C15 103.6(4) . . ? C22 C21 C20 108.0(4) . . ? C22 C21 C23 126.0(4) . . ? C20 C21 C23 125.9(3) . . ? N1 C22 C21 110.5(5) . . ? N1 C22 H22A 124.7 . . ? C21 C22 H22A 124.7 . . ? C21 C23 C24 113.5(3) . . ? C21 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? C21 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C25 C24 N2 111.4(3) . . ? C25 C24 C23 108.5(3) . . ? N2 C24 C23 112.6(3) . . ? C25 C24 H24A 108.1 . . ? N2 C24 H24A 108.1 . . ? C23 C24 H24A 108.1 . . ? O8 C25 O7 123.0(4) . . ? O8 C25 C24 121.0(3) . . ? O7 C25 C24 115.9(3) . . ? C27 C26 N3 130.2(4) . . ? C27 C26 C31 123.3(4) . . ? N3 C26 C31 106.4(3) . . ? C26 C27 C28 116.7(4) . . ? C26 C27 H27A 121.7 . . ? C28 C27 H27A 121.7 . . ? C29 C28 C27 122.2(4) . . ? C29 C28 H28A 118.9 . . ? C27 C28 H28A 118.9 . . ? C30 C29 C28 121.0(4) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C29 C30 C31 119.0(4) . . ? C29 C30 H30A 120.5 . . ? C31 C30 H30A 120.5 . . ? C32 C31 C30 134.8(4) . . ? C32 C31 C26 107.4(3) . . ? C30 C31 C26 117.7(4) . . ? C33 C32 C31 106.2(3) . . ? C33 C32 C34 124.2(3) . . ? C31 C32 C34 129.5(3) . . ? C32 C33 N3 109.6(4) . . ? C32 C33 H33A 125.2 . . ? N3 C33 H33A 125.2 . . ? C32 C34 C35 115.6(3) . . ? C32 C34 H34A 108.4 . . ? C35 C34 H34A 108.4 . . ? C32 C34 H34B 108.4 . . ? C35 C34 H34B 108.4 . . ? H34A C34 H34B 107.5 . . ? N4 C35 C34 114.0(3) . . ? N4 C35 C36 110.8(3) . . ? C34 C35 C36 112.8(3) . . ? N4 C35 H35A 106.2 . . ? C34 C35 H35A 106.2 . . ? C36 C35 H35A 106.2 . . ? O10 C36 O9 122.7(3) . . ? O10 C36 C35 122.5(3) . . ? O9 C36 C35 114.8(3) . . ? 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 O4 Co2 O1 C13 128.9(3) 2_344 . . . ? O7 Co2 O1 C13 -112.4(3) . . . . ? O9 Co2 O1 C13 6.4(3) 1_455 . . . ? O4 Co2 O7 C25 168.1(3) 2_344 . . . ? O1 Co2 O7 C25 52.3(3) . . . . ? O9 Co2 O7 C25 -68.6(3) 1_455 . . . ? O4 Co2 O7 Co1 -5.5(2) 2_344 . . . ? O1 Co2 O7 Co1 -121.32(14) . . . . ? O9 Co2 O7 Co1 117.84(14) 1_455 . . . ? O9 Co1 O7 C25 59.1(10) . . . . ? O2 Co1 O7 C25 -80.0(3) 1_655 . . . ? O3 Co1 O7 C25 -171.2(3) 2_344 . . . ? N4 Co1 O7 C25 100.6(3) . . . . ? N2 Co1 O7 C25 8.3(3) . . . . ? O9 Co1 O7 Co2 -127.4(8) . . . . ? O2 Co1 O7 Co2 93.54(15) 1_655 . . . ? O3 Co1 O7 Co2 2.38(16) 2_344 . . . ? N4 Co1 O7 Co2 -85.88(15) . . . . ? N2 Co1 O7 Co2 -178.12(17) . . . . ? O7 Co1 O9 C36 31.5(10) . . . . ? O2 Co1 O9 C36 170.2(2) 1_655 . . . ? O3 Co1 O9 C36 -98.6(2) 2_344 . . . ? N4 Co1 O9 C36 -10.8(2) . . . . ? N2 Co1 O9 C36 81.4(2) . . . . ? O7 Co1 O9 Co2 -140.4(8) . . . 1_655 ? O2 Co1 O9 Co2 -1.67(15) 1_655 . . 1_655 ? O3 Co1 O9 Co2 89.44(15) 2_344 . . 1_655 ? N4 Co1 O9 Co2 177.33(15) . . . 1_655 ? N2 Co1 O9 Co2 -90.54(14) . . . 1_655 ? O7 Co1 N2 C24 -13.8(2) . . . . ? O9 Co1 N2 C24 171.2(2) . . . . ? O2 Co1 N2 C24 75.0(2) 1_655 . . . ? O3 Co1 N2 C24 -8.6(14) 2_344 . . . ? N4 Co1 N2 C24 -110.3(2) . . . . ? O7 Co1 N4 C35 -156.4(2) . . . . ? O9 Co1 N4 C35 19.2(2) . . . . ? O2 Co1 N4 C35 29.6(13) 1_655 . . . ? O3 Co1 N4 C35 107.8(2) 2_344 . . . ? N2 Co1 N4 C35 -77.5(2) . . . . ? C6 C1 C2 C3 1.0(6) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? C1 C2 C3 C13 178.2(3) . . . . ? C2 C3 C4 C5 -0.3(6) . . . . ? C13 C3 C4 C5 -179.1(4) . . . . ? C3 C4 C5 C6 0.9(7) . . . . ? C2 C1 C6 C5 -0.4(6) . . . . ? C2 C1 C6 S1 -179.0(3) . . . . ? C4 C5 C6 C1 -0.5(6) . . . . ? C4 C5 C6 S1 178.1(3) . . . . ? O5 S1 C6 C1 132.4(3) . . . . ? O6 S1 C6 C1 2.3(4) . . . . ? C7 S1 C6 C1 -112.5(3) . . . . ? O5 S1 C6 C5 -46.2(4) . . . . ? O6 S1 C6 C5 -176.3(3) . . . . ? C7 S1 C6 C5 68.9(4) . . . . ? O5 S1 C7 C12 15.0(4) . . . . ? O6 S1 C7 C12 147.0(3) . . . . ? C6 S1 C7 C12 -100.0(3) . . . . ? O5 S1 C7 C8 -166.4(3) . . . . ? O6 S1 C7 C8 -34.4(4) . . . . ? C6 S1 C7 C8 78.7(3) . . . . ? C12 C7 C8 C9 2.2(6) . . . . ? S1 C7 C8 C9 -176.4(3) . . . . ? C7 C8 C9 C10 -0.5(6) . . . . ? C8 C9 C10 C11 -1.8(6) . . . . ? C8 C9 C10 C14 179.5(4) . . . . ? C9 C10 C11 C12 2.4(6) . . . . ? C14 C10 C11 C12 -178.8(4) . . . . ? C8 C7 C12 C11 -1.6(6) . . . . ? S1 C7 C12 C11 177.0(3) . . . . ? C10 C11 C12 C7 -0.7(6) . . . . ? Co1 O2 C13 O1 8.1(6) 1_455 . . . ? Co1 O2 C13 C3 -171.2(3) 1_455 . . . ? Co2 O1 C13 O2 -10.3(5) . . . . ? Co2 O1 C13 C3 168.9(2) . . . . ? C2 C3 C13 O2 -4.8(5) . . . . ? C4 C3 C13 O2 174.0(4) . . . . ? C2 C3 C13 O1 175.9(3) . . . . ? C4 C3 C13 O1 -5.3(5) . . . . ? Co1 O3 C14 O4 2.0(7) 2_354 . . . ? Co1 O3 C14 C10 -177.0(3) 2_354 . . . ? Co2 O4 C14 O3 -6.8(6) 2_354 . . . ? Co2 O4 C14 C10 172.3(2) 2_354 . . . ? C9 C10 C14 O3 3.5(5) . . . . ? C11 C10 C14 O3 -175.3(3) . . . . ? C9 C10 C14 O4 -175.6(3) . . . . ? C11 C10 C14 O4 5.6(5) . . . . ? C22 N1 C15 C16 -174.1(6) . . . . ? C22 N1 C15 C20 0.8(6) . . . . ? N1 C15 C16 C17 176.5(6) . . . . ? C20 C15 C16 C17 2.2(9) . . . . ? C15 C16 C17 C18 -1.2(11) . . . . ? C16 C17 C18 C19 0.0(10) . . . . ? C17 C18 C19 C20 0.0(8) . . . . ? C18 C19 C20 C21 -176.5(5) . . . . ? C18 C19 C20 C15 1.1(7) . . . . ? N1 C15 C20 C19 -177.9(4) . . . . ? C16 C15 C20 C19 -2.3(7) . . . . ? N1 C15 C20 C21 0.3(5) . . . . ? C16 C15 C20 C21 175.8(5) . . . . ? C19 C20 C21 C22 176.7(5) . . . . ? C15 C20 C21 C22 -1.2(5) . . . . ? C19 C20 C21 C23 0.9(7) . . . . ? C15 C20 C21 C23 -177.0(4) . . . . ? C15 N1 C22 C21 -1.6(6) . . . . ? C20 C21 C22 N1 1.7(6) . . . . ? C23 C21 C22 N1 177.5(4) . . . . ? C22 C21 C23 C24 114.7(5) . . . . ? C20 C21 C23 C24 -70.3(5) . . . . ? Co1 N2 C24 C25 17.3(3) . . . . ? Co1 N2 C24 C23 -104.7(3) . . . . ? C21 C23 C24 C25 170.4(3) . . . . ? C21 C23 C24 N2 -65.8(4) . . . . ? Co2 O7 C25 O8 3.9(5) . . . . ? Co1 O7 C25 O8 177.4(3) . . . . ? Co2 O7 C25 C24 -174.0(2) . . . . ? Co1 O7 C25 C24 -0.5(4) . . . . ? N2 C24 C25 O8 170.1(4) . . . . ? C23 C24 C25 O8 -65.4(5) . . . . ? N2 C24 C25 O7 -11.9(5) . . . . ? C23 C24 C25 O7 112.5(4) . . . . ? C33 N3 C26 C27 175.4(4) . . . . ? C33 N3 C26 C31 -1.9(5) . . . . ? N3 C26 C27 C28 -178.3(4) . . . . ? C31 C26 C27 C28 -1.4(7) . . . . ? C26 C27 C28 C29 -0.2(8) . . . . ? C27 C28 C29 C30 1.1(8) . . . . ? C28 C29 C30 C31 -0.4(7) . . . . ? C29 C30 C31 C32 176.1(4) . . . . ? C29 C30 C31 C26 -1.0(6) . . . . ? C27 C26 C31 C32 -175.9(4) . . . . ? N3 C26 C31 C32 1.7(4) . . . . ? C27 C26 C31 C30 1.9(6) . . . . ? N3 C26 C31 C30 179.5(4) . . . . ? C30 C31 C32 C33 -178.1(4) . . . . ? C26 C31 C32 C33 -0.8(4) . . . . ? C30 C31 C32 C34 -0.8(7) . . . . ? C26 C31 C32 C34 176.5(4) . . . . ? C31 C32 C33 N3 -0.3(5) . . . . ? C34 C32 C33 N3 -177.8(3) . . . . ? C26 N3 C33 C32 1.4(5) . . . . ? C33 C32 C34 C35 -102.4(4) . . . . ? C31 C32 C34 C35 80.7(5) . . . . ? Co1 N4 C35 C34 -153.1(2) . . . . ? Co1 N4 C35 C36 -24.6(3) . . . . ? C32 C34 C35 N4 48.0(4) . . . . ? C32 C34 C35 C36 -79.5(4) . . . . ? Co2 O9 C36 O10 -5.9(5) 1_655 . . . ? Co1 O9 C36 O10 -177.5(3) . . . . ? Co2 O9 C36 C35 171.2(2) 1_655 . . . ? Co1 O9 C36 C35 -0.4(4) . . . . ? N4 C35 C36 O10 -165.7(3) . . . . ? C34 C35 C36 O10 -36.5(5) . . . . ? N4 C35 C36 O9 17.2(4) . . . . ? C34 C35 C36 O9 146.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O6 0.90 2.39 3.093(4) 134.9 2_345 N2 H2C O8 0.90 2.39 3.231(4) 156.1 1_655 N4 H4B O6 0.90 2.56 3.346(4) 147.0 2_345 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.429 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.053 data_z4a _database_code_depnum_ccdc_archive 'CCDC 758888' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Co2 N4 O10 S' _chemical_formula_weight 828.56 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.5291(13) _cell_length_b 21.749(4) _cell_length_c 12.586(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.83(3) _cell_angle_gamma 90.00 _cell_volume 1760.