Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_address ; Department of Chemistry Fudan University Handan Road 220 Shanghai 100433 CHINA ; _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Syntheses and Structures of Heterometallic Clusters by the Reaction of ortho-Carboranyl Cobaltadichalcogenolato Complexes ; loop_ _publ_author_name 'Guo-Xin Jin' 'Shuyi Cai' 'Yin-Qiang Chen' 'Xiu-Feng Hou' ; JiaSheng Zhang ; # Attachment '4a_tri_CpstarSCo3_f60420f.cif' data_f60420f _database_code_depnum_ccdc_archive 'CCDC 621982' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H25 B10 Co3 O5 S2' _chemical_formula_weight 658.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.123(3) _cell_length_b 15.505(4) _cell_length_c 34.664(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5440(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 878 _cell_measurement_theta_min 2.330 _cell_measurement_theta_max 21.084 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 1.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7545 _exptl_absorpt_correction_T_max 0.8258 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.37 _diffrn_reflns_number 21657 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.1046 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4788 _reflns_number_gt 2454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^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 4788 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 0.773 _refine_ls_restrained_S_all 0.773 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.89673(6) 0.06873(3) 0.129901(17) 0.03456(17) Uani 1 1 d . . . Co2 Co 1.10296(6) 0.08295(4) 0.173574(18) 0.04112(18) Uani 1 1 d . . . Co3 Co 0.91398(6) 0.17779(4) 0.184735(17) 0.03750(17) Uani 1 1 d . . . S1 S 0.85309(10) 0.20731(7) 0.12348(3) 0.0346(3) Uani 1 1 d . . . S2 S 1.10289(11) 0.08070(7) 0.10935(3) 0.0357(3) Uani 1 1 d . . . C1 C 0.9821(4) 0.2483(3) 0.09304(13) 0.0328(12) Uani 1 1 d . . . C2 C 1.1124(4) 0.1861(2) 0.08711(12) 0.0300(10) Uani 1 1 d . . . B3 B 1.1292(5) 0.2784(3) 0.11422(16) 0.0364(14) Uani 1 1 d . . . H3 H 1.1472 0.2797 0.1455 0.044 Uiso 1 1 calc R . . B4 B 1.0250(5) 0.3539(3) 0.09157(16) 0.0390(15) Uani 1 1 d . . . H4 H 0.9744 0.4046 0.1081 0.047 Uiso 1 1 calc R . . B5 B 0.9473(5) 0.3044(3) 0.05162(15) 0.0416(15) Uani 1 1 d . . . H5 H 0.8472 0.3227 0.0423 0.050 Uiso 1 1 calc R . . B6 B 1.0029(5) 0.1969(3) 0.04908(15) 0.0384(14) Uani 1 1 d . . . H6 H 0.9391 0.1448 0.0382 0.046 Uiso 1 1 calc R . . B7 B 1.2522(5) 0.2455(3) 0.08151(16) 0.0383(15) Uani 1 1 d . . . H7 H 1.3505 0.2248 0.0914 0.046 Uiso 1 1 calc R . . B8 B 1.1985(5) 0.3543(4) 0.08342(16) 0.0441(16) Uani 1 1 d . . . H8 H 1.2628 0.4060 0.0944 0.053 Uiso 1 1 calc R . . B9 B 1.0869(5) 0.3718(3) 0.04464(15) 0.0457(15) Uani 1 1 d . . . H9 H 1.0785 0.4350 0.0304 0.055 Uiso 1 1 calc R . . B10 B 1.0724(6) 0.2741(4) 0.01865(16) 0.0489(17) Uani 1 1 d . . . H10 H 1.0544 0.2737 -0.0126 0.059 Uiso 1 1 calc R . . B11 B 1.1736(5) 0.1961(4) 0.04105(15) 0.0415(15) Uani 1 1 d . . . H11 H 1.2211 0.1437 0.0248 0.050 Uiso 1 1 calc R . . B12 B 1.2278(6) 0.3045(4) 0.03803(15) 0.0453(16) Uani 1 1 d . . . H12 H 1.3111 0.3236 0.0195 0.054 Uiso 1 1 calc R . . C3 C 1.2346(5) 0.1500(3) 0.18874(15) 0.0530(16) Uani 1 1 d . . . C4 C 1.1793(6) -0.0177(4) 0.18544(17) 0.0657(17) Uani 1 1 d . . . C5 C 0.9880(5) 0.0904(3) 0.21621(15) 0.0462(14) Uani 1 1 d . . . C6 C 0.7564(5) 0.1901(3) 0.20657(14) 0.0496(14) Uani 1 1 d . . . C7 C 0.9860(5) 0.2666(3) 0.20909(15) 0.0464(14) Uani 1 1 d . . . O1 O 1.3219(3) 0.1924(2) 0.19767(11) 0.0742(12) Uani 1 1 d . . . O2 O 1.2287(5) -0.0791(3) 0.19580(13) 0.1138(18) Uani 1 1 d . . . O3 O 0.9706(3) 0.0578(2) 0.24678(10) 0.0625(11) Uani 1 1 d . . . O4 O 0.6571(4) 0.2002(3) 0.22161(11) 0.0837(13) Uani 1 1 d . . . O5 O 1.0286(4) 0.3254(2) 0.22465(11) 0.0753(13) Uani 1 1 d . . . C8 C 0.8688(4) -0.0653(3) 0.13288(16) 0.0443(13) Uani 1 1 d . . . C9 C 0.7734(5) -0.0249(3) 0.15583(15) 0.0439(14) Uani 1 1 d . . . C10 C 0.6984(4) 0.0306(3) 0.13238(16) 0.0448(13) Uani 1 1 d . . . C11 C 0.7457(5) 0.0223(3) 0.09359(16) 0.0505(15) Uani 1 1 d . . . C12 C 0.8505(5) -0.0379(3) 0.09446(16) 0.0511(15) Uani 1 1 d . . . C13 C 0.9584(5) -0.1384(3) 0.14438(17) 0.085(2) Uani 1 1 d . . . H13A H 0.9117 -0.1921 0.1419 0.128 Uiso 1 1 calc R . . H13B H 0.9860 -0.1308 0.1707 0.128 Uiso 1 1 calc R . . H13C H 1.0345 -0.1391 0.1279 0.128 Uiso 1 1 calc R . . C14 C 0.7453(5) -0.0469(3) 0.19734(15) 0.0770(19) Uani 1 1 d . . . H14A H 0.6836 -0.0939 0.1985 0.115 Uiso 1 1 calc R . . H14B H 0.7086 0.0025 0.2101 0.115 Uiso 1 1 calc R . . H14C H 0.8260 -0.0635 0.2099 0.115 Uiso 1 1 calc R . . C15 C 0.5767(4) 0.0792(3) 0.14403(16) 0.0750(18) Uani 1 1 d . . . H15A H 0.5012 0.0420 0.1420 0.113 Uiso 1 1 calc R . . H15B H 0.5652 0.1280 0.1273 0.113 Uiso 1 1 calc R . . H15C H 0.5858 0.0986 0.1702 0.113 Uiso 1 1 calc R . . C16 C 0.6823(5) 0.0634(4) 0.05921(16) 0.096(2) Uani 1 1 d . . . H16A H 0.6164 0.0253 0.0489 0.144 Uiso 1 1 calc R . . H16B H 0.7482 0.0744 0.0399 0.144 Uiso 1 1 calc R . . H16C H 0.6417 0.1167 0.0668 0.144 Uiso 1 1 calc R . . C17 C 0.9243(5) -0.0707(3) 0.05956(15) 0.087(2) Uani 1 1 d . . . H17A H 0.8801 -0.1206 0.0494 0.131 Uiso 1 1 calc R . . H17B H 1.0128 -0.0859 0.0669 0.131 Uiso 1 1 calc R . . H17C H 0.9270 -0.0264 0.0402 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0358(4) 0.0329(4) 0.0350(4) -0.0004(3) 0.0003(3) -0.0030(3) Co2 0.0428(4) 0.0416(4) 0.0389(4) 0.0014(3) -0.0059(4) 0.0061(4) Co3 0.0423(4) 0.0387(4) 0.0315(4) -0.0002(3) 0.0013(4) 0.0015(3) S1 0.0310(7) 0.0366(7) 0.0361(8) 0.0015(6) 0.0025(6) 0.0007(5) S2 0.0366(7) 0.0318(7) 0.0387(7) -0.0026(6) 0.0007(6) 0.0043(6) C1 0.037(3) 0.035(3) 0.027(3) 0.001(2) -0.001(2) 0.005(2) C2 0.026(3) 0.031(3) 0.034(3) -0.004(2) 0.000(2) 0.003(2) B3 0.037(4) 0.034(3) 0.039(4) -0.005(3) -0.004(3) -0.004(2) B4 0.055(4) 0.020(3) 0.042(4) -0.003(3) 0.008(3) 0.005(3) B5 0.043(4) 0.045(4) 0.037(4) 0.014(3) -0.004(3) 0.000(3) B6 0.041(4) 0.049(4) 0.026(3) -0.003(3) -0.004(3) 0.000(3) B7 0.028(3) 0.048(4) 0.039(4) -0.004(3) 0.006(3) -0.005(3) B8 0.047(4) 0.040(4) 0.046(4) 0.005(3) 0.002(3) -0.009(3) B9 0.045(4) 0.048(4) 0.044(4) 0.014(3) 0.009(3) 0.002(3) B10 0.059(4) 0.053(4) 0.035(4) 0.009(3) 0.002(3) -0.006(3) B11 0.046(4) 0.046(4) 0.033(4) -0.009(3) 0.012(3) 0.002(3) B12 0.045(4) 0.054(4) 0.036(4) 0.007(3) 0.011(3) -0.008(3) C3 0.048(4) 0.070(4) 0.041(4) 0.007(3) -0.003(3) 0.014(3) C4 0.077(4) 0.063(4) 0.057(4) -0.009(3) -0.014(4) 0.019(3) C5 0.056(3) 0.038(3) 0.045(4) -0.005(3) -0.002(3) -0.008(3) C6 0.063(4) 0.047(4) 0.038(3) 0.000(3) -0.004(3) 0.003(3) C7 0.043(3) 0.047(4) 0.050(4) 0.006(3) 0.000(3) 0.011(3) O1 0.057(3) 0.087(3) 0.079(3) 0.004(2) -0.017(2) -0.011(2) O2 0.148(4) 0.070(3) 0.123(4) 0.002(3) -0.050(3) 0.049(3) O3 0.082(3) 0.064(3) 0.042(2) 0.013(2) 0.003(2) 0.007(2) O4 0.065(3) 0.117(4) 0.070(3) -0.009(3) 0.024(2) 0.001(3) O5 0.083(3) 0.059(3) 0.084(3) -0.023(2) -0.020(2) -0.008(2) C8 0.038(3) 0.033(3) 0.061(4) -0.002(3) 0.004(3) -0.002(2) C9 0.047(4) 0.035(3) 0.050(4) 0.001(3) 0.005(3) -0.016(3) C10 0.029(3) 0.039(3) 0.066(4) -0.009(3) -0.003(3) -0.010(2) C11 0.050(4) 0.046(4) 0.056(4) 0.004(3) -0.018(3) -0.026(3) C12 0.045(3) 0.051(4) 0.057(4) -0.015(3) 0.002(3) -0.018(3) C13 0.070(5) 0.039(3) 0.147(6) 0.002(4) -0.007(4) -0.004(3) C14 0.094(5) 0.070(4) 0.066(5) 0.012(4) 0.015(4) -0.036(3) C15 0.040(3) 0.062(4) 0.124(5) -0.027(4) -0.003(3) -0.005(3) C16 0.095(5) 0.105(5) 0.087(5) 0.029(4) -0.050(4) -0.042(4) C17 0.087(5) 0.095(5) 0.079(5) -0.050(4) 0.027(4) -0.029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C10 2.094(4) . ? Co1 C8 2.100(4) . ? Co1 C11 2.107(5) . ? Co1 C12 2.112(5) . ? Co1 C9 2.115(5) . ? Co1 S1 2.2048(13) . ? Co1 S2 2.2129(13) . ? Co1 Co3 2.5501(10) . ? Co1 Co2 2.5881(10) . ? Co2 C3 1.770(6) . ? Co2 C4 1.790(6) . ? Co2 C5 1.885(5) . ? Co2 S2 2.2267(14) . ? Co2 Co3 2.4436(10) . ? Co3 C7 1.773(5) . ? Co3 C6 1.776(5) . ? Co3 C5 1.895(5) . ? Co3 S1 2.2579(14) . ? S1 C1 1.795(4) . ? S2 C2 1.810(4) . ? C1 C2 1.647(5) . ? C1 B4 1.694(6) . ? C1 B5 1.715(6) . ? C1 B3 1.724(6) . ? C1 B6 1.733(6) . ? C2 B7 1.699(6) . ? C2 B11 1.719(6) . ? C2 B3 1.720(6) . ? C2 B6 1.731(6) . ? B3 B8 1.737(7) . ? B3 B4 1.760(7) . ? B3 B7 1.760(7) . ? B4 B9 1.765(7) . ? B4 B5 1.768(7) . ? B4 B8 1.779(7) . ? B5 B6 1.762(7) . ? B5 B10 1.769(7) . ? B5 B9 1.774(7) . ? B6 B10 1.745(7) . ? B6 B11 1.750(7) . ? B7 B8 1.773(7) . ? B7 B12 1.781(7) . ? B7 B11 1.785(7) . ? B8 B9 1.777(7) . ? B8 B12 1.777(7) . ? B9 B10 1.768(7) . ? B9 B12 1.781(7) . ? B10 B11 1.765(7) . ? B10 B12 1.774(8) . ? B11 B12 1.771(7) . ? C3 O1 1.144(5) . ? C4 O2 1.133(5) . ? C5 O3 1.187(5) . ? C6 O4 1.143(5) . ? C7 O5 1.143(5) . ? C8 C9 1.399(6) . ? C8 C12 1.410(6) . ? C8 C13 1.505(6) . ? C9 C10 1.406(6) . ? C9 C14 1.506(6) . ? C10 C11 1.433(6) . ? C10 C15 1.500(6) . ? C11 C12 1.413(6) . ? C11 C16 1.496(6) . ? C12 C17 1.510(6) . ? 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 C10 Co1 C8 65.76(17) . . ? C10 Co1 C11 39.87(18) . . ? C8 Co1 C11 66.04(19) . . ? C10 Co1 C12 65.81(19) . . ? C8 Co1 C12 39.12(17) . . ? C11 Co1 C12 39.15(17) . . ? C10 Co1 C9 39.02(17) . . ? C8 Co1 C9 38.78(16) . . ? C11 Co1 C9 65.9(2) . . ? C12 Co1 C9 65.11(19) . . ? C10 Co1 S1 95.02(13) . . ? C8 Co1 S1 160.48(13) . . ? C11 Co1 S1 97.30(15) . . ? C12 Co1 S1 131.27(17) . . ? C9 Co1 S1 126.41(15) . . ? C10 Co1 S2 160.16(15) . . ? C8 Co1 S2 103.04(13) . . ? C11 Co1 S2 121.37(17) . . ? C12 Co1 S2 95.01(14) . . ? C9 Co1 S2 138.66(15) . . ? S1 Co1 S2 94.29(5) . . ? C10 Co1 Co3 102.86(14) . . ? C8 Co1 Co3 128.96(15) . . ? C11 Co1 Co3 136.17(17) . . ? C12 Co1 Co3 165.41(15) . . ? C9 Co1 Co3 100.30(14) . . ? S1 Co1 Co3 56.13(4) . . ? S2 Co1 Co3 96.88(4) . . ? C10 Co1 Co2 140.64(16) . . ? C8 Co1 Co2 99.44(13) . . ? C11 Co1 Co2 164.54(15) . . ? C12 Co1 Co2 125.85(16) . . ? C9 Co1 Co2 106.61(14) . . ? S1 Co1 Co2 97.91(4) . . ? S2 Co1 Co2 54.59(4) . . ? Co3 Co1 Co2 56.79(2) . . ? C3 Co2 C4 96.8(2) . . ? C3 Co2 C5 101.3(2) . . ? C4 Co2 C5 98.0(2) . . ? C3 Co2 S2 107.85(17) . . ? C4 Co2 S2 102.49(19) . . ? C5 Co2 S2 141.71(15) . . ? C3 Co2 Co3 100.88(16) . . ? C4 Co2 Co3 145.74(19) . . ? C5 Co2 Co3 49.89(15) . . ? S2 Co2 Co3 99.64(4) . . ? C3 Co2 Co1 146.20(17) . . ? C4 Co2 Co1 114.12(18) . . ? C5 Co2 Co1 88.04(15) . . ? S2 Co2 Co1 54.09(4) . . ? Co3 Co2 Co1 60.82(3) . . ? C7 Co3 C6 94.8(2) . . ? C7 Co3 C5 96.8(2) . . ? C6 Co3 C5 100.8(2) . . ? C7 Co3 S1 113.75(17) . . ? C6 Co3 S1 97.69(16) . . ? C5 Co3 S1 142.61(15) . . ? C7 Co3 Co2 102.77(15) . . ? C6 Co3 Co2 146.64(16) . . ? C5 Co3 Co2 49.53(15) . . ? S1 Co3 Co2 100.76(4) . . ? C7 Co3 Co1 153.96(16) . . ? C6 Co3 Co1 109.10(16) . . ? C5 Co3 Co1 88.96(15) . . ? S1 Co3 Co1 54.18(4) . . ? Co2 Co3 Co1 62.39(3) . . ? C1 S1 Co1 105.01(14) . . ? C1 S1 Co3 115.22(15) . . ? Co1 S1 Co3 69.69(4) . . ? C2 S2 Co1 105.26(13) . . ? C2 S2 Co2 114.31(13) . . ? Co1 S2 Co2 71.32(4) . . ? C2 C1 B4 110.9(3) . . ? C2 C1 B5 110.9(3) . . ? B4 C1 B5 62.5(3) . . ? C2 C1 B3 61.3(3) . . ? B4 C1 B3 62.0(3) . . ? B5 C1 B3 113.4(4) . . ? C2 C1 B6 61.5(3) . . ? B4 C1 B6 112.8(4) . . ? B5 C1 B6 61.5(3) . . ? B3 C1 B6 113.2(3) . . ? C2 C1 S1 116.6(3) . . ? B4 C1 S1 123.1(3) . . ? B5 C1 S1 121.5(3) . . ? B3 C1 S1 118.3(3) . . ? B6 C1 S1 116.2(3) . . ? C1 C2 B7 111.4(3) . . ? C1 C2 B11 110.6(3) . . ? B7 C2 B11 63.0(3) . . ? C1 C2 B3 61.6(2) . . ? B7 C2 B3 62.0(3) . . ? B11 C2 B3 113.4(3) . . ? C1 C2 B6 61.7(3) . . ? B7 C2 B6 113.2(4) . . ? B11 C2 B6 61.0(3) . . ? B3 C2 B6 113.5(3) . . ? C1 C2 S2 115.6(3) . . ? B7 C2 S2 125.6(3) . . ? B11 C2 S2 119.7(3) . . ? B3 C2 S2 121.6(3) . . ? B6 C2 S2 112.1(3) . . ? C2 B3 C1 57.1(2) . . ? C2 B3 B8 105.5(4) . . ? C1 B3 B8 105.7(4) . . ? C2 B3 B4 104.5(4) . . ? C1 B3 B4 58.2(3) . . ? B8 B3 B4 61.1(3) . . ? C2 B3 B7 58.5(3) . . ? C1 B3 B7 105.0(4) . . ? B8 B3 B7 60.9(3) . . ? B4 B3 B7 109.2(4) . . ? C1 B4 B3 59.9(3) . . ? C1 B4 B9 105.7(4) . . ? B3 B4 B9 107.7(4) . . ? C1 B4 B5 59.3(3) . . ? B3 B4 B5 109.1(4) . . ? B9 B4 B5 60.3(3) . . ? C1 B4 B8 105.2(4) . . ? B3 B4 B8 58.8(3) . . ? B9 B4 B8 60.2(3) . . ? B5 B4 B8 108.4(4) . . ? C1 B5 B6 59.8(3) . . ? C1 B5 B10 105.1(4) . . ? B6 B5 B10 59.2(3) . . ? C1 B5 B4 58.2(3) . . ? B6 B5 B4 107.9(4) . . ? B10 B5 B4 107.6(4) . . ? C1 B5 B9 104.4(4) . . ? B6 B5 B9 107.2(4) . . ? B10 B5 B9 59.9(3) . . ? B4 B5 B9 59.8(3) . . ? C2 B6 C1 56.8(2) . . ? C2 B6 B10 105.6(4) . . ? C1 B6 B10 105.3(4) . . ? C2 B6 B11 59.2(3) . . ? C1 B6 B11 105.2(4) . . ? B10 B6 B11 60.7(3) . . ? C2 B6 B5 104.9(4) . . ? C1 B6 B5 58.8(3) . . ? B10 B6 B5 60.6(3) . . ? B11 B6 B5 109.2(4) . . ? C2 B7 B3 59.6(3) . . ? C2 B7 B8 104.8(3) . . ? B3 B7 B8 58.9(3) . . ? C2 B7 B12 105.0(4) . . ? B3 B7 B12 107.3(4) . . ? B8 B7 B12 60.0(3) . . ? C2 B7 B11 59.1(3) . . ? B3 B7 B11 108.3(4) . . ? B8 B7 B11 107.5(4) . . ? B12 B7 B11 59.6(3) . . ? B3 B8 B7 60.2(3) . . ? B3 B8 B9 108.2(4) . . ? B7 B8 B9 108.2(4) . . ? B3 B8 B12 108.5(4) . . ? B7 B8 B12 60.2(3) . . ? B9 B8 B12 60.2(3) . . ? B3 B8 B4 60.1(3) . . ? B7 B8 B4 107.8(4) . . ? B9 B8 B4 59.5(3) . . ? B12 B8 B4 107.7(4) . . ? B4 B9 B10 107.8(4) . . ? B4 B9 B5 59.9(3) . . ? B10 B9 B5 59.9(3) . . ? B4 B9 B8 60.3(3) . . ? B10 B9 B8 107.9(4) . . ? B5 B9 B8 108.3(4) . . ? B4 B9 B12 108.1(4) . . ? B10 B9 B12 60.0(3) . . ? B5 B9 B12 108.1(4) . . ? B8 B9 B12 59.9(3) . . ? B6 B10 B11 59.8(3) . . ? B6 B10 B9 108.3(4) . . ? B11 B10 B9 108.3(4) . . ? B6 B10 B5 60.2(3) . . ? B11 B10 B5 108.2(4) . . ? B9 B10 B5 60.2(3) . . ? B6 B10 B12 108.1(4) . . ? B11 B10 B12 60.1(3) . . ? B9 B10 B12 60.4(3) . . ? B5 B10 B12 108.6(4) . . ? C2 B11 B6 59.8(3) . . ? C2 B11 B10 105.1(4) . . ? B6 B11 B10 59.5(3) . . ? C2 B11 B12 104.6(4) . . ? B6 B11 B12 108.0(4) . . ? B10 B11 B12 60.2(3) . . ? C2 B11 B7 58.0(3) . . ? B6 B11 B7 108.2(4) . . ? B10 B11 B7 108.1(4) . . ? B12 B11 B7 60.1(3) . . ? B11 B12 B10 59.7(3) . . ? B11 B12 B8 107.9(4) . . ? B10 B12 B8 107.6(4) . . ? B11 B12 B9 107.4(4) . . ? B10 B12 B9 59.6(3) . . ? B8 B12 B9 59.9(3) . . ? B11 B12 B7 60.3(3) . . ? B10 B12 B7 107.9(4) . . ? B8 B12 B7 59.8(3) . . ? B9 B12 B7 107.6(4) . . ? O1 C3 Co2 178.0(5) . . ? O2 C4 Co2 174.7(6) . . ? O3 C5 Co2 140.0(4) . . ? O3 C5 Co3 139.4(4) . . ? Co2 C5 Co3 80.6(2) . . ? O4 C6 Co3 177.4(5) . . ? O5 C7 Co3 177.7(5) . . ? C9 C8 C12 108.1(4) . . ? C9 C8 C13 127.0(5) . . ? C12 C8 C13 123.8(5) . . ? C9 C8 Co1 71.2(3) . . ? C12 C8 Co1 70.9(3) . . ? C13 C8 Co1 132.7(3) . . ? C8 C9 C10 108.5(5) . . ? C8 C9 C14 124.9(5) . . ? C10 C9 C14 126.1(5) . . ? C8 C9 Co1 70.0(3) . . ? C10 C9 Co1 69.7(3) . . ? C14 C9 Co1 132.3(3) . . ? C9 C10 C11 107.9(5) . . ? C9 C10 C15 126.5(5) . . ? C11 C10 C15 124.9(5) . . ? C9 C10 Co1 71.3(3) . . ? C11 C10 Co1 70.5(3) . . ? C15 C10 Co1 131.0(3) . . ? C12 C11 C10 106.8(5) . . ? C12 C11 C16 128.3(6) . . ? C10 C11 C16 124.5(5) . . ? C12 C11 Co1 70.6(3) . . ? C10 C11 Co1 69.6(3) . . ? C16 C11 Co1 129.9(3) . . ? C8 C12 C11 108.5(5) . . ? C8 C12 C17 126.1(5) . . ? C11 C12 C17 125.2(6) . . ? C8 C12 Co1 70.0(3) . . ? C11 C12 Co1 70.2(3) . . ? C17 C12 Co1 128.3(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.398 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.065 # Attachment '5a_tri_CpSMo_f50915c.cif' data_f50915c _database_code_depnum_ccdc_archive 'CCDC 621983' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H38 B20 Co2 Mo O2 S4' _chemical_formula_weight 904.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.789(4) _cell_length_b 11.507(4) _cell_length_c 14.342(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.995(5) _cell_angle_gamma 90.00 _cell_volume 1931.