# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'David J. Harding' _publ_contact_author_email hdavid@wu.ac.th loop_ _publ_author_name D.Harding P.Harding S.Dokmaisrijan H.Adams data_dh309p21c _database_code_depnum_ccdc_archive 'CCDC 789217' #TrackingRef 'web_deposit_cif_file_0_DavidJ.Harding_1281708532.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H42 B N7 Ni S2' _chemical_formula_weight 874.55 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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)/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 14.026(3) _cell_length_b 25.042(5) _cell_length_c 12.672(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.630(3) _cell_angle_gamma 90.00 _cell_volume 4343.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1211 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 18.91 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7905 _exptl_absorpt_correction_T_max 0.8528 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 38822 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8434 _reflns_number_gt 6077 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+5.7050P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8434 _refine_ls_number_parameters 569 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.013 _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 Ni1 Ni 0.26664(3) 0.632734(14) 0.18053(3) 0.01803(12) Uani 1 1 d . . . S1 S 0.18876(6) 0.63305(3) -0.00367(6) 0.0283(2) Uani 1 1 d . . . S2 S 0.10134(6) 0.66466(3) 0.17351(6) 0.0276(2) Uani 1 1 d . . . N1 N 0.28705(18) 0.59711(9) 0.32934(19) 0.0190(5) Uani 1 1 d . . . N2 N 0.37210(18) 0.60948(9) 0.40139(19) 0.0185(5) Uani 1 1 d . . . N3 N 0.40025(18) 0.59757(9) 0.17533(19) 0.0182(5) Uani 1 1 d . . . N4 N 0.47518(17) 0.60733(9) 0.26319(18) 0.0179(5) Uani 1 1 d . . . N5 N 0.33804(18) 0.70207(9) 0.23620(18) 0.0170(5) Uani 1 1 d . . . N6 N 0.41711(18) 0.69573(9) 0.32147(19) 0.0173(5) Uani 1 1 d . . . N7 N 0.0177(2) 0.68155(12) -0.0337(2) 0.0347(7) Uani 1 1 d . A . B1 B 0.4532(3) 0.63916(13) 0.3605(3) 0.0183(7) Uani 1 1 d . . . H1B H 0.5168 0.6411 0.4211 0.022 Uiso 1 1 d R . . C1 C 0.2400(2) 0.56108(12) 0.3783(2) 0.0198(7) Uani 1 1 d . . . C2 C 0.2940(2) 0.55109(12) 0.4828(2) 0.0222(7) Uani 1 1 d . . . H2 H 0.2767 0.5279 0.5349 0.027 Uiso 1 1 calc R . . C3 C 0.3777(2) 0.58168(11) 0.4950(2) 0.0181(6) Uani 1 1 d . . . C4 C 0.4409(2) 0.57370(11) 0.1006(2) 0.0184(6) Uani 1 1 d . . . C5 C 0.5414(2) 0.56895(11) 0.1385(2) 0.0220(7) Uani 1 1 d . . . H5 H 0.5869 0.5540 0.1012 0.026 Uiso 1 1 calc R . . C6 C 0.5616(2) 0.59045(11) 0.2417(2) 0.0197(7) Uani 1 1 d . . . C7 C 0.3184(2) 0.75478(12) 0.2291(2) 0.0187(6) Uani 1 1 d . . . C8 C 0.3826(2) 0.78205(12) 0.3119(2) 0.0225(7) Uani 1 1 d . . . H8 H 0.3833 0.8193 0.3264 0.027 Uiso 1 1 calc R . . C9 C 0.4447(2) 0.74390(11) 0.3682(2) 0.0184(6) Uani 1 1 d . . . C10 C 0.5270(2) 0.75090(11) 0.4617(2) 0.0194(6) Uani 1 1 d . . . C11 C 0.5122(2) 0.77877(12) 0.5524(2) 0.0226(7) Uani 1 1 d . . . H11 H 0.4497 0.7935 0.5523 0.027 Uiso 1 1 calc R . . C12 C 0.5874(2) 0.78512(12) 0.6422(3) 0.0262(7) Uani 1 1 d . . . H12 H 0.5763 0.8040 0.7034 0.031 Uiso 1 1 calc R . . C13 C 0.6793(3) 0.76385(13) 0.6432(3) 0.0286(8) Uani 1 1 d . . . H13 H 0.7308 0.7679 0.7053 0.034 Uiso 1 1 calc R . . C14 C 0.6951(2) 0.73676(13) 0.5532(3) 0.0261(7) Uani 1 1 d . . . H14 H 0.7579 0.7224 0.5535 0.031 Uiso 1 1 calc R . . C15 C 0.6201(2) 0.73046(12) 0.4629(2) 0.0234(7) Uani 1 1 d . . . H15 H 0.6318 0.7121 0.4014 0.028 Uiso 1 1 calc R . . C16 C 0.2452(2) 0.78029(11) 0.1422(2) 0.0203(7) Uani 1 1 d . . . C17 C 0.2393(2) 0.76799(13) 0.0338(3) 0.0252(7) Uani 1 1 d . . . H17 H 0.2793 0.7405 0.0150 0.030 Uiso 1 1 calc R . . C18 C 0.1756(2) 0.79558(14) -0.0469(3) 0.0306(8) Uani 1 1 d . . . H18 H 0.1721 0.7868 -0.1206 0.037 Uiso 1 1 calc R . . C19 C 0.1172(3) 0.83562(13) -0.0210(3) 0.0330(8) Uani 1 1 d . . . H19 H 0.0733 0.8543 -0.0764 0.040 Uiso 1 1 calc R . . C20 C 0.1232(3) 0.84836(14) 0.0871(3) 0.0339(8) Uani 1 1 d . . . H20 H 0.0828 0.8758 0.1053 0.041 Uiso 1 1 calc R . . C21 C 0.1873(2) 0.82158(13) 0.1683(3) 0.0273(7) Uani 1 1 d . . . H21 H 0.1919 0.8312 0.2418 0.033 Uiso 1 1 calc R . . C22 C 0.6579(2) 0.59587(12) 0.3164(3) 0.0220(7) Uani 1 1 d . . . C23 C 0.7369(2) 0.61087(12) 0.2713(3) 0.0278(7) Uani 1 1 d . . . H23 H 0.7264 0.6179 0.1960 0.033 Uiso 1 1 calc R . . C24 C 0.8303(3) 0.61551(14) 0.3359(3) 0.0373(9) Uani 1 1 d . . . H24 H 0.8834 0.6255 0.3046 0.045 Uiso 1 1 calc R . . C25 C 0.8462(3) 0.60558(15) 0.4465(3) 0.0411(10) Uani 1 1 d . . . H25 H 0.9099 0.6093 0.4908 0.049 Uiso 1 1 calc R . . C26 C 0.7690(3) 0.59022(13) 0.4918(3) 0.0351(9) Uani 1 1 d . . . H26 H 0.7799 0.5829 0.5670 0.042 Uiso 1 1 calc R . . C27 C 0.6753(2) 0.58554(12) 0.4270(3) 0.0270(7) Uani 1 1 d . . . H27 H 0.6226 0.5752 0.4586 0.032 Uiso 1 1 calc R . . C28 C 0.3805(2) 0.55500(11) -0.0040(2) 0.0185(6) Uani 1 1 d . . . C29 C 0.3042(2) 0.51856(11) -0.0067(2) 0.0209(7) Uani 1 1 d . . . H29 H 0.2917 0.5050 0.0590 0.025 Uiso 1 1 calc R . . C30 C 0.2471(2) 0.50228(12) -0.1046(3) 0.0249(7) Uani 1 1 d . . . H30 H 0.1960 0.4772 -0.1059 0.030 Uiso 1 1 calc R . . C31 C 0.2640(2) 0.52220(13) -0.2005(3) 0.0272(7) Uani 1 1 d . . . H31 H 0.2235 0.5116 -0.2674 0.033 Uiso 1 1 calc R . . C32 C 0.3398(2) 0.55760(13) -0.1989(2) 0.0267(7) Uani 1 1 d . . . H32 H 0.3516 0.5711 -0.2650 0.032 Uiso 1 1 calc R . . C33 C 0.3988(2) 0.57346(12) -0.1013(2) 0.0233(7) Uani 1 1 d . . . H33 H 0.4519 0.5971 -0.1009 0.028 Uiso 1 1 calc R . . C34 C 0.4628(2) 0.58483(12) 0.5869(2) 0.0195(7) Uani 1 1 d . . . C35 C 0.5102(2) 0.53768(12) 0.6284(2) 0.0228(7) Uani 1 1 d . . . H35 H 0.4872 0.5044 0.5969 0.027 Uiso 1 1 calc R . . C36 C 0.5900(2) 0.53888(13) 0.7146(3) 0.0293(8) Uani 1 1 d . . . H36 H 0.6218 0.5066 0.7417 0.035 Uiso 1 1 calc R . . C37 C 0.6235(3) 0.58757(14) 0.7614(3) 0.0323(8) Uani 1 1 d . . . H37 H 0.6787 0.5886 0.8201 0.039 Uiso 1 1 calc R . . C38 C 0.5762(3) 0.63490(13) 0.7221(3) 0.0304(8) Uani 1 1 d . . . H38 H 0.5986 0.6681 0.7547 0.036 Uiso 1 1 calc R . . C39 C 0.4963(2) 0.63345(12) 0.6354(2) 0.0248(7) Uani 1 1 d . . . H39 H 0.4643 0.6657 0.6088 0.030 Uiso 1 1 calc R . . C40 C 0.1506(2) 0.53369(11) 0.3206(2) 0.0213(7) Uani 1 1 d . . . C41 C 0.1396(2) 0.51914(13) 0.2123(3) 0.0275(7) Uani 1 1 d . . . H41 H 0.1865 0.5305 0.1731 0.033 Uiso 1 1 calc R . . C42 C 0.0603(3) 0.48809(14) 0.1611(3) 0.0359(9) Uani 1 1 d . . . H42 H 0.0533 0.4783 0.0874 0.043 Uiso 1 1 calc R . . C43 C -0.0078(3) 0.47166(14) 0.2177(3) 0.0371(9) Uani 1 1 d . . . H43 H -0.0612 0.4500 0.1834 0.044 Uiso 1 1 calc R . . C44 C 0.0014(3) 0.48657(14) 0.3242(3) 0.0361(9) Uani 1 1 d . . . H44 H -0.0465 0.4757 0.3625 0.043 Uiso 1 1 calc R . . C45 C 0.0800(2) 0.51732(13) 0.3756(3) 0.0294(8) Uani 1 1 d . . . H45 H 0.0858 0.5273 0.4491 0.035 Uiso 1 1 calc R . . C46 C 0.0935(2) 0.66212(13) 0.0367(3) 0.0278(8) Uani 1 1 d . . . C47 C 0.0097(3) 0.68270(18) -0.1529(3) 0.0460(11) Uani 1 1 d D . . H47B H -0.0023 0.6471 -0.1777 0.055 Uiso 1 1 d R A . H47A H 0.0779 0.6965 -0.1684 0.055 Uiso 1 1 d R . . C48 C -0.0718(6) 0.7238(4) -0.1914(5) 0.069(2) Uani 0.657(10) 1 d PDU A 1 H48A H -0.0431 0.7586 -0.2052 0.083 Uiso 0.657(10) 1 calc PR A 1 H48B H -0.1153 0.7116 -0.2594 0.083 Uiso 0.657(10) 1 calc PR A 1 C49 C -0.1265(7) 0.7298(5) -0.1090(4) 0.069(3) Uani 0.657(10) 1 d PDU A 1 H49A H -0.1883 0.7093 -0.1285 0.082 