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11472 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 28.30 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.066 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6231 _exptl_absorpt_correction_T_max 0.7915 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 11472 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7048 _reflns_number_gt 6442 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 0.014(10) _refine_ls_number_reflns 7048 _refine_ls_number_parameters 478 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.029 _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 Co1 Co 0.89381(5) 1.495667(15) 1.14363(3) 0.02904(8) Uani 1 1 d . . . Co2 Co 1.41662(5) 1.470535(16) 1.21311(3) 0.03171(9) Uani 1 1 d . . . S1 S 1.81156(17) 1.09401(4) 1.17023(6) 0.0530(2) Uani 1 1 d . . . O1 O 1.5277(4) 1.38667(10) 1.22395(19) 0.0485(5) Uani 1 1 d . . . O2 O 1.8351(4) 1.40265(9) 1.17367(19) 0.0462(5) Uani 1 1 d . . . O3 O 1.9894(3) 1.01106(11) 1.69128(17) 0.0508(6) Uani 1 1 d . . . O4 O 1.6512(3) 0.99066(13) 1.64742(15) 0.0544(6) Uani 1 1 d . . . O5 O 1.6273(6) 1.07004(12) 1.10449(18) 0.0784(9) Uani 1 1 d . . . O6 O 2.0123(5) 1.08465(11) 1.1396(2) 0.0744(9) Uani 1 1 d . . . O7 O 1.1682(3) 1.46927(10) 1.10272(14) 0.0345(4) Uani 1 1 d . . . O8 O 1.3373(4) 1.42892(15) 0.9823(2) 0.0698(8) Uani 1 1 d . . . O9 O 0.6151(3) 1.52876(9) 1.17028(16) 0.0361(4) Uani 1 1 d . . . O10 O 0.3945(3) 1.60697(10) 1.1569(2) 0.0509(6) Uani 1 1 d . . . N1 N 0.4279(6) 1.3336(2) 0.7448(4) 0.0914(13) Uani 1 1 d . . . H1B H 0.3029 1.3196 0.7358 0.110 Uiso 1 1 calc R . . N2 N 0.8025(4) 1.47655(11) 0.97321(17) 0.0364(5) Uani 1 1 d . . . H2B H 0.6848 1.4542 0.9626 0.044 Uiso 1 1 calc R . . H2C H 0.7770 1.5121 0.9369 0.044 Uiso 1 1 calc R . . N3 N 1.1007(5) 1.73859(14) 1.3707(3) 0.0582(8) Uani 1 1 d . . . H3A H 1.2192 1.7529 1.4009 0.070 Uiso 1 1 calc R . . N4 N 0.9283(4) 1.59217(11) 1.1196(2) 0.0375(5) Uani 1 1 d . . . H4B H 1.0056 1.6088 1.1787 0.045 Uiso 1 1 calc R . . H4C H 0.9950 1.5983 1.0635 0.045 Uiso 1 1 calc R . . C1 C 1.9387(5) 1.21380(15) 1.1647(3) 0.0473(7) Uani 1 1 d . . . H1A H 2.0625 1.1978 1.1494 0.057 Uiso 1 1 calc R . . C2 C 1.9127(5) 1.27709(14) 1.1712(3) 0.0428(7) Uani 1 1 d . . . H2A H 2.0195 1.3035 1.1610 0.051 Uiso 1 1 calc R . . C3 C 1.7286(5) 1.30036(12) 1.1930(2) 0.0353(6) Uani 1 1 d . . . C4 C 1.5701(6) 1.26049(15) 1.2098(3) 0.0539(9) Uani 1 1 d . . . H4A H 1.4463 1.2763 1.2255 0.065 Uiso 1 1 calc R . . C5 C 1.5960(6) 1.19768(15) 1.2034(3) 0.0575(9) Uani 1 1 d . . . H5A H 1.4900 1.1710 1.2141 0.069 Uiso 1 1 calc R . . C6 C 1.7813(5) 1.17507(13) 1.1808(2) 0.0409(7) Uani 1 1 d . . . C7 C 1.8207(5) 1.06619(13) 1.3026(2) 0.0419(7) Uani 1 1 d . . . C8 C 2.0007(6) 1.07102(15) 1.3775(3) 0.0480(8) Uani 1 1 d . . . H8A H 2.1207 1.0868 1.3572 0.058 Uiso 1 1 calc R . . C9 C 2.0030(5) 1.05233(15) 1.4829(2) 0.0440(7) Uani 1 1 d . . . H9A H 2.1236 1.0559 1.5339 0.053 Uiso 1 1 calc R . . C10 C 1.8231(5) 1.02818(12) 1.5114(2) 0.0348(6) Uani 1 1 d . . . C11 C 1.6460(5) 1.02155(16) 1.4347(3) 0.0479(8) Uani 1 1 d . . . H11A H 1.5274 1.0043 1.4541 0.057 Uiso 1 1 calc R . . C12 C 1.6430(6) 1.04019(17) 1.3301(3) 0.0504(8) Uani 1 1 d . . . H12A H 1.5237 1.0354 1.2786 0.061 Uiso 1 1 calc R . . C13 C 1.6947(5) 1.36929(13) 1.1968(2) 0.0357(6) Uani 