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 721 _cell_measurement_theta_min 2.276 _cell_measurement_theta_max 22.921 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8161 _exptl_absorpt_correction_T_max 0.9328 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.46 _diffrn_reflns_number 9394 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.1041 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.10 _reflns_number_total 4161 _reflns_number_gt 2249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^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 4161 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 0.786 _refine_ls_restrained_S_all 0.786 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 Mo1 Mo 0.0000 0.69415(4) 0.7500 0.04395(16) Uani 1 2 d S . . Co1 Co 0.15455(5) 0.75995(5) 0.88732(4) 0.04720(18) Uani 1 1 d . . . S1 S 0.05613(8) 0.59501(9) 0.90575(7) 0.0444(3) Uani 1 1 d . . . S2 S 0.21440(8) 0.66954(9) 0.76700(7) 0.0443(3) Uani 1 1 d . . . B3 B 0.1489(4) 0.4221(4) 0.7730(3) 0.0444(12) Uani 1 1 d . . . H3A H 0.0783 0.4364 0.7166 0.053 Uiso 1 1 calc R . . B4 B 0.1317(4) 0.3362(4) 0.8730(3) 0.0491(13) Uani 1 1 d . . . H4A H 0.0498 0.2946 0.8823 0.059 Uiso 1 1 calc R . . B5 B 0.2227(4) 0.3929(4) 0.9711(4) 0.0518(13) Uani 1 1 d . . . H5A H 0.1992 0.3875 1.0429 0.062 Uiso 1 1 calc R . . B6 B 0.2966(4) 0.5132(4) 0.9331(3) 0.0474(13) Uani 1 1 d . . . H6A H 0.3215 0.5863 0.9805 0.057 Uiso 1 1 calc R . . B7 B 0.2915(4) 0.4125(4) 0.7483(4) 0.0532(14) Uani 1 1 d . . . H7A H 0.3139 0.4207 0.6764 0.064 Uiso 1 1 calc R . . B8 B 0.2192(4) 0.2900(4) 0.7876(4) 0.0542(14) Uani 1 1 d . . . H8A H 0.1944 0.2160 0.7410 0.065 Uiso 1 1 calc R . . B9 B 0.2657(4) 0.2700(4) 0.9076(4) 0.0589(15) Uani 1 1 d . . . H9 H 0.2716 0.1828 0.9392 0.071 Uiso 1 1 calc R . . B10 B 0.3674(4) 0.3805(5) 0.9444(4) 0.0599(15) Uani 1 1 d . . . H10 H 0.4393 0.3655 0.9995 0.072 Uiso 1 1 calc R . . B11 B 0.3820(4) 0.4689(5) 0.8461(3) 0.0543(14) Uani 1 1 d . . . H11 H 0.4622 0.5139 0.8367 0.065 Uiso 1 1 calc R . . B12 B 0.3636(4) 0.3181(5) 0.8312(4) 0.0609(15) Uani 1 1 d . . . H12 H 0.4334 0.2623 0.8129 0.073 Uiso 1 1 calc R . . C9 C 0.4826(13) 1.0210(6) 0.7430(10) 0.138(8) Uani 0.50 1 d PG . . C10 C 0.5518(16) 1.0303(7) 0.8284(11) 0.138(7) Uani 0.50 1 d PG . . C11 C 0.5966(13) 0.9308(12) 0.8740(8) 0.101(8) Uani 0.50 1 d PG . . C12 C 0.5722(12) 0.8221(9) 0.8343(8) 0.098(6) Uani 0.50 1 d PG . . C13 C 0.5010(11) 0.8129(6) 0.7496(9) 0.087(3) Uani 1 2 d SG . . C14 C 0.4581(8) 0.9123(9) 0.7033(7) 0.091(5) Uani 0.50 1 d PG . . C1 C 0.1580(3) 0.4821(3) 0.8848(3) 0.0397(10) Uani 1 1 d . . . C2 C 0.2474(3) 0.5251(3) 0.8143(3) 0.0417(10) Uani 1 1 d . . . C3 C -0.0503(4) 0.8205(5) 0.8283(4) 0.0816(17) Uani 1 1 d . . . C4 C 0.1324(5) 0.8717(5) 0.9944(4) 0.0783(16) Uani 1 1 d . . . H4 H 0.0646 0.8773 1.0275 0.094 Uiso 1 1 calc R . . C5 C 0.2290(5) 0.8024(4) 1.0204(3) 0.0758(15) Uani 1 1 d . . . H5 H 0.2393 0.7495 1.0743 0.091 Uiso 1 1 calc R . . C6 C 0.3072(4) 0.8208(4) 0.9572(4) 0.0655(13) Uani 1 1 d . . . H6 H 0.3823 0.7839 0.9585 0.079 Uiso 1 1 calc R . . C7 C 0.2598(4) 0.9034(4) 0.8916(4) 0.0686(14) Uani 1 1 d . . . H7 H 0.2963 0.9339 0.8388 0.082 Uiso 1 1 calc R . . C8 C 0.1534(4) 0.9363(4) 0.9149(4) 0.0716(15) Uani 1 1 d . . . H8 H 0.1020 0.9939 0.8819 0.086 Uiso 1 1 calc R . . C15 C 0.381(3) 0.906(3) 0.6163(18) 0.190(14) Uani 0.50 1 d P . . O1 O -0.0967(3) 0.8950(4) 0.8608(3) 0.1307(19) 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 Mo1 0.0432(3) 0.0362(3) 0.0538(3) 0.000 0.0117(2) 0.000 Co1 0.0529(4) 0.0407(4) 0.0507(4) -0.0107(3) 0.0170(3) -0.0071(3) S1 0.0457(6) 0.0425(6) 0.0486(7) -0.0057(5) 0.0200(5) -0.0015(5) S2 0.0447(6) 0.0460(7) 0.0450(6) -0.0017(5) 0.0165(5) -0.0038(5) B3 0.048(3) 0.043(3) 0.041(3) -0.011(2) 0.003(2) -0.004(2) B4 0.056(3) 0.040(3) 0.051(3) -0.004(2) 0.006(2) -0.003(2) B5 0.059(3) 0.047(3) 0.049(3) 0.004(3) 0.007(3) 0.001(3) B6 0.044(3) 0.052(3) 0.045(3) -0.004(2) 0.002(2) -0.007(2) B7 0.050(3) 0.059(4) 0.053(3) -0.014(3) 0.018(2) 0.010(3) B8 0.061(3) 0.040(3) 0.060(3) -0.009(3) 0.002(3) 0.007(3) B9 0.074(4) 0.042(3) 0.059(3) 0.001(3) 0.002(3) 0.006(3) B10 0.052(3) 0.067(4) 0.060(4) 0.002(3) 0.002(3) 0.007(3) B11 0.039(3) 0.061(4) 0.064(4) -0.005(3) 0.013(3) 0.004(2) B12 0.054(3) 0.059(4) 0.071(4) -0.005(3) 0.010(3) 0.016(3) C9 0.21(2) 0.050(8) 0.179(18) -0.061(16) 0.120(16) -0.052(15) C10 0.123(14) 0.150(19) 0.147(19) -0.005(13) 0.042(15) -0.021(12) C11 0.085(13) 0.074(11) 0.14(2) -0.020(11) -0.015(12) -0.011(10) C12 0.083(12) 0.104(12) 0.118(14) 0.055(10) 0.060(9) 0.049(9) C13 0.059(5) 0.108(8) 0.099(7) 0.000 0.035(5) 0.000 C14 0.036(6) 0.169(16) 0.069(8) 0.041(11) 0.013(5) 0.045(9) C1 0.039(2) 0.040(3) 0.041(2) -0.0006(19) 0.0136(18) 0.0012(18) C2 0.036(2) 0.050(3) 0.041(2) -0.002(2) 0.0123(18) -0.0011(19) C3 0.057(3) 0.062(4) 0.122(5) -0.028(3) -0.004(3) 0.005(3) C4 0.099(4) 0.058(4) 0.085(4) -0.036(3) 0.038(3) -0.008(3) C5 0.123(5) 0.053(3) 0.049(3) -0.018(3) 0.005(3) -0.014(3) C6 0.063(3) 0.057(3) 0.076(4) -0.021(3) 0.006(3) -0.014(3) C7 0.083(4) 0.049(3) 0.075(4) -0.015(3) 0.015(3) -0.028(3) C8 0.085(4) 0.044(3) 0.086(4) -0.018(3) 0.010(3) -0.004(3) C15 0.11(2) 0.36(4) 0.10(2) -0.05(2) 0.023(13) -0.04(2) O1 0.077(3) 0.098(3) 0.214(5) -0.091(3) 0.007(3) 0.019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C3 1.972(5) . ? Mo1 C3 1.972(6) 2_556 ? Mo1 S1 2.5237(13) 2_556 ? Mo1 S1 2.5237(13) . ? Mo1 S2 2.5255(13) . ? Mo1 S2 2.5255(13) 2_556 ? Mo1 Co1 2.6264(8) . ? Mo1 Co1 2.6264(8) 2_556 ? Co1 C4 2.044(5) . ? Co1 C5 2.060(4) . ? Co1 C7 2.061(4) . ? Co1 C8 2.067(5) . ? Co1 C6 2.072(4) . ? Co1 S2 2.2034(12) . ? Co1 S1 2.2568(13) . ? S1 C1 1.819(4) . ? S2 C2 1.819(4) . ? B3 C2 1.714(6) . ? B3 B8 1.731(6) . ? B3 C1 1.738(6) . ? B3 B7 1.763(6) . ? B3 B4 1.774(7) . ? B4 C1 1.712(6) . ? B4 B9 1.769(7) . ? B4 B8 1.776(7) . ? B4 B5 1.786(6) . ? B5 C1 1.714(6) . ? B5 B6 1.758(7) . ? B5 B9 1.788(7) . ? B5 B10 1.799(7) . ? B6 C1 1.733(5) . ? B6 B10 1.737(7) . ? B6 C2 1.737(6) . ? B6 B11 1.771(7) . ? B7 C2 1.721(6) . ? B7 B12 1.753(7) . ? B7 B8 1.773(7) . ? B7 B11 1.778(7) . ? B8 B9 1.757(7) . ? B8 B12 1.771(7) . ? B9 B12 1.774(8) . ? B9 B10 1.783(7) . ? B10 B11 1.764(7) . ? B10 B12 1.770(7) . ? B11 C2 1.723(6) . ? B11 B12 1.759(7) . ? C9 C9 0.43(3) 2_656 ? C9 C10 1.06(3) 2_656 ? C9 C10 1.3900 . ? C9 C14 1.3900 . ? C9 C14 1.585(11) 2_656 ? C10 C9 1.06(3) 2_656 ? C10 C11 1.3900 . ? C10 C14 1.432(6) 2_656 ? C10 C15 1.78(4) 2_656 ? C11 C15 0.40(4) 2_656 ? C11 C14 1.232(17) 2_656 ? C11 C12 1.3900 . ? C12 C14 1.203(9) 2_656 ? C12 C15 1.28(3) 2_656 ? C12 C13 1.3933 . ? C13 C14 1.385(10) 2_656 ? C13 C14 1.3871 . ? C13 C12 1.40(2) 2_656 ? C14 C12 1.203(12) 2_656 ? C14 C11 1.232(18) 2_656 ? C14 C10 1.432(9) 2_656 ? C14 C15 1.45(2) . ? C14 C14 1.564(18) 2_656 ? C14 C9 1.585(15) 2_656 ? C1 C2 1.625(5) . ? C3 O1 1.146(5) . ? C4 C5 1.403(6) . ? C4 C8 1.408(6) . ? C5 C6 1.386(6) . ? C6 C7 1.405(6) . ? C7 C8 1.390(6) . ? C15 C11 0.40(3) 2_656 ? C15 C12 1.28(3) 2_656 ? C15 C10 1.78(3) 2_656 ? 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 C3 Mo1 C3 85.0(3) . 2_556 ? C3 Mo1 S1 140.59(14) . 2_556 ? C3 Mo1 S1 83.90(16) 2_556 2_556 ? C3 Mo1 S1 83.90(16) . . ? C3 Mo1 S1 140.59(14) 2_556 . ? S1 Mo1 S1 126.25(6) 2_556 . ? C3 Mo1 S2 113.25(13) . . ? C3 Mo1 S2 76.74(13) 2_556 . ? S1 Mo1 S2 100.73(3) 2_556 . ? S1 Mo1 S2 73.29(3) . . ? C3 Mo1 S2 76.74(13) . 2_556 ? C3 Mo1 S2 113.25(13) 2_556 2_556 ? S1 Mo1 S2 73.29(3) 2_556 2_556 ? S1 Mo1 S2 100.73(3) . 2_556 ? S2 Mo1 S2 167.12(5) . 2_556 ? C3 Mo1 Co1 65.78(13) . . ? C3 Mo1 Co1 89.15(15) 2_556 . ? S1 Mo1 Co1 151.31(3) 2_556 . ? S1 Mo1 Co1 51.93(3) . . ? S2 Mo1 Co1 50.59(3) . . ? S2 Mo1 Co1 134.38(3) 2_556 . ? C3 Mo1 Co1 89.15(15) . 2_556 ? C3 Mo1 Co1 65.78(13) 2_556 2_556 ? S1 Mo1 Co1 51.93(3) 2_556 2_556 ? S1 Mo1 Co1 151.31(3) . 2_556 ? S2 Mo1 Co1 134.38(3) . 2_556 ? S2 Mo1 Co1 50.59(3) 2_556 2_556 ? Co1 Mo1 Co1 146.49(4) . 2_556 ? C4 Co1 C5 39.97(18) . . ? C4 Co1 C7 66.8(2) . . ? C5 Co1 C7 66.2(2) . . ? C4 Co1 C8 40.04(18) . . ? C5 Co1 C8 66.6(2) . . ? C7 Co1 C8 39.34(17) . . ? C4 Co1 C6 66.9(2) . . ? C5 Co1 C6 39.21(18) . . ? C7 Co1 C6 39.73(16) . . ? C8 Co1 C6 66.51(19) . . ? C4 Co1 S2 165.45(16) . . ? C5 Co1 S2 134.17(17) . . ? C7 Co1 S2 98.76(15) . . ? C8 Co1 S2 128.58(17) . . ? C6 Co1 S2 101.32(14) . . ? C4 Co1 S1 109.05(16) . . ? C5 Co1 S1 104.93(16) . . ? C7 Co1 S1 170.45(15) . . ? C8 Co1 S1 141.93(17) . . ? C6 Co1 S1 131.02(16) . . ? S2 Co1 S1 85.00(4) . . ? C4 Co1 Mo1 127.18(16) . . ? C5 Co1 Mo1 160.29(17) . . ? C7 Co1 Mo1 127.81(15) . . ? C8 Co1 Mo1 113.96(14) . . ? C6 Co1 Mo1 160.45(15) . . ? S2 Co1 Mo1 62.33(4) . . ? S1 Co1 Mo1 61.69(3) . . ? C1 S1 Co1 102.83(13) . . ? C1 S1 Mo1 106.50(13) . . ? Co1 S1 Mo1 66.38(3) . . ? C2 S2 Co1 102.36(13) . . ? C2 S2 Mo1 107.73(12) . . ? Co1 S2 Mo1 67.07(3) . . ? C2 B3 B8 105.7(3) . . ? C2 B3 C1 56.2(2) . . ? B8 B3 C1 105.2(3) . . ? C2 B3 B7 59.3(2) . . ? B8 B3 B7 61.0(3) . . ? C1 B3 B7 104.9(3) . . ? C2 B3 B4 104.2(3) . . ? B8 B3 B4 60.9(3) . . ? C1 B3 B4 58.4(2) . . ? B7 B3 B4 109.4(4) . . ? C1 B4 B9 104.5(3) . . ? C1 B4 B3 59.8(2) . . ? B9 B4 B3 106.3(4) . . ? C1 B4 B8 104.4(3) . . ? B9 B4 B8 59.4(3) . . ? B3 B4 B8 58.4(3) . . ? C1 B4 B5 58.6(2) . . ? B9 B4 B5 60.4(3) . . ? B3 B4 B5 108.5(3) . . ? B8 B4 B5 108.0(3) . . ? C1 B5 B6 59.9(2) . . ? C1 B5 B4 58.5(2) . . ? B6 B5 B4 108.4(4) . . ? C1 B5 B9 103.6(3) . . ? B6 B5 B9 106.4(4) . . ? B4 B5 B9 59.3(3) . . ? C1 B5 B10 104.1(3) . . ? B6 B5 B10 58.5(3) . . ? B4 B5 B10 107.3(4) . . ? B9 B5 B10 59.6(3) . . ? C1 B6 B10 106.0(3) . . ? C1 B6 C2 55.8(2) . . ? B10 B6 C2 105.1(3) . . ? C1 B6 B5 58.8(2) . . ? B10 B6 B5 62.0(3) . . ? C2 B6 B5 104.3(3) . . ? C1 B6 B11 104.4(3) . . ? B10 B6 B11 60.4(3) . . ? C2 B6 B11 58.8(2) . . ? B5 B6 B11 109.8(4) . . ? C2 B7 B12 104.4(3) . . ? C2 B7 B3 58.9(2) . . ? B12 B7 B3 107.4(4) . . ? C2 B7 B8 103.6(3) . . ? B12 B7 B8 60.3(3) . . ? B3 B7 B8 58.6(3) . . ? C2 B7 B11 59.0(2) . . ? B12 B7 B11 59.8(3) . . ? B3 B7 B11 108.3(3) . . ? B8 B7 B11 107.8(4) . . ? B3 B8 B9 108.7(4) . . ? B3 B8 B12 108.0(4) . . ? B9 B8 B12 60.4(3) . . ? B3 B8 B7 60.4(3) . . ? B9 B8 B7 108.1(4) . . ? B12 B8 B7 59.3(3) . . ? B3 B8 B4 60.7(3) . . ? B9 B8 B4 60.1(3) . . ? B12 B8 B4 108.4(3) . . ? B7 B8 B4 108.9(3) . . ? B8 B9 B4 60.5(3) . . ? B8 B9 B12 60.2(3) . . ? B4 B9 B12 108.6(4) . . ? B8 B9 B10 108.3(4) . . ? B4 B9 B10 108.7(4) . . ? B12 B9 B10 59.7(3) . . ? B8 B9 B5 108.8(4) . . ? B4 B9 B5 60.3(3) . . ? B12 B9 B5 108.3(4) . . ? B10 B9 B5 60.5(3) . . ? B6 B10 B11 60.8(3) . . ? B6 B10 B12 108.2(4) . . ? B11 B10 B12 59.7(3) . . ? B6 B10 B9 107.5(3) . . ? B11 B10 B9 107.6(4) . . ? B12 B10 B9 59.9(3) . . ? B6 B10 B5 59.6(3) . . ? B11 B10 B5 108.2(3) . . ? B12 B10 B5 108.0(4) . . ? B9 B10 B5 59.9(3) . . ? C2 B11 B12 104.0(3) . . ? C2 B11 B10 104.5(3) . . ? B12 B11 B10 60.3(3) . . ? C2 B11 B6 59.6(2) . . ? B12 B11 B6 107.2(4) . . ? B10 B11 B6 58.9(3) . . ? C2 B11 B7 58.9(2) . . ? B12 B11 B7 59.4(3) . . ? B10 B11 B7 108.2(4) . . ? B6 B11 B7 108.8(3) . . ? B7 B12 B11 60.8(3) . . ? B7 B12 B10 109.0(4) . . ? B11 B12 B10 60.0(3) . . ? B7 B12 B8 60.4(3) . . ? B11 B12 B8 108.8(3) . . ? B10 B12 B8 108.3(4) . . ? B7 B12 B9 108.3(3) . . ? B11 B12 B9 108.2(4) . . ? B10 B12 B9 60.4(3) . . ? B8 B12 B9 59.4(3) . . ? C9 C9 C10 132(5) 2_656 2_656 ? C9 C9 C10 34(4) 2_656 . ? C10 C9 C10 163.2(15) 2_656 . ? C9 C9 C14 109.0(14) 2_656 . ? C10 C9 C14 70.04(17) 2_656 . ? C10 C9 C14 120.0 . . ? C9 C9 C14 56.0(13) 2_656 2_656 ? C10 C9 C14 130.0(9) 2_656 2_656 ? C10 C9 C14 57.1(5) . 2_656 ? C14 C9 C14 63.0(5) . 2_656 ? C9 C10 C11 116.8(6) 2_656 . ? C9 C10 C9 13.4(17) 2_656 . ? C11 C10 C9 120.0 . . ? C9 C10 C14 65.9(7) 2_656 2_656 ? C11 C10 C14 51.7(7) . 2_656 ? C9 C10 C14 68.4(7) . 2_656 ? C9 C10 C15 116.6(14) 2_656 2_656 ? C11 C10 C15 4.2(16) . 2_656 ? C9 C10 C15 120.9(11) . 2_656 ? C14 C10 C15 52.5(8) 2_656 2_656 ? C15 C11 C14 116(5) 2_656 2_656 ? C15 C11 C10 161(7) 2_656 . ? C14 C11 C10 65.88(17) 2_656 . ? C15 C11 C12 66(5) 2_656 . ? C14 C11 C12 54.24(15) 2_656 . ? C10 C11 C12 120.0 . . ? C14 C12 C15 71.6(13) 2_656 2_656 ? C14 C12 C11 56.2(7) 2_656 . ? C15 C12 C11 16.7(17) 2_656 . ? C14 C12 C13 64.0(7) 2_656 . ? C15 C12 C13 135.5(15) 2_656 . ? C11 C12 C13 119.9 . . ? C14 C13 C14 68.7(6) 2_656 . ? C14 C13 C12 51.3(6) 2_656 . ? C14 C13 C12 120.0 . . ? C14 C13 C12 119.9(6) 2_656 2_656 ? C14 C13 C12 51.23(8) . 2_656 ? C12 C13 C12 171.2(2) . 2_656 ? C12 C14 C11 69.6(11) 2_656 2_656 ? C12 C14 C13 64.8(10) 2_656 . ? C11 C14 C13 134.0(2) 2_656 . ? C12 C14 C9 174.2(12) 2_656 . ? C11 C14 C9 105.84(16) 2_656 . ? C13 C14 C9 120.1 . . ? C12 C14 C10 131.8(15) 2_656 2_656 ? C11 C14 C10 62.4(10) 2_656 2_656 ? C13 C14 C10 160.9(12) . 2_656 ? C9 C14 C10 44.1(11) . 2_656 ? C12 C14 C15 56.6(14) 2_656 . ? C11 C14 C15 14.4(13) 2_656 . ? C13 C14 C15 121.4(13) . . ? C9 C14 C15 118.4(13) . . ? C10 C14 C15 76.0(14) 2_656 . ? C12 C14 C14 120.4(10) 2_656 2_656 ? C11 C14 C14 167.9(9) 2_656 2_656 ? C13 C14 C14 55.6 . 2_656 ? C9 C14 C14 64.62(7) . 2_656 ? C10 C14 C14 106.9(11) 2_656 2_656 ? C15 C14 C14 177.0(13) . 2_656 ? C12 C14 C9 170.7(13) 2_656 2_656 ? C11 C14 C9 116.9(8) 2_656 2_656 ? C13 C14 C9 107.8(8) . 2_656 ? C9 C14 C9 15.0(10) . 2_656 ? C10 C14 C9 54.6(3) 2_656 2_656 ? C15 C14 C9 130.5(13) . 2_656 ? C14 C14 C9 52.4(8) 2_656 2_656 ? C2 C1 B4 111.1(3) . . ? C2 C1 B5 111.5(3) . . ? B4 C1 B5 62.8(3) . . ? C2 C1 B6 62.2(2) . . ? B4 C1 B6 113.1(3) . . ? B5 C1 B6 61.3(2) . . ? C2 C1 B3 61.2(2) . . ? B4 C1 B3 61.9(3) . . ? B5 C1 B3 113.6(3) . . ? B6 C1 B3 113.6(3) . . ? C2 C1 S1 112.2(3) . . ? B4 C1 S1 127.0(3) . . ? B5 C1 S1 123.6(3) . . ? B6 C1 S1 113.4(3) . . ? B3 C1 S1 117.9(3) . . ? C1 C2 B3 62.7(2) . . ? C1 C2 B7 112.0(3) . . ? B3 C2 B7 61.7(3) . . ? C1 C2 B11 111.6(3) . . ? B3 C2 B11 113.3(3) . . ? B7 C2 B11 62.2(3) . . ? C1 C2 B6 61.9(2) . . ? B3 C2 B6 114.6(3) . . ? B7 C2 B6 113.1(3) . . ? B11 C2 B6 61.6(3) . . ? C1 C2 S2 112.6(2) . . ? B3 C2 S2 113.4(3) . . ? B7 C2 S2 123.3(3) . . ? B11 C2 S2 126.1(3) . . ? B6 C2 S2 117.9(3) . . ? O1 C3 Mo1 167.1(5) . . ? C5 C4 C8 107.4(5) . . ? C5 C4 Co1 70.6(3) . . ? C8 C4 Co1 70.9(3) . . ? C6 C5 C4 108.8(5) . . ? C6 C5 Co1 70.9(3) . . ? C4 C5 Co1 69.4(3) . . ? C5 C6 C7 107.4(5) . . ? C5 C6 Co1 69.9(3) . . ? C7 C6 Co1 69.7(3) . . ? C8 C7 C6 108.7(5) . . ? C8 C7 Co1 70.6(3) . . ? C6 C7 Co1 70.6(3) . . ? C7 C8 C4 107.7(5) . . ? C7 C8 Co1 70.1(3) . . ? C4 C8 Co1 69.1(3) . . ? C11 C15 C12 97(5) 2_656 2_656 ? C11 C15 C14 50(4) 2_656 . ? C12 C15 C14 51.8(12) 2_656 . ? C11 C15 C10 15(3) 2_656 2_656 ? C12 C15 C10 103(2) 2_656 2_656 ? C14 C15 C10 51.5(11) . 2_656 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.537 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.073 # Attachment '6a_bi_CpstarSMoPyCO_f60701a.cif' data_f60701a _database_code_depnum_ccdc_archive 'CCDC 621984' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H49 B10 Co Mo N2 O2 S2' _chemical_formula_weight 796.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.600(4) _cell_length_b 12.850(4) _cell_length_c 12.982(4) _cell_angle_alpha 86.541(4) _cell_angle_beta 77.776(4) _cell_angle_gamma 85.741(4) _cell_volume 1883.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 899 _cell_measurement_theta_min 2.476 _cell_measurement_theta_max 24.490 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7401 _exptl_absorpt_correction_T_max 0.8749 _exptl_absorpt_process_details sadabs _exptl_special_details ; Using SQUEEZE procedure in the PLATON software suite. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.64 _diffrn_reflns_number 9485 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0952 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.14 _reflns_number_total 7991 _reflns_number_gt 4492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^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 7991 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.866 _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 Mo1 Mo 0.58263(4) 0.77670(3) 0.75505(3) 0.04482(14) Uani 1 1 d . . . Co1 Co 0.73208(6) 0.63212(5) 0.69048(5) 0.0509(2) Uani 1 1 d . . . S1 S 0.62277(10) 0.61894(8) 0.85062(9) 0.0456(3) Uani 1 1 d . . . S2 S 0.66699(11) 0.87550(9) 0.88021(9) 0.0480(3) Uani 1 1 d . . . N1 N 0.4009(3) 0.7964(3) 0.8648(3) 0.0495(10) Uani 1 1 d . . . N2 N 0.5253(4) 0.9331(3) 0.6906(3) 0.0568(11) Uani 1 1 d . . . O1 O 0.7831(4) 0.8387(3) 0.5681(3) 0.0892(14) Uani 1 1 d . . . O2 O 0.4612(4) 0.6680(3) 0.6014(3) 0.0981(15) Uani 1 1 d . . . B1 B 0.8261(4) 0.6967(4) 0.9361(4) 0.0457(13) Uani 1 1 d . . . H1 H 0.8848 0.7014 0.8576 0.055 Uiso 1 1 calc R . . B2 B 0.7927(5) 0.5767(5) 1.0024(4) 0.0549(15) Uani 1 1 d . . . H2 H 0.8309 0.5025 0.9678 0.066 Uiso 1 1 calc R . . B3 B 0.6466(5) 0.5874(5) 1.0769(4) 0.0545(14) Uani 1 1 d . . . H3 H 0.5895 0.5212 1.0900 0.065 Uiso 1 1 calc R . . B4 B 0.5881(5) 0.7163(4) 1.0583(4) 0.0496(13) Uani 1 1 d . . . H4 H 0.4937 0.7343 1.0589 0.060 Uiso 1 1 calc R . . B5 B 0.6752(5) 0.8022(5) 1.1071(4) 0.0580(15) Uani 1 1 d . . . H5 H 0.6364 0.8764 1.1411 0.070 Uiso 1 1 calc R . . B6 B 0.8202(5) 0.7905(5) 1.0316(5) 0.0572(15) Uani 1 1 d . . . H6 H 0.8758 0.8578 1.0159 0.069 Uiso 1 1 calc R . . B7 B 0.8798(5) 0.6642(5) 1.0510(5) 0.0593(16) Uani 1 1 d . . . H7 H 0.9747 0.6480 1.0487 0.071 Uiso 1 1 calc R . . B8 B 0.7671(6) 0.5933(5) 1.1407(5) 0.0627(17) Uani 1 1 d . . . H8 H 0.7886 0.5309 1.1968 0.075 Uiso 1 1 calc R . . B9 B 0.6414(6) 0.6803(5) 1.1736(5) 0.0631(16) Uani 1 1 d . . . H9 H 0.5813 0.6747 1.2513 0.076 Uiso 1 1 calc R . . B10 B 0.7866(6) 0.7269(5) 1.1564(5) 0.0663(17) Uani 1 1 d . . . H10 H 0.8213 0.7512 1.2232 0.080 Uiso 1 1 calc R . . C1 C 0.6880(4) 0.6527(3) 0.9588(3) 0.0408(10) Uani 1 1 d . . . C2 C 0.7031(4) 0.7807(3) 0.9740(3) 0.0430(10) Uani 1 1 d . . . C3 C 0.7177(5) 0.7944(4) 0.6391(4) 0.0604(14) Uani 1 1 d . . . C4 C 0.5083(5) 0.7055(4) 0.6578(4) 0.0637(14) Uani 1 1 d . . . C5 C 0.3659(5) 0.8791(4) 0.9234(4) 0.0603(14) Uani 1 1 d . . . H5A H 0.4170 0.9324 0.9191 0.072 Uiso 1 1 calc R . . C6 C 0.2563(5) 0.8883(5) 0.9904(5) 0.0747(17) Uani 1 1 d . . . H6A H 0.2354 0.9465 1.0312 0.090 Uiso 1 1 calc R . . C7 C 0.1796(5) 0.8135(5) 0.9970(5) 0.0790(18) Uani 1 1 d . . . H7A H 0.1053 0.8186 1.0413 0.095 Uiso 1 1 calc R . . C8 C 0.2156(5) 0.7300(4) 0.9360(5) 0.0765(17) Uani 1 1 d . . . H8A H 0.1648 0.6770 0.9376 0.092 Uiso 1 1 calc R . . C9 C 0.3238(5) 0.7234(4) 0.8734(4) 0.0609(14) Uani 1 1 d . . . H9A H 0.3459 0.6644 0.8339 0.073 Uiso 1 1 calc R . . C10 C 0.4225(5) 0.9511(5) 0.6610(4) 0.0755(17) Uani 1 1 d . . . H10A H 0.3728 0.8962 0.6697 0.091 Uiso 1 1 calc R . . C11 C 0.3837(7) 1.0448(6) 0.6184(5) 0.097(2) Uani 1 1 d . . . H11 H 0.3099 1.0539 0.6006 0.116 Uiso 1 1 calc R . . C12 C 0.4603(9) 1.1243(6) 0.6035(5) 0.118(3) Uani 1 1 d . . . H12 H 0.4398 1.1879 0.5719 0.141 Uiso 1 1 calc R . . C13 C 0.5642(8) 1.1106(5) 0.6343(5) 0.100(2) Uani 1 1 d . . . H13 H 0.6141 1.1650 0.6281 0.120 Uiso 1 1 calc R . . C14 C 0.5949(6) 1.0122(5) 0.6759(4) 0.0808(18) Uani 1 1 d . . . H14 H 0.6683 1.0016 0.6942 0.097 Uiso 1 1 calc R . . C15 C 0.7836(6) 0.5813(5) 0.5394(4) 0.0707(17) Uani 1 1 d . . . C16 C 0.8835(6) 0.6046(5) 0.5751(5) 0.0759(17) Uani 1 1 d . . . C17 C 0.8895(6) 0.5364(5) 0.6682(5) 0.080(2) Uani 1 1 d . . . C18 C 0.7942(6) 0.4743(4) 0.6837(4) 0.0721(17) Uani 1 1 d . . . C19 C 0.7286(6) 0.4987(5) 0.6084(5) 0.0751(18) Uani 1 1 d . . . C20 C 0.7436(7) 0.6251(6) 0.4429(5) 0.129(3) Uani 1 1 d . . . H20A H 0.7926 0.6802 0.4109 0.194 Uiso 1 1 calc R . . H20B H 0.6630 0.6523 0.4619 0.194 Uiso 1 1 calc R . . H20C H 0.7494 0.5710 0.3939 0.194 Uiso 1 1 calc R . . C21 C 0.9755(7) 0.6739(6) 0.5231(7) 0.138(3) Uani 1 1 d . . . H21A H 1.0418 0.6330 0.4851 0.207 Uiso 1 1 calc R . . H21B H 1.0003 0.7118 0.5752 0.207 Uiso 1 1 calc R . . H21C H 0.9445 0.7221 0.4748 0.207 Uiso 1 1 calc R . . C22 C 0.9906(6) 0.5327(6) 0.7252(5) 0.119(3) Uani 1 1 d . . . H22A H 0.9727 0.4887 0.7882 0.178 Uiso 1 1 calc R . . H22B H 1.0020 0.6019 0.7435 0.178 Uiso 1 1 calc R . . H22C H 1.0615 0.5051 0.6801 0.178 Uiso 1 1 calc R . . C23 C 0.7711(7) 0.3876(5) 0.7675(5) 0.123(3) Uani 1 1 d . . . H23A H 0.7934 0.3215 0.7359 0.185 Uiso 1 1 calc R . . H23B H 0.6886 0.3905 0.8000 0.185 Uiso 1 1 calc R . . H23C H 0.8166 0.3956 0.8199 0.185 Uiso 1 1 calc R . . C24 C 0.6236(7) 0.4433(5) 0.5983(6) 0.128(3) Uani 1 1 d . . . H24A H 0.6492 0.3791 0.5638 0.192 Uiso 1 1 calc R . . H24B H 0.5773 0.4867 0.5574 0.192 Uiso 1 1 calc R . . H24C H 0.5766 0.4285 0.6671 0.192 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0517(3) 0.0420(2) 0.0407(2) -0.00119(17) -0.01451(19) 0.01033(18) Co1 0.0626(5) 0.0487(4) 0.0415(4) -0.0069(3) -0.0168(3) 0.0183(3) S1 0.0536(7) 0.0399(6) 0.0452(6) -0.0001(5) -0.0165(6) 0.0012(5) S2 0.0587(8) 0.0412(6) 0.0448(6) 0.0046(5) -0.0143(6) -0.0029(6) N1 0.049(2) 0.047(2) 0.051(2) 0.0002(19) -0.011(2) 0.006(2) N2 0.073(3) 0.048(2) 0.045(2) 0.0069(19) -0.014(2) 0.019(2) O1 0.110(3) 0.067(3) 0.067(3) 0.019(2) 0.022(2) 0.015(2) O2 0.109(3) 0.109(3) 0.095(3) -0.044(3) -0.060(3) 0.022(3) B1 0.034(3) 0.056(3) 0.043(3) 0.006(3) -0.001(2) -0.002(3) B2 0.054(4) 0.059(4) 0.048(3) 0.005(3) -0.009(3) 0.008(3) B3 0.057(4) 0.052(3) 0.052(3) 0.008(3) -0.008(3) -0.007(3) B4 0.049(3) 0.054(3) 0.041(3) 0.008(3) -0.002(3) -0.004(3) B5 0.075(4) 0.060(4) 0.038(3) -0.005(3) -0.010(3) -0.004(3) B6 0.057(4) 0.064(4) 0.054(3) 0.005(3) -0.019(3) -0.012(3) B7 0.048(3) 0.072(4) 0.060(4) 0.010(3) -0.022(3) -0.004(3) B8 0.074(4) 0.065(4) 0.051(3) 0.018(3) -0.026(3) 0.004(3) B9 0.072(4) 0.073(4) 0.039(3) 0.000(3) -0.003(3) 0.003(3) B10 0.073(4) 0.085(5) 0.046(3) 0.005(3) -0.025(3) -0.006(4) C1 0.042(3) 0.042(2) 0.037(2) 0.0038(19) -0.008(2) 0.000(2) C2 0.048(3) 0.045(3) 0.035(2) 0.0001(19) -0.007(2) -0.003(2) C3 0.068(4) 0.049(3) 0.065(3) -0.016(3) -0.017(3) 0.020(3) C4 0.066(4) 0.074(4) 0.051(3) -0.012(3) -0.015(3) 0.012(3) C5 0.056(3) 0.047(3) 0.080(4) -0.014(3) -0.017(3) 0.006(2) C6 0.063(4) 0.067(4) 0.085(4) -0.015(3) 0.004(3) 0.009(3) C7 0.054(4) 0.068(4) 0.105(5) -0.003(4) 0.004(3) -0.004(3) C8 0.065(4) 0.059(4) 0.102(5) 0.000(3) -0.009(4) -0.007(3) C9 0.058(3) 0.045(3) 0.078(4) 0.001(3) -0.012(3) 0.001(3) C10 0.087(4) 0.079(4) 0.058(3) -0.005(3) -0.021(3) 0.035(3) C11 0.119(6) 0.099(5) 0.066(4) 0.013(4) -0.027(4) 0.052(5) C12 0.171(9) 0.093(6) 0.064(4) 0.021(4) -0.003(5) 0.076(6) C13 0.152(7) 0.048(4) 0.085(5) 0.023(3) -0.009(5) 0.017(4) C14 0.103(5) 0.066(4) 0.064(4) 0.004(3) -0.008(4) 0.022(4) C15 0.097(5) 0.075(4) 0.037(3) -0.012(3) -0.019(3) 0.041(3) C16 0.073(4) 0.068(4) 0.071(4) -0.020(3) 0.020(4) 0.014(3) C17 0.081(4) 0.099(5) 0.060(4) -0.034(3) -0.028(3) 0.058(4) C18 0.097(5) 0.056(3) 0.061(4) -0.012(3) -0.020(4) 0.027(3) C19 0.094(5) 0.066(4) 0.071(4) -0.040(3) -0.032(4) 0.028(3) C20 0.180(8) 0.154(7) 0.048(3) -0.029(4) -0.040(4) 0.096(6) C21 0.108(6) 0.128(7) 0.138(7) -0.005(6) 0.050(6) 0.031(5) C22 0.096(5) 0.162(7) 0.099(5) -0.039(5) -0.040(4) 0.075(5) C23 0.207(9) 0.064(4) 0.083(5) -0.002(4) -0.010(5) 0.036(5) C24 0.138(7) 0.103(6) 0.153(8) -0.058(6) -0.034(6) -0.018(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 Mo1 C3 1.946(6) . ? Mo1 C4 1.973(5) . ? Mo1 N2 2.240(4) . ? Mo1 N1 2.287(4) . ? Mo1 S1 2.3805(13) . ? Mo1 Co1 2.5007(9) . ? Mo1 S2 2.5132(13) . ? Co1 C15 2.056(5) . ? Co1 C16 2.076(6) . ? Co1 C19 2.080(5) . ? Co1 C17 2.101(5) . ? Co1 C18 2.102(5) . ? Co1 C3 2.156(5) . ? Co1 S1 2.1980(15) . ? S1 C1 1.819(4) . ? S2 C2 1.762(4) . ? N1 C9 1.328(6) . ? N1 C5 1.333(6) . ? N2 C14 1.324(7) . ? N2 C10 1.329(6) . ? O1 C3 1.205(6) . ? O2 C4 1.147(6) . ? B1 C1 1.698(7) . ? B1 C2 1.726(6) . ? B1 B2 1.749(8) . ? B1 B7 1.752(7) . ? B1 B6 1.769(8) . ? B2 C1 1.672(6) . ? B2 B3 1.764(8) . ? B2 B8 1.781(8) . ? B2 B7 1.792(8) . ? B3 C1 1.696(7) . ? B3 B4 1.765(8) . ? B3 B9 1.773(8) . ? B3 B8 1.778(8) . ? B4 C1 1.741(7) . ? B4 C2 1.760(7) . ? B4 B9 1.762(8) . ? B4 B5 1.779(8) . ? B5 C2 1.725(6) . ? B5 B6 1.759(9) . ? B5 B10 1.762(8) . ? B5 B9 1.771(8) . ? B6 C2 1.700(7) . ? B6 B7 1.742(8) . ? B6 B10 1.751(8) . ? B7 B10 1.751(9) . ? B7 B8 1.816(9) . ? B8 B9 1.764(8) . ? B8 B10 1.778(9) . ? B9 B10 1.794(9) . ? C1 C2 1.694(6) . ? C5 C6 1.381(7) . ? C6 C7 1.345(7) . ? C7 C8 1.359(8) . ? C8 C9 1.343(7) . ? C10 C11 1.380(8) . ? C11 C12 1.382(10) . ? C12 C13 1.344(10) . ? C13 C14 1.396(8) . ? C15 C16 1.394(8) . ? C15 C19 1.441(8) . ? C15 C20 1.492(7) . ? C16 C17 1.459(8) . ? C16 C21 1.466(9) . ? C17 C18 1.384(8) . ? C17 C22 1.510(8) . ? C18 C19 1.370(7) . ? C18 C23 1.506(8) . ? C19 C24 1.488(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mo1 C4 87.9(2) . . ? C3 Mo1 N2 81.60(18) . . ? C4 Mo1 N2 90.91(19) . . ? C3 Mo1 N1 163.02(17) . . ? C4 Mo1 N1 88.47(19) . . ? N2 Mo1 N1 81.88(15) . . ? C3 Mo1 S1 107.10(15) . . ? C4 Mo1 S1 93.40(16) . . ? N2 Mo1 S1 170.41(10) . . ? N1 Mo1 S1 89.67(10) . . ? C3 Mo1 Co1 56.35(14) . . ? C4 Mo1 Co1 76.61(15) . . ? N2 Mo1 Co1 136.05(11) . . ? N1 Mo1 Co1 138.30(10) . . ? S1 Mo1 Co1 53.46(4) . . ? C3 Mo1 S2 93.81(15) . . ? C4 Mo1 S2 176.55(15) . . ? N2 Mo1 S2 86.37(12) . . ? N1 Mo1 S2 89.03(10) . . ? S1 Mo1 S2 88.97(4) . . ? Co1 Mo1 S2 106.83(4) . . ? C15 Co1 C16 39.4(2) . . ? C15 Co1 C19 40.8(2) . . ? C16 Co1 C19 66.8(3) . . ? C15 Co1 C17 67.1(2) . . ? C16 Co1 C17 40.9(2) . . ? C19 Co1 C17 65.5(2) . . ? C15 Co1 C18 66.3(2) . . ? C16 Co1 C18 66.3(2) . . ? C19 Co1 C18 38.2(2) . . ? C17 Co1 C18 38.5(2) . . ? C15 Co1 C3 93.7(2) . . ? C16 Co1 C3 91.6(2) . . ? C19 Co1 C3 129.7(2) . . ? C17 Co1 C3 125.2(3) . . ? C18 Co1 C3 157.3(2) . . ? C15 Co1 S1 150.7(2) . . ? C16 Co1 S1 154.61(19) . . ? C19 Co1 S1 111.1(2) . . ? C17 Co1 S1 114.09(18) . . ? C18 Co1 S1 96.02(18) . . ? C3 Co1 S1 106.54(15) . . ? C15 Co1 Mo1 127.83(14) . . ? C16 Co1 Mo1 140.29(18) . . ? C19 Co1 Mo1 134.04(16) . . ? C17 Co1 Mo1 160.28(17) . . ? C18 Co1 Mo1 153.0(2) . . ? C3 Co1 Mo1 48.71(15) . . ? S1 Co1 Mo1 60.47(3) . . ? C1 S1 Co1 117.28(15) . . ? C1 S1 Mo1 107.67(14) . . ? Co1 S1 Mo1 66.07(4) . . ? C2 S2 Mo1 105.20(15) . . ? C9 N1 C5 116.2(4) . . ? C9 N1 Mo1 120.5(3) . . ? C5 N1 Mo1 123.4(4) . . ? C14 N2 C10 116.1(5) . . ? C14 N2 Mo1 121.4(4) . . ? C10 N2 Mo1 122.4(4) . . ? C1 B1 C2 59.3(3) . . ? C1 B1 B2 58.0(3) . . ? C2 B1 B2 106.3(4) . . ? C1 B1 B7 106.0(4) . . ? C2 B1 B7 105.6(4) . . ? B2 B1 B7 61.6(3) . . ? C1 B1 B6 105.3(4) . . ? C2 B1 B6 58.2(3) . . ? B2 B1 B6 108.1(4) . . ? B7 B1 B6 59.3(3) . . ? C1 B2 B1 59.5(3) . . ? C1 B2 B3 59.1(3) . . ? B1 B2 B3 108.8(4) . . ? C1 B2 B8 105.9(4) . . ? B1 B2 B8 108.8(4) . . ? B3 B2 B8 60.2(3) . . ? C1 B2 B7 105.4(4) . . ? B1 B2 B7 59.3(3) . . ? B3 B2 B7 108.9(4) . . ? B8 B2 B7 61.1(3) . . ? C1 B3 B2 57.7(3) . . ? C1 B3 B4 60.4(3) . . ? B2 B3 B4 108.2(4) . . ? C1 B3 B9 105.7(4) . . ? B2 B3 B9 107.6(4) . . ? B4 B3 B9 59.8(3) . . ? C1 B3 B8 105.0(4) . . ? B2 B3 B8 60.4(3) . . ? B4 B3 B8 107.9(4) . . ? B9 B3 B8 59.6(3) . . ? C1 B4 C2 57.9(3) . . ? C1 B4 B9 104.3(4) . . ? C2 B4 B9 105.3(4) . . ? C1 B4 B3 57.9(3) . . ? C2 B4 B3 105.3(4) . . ? B9 B4 B3 60.4(3) . . ? C1 B4 B5 104.0(4) . . ? C2 B4 B5 58.3(3) . . ? B9 B4 B5 60.0(3) . . ? B3 B4 B5 107.8(4) . . ? C2 B5 B6 58.4(3) . . ? C2 B5 B10 105.5(4) . . ? B6 B5 B10 59.7(3) . . ? C2 B5 B9 106.4(4) . . ? B6 B5 B9 108.5(4) . . ? B10 B5 B9 61.0(4) . . ? C2 B5 B4 60.3(3) . . ? B6 B5 B4 108.3(4) . . ? B10 B5 B4 108.4(4) . . ? B9 B5 B4 59.5(3) . . ? C2 B6 B7 107.2(4) . . ? C2 B6 B10 107.0(4) . . ? B7 B6 B10 60.2(4) . . ? C2 B6 B5 59.8(3) . . ? B7 B6 B5 108.8(4) . . ? B10 B6 B5 60.3(3) . . ? C2 B6 B1 59.7(3) . . ? B7 B6 B1 59.9(3) . . ? B10 B6 B1 107.9(4) . . ? B5 B6 B1 108.5(4) . . ? B6 B7 B10 60.2(3) . . ? B6 B7 B1 60.8(3) . . ? B10 B7 B1 108.6(4) . . ? B6 B7 B2 107.4(4) . . ? B10 B7 B2 107.1(4) . . ? B1 B7 B2 59.1(3) . . ? B6 B7 B8 107.6(4) . . ? B10 B7 B8 59.7(4) . . ? B1 B7 B8 107.1(4) . . ? B2 B7 B8 59.2(3) . . ? B9 B8 B10 60.9(4) . . ? B9 B8 B3 60.1(3) . . ? B10 B8 B3 108.1(4) . . ? B9 B8 B2 107.3(4) . . ? B10 B8 B2 106.4(4) . . ? B3 B8 B2 59.4(3) . . ? B9 B8 B7 107.3(4) . . ? B10 B8 B7 58.3(3) . . ? B3 B8 B7 107.2(4) . . ? B2 B8 B7 59.7(3) . . ? B4 B9 B8 108.7(4) . . ? B4 B9 B5 60.5(3) . . ? B8 B9 B5 107.9(4) . . ? B4 B9 B3 59.9(3) . . ? B8 B9 B3 60.4(3) . . ? B5 B9 B3 107.8(4) . . ? B4 B9 B10 107.8(4) . . ? B8 B9 B10 59.9(4) . . ? B5 B9 B10 59.2(3) . . ? B3 B9 B10 107.6(4) . . ? B7 B10 B6 59.6(3) . . ? B7 B10 B5 108.2(4) . . ? B6 B10 B5 60.1(3) . . ? B7 B10 B8 61.9(4) . . ? B6 B10 B8 108.9(4) . . ? B5 B10 B8 107.7(4) . . ? B7 B10 B9 108.8(4) . . ? B6 B10 B9 107.8(4) . . ? B5 B10 B9 59.8(3) . . ? B8 B10 B9 59.2(3) . . ? B2 C1 C2 111.4(3) . . ? B2 C1 B3 63.2(3) . . ? C2 C1 B3 111.5(3) . . ? B2 C1 B1 62.5(3) . . ? C2 C1 B1 61.2(3) . . ? B3 C1 B1 114.6(3) . . ? B2 C1 B4 113.8(4) . . ? C2 C1 B4 61.6(3) . . ? B3 C1 B4 61.8(3) . . ? B1 C1 B4 113.7(3) . . ? B2 C1 S1 123.0(3) . . ? C2 C1 S1 118.1(3) . . ? B3 C1 S1 117.7(3) . . ? B1 C1 S1 121.1(3) . . ? B4 C1 S1 113.5(3) . . ? C1 C2 B6 108.6(3) . . ? C1 C2 B5 108.5(3) . . ? B6 C2 B5 61.8(3) . . ? C1 C2 B1 59.5(3) . . ? B6 C2 B1 62.2(3) . . ? B5 C2 B1 112.1(4) . . ? C1 C2 B4 60.5(3) . . ? B6 C2 B4 112.0(4) . . ? B5 C2 B4 61.4(3) . . ? B1 C2 B4 111.4(3) . . ? C1 C2 S2 119.9(3) . . ? B6 C2 S2 121.8(3) . . ? B5 C2 S2 122.5(3) . . ? B1 C2 S2 118.1(3) . . ? B4 C2 S2 118.7(3) . . ? O1 C3 Mo1 157.8(4) . . ? O1 C3 Co1 127.3(4) . . ? Mo1 C3 Co1 74.9(2) . . ? O2 C4 Mo1 176.8(5) . . ? N1 C5 C6 122.2(5) . . ? C7 C6 C5 120.3(5) . . ? C6 C7 C8 117.0(6) . . ? C9 C8 C7 120.7(6) . . ? N1 C9 C8 123.6(5) . . ? N2 C10 C11 125.1(7) . . ? C10 C11 C12 116.4(7) . . ? C13 C12 C11 120.6(6) . . ? C12 C13 C14 118.1(7) . . ? N2 C14 C13 123.6(6) . . ? C16 C15 C19 107.5(5) . . ? C16 C15 C20 127.7(7) . . ? C19 C15 C20 124.6(7) . . ? C16 C15 Co1 71.1(3) . . ? C19 C15 Co1 70.5(3) . . ? C20 C15 Co1 127.7(4) . . ? C15 C16 C17 107.3(6) . . ? C15 C16 C21 127.4(7) . . ? C17 C16 C21 124.9(7) . . ? C15 C16 Co1 69.5(3) . . ? C17 C16 Co1 70.5(3) . . ? C21 C16 Co1 131.1(4) . . ? C18 C17 C16 106.8(5) . . ? C18 C17 C22 129.7(7) . . ? C16 C17 C22 123.2(7) . . ? C18 C17 Co1 70.8(3) . . ? C16 C17 Co1 68.6(3) . . ? C22 C17 Co1 129.8(4) . . ? C19 C18 C17 110.4(6) . . ? C19 C18 C23 125.1(7) . . ? C17 C18 C23 124.4(6) . . ? C19 C18 Co1 70.0(3) . . ? C17 C18 Co1 70.7(3) . . ? C23 C18 Co1 129.0(4) . . ? C18 C19 C15 108.0(6) . . ? C18 C19 C24 124.6(7) . . ? C15 C19 C24 127.4(6) . . ? C18 C19 Co1 71.7(3) . . ? C15 C19 Co1 68.7(3) . . ? C24 C19 Co1 127.9(4) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.844 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.083 # Attachment '7b_bi_CpstarSeMo_f60412a.cif' data_f60412a _database_code_depnum_ccdc_archive 'CCDC 621985' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H35 B20 Co Mo O2 Se4' _chemical_formula_weight 946.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.709(3) _cell_length_b 10.383(3) _cell_length_c 16.570(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.060(4) _cell_angle_gamma 90.00 _cell_volume 1751.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 964 _cell_measurement_theta_min 2.585 _cell_measurement_theta_max 21.299 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 5.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4342 _exptl_absorpt_correction_T_max 0.7879 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.80 _diffrn_reflns_number 7410 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.1269 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5619 _reflns_number_gt 3695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.043(16) _refine_ls_number_reflns 5619 _refine_ls_number_parameters 417 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.41426(17) 0.35547(17) 0.24607(10) 0.0320(4) Uani 1 1 d . . . Mo1 Mo 0.61390(11) 0.53013(10) 0.28651(7) 0.0303(3) Uani 1 1 d . . . C5 C 0.5911(13) 0.4839(13) 0.3969(9) 0.043(4) Uani 1 1 d . . . O1 O 0.5833(10) 0.4601(10) 0.4645(6) 0.056(3) Uani 1 1 d . . . C6 C 0.7057(14) 0.3614(15) 0.3047(8) 0.042(4) Uani 1 1 d . . . O2 O 0.7679(10) 0.2729(10) 0.3185(7) 0.061(3) Uani 1 1 d . . . Se1 Se 0.50505(12) 0.42195(12) 0.14121(8) 0.0305(3) Uani 1 1 d . . . Se2 Se 0.36387(12) 0.57150(12) 0.25919(7) 0.0325(3) Uani 1 1 d . . . C1 C 0.3850(11) 0.5617(12) 0.0824(6) 0.029(3) Uani 1 1 d . . . C2 C 0.3113(12) 0.6324(12) 0.1416(8) 0.034(3) Uani 1 1 d . . . B3 B 0.2243(14) 0.5267(16) 0.0637(9) 0.036(4) Uani 1 1 d . . . H3 H 0.1852 0.4329 0.0754 0.043 Uiso 1 1 calc R . . B4 B 0.2959(14) 0.5522(16) -0.0211(8) 0.037(4) Uani 1 1 d . . . H4 H 0.3045 0.4750 -0.0645 0.045 Uiso 1 1 calc R . . B5 B 0.4206(16) 0.6701(16) 0.0112(9) 0.043(4) Uani 1 1 d . . . H5 H 0.5069 0.6685 -0.0115 0.051 Uiso 1 1 calc R . . B6 B 0.4342(13) 0.7155(13) 0.1189(8) 0.026(3) Uani 1 1 d U . . H6 H 0.5287 0.7411 0.1657 0.031 Uiso 1 1 calc R . . B7 B 0.1556(15) 0.6715(15) 0.0806(9) 0.037(4) Uani 1 1 d . . . H7 H 0.0699 0.6715 0.1038 0.045 Uiso 1 1 calc R . . B8 B 0.1415(17) 0.6275(17) -0.0222(11) 0.051(5) Uani 1 1 d . . . H8 H 0.0465 0.5987 -0.0672 0.062 Uiso 1 1 calc R . . B9 B 0.2596(15) 0.7146(17) -0.0539(10) 0.042(4) Uani 1 1 d . . . H9 H 0.2400 0.7424 -0.1207 0.050 Uiso 1 1 calc R . . B10 B 0.3490(17) 0.8154(15) 0.0299(10) 0.044(5) Uani 1 1 d . . . H10 H 0.3892 0.9089 0.0189 0.053 Uiso 1 1 calc R . . B11 B 0.2841(15) 0.7898(18) 0.1151(10) 0.043(4) Uani 1 1 d . . . H11 H 0.2816 0.8666 0.1603 0.051 Uiso 1 1 calc R . . B12 B 0.1758(17) 0.7904(19) 0.0071(10) 0.051(5) Uani 1 1 d . . . H12 H 0.1043 0.8678 -0.0184 0.061 Uiso 1 1 calc R . . Se3 Se 0.68128(13) 0.72821(14) 0.37475(8) 0.0400(4) Uani 1 1 d . . . Se4 Se 0.80334(13) 0.57331(14) 0.23202(9) 0.0428(4) Uani 1 1 d . . . C3 C 0.8421(12) 0.7874(13) 0.3611(8) 0.038(3) Uani 1 1 d . . . C4 C 0.8989(12) 0.7239(14) 0.2906(8) 0.040(3) Uani 1 1 d . . . B13 B 0.9806(16) 0.7003(18) 0.3979(11) 0.054(5) Uani 1 1 d . . . H13 H 0.9855 0.6093 0.4327 0.064 Uiso 1 1 calc R . . B14 B 0.9723(16) 0.8416(17) 0.4447(11) 0.050(5) Uani 1 1 d . . . H14 H 0.9712 0.8454 0.5108 0.060 Uiso 1 1 calc