Uiso 0.657(10) 1 calc PR A 1 H49B H -0.1428 0.7679 -0.1015 0.082 Uiso 0.657(10) 1 calc PR A 1 C48' C -0.1013(5) 0.6838(8) -0.1979(10) 0.070(3) Uani 0.343(10) 1 d PDU A 2 H48C H -0.1183 0.7042 -0.2663 0.084 Uiso 0.343(10) 1 calc PR A 2 H48D H -0.1284 0.6472 -0.2102 0.084 Uiso 0.343(10) 1 calc PR A 2 C49' C -0.1354(12) 0.7102(9) -0.1128(7) 0.069(3) Uani 0.343(10) 1 d PDU A 2 H49C H -0.1975 0.6933 -0.1055 0.082 Uiso 0.343(10) 1 calc PR A 2 H49D H -0.1499 0.7479 -0.1339 0.082 Uiso 0.343(10) 1 calc PR A 2 C50 C -0.0649(3) 0.7091(2) -0.0031(3) 0.0523(12) Uani 1 1 d D . . H50A H -0.0983 0.6860 0.0371 0.063 Uiso 1 1 d R A . H50B H -0.0367 0.7389 0.0528 0.063 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0184(2) 0.0186(2) 0.0150(2) -0.00029(15) -0.00095(15) 0.00049(16) S1 0.0281(5) 0.0306(4) 0.0199(4) -0.0044(3) -0.0086(3) 0.0120(4) S2 0.0227(5) 0.0365(5) 0.0221(4) 0.0010(3) 0.0015(3) 0.0035(4) N1 0.0156(14) 0.0210(13) 0.0185(13) -0.0020(10) -0.0006(11) -0.0007(10) N2 0.0183(14) 0.0187(12) 0.0152(12) 0.0027(10) -0.0030(10) 0.0003(10) N3 0.0178(14) 0.0165(12) 0.0181(13) -0.0004(10) -0.0006(10) 0.0007(10) N4 0.0155(14) 0.0190(13) 0.0165(13) -0.0001(10) -0.0025(10) 0.0009(10) N5 0.0154(13) 0.0202(13) 0.0142(12) 0.0018(9) 0.0004(10) 0.0022(10) N6 0.0156(13) 0.0192(13) 0.0153(12) 0.0020(10) -0.0009(10) -0.0004(10) N7 0.0286(17) 0.0501(19) 0.0228(15) 0.0008(13) 0.0001(13) 0.0147(14) B1 0.0173(18) 0.0188(17) 0.0160(16) 0.0017(13) -0.0025(14) 0.0010(14) C1 0.0168(16) 0.0200(15) 0.0224(16) -0.0005(12) 0.0040(13) 0.0010(12) C2 0.0235(18) 0.0210(16) 0.0219(16) 0.0033(12) 0.0045(14) -0.0001(13) C3 0.0194(17) 0.0181(15) 0.0164(15) 0.0004(11) 0.0032(13) 0.0023(12) C4 0.0186(17) 0.0165(14) 0.0204(16) 0.0012(12) 0.0049(13) -0.0002(12) C5 0.0203(17) 0.0183(15) 0.0274(17) -0.0020(12) 0.0053(14) 0.0030(12) C6 0.0187(17) 0.0157(15) 0.0235(16) 0.0013(12) 0.0021(13) 0.0014(12) C7 0.0170(17) 0.0198(15) 0.0192(15) 0.0004(12) 0.0037(13) 0.0014(12) C8 0.0254(18) 0.0182(15) 0.0231(16) -0.0008(12) 0.0038(14) 0.0023(13) C9 0.0198(17) 0.0186(15) 0.0174(15) -0.0009(12) 0.0051(13) -0.0018(12) C10 0.0198(17) 0.0178(15) 0.0189(15) 0.0005(12) 0.0007(13) -0.0028(12) C11 0.0228(18) 0.0182(15) 0.0248(17) -0.0014(12) 0.0009(14) -0.0001(13) C12 0.033(2) 0.0227(16) 0.0211(17) -0.0048(13) 0.0014(14) -0.0005(14) C13 0.031(2) 0.0267(17) 0.0230(17) -0.0029(13) -0.0054(15) -0.0012(14) C14 0.0186(17) 0.0289(17) 0.0284(18) 0.0000(13) -0.0002(14) -0.0007(13) C15 0.0254(18) 0.0226(16) 0.0212(16) -0.0031(12) 0.0028(14) -0.0029(13) C16 0.0197(17) 0.0164(15) 0.0238(16) 0.0047(12) 0.0025(13) -0.0010(12) C17 0.0236(18) 0.0266(17) 0.0245(17) 0.0024(13) 0.0031(14) 0.0045(14) C18 0.030(2) 0.038(2) 0.0215(17) 0.0059(14) -0.0001(15) 0.0021(15) C19 0.030(2) 0.0292(19) 0.035(2) 0.0118(15) -0.0039(16) 0.0058(15) C20 0.028(2) 0.0292(18) 0.041(2) 0.0020(15) -0.0013(16) 0.0108(15) C21 0.0252(19) 0.0278(18) 0.0281(18) -0.0011(13) 0.0043(15) 0.0032(14) C22 0.0158(17) 0.0164(15) 0.0315(18) -0.0037(13) 0.0000(13) 0.0015(12) C23 0.0244(19) 0.0212(16) 0.0356(19) -0.0010(14) 0.0016(15) 0.0022(14) C24 0.0204(19) 0.034(2) 0.053(2) 0.0033(17) -0.0003(17) -0.0011(15) C25 0.019(2) 0.037(2) 0.059(3) -0.0004(18) -0.0094(18) 0.0000(16) C26 0.031(2) 0.0291(18) 0.037(2) -0.0001(15) -0.0117(16) 0.0023(15) C27 0.0245(18) 0.0193(16) 0.0336(19) 0.0008(13) -0.0018(15) 0.0018(13) C28 0.0188(17) 0.0171(15) 0.0190(15) -0.0029(11) 0.0027(13) 0.0059(12) C29 0.0232(18) 0.0193(15) 0.0208(16) -0.0003(12) 0.0058(13) 0.0037(13) C30 0.0182(17) 0.0240(16) 0.0303(18) -0.0057(13) 0.0010(14) 0.0020(13) C31 0.0236(19) 0.0335(18) 0.0219(17) -0.0055(14) -0.0003(14) 0.0079(14) C32 0.031(2) 0.0317(18) 0.0174(16) 0.0007(13) 0.0050(14) 0.0075(15) C33 0.0225(18) 0.0206(16) 0.0274(17) 0.0007(13) 0.0066(14) 0.0020(13) C34 0.0218(17) 0.0226(16) 0.0136(15) 0.0018(11) 0.0030(13) 0.0006(12) C35 0.0273(18) 0.0213(16) 0.0189(16) 0.0012(12) 0.0026(14) -0.0011(13) C36 0.030(2) 0.0308(18) 0.0239(17) 0.0072(14) -0.0009(15) 0.0059(15) C37 0.028(2) 0.039(2) 0.0233(18) 0.0049(14) -0.0076(15) -0.0043(15) C38 0.037(2) 0.0287(18) 0.0223(17) -0.0005(14) 0.0005(15) -0.0084(15) C39 0.0310(19) 0.0222(16) 0.0200(16) 0.0036(13) 0.0029(14) 0.0006(14) C40 0.0182(17) 0.0176(15) 0.0269(17) 0.0021(12) 0.0021(13) 0.0025(12) C41 0.0219(18) 0.0296(18) 0.0303(18) -0.0037(14) 0.0041(15) -0.0005(14) C42 0.029(2) 0.038(2) 0.036(2) -0.0108(16) -0.0056(17) -0.0002(16) C43 0.0186(19) 0.0282(19) 0.058(3) -0.0020(17) -0.0065(18) -0.0034(14) C44 0.0201(19) 0.039(2) 0.048(2) 0.0080(17) 0.0039(16) -0.0047(15) C45 0.0234(19) 0.0345(19) 0.0295(18) 0.0021(14) 0.0040(15) -0.0005(15) C46 0.0277(19) 0.0269(18) 0.0253(17) -0.0016(13) -0.0021(15) 0.0027(14) C47 0.039(2) 0.070(3) 0.0244(19) -0.0016(18) -0.0021(17) 0.023(2) C48 0.062(3) 0.112(6) 0.029(2) 0.014(3) 0.001(2) 0.057(4) C49 0.063(3) 0.112(6) 0.028(2) 0.009(3) 0.001(2) 0.064(4) C48' 0.063(4) 0.112(6) 0.030(3) 0.014(4) -0.001(3) 0.057(5) C49' 0.062(3) 0.112(6) 0.029(2) 0.012(3) 0.001(2) 0.059(4) C50 0.031(2) 0.090(3) 0.034(2) 0.007(2) 0.0029(18) 0.029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.049(2) . ? Ni1 N5 2.051(2) . ? Ni1 N3 2.085(2) . ? Ni1 S1 2.3510(9) . ? Ni1 S2 2.4357(10) . ? S1 C46 1.696(3) . ? S2 C46 1.715(3) . ? N1 C1 1.347(4) . ? N1 N2 1.370(3) . ? N2 C3 1.363(4) . ? N2 B1 1.540(4) . ? N3 C4 1.347(4) . ? N3 N4 1.376(3) . ? N4 C6 1.366(4) . ? N4 B1 1.555(4) . ? N5 C7 1.347(4) . ? N5 N6 1.378(3) . ? N6 C9 1.362(4) . ? N6 B1 1.548(4) . ? N7 C46 1.322(4) . ? N7 C50 1.472(5) . ? N7 C47 1.490(4) . ? B1 H1B 1.0432 . ? C1 C2 1.397(4) . ? C1 C40 1.475(4) . ? C2 C3 1.381(4) . ? C2 H2 0.9500 . ? C3 C34 1.476(4) . ? C4 C5 1.392(4) . ? C4 C28 1.484(4) . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 C22 1.477(4) . ? C7 C8 1.402(4) . ? C7 C16 1.477(4) . ? C8 C9 1.382(4) . ? C8 H8 0.9500 . ? C9 C10 1.472(4) . ? C10 C11 1.399(4) . ? C10 C15 1.399(4) . ? C11 C12 1.381(4) . ? C11 H11 0.9500 . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C14 1.386(4) . ? C13 H13 0.9500 . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.392(4) . ? C16 C21 1.399(4) . ? C17 C18 1.387(4) . ? C17 H17 0.9500 . ? C18 C19 1.379(5) . ? C18 H18 0.9500 . ? C19 C20 1.391(5) . ? C19 H19 0.9500 . ? C20 C21 1.383(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.394(5) . ? C22 C23 1.404(5) . ? C23 C24 1.389(5) . ? C23 H23 0.9500 . ? C24 C25 1.393(5) . ? C24 H24 0.9500 . ? C25 C26 1.387(5) . ? C25 H25 0.9500 . ? C26 C27 1.394(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.393(4) . ? C28 C29 1.401(4) . ? C29 C30 1.383(4) . ? C29 H29 0.9500 . ? C30 C31 1.381(5) . ? C30 H30 0.9500 . ? C31 C32 1.381(5) . ? C31 H31 0.9500 . ? C32 C33 1.387(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.398(4) . ? C34 C35 1.400(4) . ? C35 C36 1.383(4) . ? C35 H35 0.9500 . ? C36 C37 1.392(5) . ? C36 H36 0.9500 . ? C37 C38 1.396(5) . ? C37 H37 0.9500 . ? C38 C39 1.387(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.392(5) . ? C40 C41 1.396(4) . ? C41 C42 1.395(5) . ? C41 H41 0.9500 . ? C42 C43 1.377(5) . ? C42 H42 0.9500 . ? C43 C44 1.379(5) . ? C43 H43 0.9500 . ? C44 C45 1.385(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C47 C48' 1.538(6) . ? C47 C48 1.538(6) . ? C47 H47B 0.9475 . ? C47 H47A 1.0749 . ? C48 C49 1.432(8) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.519(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C48' C49' 1.433(8) . ? C48' H48C 0.9900 . ? C48' H48D 0.9900 . ? C49' C50 1.519(6) . ? C49' H49C 0.9900 . ? C49' H49D 0.9900 . ? C50 H50A 0.9582 . ? C50 H50B 1.0451 . ? 