1 1 d . . . C14 C 1.8249(4) 1.00810(12) 1.6269(2) 0.0350(6) Uani 1 1 d . . . C15 C 0.5253(9) 1.35219(18) 0.6649(4) 0.0797(15) Uani 1 1 d . . . C16 C 0.4703(11) 1.3509(3) 0.5566(5) 0.110(2) Uani 1 1 d U . . H16A H 0.3401 1.3369 0.5240 0.132 Uiso 1 1 calc R . . C17 C 0.6125(12) 1.3709(2) 0.4966(4) 0.0975(18) Uani 1 1 d U . . H17A H 0.5735 1.3702 0.4220 0.117 Uiso 1 1 calc R . . C18 C 0.8147(12) 1.3926(2) 0.5387(4) 0.1078(19) Uani 1 1 d DU . . H18A H 0.9035 1.4061 0.4931 0.129 Uiso 1 1 calc R . . C19 C 0.8784(8) 1.39331(17) 0.6534(3) 0.0719(13) Uani 1 1 d D . . H19A H 1.0097 1.4067 0.6857 0.086 Uiso 1 1 calc R . . C20 C 0.7342(6) 1.37307(14) 0.7127(3) 0.0500(8) Uani 1 1 d . . . C21 C 0.7380(5) 1.36363(13) 0.8262(3) 0.0478(8) Uani 1 1 d . . . C22 C 0.5510(7) 1.33975(18) 0.8396(4) 0.0744(13) Uani 1 1 d . . . H22A H 0.5150 1.3293 0.9057 0.089 Uiso 1 1 calc R . . C23 C 0.9174(6) 1.37434(14) 0.9136(2) 0.0484(8) Uani 1 1 d . . . H23A H 1.0383 1.3534 0.8959 0.058 Uiso 1 1 calc R . . H23B H 0.8871 1.3567 0.9801 0.058 Uiso 1 1 calc R . . C24 C 0.9679(5) 1.44249(13) 0.9316(2) 0.0373(6) Uani 1 1 d . . . H24A H 0.9849 1.4606 0.8623 0.045 Uiso 1 1 calc R . . C25 C 1.1758(5) 1.44678(14) 1.0083(2) 0.0418(7) Uani 1 1 d . . . C26 C 0.9429(5) 1.72201(15) 1.4239(3) 0.0489(8) Uani 1 1 d . . . C27 C 0.9302(6) 1.72664(18) 1.5313(3) 0.0606(10) Uani 1 1 d . . . H27A H 1.0396 1.7421 1.5811 0.073 Uiso 1 1 calc R . . C28 C 0.7485(7) 1.7074(2) 1.5617(3) 0.0694(11) Uani 1 1 d . . . H28A H 0.7339 1.7104 1.6338 0.083 Uiso 1 1 calc R . . C29 C 0.5844(6) 1.6832(2) 1.4869(3) 0.0654(10) Uani 1 1 d . . . H29A H 0.4646 1.6697 1.5104 0.078 Uiso 1 1 calc R . . C30 C 0.5977(5) 1.67915(17) 1.3797(3) 0.0513(8) Uani 1 1 d . . . H30A H 0.4874 1.6635 1.3305 0.062 Uiso 1 1 calc R . . C31 C 0.7803(5) 1.69889(13) 1.3450(3) 0.0408(6) Uani 1 1 d . . . C32 C 0.8459(5) 1.70477(12) 1.2416(3) 0.0394(6) Uani 1 1 d . . . C33 C 1.0414(5) 1.72898(15) 1.2615(3) 0.0505(8) Uani 1 1 d . . . H33A H 1.1223 1.7377 1.2093 0.061 Uiso 1 1 calc R . . C34 C 0.7274(5) 1.69075(13) 1.1305(3) 0.0425(7) Uani 1 1 d . . . H34A H 0.7886 1.7141 1.0782 0.051 Uiso 1 1 calc R . . H34B H 0.5854 1.7049 1.1265 0.051 Uiso 1 1 calc R . . C35 C 0.7227(4) 1.62267(13) 1.0980(2) 0.0357(6) Uani 1 1 d . . . H35A H 0.6778 1.6216 1.0196 0.043 Uiso 1 1 calc R . . C36 C 0.5623(4) 1.58558(13) 1.1463(2) 0.0342(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02701(16) 0.03127(17) 0.02939(17) -0.00622(14) 0.00640(12) 0.00030(14) Co2 0.02851(17) 0.03490(18) 0.03317(18) -0.00279(15) 0.00939(13) 0.00337(15) S1 0.1011(7) 0.0332(4) 0.0275(4) 0.0053(3) 0.0190(4) 0.0150(4) O1 0.0516(13) 0.0386(11) 0.0608(15) 0.0089(10) 0.0251(11) 0.0130(10) O2 0.0472(12) 0.0352(11) 0.0599(14) 0.0052(10) 0.0193(11) 0.0025(9) O3 0.0446(12) 0.0761(17) 0.0306(10) 0.0156(10) 0.0031(9) -0.0067(11) O4 0.0463(12) 0.0869(17) 0.0303(10) 0.0070(11) 0.0079(8) -0.0207(12) O5 0.149(3) 0.0514(14) 0.0266(12) -0.0031(10) -0.0096(14) -0.0041(17) O6 0.131(3) 0.0506(15) 0.0553(16) 0.0183(11) 0.0555(17) 0.0394(15) O7 0.0276(8) 0.0421(9) 0.0345(9) -0.0116(9) 0.0073(7) 0.0025(9) O8 0.0490(15) 0.102(2) 0.0615(16) -0.0247(15) 0.0177(12) 0.0192(14) O9 0.0286(9) 0.0345(10) 0.0461(11) -0.0042(9) 0.0091(8) -0.0021(8) O10 0.0331(11) 0.0446(12) 0.0754(16) -0.0127(11) 0.0100(11) 0.0036(9) N1 0.056(2) 0.084(3) 0.134(4) -0.035(3) 0.016(2) -0.0176(19) N2 0.0422(12) 0.0311(11) 0.0346(11) -0.0059(10) 0.0030(9) -0.0035(10) N3 0.0507(17) 0.0564(18) 0.0635(19) -0.0111(15) -0.0013(14) -0.0168(14) N4 0.0332(12) 0.0336(12) 0.0480(14) -0.0113(11) 0.0137(10) -0.0051(10) C1 0.0548(19) 0.0430(17) 0.0485(18) 0.0090(14) 