# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hong Yan' _publ_contact_author_email chemluke@126.com _publ_author_name 'Hong Yan' #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 828291' #TrackingRef '- cif- revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H31 B10 Co O4 S2' _chemical_formula_sum 'C19 H31 B10 Co O4 S2' _chemical_formula_weight 554.59 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.9050(16) _cell_length_b 10.5449(10) _cell_length_c 15.0639(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.0330(10) _cell_angle_gamma 90.00 _cell_volume 2684.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 7917 _cell_measurement_theta_min 2.772 _cell_measurement_theta_max 24.947 _exptl_crystal_description BLOCK _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.821 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18266 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4663 _reflns_number_gt 4064 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+1.9918P] 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 4663 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 B3 B 0.40697(17) 0.4869(3) 0.1890(2) 0.0430(7) Uani 1 1 d . . . H3 H 0.4359 0.5568 0.1462 0.052 Uiso 1 1 calc R . . B4 B 0.41454(18) 0.3203(3) 0.1692(2) 0.0454(7) Uani 1 1 d . . . H4 H 0.4488 0.2820 0.1139 0.054 Uiso 1 1 calc R . . B5 B 0.3240(2) 0.2494(3) 0.2017(2) 0.0437(7) Uani 1 1 d . . . H5 H 0.3004 0.1654 0.1669 0.052 Uiso 1 1 calc R . . B6 B 0.25974(18) 0.3702(3) 0.2427(2) 0.0374(6) Uani 1 1 d . . . H6 H 0.1950 0.3653 0.2348 0.045 Uiso 1 1 calc R . . B7 B 0.30681(19) 0.4387(3) 0.3372(2) 0.0444(7) Uani 1 1 d . . . H77 H 0.2721 0.4778 0.3919 0.053 Uiso 1 1 calc R . . B8 B 0.39690(19) 0.5110(3) 0.3042(2) 0.0479(8) Uani 1 1 d . . . H8 H 0.4201 0.5967 0.3371 0.057 Uiso 1 1 calc R . . B9 B 0.4604(2) 0.3892(4) 0.2640(2) 0.0542(9) Uani 1 1 d . . . H9 H 0.5252 0.3951 0.2710 0.065 Uiso 1 1 calc R . . B10 B 0.4091(2) 0.2431(4) 0.2728(2) 0.0553(9) Uani 1 1 d . . . H10 H 0.4409 0.1539 0.2863 0.066 Uiso 1 1 calc R . . B11 B 0.3133(2) 0.2725(3) 0.3167(2) 0.0496(8) Uani 1 1 d . . . H11 H 0.2829 0.2022 0.3578 0.060 Uiso 1 1 calc R . . B12 B 0.3984(2) 0.3599(4) 0.3563(2) 0.0543(9) Uani 1 1 d . . . H12 H 0.4230 0.3467 0.4238 0.065 Uiso 1 1 calc R . . C1 C 0.32544(14) 0.3985(2) 0.15910(16) 0.0333(5) Uani 1 1 d . . . C2 C 0.31467(14) 0.5098(2) 0.23568(16) 0.0352(5) Uani 1 1 d . . . C3 C 0.20808(15) 0.6721(2) -0.07055(16) 0.0382(6) Uani 1 1 d . . . C4 C 0.29219(16) 0.6827(2) -0.05705(18) 0.0410(6) Uani 1 1 d . . . C5 C 0.30573(18) 0.7732(3) 0.01057(19) 0.0482(7) Uani 1 1 d . . . C6 C 0.23093(19) 0.8214(3) 0.03752(19) 0.0481(7) Uani 1 1 d . . . C7 C 0.17177(17) 0.7598(2) -0.01409(18) 0.0434(6) Uani 1 1 d . . . H7 H 0.1177 0.7749 -0.0112 0.052 Uiso 1 1 calc R . . C8 C 0.1665(2) 0.5918(3) -0.1389(2) 0.0569(8) Uani 1 1 d . . . H8A H 0.1163 0.5652 -0.1168 0.085 Uiso 1 1 calc R . . H8B H 0.1981 0.5186 -0.1515 0.085 Uiso 1 1 calc R . . H8C H 0.1585 0.6402 -0.1923 0.085 Uiso 1 1 calc R . . C9 C 0.3525(2) 0.6136(3) -0.1090(2) 0.0640(9) Uani 1 1 d . . . H9A H 0.3642 0.6610 -0.1616 0.096 Uiso 1 1 calc R . . H9B H 0.3323 0.5317 -0.1255 0.096 Uiso 1 1 calc R . . H9C H 0.3998 0.6036 -0.0735 0.096 Uiso 1 1 calc R . . C10 C 0.3850(2) 0.8177(4) 0.0451(3) 0.0782(12) Uani 1 1 d . . . H10A H 0.4258 0.7648 0.0215 0.117 Uiso 1 1 calc R . . H10B H 0.3864 0.8127 0.1087 0.117 Uiso 1 1 calc R . . H10C H 0.3934 0.9039 0.0270 0.117 Uiso 1 1 calc R . . C11 C 0.2183(3) 0.9286(3) 0.1018(2) 0.0765(11) Uani 1 1 d . . . H11A H 0.2259 1.0081 0.0720 0.115 Uiso 1 1 calc R . . H11B H 0.2555 0.9215 0.1504 0.115 Uiso 1 1 calc R . . H11C H 0.1654 0.9246 0.1238 0.115 Uiso 1 1 calc R . . C12 C 0.21848(15) 0.3222(2) 0.02627(16) 0.0357(5) Uani 1 1 d . . . H12A H 0.2376 0.2439 0.0079 0.043 Uiso 1 1 calc R . . C13 C 0.13992(15) 0.3375(2) 0.03259(16) 0.0369(6) Uani 1 1 d . . . C14 C 0.08890(16) 0.2294(3) 0.00103(18) 0.0415(6) Uani 1 1 d . . . C15 C 0.07794(19) 0.0541(3) -0.0962(3) 0.0625(9) Uani 1 1 d . . . H15A H 0.0638 -0.0007 -0.0482 0.094 Uiso 1 1 calc R . . H15B H 0.1099 0.0082 -0.1373 0.094 Uiso 1 1 calc R . . H15C H 0.0308 0.0838 -0.1261 0.094 Uiso 1 1 calc R . . C16 C 0.09912(15) 0.4402(3) 0.07511(18) 0.0405(6) Uani 1 1 d . . . H16 H 0.0469 0.4246 0.0903 0.049 Uiso 1 1 calc R . . C17 C 0.12769(15) 0.5569(2) 0.09568(17) 0.0366(6) Uani 1 1 d . . . C18 C 0.07503(16) 0.6394(3) 0.14911(18) 0.0426(6) Uani 1 1 d . . . C19 C -0.0324(2) 0.6449(4) 0.2480(3) 0.0789(11) Uani 1 1 d . . . H19A H -0.0027 0.6997 0.2871 0.118 Uiso 1 1 calc R . . H19B H -0.0638 0.5880 0.2824 0.118 Uiso 1 1 calc R . . H19C H -0.0664 0.6950 0.2102 0.118 Uiso 1 1 calc R . . Co1 Co 0.229548(19) 0.62739(3) 0.06195(2) 0.03115(12) Uani 1 1 d . . . O1 O 0.12209(12) 0.16102(19) -0.06172(14) 0.0521(5) Uani 1 1 d . . . O2 O 0.02443(12) 0.2075(2) 0.03131(16) 0.0640(6) Uani 1 1 d . . . O3 O 0.07902(15) 0.7525(2) 0.15587(17) 0.0700(7) Uani 1 1 d . . . O4 O 0.02071(14) 0.5737(2) 0.19492(16) 0.0680(6) Uani 1 1 d . . . S1 S 0.28671(3) 0.44304(6) 0.05105(4) 0.03255(16) Uani 1 1 d . . . S2 S 0.26253(5) 0.65081(6) 0.20724(4) 0.04386(18) 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 B3 0.0346(15) 0.0506(18) 0.0437(17) -0.0022(14) -0.0046(13) -0.0049(13) B4 0.0371(16) 0.0526(19) 0.0466(18) -0.0008(15) 0.0020(13) 0.0118(14) B5 0.0527(18) 0.0327(15) 0.0458(17) 0.0029(13) 0.0017(14) 0.0052(13) B6 0.0391(15) 0.0372(15) 0.0360(15) 0.0036(12) 0.0031(12) -0.0028(12) B7 0.0466(17) 0.0515(19) 0.0351(16) 0.0031(14) -0.0018(13) 0.0067(14) B8 0.0442(17) 0.0550(19) 0.0440(18) -0.0019(15) -0.0097(14) 0.0005(15) B9 0.0390(17) 0.069(2) 0.055(2) 0.0007(17) -0.0072(15) 0.0109(16) B10 0.057(2) 0.054(2) 0.056(2) 0.0087(17) -0.0050(16) 0.0205(16) B11 0.063(2) 0.0425(18) 0.0437(18) 0.0128(14) 0.0058(15) 0.0063(15) B12 0.056(2) 0.064(2) 0.0427(19) 0.0072(16) -0.0129(15) 0.0153(17) C1 0.0342(12) 0.0316(12) 0.0341(13) -0.0004(10) 0.0007(10) 0.0025(10) C2 0.0379(13) 0.0335(13) 0.0339(13) -0.0004(10) -0.0039(10) 0.0010(10) C3 0.0449(14) 0.0361(13) 0.0334(13) 0.0085(11) -0.0065(11) -0.0052(11) C4 0.0455(14) 0.0352(14) 0.0424(15) 0.0125(11) 0.0001(11) -0.0059(11) C5 0.0560(17) 0.0389(15) 0.0492(16) 0.0156(12) -0.0157(13) -0.0181(13) C6 0.073(2) 0.0276(13) 0.0437(15) 0.0063(11) -0.0065(14) -0.0022(13) C7 0.0474(15) 0.0377(14) 0.0449(15) 0.0109(12) -0.0073(12) 0.0067(12) C8 0.071(2) 0.0586(18) 0.0407(16) 0.0022(14) -0.0148(14) -0.0159(16) C9 0.0582(19) 0.069(2) 0.066(2) 0.0190(17) 0.0225(17) 0.0037(16) C10 0.076(2) 0.075(2) 0.082(3) 0.022(2) -0.029(2) -0.042(2) C11 0.133(4) 0.0322(16) 0.064(2) -0.0062(15) -0.007(2) -0.0005(19) C12 0.0423(14) 0.0288(12) 0.0360(13) -0.0043(10) -0.0012(11) -0.0035(10) C13 0.0394(14) 0.0368(13) 0.0343(13) 0.0022(11) -0.0028(11) -0.0045(11) C14 0.0413(15) 0.0395(14) 0.0433(15) 0.0077(12) -0.0072(12) -0.0049(11) C15 0.0568(19) 0.0427(17) 0.088(2) -0.0163(16) -0.0108(17) -0.0096(14) C16 0.0331(13) 0.0448(15) 0.0434(15) 0.0021(12) -0.0030(11) -0.0073(11) C17 0.0365(13) 0.0376(14) 0.0357(13) 0.0025(10) -0.0031(10) 0.0027(10) C18 0.0428(15) 0.0463(17) 0.0385(15) 0.0008(12) -0.0022(12) 0.0054(12) C19 0.078(3) 0.089(3) 0.071(2) -0.008(2) 0.034(2) 0.009(2) Co1 0.0347(2) 0.02702(19) 0.0315(2) 0.00051(12) -0.00510(14) -0.00049(12) O1 0.0475(11) 0.0440(11) 0.0648(13) -0.0163(10) 0.0031(10) -0.0097(9) O2 0.0474(12) 0.0703(15) 0.0748(15) -0.0124(12) 0.0097(11) -0.0230(11) O3 0.0796(16) 0.0445(13) 0.0867(17) -0.0056(11) 0.0252(13) 0.0113(11) O4 0.0739(15) 0.0607(14) 0.0705(15) -0.0095(12) 0.0325(12) -0.0014(12) S1 0.0343(3) 0.0314(3) 0.0319(3) -0.0012(2) -0.0005(2) -0.0018(2) S2 0.0603(4) 0.0321(3) 0.0388(4) -0.0070(3) -0.0129(3) 0.0090(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B3 C1 1.717(4) . ? B3 C2 1.740(4) . ? B3 B8 1.765(5) . ? B3 B9 1.765(5) . ? B3 B4 1.787(5) . ? B3 H3 1.1000 . ? B4 C1 1.722(4) . ? B4 B10 1.764(5) . ? B4 B9 1.768(5) . ? B4 B5 1.780(5) . ? B4 H4 1.1000 . ? B5 C1 1.699(4) . ? B5 B11 1.761(5) . ? B5 B10 1.780(5) . ? B5 B6 1.791(4) . ? B5 H5 1.1000 . ? B6 C1 1.721(4) . ? B6 C2 1.745(4) . ? B6 B11 1.757(4) . ? B6 B7 1.772(4) . ? B6 H6 1.1000 . ? B7 C2 1.710(4) . ? B7 B12 1.776(5) . ? B7 B8 1.782(5) . ? B7 B11 1.784(5) . ? B7 H77 1.1000 . ? B8 C2 1.716(4) . ? B8 B12 1.776(5) . ? B8 B9 1.786(5) . ? B8 H8 1.1000 . ? B9 B10 1.774(6) . ? B9 B12 1.784(5) . ? B9 H9 1.1000 . ? B10 B12 1.772(5) . ? B10 B11 1.787(5) . ? B10 H10 1.1000 . ? B11 B12 1.800(5) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1 C2 1.658(3) . ? C1 S1 1.805(3) . ? C2 S2 1.777(2) . ? C3 C7 1.405(4) . ? C3 C4 1.437(4) . ? C3 C8 1.498(4) . ? C3 Co1 2.076(2) . ? C4 C5 1.412(4) . ? C4 C9 1.486(4) . ? C4 Co1 2.178(3) . ? C5 C6 1.428(4) . ? C5 C10 1.504(4) . ? C5 Co1 2.158(3) . ? C6 C7 1.414(4) . ? C6 C11 1.506(4) . ? C6 Co1 2.079(3) . ? C7 Co1 2.043(2) . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.343(4) . ? C12 S1 1.755(2) . ? C12 H12A 0.9300 . ? C13 C16 1.440(4) . ? C13 C14 1.502(4) . ? C14 O2 1.211(3) . ? C14 O1 1.322(3) . ? C15 O1 1.444(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.356(4) . ? C16 H16 0.9300 . ? C17 C18 1.491(4) . ? C17 Co1 1.951(3) . ? C18 O3 1.198(3) . ? C18 O4 1.350(3) . ? C19 O4 1.426(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? Co1 S1 2.1784(7) . ? Co1 S2 2.2623(7) . ? 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 C1 B3 C2 57.32(15) . . ? C1 B3 B8 104.2(2) . . ? C2 B3 B8 58.65(16) . . ? C1 B3 B9 104.5(2) . . ? C2 B3 B9 106.0(2) . . ? B8 B3 B9 60.82(19) . . ? C1 B3 B4 58.82(16) . . ? C2 B3 B4 105.8(2) . . ? B8 B3 B4 108.3(2) . . ? B9 B3 B4 59.7(2) . . ? C1 B3 H3 125.0 . . ? C2 B3 H3 123.7 . . ? B8 B3 H3 122.1 . . ? B9 B3 H3 122.6 . . ? B4 B3 H3 121.8 . . ? C1 B4 B10 103.9(2) . . ? C1 B4 B9 104.2(2) . . ? B10 B4 B9 60.3(2) . . ? C1 B4 B5 58.03(16) . . ? B10 B4 B5 60.3(2) . . ? B9 B4 B5 108.5(2) . . ? C1 B4 B3 58.57(16) . . ? B10 B4 B3 107.5(2) . . ? B9 B4 B3 59.53(19) . . ? B5 B4 B3 107.6(2) . . ? C1 B4 H4 125.5 . . ? B10 B4 H4 122.5 . . ? B9 B4 H4 122.3 . . ? B5 B4 H4 121.4 . . ? B3 B4 H4 121.9 . . ? C1 B5 B11 104.2(2) . . ? C1 B5 B10 104.2(2) . . ? B11 B5 B10 60.6(2) . . ? C1 B5 B4 59.26(16) . . ? B11 B5 B4 108.4(2) . . ? B10 B5 B4 59.42(19) . . ? C1 B5 B6 59.00(15) . . ? B11 B5 B6 59.27(18) . . ? B10 B5 B6 107.9(2) . . ? B4 B5 B6 109.0(2) . . ? C1 B5 H5 124.9 . . ? B11 B5 H5 122.5 . . ? B10 B5 H5 122.6 . . ? B4 B5 H5 120.9 . . ? B6 B5 H5 121.3 . . ? C1 B6 C2 57.15(14) . . ? C1 B6 B11 103.5(2) . . ? C2 B6 B11 105.3(2) . . ? C1 B6 B7 103.3(2) . . ? C2 B6 B7 58.18(16) . . ? B11 B6 B7 60.74(19) . . ? C1 B6 B5 57.83(16) . . ? C2 B6 B5 104.6(2) . . ? B11 B6 B5 59.51(18) . . ? B7 B6 B5 107.5(2) . . ? C1 B6 H6 125.7 . . ? C2 B6 H6 124.2 . . ? B11 B6 H6 122.8 . . ? B7 B6 H6 122.5 . . ? B5 B6 H6 122.6 . . ? C2 B7 B6 60.12(16) . . ? C2 B7 B12 105.6(2) . . ? B6 B7 B12 108.4(2) . . ? C2 B7 B8 58.84(17) . . ? B6 B7 B8 108.9(2) . . ? B12 B7 B8 59.9(2) . . ? C2 B7 B11 105.6(2) . . ? B6 B7 B11 59.20(18) . . ? B12 