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 N5 95.31(9) . . ? N1 Ni1 N3 84.23(10) . . ? N5 Ni1 N3 89.64(9) . . ? N1 Ni1 S1 148.92(7) . . ? N5 Ni1 S1 115.12(7) . . ? N3 Ni1 S1 101.29(7) . . ? N1 Ni1 S2 96.71(7) . . ? N5 Ni1 S2 97.12(7) . . ? N3 Ni1 S2 173.04(7) . . ? S1 Ni1 S2 74.38(3) . . ? C46 S1 Ni1 85.87(11) . . ? C46 S2 Ni1 82.82(12) . . ? C1 N1 N2 106.7(2) . . ? C1 N1 Ni1 137.0(2) . . ? N2 N1 Ni1 116.18(18) . . ? C3 N2 N1 109.9(2) . . ? C3 N2 B1 129.3(2) . . ? N1 N2 B1 119.0(2) . . ? C4 N3 N4 106.4(2) . . ? C4 N3 Ni1 137.0(2) . . ? N4 N3 Ni1 115.62(17) . . ? C6 N4 N3 109.8(2) . . ? C6 N4 B1 130.9(2) . . ? N3 N4 B1 118.9(2) . . ? C7 N5 N6 106.4(2) . . ? C7 N5 Ni1 136.8(2) . . ? N6 N5 Ni1 114.89(17) . . ? C9 N6 N5 110.0(2) . . ? C9 N6 B1 129.0(2) . . ? N5 N6 B1 120.4(2) . . ? C46 N7 C50 123.9(3) . . ? C46 N7 C47 124.2(3) . . ? C50 N7 C47 111.6(3) . . ? N2 B1 N6 109.6(2) . . ? N2 B1 N4 108.0(2) . . ? N6 B1 N4 108.9(2) . . ? N2 B1 H1B 110.6 . . ? N6 B1 H1B 111.1 . . ? N4 B1 H1B 108.7 . . ? N1 C1 C2 109.8(3) . . ? N1 C1 C40 122.2(3) . . ? C2 C1 C40 127.8(3) . . ? C3 C2 C1 106.2(3) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? N2 C3 C2 107.5(3) . . ? N2 C3 C34 122.8(3) . . ? C2 C3 C34 129.7(3) . . ? N3 C4 C5 110.4(3) . . ? N3 C4 C28 121.4(3) . . ? C5 C4 C28 128.2(3) . . ? C6 C5 C4 105.9(3) . . ? C6 C5 H5 127.0 . . ? C4 C5 H5 127.0 . . ? N4 C6 C5 107.6(3) . . ? N4 C6 C22 124.9(3) . . ? C5 C6 C22 127.5(3) . . ? N5 C7 C8 109.8(3) . . ? N5 C7 C16 124.9(3) . . ? C8 C7 C16 125.2(3) . . ? C9 C8 C7 106.2(3) . . ? C9 C8 H8 126.9 . . ? C7 C8 H8 126.9 . . ? N6 C9 C8 107.5(3) . . ? N6 C9 C10 123.6(3) . . ? C8 C9 C10 128.9(3) . . ? C11 C10 C15 118.6(3) . . ? C11 C10 C9 119.3(3) . . ? C15 C10 C9 122.1(3) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.6(3) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C10 120.5(3) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? C17 C16 C21 119.0(3) . . ? C17 C16 C7 121.4(3) . . ? C21 C16 C7 119.2(3) . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.5(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 119.4(3) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C16 119.9(3) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? C27 C22 C23 118.6(3) . . ? C27 C22 C6 124.1(3) . . ? C23 C22 C6 117.2(3) . . ? C24 C23 C22 120.6(3) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.0(4) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 119.9(3) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.1(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C22 C27 C26 120.8(3) . . ? C22 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C33 C28 C29 118.8(3) . . ? C33 C28 C4 120.5(3) . . ? C29 C28 C4 120.7(3) . . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 120.4(3) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 119.9(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 120.2(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 120.4(3) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C39 C34 C35 118.9(3) . . ? C39 C34 C3 122.0(3) . . ? C35 C34 C3 119.1(3) . . ? C36 C35 C34 120.9(3) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 119.7(3) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C36 C37 C38 120.1(3) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C39 C38 C37 119.9(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 120.5(3) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? C45 C40 C41 118.5(3) . . ? C45 C40 C1 120.6(3) . . ? C41 C40 C1 120.5(3) . . ? C40 C41 C42 120.5(3) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C43 C42 C41 119.8(3) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 120.1(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C45 120.3(3) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C40 120.6(3) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? N7 C46 S1 121.7(3) . . ? N7 C46 S2 122.2(3) . . ? S1 C46 S2 116.11(19) . . ? N7 C47 C48' 102.8(6) . . ? N7 C47 C48 102.7(4) . . ? C48' C47 C48 41.2(6) . . ? N7 C47 H47B 106.6 . . ? C48' C47 H47B 78.5 . . ? C48 C47 H47B 117.3 . . ? N7 C47 H47A 108.6 . . ? C48' C47 H47A 142.8 . . ? C48 C47 H47A 110.9 . . ? H47B C47 H47A 110.1 . . ? C49 C48 C47 108.6(5) . . ? C49 C48 H48A 110.0 . . ? C47 C48 H48A 110.0 . . ? C49 C48 H48B 110.0 . . ? C47 C48 H48B 110.0 . . ? H48A C48 H48B 108.3 . . ? C48 C49 C50 108.4(5) . . ? C48 C49 H49A 110.0 . . ? C50 C49 H49A 110.0 . . ? C48 C49 H49B 110.0 . . ? C50 C49 H49B 110.0 . . ? H49A C49 H49B 108.4 . . ? C49' C48' C47 101.9(11) . . ? C49' C48' H48C 111.4 . . ? C47 C48' H48C 111.4 . . ? C49' C48' H48D 111.4 . . ? C47 C48' H48D 111.4 . . ? H48C C48' H48D 109.2 . . ? C48' C49' C50 115.0(9) . . ? C48' C49' H49C 108.5 . . ? C50 C49' H49C 108.5 . . ? C48' C49' H49D 108.5 . . ? C50 C49' H49D 108.5 . . ? H49C C49' H49D 107.5 . . ? N7 C50 C49 104.9(4) . . ? N7 C50 C49' 99.2(6) . . ? C49 C50 C49' 19.2(12) . . ? N7 C50 H50A 111.2 . . ? C49 C50 H50A 115.2 . . ? C49' C50 H50A 101.5 . . ? N7 C50 H50B 108.1 . . ? C49 C50 H50B 114.4 . . ? C49' C50 H50B 133.0 . . ? H50A C50 H50B 103.1 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.493 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.071 # Attachment 'web_deposit_cif_file_1_DavidJ.Harding_1281708532.cif' data_dh310p21c _database_code_depnum_ccdc_archive 'CCDC 789218' #TrackingRef 'web_deposit_cif_file_1_DavidJ.Harding_1281708532.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H42 B Co N7 S2' _chemical_formula_weight 874.77 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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)/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 13.960(5) _cell_length_b 25.122(10) _cell_length_c 12.649(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.047(5) _cell_angle_gamma 90.00 _cell_volume 4339(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1751 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 24.62 _exptl_crystal_description block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8060 _exptl_absorpt_correction_T_max 0.8643 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 38601 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8443 _reflns_number_gt 6519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+1.5088P] 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 8443 _refine_ls_number_parameters 569 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.026 _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 0.261496(19) 0.635458(10) 0.18181(2) 0.01754(9) Uani 1 1 d . . . S1 S 0.18273(4) 0.62887(2) -0.00258(4) 0.02712(14) Uani 1 1 d . . . S2 S 0.09430(4) 0.66665(2) 0.17474(4) 0.02488(13) Uani 1 1 d . . . N1 N 0.28605(12) 0.59653(6) 0.33084(13) 0.0179(4) Uani 1 1 d . . . N2 N 0.37129(12) 0.60919(6) 0.40145(13) 0.0175(4) Uani 1 1 d . . . N3 N 0.39997(12) 0.59799(6) 0.17520(13) 0.0172(3) Uani 1 1 d . . . N4 N 0.47479(11) 0.60789(6) 0.26214(13) 0.0171(4) Uani 1 1 d . . . N5 N 0.34014(12) 0.70329(6) 0.23799(13) 0.0174(4) Uani 1 1 d . . . N6 N 0.41771(12) 0.69598(6) 0.32280(13) 0.0167(3) Uani 1 1 d . . . N7 N 0.01367(13) 0.68112(8) -0.03301(14) 0.0290(4) Uani 1 1 d . A . B1 B 0.45243(17) 0.63920(9) 0.35980(18) 0.0176(5) Uani 1 1 d . . . H1B H 0.5161 