0.0214(15) 0.0172(14) C2 0.0473(17) 0.0398(16) 0.0441(17) 0.0120(13) 0.0157(13) 0.0081(13) C3 0.0444(16) 0.0310(14) 0.0323(14) 0.0055(11) 0.0117(12) 0.0078(12) C4 0.052(2) 0.0388(17) 0.078(3) 0.0106(17) 0.0314(19) 0.0125(14) C5 0.062(2) 0.0359(16) 0.081(3) 0.0099(16) 0.029(2) -0.0036(15) C6 0.065(2) 0.0308(14) 0.0286(14) 0.0062(11) 0.0125(13) 0.0117(13) C7 0.068(2) 0.0305(13) 0.0277(14) 0.0044(11) 0.0112(13) 0.0093(14) C8 0.060(2) 0.0463(17) 0.0404(17) 0.0090(14) 0.0175(15) -0.0044(15) C9 0.0456(17) 0.0521(18) 0.0340(15) 0.0105(13) 0.0060(12) -0.0033(14) C10 0.0429(15) 0.0322(13) 0.0304(14) 0.0043(11) 0.0096(11) 0.0003(11) C11 0.0454(17) 0.0593(19) 0.0375(16) 0.0118(14) 0.0028(13) -0.0094(15) C12 0.0550(19) 0.058(2) 0.0344(16) 0.0082(14) -0.0022(14) -0.0051(16) C13 0.0441(16) 0.0339(14) 0.0295(14) 0.0042(11) 0.0074(12) 0.0065(12) C14 0.0429(15) 0.0341(15) 0.0293(13) 0.0037(10) 0.0096(11) -0.0003(11) C15 0.112(4) 0.0403(19) 0.069(3) -0.0228(19) -0.035(3) 0.011(2) C16 0.133(5) 0.088(3) 0.089(4) -0.024(3) -0.042(3) 0.012(3) C17 0.164(5) 0.059(3) 0.053(3) -0.006(2) -0.026(3) 0.009(3) C18 0.185(6) 0.055(3) 0.089(4) 0.011(2) 0.040(4) 0.003(3) C19 0.129(4) 0.044(2) 0.045(2) -0.0010(16) 0.024(2) -0.008(2) C20 0.065(2) 0.0272(14) 0.0508(19) -0.0101(13) -0.0092(16) -0.0014(14) C21 0.059(2) 0.0305(15) 0.058(2) -0.0142(14) 0.0227(16) -0.0112(14) C22 0.077(3) 0.050(2) 0.104(4) -0.033(2) 0.038(3) -0.021(2) C23 0.077(2) 0.0328(15) 0.0364(16) -0.0049(12) 0.0121(15) 0.0037(15) C24 0.0486(17) 0.0341(14) 0.0296(14) -0.0097(11) 0.0077(12) 0.0029(12) C25 0.0411(16) 0.0451(15) 0.0405(16) -0.0098(13) 0.0111(13) 0.0042(13) C26 0.0526(19) 0.0392(16) 0.0519(19) -0.0047(14) 0.0004(15) 0.0027(14) C27 0.070(3) 0.060(2) 0.0469(19) -0.0128(16) -0.0061(17) 0.0056(19) C28 0.084(3) 0.077(3) 0.048(2) -0.0067(19) 0.012(2) 0.008(2) C29 0.061(2) 0.074(3) 0.064(2) 0.002(2) 0.021(2) 0.005(2) C30 0.0476(19) 0.0540(19) 0.052(2) -0.0059(16) 0.0088(15) -0.0021(15) C31 0.0432(16) 0.0314(14) 0.0470(17) -0.0039(12) 0.0053(13) 0.0027(12) C32 0.0438(16) 0.0262(13) 0.0479(17) -0.0040(12) 0.0065(13) 0.0012(11) C33 0.054(2) 0.0380(17) 0.061(2) -0.0042(15) 0.0145(16) -0.0084(14) C34 0.0509(18) 0.0311(14) 0.0452(17) 0.0011(13) 0.0070(14) 0.0033(13) C35 0.0381(15) 0.0350(14) 0.0335(14) -0.0045(11) 0.0049(11) -0.0010(11) C36 0.0272(13) 0.0370(15) 0.0368(15) -0.0134(11) 0.0006(11) 0.0012(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O7 2.0294(17) . ? Co1 O9 2.0375(19) . ? Co1 O2 2.105(2) 1_455 ? Co1 O3 2.114(2) 2_858 ? Co1 N4 2.138(2) . ? Co1 N2 2.166(2) . ? Co2 O4 1.9323(19) 2_858 ? Co2 O7 1.9477(19) . ? Co2 O9 1.9522(19) 1_655 ? Co2 O1 1.959(2) . ? S1 O5 1.437(3) . ? S1 O6 1.443(3) . ? S1 C7 1.764(3) . ? S1 C6 1.782(3) . ? O1 C13 1.255(4) . ? O2 C13 1.242(4) . ? O2 Co1 2.105(2) 1_655 ? O3 C14 1.232(4) . ? O3 Co1 2.114(2) 2_848 ? O4 C14 1.263(3) . ? O4 Co2 1.9323(19) 2_848 ? O7 C25 1.294(3) . ? O8 C25 1.220(4) . ? O9 C36 1.304(3) . ? O9 Co2 1.9522(19) 1_455 ? O10 C36 1.218(3) . ? N1 C22 1.328(6) . ? N1 C15 1.340(7) . ? N1 H1B 0.8600 . ? N2 C24 1.478(4) . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? N3 C26 1.369(4) . ? N3 C33 1.379(4) . ? N3 H3A 0.8600 . ? N4 C35 1.480(4) . ? N4 H4B 0.9000 . ? N4 H4C 0.9000 . ? C1 C6 1.371(5) . ? C1 C2 1.391(4) . ? C1 H1A 0.9300 . ? C2 C3 1.374(4) . ? C2 H2A 0.9300 . ? C3 C4 1.394(5) . ? C3 C13 1.517(4) . ? C4 C5 1.380(5) . ? C4 H4A 0.9300 . ? C5 C6 1.380(5) . ? C5 H5A 0.9300 . ? C7 C8 1.379(5) . ? C7 C12 1.387(5) . ? C8 C9 1.385(4) . ? C8 H8A 0.9300 . ? C9 C10 1.389(4) . ? C9 H9A 0.9300 . ? C10 C11 1.381(4) . ? C10 C14 1.516(4) . ? C11 C12 