B7 B11 60.8(2) . . ? B8 B7 B11 108.4(2) . . ? C2 B7 H77 123.8 . . ? B6 B7 H77 121.1 . . ? B12 B7 H77 122.0 . . ? B8 B7 H77 121.3 . . ? B11 B7 H77 122.2 . . ? C2 B8 B3 59.95(17) . . ? C2 B8 B12 105.3(2) . . ? B3 B8 B12 107.7(2) . . ? C2 B8 B7 58.51(16) . . ? B3 B8 B7 108.1(2) . . ? B12 B8 B7 59.89(19) . . ? C2 B8 B9 106.0(2) . . ? B3 B8 B9 59.60(19) . . ? B12 B8 B9 60.1(2) . . ? B7 B8 B9 108.0(3) . . ? C2 B8 H8 123.7 . . ? B3 B8 H8 121.4 . . ? B12 B8 H8 122.4 . . ? B7 B8 H8 121.7 . . ? B9 B8 H8 122.1 . . ? B3 B9 B4 60.76(19) . . ? B3 B9 B10 108.1(2) . . ? B4 B9 B10 59.7(2) . . ? B3 B9 B12 107.4(2) . . ? B4 B9 B12 107.6(3) . . ? B10 B9 B12 59.7(2) . . ? B3 B9 B8 59.58(18) . . ? B4 B9 B8 108.2(2) . . ? B10 B9 B8 107.5(2) . . ? B12 B9 B8 59.7(2) . . ? B3 B9 H9 121.7 . . ? B4 B9 H9 121.5 . . ? B10 B9 H9 121.9 . . ? B12 B9 H9 122.2 . . ? B8 B9 H9 122.0 . . ? B4 B10 B12 108.3(3) . . ? B4 B10 B9 60.0(2) . . ? B12 B10 B9 60.4(2) . . ? B4 B10 B5 60.30(19) . . ? B12 B10 B5 108.0(2) . . ? B9 B10 B5 108.3(2) . . ? B4 B10 B11 108.0(2) . . ? B12 B10 B11 60.8(2) . . ? B9 B10 B11 108.9(2) . . ? B5 B10 B11 59.18(19) . . ? B4 B10 H10 121.7 . . ? B12 B10 H10 121.3 . . ? B9 B10 H10 121.3 . . ? B5 B10 H10 122.0 . . ? B11 B10 H10 121.5 . . ? B6 B11 B5 61.22(18) . . ? B6 B11 B7 60.05(17) . . ? B5 B11 B7 108.3(2) . . ? B6 B11 B10 109.1(2) . . ? B5 B11 B10 60.20(19) . . ? B7 B11 B10 107.1(2) . . ? B6 B11 B12 108.0(2) . . ? B5 B11 B12 107.6(2) . . ? B7 B11 B12 59.39(19) . . ? B10 B11 B12 59.2(2) . . ? B6 B11 H11 120.7 . . ? B5 B11 H11 121.2 . . ? B7 B11 H11 122.2 . . ? B10 B11 H11 121.9 . . ? B12 B11 H11 122.5 . . ? B10 B12 B7 108.1(2) . . ? B10 B12 B8 108.1(2) . . ? B7 B12 B8 60.21(19) . . ? B10 B12 B9 59.9(2) . . ? B7 B12 B9 108.4(2) . . ? B8 B12 B9 60.2(2) . . ? B10 B12 B11 60.0(2) . . ? B7 B12 B11 59.85(19) . . ? B8 B12 B11 107.9(2) . . ? B9 B12 B11 107.9(2) . . ? B10 B12 H12 121.7 . . ? B7 B12 H12 121.5 . . ? B8 B12 H12 121.6 . . ? B9 B12 H12 121.6 . . ? B11 B12 H12 121.9 . . ? C2 C1 B5 112.9(2) . . ? C2 C1 B3 62.03(16) . . ? B5 C1 B3 114.8(2) . . ? C2 C1 B6 62.17(15) . . ? B5 C1 B6 63.17(17) . . ? B3 C1 B6 115.3(2) . . ? C2 C1 B4 112.6(2) . . ? B5 C1 B4 62.71(18) . . ? B3 C1 B4 62.61(18) . . ? B6 C1 B4 115.3(2) . . ? C2 C1 S1 113.62(16) . . ? B5 C1 S1 125.01(18) . . ? B3 C1 S1 111.84(17) . . ? B6 C1 S1 118.48(17) . . ? B4 C1 S1 120.46(18) . . ? C1 C2 B7 108.9(2) . . ? C1 C2 B8 109.0(2) . . ? B7 C2 B8 62.65(18) . . ? C1 C2 B3 60.66(16) . . ? B7 C2 B3 112.6(2) . . ? B8 C2 B3 61.40(17) . . ? C1 C2 B6 60.68(15) . . ? B7 C2 B6 61.70(17) . . ? B8 C2 B6 113.3(2) . . ? B3 C2 B6 112.9(2) . . ? C1 C2 S2 118.99(16) . . ? B7 C2 S2 122.42(18) . . ? B8 C2 S2 122.14(19) . . ? B3 C2 S2 117.62(18) . . ? B6 C2 S2 117.29(17) . . ? C7 C3 C4 107.8(2) . . ? C7 C3 C8 125.7(3) . . ? C4 C3 C8 126.3(3) . . ? C7 C3 Co1 68.80(14) . . ? C4 C3 Co1 74.12(15) . . ? C8 C3 Co1 127.19(19) . . ? C5 C4 C3 107.6(2) . . ? C5 C4 C9 127.4(3) . . ? C3 C4 C9 125.0(3) . . ? C5 C4 Co1 70.25(15) . . ? C3 C4 Co1 66.49(14) . . ? C9 C4 Co1 130.6(2) . . ? C4 C5 C6 108.2(2) . . ? C4 C5 C10 126.3(3) . . ? C6 C5 C10 125.4(3) . . ? C4 C5 Co1 71.74(15) . . ? C6 C5 Co1 67.33(15) . . ? C10 C5 Co1 129.2(2) . . ? C7 C6 C5 107.5(3) . . ? C7 C6 C11 126.2(3) . . ? C5 C6 C11 125.9(3) . . ? C7 C6 Co1 68.60(15) . . ? C5 C6 Co1 73.33(15) . . ? C11 C6 Co1 128.5(2) . . ? C3 C7 C6 108.8(3) . . ? C3 C7 Co1 71.32(14) . . ? C6 C7 Co1 71.31(15) . . ? C3 C7 H7 125.6 . . ? C6 C7 H7 125.6 . . ? Co1 C7 H7 123.4 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 S1 123.0(2) . . ? C13 C12 H12A 118.5 . . ? S1 C12 H12A 118.5 . . ? C12 C13 C16 127.2(2) . . ? C12 C13 C14 116.7(2) . . ? C16 C13 C14 115.7(2) . . ? O2 C14 O1 124.2(3) . . ? O2 C14 C13 122.8(3) . . ? O1 C14 C13 113.1(2) . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C13 127.8(2) . . ? C17 C16 H16 116.1 . . ? C13 C16 H16 116.1 . . ? C16 C17 C18 116.1(2) . . ? C16 C17 Co1 126.8(2) . . ? C18 C17 Co1 117.15(19) . . ? O3 C18 O4 120.3(3) . . ? O3 C18 C17 126.4(3) . . ? O4 C18 C17 113.2(2) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 Co1 C7 89.50(11) . . ? C17 Co1 C3 101.36(10) . . ? C7 Co1 C3 39.88(11) . . ? C17 Co1 C6 115.71(12) . . ? C7 Co1 C6 40.09(11) . . ? C3 Co1 C6 66.98(11) . . ? C17 Co1 C5 154.14(11) . . ? C7 Co1 C5 66.06(11) . . ? C3 Co1 C5 65.71(10) . . ? C6 Co1 C5 39.34(12) . . ? C17 Co1 C4 139.53(10) . . ? C7 Co1 C4 65.81(11) . . ? C3 Co1 C4 39.39(10) . . ? C6 Co1 C4 65.40(11) . . ? C5 Co1 C4 38.00(11) . . ? C17 Co1 S1 94.27(8) . . ? C7 Co1 S1 140.88(8) . . ? C3 Co1 S1 101.54(8) . . ? C6 Co1 S1 149.14(9) . . ? C5 Co1 S1 109.91(9) . . ? C4 Co1 S1 87.35(7) . . ? C17 Co1 S2 89.60(8) . . ? C7 Co1 S2 125.07(8) . . ? C3 Co1 S2 160.21(8) . . ? C6 Co1 S2 93.47(8) . . ? C5 Co1 S2 97.52(8) . . ? C4 Co1 S2 130.70(8) . . ? S1 Co1 S2 93.92(3) . . ? C14 O1 C15 117.4(2) . . ? C18 O4 C19 117.2(3) . . ? C12 S1 C1 103.25(12) . . ? C12 S1 Co1 111.93(9) . . ? C1 S1 Co1 108.55(8) . . ? C2 S2 Co1 104.74(8) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.201 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.055 #===END data_11a _database_code_depnum_ccdc_archive 'CCDC 828294' #TrackingRef '- cif- revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H40 B10 Co2 O2 S8' _chemical_formula_sum 'C23 H40 B10 Co2 O2 S8' _chemical_formula_weight 830.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8731(11) _cell_length_b 11.5767(11) _cell_length_c 17.9049(17) _cell_angle_alpha 73.5510(10) _cell_angle_beta 85.0580(10) _cell_angle_gamma 62.2830(10) _cell_volume 1910.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2491 _cell_measurement_theta_min 2.456 _cell_measurement_theta_max 25.234 _exptl_crystal_description PLATE _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 1.329 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10523 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7387 _reflns_number_gt 4283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The (CH~3~)~2~CH- groups of the three 2-methylpropanedithioic acid ligands were found to be disordered over two sites and consequently refined with the occupancy of 0.5 for each part, and the interatomic distances and anisotropic displacement parameters of the disordered parts were restrained to be equal. ; _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^)+(0.0136P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7387 _refine_ls_number_parameters 424 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 1.024 _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 B3 B 0.5208(5) 0.1696(4) 0.4396(3) 0.0539(13) Uani 1 1 d . . . H3 H 0.4382 0.1413 0.4365 0.065 Uiso 1 1 calc R . . B4 B 0.7124(4) 0.2605(4) 0.3561(3) 0.0524(13) Uani 1 1 d . . . H4 H 0.7527 0.2904 0.2993 0.063 Uiso 1 1 calc R . . B5 B 0.6053(5) 0.3797(5) 0.4070(3) 0.0608(14) Uani 1 1 d . . . H5 H 0.5770 0.4881 0.3839 0.073 Uiso 1 1 calc R . . B6 B 0.4881(5) 0.3234(5) 0.4579(3) 0.0625(15) Uani 1 1 d . . . H6 H 0.3825 0.3961 0.4678 0.075 Uiso 1 1 calc R . . B7 B 0.6911(5) 0.0473(5) 0.4772(3) 0.0541(13) Uani 1 1 d . . . H7 H 0.7195 -0.0613 0.4990 0.065 Uiso 1 1 calc R . . B8 B 0.8089(5) 0.1025(5) 0.4259(3) 0.0559(13) Uani 1 1 d . . . H8 H 0.9135 0.0296 0.4146 0.067 Uiso 1 1 calc R . . B9 B 0.7764(5) 0.2553(5) 0.4446(3) 0.0654(15) Uani 1 1 d . . . H9 H 0.8605 0.2822 0.4464 0.078 Uiso 1 1 calc R . . B10 B 0.5834(5) 0.1650(5) 0.5287(3) 0.0659(15) Uani 1 1 d . . . H10 H 0.5415 0.1342 0.5847 0.079 Uiso 1 1 calc R . . B11 B 0.6361(5) 0.2963(5) 0.5073(3) 0.0705(16) Uani 1 1 d . . . H31 H 0.6281 0.3511 0.5501 0.085 Uiso 1 1 calc R . . B12 B 0.7622(5) 0.1241(5) 0.5201(3) 0.0686(16) Uani 1 1 d . . . H12 H 0.8363 0.0666 0.5711 0.082 Uiso 1 1 calc R . . C1 C 0.5389(4) 0.2991(3) 0.3696(2) 0.0469(10) Uani 1 1 d . . . C2 C 0.6597(3) 0.1370(3) 0.3817(2) 0.0418(9) Uani 1 1 d . . . C3 C 0.2233(4) 0.2793(4) 0.1922(2) 0.0637(12) Uani 1 1 d U A . C4 C 0.0772(5) 0.3051(5) 0.1759(4) 0.0938(16) Uani 1 1 d DU . . H4A H 0.0191 0.4028 0.1540 0.113 Uiso 1 1 calc R A . C5 C 0.0888(11) 0.2327(12) 0.1136(7) 0.124(3) Uani 0.50 1 d PDU A -1 H5A H 0.1235 0.2711 0.0672 0.187 Uiso 0.50 1 calc PR A -1 H5B H -0.0013 0.2442 0.1017 0.187 Uiso 0.50 1 calc PR A -1 H5C H 0.1515 0.1377 0.1330 0.187 Uiso 0.50 1 calc PR A -1 C6 C 0.0135(17) 0.2577(13) 0.2437(8) 0.124(4) Uani 0.50 1 d PDU A -1 H6A H -0.0690 0.2586 0.2276 0.186 Uiso 0.50 1 calc PR A -1 H6B H -0.0107 0.3162 0.2771 0.186 Uiso 0.50 1 calc PR A -1 H6C H 0.0777 0.1668 0.2715 0.186 Uiso 0.50 1 calc PR A -1 C5' C 0.0289(11) 0.3685(12) 0.0907(6) 0.124(3) Uani 0.50 1 d PD A -2 H5'1 H 0.0203 0.4585 0.0745 0.187 Uiso 0.50 1 calc PR A -2 H5'2 H -0.0597 0.3727 0.0834 0.187 Uiso 0.50 1 calc PR A -2 H5'3 H 0.0955 0.3145 0.0600 0.187 Uiso 0.50 1 calc PR A -2 C6' C 0.0394(17) 0.2002(13) 0.2181(9) 0.124(4) Uani 0.50 1 d PD A -2 H6'1 H 0.0656 0.1743 0.2724 0.186 Uiso 0.50 1 calc PR A -2 H6'2 H 0.0868 0.1227 0.1980 0.186 Uiso 0.50 1 calc PR A -2 H6'3 H -0.0593 0.2343 0.2117 0.186 Uiso 0.50 1 calc PR A -2 C7 C 0.6540(4) 0.1987(4) 0.0920(2) 0.0620(12) Uani 1 1 d U A . C8 C 0.7497(7) 0.1793(6) 0.0265(3) 0.1072(18) Uani 1 1 d DU . . H8A H 0.8444 0.1471 0.0466 0.129 Uiso 1 1 calc R B . C9 C 0.7065(15) 0.3089(14) -0.0316(10) 0.122(4) Uani 0.50 1 d PDU B -1 H9A H 0.6978 0.3758 -0.0069 0.184 Uiso 0.50 1 calc PR B -1 H9B H 0.6185 0.3360 -0.0560 0.184 Uiso 0.50 1 calc PR B -1 H9C H 0.7747 0.3008 -0.0702 0.184 Uiso 0.50 1 calc PR B -1 C10 C 0.7499(18) 0.0824(13) -0.0115(10) 0.134(4) Uani 0.50 1 d PDU B -1 H10A H 0.7706 -0.0021 0.0269 0.201 Uiso 0.50 1 calc PR B -1 H10B H 0.8191 0.0678 -0.0497 0.201 Uiso 0.50 1 calc PR B -1 H10C H 0.6600 0.1182 -0.0366 0.201 Uiso 0.50 1 calc PR B -1 C9' C 0.7863(14) 0.2813(14) -0.0134(10) 0.122(4) Uani 0.50 1 d PD B -2 H9'1 H 0.7584 0.3476 0.0151 0.184 Uiso 0.50 1 calc PR B -2 H9'2 H 0.7402 0.3241 -0.0644 0.184 Uiso 0.50 1 calc PR B -2 H9'3 H 0.8852 0.2418 -0.0182 0.184 Uiso 0.50 1 calc PR B -2 C10' C 0.8139(18) 0.0436(13) 0.0141(10) 0.134(4) Uani 0.50 1 d PD B -2 H10D H 0.7457 0.0115 0.0193 0.201 Uiso 0.50 1 calc PR B -2 H10E H 0.8893 -0.0175 0.0522 0.201 Uiso 0.50 1 calc PR B -2 H10F H 0.8486 0.0480 -0.0372 0.201 Uiso 0.50 1 calc PR B -2 C11 C 0.8200(3) 0.0085(4) 0.2726(2) 0.0447(10) Uani 1 1 d . . . H11 H 0.8395 0.0830 0.2496 0.054 Uiso 1 1 d R . . C12 C 0.9048(4) -0.1195(4) 0.27302(19) 0.0403(9) Uani 1 1 d U . . C13 C 1.0384(4) -0.1362(4) 0.2365(3) 0.0570(11) Uani 1 1 d U . . C14 C 1.2741(4) -0.1971(5) 0.2588(3) 0.1091(19) Uani 1 1 d . . . H14A H 1.3366 -0.2202 0.3015 0.164 Uiso 1 1 calc R . . H14B H 1.2683 -0.1174 0.2205 0.164 Uiso 1 1 calc R . . H14C H 1.3081 -0.2711 0.2357 0.164 Uiso 1 1 calc R . . C15 C 0.9903(6) -0.3157(5) 0.4162(3) 0.0779(15) Uani 1 1 d U . . H15 H 1.0109 -0.2520 0.4263 0.093 Uiso 1 1 calc R . . C16 C 1.0756(5) -0.4158(6) 0.3806(3) 0.0925(18) Uani 1 1 d U . . H16 H 1.1628 -0.4310 0.3619 0.111 Uiso 1 1 calc R . . C17 C 1.0058(8) -0.4882(5) 0.3783(3) 0.099(2) Uani 1 1 d U . . H17 H 