0.6412 0.4203 0.021 Uiso 1 1 d R . . C1 C 0.23951(15) 0.56054(8) 0.38036(16) 0.0193(4) Uani 1 1 d . . . C2 C 0.29397(15) 0.55043(8) 0.48409(16) 0.0199(4) Uani 1 1 d . . . H2 H 0.2772 0.5271 0.5365 0.024 Uiso 1 1 calc R . . C3 C 0.37744(15) 0.58134(7) 0.49500(16) 0.0186(4) Uani 1 1 d . . . C4 C 0.44063(15) 0.57414(7) 0.10024(16) 0.0182(4) Uani 1 1 d . . . C5 C 0.54125(15) 0.56982(8) 0.13682(16) 0.0209(4) Uani 1 1 d . . . H5 H 0.5870 0.5552 0.0989 0.025 Uiso 1 1 calc R . . C6 C 0.56122(14) 0.59124(7) 0.24007(16) 0.0190(4) Uani 1 1 d . . . C7 C 0.32133(14) 0.75627(8) 0.23234(16) 0.0182(4) Uani 1 1 d . . . C8 C 0.38531(15) 0.78243(8) 0.31547(16) 0.0210(4) Uani 1 1 d . . . H8 H 0.3868 0.8195 0.3310 0.025 Uiso 1 1 calc R . . C9 C 0.44618(15) 0.74360(8) 0.37079(16) 0.0189(4) Uani 1 1 d . . . C10 C 0.52855(15) 0.74995(7) 0.46385(16) 0.0187(4) Uani 1 1 d . . . C11 C 0.51339(16) 0.77817(8) 0.55416(17) 0.0222(5) Uani 1 1 d . . . H11 H 0.4510 0.7933 0.5541 0.027 Uiso 1 1 calc R . . C12 C 0.58879(16) 0.78412(8) 0.64379(17) 0.0254(5) Uani 1 1 d . . . H12 H 0.5778 0.8031 0.7052 0.031 Uiso 1 1 calc R . . C13 C 0.68009(17) 0.76251(8) 0.64416(18) 0.0277(5) Uani 1 1 d . . . H13 H 0.7316 0.7664 0.7059 0.033 Uiso 1 1 calc R . . C14 C 0.69613(16) 0.73512(8) 0.55429(17) 0.0255(5) Uani 1 1 d . . . H14 H 0.7589 0.7205 0.5543 0.031 Uiso 1 1 calc R . . C15 C 0.62108(15) 0.72896(8) 0.46477(17) 0.0219(5) Uani 1 1 d . . . H15 H 0.6327 0.7103 0.4034 0.026 Uiso 1 1 calc R . . C16 C 0.24878(15) 0.78129(8) 0.14553(16) 0.0197(4) Uani 1 1 d . . . C17 C 0.23980(15) 0.76633(8) 0.03790(17) 0.0238(5) Uani 1 1 d . . . H17 H 0.2781 0.7377 0.0202 0.029 Uiso 1 1 calc R . . C18 C 0.17549(17) 0.79272(9) -0.04372(18) 0.0303(5) Uani 1 1 d . . . H18 H 0.1699 0.7822 -0.1169 0.036 Uiso 1 1 calc R . . C19 C 0.11947(17) 0.83444(9) -0.01831(19) 0.0325(5) Uani 1 1 d . . . H19 H 0.0752 0.8525 -0.0740 0.039 Uiso 1 1 calc R . . C20 C 0.12819(17) 0.84969(9) 0.0885(2) 0.0337(6) Uani 1 1 d . . . H20 H 0.0894 0.8782 0.1059 0.040 Uiso 1 1 calc R . . C21 C 0.19264(16) 0.82391(8) 0.16997(18) 0.0263(5) Uani 1 1 d . . . H21 H 0.1989 0.8351 0.2428 0.032 Uiso 1 1 calc R . . C22 C 0.65851(15) 0.59674(8) 0.31317(17) 0.0219(4) Uani 1 1 d . . . C23 C 0.73746(15) 0.61173(8) 0.26815(19) 0.0264(5) Uani 1 1 d . . . H23 H 0.7269 0.6190 0.1929 0.032 Uiso 1 1 calc R . . C24 C 0.83103(17) 0.61620(9) 0.3312(2) 0.0350(6) Uani 1 1 d . . . H24 H 0.8842 0.6263 0.2993 0.042 Uiso 1 1 calc R . . C25 C 0.84645(17) 0.60583(9) 0.4413(2) 0.0383(6) Uani 1 1 d . . . H25 H 0.9103 0.6092 0.4851 0.046 Uiso 1 1 calc R . . C26 C 0.76938(17) 0.59065(9) 0.4872(2) 0.0332(6) Uani 1 1 d . . . H26 H 0.7804 0.5835 0.5625 0.040 Uiso 1 1 calc R . . C27 C 0.67565(16) 0.58571(8) 0.42368(18) 0.0247(5) Uani 1 1 d . . . H27 H 0.6230 0.5748 0.4557 0.030 Uiso 1 1 calc R . . C28 C 0.38029(14) 0.55496(7) -0.00316(16) 0.0180(4) Uani 1 1 d . . . C29 C 0.30444(15) 0.51868(8) -0.00413(16) 0.0202(4) Uani 1 1 d . . . H29 H 0.2920 0.5056 0.0622 0.024 Uiso 1 1 calc R . . C30 C 0.24730(15) 0.50172(8) -0.10092(17) 0.0240(5) Uani 1 1 d . . . H30 H 0.1961 0.4768 -0.1010 0.029 Uiso 1 1 calc R . . C31 C 0.26447(16) 0.52098(8) -0.19758(17) 0.0253(5) Uani 1 1 d . . . H31 H 0.2242 0.5099 -0.2640 0.030 Uiso 1 1 calc R . . C32 C 0.34018(16) 0.55638(9) -0.19774(17) 0.0265(5) Uani 1 1 d . . . H32 H 0.3519 0.5696 -0.2642 0.032 Uiso 1 1 calc R . . C33 C 0.39897(15) 0.57256(8) -0.10101(17) 0.0227(5) Uani 1 1 d . . . H33 H 0.4525 0.5959 -0.1015 0.027 Uiso 1 1 calc R . . C34 C 0.46271(15) 0.58431(8) 0.58626(15) 0.0194(4) Uani 1 1 d . . . C35 C 0.50972(15) 0.53735(8) 0.62730(16) 0.0221(5) Uani 1 1 d . . . H35 H 0.4866 0.5041 0.5962 0.027 Uiso 1 1 calc R . . C36 C 0.58963(16) 0.53877(9) 0.71282(17) 0.0283(5) Uani 1 1 d . . . H36 H 0.6218 0.5067 0.7395 0.034 Uiso 1 1 calc R . . C37 C 0.62275(17) 0.58700(9) 0.75952(18) 0.0308(5) Uani 1 1 d . . . H37 H 0.6777 0.5880 0.8182 0.037 Uiso 1 1 calc R . . C38 C 0.57549(17) 0.63394(9) 0.72045(18) 0.0300(5) Uani 1 1 d . . . H38 H 0.5979 0.6670 0.7531 0.036 Uiso 1 1 calc R . . C39 C 0.49611(16) 0.63284(8) 0.63450(17) 0.0242(5) Uani 1 1 d . . . H39 H 0.4642 0.6650 0.6081 0.029 Uiso 1 1 calc R . . C40 C 0.15029(15) 0.53310(8) 0.32356(17) 0.0206(4) Uani 1 1 d . . . C41 C 0.13921(16) 0.51942(9) 0.21483(18) 0.0273(5) Uani 1 1 d . . . H41 H 0.1862 0.5310 0.1753 0.033 Uiso 1 1 calc R . . C42 C 0.05985(17) 0.48892(9) 0.1639(2) 0.0342(6) Uani 1 1 d . . . H42 H 0.0531 0.4796 0.0900 0.041 Uiso 1 1 calc R . . C43 C -0.00906(16) 0.47214(9) 0.2204(2) 0.0330(6) Uani 1 1 d . . . H43 H -0.0627 0.4508 0.1858 0.040 Uiso 1 1 calc R . . C44 C 0.00032(17) 0.48643(9) 0.3276(2) 0.0342(6) Uani 1 1 d . . . H44 H -0.0479 0.4757 0.3662 0.041 Uiso 1 1 calc R . . C45 C 0.07982(16) 0.51641(9) 0.37894(19) 0.0289(5) Uani 1 1 d . . . H45 H 0.0861 0.5256 0.4529 0.035 Uiso 1 1 calc R . . C46 C 0.08737(15) 0.66104(8) 0.03817(17) 0.0226(5) Uani 1 1 d . . . C47 C 0.00666(19) 0.67999(11) -0.15167(18) 0.0386(6) Uani 1 1 d D . . H47B H -0.0053 0.6444 -0.1764 0.046 Uiso 1 1 d R A . H47A H 0.0749 0.6938 -0.1671 0.046 Uiso 1 1 d R . . C48 C -0.0734(4) 0.7211(3) -0.1925(3) 0.0564(14) Uani 0.742(8) 1 d PDU A 1 H48A H -0.0434 0.7551 -0.2083 0.068 Uiso 0.742(8) 1 calc PR A 1 H48B H -0.1166 0.7083 -0.2599 0.068 Uiso 0.742(8) 1 calc PR A 1 C49 C -0.1288(4) 0.7291(3) -0.1118(3) 0.0579(14) Uani 0.742(8) 1 d PDU A 1 H49A H -0.1896 0.7077 -0.1283 0.069 Uiso 0.742(8) 1 calc PR A 1 H49B H -0.1472 0.7671 -0.1093 0.069 Uiso 0.742(8) 1 calc PR A 1 C48' C -0.1031(4) 0.6880(8) -0.1953(9) 0.0580(16) Uani 0.258(8) 1 d PDU A 2 H48C H -0.1143 0.7131 -0.2569 0.070 Uiso 0.258(8) 1 calc PR A 2 H48D H -0.1349 0.6537 -0.2200 0.070 Uiso 0.258(8) 1 calc PR A 2 C49' C -0.1420(8) 0.7089(7) -0.1090(6) 0.0579(16) Uani 0.258(8) 1 d PDU A 2 H49C H -0.1969 0.6861 -0.0979 0.069 Uiso 0.258(8) 1 calc PR A 2 H49D H -0.1686 0.7449 -0.1289 0.069 Uiso 0.258(8) 1 calc PR A 2 C50 C -0.06671(18) 0.71233(12) -0.0041(2) 0.0432(7) Uani 1 1 d D . . H50A H -0.1001 0.6892 0.0361 0.052 Uiso 1 1 d R A . H50B H -0.0385 0.7421 0.0518 0.052 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01770(15) 0.01619(14) 0.01634(15) 0.00015(11) -0.00197(11) 0.00062(11) S1 0.0261(3) 0.0315(3) 0.0200(3) -0.0058(2) -0.0040(2) 0.0120(2) S2 0.0207(3) 0.0327(3) 0.0193(3) 0.0011(2) -0.0003(2) 0.0041(2) N1 0.0159(9) 0.0180(8) 0.0181(9) 0.0000(7) -0.0002(7) 0.0004(7) N2 0.0173(9) 0.0174(8) 0.0153(9) -0.0001(7) -0.0022(7) 0.0002(7) N3 0.0173(9) 0.0155(8) 0.0162(8) -0.0004(7) -0.0020(7) 0.0005(7) N4 0.0156(9) 0.0148(8) 0.0182(9) 0.0012(7) -0.0027(7) 0.0009(7) N5 0.0172(9) 0.0176(8) 0.0154(9) 0.0010(7) -0.0013(7) 0.0019(7) N6 0.0162(8) 0.0165(8) 0.0155(8) 0.0006(7) -0.0011(7) 0.0003(7) N7 0.0251(10) 0.0387(11) 0.0206(10) -0.0011(8) -0.0013(8) 0.0113(8) B1 0.0171(11) 0.0167(11) 0.0170(11) 0.0018(9) -0.0008(9) -0.0001(9) C1 0.0197(11) 0.0169(10) 0.0211(11) -0.0002(8) 0.0038(9) 0.0016(8) C2 0.0221(11) 0.0181(10) 0.0188(11) 0.0030(8) 0.0026(9) 0.0000(8) C3 0.0213(11) 0.0151(9) 0.0183(10) 0.0002(8) 0.0020(8) 0.0027(8) C4 0.0212(11) 0.0123(9) 0.0202(11) 0.0009(8) 0.0020(9) 0.0010(8) C5 0.0196(11) 0.0186(10) 0.0244(11) -0.0016(8) 0.0046(9) 0.0027(8) C6 0.0200(11) 0.0122(9) 0.0234(11) 0.0013(8) 0.0016(9) 0.0011(8) C7 0.0196(11) 0.0164(10) 0.0181(10) 0.0016(8) 0.0025(8) 0.0004(8) C8 0.0220(11) 0.0160(10) 0.0234(11) -0.0008(8) 0.0011(9) 0.0003(8) C9 0.0208(11) 