1.374(4) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C15 C16 1.350(7) . ? C15 C20 1.465(6) . ? C16 C17 1.364(9) . ? C16 H16A 0.9300 . ? C17 C18 1.417(9) . ? C17 H17A 0.9300 . ? C18 C19 1.433(6) . ? C18 H18A 0.9300 . ? C19 C20 1.370(6) . ? C19 H19A 0.9300 . ? C20 C21 1.439(5) . ? C21 C22 1.364(5) . ? C21 C23 1.482(5) . ? C22 H22A 0.9300 . ? C23 C24 1.527(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.529(4) . ? C24 H24A 0.9800 . ? C26 C27 1.372(5) . ? C26 C31 1.416(4) . ? C27 C28 1.373(6) . ? C27 H27A 0.9300 . ? C28 C29 1.403(6) . ? C28 H28A 0.9300 . ? C29 C30 1.370(5) . ? C29 H29A 0.9300 . ? C30 C31 1.405(5) . ? C30 H30A 0.9300 . ? C31 C32 1.443(4) . ? C32 C33 1.364(4) . ? C32 C34 1.510(4) . ? C33 H33A 0.9300 . ? C34 C35 1.535(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.528(4) . ? C35 H35A 0.9800 . ? 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 O7 Co1 O9 173.55(8) . . ? O7 Co1 O2 88.24(9) . 1_455 ? O9 Co1 O2 96.59(8) . 1_455 ? O7 Co1 O3 96.22(8) . 2_858 ? O9 Co1 O3 87.97(9) . 2_858 ? O2 Co1 O3 91.25(10) 1_455 2_858 ? O7 Co1 N4 97.05(9) . . ? O9 Co1 N4 78.19(8) . . ? O2 Co1 N4 174.64(9) 1_455 . ? O3 Co1 N4 87.41(10) 2_858 . ? O7 Co1 N2 78.47(8) . . ? O9 Co1 N2 97.37(9) . . ? O2 Co1 N2 88.03(9) 1_455 . ? O3 Co1 N2 174.66(9) 2_858 . ? N4 Co1 N2 93.78(9) . . ? O4 Co2 O7 111.05(8) 2_858 . ? O4 Co2 O9 111.69(10) 2_858 1_655 ? O7 Co2 O9 108.87(8) . 1_655 ? O4 Co2 O1 106.69(10) 2_858 . ? O7 Co2 O1 106.85(10) . . ? O9 Co2 O1 111.58(9) 1_655 . ? O5 S1 O6 120.30(19) . . ? O5 S1 C7 108.02(17) . . ? O6 S1 C7 108.58(16) . . ? O5 S1 C6 108.03(17) . . ? O6 S1 C6 106.10(16) . . ? C7 S1 C6 104.76(13) . . ? C13 O1 Co2 126.16(19) . . ? C13 O2 Co1 140.16(19) . 1_655 ? C14 O3 Co1 139.95(19) . 2_848 ? C14 O4 Co2 127.30(19) . 2_848 ? C25 O7 Co2 120.16(18) . . ? C25 O7 Co1 120.94(18) . . ? Co2 O7 Co1 118.60(8) . . ? C36 O9 Co2 121.12(18) . 1_455 ? C36 O9 Co1 120.31(18) . . ? Co2 O9 Co1 118.03(10) 1_455 . ? C22 N1 C15 110.6(4) . . ? C22 N1 H1B 124.7 . . ? C15 N1 H1B 124.7 . . ? C24 N2 Co1 110.68(17) . . ? C24 N2 H2B 109.5 . . ? Co1 N2 H2B 109.5 . . ? C24 N2 H2C 109.5 . . ? Co1 N2 H2C 109.5 . . ? H2B N2 H2C 108.1 . . ? C26 N3 C33 109.9(3) . . ? C26 N3 H3A 125.1 . . ? C33 N3 H3A 125.1 . . ? C35 N4 Co1 110.58(17) . . ? C35 N4 H4B 109.5 . . ? Co1 N4 H4B 109.5 . . ? C35 N4 H4C 109.5 . . ? Co1 N4 H4C 109.5 . . ? H4B N4 H4C 108.1 . . ? C6 C1 C2 119.8(3) . . ? C6 C1 H1A 120.1 . . ? C2 C1 H1A 120.1 . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 119.9(3) . . ? C2 C3 C13 120.5(3) . . ? C4 C3 C13 119.6(3) . . ? C5 C4 C3 120.3(3) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C1 C6 C5 121.2(3) . . ? C1 C6 S1 120.1(2) . . ? C5 C6 S1 118.7(3) . . ? C8 C7 C12 120.8(3) . . ? C8 C7 S1 120.4(2) . . ? C12 C7 S1 118.7(3) . . ? C7 C8 C9 120.0(3) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 C10 119.2(3) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 C14 120.6(3) . . ? C9 C10 C14 119.2(3) . . ? C12 C11 C10 120.8(3) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C11 C12 C7 118.9(3) . . ? C11 C12 H12A 120.6 . . ? C7 C12 H12A 120.6 . . ? O2 C13 O1 126.7(3) . . ? O2 C13 C3 116.9(3) . . ? O1 C13 C3 116.4(3) . . ? O3 C14 O4 126.5(3) . . ? O3 C14 C10 118.6(2) . . ? O4 C14 C10 114.9(3) . . ? N1 C15 C16 132.3(6) . . ? N1 C15 C20 108.3(4) . . ? C16 C15 C20 119.3(6) . . ? C15 C16 C17 117.7(6) . . ? C15 C16 H16A 121.2 . . ? C17 C16 H16A 121.2 . . ? C16 C17 C18 125.3(5) . . ? C16 C17 H17A 117.3 . . ? C18 C17 H17A 117.3 . . ? C17 C18 C19 118.1(5) . . ? C17 C18 H18A 120.9 . . ? C19 C18 H18A 120.9 . . ? C20 C19 C18 115.9(5) . . ? C20 C19 H19A 122.0 . . ? C18 C19 H19A 