1.0392 -0.5622 0.3579 0.119 Uiso 1 1 calc R . . C18 C 0.8807(6) -0.4352(5) 0.4104(3) 0.0865(16) Uani 1 1 d U . . H18 H 0.8143 -0.4660 0.4155 0.104 Uiso 1 1 calc R . . C19 C 0.8700(5) -0.3271(5) 0.4340(2) 0.0720(14) Uani 1 1 d U . . H19 H 0.7949 -0.2720 0.4578 0.086 Uiso 1 1 calc R . . C20 C 0.7373(5) -0.2640(4) 0.1977(3) 0.0716(13) Uani 1 1 d U C . C21 C 0.6447(7) -0.2580(5) 0.1349(3) 0.114(2) Uani 1 1 d DU . . H21 H 0.5496 -0.1959 0.1442 0.137 Uiso 1 1 calc R C . C22 C 0.6647(16) -0.2032(13) 0.0574(7) 0.138(4) Uani 0.50 1 d PDU C -1 H22A H 0.6247 -0.2294 0.0235 0.208 Uiso 0.50 1 calc PR C -1 H22B H 0.7625 -0.2365 0.0498 0.208 Uiso 0.50 1 calc PR C -1 H22C H 0.6205 -0.1060 0.0456 0.208 Uiso 0.50 1 calc PR C -1 C23 C 0.645(3) -0.3955(16) 0.1463(10) 0.128(4) Uani 0.50 1 d PDU C -1 H23A H 0.6421 -0.4358 0.2009 0.192 Uiso 0.50 1 calc PR C -1 H23B H 0.7273 -0.4550 0.1262 0.192 Uiso 0.50 1 calc PR C -1 H23C H 0.5643 -0.3809 0.1189 0.192 Uiso 0.50 1 calc PR C -1 C22' C 0.7260(16) -0.2898(13) 0.0687(7) 0.138(4) Uani 0.50 1 d PD C -2 H22D H 0.6707 -0.2930 0.0311 0.208 Uiso 0.50 1 calc PR C -2 H22E H 0.8067 -0.3763 0.0856 0.208 Uiso 0.50 1 calc PR C -2 H22F H 0.7545 -0.2211 0.0455 0.208 Uiso 0.50 1 calc PR C -2 C23' C 0.612(3) -0.3780(16) 0.1756(10) 0.128(4) Uani 0.50 1 d PD C -2 H23D H 0.5615 -0.3611 0.2213 0.192 Uiso 0.50 1 calc PR C -2 H23E H 0.6972 -0.4608 0.1902 0.192 Uiso 0.50 1 calc PR C -2 H23F H 0.5564 -0.3860 0.1402 0.192 Uiso 0.50 1 calc PR C -2 Co1 Co 0.48962(5) 0.22870(5) 0.21732(3) 0.04645(16) Uani 1 1 d . A . Co2 Co 0.89108(5) -0.28625(5) 0.31626(3) 0.04837(16) Uani 1 1 d . C . O1 O 1.0578(3) -0.1218(4) 0.16991(19) 0.1231(14) Uani 1 1 d U . . O2 O 1.1369(3) -0.1709(3) 0.28733(17) 0.0882(10) Uani 1 1 d U . . S1 S 0.42148(10) 0.38145(10) 0.28662(6) 0.0574(3) Uani 1 1 d . . . S2 S 0.65164(9) 0.05925(9) 0.30879(6) 0.0435(3) Uani 1 1 d . . . S3 S 0.29570(11) 0.37401(10) 0.14130(7) 0.0651(3) Uani 1 1 d . . . S4 S 0.33352(11) 0.15026(11) 0.26276(7) 0.0641(3) Uani 1 1 d . . . S5 S 0.62416(11) 0.31121(10) 0.14157(6) 0.0587(3) Uani 1 1 d . . . S6 S 0.57107(11) 0.10649(10) 0.12952(6) 0.0580(3) Uani 1 1 d . . . S7 S 0.67144(11) -0.21059(10) 0.27446(7) 0.0632(3) Uani 1 1 d . . . S8 S 0.91198(13) -0.32657(11) 0.19966(7) 0.0715(4) 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 B3 0.049(3) 0.055(3) 0.059(3) -0.020(3) 0.017(3) -0.024(3) B4 0.050(3) 0.046(3) 0.076(4) -0.028(3) 0.019(3) -0.030(2) B5 0.058(3) 0.058(3) 0.080(4) -0.038(3) 0.015(3) -0.029(3) B6 0.057(3) 0.063(3) 0.061(3) -0.032(3) 0.012(3) -0.015(3) B7 0.052(3) 0.050(3) 0.053(3) -0.015(3) 0.003(3) -0.017(2) B8 0.040(3) 0.059(3) 0.069(4) -0.025(3) -0.002(3) -0.019(2) B9 0.058(3) 0.074(4) 0.083(4) -0.041(3) 0.003(3) -0.034(3) B10 0.069(4) 0.063(3) 0.054(3) -0.021(3) 0.015(3) -0.020(3) B11 0.070(4) 0.068(4) 0.080(4) -0.044(3) 0.008(3) -0.024(3) B12 0.063(4) 0.068(3) 0.070(4) -0.031(3) -0.003(3) -0.018(3) C1 0.040(2) 0.039(2) 0.058(3) -0.016(2) 0.007(2) -0.0145(19) C2 0.035(2) 0.038(2) 0.052(3) -0.017(2) 0.0050(19) -0.0144(18) C3 0.053(3) 0.058(3) 0.080(3) -0.020(2) -0.001(2) -0.024(2) C4 0.057(3) 0.088(3) 0.139(5) -0.013(3) -0.012(3) -0.043(3) C5 0.077(6) 0.162(7) 0.138(6) -0.036(7) -0.029(5) -0.056(6) C6 0.069(6) 0.132(8) 0.189(9) -0.043(7) 0.012(6) -0.063(6) C5' 0.077(6) 0.162(7) 0.138(6) -0.036(7) -0.029(5) -0.056(6) C6' 0.069(6) 0.132(8) 0.189(9) -0.043(7) 0.012(6) -0.063(6) C7 0.076(3) 0.063(3) 0.051(3) -0.016(2) 0.017(2) -0.036(2) C8 0.163(5) 0.092(4) 0.094(4) -0.046(3) 0.072(4) -0.080(4) C9 0.166(10) 0.125(6) 0.110(7) -0.045(5) 0.084(8) -0.099(7) C10 0.167(11) 0.119(7) 0.099(8) -0.034(6) 0.075(7) -0.061(6) C9' 0.166(10) 0.125(6) 0.110(7) -0.045(5) 0.084(8) -0.099(7) C10' 0.167(11) 0.119(7) 0.099(8) -0.034(6) 0.075(7) -0.061(6) C11 0.036(2) 0.045(2) 0.054(3) -0.017(2) 0.0078(19) -0.0177(19) C12 0.038(2) 0.050(2) 0.032(2) -0.0120(19) -0.0012(17) -0.0181(19) C13 0.051(3) 0.082(3) 0.041(2) -0.023(2) 0.013(2) -0.032(2) C14 0.037(3) 0.145(5) 0.121(5) -0.018(4) 0.013(3) -0.034(3) C15 0.102(4) 0.074(3) 0.060(3) 0.003(3) -0.027(3) -0.050(3) C16 0.053(3) 0.091(4) 0.072(4) 0.010(3) -0.010(3) -0.001(3) C17 0.142(5) 0.043(3) 0.073(4) -0.007(3) -0.020(4) -0.011(3) C18 0.109(4) 0.075(3) 0.079(4) 0.006(3) -0.016(3) -0.057(3) C19 0.082(4) 0.069(3) 0.046(3) -0.009(2) 0.006(3) -0.025(3) C20 0.098(4) 0.053(2) 0.069(3) -0.009(2) -0.021(3) -0.040(3) C21 0.178(5) 0.095(3) 0.095(4) -0.039(3) -0.025(4) -0.070(4) C22 0.198(9) 0.135(9) 0.100(6) -0.017(7) -0.045(6) -0.091(7) C23 0.180(9) 0.126(5) 0.122(10) -0.059(6) -0.027(7) -0.087(6) C22' 0.198(9) 0.135(9) 0.100(6) -0.017(7) -0.045(6) -0.091(7) C23' 0.180(9) 0.126(5) 0.122(10) -0.059(6) -0.027(7) -0.087(6) Co1 0.0405(3) 0.0451(3) 0.0540(4) -0.0125(3) 0.0041(3) -0.0208(3) Co2 0.0519(4) 0.0391(3) 0.0450(3) -0.0105(3) -0.0025(3) -0.0134(3) O1 0.086(3) 0.232(4) 0.062(2) -0.045(3) 0.029(2) -0.084(3) O2 0.0490(19) 0.140(3) 0.066(2) -0.019(2) 0.0057(17) -0.041(2) S1 0.0466(7) 0.0451(6) 0.0677(8) -0.0185(6) 0.0013(6) -0.0088(5) S2 0.0380(6) 0.0397(5) 0.0546(7) -0.0180(5) 0.0072(5) -0.0173(5) S3 0.0540(7) 0.0576(7) 0.0728(8) -0.0019(6) -0.0098(6) -0.0239(6) S4 0.0500(7) 0.0628(7) 0.0769(8) -0.0061(7) 0.0045(6) -0.0315(6) S5 0.0617(7) 0.0530(6) 0.0672(8) -0.0158(6) 0.0141(6) -0.0334(6) S6 0.0690(8) 0.0582(6) 0.0546(7) -0.0169(6) 0.0058(6) -0.0353(6) S7 0.0617(8) 0.0536(6) 0.0766(9) -0.0159(6) -0.0073(6) -0.0278(6) S8 0.0921(10) 0.0631(7) 0.0637(8) -0.0322(7) 0.0066(7) -0.0314(7) _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 B3 C2 1.710(6) . ? B3 C1 1.739(6) . ? B3 B10 1.765(6) . ? B3 B6 1.767(6) . ? B3 B7 1.768(6) . ? B3 H3 1.1000 . ? B4 C2 1.711(5) . ? B4 C1 1.736(5) . ? B4 B9 1.760(6) . ? B4 B5 1.769(6) . ? B4 B8 1.777(6) . ? B4 H4 1.1000 . ? B5 C1 1.704(5) . ? B5 B11 1.758(7) . ? B5 B6 1.764(7) . ? B5 B9 1.778(6) . ? B5 H5 1.1000 . ? B6 C1 1.684(6) . ? B6 B11 1.758(7) . ? B6 B10 1.786(6) . ? B6 H6 1.1000 . ? B7 C2 1.698(5) . ? B7 B12 1.763(6) . ? B7 B8 1.766(6) . ? B7 B10 1.767(6) . ? B7 H7 1.1000 . ? B8 C2 1.691(5) . ? B8 B9 1.760(6) . ? B8 B12 1.772(7) . ? B8 H8 1.1000 . ? B9 B11 1.774(7) . ? B9 B12 1.783(7) . ? B9 H9 1.1000 . ? B10 B12 1.778(7) . ? B10 B11 1.797(7) . ? B10 H10 1.1000 . ? B11 B12 1.777(7) . ? B11 H31 1.1000 . ? B12 H12 1.1000 . ? C1 C2 1.679(4) . ? C1 S1 1.772(4) . ? C2 S2 1.811(3) . ? C3 C4 1.512(5) . ? C3 S3 1.664(4) . ? C3 S4 1.670(4) . ? C4 C6 1.445(12) . ? C4 C6' 1.451(11) . ? C4 C5' 1.513(9) . ? C4 C5 1.540(10) . ? C4 H4A 0.9800 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C5' H5'1 0.9600 . ? C5' H5'2 0.9600 . ? C5' H5'3 0.9600 . ? C6' H6'1 0.9600 . ? C6' H6'2 0.9600 . ? C6' H6'3 0.9600 . ? C7 C8 1.494(6) . ? C7 S6 1.670(4) . ? C7 S5 1.674(4) . ? C8 C9' 1.405(12) . ? C8 C9 1.448(11) . ? C8 C10 1.466(12) . ? C8 C10' 1.467(11) . ? C8 H8A 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C9' H9'1 0.9600 . ? C9' H9'2 0.9600 . ? C9' H9'3 0.9600 . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11 C12 1.330(4) . ? C11 S2 1.768(3) . ? C11 H11 0.9553 . ? C12 C13 1.490(5) . ? C12 Co2 1.937(4) . ? C13 O1 1.170(4) . ? C13 O2 1.304(4) . ? C14 O2 1.454(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C19 1.377(6) . ? C15 C16 1.388(6) . ? C15 Co2 2.032(4) . ? C15 H15 0.9300 . ? C16 C17 1.378(7) . ? C16 Co2 2.055(4) . ? C16 H16 0.9300 . ? C17 C18 1.358(7) . ? C17 Co2 2.076(4) . ? C17 H17 0.9300 . ? C18 C19 1.384(5) . ? C18 Co2 2.081(5) . ? C18 H18 0.9300 . ? C19 Co2 2.043(4) . ? C19 H19 0.9300 . ? C20 C21 1.539(6) . ? C20 S7 1.637(5) . ? C20 S8 1.688(5) . ? C21 C22 1.398(12) . ? C21 C22' 1.444(12) . ? C21 C23 1.546(13) . ? C21 C23' 1.560(13) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? Co1 S3 2.2421(11) . ? Co1 S1 2.2540(11) . ? Co1 S2 2.2576(10) . ? Co1 S6 2.2608(11) . ? Co1 S5 2.2619(12) . ? Co1 S4 2.2682(12) . ? Co2 S8 2.2359(12) . ? Co2 S7 2.2408(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 B3 C1 58.3(2) . . ? C2 B3 B10 104.8(3) . . ? C1 B3 B10 105.6(3) . . ? C2 B3 B6 103.7(3) . . ? C1 B3 B6 57.4(2) . . ? B10 B3 B6 60.7(3) . . ? C2 B3 B7 58.4(2) . . ? C1 B3 B7 105.8(3) . . ? B10 B3 B7 60.0(3) . . ? B6 B3 B7 107.8(3) . . ? C2 B3 H3 124.7 . . ? C1 B3 H3 123.9 . . ? B10 B3 H3 122.4 . . ? B6 B3 H3 122.9 . . ? B7 B3 H3 121.9 . . ? C2 B4 C1 58.3(2) . . ? C2 B4 B9 104.1(3) . . ? C1 B4 B9 105.3(3) . . ? C2 B4 B5 104.6(3) . . ? C1 B4 B5 58.2(2) . . ? B9 B4 B5 60.5(3) . . ? C2 B4 B8 58.0(2) . . ? C1 B4 B8 105.4(3) . . ? B9 B4 B8 59.7(3) . . ? B5 B4 B8 107.9(4) . . ? C2 B4 H4 124.8 . . ? C1 B4 H4 123.8 . . ? B9 B4 H4 123.0 . . ? B5 B4 H4 122.2 . . ? B8 B4 H4 122.3 . . ? C1 B5 B11 105.2(4) . . ? C1 B5 B6 58.1(2) . . ? B11 B5 B6 59.9(3) . . ? C1 B5 B4 60.0(2) . . ? B11 B5 B4 107.8(3) . . ? B6 B5 B4 107.6(3) . . ? C1 B5 B9 105.8(3) . . ? B11 B5 B9 60.2(3) . . ? B6 B5 B9 107.7(4) . . ? B4 B5 B9 59.5(2) . . ? C1 B5 H5 123.9 . . ? B11 B5 H5 122.3 . . ? B6 B5 H5 122.1 . . ? B4 B5 H5 121.5 . . ? B9 B5 H5 122.2 . . ? C1 B6 B11 106.1(4) . . ? C1 B6 B5 59.2(3) . . ? B11 B6 B5 59.9(3) . . ? C1 B6 B3 60.5(2) . . ? B11 B6 B3 108.4(3) . . ? B5 B6 B3 109.2(3) . . ? C1 B6 B10 107.1(3) . . ? B11 B6 B10 60.9(3) . . ? B5 B6 B10 109.2(4) . . ? B3 B6 B10 59.6(3) . . ? C1 B6 H6 123.1 . . ? B11 B6 H6 122.1 . . ? B5 B6 H6 121.1 . . ? B3 B6 H6 121.1 . . ? B10 B6 H6 121.4 . . ? C2 B7 B12 104.8(3) . . ? C2 B7 B8 58.4(2) . . ? B12 B7 B8 60.3(3) . . ? C2 B7 B10 105.2(3) . . ? B12 B7 B10 60.5(3) . . ? B8 B7 B10 108.8(3) . . ? C2 B7 B3 59.1(2) . . ? B12 B7 B3 108.2(3) . . ? B8 B7 B3 108.2(3) . . ? B10 B7 B3 59.9(2) . . ? C2 B7 H7 124.7 . . ? B12 B7 H7 122.2 . . ? B8 B7 H7 121.3 . . ? B10 B7 H7 121.9 . . ? B3 B7 H7 121.4 . . ? C2 B8 B9 104.9(3) . . ? C2 B8 B7 58.8(2) . . ? B9 B8 B7 108.5(3) . . ? C2 B8 B12 104.7(3) . . ? B9 B8 B12 60.6(3) . . ? B7 B8 B12 59.8(3) . . ? C2 B8 B4 59.1(2) . . ? B9 B8 B4 59.7(2) . . ? B7 B8 B4 108.4(3) . . ? B12 B8 B4 108.2(3) . . ? C2 B8 H8 124.7 . . ? B9 B8 H8 122.1 . . ? B7 B8 H8 121.3 . . ? B12 B8 H8 122.3 . . ? B4 B8 H8 121.3 . . ? B4 B9 B8 60.6(2) . . ? B4 B9 B11 107.5(3) . . ? B8 B9 B11 107.7(4) . . ? B4 B9 B5 60.0(2) . . ? B8 B9 B5 108.2(3) . . ? B11 B9 B5 59.3(3) . . ? B4 B9 B12 108.5(3) . . ? B8 B9 B12 60.0(3) . . ? B11 B9 B12 60.0(3) . . ? B5 B9 B12 107.7(4) . . ? B4 B9 H9 121.5 . . ? B8 B9 H9 121.5 . . ? B11 B9 H9 122.3 . . ? B5 B9 H9 122.0 . . ? B12 B9 H9 121.6 . . ? B3 B10 B7 60.1(2) . . ? B3 B10 B12 107.7(4) . . ? B7 B10 B12 59.6(3) . . ? B3 B10 B6 59.7(3) . . ? B7 B10 B6 107.0(3) . . ? B12 B10 B6 106.6(4) . . ? B3 B10 B11 106.7(4) . . ? B7 B10 B11 106.7(4) . . ? B12 B10 B11 59.6(3) . . ? B6 B10 B11 58.8(3) . . ? B3 B10 H10 121.9 . . ? B7 B10 H10 122.2 . . ? B12 B10 H10 122.1 . . ? B6 B10 H10 122.7 . . ? B11 B10 H10 122.8 . . ? B5 B11 B6 60.2(3) . . ? B5 B11 B9 60.5(3) . . ? B6 B11 B9 108.2(4) . . ? B5 B11 B12 108.9(4) . . ? B6 B11 B12 107.9(3) . . ? B9 B11 B12 60.3(3) . . ? B5 B11 B10 109.0(3) . . ? B6 B11 B10 60.3(3) . . ? B9 B11 B10 108.2(3) . . ? B12 B11 B10 59.7(3) . . ? B5 B11 H31 120.9 . . ? B6 B11 H31 121.7 . . ? B9 B11 H31 121.5 . . ? B12 B11 H31 121.7 . . ? B10 B11 H31 121.5 . . ? B7 B12 B8 59.9(3) . . ? B7 B12 B11 107.8(4) . . ? B8 B12 B11 107.1(4) . . ? B7 B12 B10 59.9(3) . . ? B8 B12 B10 108.0(3) . . ? B11 B12 B10 60.7(3) . . ? B7 B12 B9 107.6(3) . . ? B8 B12 B9 59.4(3) . . ? B11 B12 B9 59.8(3) . . ? B10 B12 B9 108.7(4) . . ? B7 B12 H12 122.0 . . ? B8 B12 H12 122.3 . . ? B11 B12 H12 121.9 . . ? B10 B12 H12 121.1 . . ? B9 B12 H12 121.8 . . ? C2 C1 B6 108.8(3) . . ? C2 C1 B5 108.9(3) . . ? B6 C1 B5 62.7(3) . . ? C2 C1 B4 60.1(2) . . ? B6 C1 B4 113.0(3) . . ? B5 C1 B4 61.9(2) . . ? C2 C1 B3 60.0(2) . . ? B6 C1 B3 62.1(3) . . ? B5 C1 B3 113.4(3) . . ? B4 C1 B3 112.0(3) . . ? C2 C1 S1 118.8(2) . . ? B6 C1 S1 122.0(3) . . ? B5 C1 S1 122.9(3) . . ? B4 C1 S1 118.4(3) . . ? B3 C1 S1 116.6(3) . . ? C1 C2 B8 112.1(3) . . ? C1 C2 B7 111.9(3) . . ? B8 C2 B7 62.8(2) . . ? C1 C2 B3 61.7(2) . . ? B8 C2 B3 114.6(3) . . ? B7 C2 B3 62.5(2) . . ? C1 C2 B4 61.6(2) . . ? B8 C2 B4 63.0(2) . . ? B7 C2 B4 114.9(3) . . ? B3 C2 B4 114.7(3) . . ? C1 C2 S2 115.5(2) . . ? B8 C2 S2 124.2(2) . . ? B7 C2 S2 119.8(2) . . ? B3 C2 S2 112.6(3) . . ? B4 C2 S2 119.1(3) . . ? C4 C3 S3 124.4(3) . . ? C4 C3 S4 124.3(4) . . ? S3 C3 S4 111.4(2) . . ? C6 C4 C3 114.0(8) . . ? C6' C4 C3 116.6(8) . . ? C6 C4 C5' 132.2(9) . . ? C6' C4 C5' 116.2(9) . . ? C3 C4 C5' 113.6(6) . . ? C6 C4 C5 110.5(8) . . ? C6' C4 C5 78.0(7) . . ? C3 C4 C5 105.9(6) . . ? C5' C4 C5 52.0(5) . . ? C6 C4 H4A 108.7 . . ? C6' C4 H4A 130.3 . . ? C3 C4 H4A 108.7 . . ? C5' C4 H4A 57.3 . . ? C5 C4 H4A 108.