0.0173(10) 0.0179(11) -0.0004(8) 0.0027(8) -0.0008(8) C10 0.0222(11) 0.0136(9) 0.0191(11) 0.0020(8) 0.0013(8) -0.0028(8) C11 0.0239(11) 0.0155(10) 0.0258(12) -0.0015(9) 0.0020(9) -0.0007(8) C12 0.0325(13) 0.0204(10) 0.0214(11) -0.0042(9) 0.0008(9) -0.0003(9) C13 0.0298(13) 0.0252(11) 0.0226(12) -0.0008(9) -0.0069(10) -0.0017(9) C14 0.0200(11) 0.0250(11) 0.0289(12) -0.0003(9) -0.0012(9) -0.0001(9) C15 0.0252(12) 0.0197(10) 0.0199(11) -0.0018(8) 0.0026(9) -0.0039(9) C16 0.0186(10) 0.0160(9) 0.0231(11) 0.0030(8) 0.0010(9) -0.0012(8) C17 0.0218(11) 0.0241(11) 0.0241(11) 0.0011(9) 0.0018(9) 0.0033(9) C18 0.0317(13) 0.0345(13) 0.0227(12) 0.0058(10) 0.0010(10) 0.0010(10) C19 0.0295(13) 0.0294(12) 0.0331(14) 0.0124(10) -0.0057(10) 0.0055(10) C20 0.0308(13) 0.0243(11) 0.0425(15) 0.0048(10) -0.0005(11) 0.0102(10) C21 0.0272(12) 0.0219(11) 0.0283(12) -0.0008(9) 0.0019(10) 0.0020(9) C22 0.0216(11) 0.0110(9) 0.0298(12) -0.0037(8) -0.0025(9) 0.0018(8) C23 0.0229(12) 0.0197(10) 0.0350(13) -0.0014(9) 0.0021(10) 0.0016(9) C24 0.0217(12) 0.0287(12) 0.0517(16) -0.0001(11) 0.0011(11) -0.0025(10) C25 0.0218(12) 0.0326(13) 0.0524(17) 0.0002(12) -0.0111(11) -0.0007(10) C26 0.0329(13) 0.0243(11) 0.0359(14) 0.0006(10) -0.0081(11) 0.0027(10) C27 0.0236(11) 0.0157(10) 0.0314(12) 0.0011(9) -0.0021(9) 0.0042(8) C28 0.0184(10) 0.0145(9) 0.0204(11) -0.0013(8) 0.0023(8) 0.0053(8) C29 0.0223(11) 0.0185(10) 0.0199(11) 0.0001(8) 0.0045(9) 0.0037(8) C30 0.0194(11) 0.0204(10) 0.0296(12) -0.0058(9) -0.0009(9) 0.0022(9) C31 0.0230(11) 0.0295(12) 0.0200(11) -0.0049(9) -0.0031(9) 0.0078(9) C32 0.0328(13) 0.0288(11) 0.0184(11) 0.0025(9) 0.0070(10) 0.0081(10) C33 0.0239(11) 0.0178(10) 0.0264(12) 0.0013(9) 0.0055(9) 0.0026(8) C34 0.0214(11) 0.0203(10) 0.0159(10) 0.0021(8) 0.0026(8) 0.0002(8) C35 0.0276(12) 0.0187(10) 0.0188(11) 0.0020(8) 0.0020(9) -0.0001(9) C36 0.0290(13) 0.0285(12) 0.0243(12) 0.0068(9) -0.0014(10) 0.0057(10) C37 0.0294(13) 0.0360(13) 0.0215(12) 0.0041(10) -0.0075(10) -0.0050(10) C38 0.0372(14) 0.0272(12) 0.0220(12) -0.0017(9) -0.0016(10) -0.0078(10) C39 0.0311(12) 0.0199(10) 0.0198(11) 0.0030(8) 0.0007(9) 0.0008(9) C40 0.0187(11) 0.0160(10) 0.0252(11) 0.0018(8) 0.0000(9) 0.0019(8) C41 0.0236(12) 0.0287(12) 0.0280(12) -0.0015(9) 0.0019(10) -0.0023(9) C42 0.0297(13) 0.0355(13) 0.0321(13) -0.0091(11) -0.0055(11) 0.0004(10) C43 0.0206(12) 0.0239(11) 0.0490(16) -0.0008(11) -0.0050(11) -0.0031(9) C44 0.0230(12) 0.0352(13) 0.0432(15) 0.0058(11) 0.0039(11) -0.0050(10) C45 0.0262(12) 0.0310(12) 0.0283(12) 0.0025(10) 0.0034(10) -0.0033(10) C46 0.0212(11) 0.0212(10) 0.0223(11) -0.0017(9) -0.0022(9) 0.0010(9) C47 0.0371(14) 0.0535(16) 0.0207(12) -0.0027(11) -0.0040(11) 0.0185(12) C48 0.049(2) 0.087(3) 0.0312(15) 0.015(2) 0.0023(14) 0.039(2) C49 0.052(2) 0.085(3) 0.0320(15) 0.0116(18) -0.0017(14) 0.044(2) C48' 0.051(2) 0.087(4) 0.032(2) 0.013(3) -0.002(2) 0.040(3) C49' 0.050(2) 0.088(4) 0.032(2) 0.013(2) 0.000(2) 0.040(3) C50 0.0300(14) 0.0689(18) 0.0285(13) 0.0059(13) 0.0014(11) 0.0260(13) _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 2.0709(17) . ? Co1 N1 2.0876(17) . ? Co1 N3 2.1674(17) . ? Co1 S1 2.3676(10) . ? Co1 S2 2.4461(10) . ? S1 C46 1.726(2) . ? S2 C46 1.716(2) . ? N1 C1 1.342(3) . ? N1 N2 1.368(2) . ? N2 C3 1.362(3) . ? N2 B1 1.542(3) . ? N3 C4 1.343(3) . ? N3 N4 1.372(2) . ? N4 C6 1.360(3) . ? N4 B1 1.550(3) . ? N5 C7 1.356(2) . ? N5 N6 1.368(2) . ? N6 C9 1.363(2) . ? N6 B1 1.547(3) . ? N7 C46 1.318(3) . ? N7 C50 1.476(3) . ? N7 C47 1.484(3) . ? B1 H1B 1.0460 . ? C1 C2 1.396(3) . ? C1 C40 1.473(3) . ? C2 C3 1.383(3) . ? C2 H2 0.9500 . ? C3 C34 1.477(3) . ? C4 C5 1.388(3) . ? C4 C28 1.481(3) . ? C5 C6 1.386(3) . ? C5 H5 0.9500 . ? C6 C22 1.481(3) . ? C7 C8 1.394(3) . ? C7 C16 1.470(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.473(3) . ? C10 C15 1.393(3) . ? C10 C11 1.398(3) . ? C11 C12 1.385(3) . ? C11 H11 0.9500 . ? C12 C13 1.384(3) . ? C12 H12 0.9500 . ? C13 C14 1.386(3) . ? C13 H13 0.9500 . ? C14 C15 1.382(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.393(3) . ? C16 C21 1.399(3) . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 C19 1.385(3) . ? C18 H18 0.9500 . ? C19 C20 1.385(3) . ? C19 H19 0.9500 . ? C20 C21 1.380(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.394(3) . ? C22 C27 1.396(3) . ? C23 C24 1.385(3) . ? C23 H23 0.9500 . ? C24 C25 1.389(4) . ? C24 H24 0.9500 . ? C25 C26 1.379(4) . ? C25 H25 0.9500 . ? C26 C27 1.391(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.389(3) . ? C28 C29 1.395(3) . ? C29 C30 1.382(3) . ? C29 H29 0.9500 . ? C30 C31 1.381(3) . ? C30 H30 0.9500 . ? C31 C32 1.382(3) . ? C31 H31 0.9500 . ? C32 C33 1.385(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.396(3) . ? C34 C39 1.399(3) . ? C35 C36 1.383(3) . ? C35 H35 0.9500 . ? C36 C37 1.384(3) . ? C36 H36 0.9500 . ? C37 C38 1.391(3) . ? C37 H37 0.9500 . ? C38 C39 1.381(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.386(3) . ? C40 C41 1.395(3) . ? C41 C42 1.390(3) . ? C41 H41 0.9500 . ? C42 C43 1.378(3) . ? C42 H42 0.9500 . ? C43 C44 1.383(3) . ? C43 H43 0.9500 . ? C44 C45 1.385(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C47 C48' 1.530(4) . ? C47 C48 1.531(4) . ? C47 H47B 0.9505 . ? C47 H47A 1.0692 . ? C48 C49 1.418(4) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.514(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C48' C49' 1.417(5) . ? C48' H48C 0.9900 . ? C48' H48D 0.9900 . ? C49' C50 1.513(4) . ? C49' H49C 0.9900 . ? C49' H49D 0.9900 . ? C50 H50A 0.9549 . ? C50 H50B 1.0483 . ? 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 N1 95.75(7) . . ? N5 Co1 N3 87.56(7) . . ? N1 Co1 N3 81.47(6) . . ? N5 Co1 S1 119.97(5) . . ? N1 Co1 S1 144.27(5) . . ? N3 Co1 S1 99.57(5) . . ? N5 Co1 S2 100.51(5) . . ? N1 Co1 S2 99.13(5) . . ? N3 Co1 S2 171.78(4) . . ? S1 Co1 S2 75.11(2) . . ? C46 S1 Co1 84.35(7) . . ? C46 S2 Co1 82.14(7) . . ? C1 N1 N2 106.97(15) . . ? C1 N1 Co1 137.11(13) . . ? N2 N1 Co1 115.92(12) . . ? C3 N2 N1 109.65(16) . . ? C3 N2 B1 129.08(16) . . ? N1 N2 B1 119.44(15) . . ? C4 N3 N4 106.46(16) . . ? C4 N3 Co1 137.10(13) . . ? N4 N3 Co1 115.23(12) . . ? C6 N4 N3 109.83(15) . . ? C6 N4 B1 130.89(16) . . ? N3 N4 B1 118.97(15) . . ? C7 N5 N6 106.62(15) . . ? C7 N5 Co1 134.98(14) . . ? N6 N5 Co1 115.77(11) . . ? C9 N6 N5 109.93(15) . . ? C9 N6 B1 129.11(16) . . ? N5 N6 B1 120.50(15) . . ? C46 N7 C50 124.01(19) . . ? C46 N7 C47 124.12(18) . . ? C50 N7 C47 111.58(17) . . ? N2 B1 N6 110.37(16) . . ? N2 B1 N4 107.98(16) . . ? N6 B1 N4 109.22(16) . . ? N2 B1 H1B 110.2 . . ? N6 B1 H1B 110.0 . . ? N4 B1 H1B 109.0 . . ? N1 C1 C2 109.85(17) . . ? N1 C1 C40 122.01(18) . . ? C2 C1 C40 127.79(18) . . ? C3 C2 C1 105.90(18) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? N2 C3 C2 107.62(17) . . ? N2 C3 C34 123.20(17) . . ? C2 C3 C34 129.13(18) . . ? N3 C4 C5 110.29(18) . . ? N3 C4 C28 121.48(18) . . ? C5 C4 C28 128.20(18) . . ? C6 C5 C4 105.92(18) . . ? C6 C5 H5 127.0 . . ? C4 C5 H5 127.0 . . ? N4 C6 C5 107.47(17) . . ? N4 C6 C22 125.47(18) . . ? C5 C6 C22 127.04(18) . . ? N5 C7 C8 109.67(17) . . ? N5 C7 C16 123.69(17) . . ? C8 C7 C16 126.50(18) . . ? C9 C8 C7 106.16(17) . . ? C9 C8 H8 126.9 . . ? C7 C8 H8 126.9 . . ? N6 C9 C8 107.60(17) . . ? N6 C9 C10 123.89(17) . . ? C8 C9 C10 128.50(18) . . ? C15 C10 C11 118.92(19) . . ? C15 C10 C9 122.26(18) . . ? C11 C10 C9 118.82(18) . . ? C12 C11 C10 