122.0 . . ? C19 C20 C21 133.6(4) . . ? C19 C20 C15 123.7(4) . . ? C21 C20 C15 102.7(4) . . ? C22 C21 C20 108.3(4) . . ? C22 C21 C23 125.3(4) . . ? C20 C21 C23 126.3(3) . . ? N1 C22 C21 110.1(4) . . ? N1 C22 H22A 124.9 . . ? C21 C22 H22A 124.9 . . ? C21 C23 C24 112.7(3) . . ? C21 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C21 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? N2 C24 C23 112.7(3) . . ? N2 C24 C25 111.7(2) . . ? C23 C24 C25 107.4(3) . . ? N2 C24 H24A 108.3 . . ? C23 C24 H24A 108.3 . . ? C25 C24 H24A 108.3 . . ? O8 C25 O7 122.5(3) . . ? O8 C25 C24 121.7(3) . . ? O7 C25 C24 115.7(2) . . ? N3 C26 C27 129.7(4) . . ? N3 C26 C31 106.7(3) . . ? C27 C26 C31 123.5(3) . . ? C26 C27 C28 117.0(4) . . ? C26 C27 H27A 121.5 . . ? C28 C27 H27A 121.5 . . ? C27 C28 C29 121.6(4) . . ? C27 C28 H28A 119.2 . . ? C29 C28 H28A 119.2 . . ? C30 C29 C28 121.1(4) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C29 C30 C31 119.1(3) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? C30 C31 C26 117.7(3) . . ? C30 C31 C32 134.9(3) . . ? C26 C31 C32 107.3(3) . . ? C33 C32 C31 106.4(3) . . ? C33 C32 C34 124.3(3) . . ? C31 C32 C34 129.3(3) . . ? C32 C33 N3 109.6(3) . . ? C32 C33 H33A 125.2 . . ? N3 C33 H33A 125.2 . . ? C32 C34 C35 115.2(2) . . ? C32 C34 H34A 108.5 . . ? C35 C34 H34A 108.5 . . ? C32 C34 H34B 108.5 . . ? C35 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? N4 C35 C34 114.0(2) . . ? N4 C35 C36 110.6(2) . . ? C34 C35 C36 112.8(2) . . ? N4 C35 H35A 106.3 . . ? C34 C35 H35A 106.3 . . ? C36 C35 H35A 106.3 . . ? O10 C36 O9 122.9(3) . . ? O10 C36 C35 122.1(3) . . ? O9 C36 C35 114.8(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 O4 Co2 O1 C13 -129.3(2) 2_858 . . . ? O7 Co2 O1 C13 111.8(3) . . . . ? O9 Co2 O1 C13 -7.1(3) 1_655 . . . ? O4 Co2 O7 C25 -168.3(2) 2_858 . . . ? O9 Co2 O7 C25 68.3(2) 1_655 . . . ? O1 Co2 O7 C25 -52.3(2) . . . . ? O4 Co2 O7 Co1 5.54(16) 2_858 . . . ? O9 Co2 O7 Co1 -117.83(11) 1_655 . . . ? O1 Co2 O7 Co1 121.53(12) . . . . ? O9 Co1 O7 C25 -58.4(8) . . . . ? O2 Co1 O7 C25 80.2(2) 1_455 . . . ? O3 Co1 O7 C25 171.3(2) 2_858 . . . ? N4 Co1 O7 C25 -100.6(2) . . . . ? N2 Co1 O7 C25 -8.1(2) . . . . ? O9 Co1 O7 Co2 127.8(7) . . . . ? O2 Co1 O7 Co2 -93.60(12) 1_455 . . . ? O3 Co1 O7 Co2 -2.54(13) 2_858 . . . ? N4 Co1 O7 Co2 85.60(13) . . . . ? N2 Co1 O7 Co2 178.05(14) . . . . ? O7 Co1 O9 C36 -31.9(8) . . . . ? O2 Co1 O9 C36 -170.20(19) 1_455 . . . ? O3 Co1 O9 C36 98.8(2) 2_858 . . . ? N4 Co1 O9 C36 11.00(19) . . . . ? N2 Co1 O9 C36 -81.3(2) . . . . ? O7 Co1 O9 Co2 139.8(7) . . . 1_455 ? O2 Co1 O9 Co2 1.49(13) 1_455 . . 1_455 ? O3 Co1 O9 Co2 -89.54(12) 2_858 . . 1_455 ? N4 Co1 O9 Co2 -177.31(13) . . . 1_455 ? N2 Co1 O9 Co2 90.34(12) . . . 1_455 ? O7 Co1 N2 C24 13.44(17) . . . . ? O9 Co1 N2 C24 -171.56(18) . . . . ? O2 Co1 N2 C24 -75.17(18) 1_455 . . . ? O3 Co1 N2 C24 7.1(11) 2_858 . . . ? N4 Co1 N2 C24 109.87(18) . . . . ? O7 Co1 N4 C35 156.06(18) . . . . ? O9 Co1 N4 C35 -19.52(18) . . . . ? O2 Co1 N4 C35 -32.4(12) 1_455 . . . ? O3 Co1 N4 C35 -107.98(19) 2_858 . . . ? N2 Co1 N4 C35 77.23(19) . . . . ? C6 C1 C2 C3 -0.6(5) . . . . ? C1 C2 C3 C4 0.9(5) . . . . ? C1 C2 C3 C13 -178.0(3) . . . . ? C2 C3 C4 C5 -0.9(5) . . . . ? C13 C3 C4 C5 178.0(3) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C2 C1 C6 C5 0.2(5) . . . . ? C2 C1 C6 S1 178.9(3) . . . . ? C4 C5 C6 C1 -0.1(6) . . . . ? C4 C5 C6 S1 -178.9(3) . . . . ? O5 S1 C6 C1 -132.7(3) . . . . ? O6 S1 C6 C1 -2.4(3) . . . . ? C7 S1 C6 C1 112.3(3) . . . . ? O5 S1 C6 C5 46.1(3) . . . . ? O6 S1 C6 C5 176.3(3) . . . . ? C7 S1 C6 C5 -68.9(3) . . . . ? O5 S1 C7 C8 166.3(3) . . . . ? O6 