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C5' H5'1 109.5 . . ? C4 C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C4 C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? C4 C6' H6'1 109.5 . . ? C4 C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? C4 C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? C8 C7 S6 125.4(3) . . ? C8 C7 S5 123.6(4) . . ? S6 C7 S5 110.8(2) . . ? C9' C8 C10 121.2(12) . . ? C9 C8 C10 108.2(12) . . ? C9' C8 C10' 123.4(12) . . ? C9 C8 C10' 128.1(11) . . ? C9' C8 C7 120.5(9) . . ? C9 C8 C7 108.6(8) . . ? C10 C8 C7 113.2(9) . . ? C10' C8 C7 115.7(9) . . ? C9' C8 H8A 75.1 . . ? C9 C8 H8A 108.9 . . ? C10 C8 H8A 108.9 . . ? C10' C8 H8A 81.4 . . ? C7 C8 H8A 108.9 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C9' H9'1 109.5 . . ? C8 C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C8 C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C8 C10' H10D 109.5 . . ? C8 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C8 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C12 C11 S2 122.4(3) . . ? C12 C11 H11 124.5 . . ? S2 C11 H11 113.0 . . ? C11 C12 C13 112.6(3) . . ? C11 C12 Co2 132.4(3) . . ? C13 C12 Co2 115.0(3) . . ? O1 C13 O2 121.5(4) . . ? O1 C13 C12 125.9(4) . . ? O2 C13 C12 112.6(3) . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C19 C15 C16 108.3(5) . . ? C19 C15 Co2 70.7(3) . . ? C16 C15 Co2 71.0(3) . . ? C19 C15 H15 125.9 . . ? C16 C15 H15 125.9 . . ? Co2 C15 H15 124.0 . . ? C17 C16 C15 106.5(5) . . ? C17 C16 Co2 71.4(3) . . ? C15 C16 Co2 69.3(2) . . ? C17 C16 H16 126.7 . . ? C15 C16 H16 126.7 . . ? Co2 C16 H16 124.3 . . ? C18 C17 C16 109.8(5) . . ? C18 C17 Co2 71.1(3) . . ? C16 C17 Co2 69.7(3) . . ? C18 C17 H17 125.1 . . ? C16 C17 H17 125.1 . . ? Co2 C17 H17 125.7 . . ? C17 C18 C19 107.5(5) . . ? C17 C18 Co2 70.7(3) . . ? C19 C18 Co2 68.9(3) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? Co2 C18 H18 125.6 . . ? C15 C19 C18 107.9(5) . . ? C15 C19 Co2 69.8(3) . . ? C18 C19 Co2 71.9(3) . . ? C15 C19 H19 126.0 . . ? C18 C19 H19 126.0 . . ? Co2 C19 H19 123.9 . . ? C21 C20 S7 121.4(4) . . ? C21 C20 S8 126.8(4) . . ? S7 C20 S8 111.8(2) . . ? C22 C21 C20 116.7(9) . . ? C22' C21 C20 109.2(9) . . ? C22 C21 C23 111.4(10) . . ? C22' C21 C23 84.4(9) . . ? C20 C21 C23 112.2(9) . . ? C22 C21 C23' 132.8(10) . . ? C22' C21 C23' 108.0(10) . . ? C20 C21 C23' 102.4(8) . . ? C22 C21 H21 105.1 . . ? C22' C21 H21 137.5 . . ? C20 C21 H21 105.1 . . ? C23 C21 H21 105.1 . . ? C23' C21 H21 88.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C22' H22D 109.5 . . ? C21 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C21 C23' H23D 109.5 . . ? C21 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C21 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? S3 Co1 S1 86.54(4) . . ? S3 Co1 S2 165.91(5) . . ? S1 Co1 S2 94.54(4) . . ? S3 Co1 S6 90.55(4) . . ? S1 Co1 S6 167.84(5) . . ? S2 Co1 S6 91.16(4) . . ? S3 Co1 S5 94.10(5) . . ? S1 Co1 S5 93.42(4) . . ? S2 Co1 S5 99.85(4) . . ? S6 Co1 S5 75.00(4) . . ? S3 Co1 S4 75.24(4) . . ? S1 Co1 S4 96.37(5) . . ? S2 Co1 S4 90.68(4) . . ? S6 Co1 S4 94.30(4) . . ? S5 Co1 S4 165.01(5) . . ? C12 Co2 C15 89.04(16) . . ? C12 Co2 C19 112.59(18) . . ? C15 Co2 C19 39.49(16) . . ? C12 Co2 C16 103.8(2) . . ? C15 Co2 C16 39.71(17) . . ? C19 Co2 C16 66.28(19) . . ? C12 Co2 C17 142.3(2) . . ? C15 Co2 C17 65.29(19) . . ? C19 Co2 C17 64.9(2) . . ? C16 Co2 C17 38.96(18) . . ? C12 Co2 C18 151.57(19) . . ? C15 Co2 C18 65.74(19) . . ? C19 Co2 C18 39.20(16) . . ? C16 Co2 C18 65.5(2) . . ? C17 Co2 C18 38.14(19) . . ? C12 Co2 S8 92.12(11) . . ? C15 Co2 S8 146.67(19) . . ? C19 Co2 S8 155.28(16) . . ? C16 Co2 S8 108.35(18) . . ? C17 Co2 S8 95.30(16) . . ? C18 Co2 S8 116.10(17) . . ? C12 Co2 S7 98.23(10) . . ? C15 Co2 S7 136.79(19) . . ? C19 Co2 S7 100.18(15) . . ? C16 Co2 S7 157.27(18) . . ? C17 Co2 S7 119.5(2) . . ? C18 Co2 S7 92.31(15) . . ? S8 Co2 S7 75.93(5) . . ? C13 O2 C14 117.5(3) . . ? C1 S1 Co1 105.11(11) . . ? C11 S2 C2 101.77(16) . . ? C11 S2 Co1 110.70(12) . . ? C2 S2 Co1 105.41(11) . . ? C3 S3 Co1 87.18(14) . . ? C3 S4 Co1 86.17(16) . . ? C7 S5 Co1 87.02(15) . . ? C7 S6 Co1 87.14(14) . . ? C20 S7 Co2 86.58(16) . . ? C20 S8 Co2 85.56(16) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.423 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.066 #===END #===END data_10a _database_code_depnum_ccdc_archive 'CCDC 828295' #TrackingRef '- cif- revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H27 B10 Co O2 S4' _chemical_formula_sum 'C15 H27 B10 Co O2 S4' _chemical_formula_weight 534.68 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7245(12) _cell_length_b 14.4172(13) _cell_length_c 14.6045(14) _cell_angle_alpha 90.00 _cell_angle_beta 103.4240(10) _cell_angle_gamma 90.00 _cell_volume 2606.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3057 _cell_measurement_theta_min 2.434 _cell_measurement_theta_max 25.653 _exptl_crystal_description BLOCK _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096.0 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.587 _exptl_absorpt_correction_T_max 0.660 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14030 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5072 _reflns_number_gt 3222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Rigid-bond restraint was applied to the anisotropic displacement parameters of the Cp atoms. ; _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^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5072 _refine_ls_number_parameters 292 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.913 _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 B3 B 0.3227(3) 0.2735(2) 1.1058(3) 0.0539(9) Uani 1 1 d . . . H3 H 0.2955 0.3138 1.1617 0.065 Uiso 1 1 d R . . B4 B 0.3467(3) 0.1514(2) 1.1192(3) 0.0593(9) Uani 1 1 d . . . H4 H 0.3349 0.1236 1.1862 0.071 Uiso 1 1 d R . . B5 B 0.2989(3) 0.1010(3) 1.0063(3) 0.0661(10) Uani 1 1 d . . . H5 H 0.2606 0.0268 0.9956 0.079 Uiso 1 1 d R . . B6 B 0.2474(3) 0.1936(2) 0.9270(3) 0.0574(9) Uani 1 1 d . . . H6 H 0.1664 0.1863 0.8686 0.069 Uiso 1 1 d R . . B7 B 0.3570(3) 0.2670(3) 0.9191(3) 0.0658(10) Uani 1 1 d . . . H7 H 0.3545 0.3070 0.8571 0.079 Uiso 1 1 d R . . B8 B 0.4050(3) 0.3180(3) 1.0314(3) 0.0613(10) Uani 1 1 d . . . H8 H 0.4350 0.3890 1.0498 0.074 Uiso 1 1 d R . . B9 B 0.4529(3) 0.2280(3) 1.1137(3) 0.0636(10) Uani 1 1 d . . . H9 H 0.5180 0.2424 1.1763 0.076 Uiso 1 1 d R . . B10 B 0.4391(3) 0.1209(3) 1.0499(3) 0.0704(11) Uani 1 1 d . . . H10 H 0.4950 0.0655 1.0777 0.085 Uiso 1 1 d R . . B11 B 0.3768(3) 0.1458(3) 0.9307(3) 0.0728(11) Uani 1 1 d . . . H11 H 0.3925 0.1006 0.8730 0.087 Uiso 1 1 d R . . B12 B 0.4727(3) 0.2221(3) 0.9960(3) 0.0734(12) Uani 1 1 d . . . H12 H 0.5521 0.2332 0.9767 0.088 Uiso 1 1 d R . . C1 C 0.2720(2) 0.29782(19) 0.9879(2) 0.0526(7) Uani 1 1 d . . . C2 C 0.2376(2) 0.19406(19) 1.0421(2) 0.0516(7) Uani 1 1 d . . . C3 C 0.3006(4) 0.5185(2) 1.1367(3) 0.0804(10) Uani 1 1 d U . . H33 H 0.3550 0.4719 1.1678 0.096 Uiso 1 1 d R . . C4 C 0.1923(4) 0.5138(3) 1.1298(3) 0.0941(12) Uani 1 1 d U . . H44 H 0.1490 0.4576 1.1514 0.113 Uiso 1 1 d R . . C5 C 0.1461(4) 0.5962(4) 1.0878(3) 0.1071(14) Uani 1 1 d U . . H55 H 0.0587 0.5886 1.0618 0.129 Uiso 1 1 d R . . C6 C 0.2312(4) 0.6498(3) 1.0676(3) 0.0985(13) Uani 1 1 d U . . H66 H 0.2309 0.7198 1.0449 0.118 Uiso 1 1 d R . . C7 C 0.3245(3) 0.6011(3) 1.0998(3) 0.0820(10) Uani 1 1 d U . . H77 H 0.3948 0.6253 1.0953 0.098 Uiso 1 1 d R . . C8 C 0.1086(3) 0.1923(2) 1.1689(2) 0.0593(8) Uani 1 1 d . . . H18 H 0.1852 0.2005 1.2050 0.071 Uiso 1 1 d R . . C9 C 0.0250(3) 0.1850(2) 1.2075(2) 0.0631(9) Uani 1 1 d . . . H19 H 0.0380 0.1955 1.2796 0.076 Uiso 1 1 d R . . C10 C -0.0838(3) 0.1710(2) 1.1516(2) 0.0575(8) Uani 1 1 d . . . C11 C -0.2663(3) 0.1488(3) 1.1537(3) 0.0953(13) Uani 1 1 d . . . H11A H -0.2910 0.2026 1.1161 0.143 Uiso 1 1 calc R . . H11B H -0.3106 0.1394 1.1979 0.143 Uiso 1 1 calc R . . H11C H -0.2710 0.0955 1.1136 0.143 Uiso 1 1 calc R . . C12 C 0.2095(3) 0.5626(2) 0.8129(2) 0.0690(9) Uani 1 1 d . . . C13 C 0.1988(4) 0.5686(3) 0.7075(3) 0.0922(12) Uani 1 1 d . . . H13 H 0.2039 0.5041 0.6877 0.111 Uiso 1 1 calc R . . C14 C 0.2960(4) 0.6154(3) 0.6856(3) 0.1175(17) Uani 1 1 d . . . H14A H 0.2893 0.6157 0.6187 0.176 Uiso 1 1 calc R . . H14B H 0.3602 0.5823 0.7157 0.176 Uiso 1 1 calc R . . H14C H 0.3005 0.6781 0.7084 0.176 Uiso 1 1 calc R . . C15 C 0.0940(5) 0.5990(4) 0.6553(3) 0.164(3) Uani 1 1 d . . . H15A H 0.0388 0.5644 0.6754 0.245 Uiso 1 1 calc R . . H15B H 0.0879 0.5889 0.5893 0.245 Uiso 1 1 calc R . . H15C H 0.0854 0.6639 0.6666 0.245 Uiso 1 1 calc R . . Co1 Co 0.21959(4) 0.52604(3) 0.99719(3) 0.05699(16) Uani 1 1 d . . . O1 O -0.10748(18) 0.16783(16) 1.06690(16) 0.0722(6) Uani 1 1 d . . . O2 O -0.15562(18) 0.16230(17) 1.20396(16) 0.0776(7) Uani 1 1 d . . . S1 S 0.16745(6) 0.38024(5) 0.95325(6) 0.0613(2) Uani 1 1 d . . . S2 S 0.09982(6) 0.18453(6) 1.04864(6) 0.0611(2) Uani 1 1 d . . . S3 S 0.32176(8) 0.53446(6) 0.89151(7) 0.0719(3) Uani 1 1 d . . . S4 S 0.10497(8) 0.57170(6) 0.86474(6) 0.0712(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B3 0.049(2) 0.055(2) 0.052(2) 0.0038(16) 0.0013(17) 0.0011(17) B4 0.059(2) 0.057(2) 0.057(2) 0.0029(17) 0.0039(19) 0.0054(18) B5 0.080(3) 0.057(2) 0.060(2) -0.0016(18) 0.012(2) 0.011(2) B6 0.062(2) 0.058(2) 0.052(2) -0.0029(17) 0.0128(19) 0.0003(18) B7 0.059(2) 0.079(3) 