120.3(2) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 119.9(2) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.2(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C10 120.5(2) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C17 C16 C21 118.84(19) . . ? C17 C16 C7 121.47(18) . . ? C21 C16 C7 119.50(19) . . ? C18 C17 C16 120.7(2) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 119.9(2) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 119.8(2) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 120.6(2) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C16 120.2(2) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? C23 C22 C27 118.55(19) . . ? C23 C22 C6 118.06(19) . . ? C27 C22 C6 123.35(19) . . ? C24 C23 C22 121.2(2) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 119.5(2) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 120.2(2) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 120.3(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 120.3(2) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C33 C28 C29 118.90(19) . . ? C33 C28 C4 120.35(18) . . ? C29 C28 C4 120.75(18) . . ? C30 C29 C28 120.39(19) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 120.1(2) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.1(2) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 120.0(2) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.5(2) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C35 C34 C39 119.09(19) . . ? C35 C34 C3 119.18(18) . . ? C39 C34 C3 121.72(18) . . ? C36 C35 C34 120.59(19) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 120.0(2) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C36 C37 C38 119.9(2) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 120.4(2) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C34 120.03(19) . . ? C38 C39 H39 120.0 . . ? C34 C39 H39 120.0 . . ? C45 C40 C41 118.65(19) . . ? C45 C40 C1 120.81(19) . . ? C41 C40 C1 120.32(19) . . ? C42 C41 C40 120.4(2) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 120.3(2) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 119.7(2) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C45 120.2(2) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C40 120.7(2) . . ? C44 C45 H45 119.6 . . ? C40 C45 H45 119.6 . . ? N7 C46 S2 121.90(16) . . ? N7 C46 S1 121.07(16) . . ? S2 C46 S1 117.02(12) . . ? N7 C47 C48' 102.2(5) . . ? N7 C47 C48 102.6(2) . . ? C48' C47 C48 35.3(6) . . ? N7 C47 H47B 108.7 . . ? C48' C47 H47B 84.9 . . ? C48 C47 H47B 117.2 . . ? N7 C47 H47A 107.8 . . ? C48' C47 H47A 139.0 . . ? C48 C47 H47A 109.5 . . ? H47B C47 H47A 110.3 . . ? C49 C48 C47 108.8(3) . . ? C49 C48 H48A 109.9 . . ? C47 C48 H48A 109.9 . . ? C49 C48 H48B 109.9 . . ? C47 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? C48 C49 C50 108.2(3) . . ? C48 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? C48 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? C49' C48' C47 106.7(9) . . ? C49' C48' H48C 110.4 . . ? C47 C48' H48C 110.4 . . ? C49' C48' H48D 110.4 . . ? C47 C48' H48D 110.4 . . ? H48C C48' H48D 108.6 . . ? C48' C49' C50 112.9(8) . . ? C48' C49' H49C 109.0 . . ? C50 C49' H49C 109.0 . . ? C48' C49' H49D 109.0 . . ? C50 C49' H49D 109.0 . . ? H49C C49' H49D 107.8 . . ? N7 C50 C49' 100.2(5) . . ? N7 C50 C49 104.3(2) . . ? C49' C50 C49 20.7(8) . . ? N7 C50 H50A 106.8 . . ? C49' C50 H50A 96.0 . . ? C49 C50 H50A 113.4 . . ? N7 C50 H50B 110.4 . . ? C49' C50 H50B 136.6 . . ? C49 C50 H50B 118.2 . . ? H50A C50 H50B 103.4 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.450 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.056 # Attachment '2138_web_deposit_cif_file_2_DavidJ.Harding_1281708532.cif' data_dh311p21c _database_code_depnum_ccdc_archive 'CCDC 789219' #TrackingRef '2138_web_deposit_cif_file_2_DavidJ.Harding_1281708532.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H44 B Co N7 S2' _chemical_formula_weight 876.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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)/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 14.076(2) _cell_length_b 25.405(4) _cell_length_c 12.5980(19) _cell_angle_alpha 90.00 _cell_angle_beta 103.749(9) _cell_angle_gamma 90.00 _cell_volume 4376.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7508 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.24 _exptl_crystal_description PLATE _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1828 _exptl_absorpt_coefficient_mu 0.532 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8234 _exptl_absorpt_correction_T_max 0.9438 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 95001 _diffrn_reflns_av_R_equivalents 0.0990 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10063 _reflns_number_gt 6550 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+2.3537P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10063 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1012 _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 0.23220(2) 0.638285(13) 0.32255(3) 0.02009(10) Uani 1 1 d . . . S1 S 0.39912(5) 0.66536(3) 0.33076(6) 0.02709(17) Uani 1 1 d . . . S2 S 0.31466(5) 0.63384(3) 0.51140(5) 0.02690(17) Uani 1 1 d . . . N1 N 0.09570(15) 0.60001(8) 0.32647(16) 0.0196(5) Uani 1 1 d . . . N2 N 0.01915(14) 0.60905(8) 0.23659(16) 0.0186(5) Uani 1 1 d . . . N3 N 0.15101(14) 0.70412(8) 0.25787(16) 0.0197(5) Uani 1 1 d . . . N4 N 0.07181(14) 0.69564(8) 0.17094(16) 0.0185(5) Uani 1 1 d . . . N5 N 0.20744(15) 0.59835(8) 0.17196(17) 0.0210(5) Uani 1 1 d . . . N6 N 0.12088(14) 0.60938(8) 0.09797(17) 0.0198(5) Uani 1 1 d . . . N7 N 0.49926(16) 0.66983(9) 0.53959(18) 0.0292(6) Uani 1 1 d . . . B1 B 0.0394(2) 0.63861(11) 0.1366(2) 0.0196(6) Uani 1 1 d . . . H1B H -0.0306 0.6413 0.0800 0.024 Uiso 1 1 d R . . C1 C 0.05617(18) 0.57647(9) 0.4018(2) 0.0204(6) Uani 1 1 d . . . C2 C -0.04457(18) 0.57148(10) 0.3632(2) 0.0228(6) Uani 1 1 d . . . H2 H -0.0894 0.5570 0.4010 0.027 Uiso 1 1 calc R . . C3 C -0.06621(18) 0.59196(10) 0.2577(2) 0.0208(6) Uani 1 1 d . . . C4 C 0.16892(18) 0.75675(10) 0.2603(2) 0.0209(6) Uani 1 1 d . . . C5 C 0.10345(19) 0.78130(10) 0.1735(2) 0.0252(6) Uani 1 1 d . . . H5 H 0.1012 0.8176 0.1554 0.030 Uiso 1 1 calc R . . C6 C 0.04262(19) 0.74212(10) 0.1194(2) 0.0222(6) Uani 1 1 d . . . C7 C 0.25486(18) 0.56301(10) 0.1228(2) 0.0209(6) Uani 1 1 d . . . C8 C 0.20002(18) 0.55259(10) 0.0174(2) 0.0228(6) Uani 1 1 d . . . H8 H 0.2175 0.5298 -0.0346 0.027 Uiso 1 1 calc R . . C9 C 0.11503(18) 0.58189(9) 0.0033(2) 0.0193(6) Uani 1 1 d . . . C10 C 0.02907(18) 0.58344(10) -0.0911(2) 0.0206(6) Uani 1 1 d . . . C11 C -0.01620(19) 0.53621(11) -0.1314(2) 0.0248(6) Uani 1 1 d . . . H11 H 0.0080 0.5039 -0.0976 0.030 Uiso 1 1 calc R . . C12 C -0.0962(2) 0.53596(12) -0.2204(2) 0.0322(7) Uani 1 1 d . . . H12 H -0.1270 0.5037 -0.2470 0.039 Uiso 1 1 calc R . . C13 C -0.1310(2) 0.58315(12) -0.2704(2) 0.0384(8) Uani 1 1 d . . . H13 H -0.1860 0.5831 -0.3310 0.046 Uiso 1 1 calc R . . C14 C -0.0861(2) 0.63022(12) -0.2322(2) 0.0362(7) Uani 1 1 d . . . H14 H -0.1098 0.6623 -0.2675 0.043 Uiso 1 1 calc R . . C15 C -0.0065(2) 0.63078(10) -0.1426(2) 0.0281(7) Uani 1 1 d . . . H15 H 0.0238 0.6632 -0.1163 0.034 Uiso 1 1 calc R . . C16 C 0.34642(18) 0.53691(10) 0.1814(2) 0.0230(6) Uani 1 1 d . . . C17 C 0.3599(2) 0.52248(11) 0.2910(2) 0.0309(7) Uani 1 1 d . . . H17 H 0.3141 0.5335 0.3311 0.037 