R . . B15 B 0.8764(18) 0.952(2) 0.3673(11) 0.061(6) Uani 1 1 d . . . H15 H 0.8138 1.0248 0.3834 0.073 Uiso 1 1 calc R . . B16 B 0.832(2) 0.8707(17) 0.2689(10) 0.056(5) Uani 1 1 d . . . H16 H 0.7386 0.8922 0.2195 0.067 Uiso 1 1 calc R . . B17 B 1.0623(16) 0.7213(18) 0.3197(11) 0.054(5) Uani 1 1 d . . . H17 H 1.1200 0.6448 0.3020 0.064 Uiso 1 1 calc R . . B18 B 1.1122(18) 0.804(2) 0.4228(12) 0.066(6) Uani 1 1 d . . . H18 H 1.2037 0.7833 0.4741 0.079 Uiso 1 1 calc R . . B19 B 1.0521(17) 0.963(2) 0.3999(11) 0.059(6) Uani 1 1 d . . . H19 H 1.1044 1.0477 0.4346 0.071 Uiso 1 1 calc R . . B20 B 0.963(2) 0.976(2) 0.2916(13) 0.072(6) Uani 1 1 d . . . H20 H 0.9589 1.0673 0.2571 0.086 Uiso 1 1 calc R . . B21 B 0.9697(16) 0.8310(17) 0.2456(11) 0.047(5) Uani 1 1 d . . . H21 H 0.9679 0.8271 0.1789 0.056 Uiso 1 1 calc R . . B22 B 1.1070(19) 0.8800(19) 0.3266(14) 0.072(7) Uani 1 1 d . . . H22 H 1.1996 0.9067 0.3154 0.087 Uiso 1 1 calc R . . C7 C 0.3196(13) 0.2699(13) 0.3235(8) 0.039(3) Uani 1 1 d . . . C8 C 0.2366(13) 0.2695(13) 0.2361(9) 0.041(4) Uani 1 1 d . . . C9 C 0.2970(11) 0.2002(12) 0.1841(8) 0.031(3) Uani 1 1 d . . . C10 C 0.4203(14) 0.1549(14) 0.2414(9) 0.048(4) Uani 1 1 d . . . C11 C 0.4332(13) 0.1960(12) 0.3276(8) 0.038(3) Uani 1 1 d . . . C12 C 0.2860(15) 0.3174(16) 0.3973(8) 0.063(5) Uani 1 1 d . . . H12A H 0.2403 0.2514 0.4174 0.094 Uiso 1 1 calc R . . H12B H 0.2307 0.3919 0.3815 0.094 Uiso 1 1 calc R . . H12C H 0.3649 0.3400 0.4415 0.094 Uiso 1 1 calc R . . C13 C 0.0995(12) 0.3237(13) 0.2080(9) 0.045(4) Uani 1 1 d . . . H13A H 0.0382 0.2576 0.2107 0.068 Uiso 1 1 calc R . . H13B H 0.0789 0.3545 0.1508 0.068 Uiso 1 1 calc R . . H13C H 0.0939 0.3936 0.2447 0.068 Uiso 1 1 calc R . . C14 C 0.2474(13) 0.1661(14) 0.0925(9) 0.050(4) Uani 1 1 d . . . H14A H 0.1968 0.0883 0.0855 0.074 Uiso 1 1 calc R . . H14B H 0.3203 0.1534 0.0712 0.074 Uiso 1 1 calc R . . H14C H 0.1931 0.2346 0.0616 0.074 Uiso 1 1 calc R . . C15 C 0.5192(15) 0.0737(15) 0.2176(10) 0.072(5) Uani 1 1 d . . . H15A H 0.4980 -0.0156 0.2205 0.108 Uiso 1 1 calc R . . H15B H 0.6051 0.0904 0.2561 0.108 Uiso 1 1 calc R . . H15C H 0.5177 0.0945 0.1608 0.108 Uiso 1 1 calc R . . C16 C 0.5403(13) 0.1533(13) 0.4050(9) 0.058(5) Uani 1 1 d . . . H16A H 0.5149 0.0745 0.4258 0.087 Uiso 1 1 calc R . . H16B H 0.5550 0.2185 0.4480 0.087 Uiso 1 1 calc R . . H16C H 0.6196 0.1396 0.3907 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0318(11) 0.0323(11) 0.0314(10) 0.0022(9) 0.0093(8) -0.0014(9) Mo1 0.0313(6) 0.0276(7) 0.0311(6) -0.0019(5) 0.0083(5) 0.0001(5) C5 0.038(9) 0.032(9) 0.047(9) -0.003(7) -0.004(7) 0.002(7) O1 0.077(8) 0.054(7) 0.036(6) -0.001(5) 0.018(5) -0.003(6) C6 0.062(10) 0.042(10) 0.022(7) -0.003(7) 0.013(7) 0.017(8) O2 0.061(7) 0.031(7) 0.081(8) 0.011(6) 0.007(6) 0.012(6) Se1 0.0325(8) 0.0258(8) 0.0336(8) -0.0028(6) 0.0107(6) 0.0043(6) Se2 0.0348(7) 0.0320(8) 0.0323(7) -0.0011(7) 0.0128(6) 0.0041(7) C1 0.036(7) 0.027(8) 0.022(6) -0.007(6) 0.006(5) -0.010(6) C2 0.023(7) 0.023(7) 0.061(9) 0.004(7) 0.018(6) 0.005(6) B3 0.035(8) 0.031(9) 0.035(9) -0.012(8) 0.001(7) 0.010(8) B4 0.050(10) 0.042(11) 0.019(7) -0.011(8) 0.011(7) 0.000(8) B5 0.056(11) 0.047(11) 0.016(8) 0.005(7) -0.002(7) -0.008(9) B6 0.031(5) 0.018(5) 0.028(5) 0.000(4) 0.008(4) -0.002(4) B7 0.032(9) 0.038(10) 0.039(10) 0.004(8) 0.007(7) 0.001(8) B8 0.039(10) 0.040(11) 0.062(12) -0.018(9) -0.002(9) 0.007(9) B9 0.043(10) 0.052(12) 0.032(9) -0.003(8) 0.015(7) -0.004(9) B10 0.072(13) 0.023(9) 0.039(10) -0.008(7) 0.019(9) 0.020(9) B11 0.032(10) 0.056(12) 0.043(10) 0.001(9) 0.014(8) 0.000(8) B12 0.043(11) 0.060(13) 0.039(10) -0.006(9) -0.004(8) 0.003(9) Se3 0.0403(8) 0.0401(9) 0.0419(9) -0.0123(7) 0.0162(7) -0.0065(7) Se4 0.0422(8) 0.0383(10) 0.0546(9) -0.0126(8) 0.0250(7) -0.0039(7) C3 0.037(8) 0.041(9) 0.033(8) 0.017(7) 0.006(6) 0.006(7) C4 0.039(8) 0.038(9) 0.040(8) -0.008(7) 0.009(6) -0.013(7) B13 0.045(11) 0.046(12) 0.060(12) -0.004(10) 0.002(9) 0.020(9) B14 0.041(10) 0.046(12) 0.049(11) 0.007(9) -0.005(8) -0.017(9) B15 0.059(13) 0.066(15) 0.048(11) -0.010(11) 0.002(9) 0.006(11) B16 0.099(16) 0.042(12) 0.032(10) -0.001(9) 0.026(10) -0.001(11) B17 0.055(12) 0.048(12) 0.066(12) -0.001(10) 0.031(10) 0.011(10) B18 0.039(11) 0.092(17) 0.061(13) -0.012(12) 0.008(9) -0.012(11) B19 0.040(11) 0.070(15) 0.058(12) -0.012(11) 0.001(9) -0.014(10) B20 0.110(19) 0.038(11) 0.083(15) 0.012(11) 0.054(13) 0.002(12) B21 0.048(11) 0.049(13) 0.049(11) -0.001(9) 0.022(9) -0.010(9) B22 0.055(12) 0.047(13) 0.119(18) -0.047(13) 0.032(12) -0.022(10) C7 0.047(9) 0.029(8) 0.042(9) 0.012(7) 0.017(7) -0.002(7) C8 0.032(8) 0.032(9) 0.055(10) 0.008(7) 0.007(7) -0.006(7) C9 0.022(7) 0.022(8) 0.045(8) 0.020(6) 0.004(6) 0.004(6) C10 0.046(9) 0.038(9) 0.050(10) -0.012(7) 0.001(7) 0.023(8) C11 0.040(8) 0.027(8) 0.047(9) 0.000(7) 0.014(7) 0.001(7) C12 0.071(12) 0.080(14) 0.040(9) 0.003(9) 0.020(8) -0.003(10) C13 0.032(8) 0.042(10) 0.064(10) 0.001(8) 0.020(7) 0.003(7) C14 0.042(9) 0.032(9) 0.067(11) 0.005(8) 0.006(8) -0.002(7) C15 0.080(12) 0.034(10) 0.086(12) 0.022(10) 0.001(9) -0.027(10) C16 0.058(10) 0.032(9) 0.062(10) 0.023(8) -0.012(8) -0.006(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C8 2.061(13) . ? Co1 C7 2.065(13) . ? Co1 C10 2.086(14) . ? Co1 C9 2.105(13) . ? Co1 C11 2.107(13) . ? Co1 Se2 2.333(2) . ? Co1 Se1 2.343(2) . ? Co1 Mo1 2.724(2) . ? Mo1 C5 1.979(16) . ? Mo1 C6 1.985(15) . ? Mo1 Se3 2.4968(18) . ? Mo1 Se4 2.5035(18) . ? Mo1 Se1 2.5841(17) . ? Mo1 Se2 2.6090(18) . ? C5 O1 1.174(15) . ? C6 O2 1.117(15) . ? Se1 C1 1.982(12) . ? Se2 C2 1.958(13) . ? C1 C2 1.614(16) . ? C1 B4 1.687(16) . ? C1 B3 1.691(17) . ? C1 B6 1.731(18) . ? C1 B5 1.757(19) . ? C2 B11 1.69(2) . ? C2 B7 1.709(18) . ? C2 B6 1.710(18) . ? C2 B3 1.730(19) . ? B3 B7 1.73(2) . ? B3 B8 1.77(2) . ? B3 B4 1.82(2) . ? B4 B5 1.77(2) . ? B4 B9 1.78(2) . ? B4 B8 1.82(2) . ? B5 B10 1.76(2) . ? B5 B9 1.79(2) . ? B5 B6 1.81(2) . ? B6 B11 1.77(2) . ? B6 B10 1.80(2) . ? B7 B8 1.72(2) . ? B7 B12 1.79(2) . ? B7 B11 1.80(2) . ? B8 B9 1.76(2) . ? B8 B12 1.77(2) . ? B9 B12 1.73(2) . ? B9 B10 1.77(2) . ? B10 B11 1.78(2) . ? B10 B12 1.79(2) . ? B11 B12 1.81(2) . ? Se3 C3 1.907(13) . ? Se4 C4 1.954(13) . ? C3 C4 1.616(18) . ? C3 B13 1.68(2) . ? C3 B14 1.73(2) . ? C3 B16 1.73(2) . ? C3 B15 1.74(2) . ? C4 B21 1.65(2) . ? C4 B17 1.665(19) . ? C4 B16 1.68(2) . ? C4 B13 1.74(2) . ? B13 B14 1.67(2) . ? B13 B18 1.72(3) . ? B13 B17 1.79(2) . ? B14 B18 1.69(2) . ? B14 B15 1.79(2) . ? B14 B19 1.81(3) . ? B15 B16 1.76(2) . ? B15 B19 1.79(2) . ? B15 B20 1.80(3) . ? B16 B21 1.69(2) . ? B16 B20 1.73(3) . ? B17 B22 1.71(3) . ? B17 B21 1.74(2) . ? B17 B18 1.84(3) . ? B18 B22 1.76(3) . ? B18 B19 1.78(3) . ? B19 B22 1.74(3) . ? B19 B20 1.76(3) . ? B20 B21 1.70(3) . ? B20 B22 1.77(3) . ? B21 B22 1.73(2) . ? C7 C11 1.422(17) . ? C7 C8 1.445(17) . ? C7 C12 1.464(18) . ? C8 C9 1.422(18) . ? C8 C13 1.505(17) . ? C9 C10 1.445(16) . ? C9 C14 1.488(17) . ? C10 C11 1.456(17) . ? C10 C15 1.50(2) . ? C11 C16 1.498(17) . ? 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 C8 Co1 C7 41.0(5) . . ? C8 Co1 C10 66.6(6) . . ? C7 Co1 C10 67.7(6) . . ? C8 Co1 C9 39.9(5) . . ? C7 Co1 C9 68.9(5) . . ? C10 Co1 C9 40.3(5) . . ? C8 Co1 C11 67.3(5) . . ? C7 Co1 C11 39.8(5) . . ? C10 Co1 C11 40.6(5) . . ? C9 Co1 C11 68.6(5) . . ? C8 Co1 Se2 100.9(4) . . ? C7 Co1 Se2 100.6(4) . . ? C10 Co1 Se2 167.0(4) . . ? C9 Co1 Se2 131.4(3) . . ? C11 Co1 Se2 132.5(4) . . ? C8 Co1 Se1 130.8(4) . . ? C7 Co1 Se1 169.6(4) . . ? C10 Co1 Se1 104.0(4) . . ? C9 Co1 Se1 100.7(4) . . ? C11 Co1 Se1 136.7(4) . . ? Se2 Co1 Se1 86.96(7) . . ? C8 Co1 Mo1 160.5(4) . . ? C7 Co1 Mo1 129.2(4) . . ? C10 Co1 Mo1 130.0(4) . . ? C9 Co1 Mo1 159.0(4) . . ? C11 Co1 Mo1 117.0(4) . . ? Se2 Co1 Mo1 61.55(6) . . ? Se1 Co1 Mo1 60.78(6) . . ? C5 Mo1 C6 80.9(5) . . ? C5 Mo1 Se3 75.8(4) . . ? C6 Mo1 Se3 126.7(4) . . ? C5 Mo1 Se4 136.3(4) . . ? C6 Mo1 Se4 78.1(4) . . ? Se3 Mo1 Se4 86.81(6) . . ? C5 Mo1 Se1 127.4(4) . . ? C6 Mo1 Se1 79.5(4) . . ? Se3 Mo1 Se1 150.31(6) . . ? Se4 Mo1 Se1 85.62(6) . . ? C5 Mo1 Se2 77.7(4) . . ? C6 Mo1 Se2 127.2(4) . . ? Se3 Mo1 Se2 93.48(5) . . ? Se4 Mo1 Se2 144.17(6) . . ? Se1 Mo1 Se2 76.56(5) . . ? C5 Mo1 Co1 75.7(4) . . ? C6 Mo1 Co1 76.3(4) . . ? Se3 Mo1 Co1 139.00(6) . . ? Se4 Mo1 Co1 133.82(7) . . ? Se1 Mo1 Co1 52.30(5) . . ? Se2 Mo1 Co1 51.83(5) . . ? O1 C5 Mo1 176.5(12) . . ? O2 C6 Mo1 173.4(14) . . ? C1 Se1 Co1 103.0(3) . . ? C1 Se1 Mo1 100.2(3) . . ? Co1 Se1 Mo1 66.92(6) . . ? C2 Se2 Co1 102.8(4) . . ? C2 Se2 Mo1 100.9(3) . . ? Co1 Se2 Mo1 66.63(6) . . ? C2 C1 B4 114.5(10) . . ? C2 C1 B3 63.1(8) . . ? B4 C1 B3 65.1(8) . . ? C2 C1 B6 61.4(7) . . ? B4 C1 B6 115.1(10) . . ? B3 C1 B6 116.4(10) . . ? C2 C1 B5 111.5(10) . . ? B4 C1 B5 61.7(8) . . ? B3 C1 B5 115.8(10) . . ? B6 C1 B5 62.5(8) . . ? C2 C1 Se1 113.5(7) . . ? B4 C1 Se1 122.2(9) . . ? B3 C1 Se1 113.6(8) . . ? B6 C1 Se1 115.0(7) . . ? B5 C1 Se1 123.8(9) . . ? C1 C2 B11 111.0(10) . . ? C1 C2 B7 108.7(10) . . ? B11 C2 B7 63.9(9) . . ? C1 C2 B6 62.7(8) . . ? B11 C2 B6 62.5(8) . . ? B7 C2 B6 115.2(10) . . ? C1 C2 B3 60.6(7) . . ? B11 C2 B3 114.2(11) . . ? B7 C2 B3 60.6(8) . . ? B6 C2 B3 115.4(10) . . ? C1 C2 Se2 114.5(8) . . ? B11 C2 Se2 122.9(9) . . ? B7 C2 Se2 126.3(9) . . ? B6 C2 Se2 112.2(8) . . ? B3 C2 Se2 117.4(9) . . ? C1 B3 C2 56.3(7) . . ? C1 B3 B7 104.0(11) . . ? C2 B3 B7 59.1(8) . . ? C1 B3 B8 104.4(12) . . ? C2 B3 B8 104.1(12) . . ? B7 B3 B8 59.0(9) . . ? C1 B3 B4 57.3(7) . . ? C2 B3 B4 103.0(11) . . ? B7 B3 B4 107.4(12) . . ? B8 B3 B4 61.2(9) . . ? C1 B4 B5 61.1(8) . . ? C1 B4 B9 104.9(10) . . ? B5 B4 B9 60.6(9) . . ? C1 B4 B3 57.6(7) . . ? B5 B4 B3 109.1(10) . . ? B9 B4 B3 105.7(10) . . ? C1 B4 B8 102.1(10) . . ? B5 B4 B8 107.7(12) . . ? B9 B4 B8 58.6(9) . . ? B3 B4 B8 58.1(9) . . ? C1 B5 B10 103.5(11) . . ? C1 B5 B4 57.2(8) . . ? B10 B5 B4 108.5(12) . . ? C1 B5 B9 101.6(11) . . ? B10 B5 B9 59.6(9) . . ? B4 B5 B9 60.0(9) . . ? C1 B5 B6 58.1(7) . . ? B10 B5 B6 60.6(9) . . ? B4 B5 B6 107.5(11) . . ? B9 B5 B6 107.2(12) . . ? C2 B6 C1 55.9(7) . . ? C2 B6 B11 58.3(8) . . ? C1 B6 B11 102.5(10) . . ? C2 B6 B10 104.0(10) . . ? C1 B6 B10 102.9(9) . . ? B11 B6 B10 59.7(9) . . ? C2 B6 B5 104.7(10) . . ? C1 B6 B5 59.5(8) . . ? B11 B6 B5 106.6(11) . . ? B10 B6 B5 58.5(8) . . ? C2 B7 B8 107.0(11) . . ? C2 B7 B3 60.3(8) . . ? B8 B7 B3 61.5(9) . . ? C2 B7 B12 105.3(11) . . ? B8 B7 B12 60.2(9) . . ? B3 B7 B12 109.9(12) . . ? C2 B7 B11 57.6(8) . . ? B8 B7 B11 108.6(12) . . ? B3 B7 B11 108.8(11) . . ? B12 B7 B11 60.4(9) . . ? B7 B8 B9 107.9(12) . . ? B7 B8 B12 61.9(9) . . ? B9 B8 B12 58.9(10) . . ? B7 B8 B3 59.5(9) . . ? B9 B8 B3 108.4(12) . . ? B12 B8 B3 109.7(12) . . ? B7 B8 B4 107.6(11) . . ? B9 B8 B4 59.3(9) . . ? B12 B8 B4 107.2(13) . . ? B3 B8 B4 60.7(8) . . ? B12 B9 B8 60.7(9) . . ? B12 B9 B10 61.6(9) . . ? B8 B9 B10 109.5(11) . . ? B12 B9 B4 110.9(12) . . ? B8 B9 B4 62.1(9) . . ? B10 B9 B4 107.9(11) . . ? B12 B9 B5 110.0(11) . . ? B8 B9 B5 109.6(12) . . ? B10 B9 B5 59.5(8) . . ? B4 B9 B5 59.5(9) . . ? B5 B10 B9 60.9(8) . . ? B5 B10 B11 108.1(12) . . ? B9 B10 B11 106.6(12) . . ? B5 B10 B12 108.4(12) . . ? B9 B10 B12 58.3(9) . . ? B11 B10 B12 60.8(9) . . ? B5 B10 B6 60.9(8) . . ? B9 B10 B6 108.4(11) . . ? B11 B10 B6 59.1(9) . . ? B12 B10 B6 108.5(12) . . ? C2 B11 B6 59.2(9) . . ? C2 B11 B10 105.8(11) . . ? B6 B11 B10 61.2(8) . . ? C2 B11 B7 58.5(9) . . ? B6 B11 B7 108.1(12) . . ? B10 B11 B7 107.4(11) . . ? C2 B11 B12 105.4(12) . . ? B6 B11 B12 109.5(11) . . ? B10 B11 B12 60.1(9) . . ? B7 B11 B12 59.7(9) . . ? B9 B12 B8 60.5(10) . . ? B9 B12 B10 60.1(9) . . ? B8 B12 B10 108.1(12) . . ? B9 B12 B7 106.0(13) . . ? B8 B12 B7 57.9(10) . . ? B10 B12 B7 106.9(11) . . ? B9 B12 B11 106.6(12) . . ? B8 B12 B11 106.5(13) . . ? B10 B12 B11 59.1(8) . . ? B7 B12 B11 60.0(9) . . ? C3 Se3 Mo1 107.7(4) . . ? C4 Se4 Mo1 108.8(4) . . ? C4 C3 B13 63.6(9) . . ? C4 C3 B14 108.8(11) . . ? B13 C3 B14 58.8(9) . . ? C4 C3 B16 60.0(9) . . ? B13 C3 B16 113.3(12) . . ? B14 C3 B16 111.1(12) . . ? C4 C3 B15 108.8(11) . . ? B13 C3 B15 111.0(12) . . ? B14 C3 B15 62.0(9) . . ? B16 C3 B15 61.1(9) . . ? C4 C3 Se3 120.7(9) . . ? B13 C3 Se3 120.8(10) . . ? B14 C3 Se3 123.0(10) . . ? B16 C3 Se3 117.0(10) . . ? B15 C3 Se3 119.4(10) . . ? C3 C4 B21 112.4(11) . . ? C3 C4 B17 113.2(10) . . ? B21 C4 B17 63.4(9) . . ? C3 C4 B16 63.4(9) . . ? B21 C4 B16 61.1(10) . . ? B17 C4 B16 114.8(12) . . ? C3 C4 B13 60.0(8) . . ? B21 C4 B13 113.7(11) . . ? B17 C4 B13 63.3(9) . . ? B16 C4 B13 113.2(11) . . ? C3 C4 Se4 115.4(8) . . ? B21 C4 Se4 124.0(9) . . ? B17 C4 Se4 118.2(10) . . ? B16 C4 Se4 119.9(10) . . ? B13 C4 Se4 114.5(10) . . ? B14 B13 C3 61.9(9) . . ? B14 B13 B18 59.9(11) . . ? C3 B13 B18 108.4(14) . . ? B14 B13 C4 105.6(12) . . ? C3 B13 C4 56.4(8) . . ? B18 B13 C4 105.8(13) . . ? B14 B13 B17 109.7(14) . . ? C3 B13 B17 104.3(12) . . ? B18 B13 B17 63.2(11) . . ? C4 B13 B17 56.3(9) . . ? B13 B14 B18 61.3(11) . . ? B13 B14 C3 59.2(9) . . ? B18 B14 C3 107.5(13) . . ? B13 B14 B15 109.2(13) . . ? B18 B14 B15 110.1(14) . . ? C3 B14 B15 59.4(9) . . ? B13 B14 B19 108.8(14) . . ? B18 B14 B19 60.8(11) . . ? C3 B14 B19 105.4(12) . . ? B15 B14 B19 59.8(10) . . ? C3 B15 B16 59.2(9) . . ? C3 B15 B14 58.6(9) . . ? B16 B15 B14 106.9(14) . . ? C3 B15 B19 105.5(13) . . ? B16 B15 B19 105.6(14) . . ? B14 B15 B19 60.8(10) . . ? C3 B15 B20 104.1(13) . . ? B16 B15 B20 58.1(11) . . ? B14 B15 B20 106.5(14) . . ? B19 B15 B20 58.5(11) . . ? C4 B16 B21 58.7(10) . . ? C4 B16 B20 105.2(14) . . ? B21 B16 B20 59.6(11) . . ? C4 B16 C3 56.6(8) . . ? B21 B16 C3 105.0(13) . . ? B20 B16 C3 107.4(13) . . ? C4 B16 B15 105.1(12) . . ? B21 B16 B15 108.8(14) . . ? B20 B16 B15 61.9(11) . . ? C3 B16 B15 59.8(9) . . ? C4 B17 B22 104.5(13) . . ? C4 B17 B21 57.8(9) . . ? B22 B17 B21 60.2(11) . . ? C4 B17 B13 60.4(9) . . ? B22 B17 B13 105.0(13) . . ? B21 B17 B13 106.9(12) . . ? C4 B17 B18 103.8(11) . . ? B22 B17 B18 59.5(12) . . ? B21 B17 B18 106.8(13) . . ? B13 B17 B18 56.6(9) . . ? B14 B18 B13 58.8(10) . . ? B14 B18 B22 107.9(15) . . ? B13 B18 B22 105.6(13) . . ? B14 B18 B19 62.9(11) . . ? B13 B18 B19 108.4(13) . . ? B22 B18 B19 58.7(11) . . ? B14 B18 B17 106.6(12) . . ? B13 B18 B17 60.2(10) . . ? B22 B18 B17 56.6(10) . . ? B19 B18 B17 104.7(13) . . ? B22 B19 B20 61.0(11) . . ? B22 B19 B18 60.3(12) . . ? B20 B19 B18 109.5(14) . . ? B22 B19 B15 107.8(13) . . ? B20 B19 B15 60.8(11) . . ? B18 B19 B15 106.1(13) . . ? B22 B19 B14 104.1(14) . . ? B20 B19 B14 107.3(13) . . ? B18 B19 B14 56.3(10) . . ? B15 B19 B14 59.4(10) . . ? B21 B20 B16 59.0(11) . . ? B21 B20 B19 108.0(15) . . ? B16 B20 B19 108.7(14) . . ? B21 B20 B22 59.8(11) . . ? B16 B20 B22 106.3(15) . . ? B19 B20 B22 58.9(12) . . ? B21 B20 B15 106.8(14) . . ? B16 B20 B15 59.9(10) . . ? B19 B20 B15 60.6(10) . . ? B22 B20 B15 106.1(15) . . ? C4 B21 B16 60.3(9) . . ? C4 B21 B20 107.9(13) . . ? B16 B21 B20 61.4(11) . . ? C4 B21 B22 104.3(13) . . ? B16 B21 B22 110.1(13) . . ? B20 B21 B22 62.2(12) . . ? C4 B21 B17 58.8(9) . . ? B16 B21 B17 110.2(12) . . ? B20 B21 B17 110.9(14) . . ? B22 B21 B17 59.0(11) . . ? B17 B22 B21 60.8(10) . . ? B17 B22 B19 112.3(15) . . ? B21 B22 B19 107.4(13) . . ? B17 B22 B18 63.8(12) . . ? B21 B22 B18 110.5(14) . . ? B19 B22 B18 61.0(12) . . ? B17 B22 B20 108.9(14) . . ? B21 B22 B20 57.9(11) . . ? B19 B22 B20 60.1(11) . . ? B18 B22 B20 109.2(15) . . ? C11 C7 C8 107.3(12) . . ? C11 C7 C12 124.7(13) . . ? C8 C7 C12 127.2(13) . . ? C11 C7 Co1 71.6(7) . . ? C8 C7 Co1 69.3(7) . . ? C12 C7 Co1 132.0(10) . . ? C9 C8 C7 110.7(11) . . ? C9 C8 C13 125.8(12) . . ? C7 C8 C13 123.1(13) . . ? C9 C8 Co1 71.7(8) . . ? C7 C8 Co1 69.6(7) . . ? C13 C8 Co1 130.6(10) . . ? C8 C9 C10 105.2(11) . . ? C8 C9 C14 130.7(11) . . ? C10 C9 C14 123.9(12) . . ? C8 C9 Co1 68.4(7) . . ? C10 C9 Co1 69.1(8) . . ? C14 C9 Co1 130.6(9) . . ? C9 C10 C11 109.8(12) . . ? C9 C10 C15 125.9(13) . . ? C11 C10 C15 124.3(12) . . ? C9 C10 Co1 70.5(7) . . ? C11 C10 Co1 70.5(8) . . ? C15 C10 Co1 127.2(11) . . ? C7 C11 C10 107.0(11) . . ? C7 C11 C16 128.1(13) . . ? C10 C11 C16 124.6(12) . . ? C7 C11 Co1 68.5(7) . . ? C10 C11 Co1 68.9(8) . . ? C16 C11 Co1 132.6(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.158 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.160 # Attachment '9a_bi_CpstarSW_f60610a3.cif' data_f60610a _database_code_depnum_ccdc_archive 'CCDC 621986' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H35 B20 Co O2 S4 W' _chemical_formula_weight 846.66 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' W W -0.8490 6.8722 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.778(3) _cell_length_b 14.753(3) _cell_length_c 17.735(4) _cell_angle_alpha 95.409(4) _cell_angle_beta 101.631(4) _cell_angle_gamma 90.833(4) _cell_volume 3513.