0.061(2) 0.010(2) 0.015(2) 0.004(2) B8 0.046(2) 0.067(2) 0.067(3) 0.0065(19) 0.0072(19) 0.0011(18) B9 0.045(2) 0.071(2) 0.071(3) 0.010(2) 0.006(2) 0.0059(19) B10 0.063(3) 0.071(2) 0.077(3) 0.013(2) 0.015(2) 0.016(2) B11 0.073(3) 0.073(3) 0.076(3) -0.004(2) 0.027(2) 0.016(2) B12 0.055(2) 0.087(3) 0.080(3) 0.014(2) 0.019(2) 0.015(2) C1 0.0473(18) 0.0544(17) 0.0550(19) 0.0024(14) 0.0101(15) 0.0018(14) C2 0.0497(18) 0.0522(17) 0.0513(18) -0.0011(14) 0.0080(15) -0.0016(14) C3 0.114(3) 0.068(2) 0.051(2) -0.0022(16) 0.003(2) 0.005(2) C4 0.116(3) 0.114(3) 0.056(2) -0.017(2) 0.029(3) -0.034(3) C5 0.089(3) 0.157(4) 0.072(3) -0.048(3) 0.012(2) 0.028(3) C6 0.161(4) 0.059(2) 0.065(3) -0.0099(18) 0.005(3) 0.015(2) C7 0.099(3) 0.079(2) 0.064(2) -0.0136(19) 0.010(2) -0.023(2) C8 0.0531(19) 0.075(2) 0.0457(18) -0.0004(15) 0.0027(16) 0.0024(17) C9 0.057(2) 0.086(2) 0.0447(18) 0.0000(16) 0.0081(17) 0.0078(18) C10 0.057(2) 0.0655(19) 0.051(2) 0.0056(16) 0.0151(17) 0.0071(16) C11 0.051(2) 0.155(4) 0.080(3) 0.010(3) 0.015(2) -0.001(2) C12 0.079(2) 0.068(2) 0.060(2) 0.0093(17) 0.0144(19) 0.0084(18) C13 0.111(3) 0.106(3) 0.062(2) 0.012(2) 0.025(2) 0.023(3) C14 0.187(5) 0.100(3) 0.074(3) 0.004(2) 0.047(3) -0.045(3) C15 0.172(5) 0.249(7) 0.062(3) 0.045(4) 0.011(3) 0.086(5) Co1 0.0648(3) 0.0562(3) 0.0478(3) 0.00114(19) 0.0086(2) 0.0034(2) O1 0.0582(14) 0.1082(17) 0.0492(14) -0.0039(13) 0.0105(12) -0.0079(13) O2 0.0549(14) 0.1223(19) 0.0578(14) 0.0142(14) 0.0177(12) 0.0073(14) S1 0.0512(5) 0.0577(5) 0.0655(5) -0.0004(4) -0.0057(4) 0.0050(4) S2 0.0500(5) 0.0819(6) 0.0488(5) -0.0041(4) 0.0065(4) -0.0120(4) S3 0.0681(6) 0.0856(6) 0.0621(6) 0.0073(5) 0.0155(5) -0.0009(5) S4 0.0750(6) 0.0747(6) 0.0607(6) 0.0098(4) 0.0092(5) 0.0204(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B3 C2 1.698(4) . ? B3 C1 1.730(4) . ? B3 B9 1.760(5) . ? B3 B4 1.789(5) . ? B3 B8 1.794(5) . ? B3 H3 1.1193 . ? B4 C2 1.687(5) . ? B4 B9 1.762(5) . ? B4 B5 1.775(5) . ? B4 B10 1.776(5) . ? B4 H4 1.0988 . ? B5 C2 1.694(5) . ? B5 B11 1.769(5) . ? B5 B10 1.773(6) . ? B5 B6 1.789(5) . ? B5 H5 1.1703 . ? B6 C2 1.713(4) . ? B6 C1 1.736(4) . ? B6 B11 1.774(5) . ? B6 B7 1.776(5) . ? B6 H6 1.1809 . ? B7 C1 1.696(4) . ? B7 B12 1.755(5) . ? B7 B11 1.768(6) . ? B7 B8 1.771(6) . ? B7 H7 1.0680 . ? B8 C1 1.688(5) . ? B8 B12 1.768(5) . ? B8 B9 1.778(5) . ? B8 H8 1.1037 . ? B9 B10 1.791(6) . ? B9 B12 1.796(6) . ? B9 H9 1.1016 . ? B10 B12 1.756(6) . ? B10 B11 1.773(6) . ? B10 H10 1.0838 . ? B11 B12 1.751(6) . ? B11 H11 1.1202 . ? B12 H12 1.1224 . ? C1 S1 1.768(3) . ? C1 C2 1.794(4) . ? C2 S2 1.784(3) . ? C3 C4 1.361(6) . ? C3 C7 1.369(5) . ? C3 Co1 2.061(4) . ? C3 H33 0.9953 . ? C4 C5 1.402(6) . ? C4 Co1 2.053(4) . ? C4 H44 1.0679 . ? C5 C6 1.416(6) . ? C5 Co1 2.055(4) . ? C5 H55 1.0937 . ? C6 C7 1.366(5) . ? C6 Co1 2.048(4) . ? C6 H66 1.0621 . ? C7 Co1 2.066(4) . ? C7 H77 0.9770 . ? C8 C9 1.319(4) . ? C8 S2 1.737(3) . ? C8 H18 1.0025 . ? C9 C10 1.448(4) . ? C9 H19 1.0377 . ? C10 O1 1.204(4) . ? C10 O2 1.327(3) . ? C11 O2 1.442(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.517(5) . ? C12 S3 1.662(4) . ? C12 S4 1.681(4) . ? C13 C15 1.442(6) . ? C13 C14 1.507(5) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? Co1 S4 2.2344(10) . ? Co1 S3 2.2402(10) . ? Co1 S1 2.2522(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 B3 C1 63.11(18) . . ? C2 B3 B9 104.8(2) . . ? C1 B3 B9 105.6(2) . . ? C2 B3 B4 57.79(18) . . ? C1 B3 B4 108.8(2) . . ? B9 B3 B4 59.5(2) . . ? C2 B3 B8 107.2(3) . . ? C1 B3 B8 57.23(19) . . ? B9 B3 B8 60.0(2) . . ? B4 B3 B8 108.0(3) . . ? C2 B3 H3 119.0 . . ? C1 B3 H3 120.9 . . ? B9 B3 H3 126.2 . . ? B4 B3 H3 120.4 . . ? B8 B3 H3 125.3 . . ? C2 B4 B9 105.2(2) . . ? C2 B4 B5 58.5(2) . . ? B9 B4 B5 108.4(3) . . ? C2 B4 B10 105.1(3) . . ? B9 B4 B10 60.8(2) . . ? B5 B4 B10 59.9(2) . . ? C2 B4 B3 58.37(18) . . ? B9 B4 B3 59.4(2) . . ? B5 B4 B3 106.8(3) . . ? B10 B4 B3 107.5(3) . . ? C2 B4 H4 117.8 . . ? B9 B4 H4 122.2 . . ? B5 B4 H4 126.1 . . ? B10 B4 H4 131.5 . . ? B3 B4 H4 113.6 . . ? C2 B5 B11 105.5(3) . . ? C2 B5 B10 104.9(3) . . ? B11 B5 B10 60.1(2) . . ? C2 B5 B4 58.12(19) . . ? B11 B5 B4 108.0(3) . . ? B10 B5 B4 60.1(2) . . ? C2 B5 B6 58.85(19) . . ? B11 B5 B6 59.8(2) . . ? B10 B5 B6 107.3(3) . . ? B4 B5 B6 106.9(3) . . ? C2 B5 H5 123.9 . . ? B11 B5 H5 121.8 . . ? B10 B5 H5 123.3 . . ? B4 B5 H5 122.7 . . ? B6 B5 H5 121.2 . . ? C2 B6 C1 62.66(18) . . ? C2 B6 B11 104.5(3) . . ? C1 B6 B11 105.3(3) . . ? C2 B6 B7 107.4(3) . . ? C1 B6 B7 57.74(19) . . ? B11 B6 B7 59.7(2) . . ? C2 B6 B5 57.81(19) . . ? C1 B6 B5 108.6(3) . . ? B11 B6 B5 59.5(2) . . ? B7 B6 B5 108.2(3) . . ? C2 B6 H6 117.4 . . ? C1 B6 H6 118.0 . . ? B11 B6 H6 129.5 . . ? B7 B6 H6 124.9 . . ? B5 B6 H6 121.9 . . ? C1 B7 B12 105.8(3) . . ? C1 B7 B11 107.3(3) . . ? B12 B7 B11 59.6(2) . . ? C1 B7 B8 58.24(19) . . ? B12 B7 B8 60.2(2) . . ? B11 B7 B8 108.1(3) . . ? C1 B7 B6 59.96(19) . . ? B12 B7 B6 107.0(3) . . ? B11 B7 B6 60.1(2) . . ? B8 B7 B6 107.1(3) . . ? C1 B7 H7 117.6 . . ? B12 B7 H7 126.7 . . ? B11 B7 H7 126.2 . . ? B8 B7 H7 119.8 . . ? B6 B7 H7 120.5 . . ? C1 B8 B12 105.6(3) . . ? C1 B8 B7 58.7(2) . . ? B12 B8 B7 59.5(2) . . ? C1 B8 B9 106.6(3) . . ? B12 B8 B9 60.9(2) . . ? B7 B8 B9 108.3(3) . . ? C1 B8 B3 59.46(19) . . ? B12 B8 B3 106.8(3) . . ? B7 B8 B3 106.8(3) . . ? B9 B8 B3 59.1(2) . . ? C1 B8 H8 120.7 . . ? B12 B8 H8 129.2 . . ? B7 B8 H8 129.5 . . ? B9 B8 H8 117.9 . . ? B3 B8 H8 113.7 . . ? B3 B9 B4 61.1(2) . . ? B3 B9 B8 60.9(2) . . ? B4 B9 B8 110.0(3) . . ? B3 B9 B10 108.1(3) . . ? B4 B9 B10 60.0(2) . . ? B8 B9 B10 107.5(3) . . ? B3 B9 B12 107.1(3) . . ? B4 B9 B12 107.0(3) . . ? B8 B9 B12 59.3(2) . . ? B10 B9 B12 58.6(2) . . ? B3 B9 H9 120.0 . . ? B4 B9 H9 121.2 . . ? B8 B9 H9 119.9 . . ? B10 B9 H9 123.9 . . ? B12 B9 H9 123.9 . . ? B12 B10 B11 59.5(2) . . ? B12 B10 B5 107.7(3) . . ? B11 B10 B5 59.8(2) . . ? B12 B10 B4 108.2(3) . . ? B11 B10 B4 107.8(3) . . ? B5 B10 B4 60.0(2) . . ? B12 B10 B9 60.8(2) . . ? B11 B10 B9 107.7(3) . . ? B5 B10 B9 107.2(3) . . ? B4 B10 B9 59.2(2) . . ? B12 B10 H10 125.0 . . ? B11 B10 H10 128.5 . . ? B5 B10 H10 122.2 . . ? B4 B10 H10 115.6 . . ? B9 B10 H10 117.6 . . ? B12 B11 B7 59.8(2) . . ? B12 B11 B5 108.1(3) . . ? B7 B11 B5 109.5(3) . . ? B12 B11 B10 59.8(2) . . ? B7 B11 B10 108.4(3) . . ? B5 B11 B10 60.1(2) . . ? B12 B11 B6 107.3(3) . . ? B7 B11 B6 60.2(2) . . ? B5 B11 B6 60.7(2) . . ? B10 B11 B6 108.0(3) . . ? B12 B11 H11 123.5 . . ? B7 B11 H11 123.4 . . ? B5 B11 H11 118.7 . . ? B10 B11 H11 120.2 . . ? B6 B11 H11 122.0 . . ? B11 B12 B7 60.6(2) . . ? B11 B12 B10 60.7(2) . . ? B7 B12 B10 109.8(3) . . ? B11 B12 B8 109.0(3) . . ? B7 B12 B8 60.3(2) . . ? B10 B12 B8 109.5(3) . . ? B11 B12 B9 108.5(3) . . ? B7 B12 B9 108.2(3) . . ? B10 B12 B9 60.6(2) . . ? B8 B12 B9 59.8(2) . . ? B11 B12 H12 120.4 . . ? B7 B12 H12 117.1 . . ? B10 B12 H12 124.0 . . ? B8 B12 H12 119.3 . . ? B9 B12 H12 124.7 . . ? B8 C1 B7 63.1(2) . . ? B8 C1 B3 63.3(2) . . ? B7 C1 B3 113.3(2) . . ? B8 C1 B6 112.8(2) . . ? B7 C1 B6 62.3(2) . . ? B3 C1 B6 108.4(2) . . ? B8 C1 S1 127.9(2) . . ? B7 C1 S1 123.2(2) . . ? B3 C1 S1 120.2(2) . . ? B6 C1 S1 113.6(2) . . ? B8 C1 C2 107.7(2) . . ? B7 C1 C2 107.3(2) . . ? B3 C1 C2 57.57(17) . . ? B6 C1 C2 58.04(17) . . ? S1 C1 C2 116.24(18) . . ? B4 C2 B5 63.3(2) . . ? B4 C2 B3 63.84(19) . . ? B5 C2 B3 115.1(2) . . ? B4 C2 B6 114.7(2) . . ? B5 C2 B6 63.3(2) . . ? B3 C2 B6 111.0(2) . . ? B4 C2 S2 127.1(2) . . ? B5 C2 S2 118.9(2) . . ? B3 C2 S2 122.1(2) . . ? B6 C2 S2 110.4(2) . . ? B4 C2 C1 110.6(2) . . ? B5 C2 C1 110.3(2) . . ? B3 C2 C1 59.32(17) . . ? B6 C2 C1 59.30(17) . . ? S2 C2 C1 115.57(18) . . ? C4 C3 C7 109.1(4) . . ? C4 C3 Co1 70.4(2) . . ? C7 C3 Co1 70.8(2) . . ? C4 C3 H33 125.9 . . ? C7 C3 H33 124.9 . . ? Co1 C3 H33 128.5 . . ? C3 C4 C5 107.8(4) . . ? C3 C4 Co1 71.0(2) . . ? C5 C4 Co1 70.1(2) . . ? C3 C4 H44 126.8 . . ? C5 C4 H44 125.4 . . ? Co1 C4 H44 123.7 . . ? C4 C5 C6 106.9(4) . . ? C4 C5 Co1 70.0(2) . . ? C6 C5 Co1 69.5(2) . . ? C4 C5 H55 110.9 . . ? C6 C5 H55 138.4 . . ? Co1 C5 H55 107.7 . . ? C7 C6 C5 107.0(4) . . ? C7 C6 Co1 71.4(2) . . ? C5 C6 Co1 70.1(2) . . ? C7 C6 H66 122.5 . . ? C5 C6 H66 129.5 . . ? Co1 C6 H66 132.6 . . ? C6 C7 C3 109.2(4) . . ? C6 C7 Co1 69.9(2) . . ? C3 C7 Co1 70.4(2) . . ? C6 C7 H77 121.9 . . ? C3 C7 H77 128.9 . . ? Co1 C7 H77 125.8 . . ? C9 C8 S2 124.0(3) . . ? C9 C8 H18 124.6 . . ? S2 C8 H18 111.4 . . ? C8 C9 C10 122.0(3) . . ? C8 C9 H19 117.8 . . ? C10 C9 H19 120.0 . . ? O1 C10 O2 123.1(3) . . ? O1 C10 C9 124.3(3) . . ? O2 C10 C9 112.6(3) . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 S3 125.1(3) . . ? C13 C12 S4 124.0(3) . . ? S3 C12 S4 110.5(2) . . ? C15 C13 C14 117.1(4) . . ? C15 C13 C12 114.0(4) . . ? C14 C13 C12 110.9(4) . . ? C15 C13 H13 104.4 . . ? C14 C13 H13 104.4 . . ? C12 C13 H13 104.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C6 Co1 C4 67.00(17) . . ? C6 Co1 C5 40.39(17) . . ? C4 Co1 C5 39.90(17) . . ? C6 Co1 C3 65.71(15) . . ? C4 Co1 C3 38.62(17) . . ? C5 Co1 C3 65.66(17) . . ? C6 Co1 C7 38.77(15) . . ? C4 Co1 C7 65.33(16) . . ? C5 Co1 C7 65.74(17) . . ? C3 Co1 C7 38.74(14) . . ? C6 Co1 S4 97.74(13) . . ? C4 Co1 S4 128.50(16) . . ? C5 Co1 S4 96.27(14) . . ? C3 Co1 S4 161.33(11) . . ? C7 Co1 S4 130.98(12) . . ? C6 Co1 S3 108.23(15) . . ? C4 Co1 S3 155.08(15) . . ? C5 Co1 S3 147.19(17) . . ? C3 Co1 S3 116.51(14) . . ? C7 Co1 S3 95.22(11) . . ? S4 Co1 S3 75.77(4) . . ? C6 Co1 S1 159.81(15) . . ? C4 Co1 S1 94.92(12) . . ? C5 Co1 S1 119.66(17) . . ? C3 Co1 S1 106.19(11) . . ? C7 Co1 S1 142.48(12) . . ? S4 Co1 S1 86.47(3) . . ? S3 Co1 S1 91.95(4) . . ? C10 O2 C11 116.2(3) . . ? C1 S1 Co1 113.16(10) . . ? C8 S2 C2 102.49(15) . . ? C12 S3 Co1 86.90(12) . . ? C12 S4 Co1 86.63(12) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.372 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.055 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 828297' #TrackingRef '- cif- revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H21 B10 Co O2 S2' _chemical_formula_sum 'C12 H21 B10 Co O2 S2' _chemical_formula_weight 428.46 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.8123(6) _cell_length_b 20.9271(17) _cell_length_c 14.1251(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.8790(10) _cell_angle_gamma 90.00 _cell_volume 1977.