Uiso 1 1 calc R . . C18 C 0.4404(2) 0.49191(12) 0.3418(3) 0.0412(8) Uani 1 1 d . . . H18 H 0.4488 0.4816 0.4159 0.049 Uiso 1 1 calc R . . C19 C 0.5082(2) 0.47662(12) 0.2838(3) 0.0445(9) Uani 1 1 d . . . H19 H 0.5628 0.4557 0.3181 0.053 Uiso 1 1 calc R . . C20 C 0.4964(2) 0.49175(12) 0.1770(3) 0.0428(8) Uani 1 1 d . . . H20 H 0.5435 0.4819 0.1378 0.051 Uiso 1 1 calc R . . C21 C 0.4155(2) 0.52156(11) 0.1259(2) 0.0332(7) Uani 1 1 d . . . H21 H 0.4076 0.5315 0.0516 0.040 Uiso 1 1 calc R . . C22 C -0.04139(18) 0.74697(10) 0.0230(2) 0.0218(6) Uani 1 1 d . . . C23 C -0.0285(2) 0.77503(10) -0.0683(2) 0.0265(6) Uani 1 1 d . . . H23 H 0.0330 0.7908 -0.0670 0.032 Uiso 1 1 calc R . . C24 C -0.1047(2) 0.77988(11) -0.1606(2) 0.0321(7) Uani 1 1 d . . . H24 H -0.0949 0.7987 -0.2222 0.038 Uiso 1 1 calc R . . C25 C -0.1950(2) 0.75741(11) -0.1634(2) 0.0342(7) Uani 1 1 d . . . H25 H -0.2467 0.7604 -0.2271 0.041 Uiso 1 1 calc R . . C26 C -0.2094(2) 0.73067(11) -0.0730(2) 0.0312(7) Uani 1 1 d . . . H26 H -0.2716 0.7158 -0.0744 0.037 Uiso 1 1 calc R . . C27 C -0.13350(19) 0.72542(10) 0.0200(2) 0.0266(6) Uani 1 1 d . . . H27 H -0.1443 0.7071 0.0818 0.032 Uiso 1 1 calc R . . C28 C 0.24228(18) 0.78276(10) 0.3482(2) 0.0217(6) Uani 1 1 d . . . C29 C 0.25029(19) 0.76995(11) 0.4576(2) 0.0276(6) Uani 1 1 d . . . H29 H 0.2118 0.7422 0.4760 0.033 Uiso 1 1 calc R . . C30 C 0.3142(2) 0.79746(11) 0.5401(2) 0.0318(7) Uani 1 1 d . . . H30 H 0.3183 0.7889 0.6144 0.038 Uiso 1 1 calc R . . C31 C 0.3718(2) 0.83736(11) 0.5143(2) 0.0347(7) Uani 1 1 d . . . H31 H 0.4166 0.8556 0.5705 0.042 Uiso 1 1 calc R . . C32 C 0.3635(2) 0.85037(11) 0.4059(3) 0.0356(7) Uani 1 1 d . . . H32 H 0.4026 0.8780 0.3881 0.043 Uiso 1 1 calc R . . C33 C 0.2993(2) 0.82391(10) 0.3228(2) 0.0291(7) Uani 1 1 d . . . H33 H 0.2939 0.8336 0.2488 0.035 Uiso 1 1 calc R . . C34 C -0.16416(19) 0.59648(10) 0.1809(2) 0.0231(6) Uani 1 1 d . . . C35 C -0.24279(19) 0.61262(10) 0.2225(2) 0.0294(7) Uani 1 1 d . . . H35 H -0.2322 0.6210 0.2979 0.035 Uiso 1 1 calc R . . C36 C -0.3366(2) 0.61664(12) 0.1554(3) 0.0386(8) Uani 1 1 d . . . H36 H -0.3895 0.6277 0.1850 0.046 Uiso 1 1 calc R . . C37 C -0.3524(2) 0.60451(12) 0.0456(3) 0.0407(8) Uani 1 1 d . . . H37 H -0.4162 0.6077 -0.0005 0.049 Uiso 1 1 calc R . . C38 C -0.2763(2) 0.58793(11) 0.0026(2) 0.0330(7) Uani 1 1 d . . . H38 H -0.2879 0.5795 -0.0728 0.040 Uiso 1 1 calc R . . C39 C -0.18198(19) 0.58345(10) 0.0698(2) 0.0260(6) Uani 1 1 d . . . H39 H -0.1298 0.5715 0.0399 0.031 Uiso 1 1 calc R . . C40 C 0.11785(18) 0.55694(10) 0.5073(2) 0.0201(6) Uani 1 1 d . . . C41 C 0.19371(18) 0.52117(10) 0.5093(2) 0.0224(6) Uani 1 1 d . . . H41 H 0.2060 0.5091 0.4424 0.027 Uiso 1 1 calc R . . C42 C 0.25128(19) 0.50311(11) 0.6074(2) 0.0273(6) Uani 1 1 d . . . H42 H 0.3019 0.4784 0.6076 0.033 Uiso 1 1 calc R . . C43 C 0.2348(2) 0.52129(11) 0.7056(2) 0.0284(7) Uani 1 1 d . . . H43 H 0.2752 0.5096 0.7730 0.034 Uiso 1 1 calc R . . C44 C 0.1594(2) 0.55644(11) 0.7052(2) 0.0295(7) Uani 1 1 d . . . H44 H 0.1483 0.5691 0.7722 0.035 Uiso 1 1 calc R . . C45 C 0.09983(19) 0.57322(10) 0.6060(2) 0.0256(6) Uani 1 1 d . . . H45 H 0.0463 0.5960 0.6060 0.031 Uiso 1 1 calc R . . C46 C 0.41483(19) 0.65823(10) 0.4693(2) 0.0237(6) Uani 1 1 d . . . C47 C 0.5164(2) 0.66226(13) 0.6596(2) 0.0403(8) Uani 1 1 d . . . H47A H 0.5806 0.6450 0.6873 0.048 Uiso 1 1 calc R . . H47B H 0.4653 0.6387 0.6752 0.048 Uiso 1 1 calc R . . C48 C 0.5148(3) 0.71311(14) 0.7181(3) 0.0588(10) Uani 1 1 d . . . H48A H 0.5650 0.7366 0.7026 0.088 Uiso 1 1 calc R . . H48B H 0.5278 0.7066 0.7969 0.088 Uiso 1 1 calc R . . H48C H 0.4504 0.7296 0.6932 0.088 Uiso 1 1 calc R . . C49 C 0.5857(2) 0.68739(14) 0.5013(3) 0.0438(9) Uani 1 1 d . . . H49A H 0.6271 0.7101 0.5578 0.053 Uiso 1 1 calc R . . H49B H 0.5638 0.7086 0.4341 0.053 Uiso 1 1 calc R . . C50 C 0.6456(2) 0.64136(16) 0.4781(3) 0.0639(11) Uani 1 1 d . . . H50A H 0.6617 0.6183 0.5422 0.096 Uiso 1 1 calc R . . H50B H 0.7061 0.6544 0.4616 0.096 Uiso 1 1 calc R . . H50C H 0.6079 0.6216 0.4153 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02005(19) 0.01987(19) 0.0186(2) -0.00034(15) 0.00103(15) -0.00084(15) S1 0.0233(4) 0.0349(4) 0.0217(4) 0.0014(3) 0.0026(3) -0.0039(3) S2 0.0253(4) 0.0329(4) 0.0206(4) 0.0018(3) 0.0018(3) -0.0072(3) N1 0.0221(11) 0.0184(11) 0.0164(11) -0.0013(9) 0.0007(9) -0.0007(9) N2 0.0163(11) 0.0172(11) 0.0204(12) -0.0009(9) 0.0004(9) 0.0004(9) N3 0.0197(11) 0.0195(11) 0.0180(12) -0.0014(9) 0.0006(9) -0.0031(9) N4 0.0193(11) 0.0169(11) 0.0179(11) 0.0000(9) 0.0016(9) 0.0006(9) N5 0.0185(11) 0.0214(12) 0.0215(12) -0.0001(9) 0.0013(10) -0.0009(9) N6 0.0173(11) 0.0200(11) 0.0209(12) -0.0012(9) 0.0021(9) 0.0006(9) N7 0.0253(13) 0.0372(14) 0.0225(13) 0.0023(11) 0.0005(11) -0.0079(11) B1 0.0169(14) 0.0203(15) 0.0198(15) 0.0007(13) 0.0007(12) -0.0010(12) C1 0.0235(14) 0.0165(13) 0.0208(14) -0.0015(11) 0.0046(12) -0.0026(11) C2 0.0227(14) 0.0227(14) 0.0233(15) 0.0023(12) 0.0059(12) -0.0015(11) C3 0.0187(14) 0.0174(13) 0.0258(15) -0.0017(11) 0.0042(12) -0.0013(11) C4 0.0214(14) 0.0201(14) 0.0211(14) -0.0011(11) 0.0043(12) -0.0005(11) C5 0.0301(15) 0.0174(14) 0.0264(15) 0.0042(12) 0.0034(13) 0.0006(12) C6 0.0252(14) 0.0195(14) 0.0220(14) -0.0004(11) 0.0059(12) 0.0012(11) C7 0.0196(13) 0.0207(14) 0.0225(14) 0.0001(11) 0.0050(11) -0.0019(11) C8 0.0274(15) 0.0206(14) 0.0204(14) -0.0014(11) 0.0056(12) -0.0026(11) C9 0.0239(14) 0.0179(13) 0.0164(13) 0.0000(11) 0.0052(11) -0.0019(11) C10 0.0220(14) 0.0219(14) 0.0181(14) -0.0015(11) 0.0053(11) 0.0015(11) C11 0.0296(15) 0.0233(14) 0.0206(14) 0.0001(12) 0.0039(12) 0.0022(12) C12 0.0336(16) 0.0327(17) 0.0269(16) -0.0068(13) 0.0001(13) -0.0059(13) C13 0.0342(17) 0.045(2) 0.0272(17) -0.0050(15) -0.0097(14) 0.0070(15) C14 0.0443(19) 0.0333(18) 0.0259(16) 0.0013(13) -0.0018(14) 0.0104(14) C15 0.0406(17) 0.0209(15) 0.0205(15) -0.0020(12) 0.0028(13) -0.0011(12) C16 0.0211(14) 0.0196(14) 0.0264(15) -0.0020(12) 0.0015(12) -0.0027(11) C17 0.0253(15) 0.0300(16) 0.0349(17) 0.0012(13) 0.0018(13) -0.0015(12) C18 0.0331(18) 0.0383(18) 0.043(2) 0.0098(15) -0.0098(15) -0.0055(15) C19 0.0218(16) 0.0262(17) 0.075(3) 0.0032(17) -0.0102(17) 0.0020(13) C20 0.0273(17) 0.0353(18) 0.063(2) -0.0095(17) 0.0051(16) 0.0067(14) C21 0.0271(16) 0.0339(17) 0.0385(18) -0.0032(14) 0.0074(14) 0.0025(13) C22 0.0220(14) 0.0191(14) 0.0223(14) -0.0003(11) 0.0011(12) 0.0031(11) C23 0.0294(15) 0.0197(14) 0.0290(16) 0.0019(12) 0.0038(13) 0.0013(12) C24 0.0416(18) 0.0275(16) 0.0254(16) 0.0061(13) 0.0047(14) 0.0023(14) C25 0.0327(17) 0.0325(17) 0.0298(17) 0.0041(14) -0.0080(14) 0.0028(13) C26 0.0250(15) 0.0306(16) 0.0348(18) 0.0055(14) 0.0011(14) 0.0022(12) C27 0.0304(16) 0.0239(15) 0.0247(15) 0.0026(12) 0.0052(13) 0.0040(12) C28 0.0185(13) 0.0201(14) 0.0251(15) -0.0037(11) 0.0021(12) 0.0014(11) C29 0.0280(15) 0.0246(15) 0.0296(16) -0.0028(13) 0.0054(13) -0.0026(12) C30 0.0346(17) 0.0340(17) 0.0240(16) -0.0054(13) 0.0015(13) 0.0025(14) C31 0.0314(17) 0.0310(17) 0.0371(19) -0.0119(14) -0.0010(14) -0.0031(14) C32 0.0310(17) 0.0264(16) 0.046(2) -0.0033(14) 0.0023(15) -0.0099(13) C33 0.0312(16) 0.0246(15) 0.0309(17) 0.0020(13) 0.0059(13) -0.0046(12) C34 0.0247(14) 0.0140(13) 0.0286(16) 0.0028(11) 0.0028(12) -0.0047(11) C35 0.0274(16) 0.0250(15) 0.0347(17) 0.0014(13) 0.0050(13) -0.0019(12) C36 0.0242(16) 0.0383(18) 0.051(2) -0.0027(16) 0.0042(15) 0.0051(13) C37 0.0238(16) 0.0385(19) 