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 835 _cell_measurement_theta_min 2.356 _cell_measurement_theta_max 17.841 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 4.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2396 _exptl_absorpt_correction_T_max 0.8250 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.91 _diffrn_reflns_number 14941 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.1956 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12251 _reflns_number_gt 5919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^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 12251 _refine_ls_number_parameters 843 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1305 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1623 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.833 _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 W1 W 0.08675(4) 0.87645(4) 0.20422(4) 0.03637(19) Uani 1 1 d . . . W2 W 0.26063(4) 0.37806(4) 0.20651(4) 0.03817(19) Uani 1 1 d . . . Co1 Co 0.28261(14) 0.87001(12) 0.23635(11) 0.0357(5) Uani 1 1 d . . . Co2 Co 0.08318(14) 0.36973(12) 0.24249(11) 0.0354(5) Uani 1 1 d . . . O1 O 0.1358(8) 0.7633(8) 0.0592(7) 0.065(3) Uani 1 1 d . . . O2 O 0.1500(8) 1.0382(8) 0.1194(7) 0.072(4) Uani 1 1 d . . . O3 O 0.1568(9) 0.5416(8) 0.1288(8) 0.080(4) Uani 1 1 d . . . O4 O 0.1297(9) 0.2722(8) 0.0583(7) 0.069(3) Uani 1 1 d . . . S1 S 0.1927(3) 0.7580(2) 0.2687(2) 0.0376(9) Uani 1 1 d . . . S2 S 0.2057(3) 0.9615(2) 0.3132(2) 0.0418(10) Uani 1 1 d . . . S3 S -0.0480(3) 0.7696(3) 0.1640(3) 0.0474(11) Uani 1 1 d . . . S4 S -0.0364(3) 0.9865(3) 0.2117(3) 0.0487(11) Uani 1 1 d . . . S5 S 0.1871(3) 0.2555(2) 0.2680(2) 0.0384(9) Uani 1 1 d . . . S6 S 0.2044(3) 0.4577(3) 0.3192(2) 0.0447(10) Uani 1 1 d . . . S7 S 0.3924(3) 0.4878(3) 0.2195(3) 0.0523(12) Uani 1 1 d . . . S8 S 0.3691(3) 0.2737(3) 0.1595(3) 0.0489(11) Uani 1 1 d . . . B1 B 0.3036(14) 0.8348(12) 0.4275(11) 0.049(5) Uani 1 1 d . . . H1 H 0.3746 0.8402 0.4087 0.059 Uiso 1 1 calc R . . B2 B 0.2563(16) 0.7296(15) 0.4433(11) 0.065(6) Uani 1 1 d . . . H2 H 0.2958 0.6664 0.4347 0.078 Uiso 1 1 calc R . . B3 B 0.1243(16) 0.7311(14) 0.4216(11) 0.065(6) Uani 1 1 d . . . H3 H 0.0793 0.6684 0.3994 0.078 Uiso 1 1 calc R . . B4 B 0.0886(14) 0.8377(13) 0.3902(12) 0.058(6) Uani 1 1 d . . . H4 H 0.0197 0.8443 0.3475 0.070 Uiso 1 1 calc R . . B5 B 0.1375(16) 0.9272(15) 0.4655(11) 0.064(6) Uani 1 1 d . . . H5 H 0.1013 0.9928 0.4713 0.077 Uiso 1 1 calc R . . B6 B 0.2662(16) 0.9226(16) 0.4879(11) 0.069(6) Uani 1 1 d . . . H6 H 0.3124 0.9849 0.5087 0.083 Uiso 1 1 calc R . . B7 B 0.2980(19) 0.8164(17) 0.5190(12) 0.083(8) Uani 1 1 d . . . H7 H 0.3660 0.8086 0.5623 0.099 Uiso 1 1 calc R . . B8 B 0.1888(17) 0.7524(16) 0.5184(12) 0.074(7) Uani 1 1 d . . . H8 H 0.1846 0.7032 0.5607 0.089 Uiso 1 1 calc R . . B9 B 0.0861(18) 0.8212(16) 0.4853(12) 0.077(7) Uani 1 1 d . . . H9 H 0.0159 0.8175 0.5055 0.092 Uiso 1 1 calc R . . B10 B 0.1958(15) 0.8722(16) 0.5443(13) 0.075(7) Uani 1 1 d . . . H10 H 0.1961 0.9009 0.6039 0.090 Uiso 1 1 calc R . . B11 B -0.1980(10) 0.8652(11) 0.2462(9) 0.041(4) Uani 1 1 d D . . H11 H -0.1549 0.8547 0.3039 0.049 Uiso 1 1 calc R . . B12 B -0.2650(14) 0.7757(12) 0.1916(12) 0.071(7) Uani 1 1 d D . . H12 H -0.2656 0.7085 0.2135 0.085 Uiso 1 1 calc R . . B13 B -0.2660(13) 0.7921(13) 0.0918(12) 0.053(5) Uani 1 1 d . . . H13 H -0.2683 0.7336 0.0480 0.063 Uiso 1 1 calc R . . B14 B -0.1987(14) 0.8911(12) 0.0873(12) 0.054(5) Uani 1 1 d . . . H14 H -0.1577 0.8986 0.0409 0.065 Uiso 1 1 calc R . . B15 B -0.2559(14) 0.9820(15) 0.1306(12) 0.062(6) Uani 1 1 d . . . H15 H -0.2515 1.0508 0.1121 0.074 Uiso 1 1 calc R . . B16 B -0.2518(12) 0.9652(11) 0.2315(12) 0.066(6) Uani 1 1 d D . . H16 H -0.2435 1.0202 0.2789 0.079 Uiso 1 1 calc R . . B18 B -0.3712(14) 0.8190(13) 0.1314(9) 0.061(6) Uani 1 1 d D . . H18 H -0.4413 0.7789 0.1131 0.073 Uiso 1 1 calc R . . B19 B -0.3273(14) 0.8934(13) 0.0704(12) 0.056(5) Uani 1 1 d . . . H19 H -0.3708 0.9029 0.0127 0.067 Uiso 1 1 calc R . . B21 B 0.3599(13) 0.3322(14) 0.3888(12) 0.058(6) Uani 1 1 d . . . H21 H 0.4036 0.3414 0.3444 0.070 Uiso 1 1 calc R . . B22 B 0.3427(15) 0.2242(15) 0.4180(12) 0.065(6) Uani 1 1 d . . . H22 H 0.3762 0.1641 0.3933 0.078 Uiso 1 1 calc R . . B23 B 0.2242(15) 0.2188(15) 0.4424(11) 0.061(6) Uani 1 1 d . . . H23 H 0.1797 0.1547 0.4328 0.073 Uiso 1 1 calc R . . B24 B 0.1721(16) 0.3259(13) 0.4314(10) 0.055(5) Uani 1 1 d . . . H24 H 0.0912 0.3321 0.4152 0.066 Uiso 1 1 calc R . . B25 B 0.2389(15) 0.4099(15) 0.4907(11) 0.063(6) Uani 1 1 d . . . H25 H 0.2036 0.4698 0.5138 0.076 Uiso 1 1 calc R . . B26 B 0.3608(14) 0.4170(15) 0.4650(12) 0.063(6) Uani 1 1 d . . . H26 H 0.4038 0.4816 0.4706 0.076 Uiso 1 1 calc R . . B27 B 0.4158(17) 0.3096(16) 0.4830(11) 0.075(7) Uani 1 1 d . . . H27 H 0.4963 0.3043 0.5028 0.090 Uiso 1 1 calc R . . B28 B 0.3276(19) 0.2376(18) 0.5130(13) 0.087(8) Uani 1 1 d . . . H28 H 0.3500 0.1846 0.5522 0.104 Uiso 1 1 calc R . . B29 B 0.2256(19) 0.3005(17) 0.5202(13) 0.086(8) Uani 1 1 d . . . H29 H 0.1828 0.2898 0.5649 0.103 Uiso 1 1 calc R . . B30 B 0.3454(17) 0.3577(18) 0.5437(14) 0.089(8) Uani 1 1 d . . . H30 H 0.3816 0.3847 0.6028 0.107 Uiso 1 1 calc R . . B31 B 0.5659(14) 0.3658(11) 0.2449(9) 0.042(5) Uani 1 1 d . . . H31 H 0.5556 0.3525 0.3028 0.051 Uiso 1 1 calc R . . B32 B 0.6144(15) 0.4663(14) 0.2327(12) 0.069(7) Uani 1 1 d D . . H32 H 0.6346 0.5196 0.2814 0.083 Uiso 1 1 calc R . . B33 B 0.5649(11) 0.4936(13) 0.1367(13) 0.065(6) Uani 1 1 d D . . H33 H 0.5536 0.5644 0.1232 0.077 Uiso 1 1 calc R . . B34 B 0.4800(14) 0.4057(13) 0.0895(12) 0.058(6) Uani 1 1 d . . . H34 H 0.4145 0.4187 0.0455 0.069 Uiso 1 1 calc R . . B35 B 0.5433(14) 0.3035(13) 0.0861(12) 0.060(6) Uani 1 1 d . . . H35 H 0.5185 0.2493 0.0388 0.072 Uiso 1 1 calc R . . B36 B 0.5922(13) 0.2770(13) 0.1790(12) 0.053(5) Uani 1 1 d . . . H36 H 0.5981 0.2055 0.1918 0.063 Uiso 1 1 calc R . . B39 B 0.6012(13) 0.4097(14) 0.0717(10) 0.068(6) Uani 1 1 d D . . H39 H 0.6164 0.4244 0.0154 0.081 Uiso 1 1 calc R . . B40 B 0.6690(14) 0.3312(11) 0.1291(13) 0.076(7) Uani 1 1 d D . . H40 H 0.7292 0.2936 0.1095 0.092 Uiso 1 1 calc R . . C1 C 0.1254(11) 0.8046(11) 0.1155(9) 0.047(4) Uani 1 1 d . . . C2 C 0.1306(12) 0.9779(11) 0.1537(9) 0.054(5) Uani 1 1 d . . . C3 C 0.1938(11) 0.7865(10) 0.3711(8) 0.045(4) Uani 1 1 d . . . C4 C 0.2005(10) 0.8962(10) 0.3952(8) 0.043(4) Uani 1 1 d . . . C5 C -0.1626(11) 0.8233(10) 0.1620(9) 0.046(4) Uani 1 1 d . . . C6 C -0.1592(10) 0.9340(10) 0.1855(9) 0.049(4) Uani 1 1 d . . . C7 C 0.3751(10) 0.8019(9) 0.1731(8) 0.034(4) Uani 1 1 d . . . C8 C 0.3566(11) 0.8880(11) 0.1454(9) 0.046(4) Uani 1 1 d . . . C9 C 0.3887(11) 0.9555(10) 0.2090(10) 0.047(4) Uani 1 1 d . . . C10 C 0.4336(10) 0.9105(9) 0.2759(9) 0.040(4) Uani 1 1 d . . . C11 C 0.4207(10) 0.8143(10) 0.2508(9) 0.042(4) Uani 1 1 d . . . C12 C 0.3575(10) 0.7136(9) 0.1255(8) 0.045(4) Uani 1 1 d . . . H12A H 0.4193 0.6919 0.1149 0.067 Uiso 1 1 calc R . . H12B H 0.3126 0.7209 0.0776 0.067 Uiso 1 1 calc R . . H12C H 0.3293 0.6704 0.1528 0.067 Uiso 1 1 calc R . . C13 C 0.3237(12) 0.9056(11) 0.0637(9) 0.061(5) Uani 1 1 d . . . H13A H 0.3803 0.9213 0.0430 0.092 Uiso 1 1 calc R . . H13B H 0.2791 0.9551 0.0606 0.092 Uiso 1 1 calc R . . H13C H 0.2905 0.8520 0.0345 0.092 Uiso 1 1 calc R . . C14 C 0.3876(12) 1.0574(9) 0.2081(10) 0.061(5) Uani 1 1 d . . . H14A H 0.4531 1.0830 0.2286 0.092 Uiso 1 1 calc R . . H14B H 0.3430 1.0820 0.2393 0.092 Uiso 1 1 calc R . . H14C H 0.3660 1.0722 0.1560 0.092 Uiso 1 1 calc R . . C15 C 0.4860(11) 0.9597(11) 0.3524(10) 0.066(5) Uani 1 1 d . . . H15A H 0.4414 1.0007 0.3720 0.099 Uiso 1 1 calc R . . H15B H 0.5428 0.9935 0.3449 0.099 Uiso 1 1 calc R . . H15C H 0.5069 0.9161 0.3887 0.099 Uiso 1 1 calc R . . C16 C 0.4652(10) 0.7394(10) 0.2991(9) 0.051(4) Uani 1 1 d . . . H16A H 0.4167 0.6908 0.2949 0.076 Uiso 1 1 calc R . . H16B H 0.4852 0.7637 0.3522 0.076 Uiso 1 1 calc R . . H16C H 0.5219 0.7164 0.2806 0.076 Uiso 1 1 calc R . . C17 C 0.1916(13) 0.4807(12) 0.1581(10) 0.058(5) Uani 1 1 d . . . C18 C 0.1753(11) 0.3094(11) 0.1157(10) 0.048(4) Uani 1 1 d . . . C19 C 0.2431(10) 0.2805(10) 0.3693(8) 0.041(4) Uani 1 1 d . . . C20 C 0.2548(11) 0.3899(10) 0.3982(9) 0.046(4) Uani 1 1 d . . . C21 C 0.4963(10) 0.4359(9) 0.1889(9) 0.044(4) Uani 1 1 d . . . C22 C 0.4863(11) 0.3283(9) 0.1587(9) 0.043(4) Uani 1 1 d . . . C23 C -0.0446(11) 0.3014(9) 0.1796(8) 0.037(4) Uani 1 1 d . . . C24 C -0.0498(10) 0.3122(9) 0.2593(9) 0.039(4) Uani 1 1 d . . . C25 C -0.0434(9) 0.4072(10) 0.2848(9) 0.041(4) Uani 1 1 d . . . C26 C -0.0345(10) 0.4572(9) 0.2216(9) 0.039(4) Uani 1 1 d . . . C27 C -0.0388(10) 0.3945(10) 0.1554(9) 0.043(4) Uani 1 1 d . . . C28 C -0.0550(10) 0.2172(9) 0.1292(8) 0.043(4) Uani 1 1 d . . . H28A H -0.0154 0.1718 0.1549 0.065 Uiso 1 1 calc R . . H28B H -0.0333 0.2273 0.0824 0.065 Uiso 1 1 calc R . . H28C H -0.1233 0.1966 0.1168 0.065 Uiso 1 1 calc R . . C29 C -0.0673(11) 0.2323(10) 0.3030(9) 0.052(4) Uani 1 1 d . . . H29A H -0.1308 0.2036 0.2803 0.077 Uiso 1 1 calc R . . H29B H -0.0658 0.2534 0.3561 0.077 Uiso 1 1 calc R . . H29C H -0.0163 0.1891 0.3003 0.077 Uiso 1 1 calc R . . C30 C -0.0551(12) 0.4495(10) 0.3634(9) 0.062(5) Uani 1 1 d . . . H30A H -0.0120 0.5027 0.3784 0.093 Uiso 1 1 calc R . . H30B H -0.0380 0.4063 0.4008 0.093 Uiso 1 1 calc R . . H30C H -0.1225 0.4664 0.3610 0.093 Uiso 1 1 calc R . . C31 C -0.0312(11) 0.5590(10) 0.2251(12) 0.078(6) Uani 1 1 d . . . H31A H -0.0388 0.5771 0.1737 0.117 Uiso 1 1 calc R . . H31B H 0.0312 0.5824 0.2557 0.117 Uiso 1 1 calc R . . H31C H -0.0841 0.5826 0.2483 0.117 Uiso 1 1 calc R . . C32 C -0.0489(11) 0.4162(10) 0.0725(9) 0.053(4) Uani 1 1 d . . . H32A H -0.1179 0.4190 0.0492 0.079 Uiso 1 1 calc R . . H32B H -0.0191 0.3695 0.0442 0.079 Uiso 1 1 calc R . . H32C H -0.0162 0.4739 0.0716 0.079 Uiso 1 1 calc R . . B20 B -0.3647(16) 0.9420(13) 0.1560(11) 0.067(6) Uani 1 1 d DU . . H20 H -0.4306 0.9836 0.1536 0.080 Uiso 1 1 calc R . . B38 B 0.6819(11) 0.4478(10) 0.1588(8) 0.068(6) Uani 1 1 d DU . . H38 H 0.7490 0.4888 0.1584 0.081 Uiso 1 1 calc R . . B17 B -0.3286(10) 0.8681(9) 0.2261(8) 0.044(4) Uani 1 1 d DU . . H17 H -0.3753 0.8614 0.2689 0.053 Uiso 1 1 calc R . . B37 B 0.6823(15) 0.3690(12) 0.2258(10) 0.059(5) Uani 1 1 d DU . . H37 H 0.7495 0.3576 0.2687 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0388(4) 0.0344(4) 0.0371(4) 0.0063(3) 0.0091(3) 0.0017(3) W2 0.0366(4) 0.0349(4) 0.0427(4) 0.0045(3) 0.0070(3) 0.0017(3) Co1 0.0396(12) 0.0328(11) 0.0359(12) 0.0052(9) 0.0097(9) 0.0011(9) Co2 0.0387(12) 0.0310(11) 0.0363(12) 0.0062(9) 0.0057(9) 0.0020(9) O1 0.062(8) 0.084(9) 0.046(8) -0.005(7) 0.012(6) 0.002(7) O2 0.076(9) 0.062(8) 0.087(10) 0.043(7) 0.025(7) 0.012(7) O3 0.064(9) 0.073(9) 0.107(11) 0.047(8) 0.012(8) 0.007(7) O4 0.063(8) 0.086(9) 0.057(9) -0.003(7) 0.018(7) -0.008(7) S1 0.049(2) 0.037(2) 0.028(2) 0.0058(17) 0.0085(18) -0.0008(18) S2 0.045(2) 0.037(2) 0.044(3) -0.0001(19) 0.013(2) 0.0005(19) S3 0.042(2) 0.035(2) 0.065(3) 0.007(2) 0.010(2) -0.0005(19) S4 0.043(2) 0.036(2) 0.066(3) 0.001(2) 0.011(2) -0.0006(19) S5 0.044(2) 0.039(2) 0.032(2) 0.0051(17) 0.0059(18) 0.0046(18) S6 0.046(2) 0.039(2) 0.046(3) -0.0007(19) 0.004(2) 0.0021(19) S7 0.040(2) 0.041(2) 0.075(3) -0.005(2) 0.015(2) 0.000(2) S8 0.050(3) 0.033(2) 0.066(3) 0.002(2) 0.017(2) 0.0030(19) B1 0.051(12) 0.046(12) 0.047(13) 0.004(10) 0.006(10) -0.002(10) B2 0.086(17) 0.065(14) 0.042(13) 0.020(11) 0.003(12) -0.017(12) B3 0.091(17) 0.065(14) 0.044(13) 0.013(11) 0.022(12) -0.017(13) B4 0.037(11) 0.071(14) 0.069(15) -0.001(12) 0.021(11) -0.007(10) B5 0.092(17) 0.076(15) 0.030(12) -0.003(10) 0.029(12) 0.020(13) B6 0.073(16) 0.102(18) 0.025(11) -0.011(11) -0.002(10) 0.007(14) B7 0.11(2) 0.11(2) 0.039(14) 0.028(14) 0.036(14) 0.028(17) B8 0.101(19) 0.087(17) 0.043(14) 0.030(13) 0.024(13) 0.008(15) B9 0.102(19) 0.096(18) 0.041(14) 0.014(13) 0.031(13) 0.007(16) B10 0.061(15) 0.12(2) 0.047(14) -0.007(14) 0.014(12) 0.015(14) B11 0.065(13) 0.048(11) 0.010(9) -0.001(8) 0.011(8) -0.009(10) B12 0.050(13) 0.109(18) 0.062(16) 0.034(14) 0.020(11) -0.027(13) B13 0.038(11) 0.049(12) 0.074(16) 0.001(11) 0.022(11) -0.006(9) B14 0.061(14) 0.050(12) 0.052(14) -0.009(10) 0.019(11) 0.002(10) B15 0.056(14) 0.077(15) 0.052(14) 0.008(12) 0.009(11) 0.003(12) B16 0.047(13) 0.095(18) 0.060(15) 0.002(13) 0.025(11) 0.015(12) B18 0.048(13) 0.075(15) 0.064(15) 0.012(12) 0.019(11) -0.004(11) B19 0.046(12) 0.059(13) 0.054(13) 0.000(10) -0.005(10) 0.002(10) B21 0.036(11) 0.078(15) 0.054(14) -0.013(11) 0.004(10) -0.005(11) B22 0.064(14) 0.071(15) 0.050(14) 0.005(11) -0.013(11) 0.023(12) B23 0.075(15) 0.076(15) 0.036(12) 0.025(11) 0.013(11) 0.023(12) B24 0.081(15) 0.058(13) 0.028(11) 0.001(9) 0.017(10) 0.011(12) B25 0.061(14) 0.077(15) 0.041(13) -0.020(11) -0.006(10) 0.015(12) B26 0.052(13) 0.069(15) 0.058(15) -0.005(12) -0.009(11) 0.000(11) B27 0.068(15) 0.11(2) 0.036(13) -0.002(13) -0.016(11) 0.027(15) B28 0.10(2) 0.10(2) 0.052(16) 0.022(14) -0.003(14) 0.032(17) B29 0.11(2) 0.11(2) 0.045(15) 0.026(14) 0.017(14) 0.032(17) B30 0.069(17) 0.13(2) 0.057(16) 0.008(15) -0.022(13) 0.016(16) B31 0.072(13) 0.032(10) 0.011(8) -0.010(7) -0.015(8) 0.016(9) B32 0.055(14) 0.067(15) 0.090(19) -0.024(13) 0.039(13) -0.010(11) B33 0.051(13) 0.049(13) 0.096(19) 0.013(12) 0.019(13) -0.006(11) B34 0.045(12) 0.062(14) 0.068(16) 0.007(12) 0.015(11) -0.005(10) B35 0.055(13) 0.049(13) 0.067(15) -0.022(11) 0.006(11) -0.005(10) B36 0.039(12) 0.047(12) 0.072(15) 0.000(11) 0.016(11) 0.003(10) B39 0.070(15) 0.078(16) 0.064(16) 0.018(13) 0.033(13) -0.007(13) B40 0.039(12) 0.098(19) 0.10(2) 0.018(15) 0.018(13) 0.030(13) C1 0.053(11) 0.057(11) 0.031(10) 0.003(8) 0.012(8) 0.013(8) C2 0.065(12) 0.055(11) 0.040(10) 0.016(9) 0.002(9) 0.023(9) C3 0.048(10) 0.057(10) 0.029(9) 0.011(8) 0.008(7) -0.009(8) C4 0.042(9) 0.049(10) 0.036(9) 0.005(8) 0.007(7) -0.013(8) C5 0.056(11) 0.037(9) 0.042(10) 0.009(8) 0.000(8) -0.003(8) C6 0.028(8) 0.041(9) 0.071(12) 0.026(9) -0.015(8) 0.005(7) C7 0.050(10) 0.027(8) 0.029(9) 0.010(7) 0.017(7) 0.006(7) C8 0.043(10) 0.063(11) 0.038(10) 0.007(9) 0.022(8) 0.006(9) C9 0.053(11) 0.027(9) 0.074(13) 0.020(9) 0.037(10) 0.024(8) C10 0.030(8) 0.027(8) 0.064(12) 0.000(8) 0.014(8) -0.010(7) C11 0.023(8) 0.043(10) 0.062(12) 0.004(8) 0.013(8) 0.005(7) C12 0.051(10) 0.039(9) 0.048(10) 0.015(8) 0.017(8) 0.005(8) C13 0.073(13) 0.060(11) 0.051(12) 0.010(9) 0.013(10) 0.002(10) C14 0.082(13) 0.033(9) 0.086(14) 0.019(9) 0.049(11) 0.005(9) C15 0.039(10) 0.063(12) 0.095(16) 0.001(11) 0.013(10) -0.010(9) C16 0.042(9) 0.055(11) 0.060(11) 0.019(9) 0.013(8) 0.021(8) C17 0.062(12) 0.052(11) 0.069(13) 0.020(10) 0.030(10) -0.003(9) C18 0.037(10) 0.053(11) 0.056(12) 0.016(9) 0.011(9) -0.010(8) C19 0.041(9) 0.049(10) 0.030(9) 0.004(7) -0.001(7) 0.003(8) C20 0.052(10) 0.042(9) 0.045(10) -0.005(8) 0.017(8) -0.002(8) C21 0.037(9) 0.033(9) 0.058(11) -0.004(8) 0.007(8) -0.004(7) C22 0.045(10) 0.033(9) 0.049(11) -0.006(7) 0.011(8) -0.001(7) C23 0.056(10) 0.027(8) 0.026(8) -0.001(7) 0.008(7) 0.007(7) C24 0.030(8) 0.036(9) 0.050(10) 0.002(8) 0.005(7) 0.005(7) C25 0.021(8) 0.039(9) 0.067(12) 0.012(9) 0.010(8) 0.012(7) C26 0.026(8) 0.031(9) 0.057(11) -0.002(8) 0.008(7) -0.010(7) C27 0.028(8) 0.051(10) 0.051(11) 0.029(9) 0.001(7) 0.011(7) C28 0.043(9) 0.031(8) 0.054(11) 0.014(8) 0.001(8) -0.007(7) C29 0.052(10) 0.055(10) 0.052(11) 0.020(9) 0.013(8) 0.001(8) C30 0.063(12) 0.051(11) 0.070(13) -0.015(9) 0.018(10) 0.002(9) C31 0.041(11) 0.051(11) 0.135(19) 0.011(12) -0.002(11) -0.001(9) C32 0.050(10) 0.058(11) 0.050(11) 0.021(9) 0.003(8) -0.004(9) B20 0.063(7) 0.069(7) 0.066(7) 0.003(5) 0.011(5) 0.004(5) B38 0.064(7) 0.068(7) 0.070(8) -0.001(5) 0.014(5) 0.002(5) B17 0.054(6) 0.037(6) 0.044(6) -0.006(4) 0.021(5) -0.008(4) B37 0.060(7) 0.053(7) 0.059(7) 0.003(5) 0.000(5) 0.007(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 W1 C2 1.962(17) . ? W1 C1 1.981(15) . ? W1 S3 2.369(4) . ? W1 S4 2.380(4) . ? W1 S2 2.490(4) . ? W1 S1 2.505(4) . ? W1 Co1 2.648(2) . ? W2 C17 1.973(18) . ? W2 C18 1.974(18) . ? W2 S8 2.372(4) . ? W2 S7 2.376(4) . ? W2 S6 2.487(4) . ? W2 S5 2.500(4) . ? W2 Co2 2.652(2) . ? Co1 C11 2.061(13) . ? Co1 C7 2.072(13) . ? Co1 C9 2.076(15) . ? Co1 C8 2.108(14) . ? Co1 C10 2.116(14) . ? Co1 S1 2.237(4) . ? Co1 