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2362 _cell_measurement_theta_min 2.445 _cell_measurement_theta_max 25.321 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.46 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872.0 _exptl_absorpt_coefficient_mu 1.083 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.557 _exptl_absorpt_correction_T_max 0.608 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10764 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3885 _reflns_number_gt 2577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The MeCp group was disordered over two sites and consequently refined with the occupancy of 0.5 and the anisotropic displacement parameters of the disordered parts were restrained to be equal. ; _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^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3885 _refine_ls_number_parameters 265 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.050 _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 B3 B 0.0878(5) 0.55151(15) 0.3134(2) 0.0406(8) Uani 1 1 d . . . B4 B 0.4719(5) 0.58295(15) 0.2658(3) 0.0511(9) Uani 1 1 d . . . H4 H 0.5963 0.5671 0.2320 0.061 Uiso 1 1 calc R . . B5 B 0.2949(5) 0.64138(15) 0.2130(3) 0.0532(10) Uani 1 1 d . . . H5 H 0.3063 0.6647 0.1445 0.064 Uiso 1 1 calc R . . B6 B 0.0590(5) 0.62205(14) 0.2436(2) 0.0497(9) Uani 1 1 d . . . H6 H -0.0833 0.6329 0.1951 0.060 Uiso 1 1 calc R . . B7 B 0.0830(5) 0.62687(15) 0.3703(3) 0.0526(10) Uani 1 1 d . . . H7 H -0.0424 0.6412 0.4046 0.063 Uiso 1 1 calc R . . B8 B 0.2596(5) 0.56892(16) 0.4224(2) 0.0490(9) Uani 1 1 d . . . H8 H 0.2492 0.5445 0.4902 0.059 Uiso 1 1 calc R . . B9 B 0.4961(5) 0.58810(15) 0.3931(3) 0.0504(9) Uani 1 1 d . . . H9 H 0.6373 0.5762 0.4418 0.061 Uiso 1 1 calc R . . B10 B 0.4657(5) 0.65772(15) 0.3220(3) 0.0545(10) Uani 1 1 d . . . H10 H 0.5883 0.6923 0.3247 0.065 Uiso 1 1 calc R . . B11 B 0.2113(5) 0.68182(16) 0.3076(3) 0.0541(10) Uani 1 1 d . . . H11 H 0.1683 0.7325 0.3007 0.065 Uiso 1 1 calc R . . B12 B 0.3341(5) 0.64943(16) 0.4185(3) 0.0552(10) Uani 1 1 d . . . H12 H 0.3707 0.6787 0.4841 0.066 Uiso 1 1 calc R . . C1 C 0.2208(4) 0.56491(12) 0.22145(19) 0.0415(7) Uani 1 1 d . . . C2 C 0.3385(4) 0.53526(11) 0.32719(18) 0.0386(7) Uani 1 1 d . . . C3 C 0.3535(19) 0.3834(7) 0.0709(10) 0.055(3) Uani 0.50 1 d PU A -1 C4 C 0.4938(14) 0.3620(4) 0.1531(7) 0.066(2) Uani 0.50 1 d PU A -1 H4A H 0.6309 0.3691 0.1678 0.079 Uiso 0.50 1 calc PR A -1 C5 C 0.3675(18) 0.3256(4) 0.2097(7) 0.073(2) Uani 0.50 1 d PU A -1 H5A H 0.4156 0.3104 0.2715 0.087 Uiso 0.50 1 calc PR A -1 C6 C 0.2093(18) 0.3182(4) 0.1712(6) 0.0611(18) Uani 0.50 1 d PU A -1 H6A H 0.1241 0.2906 0.1957 0.073 Uiso 0.50 1 calc PR A -1 C7 C 0.146(2) 0.3507(5) 0.0881(9) 0.088(3) Uani 0.50 1 d PU A -1 H7A H 0.0189 0.3534 0.0507 0.106 Uiso 0.50 1 calc PR A -1 C8 C 0.4187(13) 0.4212(4) -0.0077(6) 0.1059(19) Uani 0.50 1 d PU A -1 H8A H 0.4560 0.3925 -0.0543 0.159 Uiso 0.50 1 calc PR A -1 H8B H 0.5313 0.4473 0.0192 0.159 Uiso 0.50 1 calc PR A -1 H8C H 0.3108 0.4479 -0.0384 0.159 Uiso 0.50 1 calc PR A -1 C3' C 0.4197(18) 0.3723(7) 0.0974(10) 0.055(3) Uani 0.50 1 d PU A -2 C4' C 0.3859(17) 0.3345(5) 0.1691(7) 0.066(2) Uani 0.50 1 d PU A -2 H4' H 0.4760 0.3165 0.2198 0.079 Uiso 0.50 1 calc PR A -2 C5' C 0.1363(17) 0.3285(5) 0.1422(8) 0.073(2) Uani 0.50 1 d PU A -2 H5' H 0.0446 0.3066 0.1713 0.087 Uiso 0.50 1 calc PR A -2 C6' C 0.1128(18) 0.3691(4) 0.0579(6) 0.0611(18) Uani 0.50 1 d PU A -2 H6' H -0.0125 0.3781 0.0212 0.073 Uiso 0.50 1 calc PR A -2 C7' C 0.2520(19) 0.3893(5) 0.0390(7) 0.088(3) Uani 0.50 1 d PU A -2 H7' H 0.2505 0.4160 -0.0138 0.106 Uiso 0.50 1 calc PR A -2 C8' C 0.6302(12) 0.3865(4) 0.0949(6) 0.1059(19) Uani 0.50 1 d PU A -2 H8'1 H 0.6843 0.3532 0.0608 0.159 Uiso 0.50 1 calc PR A -2 H8'2 H 0.7050 0.3891 0.1596 0.159 Uiso 0.50 1 calc PR A -2 H8'3 H 0.6385 0.4265 0.0627 0.159 Uiso 0.50 1 calc PR A -2 C9 C -0.0324(4) 0.48673(12) 0.3019(2) 0.0450(7) Uani 1 1 d . . . H9A H -0.1020 0.4816 0.3553 0.054 Uiso 1 1 calc R . . H9B H -0.1311 0.4875 0.2426 0.054 Uiso 1 1 calc R . . C10 C 0.1098(4) 0.43083(12) 0.29972(19) 0.0413(7) Uani 1 1 d . A . C11 C 0.0473(5) 0.37094(14) 0.3438(2) 0.0532(8) Uani 1 1 d . . . C12 C 0.1583(5) 0.27524(14) 0.4261(2) 0.0894(13) Uani 1 1 d . . . H12A H 0.0424 0.2796 0.4551 0.134 Uiso 1 1 calc R . . H12B H 0.2697 0.2615 0.4739 0.134 Uiso 1 1 calc R . . H12C H 0.1323 0.2442 0.3752 0.134 Uiso 1 1 calc R . . Co1 Co 0.24259(6) 0.416718(17) 0.18674(3) 0.05526(16) Uani 1 1 d . . . O1 O -0.1223(3) 0.35582(10) 0.33898(17) 0.0744(7) Uani 1 1 d . . . O2 O 0.2042(3) 0.33603(9) 0.38716(16) 0.0696(7) Uani 1 1 d . . . S1 S 0.16514(13) 0.51266(4) 0.12159(5) 0.0585(2) Uani 1 1 d . . . S2 S 0.37170(11) 0.45025(3) 0.32996(6) 0.0491(2) Uani 1 1 d . A . 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 B3 0.0402(19) 0.0370(18) 0.0451(19) -0.0029(16) 0.0095(16) 0.0083(15) B4 0.046(2) 0.0351(19) 0.075(3) 0.0104(19) 0.0181(19) 0.0025(16) B5 0.063(2) 0.0304(19) 0.067(2) 0.0093(18) 0.014(2) 0.0040(17) B6 0.050(2) 0.0336(19) 0.063(2) -0.0020(17) 0.0043(19) 0.0145(16) B7 0.047(2) 0.043(2) 0.067(2) -0.0161(19) 0.0095(19) 0.0046(17) B8 0.051(2) 0.050(2) 0.045(2) -0.0082(17) 0.0059(17) -0.0036(17) B9 0.045(2) 0.036(2) 0.064(2) -0.0004(18) -0.0051(18) -0.0041(16) B10 0.052(2) 0.0296(19) 0.080(3) 0.0052(19) 0.007(2) 0.0000(16) B11 0.052(2) 0.0331(19) 0.075(3) -0.0067(19) 0.006(2) 0.0106(16) B12 0.056(2) 0.041(2) 0.065(2) -0.0163(19) 0.001(2) -0.0048(18) C1 0.0479(18) 0.0279(15) 0.0483(17) 0.0023(13) 0.0082(14) 0.0060(13) C2 0.0382(17) 0.0281(15) 0.0480(17) 0.0022(13) 0.0044(14) 0.0037(12) C3 0.057(7) 0.051(4) 0.060(6) -0.012(4) 0.022(5) 0.004(4) C4 0.076(5) 0.051(4) 0.079(4) -0.008(3) 0.036(4) 0.019(3) C5 0.122(5) 0.032(3) 0.076(4) -0.007(3) 0.047(4) 0.001(3) C6 0.088(4) 0.034(3) 0.063(4) -0.016(3) 0.019(3) -0.004(3) C7 0.116(6) 0.063(5) 0.075(5) -0.037(4) -0.009(4) 0.019(4) C8 0.125(5) 0.112(5) 0.099(4) -0.022(4) 0.066(4) -0.006(4) C3' 0.057(7) 0.051(4) 0.060(6) -0.012(4) 0.022(5) 0.004(4) C4' 0.076(5) 0.051(4) 0.079(4) -0.008(3) 0.036(4) 0.019(3) C5' 0.122(5) 0.032(3) 0.076(4) -0.007(3) 0.047(4) 0.001(3) C6' 0.088(4) 0.034(3) 0.063(4) -0.016(3) 0.019(3) -0.004(3) C7' 0.116(6) 0.063(5) 0.075(5) -0.037(4) -0.009(4) 0.019(4) C8' 0.125(5) 0.112(5) 0.099(4) -0.022(4) 0.066(4) -0.006(4) C9 0.0382(17) 0.0428(17) 0.0536(18) -0.0059(15) 0.0075(14) -0.0014(14) C10 0.0406(17) 0.0332(16) 0.0489(17) -0.0041(13) 0.0051(14) -0.0033(13) C11 0.068(2) 0.0381(19) 0.052(2) -0.0075(15) 0.0083(19) -0.0128(18) C12 0.132(3) 0.038(2) 0.090(3) 0.0151(19) 0.000(2) -0.020(2) Co1 0.0692(3) 0.0321(2) 0.0704(3) -0.0104(2) 0.0280(2) 0.0015(2) O1 0.0693(16) 0.0636(15) 0.0913(17) 0.0043(13) 0.0173(14) -0.0235(13) O2 0.0795(16) 0.0352(12) 0.0854(16) 0.0135(12) -0.0067(13) -0.0100(11) S1 0.0861(7) 0.0438(5) 0.0465(5) -0.0055(4) 0.0146(4) 0.0024(4) S2 0.0453(5) 0.0275(4) 0.0716(5) 0.0052(4) 0.0041(4) 0.0039(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B3 C9 1.576(4) . ? B3 C2 1.716(4) . ? B3 C1 1.741(4) . ? B3 B6 1.766(4) . ? B3 B7 1.773(4) . ? B3 B8 1.786(4) . ? B4 C2 1.694(4) . ? B4 C1 1.749(4) . ? B4 B10 1.758(5) . ? B4 B9 1.776(5) . ? B4 B5 1.779(4) . ? B4 H4 1.1000 . ? B5 C1 1.689(4) . ? B5 B11 1.764(5) . ? B5 B10 1.779(5) . ? B5 B6 1.788(5) . ? B5 H5 1.1000 . ? B6 C1 1.695(4) . ? B6 B11 1.762(4) . ? B6 B7 1.770(5) . ? B6 H6 1.1000 . ? B7 B8 1.768(5) . ? B7 B11 1.779(5) . ? B7 B12 1.781(5) . ? B7 H7 1.1000 . ? B8 C2 1.693(4) . ? B8 B12 1.763(5) . ? B8 B9 1.783(5) . ? B8 H8 1.1000 . ? B9 C2 1.692(4) . ? B9 B10 1.759(5) . ? B9 B12 1.773(5) . ? B9 H9 1.1000 . ? B10 B12 1.776(5) . ? B10 B11 1.779(5) . ? B10 H10 1.1000 . ? B11 B12 1.767(5) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1 C2 1.675(3) . ? C1 S1 1.768(3) . ? C2 S2 1.793(2) . ? C3 C4 1.429(14) . ? C3 C8 1.497(16) . ? C3 C7 1.63(2) . ? C3 Co1 2.049(14) . ? C4 C5 1.490(12) . ? C4 Co1 2.184(8) . ? C4 H4A 0.9300 . ? C5 C6 1.122(14) . ? C5 Co1 2.088(9) . ? C5 H5A 0.9300 . ? C6 C7 1.355(12) . ? C6 Co1 2.081(9) . ? C6 H6A 0.9300 . ? C7 Co1 1.985(12) . ? C7 H7A 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C3' C7' 1.326(14) . ? C3' C4' 1.339(17) . ? C3' C8' 1.471(15) . ? C3' Co1 2.118(14) . ? C4' C5' 1.676(17) . ? C4' Co1 2.017(9) . ? C4' H4' 0.9300 . ? C5' C6' 1.448(12) . ? C5' Co1 2.039(11) . ? C5' H5' 0.9300 . ? C6' C7' 1.115(14) . ? C6' Co1 2.116(9) . ? C6' H6' 0.9300 . ? C7' Co1 2.177(10) . ? C7' H7' 0.9300 . ? C8' H8'1 0.9600 . ? C8' H8'2 0.9600 . ? C8' H8'3 0.9600 . ? C9 C10 1.523(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.497(4) . ? C10 S2 1.801(3) . ? C10 Co1 1.999(3) . ? C11 O1 1.187(3) . ? C11 O2 1.344(3) . ? C12 O2 1.444(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? Co1 S2 2.1649(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 B3 C2 109.1(2) . . ? C9 B3 C1 113.2(2) . . ? C2 B3 C1 57.96(15) . . ? C9 B3 B6 131.3(2) . . ? C2 B3 B6 103.4(2) . . ? C1 B3 B6 57.80(17) . . ? C9 B3 B7 139.3(3) . . ? C2 B3 B7 103.2(2) . . ? C1 B3 B7 104.6(2) . . ? B6 B3 B7 60.00(18) . . ? C9 B3 B8 120.5(2) . . ? C2 B3 B8 57.76(16) . . ? C1 B3 B8 105.1(2) . . ? B6 B3 B8 107.2(2) . . ? B7 B3 B8 59.55(18) . . ? C2 B4 C1 58.22(16) . . ? C2 B4 B10 103.5(2) . . ? C1 B4 B10 104.4(2) . . ? C2 B4 B9 58.32(17) . . ? C1 B4 B9 105.9(2) . . ? B10 B4 B9 59.70(19) . . ? C2 B4 B5 103.5(2) . . ? C1 B4 B5 57.21(16) . . ? B10 B4 B5 60.38(19) . . ? B9 B4 B5 108.0(3) . . ? C2 B4 H4 125.1 . . ? C1 B4 H4 124.1 . . ? B10 B4 H4 123.4 . . ? B9 B4 H4 121.7 . . ? B5 B4 H4 122.8 . . ? C1 B5 B11 104.9(3) . . ? C1 B5 B10 106.0(2) . . ? B11 B5 B10 60.3(2) . . ? C1 B5 B4 60.48(17) . . ? B11 B5 B4 107.6(3) . . ? B10 B5 B4 59.22(18) . . ? C1 B5 B6 58.26(17) . . ? B11 B5 B6 59.46(19) . . ? B10 B5 B6 107.8(3) . . ? B4 B5 B6 108.2(2) . . ? C1 B5 H5 123.7 . . ? B11 B5 H5 122.7 . . ? B10 B5 H5 122.2 . . ? B4 B5 H5 121.3 . . ? B6 B5 H5 122.0 . . ? C1 B6 B11 104.8(2) . . ? C1 B6 B3 60.37(17) . . ? B11 B6 B3 108.3(2) . . ? C1 B6 B7 106.7(2) . . ? B11 B6 B7 60.49(19) . . ? B3 B6 B7 60.20(18) . . ? C1 B6 B5 57.96(17) . . ? B11 B6 B5 59.61(19) . . ? B3 B6 B5 108.3(2) . . ? B7 B6 B5 108.4(2) . . ? C1 B6 H6 123.9 . . ? B11 B6 H6 122.5 . . ? B3 B6 H6 120.8 . . ? B7 B6 H6 121.4 . . ? B5 B6 H6 121.9 . . ? B8 B7 B6 107.9(2) . . ? B8 B7 B3 60.59(17) . . ? B6 B7 B3 59.79(18) . . ? B8 B7 B11 106.9(2) . . ? B6 B7 B11 59.5(2) . . ? B3 B7 B11 107.2(2) . . ? B8 B7 B12 59.59(18) . . ? B6 B7 B12 107.5(3) . . ? B3 B7 B12 108.1(2) . . ? B11 B7 B12 59.51(19) . . ? B8 B7 H7 121.9 . . ? B6 B7 H7 122.0 . . ? B3 B7 H7 121.6 . . ? B11 B7 H7 122.6 . . ? B12 B7 H7 122.0 . . ? C2 B8 B12 103.7(2) . . ? C2 B8 B7 104.4(2) . . ? B12 B8 B7 60.58(19) . . ? C2 B8 B9 58.21(17) . . ? B12 B8 B9 60.00(19) . . ? B7 B8 B9 108.8(2) . . ? C2 B8 B3 59.04(17) . . ? B12 B8 B3 108.3(2) . . ? B7 B8 B3 59.85(17) . . ? B9 B8 B3 108.7(2) . . ? C2 B8 H8 125.5 . . ? B12 B8 H8 122.5 . . ? B7 B8 H8 122.0 . . ? B9 B8 H8 121.1 . . ? B3 B8 H8 121.1 . . ? C2 B9 B10 103.5(2) . . ? C2 B9 B12 103.3(2) . . ? B10 B9 B12 60.4(2) . . ? C2 B9 B4 58.41(17) . . ? B10 B9 B4 59.64(19) . . ? B12 B9 B4 107.8(2) . . ? C2 B9 B8 58.22(17) . . ? B10 B9 B8 107.7(2) . . ? B12 B9 B8 59.44(19) . . ? B4 B9 B8 107.8(2) . . ? C2 B9 H9 125.8 . . ? B10 B9 H9 122.6 . . ? B12 B9 H9 122.7 . . ? B4 B9 H9 121.5 . . ? B8 B9 H9 121.7 . . ? B4 B10 B9 60.66(19) . . ? B4 B10 B12 108.5(2) . . ? B9 B10 B12 60.2(2) . . ? B4 B10 B5 60.40(18) . . ? B9 B10 B5 108.8(2) . . ? B12 B10 B5 107.7(2) . . ? B4 B10 B11 107.8(2) . . ? B9 B10 B11 107.9(3) . . ? B12 B10 B11 59.6(2) . . ? B5 B10 B11 59.45(18) . . ? B4 B10 H10 121.2 . . ? B9 B10 H10 121.2 . . ? B12 B10 H10 121.8 . . ? B5 