S1 C7 C8 34.3(3) . . . . ? C6 S1 C7 C8 -78.7(3) . . . . ? O5 S1 C7 C12 -14.5(3) . . . . ? O6 S1 C7 C12 -146.5(3) . . . . ? C6 S1 C7 C12 100.5(3) . . . . ? C12 C7 C8 C9 -2.9(5) . . . . ? S1 C7 C8 C9 176.3(3) . . . . ? C7 C8 C9 C10 0.7(5) . . . . ? C8 C9 C10 C11 1.6(5) . . . . ? C8 C9 C10 C14 -179.6(3) . . . . ? C9 C10 C11 C12 -1.8(5) . . . . ? C14 C10 C11 C12 179.4(3) . . . . ? C10 C11 C12 C7 -0.4(5) . . . . ? C8 C7 C12 C11 2.7(5) . . . . ? S1 C7 C12 C11 -176.5(3) . . . . ? Co1 O2 C13 O1 -9.5(5) 1_655 . . . ? Co1 O2 C13 C3 171.0(2) 1_655 . . . ? Co2 O1 C13 O2 11.7(4) . . . . ? Co2 O1 C13 C3 -168.87(19) . . . . ? C2 C3 C13 O2 3.9(4) . . . . ? C4 C3 C13 O2 -175.0(3) . . . . ? C2 C3 C13 O1 -175.6(3) . . . . ? C4 C3 C13 O1 5.5(4) . . . . ? Co1 O3 C14 O4 -1.6(5) 2_848 . . . ? Co1 O3 C14 C10 177.1(2) 2_848 . . . ? Co2 O4 C14 O3 6.1(5) 2_848 . . . ? Co2 O4 C14 C10 -172.6(2) 2_848 . . . ? C11 C10 C14 O3 175.3(3) . . . . ? C9 C10 C14 O3 -3.4(4) . . . . ? C11 C10 C14 O4 -5.8(4) . . . . ? C9 C10 C14 O4 175.4(3) . . . . ? C22 N1 C15 C16 174.9(5) . . . . ? C22 N1 C15 C20 -0.4(5) . . . . ? N1 C15 C16 C17 -176.5(5) . . . . ? C20 C15 C16 C17 -1.6(7) . . . . ? C15 C16 C17 C18 0.4(9) . . . . ? C16 C17 C18 C19 0.8(8) . . . . ? C17 C18 C19 C20 -0.7(6) . . . . ? C18 C19 C20 C21 176.4(4) . . . . ? C18 C19 C20 C15 -0.6(6) . . . . ? N1 C15 C20 C19 177.8(4) . . . . ? C16 C15 C20 C19 1.8(6) . . . . ? N1 C15 C20 C21 0.1(4) . . . . ? C16 C15 C20 C21 -176.0(4) . . . . ? C19 C20 C21 C22 -177.2(4) . . . . ? C15 C20 C21 C22 0.2(4) . . . . ? C19 C20 C21 C23 -0.5(6) . . . . ? C15 C20 C21 C23 176.9(3) . . . . ? C15 N1 C22 C21 0.5(5) . . . . ? C20 C21 C22 N1 -0.5(4) . . . . ? C23 C21 C22 N1 -177.2(3) . . . . ? C22 C21 C23 C24 -113.8(4) . . . . ? C20 C21 C23 C24 70.1(4) . . . . ? Co1 N2 C24 C23 104.2(2) . . . . ? Co1 N2 C24 C25 -16.8(3) . . . . ? C21 C23 C24 N2 66.5(3) . . . . ? C21 C23 C24 C25 -170.1(3) . . . . ? Co2 O7 C25 O8 -4.2(4) . . . . ? Co1 O7 C25 O8 -177.9(3) . . . . ? Co2 O7 C25 C24 174.41(19) . . . . ? Co1 O7 C25 C24 0.7(4) . . . . ? N2 C24 C25 O8 -170.0(3) . . . . ? C23 C24 C25 O8 65.9(4) . . . . ? N2 C24 C25 O7 11.4(4) . . . . ? C23 C24 C25 O7 -112.7(3) . . . . ? C33 N3 C26 C27 -176.4(4) . . . . ? C33 N3 C26 C31 2.2(4) . . . . ? N3 C26 C27 C28 178.5(4) . . . . ? C31 C26 C27 C28 0.2(6) . . . . ? C26 C27 C28 C29 0.9(6) . . . . ? C27 C28 C29 C30 -1.4(6) . . . . ? C28 C29 C30 C31 0.8(6) . . . . ? C29 C30 C31 C26 0.2(5) . . . . ? C29 C30 C31 C32 -176.0(3) . . . . ? N3 C26 C31 C30 -179.4(3) . . . . ? C27 C26 C31 C30 -0.7(5) . . . . ? N3 C26 C31 C32 -2.2(3) . . . . ? C27 C26 C31 C32 176.5(3) . . . . ? C30 C31 C32 C33 178.0(3) . . . . ? C26 C31 C32 C33 1.5(3) . . . . ? C30 C31 C32 C34 0.6(5) . . . . ? C26 C31 C32 C34 -175.9(3) . . . . ? C31 C32 C33 N3 -0.1(4) . . . . ? C34 C32 C33 N3 177.4(3) . . . . ? C26 N3 C33 C32 -1.3(4) . . . . ? C33 C32 C34 C35 102.1(3) . . . . ? C31 C32 C34 C35 -80.9(4) . . . . ? Co1 N4 C35 C34 153.3(2) . . . . ? Co1 N4 C35 C36 25.0(3) . . . . ? C32 C34 C35 N4 -47.6(4) . . . . ? C32 C34 C35 C36 79.7(3) . . . . ? Co2 O9 C36 O10 5.8(4) 1_455 . . . ? Co1 O9 C36 O10 177.2(2) . . . . ? Co2 O9 C36 C35 -171.06(17) 1_455 . . . ? Co1 O9 C36 C35 0.4(3) . . . . ? N4 C35 C36 O10 165.7(3) . . . . ? C34 C35 C36 O10 36.7(4) . . . . ? N4 C35 C36 O9 -17.4(3) . . . . ? C34 C35 C36 O9 -146.5(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O8 0.90 2.39 3.229(4) 155.7 1_455 N2 H2C O6 0.90 2.40 3.097(3) 134.4 2_857 N4 H4C O6 0.90 2.57 3.353(3) 146.5 2_857 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.487 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.048