S2 2.253(4) . ? Co2 C23 2.075(15) . ? Co2 C26 2.083(14) . ? Co2 C25 2.095(13) . ? Co2 C24 2.096(14) . ? Co2 C27 2.103(13) . ? Co2 S6 2.239(4) . ? Co2 S5 2.246(4) . ? O1 C1 1.154(16) . ? O2 C2 1.182(16) . ? O3 C17 1.143(16) . ? O4 C18 1.166(18) . ? S1 C3 1.821(15) . ? S2 C4 1.832(14) . ? S3 C5 1.772(15) . ? S4 C6 1.805(14) . ? S5 C19 1.808(14) . ? S6 C20 1.826(15) . ? S7 C21 1.788(14) . ? S8 C22 1.797(15) . ? B1 B7 1.69(3) . ? B1 C4 1.72(2) . ? B1 C3 1.74(2) . ? B1 B2 1.74(3) . ? B1 B6 1.75(3) . ? B2 C3 1.69(2) . ? B2 B7 1.77(3) . ? B2 B3 1.78(3) . ? B2 B8 1.78(3) . ? B3 C3 1.69(2) . ? B3 B4 1.76(3) . ? B3 B8 1.76(3) . ? B3 B9 1.82(3) . ? B4 C3 1.72(2) . ? B4 B9 1.73(3) . ? B4 C4 1.74(2) . ? B4 B5 1.81(3) . ? B5 C4 1.69(2) . ? B5 B6 1.74(3) . ? B5 B10 1.74(3) . ? B5 B9 1.80(3) . ? B6 C4 1.72(2) . ? B6 B10 1.73(3) . ? B6 B7 1.74(3) . ? B7 B10 1.75(3) . ? B7 B8 1.76(3) . ? B8 B10 1.78(3) . ? B8 B9 1.79(3) . ? B9 B10 1.77(3) . ? B11 B16 1.68(2) . ? B11 B12 1.70(2) . ? B11 C6 1.70(2) . ? B11 C5 1.73(2) . ? B11 B17 1.765(9) . ? B12 B17 1.759(10) . ? B12 C5 1.76(2) . ? B12 B18 1.79(3) . ? B12 B13 1.81(3) . ? B13 C5 1.72(2) . ? B13 B14 1.74(3) . ? B13 B19 1.76(3) . ? B13 B18 1.77(2) . ? B14 C5 1.73(2) . ? B14 B19 1.74(3) . ? B14 B15 1.76(3) . ? B14 C6 1.77(2) . ? B15 C6 1.69(2) . ? B15 B19 1.76(3) . ? B15 B20 1.76(3) . ? B15 B16 1.82(3) . ? B16 C6 1.69(2) . ? B16 B17 1.752(10) . ? B16 B20 1.84(3) . ? B18 B17 1.745(10) . ? B18 B19 1.79(3) . ? B18 B20 1.82(3) . ? B19 B20 1.79(3) . ? B21 C20 1.72(2) . ? B21 C19 1.73(2) . ? B21 B22 1.75(3) . ? B21 B26 1.75(3) . ? B21 B27 1.76(3) . ? B22 B28 1.73(3) . ? B22 C19 1.74(2) . ? B22 B23 1.77(3) . ? B22 B27 1.78(3) . ? B23 B28 1.70(3) . ? B23 C19 1.71(2) . ? B23 B29 1.74(3) . ? B23 B24 1.76(3) . ? B24 B29 1.68(3) . ? B24 B25 1.68(3) . ? B24 C20 1.70(2) . ? B24 C19 1.71(2) . ? B25 C20 1.70(2) . ? B25 B29 1.76(3) . ? B25 B30 1.80(3) . ? B25 B26 1.83(3) . ? B26 C20 1.70(2) . ? B26 B30 1.76(3) . ? B26 B27 1.79(3) . ? B27 B30 1.70(3) . ? B27 B28 1.79(3) . ? B28 B29 1.71(3) . ? B28 B30 1.80(4) . ? B29 B30 1.80(3) . ? B31 B32 1.67(3) . ? B31 C21 1.68(2) . ? B31 B37 1.70(3) . ? B31 C22 1.73(2) . ? B31 B36 1.76(2) . ? B32 C21 1.69(2) . ? B32 B37 1.73(3) . ? B32 B38 1.757(10) . ? B32 B33 1.79(3) . ? B33 C21 1.72(2) . ? B33 B38 1.743(10) . ? B33 B39 1.76(3) . ? B33 B34 1.76(3) . ? B34 C22 1.74(2) . ? B34 C21 1.75(2) . ? B34 B35 1.75(3) . ? B34 B39 1.76(3) . ? B35 C22 1.65(2) . ? B35 B36 1.73(3) . ? B35 B40 1.77(3) . ? B35 B39 1.81(3) . ? B36 C22 1.64(2) . ? B36 B40 1.74(3) . ? B36 B37 1.84(3) . ? B39 B38 1.751(10) . ? B39 B40 1.77(3) . ? B40 B37 1.73(3) . ? B40 B38 1.747(10) . ? C3 C4 1.63(2) . ? C5 C6 1.65(2) . ? C7 C11 1.388(19) . ? C7 C8 1.411(18) . ? C7 C12 1.474(18) . ? C8 C9 1.43(2) . ? C8 C13 1.478(19) . ? C9 C10 1.45(2) . ? C9 C14 1.505(17) . ? C10 C11 1.446(18) . ? C10 C15 1.51(2) . ? C11 C16 1.523(18) . ? C19 C20 1.642(19) . ? C21 C22 1.621(18) . ? C23 C24 1.425(18) . ? C23 C28 1.448(18) . ? C23 C27 1.482(18) . ? C24 C25 1.428(19) . ? C24 C29 1.512(18) . ? C25 C26 1.423(19) . ? C25 C30 1.51(2) . ? C26 C27 1.41(2) . ? C26 C31 1.497(19) . ? C27 C32 1.513(18) . ? B20 B17 1.732(10) . ? B38 B37 1.738(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 C2 W1 C1 81.7(6) . . ? C2 W1 S3 131.3(5) . . ? C1 W1 S3 78.1(5) . . ? C2 W1 S4 76.3(5) . . ? C1 W1 S4 132.3(4) . . ? S3 W1 S4 85.56(13) . . ? C2 W1 S2 78.4(5) . . ? C1 W1 S2 124.4(5) . . ? S3 W1 S2 147.94(14) . . ? S4 W1 S2 91.83(13) . . ? C2 W1 S1 127.0(4) . . ? C1 W1 S1 77.7(4) . . ? S3 W1 S1 90.92(13) . . ? S4 W1 S1 147.77(14) . . ? S2 W1 S1 74.55(12) . . ? C2 W1 Co1 76.1(4) . . ? C1 W1 Co1 73.1(5) . . ? S3 W1 Co1 136.23(10) . . ? S4 W1 Co1 138.03(11) . . ? S2 W1 Co1 51.90(9) . . ? S1 W1 Co1 51.37(9) . . ? C17 W2 C18 81.0(7) . . ? C17 W2 S8 129.8(5) . . ? C18 W2 S8 76.2(5) . . ? C17 W2 S7 78.1(5) . . ? C18 W2 S7 132.7(4) . . ? S8 W2 S7 85.62(13) . . ? C17 W2 S6 79.5(5) . . ? C18 W2 S6 126.2(4) . . ? S8 W2 S6 148.45(14) . . ? S7 W2 S6 90.82(14) . . ? C17 W2 S5 127.2(5) . . ? C18 W2 S5 78.5(4) . . ? S8 W2 S5 91.04(13) . . ? S7 W2 S5 146.00(14) . . ? S6 W2 S5 74.73(12) . . ? C17 W2 Co2 76.3(4) . . ? C18 W2 Co2 75.2(4) . . ? S8 W2 Co2 136.57(11) . . ? S7 W2 Co2 137.48(10) . . ? S6 W2 Co2 51.53(10) . . ? S5 W2 Co2 51.59(9) . . ? C11 Co1 C7 39.2(5) . . ? C11 Co1 C9 67.4(5) . . ? C7 Co1 C9 67.0(5) . . ? C11 Co1 C8 66.3(6) . . ? C7 Co1 C8 39.5(5) . . ? C9 Co1 C8 39.8(6) . . ? C11 Co1 C10 40.5(5) . . ? C7 Co1 C10 67.1(6) . . ? C9 Co1 C10 40.4(6) . . ? C8 Co1 C10 67.1(6) . . ? C11 Co1 S1 101.1(4) . . ? C7 Co1 S1 103.7(4) . . ? C9 Co1 S1 168.5(4) . . ? C8 Co1 S1 135.9(5) . . ? C10 Co1 S1 130.8(4) . . ? C11 Co1 S2 133.9(5) . . ? C7 Co1 S2 169.6(4) . . ? C9 Co1 S2 103.9(4) . . ? C8 Co1 S2 135.5(5) . . ? C10 Co1 S2 102.8(4) . . ? S1 Co1 S2 84.72(15) . . ? C11 Co1 W1 158.5(4) . . ? C7 Co1 W1 128.9(4) . . ? C9 Co1 W1 129.9(4) . . ? C8 Co1 W1 116.9(4) . . ? C10 Co1 W1 160.8(4) . . ? S1 Co1 W1 61.00(11) . . ? S2 Co1 W1 60.44(11) . . ? C23 Co2 C26 68.5(5) . . ? C23 Co2 C25 67.4(6) . . ? C26 Co2 C25 39.8(5) . . ? C23 Co2 C24 40.0(5) . . ? C26 Co2 C24 67.5(5) . . ? C25 Co2 C24 39.8(5) . . ? C23 Co2 C27 41.5(5) . . ? C26 Co2 C27 39.5(5) . . ? C25 Co2 C27 66.4(6) . . ? C24 Co2 C27 67.4(5) . . ? C23 Co2 S6 170.7(4) . . ? C26 Co2 S6 103.5(4) . . ? C25 Co2 S6 103.5(4) . . ? C24 Co2 S6 133.4(4) . . ? C27 Co2 S6 134.3(4) . . ? C23 Co2 S5 102.4(4) . . ? C26 Co2 S5 168.7(4) . . ? C25 Co2 S5 131.3(4) . . ? C24 Co2 S5 101.3(4) . . ? C27 Co2 S5 136.6(5) . . ? S6 Co2 S5 84.87(15) . . ? C23 Co2 W2 128.2(4) . . ? C26 Co2 W2 130.0(4) . . ? C25 Co2 W2 161.2(4) . . ? C24 Co2 W2 158.7(4) . . ? C27 Co2 W2 116.7(4) . . ? S6 Co2 W2 60.42(11) . . ? S5 Co2 W2 60.70(11) . . ? C3 S1 Co1 104.9(5) . . ? C3 S1 W1 103.6(5) . . ? Co1 S1 W1 67.64(11) . . ? C4 S2 Co1 104.2(5) . . ? C4 S2 W1 103.4(5) . . ? Co1 S2 W1 67.67(12) . . ? C5 S3 W1 111.0(5) . . ? C6 S4 W1 111.0(5) . . ? C19 S5 Co2 104.1(5) . . ? C19 S5 W2 102.8(5) . . ? Co2 S5 W2 67.71(11) . . ? C20 S6 Co2 105.2(5) . . ? C20 S6 W2 103.2(5) . . ? Co2 S6 W2 68.06(12) . . ? C21 S7 W2 110.0(5) . . ? C22 S8 W2 111.2(5) . . ? B7 B1 C4 105.3(14) . . ? B7 B1 C3 105.0(15) . . ? C4 B1 C3 56.2(9) . . ? B7 B1 B2 62.0(12) . . ? C4 B1 B2 104.8(14) . . ? C3 B1 B2 58.2(10) . . ? B7 B1 B6 60.8(12) . . ? C4 B1 B6 59.1(10) . . ? C3 B1 B6 104.7(13) . . ? B2 B1 B6 110.8(15) . . ? C3 B2 B1 60.8(10) . . ? C3 B2 B7 103.6(15) . . ? B1 B2 B7 57.5(11) . . ? C3 B2 B3 58.0(10) . . ? B1 B2 B3 108.8(14) . . ? B7 B2 B3 107.0(16) . . ? C3 B2 B8 103.0(15) . . ? B1 B2 B8 105.9(15) . . ? B7 B2 B8 59.5(13) . . ? B3 B2 B8 59.3(12) . . ? C3 B3 B4 59.9(10) . . ? C3 B3 B8 104.0(15) . . ? B4 B3 B8 106.5(15) . . ? C3 B3 B2 58.3(10) . . ? B4 B3 B2 108.6(14) . . ? B8 B3 B2 60.4(12) . . ? C3 B3 B9 103.8(14) . . ? B4 B3 B9 58.0(11) . . ? B8 B3 B9 59.9(12) . . ? B2 B3 B9 108.1(16) . . ? C3 B4 B9 105.9(14) . . ? C3 B4 C4 56.2(9) . . ? B9 B4 C4 104.7(15) . . ? C3 B4 B3 57.9(10) . . ? B9 B4 B3 62.6(12) . . ? C4 B4 B3 103.9(13) . . ? C3 B4 B5 103.0(13) . . ? B9 B4 B5 61.1(12) . . ? C4 B4 B5 56.9(10) . . ? B3 B4 B5 109.8(15) . . ? C4 B5 B6 60.0(10) . . ? C4 B5 B10 104.5(14) . . ? B6 B5 B10 59.7(12) . . ? C4 B5 B9 103.9(13) . . ? B6 B5 B9 108.2(15) . . ? B10 B5 B9 59.9(12) . . ? C4 B5 B4 59.5(9) . . ? B6 B5 B4 109.1(13) . . ? B10 B5 B4 105.7(15) . . ? B9 B5 B4 57.5(11) . . ? C4 B6 B10 103.8(15) . . ? C4 B6 B5 58.6(10) . . ? B10 B6 B5 60.2(12) . . ? C4 B6 B7 103.3(15) . . ? B10 B6 B7 60.6(13) . . ? B5 B6 B7 108.7(17) . . ? C4 B6 B1 59.6(10) . . ? B10 B6 B1 107.0(16) . . ? B5 B6 B1 109.0(15) . . ? B7 B6 B1 57.7(11) . . ? B1 B7 B6 61.5(11) . . ? B1 B7 B10 109.0(16) . . ? B6 B7 B10 59.4(12) . . ? B1 B7 B8 109.3(17) . . ? B6 B7 B8 109.1(17) . . ? B10 B7 B8 60.8(13) . . ? B1 B7 B2 60.6(11) . . ? B6 B7 B2 110.2(15) . . ? B10 B7 B2 109.6(19) . . ? B8 B7 B2 60.7(14) . . ? B7 B8 B3 107.9(14) . . ? B7 B8 B10 59.4(13) . . ? B3 B8 B10 108.4(15) . . ? B7 B8 B2 59.7(12) . . ? B3 B8 B2 60.3(11) . . ? B10 B8 B2 107.7(15) . . ? B7 B8 B9 107.5(16) . . ? B3 B8 B9 61.5(12) . . ? B10 B8 B9 59.4(12) . . ? B2 B8 B9 109.4(14) . . ? B4 B9 B10 107.8(16) . . ? B4 B9 B8 106.7(15) . . ? B10 B9 B8 60.1(13) . . ? B4 B9 B5 61.4(11) . . ? B10 B9 B5 58.5(13) . . ? B8 B9 B5 106.6(17) . . ? B4 B9 B3 59.4(11) . . ? B10 B9 B3 106.7(16) . . ? B8 B9 B3 58.6(12) . . ? B5 B9 B3 107.6(14) . . ? B6 B10 B5 60.1(12) . . ? B6 B10 B7 59.9(12) . . ? B5 B10 B7 108.1(15) . . ? B6 B10 B9 110.0(16) . . ? B5 B10 B9 61.7(12) . . ? B7 B10 B9 108.7(17) . . ? B6 B10 B8 108.7(15) . . ? B5 B10 B8 109.4(16) . . ? B7 B10 B8 59.8(13) . . ? B9 B10 B8 60.5(13) . . ? B16 B11 B12 112.5(10) . . ? B16 B11 C6 60.1(9) . . ? B12 B11 C6 108.2(12) . . ? B16 B11 C5 108.2(12) . . ? B12 B11 C5 61.8(9) . . ? C6 B11 C5 57.4(8) . . ? B16 B11 B17 61.1(6) . . ? B12 B11 B17 60.9(6) . . ? C6 B11 B17 105.8(10) . . ? C5 B11 B17 107.3(10) . . ? B11 B12 B17 61.3(6) . . ? B11 B12 C5 59.8(9) . . ? B17 B12 C5 106.1(12) . . ? B11 B12 B18 108.4(10) . . ? B17 B12 B18 58.9(6) . . ? C5 B12 B18 104.8(13) . . ? B11 B12 B13 106.7(13) . . ? B17 B12 B13 105.2(12) . . ? C5 B12 B13 57.6(9) . . ? B18 B12 B13 58.9(10) . . ? C5 B13 B14 60.2(10) . . ? C5 B13 B19 106.3(13) . . ? B14 B13 B19 59.6(10) . . ? C5 B13 B18 107.6(13) . . ? B14 B13 B18 109.9(13) . . ? B19 B13 B18 61.0(10) . . ? C5 B13 B12 59.8(10) . . ? B14 B13 B12 109.6(14) . . ? B19 B13 B12 108.3(13) . . ? B18 B13 B12 60.2(10) . . ? C5 B14 B13 59.4(10) . . ? C5 B14 B19 106.7(13) . . ? B13 B14 B19 60.9(11) . . ? C5 B14 B15 103.3(14) . . ? B13 B14 B15 107.4(14) . . ? B19 B14 B15 60.4(10) . . ? C5 B14 C6 56.1(9) . . ? B13 B14 C6 103.5(13) . . ? B19 B14 C6 104.7(13) . . ? B15 B14 C6 57.3(10) . . ? C6 B15 B14 61.7(10) . . ? C6 B15 B19 107.2(14) . . ? B14 B15 B19 59.2(11) . . ? C6 B15 B20 107.3(14) . . ? B14 B15 B20 109.8(15) . . ? B19 B15 B20 61.1(12) . . ? C6 B15 B16 57.5(10) . . ? B14 B15 B16 109.3(14) . . ? B19 B15 B16 109.7(14) . . ? B20 B15 B16 61.9(10) . . ? B11 B16 C6 60.6(9) . . ? B11 B16 B17 61.9(6) . . ? C6 B16 B17 106.8(12) . . ? B11 B16 B15 106.4(13) . . ? C6 B16 B15 57.4(10) . . ? B17 B16 B15 103.5(13) . . ? B11 B16 B20 107.4(11) . . ? C6 B16 B20 103.6(14) . . ? B17 B16 B20 57.6(6) . . ? B15 B16 B20 57.5(11) . . ? B17 B18 B13 107.5(12) . . ? B17 B18 B19 105.9(12) . . ? B13 B18 B19 59.3(10) . . ? B17 B18 B12 59.6(6) . . ? B13 B18 B12 61.0(10) . . ? B19 B18 B12 107.6(13) . . ? B17 B18 B20 58.1(6) . . ? B13 B18 B20 106.4(13) . . ? B19 B18 B20 59.3(10) . . ? B12 B18 B20 106.1(10) . . ? B14 B19 B15 60.4(10) . . ? B14 B19 B13 59.5(10) . . ? B15 B19 B13 106.3(14) . . ? B14 B19 B20 109.3(14) . . ? B15 B19 B20 59.5(11) . . ? B13 B19 B20 108.2(13) . . ? B14 B19 B18 108.7(13) . . ? B15 B19 B18 107.7(14) . . ? B13 B19 B18 59.7(10) . . ? B20 B19 B18 61.2(10) . . ? C20 B21 C19 56.9(9) . . ? C20 B21 B22 105.8(14) . . ? C19 B21 B22 59.9(10) . . ? C20 B21 B26 58.7(10) . . ? C19 B21 B26 106.1(13) . . ? B22 B21 B26 110.9(16) . . ? C20 B21 B27 105.5(14) . . ? C19 B21 B27 106.5(15) . . ? B22 B21 B27 60.9(12) . . ? B26 B21 B27 61.5(12) . . ? B28 B22 C19 103.2(14) . . ? B28 B22 B21 108.2(16) . . ? C19 B22 B21 59.4(10) . . ? B28 B22 B23 57.9(12) . . ? C19 B22 B23 58.4(10) . . ? B21 B22 B23 108.0(14) . . ? B28 B22 B27 61.5(13) . . ? C19 B22 B27 105.2(14) . . ? B21 B22 B27 59.8(12) . . ? B23 B22 B27 107.9(15) . . ? B28 B23 C19 105.7(16) . . ? B28 B23 B29 59.8(13) . . ? C19 B23 B29 104.1(15) . . ? B28 B23 B24 105.6(16) . . ? C19 B23 B24 59.2(9) . . ? B29 B23 B24 57.3(11) . . ? B28 B23 B22 59.9(12) . . ? C19 B23 B22 59.7(10) . . ? B29 B23 B22 107.2(17) . . ? B24 B23 B22 107.4(14) . . ? B29 B24 B25 63.3(13) . . ? B29 B24 C20 108.0(16) . . ? B25 B24 C20 60.3(11) . . ? B29 B24 C19 106.9(15) . . ? B25 B24 C19 108.3(15) . . ? C20 B24 C19 57.5(9) . . ? B29 B24 B23 60.9(12) . . ? B25 B24 B23 112.7(15) . . ? C20 B24 B23 106.3(13) . . ? C19 B24 B23 59.1(9) . . ? B24 B25 C20 60.4(10) . . ? B24 B25 B29 58.3(12) . . ? C20 B25 B29 104.3(14) . . ? B24 B25 B30 106.3(16) . . ? C20 B25 B30 102.0(14) . . ? B29 B25 B30 60.5(13) . . ? B24 B25 B26 107.8(14) . . ? C20 B25 B26 57.5(10) . . ? B29 B25 B26 107.0(14) . . ? B30 B25 B26 58.0(11) . . ? C20 B26 B21 59.7(10) . . ? C20 B26 B30 103.5(15) . . ? B21 B26 B30 104.9(16) . . ? C20 B26 B27 104.6(14) . . ? B21 B26 B27 59.4(11) . . ? B30 B26 B27 57.3(12) . . ? C20 B26 B25 57.3(10) . . ? B21 B26 B25 106.5(14) . . ? B30 B26 B25 60.2(11) . . ? B27 B26 B25 105.7(15) . . ? B30 B27 B21 107.2(15) . . ? B30 B27 B22 108.6(17) . . ? B21 B27 B22 59.3(11) . . ? B30 B27 B26 60.4(12) . . ? B21 B27 B26 59.1(11) . . ? B22 B27 B26 107.6(13) . . ? B30 B27 B28 61.9(14) . . ? B21 B27 B28 105.1(15) . . ? B22 B27 B28 58.1(13) . . ? B26 B27 B28 108.5(15) . . ? B23 B28 B29 61.4(13) . . ? B23 B28 B22 62.3(12) . . ? B29 B28 B22 110.3(15) . . ? B23 B28 B27 110.5(16) . . ? B29 B28 B27 107.6(17) . . ? B22 B28 B27 60.4(12) . . ? B23 B28 B30 110.0(16) . . ? B29 B28 B30 61.3(14) . . ? B22 B28 B30 106.2(17) . . ? B27 B28 B30 56.6(13) . . ? B24 B29 B28 108.4(16) . . ? B24 B29 B23 61.8(12) . . ? B28 B29 B23 58.8(13) . . ? B24 B29 B25 58.4(11) . . ? B28 B29 B25 110.9(19) . . ? B23 B29 B25 109.5(15) . . ? B24 B29 B30 106.7(17) . . ? B28 B29 B30 61.7(15) . . ? B23 B29 B30 108.2(17) . . ? B25 B29 B30 60.9(13) . . ? B27 B30 B26 62.3(13) . . ? B27 B30 B29 108.1(19) . . ? B26 B30 B29 108.5(15) . . ? B27 B30 B28 61.5(14) . . ? B26 B30 B28 109.6(17) . . ? B29 B30 B28 56.9(13) . . ? B27 B30 B25 111.0(16) . . ? B26 B30 B25 61.8(12) . . ? B29 B30 B25 58.6(12) . . ? B28 B30 B25 105.2(16) . . ? B32 B31 C21 60.7(10) . . ? B32 B31 B37 61.8(11) . . ? C21 B31 B37 108.0(12) . . ? B32 B31 C22 106.8(13) . . ? C21 B31 C22 56.8(8) . . ? B37 B31 C22 106.6(12) . . ? B32 B31 B36 112.6(13) . . ? C21 B31 B36 104.2(12) . . ? B37 B31 B36 64.1(10) . . ? C22 B31 B36 56.2(9) . . ? B31 B32 C21 59.9(10) . . ? B31 B32 B37 60.2(11) . . ? C21 B32 B37 106.1(14) . . ? B31 B32 B38 107.4(13) . . ? C21 B32 B38 104.3(13) . . ? B37 B32 B38 59.7(6) . . ? B31 B32 B33 108.9(15) . . ? C21 B32 B33 59.1(11) . . ? B37 B32 B33 107.8(11) . . ? B38 B32 B33 58.9(7) . . ? C21 B33 B38 103.7(12) . . ? C21 B33 B39 105.2(13) . . ? B38 B33 B39 60.0(6) . . ? C21 B33 B34 60.2(10) . . ? B38 B33 B34 108.1(13) . . ? B39 B33 B34 60.0(11) . . ? C21 B33 B32 57.6(10) . . ? B38 B33 B32 59.7(7) . . ? B39 B33 B32 107.9(11) . . ? B34 B33 B32 108.5(14) . . ? C22 B34 C21 55.4(9) . . ? C22 B34 B35 56.4(10) . . ? C21 B34 B35 102.0(14) . . ? C22 B34 B39 103.8(13) . . ? C21 B34 B39 104.0(13) . . ? B35 B34 B39 62.0(11) . . ? C22 B34 B33 103.1(14) . . ? C21 B34 B33 58.6(11) . . ? B35 B34 B33 108.5(13) . . ? B39 B34 B33 59.9(11) . . ? C22 B35 B36 58.1(10) . . ? C22 B35 B34 61.4(10) . . ? B36 B35 B34 110.2(14) . . ? C22 B35 B40 102.6(14) . . ? B36 B35 B40 59.6(11) . . ? B34 B35 B40 106.5(13) . . ? C22 B35 B39 105.5(13) . . ? B36 B35 B39 108.4(13) . . ? B34 B35 B39 59.2(11) . . ? B40 B35 B39 59.1(11) . . ? C22 B36 B35 58.6(10) . . ? C22 B36 B40 104.4(14) . . ? B35 B36 B40 61.3(12) . . ? C22 B36 B31 60.9(9) . . ? B35 B36 B31 108.2(13) . . ? B40 B36 B31 102.8(13) . . ? C22 B36 B37 104.3(12) . . ? B35 B36 B37 107.6(13) . . ? B40 B36 B37 57.5(11) . . ? B31 B36 B37 56.4(10) . . ? B38 B39 B33 59.5(7) . . ? B38 B39 B34 107.8(13) . . ? B33 B39 B34 60.1(10) . . ? B38 B39 B40 59.6(7) . . ? B33 B39 B40 106.1(11) . . ? B34 B39 B40 106.3(14) . . ? B38 B39 B35 107.1(13) . . ? B33 B39 B35 106.2(13) . . ? B34 B39 B35 58.8(10) . . ? B40 B39 B35 59.3(11) . . ? B37 B40 B36 64.2(12) . . ? B37 B40 B38 60.0(7) . . ? B36 B40 B38 111.0(13) . . ? B37 B40 B39 109.9(10) . . ? B36 B40 B39 110.1(14) . . ? B38 B40 B39 59.8(6) . . ? B37 B40 B35 111.1(15) . . ? B36 B40 B35 59.1(11) . . ? B38 B40 B35 109.1(12) . . ? B39 B40 B35 61.6(11) . . ? O1 C1 W1 171.5(14) . . ? O2 C2 W1 174.8(14) . . ? C4 C3 B3 112.3(12) . . ? C4 C3 B2 111.4(13) . . ? B3 C3 B2 63.7(11) . . ? C4 C3 B4 62.4(9) . . ? B3 C3 B4 62.2(11) . . ? B2 C3 B4 114.8(13) . . ? C4 C3 B1 61.5(9) . . ? B3 C3 B1 113.5(13) . . ? B2 C3 B1 61.0(10) . . ? B4 C3 B1 114.1(13) . . ? C4 C3 S1 112.3(9) . . ? B3 C3 S1 124.2(12) . . ? B2 C3 S1 124.7(12) . . ? B4 C3 S1 114.6(11) . . ? B1 C3 S1 116.5(10) . . ? C3 C4 B5 112.5(12) . . ? C3 C4 B6 111.4(12) . . ? B5 C4 B6 61.5(11) . . ? C3 C4 B1 62.4(9) . . ? B5 C4 B1 112.8(13) . . ? B6 C4 B1 61.3(10) . . ? C3 C4 B4 61.4(9) . . ? B5 C4 B4 63.5(11) . . ? B6 C4 B4 113.6(13) . . ? B1 C4 B4 114.0(12) . . ? C3 C4 S2 112.5(10) . . ? B5 C4 S2 124.3(11) . . ? B6 C4 S2 125.4(12) . . ? B1 C4 S2 116.2(10) . . ? B4 