B10 H10 121.7 . . ? B11 B10 H10 122.3 . . ? B6 B11 B5 60.93(19) . . ? B6 B11 B12 108.5(2) . . ? B5 B11 B12 108.7(2) . . ? B6 B11 B7 59.97(19) . . ? B5 B11 B7 109.1(2) . . ? B12 B11 B7 60.30(19) . . ? B6 B11 B10 108.9(2) . . ? B5 B11 B10 60.3(2) . . ? B12 B11 B10 60.12(19) . . ? B7 B11 B10 108.6(2) . . ? B6 B11 H11 121.2 . . ? B5 B11 H11 120.9 . . ? B12 B11 H11 121.5 . . ? B7 B11 H11 121.3 . . ? B10 B11 H11 121.4 . . ? B8 B12 B11 107.6(2) . . ? B8 B12 B9 60.56(19) . . ? B11 B12 B9 107.8(3) . . ? B8 B12 B10 107.9(2) . . ? B11 B12 B10 60.3(2) . . ? B9 B12 B10 59.42(19) . . ? B8 B12 B7 59.83(18) . . ? B11 B12 B7 60.18(18) . . ? B9 B12 B7 108.7(2) . . ? B10 B12 B7 108.7(2) . . ? B8 B12 H12 121.9 . . ? B11 B12 H12 121.8 . . ? B9 B12 H12 121.6 . . ? B10 B12 H12 121.7 . . ? B7 B12 H12 121.2 . . ? C2 C1 B5 108.3(2) . . ? C2 C1 B6 108.4(2) . . ? B5 C1 B6 63.78(19) . . ? C2 C1 B3 60.27(16) . . ? B5 C1 B3 114.2(2) . . ? B6 C1 B3 61.83(18) . . ? C2 C1 B4 59.26(16) . . ? B5 C1 B4 62.31(17) . . ? B6 C1 B4 114.1(2) . . ? B3 C1 B4 112.3(2) . . ? C2 C1 S1 118.46(17) . . ? B5 C1 S1 123.4(2) . . ? B6 C1 S1 122.32(19) . . ? B3 C1 S1 115.62(18) . . ? B4 C1 S1 117.87(19) . . ? C1 C2 B9 113.3(2) . . ? C1 C2 B8 112.6(2) . . ? B9 C2 B8 63.57(19) . . ? C1 C2 B4 62.52(17) . . ? B9 C2 B4 63.28(18) . . ? B8 C2 B4 116.3(2) . . ? C1 C2 B3 61.77(16) . . ? B9 C2 B3 116.6(2) . . ? B8 C2 B3 63.20(17) . . ? B4 C2 B3 116.3(2) . . ? C1 C2 S2 115.10(17) . . ? B9 C2 S2 124.89(18) . . ? B8 C2 S2 116.96(19) . . ? B4 C2 S2 121.21(19) . . ? B3 C2 S2 108.54(17) . . ? C4 C3 C8 121.4(11) . . ? C4 C3 C7 102.3(10) . . ? C8 C3 C7 136.0(11) . . ? C4 C3 Co1 75.4(7) . . ? C8 C3 Co1 128.2(9) . . ? C7 C3 Co1 64.1(6) . . ? C3 C4 C5 103.3(9) . . ? C3 C4 Co1 65.3(6) . . ? C5 C4 Co1 66.2(5) . . ? C3 C4 H4A 128.3 . . ? C5 C4 H4A 128.3 . . ? Co1 C4 H4A 131.6 . . ? C6 C5 C4 114.2(9) . . ? C6 C5 Co1 74.1(7) . . ? C4 C5 Co1 73.1(4) . . ? C6 C5 H5A 122.9 . . ? C4 C5 H5A 122.9 . . ? Co1 C5 H5A 121.4 . . ? C5 C6 C7 117.9(12) . . ? C5 C6 Co1 74.7(7) . . ? C7 C6 Co1 66.7(6) . . ? C5 C6 H6A 121.1 . . ? C7 C6 H6A 121.1 . . ? Co1 C6 H6A 129.7 . . ? C6 C7 C3 101.5(10) . . ? C6 C7 Co1 74.4(5) . . ? C3 C7 Co1 68.3(7) . . ? C6 C7 H7A 129.2 . . ? C3 C7 H7A 129.2 . . ? Co1 C7 H7A 120.3 . . ? C7' C3' C4' 112.2(13) . . ? C7' C3' C8' 131.3(14) . . ? C4' C3' C8' 116.5(11) . . ? C7' C3' Co1 74.4(7) . . ? C4' C3' Co1 67.1(7) . . ? C8' C3' Co1 126.4(9) . . ? C3' C4' C5' 100.6(9) . . ? C3' C4' Co1 75.2(7) . . ? C5' C4' Co1 66.3(5) . . ? C3' C4' H4' 129.7 . . ? C5' C4' H4' 129.7 . . ? Co1 C4' H4' 121.0 . . ? C6' C5' C4' 95.3(8) . . ? C6' C5' Co1 72.5(5) . . ? C4' C5' Co1 64.9(5) . . ? C6' C5' H5' 132.3 . . ? C4' C5' H5' 132.3 . . ? Co1 C5' H5' 122.5 . . ? C7' C6' C5' 116.9(10) . . ? C7' C6' Co1 78.0(7) . . ? C5' C6' Co1 66.8(5) . . ? C7' C6' H6' 121.6 . . ? C5' C6' H6' 121.6 . . ? Co1 C6' H6' 125.1 . . ? C6' C7' C3' 114.9(13) . . ? C6' C7' Co1 71.9(7) . . ? C3' C7' Co1 69.6(8) . . ? C6' C7' H7' 122.5 . . ? C3' C7' H7' 122.5 . . ? Co1 C7' H7' 127.7 . . ? C3' C8' H8'1 109.5 . . ? C3' C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C3' C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C10 C9 B3 110.1(2) . . ? C10 C9 H9A 109.6 . . ? B3 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? B3 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 113.8(3) . . ? C11 C10 S2 115.9(2) . . ? C9 C10 S2 115.30(18) . . ? C11 C10 Co1 114.54(19) . . ? C9 C10 Co1 121.0(2) . . ? S2 C10 Co1 69.24(10) . . ? O1 C11 O2 124.3(3) . . ? O1 C11 C10 123.4(3) . . ? O2 C11 C10 112.4(3) . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 Co1 C10 121.6(4) . . ? C7 Co1 C4' 54.7(5) . . ? C10 Co1 C4' 121.8(3) . . ? C7 Co1 C5' 26.1(4) . . ? C10 Co1 C5' 101.1(3) . . ? C4' Co1 C5' 48.8(5) . . ? C7 Co1 C3 47.5(6) . . ? C10 Co1 C3 168.0(4) . . ? C4' Co1 C3 49.6(4) . . ? C5' Co1 C3 67.0(5) . . ? C7 Co1 C6 38.8(3) . . ? C10 Co1 C6 100.0(3) . . ? C4' Co1 C6 35.6(4) . . ? C5' Co1 C6 17.3(3) . . ? C3 Co1 C6 68.2(5) . . ? C7 Co1 C5 62.9(4) . . ? C10 Co1 C5 104.1(2) . . ? C4' Co1 C5 17.7(3) . . ? C5' Co1 C5 48.1(4) . . ? C3 Co1 C5 67.2(4) . . ? C6 Co1 C5 31.2(4) . . ? C7 Co1 C6' 16.1(4) . . ? C10 Co1 C6' 125.3(3) . . ? C4' Co1 C6' 68.0(4) . . ? C5' Co1 C6' 40.7(3) . . ? C3 Co1 C6' 46.4(5) . . ? C6 Co1 C6' 54.8(3) . . ? C5 Co1 C6' 78.2(4) . . ? C7 Co1 C3' 54.9(6) . . ? C10 Co1 C3' 159.2(4) . . ? C4' Co1 C3' 37.7(4) . . ? C5' Co1 C3' 68.2(5) . . ? C3 Co1 C3' 15.8(5) . . ? C6 Co1 C3' 64.2(5) . . ? C5 Co1 C3' 55.3(4) . . ? C6' Co1 C3' 58.3(5) . . ? C7 Co1 S2 154.7(3) . . ? C10 Co1 S2 51.05(7) . . ? C4' Co1 S2 105.7(3) . . ? C5' Co1 S2 129.8(3) . . ? C3 Co1 S2 135.2(4) . . ? C6 Co1 S2 115.9(2) . . ? C5 Co1 S2 94.0(3) . . ? C6' Co1 S2 170.5(2) . . ? C3' Co1 S2 121.5(3) . . ? C7 Co1 C7' 37.7(4) . . ? C10 Co1 C7' 154.7(4) . . ? C4' Co1 C7' 63.5(4) . . ? C5' Co1 C7' 62.5(4) . . ? C3 Co1 C7' 20.5(3) . . ? C6 Co1 C7' 70.1(4) . . ? C5 Co1 C7' 79.8(4) . . ? C6' Co1 C7' 30.1(4) . . ? C3' Co1 C7' 35.9(4) . . ? S2 Co1 C7' 154.3(4) . . ? C7 Co1 C4 69.5(5) . . ? C10 Co1 C4 137.9(3) . . ? C4' Co1 C4 27.0(3) . . ? C5' Co1 C4 72.9(4) . . ? C3 Co1 C4 39.3(4) . . ? C6 Co1 C4 62.1(4) . . ? C5 Co1 C4 40.7(3) . . ? C6' Co1 C4 77.5(4) . . ? C3' Co1 C4 23.5(3) . . ? S2 Co1 C4 100.2(2) . . ? C7' Co1 C4 59.2(3) . . ? C11 O2 C12 116.2(3) . . ? C1 S1 Co1 103.24(9) . . ? C2 S2 C10 95.94(12) . . ? C2 S2 Co1 105.90(9) . . ? C10 S2 Co1 59.71(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.457 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.053 data_4 _database_code_depnum_ccdc_archive 'CCDC 828298' #TrackingRef '- cif- revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H29 B10 Co O6 S2' _chemical_formula_sum 'C20 H29 B10 Co O6 S2' _chemical_formula_weight 596.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.876(3) _cell_length_b 7.2866(11) _cell_length_c 20.337(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.195(2) _cell_angle_gamma 90.00 _cell_volume 2785.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2396 _cell_measurement_theta_min 2.467 _cell_measurement_theta_max 24.768 _exptl_crystal_description BLOCK _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.838 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13363 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4909 _reflns_number_gt 3017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0039P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4909 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _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 B3 B 0.27205(19) 1.0242(5) 0.67124(18) 0.0313(9) Uani 1 1 d . . . B4 B 0.41517(19) 0.9991(5) 0.74316(19) 0.0353(10) Uani 1 1 d . . . H4 H 0.4470 0.9771 0.7905 0.042 Uiso 1 1 calc R . . B5 B 0.40796(19) 0.8290(6) 0.68084(18) 0.0358(10) Uani 1 1 d . . . H5 H 0.4357 0.6967 0.6879 0.043 Uiso 1 1 calc R . . B6 B 0.3142(2) 1.0615(5) 0.59828(18) 0.0372(10) Uani 1 1 d . . . H6 H 0.2823 1.0822 0.5509 0.045 Uiso 1 1 calc R . . B7 B 0.3216(2) 0.8409(5) 0.63766(18) 0.0351(10) Uani 1 1 d . . . H7 H 0.2945 0.7169 0.6173 0.042 Uiso 1 1 calc R . . B8 B 0.3214(2) 1.2323(5) 0.66202(18) 0.0371(10) Uani 1 1 d . . . H8 H 0.2933 1.3646 0.6571 0.045 Uiso 1 1 calc R . . B9 B 0.4078(2) 1.2168(5) 0.70486(19) 0.0386(10) Uani 1 1 d . . . H9 H 0.4355 1.3377 0.7271 0.046 Uiso 1 1 calc R . . B10 B 0.4540(2) 1.0355(5) 0.66837(18) 0.0383(10) Uani 1 1 d . . . H10 H 0.5120 1.0387 0.6661 0.046 Uiso 1 1 calc R . . B11 B 0.3968(2) 0.9401(6) 0.60373(19) 0.0398(10) Uani 1 1 d . . . H11 H 0.4179 0.8818 0.5596 0.048 Uiso 1 1 calc R . . B12 B 0.3958(2) 1.1811(6) 0.61897(19) 0.0416(11) Uani 1 1 d . . . H12 H 0.4161 1.2807 0.5846 0.050 Uiso 1 1 calc R . . C1 C 0.33478(15) 0.8943(4) 0.71978(14) 0.0267(8) Uani 1 1 d . . . C2 C 0.33509(16) 1.1161(4) 0.73458(14) 0.0300(8) Uani 1 1 d . . . C3 C 0.3887(2) 1.0169(6) 0.93748(16) 0.0516(11) Uani 1 1 d . . . C4 C 0.3222(2) 1.0379(6) 0.96478(16) 0.0554(11) Uani 1 1 d . . . H4A H 0.3033 1.1475 0.9787 0.067 Uiso 1 1 calc R . . C5 C 0.2900(2) 0.8629(6) 0.96695(17) 0.0590(12) Uani 1 1 d . . . H5A H 0.2473 0.8366 0.9845 0.071 Uiso 1 1 calc R . . C6 C 0.3333(2) 0.7372(6) 0.93829(18) 0.0568(11) Uani 1 1 d . . . H6A H 0.3240 0.6129 0.9317 0.068 Uiso 1 1 calc R . . C7 C 0.3941(2) 0.8332(6) 0.92108(17) 0.0544(11) Uani 1 1 d . . . H7A H 0.4321 0.7808 0.9017 0.065 Uiso 1 1 calc R . . C8 C 0.4422(2) 1.1653(6) 0.93003(19) 0.0796(14) Uani 1 1 d . . . H8A H 0.4614 1.2059 0.9729 0.119 Uiso 1 1 calc R . . H8B H 0.4196 1.2665 0.9063 0.119 Uiso 1 1 calc R . . H8C H 0.4799 1.1186 0.9061 0.119 Uiso 1 1 calc R . . C9 C 0.1495(2) 1.3985(5) 0.9280(2) 0.0873(16) Uani 1 1 d . . . H9A H 0.1023 1.4159 0.9071 0.131 Uiso 1 1 calc R . . H9B H 0.1761 1.5103 0.9257 0.131 Uiso 1 1 calc R . . H9C H 0.1469 1.3654 0.9734 0.131 Uiso 1 1 calc R . . C10 C 0.1603(2) 1.0885(6) 0.89884(18) 0.0479(10) Uani 1 1 d . . . C11 C 0.19537(18) 0.9468(5) 0.86071(16) 0.0401(9) Uani 1 1 d . . . C12 C 0.15050(19) 0.8355(5) 0.82406(17) 0.0458(10) Uani 1 1 d . . . H12A H 0.1025 0.8515 0.8296 0.055 Uiso 1 1 calc R . . C13 C 0.16601(18) 0.6957(5) 0.77762(17) 0.0407(9) Uani 1 1 d . . . C14 C 0.22868(17) 0.6556(4) 0.75538(16) 0.0377(9) Uani 1 1 d . . . H14 H 0.2294 0.5716 0.7210 0.045 Uiso 1 1 calc R . . C15 C 0.1018(2) 0.5942(5) 0.7470(2) 0.0552(11) Uani 1 1 d . . . C16 C 0.0524(2) 0.4279(5) 0.6553(2) 0.0898(16) Uani 1 1 d . . . H16A H 0.0333 0.3390 0.6837 0.135 Uiso 1 1 calc R . . H16B H 0.0674 0.3675 0.6169 0.135 Uiso 1 1 calc R . . H16C H 0.0166 0.5174 0.6420 0.135 Uiso 1 1 calc R . . C17 C 0.19293(17) 1.0418(4) 0.68465(16) 0.0390(9) Uani 1 1 d . . . H17 H 0.1862 1.1031 0.7237 0.047 Uiso 1 1 calc R . . C18 C 0.13229(18) 0.9866(4) 0.65146(18) 0.0449(10) Uani 1 1 d . . . H18 H 0.0903 1.0175 0.6694 0.054 Uiso 1 1 calc R . . C19 C 0.1254(2) 0.8819(5) 0.58938(19) 0.0460(10) Uani 1 1 d . . . C20 C 0.0402(2) 0.7565(6) 0.5090(2) 0.0783(14) Uani 1 1 d . . . H20A H 0.0497 0.8303 0.4716 0.117 Uiso 1 1 calc R . . H20B H -0.0091 0.7218 0.5052 0.117 Uiso 1 1 calc R . . H20C H 0.0693 0.6483 0.5102 0.117 Uiso 1 1 calc R . . Co1 Co 0.29807(2) 0.93624(6) 0.87050(2) 0.03642(14) Uani 1 1 d . . . O1 O 0.17205(13) 0.8229(4) 0.56004(12) 0.0658(8) Uani 1 1 d . . . O2 O 0.05631(13) 0.8611(4) 0.56918(13) 0.0667(8) Uani 1 1 d . . . O3 O 0.11270(13) 0.5181(3) 0.69030(14) 0.0652(8) Uani 1 1 d . . . O4 O 0.04666(16) 0.5878(4) 0.77232(17) 0.0995(12) Uani 1 1 d . . . O5 O 0.18448(16) 1.2540(4) 0.89474(15) 0.0844(10) Uani 1 1 d . . . O6 O 0.11084(18) 1.0593(4) 0.93011(16) 0.1081(13) Uani 1 1 d . . . S1 S 0.30941(4) 0.75229(11) 0.78729(4) 0.0342(2) Uani 1 1 d . . . S2 S 0.30084(5) 1.19316(12) 0.80875(4) 0.0386(2) 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 B3 0.030(2) 0.036(2) 0.027(2) 0.0008(18) -0.0032(18) 0.0032(18) B4 0.025(2) 0.049(3) 0.031(2) 0.0024(19) -0.0002(18) 0.0023(19) B5 0.027(2) 0.051(3) 0.030(2) -0.005(2) 0.0033(18) 0.007(2) B6 0.033(2) 0.054(3) 0.024(2) 0.003(2) -0.0022(18) 0.004(2) B7 0.030(2) 0.050(3) 