0.050(2) -0.0020(16) -0.0109(15) 0.0014(14) C38 0.0357(18) 0.0264(16) 0.0312(17) -0.0030(13) -0.0031(14) -0.0038(13) C39 0.0216(14) 0.0196(14) 0.0333(17) -0.0003(12) -0.0002(12) -0.0023(11) C40 0.0215(14) 0.0189(13) 0.0194(14) 0.0019(11) 0.0037(11) -0.0052(11) C41 0.0227(14) 0.0213(14) 0.0224(15) -0.0016(11) 0.0035(12) -0.0027(11) C42 0.0234(14) 0.0228(15) 0.0337(17) 0.0041(12) 0.0027(13) -0.0027(12) C43 0.0299(16) 0.0308(16) 0.0203(15) 0.0047(12) -0.0021(13) -0.0062(13) C44 0.0365(17) 0.0313(16) 0.0216(15) -0.0019(13) 0.0088(13) -0.0052(13) C45 0.0275(15) 0.0207(14) 0.0276(16) -0.0009(12) 0.0047(13) -0.0014(12) C46 0.0236(14) 0.0213(14) 0.0234(15) 0.0007(12) -0.0003(12) 0.0002(11) C47 0.0364(18) 0.049(2) 0.0313(18) -0.0012(16) -0.0001(15) -0.0093(15) C48 0.061(2) 0.064(3) 0.051(2) -0.011(2) 0.0135(19) -0.004(2) C49 0.0304(17) 0.066(2) 0.0318(18) -0.0002(16) 0.0008(14) -0.0166(16) C50 0.036(2) 0.101(3) 0.056(2) 0.014(2) 0.0144(18) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.080(2) . ? Co1 N5 2.106(2) . ? Co1 N1 2.164(2) . ? Co1 S2 2.3891(8) . ? Co1 S1 2.4267(8) . ? S1 C46 1.716(3) . ? S2 C46 1.735(3) . ? N1 C1 1.349(3) . ? N1 N2 1.384(3) . ? N2 C3 1.362(3) . ? N2 B1 1.551(3) . ? N3 C4 1.360(3) . ? N3 N4 1.381(3) . ? N4 C6 1.363(3) . ? N4 B1 1.549(3) . ? N5 C7 1.353(3) . ? N5 N6 1.375(3) . ? N6 C9 1.367(3) . ? N6 B1 1.539(4) . ? N7 C46 1.335(3) . ? N7 C49 1.480(4) . ? N7 C47 1.486(4) . ? B1 H1B 1.0725 . ? C1 C2 1.391(3) . ? C1 C40 1.488(3) . ? C2 C3 1.392(3) . ? C2 H2 0.9500 . ? C3 C34 1.488(3) . ? C4 C5 1.398(3) . ? C4 C28 1.478(3) . ? C5 C6 1.382(3) . ? C5 H5 0.9500 . ? C6 C22 1.485(3) . ? C7 C8 1.394(3) . ? C7 C16 1.481(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.482(3) . ? C10 C11 1.397(3) . ? C10 C15 1.401(3) . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 C13 1.388(4) . ? C12 H12 0.9500 . ? C13 C14 1.384(4) . ? C13 H13 0.9500 . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.382(4) . ? C16 C17 1.397(4) . ? C17 C18 1.398(4) . ? C17 H17 0.9500 . ? C18 C19 1.388(4) . ? C18 H18 0.9500 . ? C19 C20 1.371(5) . ? C19 H19 0.9500 . ? C20 C21 1.391(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.399(4) . ? C22 C23 1.402(4) . ? C23 C24 1.388(4) . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 H24 0.9500 . ? C25 C26 1.381(4) . ? C25 H25 0.9500 . ? C26 C27 1.391(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.395(4) . ? C28 C33 1.401(4) . ? C29 C30 1.390(4) . ? C29 H29 0.9500 . ? C30 C31 1.384(4) . ? C30 H30 0.9500 . ? C31 C32 1.383(4) . ? C31 H31 0.9500 . ? C32 C33 1.384(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.394(4) . ? C34 C39 1.402(4) . ? C35 C36 1.392(4) . ? C35 H35 0.9500 . ? C36 C37 1.383(4) . ? C36 H36 0.9500 . ? C37 C38 1.376(4) . ? C37 H37 0.9500 . ? C38 C39 1.400(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.390(4) . ? C40 C41 1.398(3) . ? C41 C42 1.385(4) . ? C41 H41 0.9500 . ? C42 C43 1.392(4) . ? C42 H42 0.9500 . ? C43 C44 1.386(4) . ? C43 H43 0.9500 . ? C44 C45 1.396(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C47 C48 1.490(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.511(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 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 N3 Co1 N5 94.39(8) . . ? N3 Co1 N1 87.83(8) . . ? N5 Co1 N1 81.16(8) . . ? N3 Co1 S2 121.32(6) . . ? N5 Co1 S2 144.24(6) . . ? N1 Co1 S2 100.36(6) . . ? N3 Co1 S1 103.01(6) . . ? N5 Co1 S1 97.25(6) . . ? N1 Co1 S1 169.15(6) . . ? S2 Co1 S1 74.61(3) . . ? C46 S1 Co1 84.43(9) . . ? C46 S2 Co1 85.20(9) . . ? C1 N1 N2 106.15(19) . . ? C1 N1 Co1 137.06(17) . . ? N2 N1 Co1 115.44(14) . . ? C3 N2 N1 109.82(19) . . ? C3 N2 B1 130.9(2) . . ? N1 N2 B1 119.15(19) . . ? C4 N3 N4 106.35(19) . . ? C4 N3 Co1 134.47(17) . . ? N4 N3 Co1 116.74(14) . . ? C6 N4 N3 109.73(19) . . ? C6 N4 B1 129.9(2) . . ? N3 N4 B1 119.72(19) . . ? C7 N5 N6 106.21(19) . . ? C7 N5 Co1 137.53(17) . . ? N6 N5 Co1 116.26(15) . . ? C9 N6 N5 110.29(19) . . ? C9 N6 B1 128.8(2) . . ? N5 N6 B1 119.4(2) . . ? C46 N7 C49 121.4(2) . . ? C46 N7 C47 123.4(2) . . ? C49 N7 C47 115.0(2) . . ? N6 B1 N2 108.5(2) . . ? N6 B1 N4 110.4(2) . . ? N2 B1 N4 108.9(2) . . ? N6 B1 H1B 117.2 . . ? N2 B1 H1B 104.7 . . ? N4 B1 H1B 106.8 . . ? N1 C1 C2 110.5(2) . . ? N1 C1 C40 121.7(2) . . ? C2 C1 C40 127.7(2) . . ? C3 C2 C1 105.9(2) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? N2 C3 C2 107.6(2) . . ? N2 C3 C34 124.9(2) . . ? C2 C3 C34 127.4(2) . . ? N3 C4 C5 109.7(2) . . ? N3 C4 C28 123.3(2) . . ? C5 C4 C28 126.8(2) . . ? C6 C5 C4 106.3(2) . . ? C6 C5 H5 126.9 . . ? C4 C5 H5 126.9 . . ? N4 C6 C5 107.9(2) . . ? N4 C6 C22 123.6(2) . . ? C5 C6 C22 128.5(2) . . ? N5 C7 C8 109.9(2) . . ? N5 C7 C16 122.3(2) . . ? C8 C7 C16 127.5(2) . . ? C9 C8 C7 106.6(2) . . ? C9 C8 H8 126.7 . . ? C7 C8 H8 126.7 . . ? N6 C9 C8 107.0(2) . . ? N6 C9 C10 123.7(2) . . ? C8 C9 C10 129.3(2) . . ? C11 C10 C15 119.1(2) . . ? C11 C10 C9 119.0(2) . . ? C15 C10 C9 121.9(2) . . ? C12 C11 C10 120.7(2) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 119.6(3) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 119.9(2) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? C21 C16 C17 118.7(3) . . ? C21 C16 C7 120.5(2) . . ? C17 C16 C7 120.5(2) . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C16 C21 C20 121.1(3) . . ? C16 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C27 C22 C23 118.5(2) . . ? C27 C22 C6 122.9(2) . . ? C23 C22 C6 118.7(2) . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.6(3) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.5(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 120.4(3) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C29 C28 C33 118.9(2) . . ? C29 C28 C4 120.9(2) . . ? C33 C28 C4 119.9(2) . . ? C30 C29 C28 120.5(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 119.4(3) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C33 C32 C31 121.1(3) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C28 119.8(3) . . ? C32 C33 H33 120.1 . . ? C28 C33 H33 120.1 . . ? C35 C34 C39 118.4(2) . . ? C35 C34 C3 118.3(2) . . ? C39 C34 C3 123.3(2) . . ? C34 C35 C36 121.1(3) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 119.7(3) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C38 C37 C36 120.4(3) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 120.2(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C34 C39 C38 120.2(3) . . ? C34 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C45 C40 C41 118.5(2) . . ? C45 C40 C1 120.5(2) . . ? C41 C40 C1 120.9(2) . . ? C42 C41 C40 121.0(2) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C41 C42 C43 119.9(3) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 120.0(2) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 119.8(3) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C40 C45 C44 120.8(3) . . ? C40 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? N7 C46 S1 122.0(2) . . ? N7 C46 S2 122.4(2) . . ? S1 C46 S2 115.54(15) . . ? N7 C47 C48 111.9(3) . . ? N7 C47 H47A 109.2 . . ? C48 C47 H47A 109.2 . . ? N7 C47 H47B 109.2 . . ? C48 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N7 C49 C50 111.7(3) . . ? N7 C49 H49A 109.3 . . ? C50 C49 H49A 109.3 . . ? N7 C49 H49B 109.3 . . ? C50 C49 H49B 109.3 . . ? H49A C49 H49B 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.694 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.072