C4 S2 115.1(11) . . ? C6 C5 B13 109.9(11) . . ? C6 C5 B11 60.6(9) . . ? B13 C5 B11 109.7(11) . . ? C6 C5 B14 63.1(9) . . ? B13 C5 B14 60.4(10) . . ? B11 C5 B14 112.7(11) . . ? C6 C5 B12 108.1(11) . . ? B13 C5 B12 62.6(11) . . ? B11 C5 B12 58.4(9) . . ? B14 C5 B12 112.0(12) . . ? C6 C5 S3 117.6(10) . . ? B13 C5 S3 122.2(11) . . ? B11 C5 S3 121.3(10) . . ? B14 C5 S3 115.6(11) . . ? B12 C5 S3 124.6(10) . . ? C5 C6 B15 110.2(13) . . ? C5 C6 B16 111.4(11) . . ? B15 C6 B16 65.0(11) . . ? C5 C6 B11 62.0(9) . . ? B15 C6 B11 111.5(12) . . ? B16 C6 B11 59.3(10) . . ? C5 C6 B14 60.8(10) . . ? B15 C6 B14 61.0(10) . . ? B16 C6 B14 114.9(12) . . ? B11 C6 B14 112.0(12) . . ? C5 C6 S4 114.9(9) . . ? B15 C6 S4 123.0(11) . . ? B16 C6 S4 122.9(11) . . ? B11 C6 S4 119.5(9) . . ? B14 C6 S4 115.9(11) . . ? C11 C7 C8 109.0(13) . . ? C11 C7 C12 125.3(13) . . ? C8 C7 C12 125.4(14) . . ? C11 C7 Co1 70.0(8) . . ? C8 C7 Co1 71.7(8) . . ? C12 C7 Co1 128.8(10) . . ? C7 C8 C9 107.6(13) . . ? C7 C8 C13 126.2(15) . . ? C9 C8 C13 125.7(15) . . ? C7 C8 Co1 68.9(8) . . ? C9 C8 Co1 68.9(8) . . ? C13 C8 Co1 134.1(11) . . ? C8 C9 C10 108.6(12) . . ? C8 C9 C14 127.6(15) . . ? C10 C9 C14 123.5(16) . . ? C8 C9 Co1 71.3(9) . . ? C10 C9 Co1 71.3(8) . . ? C14 C9 Co1 128.0(9) . . ? C11 C10 C9 105.0(14) . . ? C11 C10 C15 130.5(14) . . ? C9 C10 C15 124.4(13) . . ? C11 C10 Co1 67.7(8) . . ? C9 C10 Co1 68.3(8) . . ? C15 C10 Co1 130.1(10) . . ? C7 C11 C10 109.6(14) . . ? C7 C11 C16 125.4(13) . . ? C10 C11 C16 124.3(15) . . ? C7 C11 Co1 70.8(8) . . ? C10 C11 Co1 71.8(8) . . ? C16 C11 Co1 131.2(10) . . ? O3 C17 W2 175.9(14) . . ? O4 C18 W2 174.2(14) . . ? C20 C19 B23 111.1(12) . . ? C20 C19 B24 60.8(9) . . ? B23 C19 B24 61.7(10) . . ? C20 C19 B21 61.3(10) . . ? B23 C19 B21 112.0(13) . . ? B24 C19 B21 111.4(13) . . ? C20 C19 B22 109.9(13) . . ? B23 C19 B22 61.9(10) . . ? B24 C19 B22 111.2(13) . . ? B21 C19 B22 60.7(11) . . ? C20 C19 S5 113.7(10) . . ? B23 C19 S5 125.7(12) . . ? B24 C19 S5 119.0(11) . . ? B21 C19 S5 115.7(10) . . ? B22 C19 S5 124.7(11) . . ? C19 C20 B25 110.8(12) . . ? C19 C20 B24 61.7(9) . . ? B25 C20 B24 59.2(10) . . ? C19 C20 B26 112.3(12) . . ? B25 C20 B26 65.2(11) . . ? B24 C20 B26 113.1(14) . . ? C19 C20 B21 61.7(9) . . ? B25 C20 B21 114.3(13) . . ? B24 C20 B21 112.5(13) . . ? B26 C20 B21 61.6(10) . . ? C19 C20 S6 111.1(10) . . ? B25 C20 S6 125.3(11) . . ? B24 C20 S6 116.6(11) . . ? B26 C20 S6 124.8(11) . . ? B21 C20 S6 115.8(11) . . ? C22 C21 B31 63.2(9) . . ? C22 C21 B32 110.9(12) . . ? B31 C21 B32 59.4(11) . . ? C22 C21 B33 110.7(12) . . ? B31 C21 B33 111.8(12) . . ? B32 C21 B33 63.3(11) . . ? C22 C21 B34 62.2(10) . . ? B31 C21 B34 115.2(11) . . ? B32 C21 B34 114.1(12) . . ? B33 C21 B34 61.2(11) . . ? C22 C21 S7 118.0(10) . . ? B31 C21 S7 119.9(11) . . ? B32 C21 S7 122.1(10) . . ? B33 C21 S7 120.1(10) . . ? B34 C21 S7 115.0(10) . . ? C21 C22 B36 112.5(12) . . ? C21 C22 B35 112.3(12) . . ? B36 C22 B35 63.3(11) . . ? C21 C22 B31 60.0(9) . . ? B36 C22 B31 62.9(10) . . ? B35 C22 B31 113.6(12) . . ? C21 C22 B34 62.4(10) . . ? B36 C22 B34 115.1(13) . . ? B35 C22 B34 62.1(10) . . ? B31 C22 B34 112.6(12) . . ? C21 C22 S8 115.3(9) . . ? B36 C22 S8 122.8(11) . . ? B35 C22 S8 120.5(11) . . ? B31 C22 S8 120.1(11) . . ? B34 C22 S8 113.8(10) . . ? C24 C23 C28 127.1(13) . . ? C24 C23 C27 106.5(12) . . ? C28 C23 C27 126.1(13) . . ? C24 C23 Co2 70.8(8) . . ? C28 C23 Co2 129.3(10) . . ? C27 C23 Co2 70.2(8) . . ? C23 C24 C25 108.4(13) . . ? C23 C24 C29 122.3(13) . . ? C25 C24 C29 129.1(14) . . ? C23 C24 Co2 69.2(8) . . ? C25 C24 Co2 70.0(8) . . ? C29 C24 Co2 130.0(10) . . ? C26 C25 C24 109.0(14) . . ? C26 C25 C30 124.7(13) . . ? C24 C25 C30 126.0(14) . . ? C26 C25 Co2 69.6(8) . . ? C24 C25 Co2 70.1(8) . . ? C30 C25 Co2 131.2(11) . . ? C27 C26 C25 108.2(13) . . ? C27 C26 C31 127.2(15) . . ? C25 C26 C31 124.3(15) . . ? C27 C26 Co2 71.0(8) . . ? C25 C26 Co2 70.5(8) . . ? C31 C26 Co2 128.6(10) . . ? C26 C27 C23 107.8(12) . . ? C26 C27 C32 127.1(13) . . ? C23 C27 C32 124.7(14) . . ? C26 C27 Co2 69.5(9) . . ? C23 C27 Co2 68.2(7) . . ? C32 C27 Co2 133.4(10) . . ? B17 B20 B15 106.9(13) . . ? B17 B20 B19 106.6(13) . . ? B15 B20 B19 59.4(11) . . ? B17 B20 B18 58.8(6) . . ? B15 B20 B18 106.3(14) . . ? B19 B20 B18 59.5(11) . . ? B17 B20 B16 58.6(6) . . ? B15 B20 B16 60.7(11) . . ? B19 B20 B16 107.4(14) . . ? B18 B20 B16 105.5(10) . . ? B37 B38 B33 109.7(12) . . ? B37 B38 B40 59.4(11) . . ? B33 B38 B40 107.7(12) . . ? B37 B38 B39 110.1(12) . . ? B33 B38 B39 60.5(11) . . ? B40 B38 B39 60.7(11) . . ? B37 B38 B32 59.4(10) . . ? B33 B38 B32 61.4(11) . . ? B40 B38 B32 106.0(13) . . ? B39 B38 B32 109.7(13) . . ? B20 B17 B18 63.2(10) . . ? B20 B17 B16 63.8(11) . . ? B18 B17 B16 113.0(12) . . ? B20 B17 B12 111.6(12) . . ? B18 B17 B12 61.5(10) . . ? B16 B17 B12 106.4(11) . . ? B20 B17 B11 108.5(11) . . ? B18 B17 B11 107.7(11) . . ? B16 B17 B11 57.1(9) . . ? B12 B17 B11 57.7(9) . . ? B31 B37 B40 105.9(14) . . ? B31 B37 B32 58.0(10) . . ? B40 B37 B32 108.0(11) . . ? B31 B37 B38 106.6(12) . . ? B40 B37 B38 60.6(7) . . ? B32 B37 B38 60.8(6) . . ? B31 B37 B36 59.5(10) . . ? B40 B37 B36 58.3(11) . . ? B32 B37 B36 106.0(14) . . ? B38 B37 B36 106.8(13) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.418 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.195 # Attachment '9b_bi_CpstarSeW_f60401c.cif' data_f60401cs _database_code_depnum_ccdc_archive 'CCDC 621987' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H35 B20 Co O2 Se4 W' _chemical_formula_weight 1034.26 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' Se Se -0.0929 2.2259 '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' W W -0.8490 6.8722 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.095(7) _cell_length_b 13.725(8) _cell_length_c 14.006(8) _cell_angle_alpha 72.538(7) _cell_angle_beta 68.770(7) _cell_angle_gamma 66.640(7) _cell_volume 1956.1(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 897 _cell_measurement_theta_min 3.225 _cell_measurement_theta_max 26.875 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 7.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2698 _exptl_absorpt_correction_T_max 0.5370 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.48 _diffrn_reflns_number 8216 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6794 _reflns_number_gt 5298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^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 6794 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.67433(8) 0.38516(8) 0.73796(7) 0.0315(2) Uani 1 1 d . . . W1 W 0.51972(2) 0.59023(2) 0.72050(2) 0.03082(11) Uani 1 1 d . . . O1 O 0.7418(5) 0.6032(5) 0.5201(5) 0.0623(17) Uani 1 1 d . . . O2 O 0.7159(6) 0.5910(5) 0.8159(5) 0.0628(17) Uani 1 1 d . . . Se1 Se 0.50420(6) 0.43714(6) 0.88206(5) 0.03241(18) Uani 1 1 d . . . Se2 Se 0.52720(6) 0.43517(6) 0.64637(5) 0.03491(19) Uani 1 1 d . . . Se4 Se 0.41139(7) 0.72042(6) 0.58888(6) 0.0454(2) Uani 1 1 d . . . Se5 Se 0.40062(7) 0.72695(6) 0.83496(6) 0.0427(2) Uani 1 1 d . . . C1 C 0.3771(6) 0.3906(6) 0.8692(6) 0.0362(17) Uani 1 1 d . . . C2 C 0.3888(6) 0.3883(6) 0.7503(6) 0.0368(17) Uani 1 1 d . . . C3 C 0.6640(7) 0.5943(6) 0.5903(6) 0.0411(19) Uani 1 1 d . . . C4 C 0.6454(7) 0.5859(6) 0.7826(6) 0.0411(19) Uani 1 1 d . . . C5 C 0.8675(6) 0.3640(6) 0.6938(6) 0.0398(19) Uani 1 1 d . . . C6 C 0.8386(7) 0.3169(6) 0.6328(6) 0.044(2) Uani 1 1 d . . . C7 C 0.7844(6) 0.2347(6) 0.6977(6) 0.0381(18) Uani 1 1 d . . . C8 C 0.7772(6) 0.2331(6) 0.8005(6) 0.0367(18) Uani 1 1 d . . . C9 C 0.8256(6) 0.3128(6) 0.8005(6) 0.0410(19) Uani 1 1 d . . . C10 C 0.9393(7) 0.4385(7) 0.6568(7) 0.059(3) Uani 1 1 d . . . H10A H 1.0272 0.3990 0.6357 0.088 Uiso 1 1 calc R . . H10B H 0.9231 0.4747 0.7119 0.088 Uiso 1 1 calc R . . H10C H 0.9151 0.4909 0.5986 0.088 Uiso 1 1 calc R . . C11 C 0.8690(8) 0.3391(7) 0.5146(6) 0.063(3) Uani 1 1 d . . . H11A H 0.8813 0.4083 0.4874 0.094 Uiso 1 1 calc R . . H11B H 0.8009 0.3391 0.4949 0.094 Uiso 1 1 calc R . . H11C H 0.9441 0.2841 0.4870 0.094 Uiso 1 1 calc R . . C12 C 0.7553(8) 0.1615(7) 0.6605(7) 0.057(2) Uani 1 1 d . . . H12A H 0.8318 0.1136 0.6244 0.085 Uiso 1 1 calc R . . H12B H 0.7042 0.2026 0.6138 0.085 Uiso 1 1 calc R . . H12C H 0.7109 0.1202 0.7187 0.085 Uiso 1 1 calc R . . C13 C 0.7423(7) 0.1550(6) 0.8947(6) 0.050(2) Uani 1 1 d . . . H13A H 0.7051 0.1132 0.8797 0.075 Uiso 1 1 calc R . . H13B H 0.6832 0.1931 0.9496 0.075 Uiso 1 1 calc R . . H13C H 0.8159 0.1078 0.9162 0.075 Uiso 1 1 calc R . . C14 C 0.8429(7) 0.3316(7) 0.8946(6) 0.048(2) Uani 1 1 d . . . H14A H 0.7661 0.3396 0.9497 0.072 Uiso 1 1 calc R . . H14B H 0.8652 0.3959 0.8762 0.072 Uiso 1 1 calc R . . H14C H 0.9083 0.2711 0.9175 0.072 Uiso 1 1 calc R . . C15 C 0.2964(7) 0.8520(6) 0.7636(6) 0.0420(19) Uani 1 1 d . . . C16 C 0.3007(7) 0.8495(6) 0.6462(6) 0.044(2) Uani 1 1 d . . . B3 B 0.2678(8) 0.4898(8) 0.8086(7) 0.043(2) Uani 1 1 d . . . H3 H 0.2582 0.5762 0.7853 0.052 Uiso 1 1 calc R . . B4 B 0.2221(8) 0.4238(9) 0.9452(7) 0.050(3) Uani 1 1 d . . . H4 H 0.1827 0.4681 1.0101 0.060 Uiso 1 1 calc R . . B5 B 0.3253(9) 0.2902(9) 0.9559(8) 0.053(3) Uani 1 1 d . . . H5 H 0.3526 0.2489 1.0284 0.063 Uiso 1 1 calc R . . B6 B 0.4309(9) 0.2654(8) 0.8331(7) 0.046(2) Uani 1 1 d . . . H6 H 0.5263 0.2076 0.8260 0.055 Uiso 1 1 calc R . . B7 B 0.2475(8) 0.4185(9) 0.7323(9) 0.053(3) Uani 1 1 d . . . H7 H 0.2229 0.4599 0.6588 0.064 Uiso 1 1 calc R . . B8 B 0.1389(9) 0.4400(9) 0.8569(9) 0.058(3) Uani 1 1 d . . . H8 H 0.0423 0.4956 0.8651 0.070 Uiso 1 1 calc R . . B9 B 0.1735(10) 0.3208(9) 0.9464(9) 0.060(3) Uani 1 1 d . . . H9 H 0.0996 0.2981 1.0131 0.072 Uiso 1 1 calc R . . B10 B 0.3041(10) 0.2231(9) 0.8764(9) 0.059(3) Uani 1 1 d . . . H10 H 0.3146 0.1365 0.8978 0.071 Uiso 1 1 calc R . . B11 B 0.3500(9) 0.2858(8) 0.7454(8) 0.050(3) Uani 1 1 d . . . H11 H 0.3931 0.2419 0.6800 0.060 Uiso 1 1 calc R . . B12 B 0.1895(10) 0.3165(10) 0.8152(9) 0.068(3) Uani 1 1 d . . . H12 H 0.1255 0.2909 0.7964 0.082 Uiso 1 1 calc R . . B13 B 0.1684(8) 0.8386(8) 0.7466(8) 0.050(2) Uani 1 1 d . . . H13 H 0.1401 0.7657 0.7769 0.060 Uiso 1 1 calc R . . B14 B 0.1574(9) 0.9179(9) 0.6232(8) 0.062(3) Uani 1 1 d . . . H14 H 0.1213 0.8970 0.5730 0.075 Uiso 1 1 calc R . . B15 B 0.2790(11) 0.9703(8) 0.5695(9) 0.067(3) Uani 1 1 d . . . H15 H 0.3217 0.9829 0.4848 0.081 Uiso 1 1 calc R . . B16 B 0.3699(11) 0.9305(8) 0.6584(9) 0.067(3) Uani 1 1 d . . . H16 H 0.4712 0.9181 0.6326 0.080 Uiso 1 1 calc R . . B17 B 0.1491(9) 0.9233(8) 0.8291(8) 0.054(3) Uani 1 1 d . . . H17 H 0.1084 0.9056 0.9139 0.065 Uiso 1 1 calc R . . B18 B 0.0586(10) 0.9684(9) 0.7398(9) 0.061(3) Uani 1 1 d . . . H18 H -0.0429 0.9818 0.7663 0.073 Uiso 1 1 calc R . . B19 B 0.1262(11) 1.0501(9) 0.6294(10) 0.073(4) Uani 1 1 d . . . H19 H 0.0684 1.1176 0.5838 0.087 Uiso 1 1 calc R . . B20 B 0.2600(12) 1.0601(9) 0.6488(12) 0.088(4) Uani 1 1 d . . . H20 H 0.2888 1.1327 0.6160 0.105 Uiso 1 1 calc R . . B21 B 0.2723(11) 0.9789(8) 0.7759(10) 0.069(3) Uani 1 1 d . . . H21 H 0.3101 0.9979 0.8262 0.082 Uiso 1 1 calc R . . B22 B 0.1203(11) 1.0545(9) 0.7579(11) 0.077(4) Uani 1 1 d . . . H22 H 0.0591 1.1244 0.7960 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0288(5) 0.0312(5) 0.0319(5) -0.0072(4) -0.0111(4) -0.0038(4) W1 0.03042(16) 0.02793(17) 0.03224(17) -0.00754(12) -0.01127(12) -0.00376(12) O1 0.050(4) 0.066(4) 0.048(4) -0.006(3) 0.005(3) -0.015(3) O2 0.065(4) 0.065(4) 0.082(5) -0.023(3) -0.037(4) -0.023(3) Se1 0.0340(4) 0.0355(4) 0.0315(4) -0.0083(3) -0.0124(3) -0.0106(3) Se2 0.0366(4) 0.0347(4) 0.0336(4) -0.0116(3) -0.0139(3) -0.0039(3) Se4 0.0506(5) 0.0391(5) 0.0372(4) -0.0106(4) -0.0203(4) 0.0046(4) Se5 0.0458(4) 0.0388(5) 0.0419(4) -0.0168(4) -0.0181(4) 0.0000(4) C1 0.029(4) 0.037(4) 0.043(4) -0.010(4) -0.011(3) -0.009(3) C2 0.032(4) 0.041(5) 0.039(4) -0.013(4) -0.011(3) -0.008(3) C3 0.034(4) 0.038(5) 0.043(5) -0.005(4) -0.012(4) -0.004(3) C4 0.042(4) 0.033(4) 0.045(5) -0.007(4) -0.012(4) -0.010(4) C5 0.025(4) 0.047(5) 0.038(4) -0.005(4) -0.009(3) -0.005(3) C6 0.034(4) 0.044(5) 0.036(4) -0.008(4) -0.011(3) 0.006(4) C7 0.033(4) 0.032(4) 0.039(4) -0.015(4) -0.011(3) 0.006(3) C8 0.033(4) 0.029(4) 0.047(5) -0.006(4) -0.019(3) -0.003(3) C9 0.025(4) 0.041(5) 0.044(5) -0.010(4) -0.009(3) 0.005(3) C10 0.036(4) 0.076(7) 0.056(5) 0.005(5) -0.013(4) -0.023(4) C11 0.065(6) 0.056(6) 0.040(5) -0.005(4) -0.014(4) 0.004(5) C12 0.060(5) 0.043(5) 0.053(5) -0.021(4) -0.024(4) 0.014(4) C13 0.048(5) 0.039(5) 0.051(5) -0.006(4) -0.017(4) -0.002(4) C14 0.042(4) 0.061(6) 0.042(5) -0.011(4) -0.014(4) -0.016(4) C15 0.046(4) 0.033(4) 0.050(5) -0.016(4) -0.016(4) -0.008(4) C16 0.045(4) 0.036(5) 0.041(5) -0.002(4) -0.021(4) 0.002(4) B3 0.034(4) 0.048(6) 0.050(6) -0.022(5) -0.017(4) 0.000(4) B4 0.033(5) 0.072(7) 0.045(6) -0.018(5) 0.000(4) -0.022(5) B5 0.062(6) 0.059(7) 0.044(6) -0.004(5) -0.009(5) -0.037(5) B6 0.048(5) 0.040(5) 0.053(6) -0.009(5) -0.023(5) -0.011(4) B7 0.044(5) 0.068(7) 0.067(7) -0.021(6) -0.030(5) -0.018(5) B8 0.033(5) 0.078(8) 0.073(7) -0.031(6) -0.012(5) -0.016(5) B9 0.057(6) 0.075(8) 0.060(7) -0.017(6) -0.009(5) -0.035(6) B10 0.067(7) 0.055(7) 0.071(7) -0.009(6) -0.026(6) -0.032(6) B11 0.049(5) 0.050(6) 0.069(7) -0.029(5) -0.016(5) -0.022(5) B12 0.061(7) 0.089(9) 0.081(8) -0.028(7) -0.025(6) -0.038(6) B13 0.034(5) 0.046(6) 0.063(6) -0.016(5) -0.016(5) -0.001(4) B14 0.052(6) 0.053(7) 0.063(7) -0.015(6) -0.030(5) 0.016(5) B15 0.081(8) 0.039(6) 0.065(7) 0.008(5) -0.029(6) -0.008(6) B16 0.061(7) 0.038(6) 0.081(8) -0.004(6) -0.014(6) -0.005(5) B17 0.048(5) 0.051(6) 0.056(6) -0.024(5) -0.018(5) 0.004(5) B18 0.054(6) 0.051(6) 0.071(7) -0.022(6) -0.031(6) 0.009(5) B19 0.077(8) 0.040(6) 0.085(9) -0.009(6) -0.038(7) 0.009(6) B20 0.086(9) 0.034(6) 0.125(12) -0.005(7) -0.036(9) -0.002(6) B21 0.083(8) 0.038(6) 0.098(9) -0.033(6) -0.041(7) -0.004(6) B22 0.072(8) 0.041(6) 0.114(11) -0.037(7) -0.039(8) 0.014(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C6 2.056(7) . ? Co1 C9 2.073(7) . ? Co1 C8 2.074(7) . ? Co1 C7 2.080(7) . ? Co1 C5 2.109(7) . ? Co1 Se2 2.3324(15) . ? Co1 Se1 2.3472(14) . ? Co1 W1 2.6875(16) . ? W1 C4 1.981(9) . ? W1 C3 2.021(8) . ? W1 Se5 2.4811(13) . ? W1 Se4 2.4948(12) . ? W1 Se2 2.5924(14) . ? W1 Se1 2.5927(13) . ? O1 C3 1.103(8) . ? O2 C4 1.142(9) . ? Se1 C1 1.963(7) . ? Se2 C2 1.965(7) . ? Se4 C16 1.942(8) . ? Se5 C15 1.923(8) . ? C1 C2 1.629(10) . ? C1 B5 1.702(12) . ? C1 B3 1.736(11) . ? C1 B4 1.739(10) . ? C1 B6 1.740(12) . ? C2 B11 1.677(12) . ? C2 B7 1.686(11) . ? C2 B3 1.718(11) . ? C2 B6 1.739(12) . ? C5 C6 1.413(11) . ? C5 C9 1.444(10) . ? C5 C10 1.460(11) . ? C6 C7 1.438(11) . ? C6 C11 1.521(10) . ? C7 C8 1.405(10) . ? C7 C12 1.460(11) . ? C8 C9 1.431(11) . ? C8 C13 1.475(10) . ? C9 C14 1.514(11) . ? 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 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.636(11) . ? C15 B21 1.700(12) . ? C15 B17 1.717(11) . ? C15 B16 1.726(14) . ? C15 B13 1.735(12) . ? C16 B15 1.662(13) . ? C16 B16 1.709(15) . ? C16 B14 1.710(12) . ? C16 B13 1.730(12) . ? B3 B8 1.778(14) . ? B3 B7 1.780(13) . ? B3 B4 1.838(14) . ? B3 H3 1.1000 . ? B4 B9 1.727(15) . ? B4 B5 1.761(15) . ? B4 B8 1.775(14) . ? B4 H4 1.1000 . ? B5 B9 1.760(14) . ? B5 B6 1.767(14) . ? B5 B10 1.779(15) . ? B5 H5 1.1000 . ? B6 B10 1.697(14) . ? B6 B11 1.729(13) . ? B6 H6 1.1000 . ? B7 B12 1.735(16) . ? B7 B11 1.749(14) . ? B7 B8 1.788(15) . ? B7 H7 1.1000 . ? B8 B9 1.740(16) . ? B8 B12 1.761(16) . ? B8 H8 1.1000 . ? B9 B12 1.794(16) . ? B9 B10 1.801(15) . ? B9 H9 1.1000 . ? B10 B12 1.758(16) . ? B10 B11 1.763(15) . ? B10 H10 1.1000 . ? B11 B12 1.767(14) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? B13 B18 1.750(13) . ? B13 B14 1.765(15) . ? B13 B17 1.772(14) . ? B13 H13 1.1000 . ? B14 B15 1.721(17) . ? B14 B19 1.723(16) . ? B14 B18 1.785(14) . ? B14 H14 1.1000 . ? B15 B19 1.772(16) . ? B15 B16 1.779(17) . ? B15 B20 1.793(19) . ? B15 H15 1.1000 . ? B16 B20 1.750(15) . ? B16 B21 1.780(16) . ? B16 H16 1.1000 . ? B17 B22 1.742(16) . ? B17 B21 1.765(17) . ? B17 B18 1.771(14) . ? B17 H17 1.1000 . ? B18 B22 1.743(17) . ? B18 B19 1.757(17) . ? B18 H18 1.1000 . ? B19 B22 1.795(18) . ? B19 B20 1.797(19) . ? B19 H19 1.1000 . ? B20 B21 1.818(18) . ? B20 B22 1.833(19) . ? B20 H20 1.1000 . ? B21 B22 1.785(16) . ? B21 H21 1.1000 . ? B22 H22 1.1000 . ? 