0.025(2) -0.0029(19) -0.0028(18) 0.006(2) B8 0.040(3) 0.042(3) 0.030(2) 0.007(2) 0.0045(19) 0.003(2) B9 0.037(2) 0.044(3) 0.034(2) 0.002(2) -0.0004(19) -0.008(2) B10 0.027(2) 0.058(3) 0.031(2) 0.006(2) 0.0046(18) 0.002(2) B11 0.031(2) 0.062(3) 0.027(2) 0.002(2) 0.0022(18) 0.005(2) B12 0.042(3) 0.056(3) 0.027(2) 0.008(2) 0.0038(19) -0.002(2) C1 0.0231(18) 0.033(2) 0.0240(18) 0.0023(15) 0.0009(14) 0.0015(14) C2 0.0295(19) 0.036(2) 0.0250(18) 0.0013(15) 0.0023(15) 0.0015(15) C3 0.045(3) 0.089(3) 0.019(2) 0.004(2) -0.0037(18) -0.012(2) C4 0.058(3) 0.087(3) 0.021(2) -0.008(2) 0.0022(19) 0.006(3) C5 0.047(3) 0.104(4) 0.026(2) 0.023(2) 0.0006(19) -0.014(3) C6 0.059(3) 0.067(3) 0.043(3) 0.019(2) -0.005(2) 0.004(2) C7 0.040(2) 0.092(3) 0.030(2) 0.013(2) -0.0029(18) 0.016(2) C8 0.063(3) 0.128(4) 0.045(3) -0.005(3) -0.008(2) -0.042(3) C9 0.092(4) 0.072(3) 0.105(4) -0.027(3) 0.045(3) 0.011(3) C10 0.041(2) 0.059(3) 0.045(2) -0.003(2) 0.015(2) 0.002(2) C11 0.036(2) 0.049(2) 0.037(2) 0.0036(18) 0.0107(17) 0.0035(18) C12 0.031(2) 0.055(3) 0.052(3) -0.005(2) 0.0090(19) -0.0018(19) C13 0.035(2) 0.040(2) 0.048(2) -0.0013(18) 0.0047(18) -0.0065(18) C14 0.036(2) 0.039(2) 0.038(2) -0.0032(17) 0.0017(17) -0.0064(17) C15 0.037(3) 0.056(3) 0.073(3) -0.008(2) 0.004(2) -0.008(2) C16 0.066(3) 0.072(3) 0.126(5) -0.028(3) -0.018(3) -0.020(3) C17 0.040(2) 0.044(2) 0.032(2) -0.0013(17) 0.0002(17) 0.0082(18) C18 0.033(2) 0.057(3) 0.045(2) 0.0003(19) 0.0044(19) 0.0062(19) C19 0.031(2) 0.057(3) 0.049(3) 0.000(2) -0.001(2) -0.003(2) C20 0.056(3) 0.104(4) 0.073(3) -0.035(3) -0.006(2) -0.018(3) Co1 0.0329(3) 0.0531(3) 0.0232(2) 0.0033(2) 0.0028(2) -0.0002(2) O1 0.0356(16) 0.108(2) 0.0536(18) -0.0229(16) 0.0051(14) -0.0002(15) O2 0.0338(16) 0.092(2) 0.073(2) -0.0298(17) -0.0046(14) -0.0033(14) O3 0.0439(17) 0.080(2) 0.071(2) -0.0243(16) -0.0016(15) -0.0193(15) O4 0.049(2) 0.115(3) 0.139(3) -0.050(2) 0.036(2) -0.0317(19) O5 0.095(2) 0.060(2) 0.108(3) -0.0216(18) 0.062(2) -0.0062(18) O6 0.115(3) 0.094(2) 0.129(3) -0.008(2) 0.087(3) 0.000(2) S1 0.0311(5) 0.0402(5) 0.0312(5) 0.0057(4) 0.0027(4) 0.0023(4) S2 0.0471(6) 0.0435(6) 0.0258(5) -0.0036(4) 0.0061(4) 0.0018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B3 C17 1.548(5) . ? B3 C1 1.750(4) . ? B3 B6 1.766(5) . ? B3 B8 1.798(5) . ? B3 B7 1.801(5) . ? B3 C2 1.802(5) . ? B4 C1 1.727(5) . ? B4 C2 1.730(5) . ? B4 B9 1.767(5) . ? B4 B10 1.768(5) . ? B4 B5 1.769(5) . ? B4 H4 1.1000 . ? B5 C1 1.720(4) . ? B5 B11 1.760(5) . ? B5 B10 1.768(5) . ? B5 B7 1.782(5) . ? B5 H5 1.1000 . ? B6 B11 1.788(5) . ? B6 B12 1.787(6) . ? B6 B8 1.794(5) . ? B6 B7 1.796(5) . ? B6 H6 1.1000 . ? B7 C1 1.711(4) . ? B7 B11 1.786(5) . ? B7 H7 1.1000 . ? B8 C2 1.701(5) . ? B8 B12 1.761(5) . ? B8 B9 1.782(5) . ? B8 H8 1.1000 . ? B9 C2 1.714(5) . ? B9 B12 1.760(5) . ? B9 B10 1.782(5) . ? B9 H9 1.1000 . ? B10 B11 1.767(5) . ? B10 B12 1.773(5) . ? B10 H10 1.1000 . ? B11 B12 1.784(5) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1 C2 1.644(4) . ? C1 S1 1.818(3) . ? C2 S2 1.785(3) . ? C3 C7 1.386(5) . ? C3 C4 1.426(5) . ? C3 C8 1.496(5) . ? C3 Co1 2.169(4) . ? C4 C5 1.415(5) . ? C4 Co1 2.068(3) . ? C4 H4A 0.9300 . ? C5 C6 1.391(5) . ? C5 Co1 2.052(3) . ? C5 H5A 0.9300 . ? C6 C7 1.415(5) . ? C6 Co1 2.069(3) . ? C6 H6A 0.9300 . ? C7 Co1 2.138(4) . ? C7 H7A 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O5 1.443(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 O6 1.195(4) . ? C10 O5 1.294(4) . ? C10 C11 1.483(4) . ? C11 C12 1.348(4) . ? C11 Co1 1.932(3) . ? C12 C13 1.437(4) . ? C12 H12A 0.9300 . ? C13 C14 1.337(4) . ? C13 C15 1.505(5) . ? C14 S1 1.750(3) . ? C14 H14 0.9300 . ? C15 O4 1.203(4) . ? C15 O3 1.313(4) . ? C16 O3 1.444(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.337(4) . ? C17 H17 0.9300 . ? C18 C19 1.471(5) . ? C18 H18 0.9300 . ? C19 O1 1.188(4) . ? C19 O2 1.340(4) . ? C20 O2 1.451(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? Co1 S1 2.1843(10) . ? Co1 S2 2.2575(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 B3 C1 124.0(3) . . ? C17 B3 B6 130.6(3) . . ? C1 B3 B6 103.0(2) . . ? C17 B3 B8 117.8(3) . . ? C1 B3 B8 100.6(2) . . ? B6 B3 B8 60.4(2) . . ? C17 B3 B7 132.1(3) . . ? C1 B3 B7 57.60(18) . . ? B6 B3 B7 60.4(2) . . ? B8 B3 B7 107.1(3) . . ? C17 B3 C2 115.4(3) . . ? C1 B3 C2 55.12(17) . . ? B6 B3 C2 103.0(2) . . ? B8 B3 C2 56.39(19) . . ? B7 B3 C2 102.4(2) . . ? C1 B4 C2 56.79(19) . . ? C1 B4 B9 104.1(3) . . ? C2 B4 B9 58.68(19) . . ? C1 B4 B10 104.6(3) . . ? C2 B4 B10 105.4(3) . . ? B9 B4 B10 60.5(2) . . ? C1 B4 B5 58.95(19) . . ? C2 B4 B5 105.3(3) . . ? B9 B4 B5 108.4(3) . . ? B10 B4 B5 60.0(2) . . ? C1 B4 H4 125.0 . . ? C2 B4 H4 124.3 . . ? B9 B4 H4 122.1 . . ? B10 B4 H4 122.6 . . ? B5 B4 H4 121.7 . . ? C1 B5 B11 104.3(3) . . ? C1 B5 B10 104.9(3) . . ? B11 B5 B10 60.1(2) . . ? C1 B5 B4 59.29(19) . . ? B11 B5 B4 108.1(3) . . ? B10 B5 B4 60.0(2) . . ? C1 B5 B7 58.45(19) . . ? B11 B5 B7 60.5(2) . . ? B10 B5 B7 109.1(3) . . ? B4 B5 B7 109.1(3) . . ? C1 B5 H5 125.0 . . ? B11 B5 H5 122.5 . . ? B10 B5 H5 122.0 . . ? B4 B5 H5 121.0 . . ? B7 B5 H5 120.7 . . ? B3 B6 B11 109.2(3) . . ? B3 B6 B12 108.7(3) . . ? B11 B6 B12 59.9(2) . . ? B3 B6 B8 60.7(2) . . ? B11 B6 B8 106.8(3) . . ? B12 B6 B8 58.9(2) . . ? B3 B6 B7 60.7(2) . . ? B11 B6 B7 59.8(2) . . ? B12 B6 B7 107.5(3) . . ? B8 B6 B7 107.5(3) . . ? B3 B6 H6 120.4 . . ? B11 B6 H6 121.8 . . ? B12 B6 H6 122.1 . . ? B8 B6 H6 122.5 . . ? B7 B6 H6 121.9 . . ? C1 B7 B5 58.96(19) . . ? C1 B7 B11 103.6(3) . . ? B5 B7 B11 59.1(2) . . ? C1 B7 B6 103.3(3) . . ? B5 B7 B6 107.1(3) . . ? B11 B7 B6 59.9(2) . . ? C1 B7 B3 59.71(19) . . ? B5 B7 B3 109.4(3) . . ? B11 B7 B3 107.7(3) . . ? B6 B7 B3 58.83(19) . . ? C1 B7 H7 125.1 . . ? B5 B7 H7 121.2 . . ? B11 B7 H7 123.1 . . ? B6 B7 H7 123.6 . . ? B3 B7 H7 120.8 . . ? C2 B8 B12 105.1(3) . . ? C2 B8 B9 58.9(2) . . ? B12 B8 B9 59.6(2) . . ? C2 B8 B6 106.1(3) . . ? B12 B8 B6 60.4(2) . . ? B9 B8 B6 108.4(3) . . ? C2 B8 B3 61.91(19) . . ? B12 B8 B3 108.5(3) . . ? B9 B8 B3 110.8(3) . . ? B6 B8 B3 58.9(2) . . ? C2 B8 H8 123.3 . . ? B12 B8 H8 122.7 . . ? B9 B8 H8 120.8 . . ? B6 B8 H8 122.5 . . ? B3 B8 H8 119.9 . . ? C2 B9 B12 104.6(3) . . ? C2 B9 B4 59.60(19) . . ? B12 B9 B4 107.6(3) . . ? C2 B9 B8 58.19(19) . . ? B12 B9 B8 59.6(2) . . ? B4 B9 B8 107.7(3) . . ? C2 B9 B10 105.5(3) . . ? B12 B9 B10 60.1(2) . . ? B4 B9 B10 59.7(2) . . ? B8 B9 B10 107.7(3) . . ? C2 B9 H9 124.3 . . ? B12 B9 H9 122.7 . . ? B4 B9 H9 121.5 . . ? B8 B9 H9 122.0 . . ? B10 B9 H9 122.2 . . ? B4 B10 B5 60.0(2) . . ? B4 B10 B11 107.9(3) . . ? B5 B10 B11 59.7(2) . . ? B4 B10 B12 107.0(3) . . ? B5 B10 B12 107.6(3) . . ? B11 B10 B12 60.5(2) . . ? B4 B10 B9 59.7(2) . . ? B5 B10 B9 107.8(3) . . ? B11 B10 B9 108.2(3) . . ? B12 B10 B9 59.4(2) . . ? B4 B10 H10 122.1 . . ? B5 B10 H10 121.9 . . ? B11 B10 H10 121.4 . . ? B12 B10 H10 122.2 . . ? B9 B10 H10 121.9 . . ? B5 B11 B10 60.2(2) . . ? B5 B11 B12 107.5(3) . . ? B10 B11 B12 59.9(2) . . ? B5 B11 B7 60.3(2) . . ? B10 B11 B7 109.0(3) . . ? B12 B11 B7 108.1(3) . . ? B5 B11 B6 108.4(3) . . ? B10 B11 B6 108.8(3) . . ? B12 B11 B6 60.1(2) . . ? B7 B11 B6 60.3(2) . . ? B5 B11 H11 121.8 . . ? B10 B11 H11 121.1 . . ? B12 B11 H11 122.1 . . ? B7 B11 H11 121.2 . . ? B6 B11 H11 121.2 . . ? B9 B12 B8 60.8(2) . . ? B9 B12 B10 60.6(2) . . ? B8 B12 B10 109.1(3) . . ? B9 B12 B11 108.4(3) . . ? B8 B12 B11 108.4(3) . . ? B10 B12 B11 59.6(2) . . ? B9 B12 B6 109.6(3) . . ? B8 B12 B6 60.7(2) . . ? B10 B12 B6 108.6(3) . . ? B11 B12 B6 60.1(2) . . ? B9 B12 H12 120.8 . . ? B8 B12 H12 121.0 . . ? B10 B12 H12 121.4 . . ? B11 B12 H12 122.0 . . ? B6 B12 H12 120.9 . . ? C2 C1 B7 113.6(2) . . ? C2 C1 B5 111.5(2) . . ? B7 C1 B5 62.6(2) . . ? C2 C1 B4 61.72(19) . . ? B7 C1 B4 114.6(2) . . ? B5 C1 B4 61.8(2) . . ? C2 C1 B3 64.03(19) . . ? B7 C1 B3 62.7(2) . . ? B5 C1 B3 114.9(2) . . ? B4 C1 B3 116.7(2) . . ? C2 C1 S1 114.72(18) . . ? B7 C1 S1 125.7(2) . . ? B5 C1 S1 117.9(2) . . ? B4 C1 S1 109.2(2) . . ? B3 C1 S1 121.5(2) . . ? C1 C2 B8 109.5(2) . . ? C1 C2 B9 110.2(2) . . ? B8 C2 B9 62.9(2) . . ? C1 C2 B4 61.49(18) . . ? B8 C2 B4 113.3(2) . . ? B9 C2 B4 61.7(2) . . ? C1 C2 S2 117.94(19) . . ? B8 C2 S2 122.6(2) . . ? B9 C2 S2 121.8(2) . . ? B4 C2 S2 116.7(2) . . ? C1 C2 B3 60.84(18) . . ? B8 C2 B3 61.7(2) . . ? B9 C2 B3 113.9(2) . . ? B4 C2 B3 113.8(2) . . ? S2 C2 B3 117.1(2) . . ? C7 C3 C4 106.5(4) . . ? C7 C3 C8 127.5(4) . . ? C4 C3 C8 126.0(4) . . ? C7 C3 Co1 70.0(2) . . ? C4 C3 Co1 66.5(2) . . ? C8 C3 Co1 129.3(3) . . ? C5 C4 C3 108.1(4) . . ? C5 C4 Co1 69.3(2) . . ? C3 C4 Co1 74.2(2) . . ? C5 C4 H4A 125.9 . . ? C3 C4 H4A 125.9 . . ? Co1 C4 H4A 122.2 . . ? C6 C5 C4 108.1(4) . . ? C6 C5 Co1 71.0(2) . . ? C4 C5 Co1 70.51(19) . . ? C6 C5 H5A 126.0 . . ? C4 C5 H5A 126.0 . . ? Co1 C5 H5A 124.2 . . ? C5 C6 C7 107.4(4) . . ? C5 C6 Co1 69.6(2) . . ? C7 C6 Co1 73.0(2) . . ? C5 C6 H6A 126.3 . . ? C7 C6 H6A 126.3 . . ? Co1 C6 H6A 122.7 . . ? C3 C7 C6 109.8(4) . . ? C3 C7 Co1 72.4(2) . . ? C6 C7 Co1 67.7(2) . . ? C3 C7 H7A 125.1 . . ? C6 C7 H7A 125.1 . . ? Co1 C7 H7A 126.3 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O6 C10 O5 119.8(4) . . ? O6 C10 C11 124.2(4) . . ? O5 C10 C11 116.0(3) . . ? C12 C11 C10 114.9(3) . . ? C12 C11 Co1 127.4(3) . . ? C10 C11 Co1 117.7(3) . . ? C11 C12 C13 129.4(3) . . ? C11 C12 H12A 115.3 . . ? C13 C12 H12A 115.3 . . ? C14 C13 C12 128.1(3) . . ? C14 C13 C15 117.2(3) . . ? C12 C13 C15 114.6(3) . . ? C13 C14 S1 123.7(3) . . ? C13 C14 H14 118.2 . . ? S1 C14 H14 118.2 . . ? O4 C15 O3 124.7(4) . . ? O4 C15 C13 122.5(4) . . ? O3 C15 C13 112.8(3) . . ? O3 C16 H16A 109.5 . . ? O3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 B3 133.0(3) . . ? C18 C17 H17 113.5 . . ? B3 C17 H17 113.5 . . ? C17 C18 C19 126.5(3) . . ? C17 C18 H18 116.8 . . ? C19 C18 H18 116.8 . . ? O1 C19 O2 123.4(4) . . ? O1 C19 C18 127.4(3) . . ? O2 C19 C18 109.3(3) . . ? O2 C20 H20A 109.5 . . ? O2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C11 Co1 C5 87.04(15) . . ? C11 Co1 C4 102.48(15) . . ? C5 Co1 C4 40.17(13) . . ? C11 Co1 C6 110.84(15) . . ? C5 Co1 C6 39.44(13) . . ? C4 Co1 C6 66.58(16) . . ? C11 Co1 C7 149.62(14) . . ? C5 Co1 C7 65.27(15) . . ? C4 Co1 C7 64.75(15) . . ? C6 Co1 C7 39.25(13) . . ? C11 Co1 C3 141.33(15) . . ? C5 Co1 C3 65.96(14) . . ? C4 Co1 C3 39.24(13) . . ? C6 Co1 C3 65.40(15) . . ? C7 Co1 C3 37.52(13) . . ? C11 Co1 S1 96.45(11) . . ? C5 Co1 S1 126.99(14) . . ? C4 Co1 S1 155.42(11) . . ? C6 Co1 S1 92.17(12) . . ? C7 Co1 S1 91.08(11) . . ? C3 Co1 S1 121.71(12) . . ? C11 Co1 S2 89.03(10) . . ? C5 Co1 S2 139.04(14) . . ? C4 Co1 S2 101.81(12) . . ? C6 Co1 S2 158.40(12) . . ? C7 Co1 S2 119.85(12) . . ? C3 Co1 S2 93.90(11) . . ? S1 Co1 S2 93.96(4) . . ? C19 O2 C20 116.2(3) . . ? C15 O3 C16 116.5(3) . . ? C10 O5 C9 118.1(3) . . ? C14 S1 C1 103.25(15) . . ? C14 S1 Co1 113.04(12) . . ? C1 S1 Co1 106.67(10) . . ? C2 S2 Co1 103.74(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.442 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.058