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 C6 Co1 C9 67.1(3) . . ? C6 Co1 C8 66.9(3) . . ? C9 Co1 C8 40.4(3) . . ? C6 Co1 C7 40.7(3) . . ? C9 Co1 C7 67.6(3) . . ? C8 Co1 C7 39.5(3) . . ? C6 Co1 C5 39.6(3) . . ? C9 Co1 C5 40.4(3) . . ? C8 Co1 C5 67.6(3) . . ? C7 Co1 C5 67.9(3) . . ? C6 Co1 Se2 102.1(2) . . ? C9 Co1 Se2 167.1(2) . . ? C8 Co1 Se2 130.1(2) . . ? C7 Co1 Se2 99.7(2) . . ? C5 Co1 Se2 134.1(2) . . ? C6 Co1 Se1 168.9(2) . . ? C9 Co1 Se1 103.1(2) . . ? C8 Co1 Se1 102.4(2) . . ? C7 Co1 Se1 132.0(2) . . ? C5 Co1 Se1 135.1(2) . . ? Se2 Co1 Se1 86.90(6) . . ? C6 Co1 W1 128.4(2) . . ? C9 Co1 W1 130.2(2) . . ? C8 Co1 W1 161.6(2) . . ? C7 Co1 W1 158.6(2) . . ? C5 Co1 W1 116.2(2) . . ? Se2 Co1 W1 61.71(3) . . ? Se1 Co1 W1 61.55(3) . . ? C4 W1 C3 80.7(3) . . ? C4 W1 Se5 76.5(2) . . ? C3 W1 Se5 128.2(2) . . ? C4 W1 Se4 135.4(2) . . ? C3 W1 Se4 77.7(2) . . ? Se5 W1 Se4 87.11(5) . . ? C4 W1 Se2 125.8(2) . . ? C3 W1 Se2 80.2(2) . . ? Se5 W1 Se2 149.11(3) . . ? Se4 W1 Se2 88.09(5) . . ? C4 W1 Se1 77.1(2) . . ? C3 W1 Se1 128.9(2) . . ? Se5 W1 Se1 90.09(5) . . ? Se4 W1 Se1 144.93(4) . . ? Se2 W1 Se1 76.73(5) . . ? C4 W1 Co1 74.0(2) . . ? C3 W1 Co1 77.1(2) . . ? Se5 W1 Co1 136.57(4) . . ? Se4 W1 Co1 135.96(3) . . ? Se2 W1 Co1 52.39(4) . . ? Se1 W1 Co1 52.75(3) . . ? C1 Se1 Co1 102.8(2) . . ? C1 Se1 W1 101.2(2) . . ? Co1 Se1 W1 65.70(4) . . ? C2 Se2 Co1 103.3(2) . . ? C2 Se2 W1 101.8(2) . . ? Co1 Se2 W1 65.90(4) . . ? C16 Se4 W1 108.4(2) . . ? C15 Se5 W1 109.2(2) . . ? C2 C1 B5 111.6(6) . . ? C2 C1 B3 61.3(4) . . ? B5 C1 B3 114.8(6) . . ? C2 C1 B4 111.9(6) . . ? B5 C1 B4 61.6(5) . . ? B3 C1 B4 63.9(5) . . ? C2 C1 B6 62.0(5) . . ? B5 C1 B6 61.8(5) . . ? B3 C1 B6 114.4(6) . . ? B4 C1 B6 112.8(6) . . ? C2 C1 Se1 114.5(5) . . ? B5 C1 Se1 123.2(5) . . ? B3 C1 Se1 115.5(5) . . ? B4 C1 Se1 123.8(5) . . ? B6 C1 Se1 116.0(5) . . ? C1 C2 B11 111.5(6) . . ? C1 C2 B7 111.8(6) . . ? B11 C2 B7 62.7(6) . . ? C1 C2 B3 62.4(5) . . ? B11 C2 B3 115.7(6) . . ? B7 C2 B3 63.1(5) . . ? C1 C2 B6 62.1(5) . . ? B11 C2 B6 60.8(5) . . ? B7 C2 B6 112.6(7) . . ? B3 C2 B6 115.4(6) . . ? C1 C2 Se2 113.3(5) . . ? B11 C2 Se2 123.9(5) . . ? B7 C2 Se2 124.4(6) . . ? B3 C2 Se2 114.1(5) . . ? B6 C2 Se2 116.3(5) . . ? O1 C3 W1 175.3(7) . . ? O2 C4 W1 175.2(7) . . ? C6 C5 C9 106.0(7) . . ? C6 C5 C10 127.4(7) . . ? C9 C5 C10 126.2(8) . . ? C6 C5 Co1 68.2(4) . . ? C9 C5 Co1 68.5(4) . . ? C10 C5 Co1 133.6(6) . . ? C5 C6 C7 110.4(7) . . ? C5 C6 C11 126.9(8) . . ? C7 C6 C11 122.6(8) . . ? C5 C6 Co1 72.2(4) . . ? C7 C6 Co1 70.6(4) . . ? C11 C6 Co1 128.1(5) . . ? C8 C7 C6 106.4(7) . . ? C8 C7 C12 127.8(8) . . ? C6 C7 C12 125.5(7) . . ? C8 C7 Co1 70.0(4) . . ? C6 C7 Co1 68.8(4) . . ? C12 C7 Co1 130.5(5) . . ? C7 C8 C9 109.2(7) . . ? C7 C8 C13 127.7(7) . . ? C9 C8 C13 122.7(7) . . ? C7 C8 Co1 70.5(4) . . ? C9 C8 Co1 69.8(4) . . ? C13 C8 Co1 131.9(5) . . ? C8 C9 C5 108.0(7) . . ? C8 C9 C14 125.8(7) . . ? C5 C9 C14 125.9(7) . . ? C8 C9 Co1 69.9(4) . . ? C5 C9 Co1 71.1(4) . . ? C14 C9 Co1 129.6(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 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 B21 111.1(7) . . ? C16 C15 B17 110.9(6) . . ? B21 C15 B17 62.2(6) . . ? C16 C15 B16 61.0(6) . . ? B21 C15 B16 62.6(6) . . ? B17 C15 B16 113.6(7) . . ? C16 C15 B13 61.7(5) . . ? B21 C15 B13 113.2(7) . . ? B17 C15 B13 61.8(5) . . ? B16 C15 B13 113.6(7) . . ? C16 C15 Se5 117.8(5) . . ? B21 C15 Se5 121.5(6) . . ? B17 C15 Se5 121.2(6) . . ? B16 C15 Se5 117.6(5) . . ? B13 C15 Se5 117.0(5) . . ? C15 C16 B15 113.0(7) . . ? C15 C16 B16 62.1(6) . . ? B15 C16 B16 63.7(7) . . ? C15 C16 B14 111.4(6) . . ? B15 C16 B14 61.3(6) . . ? B16 C16 B14 113.8(7) . . ? C15 C16 B13 62.0(5) . . ? B15 C16 B13 113.3(7) . . ? B16 C16 B13 114.7(7) . . ? B14 C16 B13 61.7(5) . . ? C15 C16 Se4 117.5(5) . . ? B15 C16 Se4 120.4(6) . . ? B16 C16 Se4 116.9(6) . . ? B14 C16 Se4 121.1(6) . . ? B13 C16 Se4 117.0(6) . . ? C2 B3 C1 56.3(4) . . ? C2 B3 B8 103.5(7) . . ? C1 B3 B8 102.7(7) . . ? C2 B3 B7 57.6(5) . . ? C1 B3 B7 102.7(6) . . ? B8 B3 B7 60.3(6) . . ? C2 B3 B4 103.4(7) . . ? C1 B3 B4 58.2(5) . . ? B8 B3 B4 58.8(6) . . ? B7 B3 B4 106.8(7) . . ? C2 B3 H3 125.4 . . ? C1 B3 H3 125.8 . . ? B8 B3 H3 123.8 . . ? B7 B3 H3 122.9 . . ? B4 B3 H3 122.9 . . ? B9 B4 C1 104.1(7) . . ? B9 B4 B5 60.6(6) . . ? C1 B4 B5 58.2(5) . . ? B9 B4 B8 59.6(6) . . ? C1 B4 B8 102.7(6) . . ? B5 B4 B8 107.3(8) . . ? B9 B4 B3 107.1(7) . . ? C1 B4 B3 58.0(4) . . ? B5 B4 B3 107.1(6) . . ? B8 B4 B3 59.0(5) . . ? B9 B4 H4 122.3 . . ? C1 B4 H4 125.7 . . ? B5 B4 H4 121.5 . . ? B8 B4 H4 123.5 . . ? B3 B4 H4 122.3 . . ? C1 B5 B9 104.3(7) . . ? C1 B5 B4 60.2(5) . . ? B9 B5 B4 58.7(6) . . ? C1 B5 B6 60.2(5) . . ? B9 B5 B6 107.2(7) . . ? B4 B5 B6 110.4(7) . . ? C1 B5 B10 103.6(7) . . ? B9 B5 B10 61.2(6) . . ? B4 B5 B10 108.4(8) . . ? B6 B5 B10 57.2(6) . . ? C1 B5 H5 124.3 . . ? B9 B5 H5 123.0 . . ? B4 B5 H5 120.3 . . ? B6 B5 H5 121.3 . . ? B10 B5 H5 123.3 . . ? B10 B6 B11 61.9(6) . . ? B10 B6 C2 105.1(7) . . ? B11 B6 C2 57.8(5) . . ? B10 B6 C1 105.5(7) . . ? B11 B6 C1 103.9(6) . . ? C2 B6 C1 55.8(4) . . ? B10 B6 B5 61.8(6) . . ? B11 B6 B5 110.4(7) . . ? C2 B6 B5 103.6(6) . . ? C1 B6 B5 58.1(5) . . ? B10 B6 H6 121.3 . . ? B11 B6 H6 121.3 . . ? C2 B6 H6 125.9 . . ? C1 B6 H6 125.5 . . ? B5 B6 H6 121.4 . . ? C2 B7 B12 105.0(7) . . ? C2 B7 B11 58.4(5) . . ? B12 B7 B11 60.9(6) . . ? C2 B7 B3 59.3(5) . . ? B12 B7 B3 108.7(8) . . ? B11 B7 B3 109.0(6) . . ? C2 B7 B8 104.4(7) . . ? B12 B7 B8 59.9(6) . . ? B11 B7 B8 108.5(8) . . ? B3 B7 B8 59.8(6) . . ? C2 B7 H7 124.9 . . ? B12 B7 H7 121.9 . . ? B11 B7 H7 120.8 . . ? B3 B7 H7 120.9 . . ? B8 B7 H7 122.7 . . ? B9 B8 B12 61.7(7) . . ? B9 B8 B4 58.8(6) . . ? B12 B8 B4 108.5(8) . . ? B9 B8 B3 109.2(7) . . ? B12 B8 B3 107.6(7) . . ? B4 B8 B3 62.3(5) . . ? B9 B8 B7 108.3(8) . . ? B12 B8 B7 58.5(6) . . ? B4 B8 B7 109.2(6) . . ? B3 B8 B7 59.9(5) . . ? B9 B8 H8 121.2 . . ? B12 B8 H8 121.9 . . ? B4 B8 H8 120.9 . . ? B3 B8 H8 120.9 . . ? B7 B8 H8 122.0 . . ? B4 B9 B8 61.6(6) . . ? B4 B9 B5 60.7(6) . . ? B8 B9 B5 108.9(7) . . ? B4 B9 B12 109.1(8) . . ? B8 B9 B12 59.7(6) . . ? B5 B9 B12 107.0(7) . . ? B4 B9 B10 108.9(7) . . ? B8 B9 B10 107.1(8) . . ? B5 B9 B10 59.9(6) . . ? B12 B9 B10 58.5(6) . . ? B4 B9 H9 120.1 . . ? B8 B9 H9 121.3 . . ? B5 B9 H9 121.7 . . ? B12 B9 H9 122.5 . . ? B10 B9 H9 122.4 . . ? B6 B10 B12 108.6(8) . . ? B6 B10 B11 59.9(6) . . ? B12 B10 B11 60.3(6) . . ? B6 B10 B5 61.0(6) . . ? B12 B10 B5 107.7(8) . . ? B11 B10 B5 108.3(7) . . ? B6 B10 B9 108.4(8) . . ? B12 B10 B9 60.5(6) . . ? B11 B10 B9 108.4(8) . . ? B5 B10 B9 58.9(6) . . ? B6 B10 H10 121.1 . . ? B12 B10 H10 121.4 . . ? B11 B10 H10 121.5 . . ? B5 B10 H10 121.9 . . ? B9 B10 H10 121.8 . . ? C2 B11 B6 61.4(5) . . ? C2 B11 B7 58.9(5) . . ? B6 B11 B7 109.9(7) . . ? C2 B11 B10 105.0(7) . . ? B6 B11 B10 58.2(6) . . ? B7 B11 B10 107.6(7) . . ? C2 B11 B12 104.0(7) . . ? B6 B11 B12 106.8(7) . . ? B7 B11 B12 59.1(6) . . ? B10 B11 B12 59.7(6) . . ? C2 B11 H11 123.8 . . ? B6 B11 H11 120.8 . . ? B7 B11 H11 121.1 . . ? B10 B11 H11 123.2 . . ? B12 B11 H11 123.6 . . ? B7 B12 B10 108.4(7) . . ? B7 B12 B8 61.5(6) . . ? B10 B12 B8 108.1(8) . . ? B7 B12 B11 59.9(6) . . ? B10 B12 B11 60.0(6) . . ? B8 B12 B11 108.9(8) . . ? B7 B12 B9 108.3(8) . . ? B10 B12 B9 60.9(6) . . ? B8 B12 B9 58.6(6) . . ? B11 B12 B9 108.5(8) . . ? B7 B12 H12 121.1 . . ? B10 B12 H12 121.4 . . ? B8 B12 H12 121.5 . . ? B11 B12 H12 121.4 . . ? B9 B12 H12 121.8 . . ? C16 B13 C15 56.4(5) . . ? C16 B13 B18 105.5(7) . . ? C15 B13 B18 105.3(7) . . ? C16 B13 B14 58.6(5) . . ? C15 B13 B14 104.3(8) . . ? B18 B13 B14 61.0(6) . . ? C16 B13 B17 104.2(7) . . ? C15 B13 B17 58.6(5) . . ? B18 B13 B17 60.4(6) . . ? B14 B13 B17 108.6(8) . . ? C16 B13 H13 124.9 . . ? C15 B13 H13 124.9 . . ? B18 B13 H13 122.0 . . ? B14 B13 H13 121.8 . . ? B17 B13 H13 122.1 . . ? C16 B14 B15 58.0(6) . . ? C16 B14 B19 105.3(9) . . ? B15 B14 B19 61.9(7) . . ? C16 B14 B13 59.7(5) . . ? B15 B14 B13 108.8(8) . . ? B19 B14 B13 107.9(8) . . ? C16 B14 B18 104.8(7) . . ? B15 B14 B18 109.6(9) . . ? B19 B14 B18 60.1(7) . . ? B13 B14 B18 59.1(6) . . ? C16 B14 H14 124.8 . . ? B15 B14 H14 120.3 . . ? B19 B14 H14 121.7 . . ? B13 B14 H14 121.5 . . ? B18 B14 H14 122.3 . . ? C16 B15 B14 60.7(6) . . ? C16 B15 B19 105.2(8) . . ? B14 B15 B19 59.1(7) . . ? C16 B15 B16 59.4(6) . . ? B14 B15 B16 109.9(8) . . ? B19 B15 B16 107.3(9) . . ? C16 B15 B20 105.0(8) . . ? B14 B15 B20 108.6(9) . . ? B19 B15 B20 60.5(7) . . ? B16 B15 B20 58.7(7) . . ? C16 B15 H15 123.7 . . ? B14 B15 H15 120.3 . . ? B19 B15 H15 122.9 . . ? B16 B15 H15 121.5 . . ? B20 B15 H15 122.6 . . ? C16 B16 C15 56.9(5) . . ? C16 B16 B20 104.9(8) . . ? C15 B16 B20 105.9(8) . . ? C16 B16 B15 56.9(6) . . ? C15 B16 B15 103.4(8) . . ? B20 B16 B15 61.1(7) . . ? C16 B16 B21 104.1(8) . . ? C15 B16 B21 58.0(6) . . ? B20 B16 B21 62.0(7) . . ? B15 B16 B21 109.0(8) . . ? C16 B16 H16 125.6 . . ? C15 B16 H16 125.0 . . ? B20 B16 H16 121.3 . . ? B15 B16 H16 122.6 . . ? B21 B16 H16 121.5 . . ? C15 B17 B22 105.3(8) . . ? C15 B17 B21 58.4(5) . . ? B22 B17 B21 61.2(7) . . ? C15 B17 B18 105.1(7) . . ? B22 B17 B18 59.5(6) . . ? B21 B17 B18 108.6(9) . . ? C15 B17 B13 59.6(5) . . ? B22 B17 B13 107.2(8) . . ? B21 B17 B13 108.4(7) . . ? B18 B17 B13 59.2(6) . . ? C15 B17 H17 124.2 . . ? B22 B17 H17 122.3 . . ? B21 B17 H17 120.9 . . ? B18 B17 H17 122.6 . . ? B13 B17 H17 121.8 . . ? B22 B18 B13 108.1(8) . . ? B22 B18 B19 61.7(8) . . ? B13 B18 B19 107.0(7) . . ? B22 B18 B17 59.4(7) . . ? B13 B18 B17 60.4(5) . . ? B19 B18 B17 108.4(9) . . ? B22 B18 B14 107.8(9) . . ? B13 B18 B14 59.9(6) . . ? B19 B18 B14 58.2(6) . . ? B17 B18 B14 107.7(7) . . ? B22 B18 H18 121.2 . . ? B13 B18 H18 121.9 . . ? B19 B18 H18 121.9 . . ? B17 B18 H18 121.6 . . ? B14 B18 H18 122.6 . . ? B14 B19 B18 61.7(7) . . ? B14 B19 B15 59.0(6) . . ? B18 B19 B15 108.6(8) . . ? B14 B19 B22 108.2(8) . . ? B18 B19 B22 58.8(7) . . ? B15 B19 B22 108.6(8) . . ? B14 B19 B20 108.3(8) . . ? B18 B19 B20 108.9(9) . . ? B15 B19 B20 60.3(7) . . ? B22 B19 B20 61.4(8) . . ? B14 B19 H19 121.5 . . ? B18 B19 H19 121.2 . . ? B15 B19 H19 121.8 . . ? B22 B19 H19 121.6 . . ? B20 B19 H19 120.8 . . ? B16 B20 B15 60.3(7) . . ? B16 B20 B19 107.5(9) . . ? B15 B20 B19 59.2(7) . . ? B16 B20 B21 59.8(6) . . ? B15 B20 B21 106.8(8) . . ? B19 B20 B21 106.1(9) . . ? B16 B20 B22 106.6(8) . . ? B15 B20 B22 106.0(9) . . ? B19 B20 B22 59.2(7) . . ? B21 B20 B22 58.5(7) . . ? B16 B20 H20 121.7 . . ? B15 B20 H20 122.5 . . ? B19 B20 H20 122.5 . . ? B21 B20 H20 122.9 . . ? B22 B20 H20 123.2 . . ? C15 B21 B17 59.4(6) . . ? C15 B21 B16 59.4(6) . . ? B17 B21 B16 108.7(8) . . ? C15 B21 B22 104.2(8) . . ? B17 B21 B22 58.8(7) . . ? B16 B21 B22 107.4(9) . . ? C15 B21 B20 104.1(8) . . ? B17 B21 B20 108.0(9) . . ? B16 B21 B20 58.2(6) . . ? B22 B21 B20 61.2(7) . . ? C15 B21 H21 124.6 . . ? B17 B21 H21 121.3 . . ? B16 B21 H21 121.7 . . ? B22 B21 H21 122.7 . . ? B20 B21 H21 122.7 . . ? B17 B22 B18 61.1(6) . . ? B17 B22 B21 60.1(6) . . ? B18 B22 B21 109.0(7) . . ? B17 B22 B19 108.0(8) . . ? B18 B22 B19 59.5(7) . . ? B21 B22 B19 107.6(8) . . ? B17 B22 B20 108.3(7) . . ? B18 B22 B20 107.9(9) . . ? B21 B22 B20 60.3(7) . . ? B19 B22 B20 59.4(7) . . ? B17 B22 H22 121.2 . . ? B18 B22 H22 121.2 . . ? B21 B22 H22 121.4 . . ? B19 B22 H22 122.4 . . ? B20 B22 H22 121.8 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.013 _refine_diff_density_min -2.842 _refine_diff_density_rms 0.187 data_f60311b _database_code_depnum_ccdc_archive 'CCDC 621988' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H30 B20 Co2 Ni S4' _chemical_formula_weight 719.19 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.295(4) _cell_length_b 36.040(11) _cell_length_c 15.458(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.897(6) _cell_angle_gamma 90.00 _cell_volume 6199(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1005 _cell_measurement_theta_min 2.260 _cell_measurement_theta_max 20.340 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 1.940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8297 _exptl_absorpt_correction_T_max 0.9092 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.31 _diffrn_reflns_number 25934 _diffrn_reflns_av_R_equivalents 0.1402 _diffrn_reflns_av_sigmaI/netI 0.2921 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10928 _reflns_number_gt 3716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0174P)^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 10928 _refine_ls_number_parameters 779 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1844 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 0.706 _refine_ls_restrained_S_all 0.706 _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 Co1A Co 0.03543(11) -0.04418(3) 0.69193(7) 0.0461(4) Uani 1 1 d . . . Co2A Co 0.19581(11) 0.03595(3) 0.85497(7) 0.0473(4) Uani 1 1 d . . . Ni1A Ni 0.03991(11) 0.01826(2) 0.73932(7) 0.0444(3) Uani 1 1 d . . . S1A S -0.0808(2) -0.00355(5) 0.61047(13) 0.0490(7) Uani 1 1 d . . . S2A S -0.0520(2) -0.02678(5) 0.80260(13) 0.0450(6) Uani 1 1 d . . . S3A S 0.2215(2) 0.03682(5) 0.71724(13) 0.0446(6) Uani 1 1 d . . . S4A S 0.0419(2) 0.07381(5) 0.81709(13) 0.0464(6) Uani 1 1 d . . . C1A C -0.2209(8) -0.00886(19) 0.6474(5) 0.045(2) Uani 1 1 d . . . C2A C -0.2040(8) -0.02078(19) 0.7504(5) 0.041(2) Uani 1 1 d . . . C3A C 0.1918(7) 0.08535(17) 0.6874(5) 0.038(2) Uani 1 1 d . . . C4A C 0.0983(7) 0.10556(19) 0.7428(5) 0.040(2) Uani 1 1 d . . . C5A C 0.0875(13) -0.0742(3) 0.5941(6) 0.080(4) Uani 1 1 d . . . H5AA H 0.0563 -0.0719 0.5311 0.096 Uiso 1 1 calc R . . C6A C 0.1880(11) -0.0552(3) 0.6419(10) 0.079(4) Uani 1 1 d . . . H6AA H 0.2365 -0.0367 0.6174 0.094 Uiso 1 1 calc R . . C7A C 0.2046(11) -0.0659(3) 0.7273(9) 0.088(4) Uani 1 1 d . . . H7AA H 0.2672 -0.0570 0.7747 0.106 Uiso 1 1 calc R . . C8A C 0.1166(14) -0.0928(3) 0.7347(8) 0.083(4) Uani 1 1 d . . . H8AA H 0.1070 -0.1061 0.7884 0.100 Uiso 1 1 calc R . . C9A C 0.0470(10) -0.0979(2) 0.6522(10) 0.071(3) Uani 1 1 d . . . H9AA H -0.0204 -0.1153 0.6381 0.085 Uiso 1 1 calc R . . C10A C 0.1774(10) 0.0269(3) 0.9811(6) 0.071(3) Uani 1 1 d . . . H10C H 0.1045 0.0306 1.0065 0.085 Uiso 1 1 calc R . . C11A C 0.2638(13) 0.0522(3) 0.9762(6) 0.078(4) Uani 1 1 d . . . H11C H 0.2644 0.0777 0.9979 0.094 Uiso 1 1 calc R . . C12A C 0.3541(10) 0.0358(3) 0.9398(6) 0.069(3) Uani 1 1 d . . . H12C H 0.4288 0.0478 0.9304 0.083 Uiso 1 1 calc R . . C13A C 0.3208(10) -0.0001(3) 0.9192(6) 0.065(3) Uani 1 1 d . . . H13C H 0.3667 -0.0186 0.8923 0.078 Uiso 1 1 calc R . . C14A C 0.2134(11) -0.0056(2) 0.9473(6) 0.066(3) Uani 1 1 d . . . H14C H 0.1677 -0.0289 0.9418 0.080 Uiso 1 1 calc R . . B3A B -0.2609(10) -0.0537(2) 0.6763(6) 0.049(3) Uani 1 1 d . . . H3A H -0.2134 -0.0793 0.6644 0.058 Uiso 1 1 calc R . . B4A B -0.3476(11) -0.0281(3) 0.5916(7) 0.069(4) Uani 1 1 d . . . H4A H -0.3564 -0.0367 0.5225 0.083 Uiso 1 1 calc R . . B5A B -0.3447(9) 0.0191(2) 0.6185(6) 0.051(3) Uani 1 1 d . . . H5A H -0.3515 0.0409 0.5682 0.062 Uiso 1 1 calc R . . B6A B -0.2534(10) 0.0244(2) 0.7226(6) 0.044(3) Uani 1 1 d . . . H6A H -0.2007 0.0497 0.7413 0.052 Uiso 1 1 calc R . . B7A B -0.3181(10) -0.0485(2) 0.7719(7) 0.056(3) Uani 1 1 d . . . H7A H -0.3084 -0.0700 0.8232 0.068 Uiso 1 1 calc R . . B8A B -0.4105(10) -0.0533(3) 0.6672(6) 0.061(3) Uani 1 1 d . . . H8A H -0.4626 -0.0788 0.6486 0.074 Uiso 1 1 calc R . . B9A B -0.4678(10) -0.0089(3) 0.6330(7) 0.060(3) Uani 1 1 d . . . H9A H -0.5574 -0.0054 0.5928 0.072 Uiso 1 1 calc R . . B10A B -0.4068(10) 0.0237(3) 0.7146(6) 0.058(3) Uani 1 1 d . . . H10A H -0.4565 0.0487 0.7275 0.070 Uiso 1 1 calc R . . B11A B -0.3153(10) -0.0003(3) 0.7992(6) 0.058(3) Uani 1 1 d . . . H11A H -0.3029 0.0088 0.8680 0.069 Uiso 1 1 calc R . . B12A B -0.4494(10) -0.0205(3) 0.7444(7) 0.060(3) Uani 1 1 d . . . H12A H -0.5277 -0.0243 0.7771 0.071 Uiso 1 1 calc R . . B13A B 0.0483(9) 0.0957(2) 0.6357(6) 0.040(3) Uani 1 1 d . . . H13A H -0.0215 0.0751 0.6119 0.048 Uiso 1 1 calc R . . B14A B 0.1748(9) 0.1024(2) 0.5847(6) 0.041(3) Uani 1 1 d . . . H14A H 0.1876 0.0860 0.5271 0.050 Uiso 1 1 calc R . . B15A B 0.2967(10) 0.1156(2) 0.6655(6) 0.053(3) Uani 1 1 d . . . H15A H 0.3893 0.1078 0.6601 0.064 Uiso 1 1 calc R . . B16A B 0.2474(9) 0.1164(2) 0.7678(6) 0.041(3) Uani 1 1 d . . . H16A H 0.3067 0.1090 0.8296 0.049 Uiso 1 1 calc R . . B17A B 0.0130(10) 0.1376(2) 0.6825(6) 0.048(3) Uani 1 1 d . . . H17A H -0.0801 0.1444 0.6890 0.057 Uiso 1 1 calc R . . B18A B 0.0634(10) 0.1375(2) 0.5791(7) 0.045(3) Uani 1 1 d . . . H18A H 0.0047 0.1447 0.5169 0.054 Uiso 1 1 calc R . . B19A B 0.2174(9) 0.1501(2) 0.5989(6) 0.047(3) Uani 1 1 d . . . H19A H 0.2583 0.1655 0.5501 0.056 Uiso 1 1 calc R . . B20A B 0.2616(10) 0.1582(2) 0.7115(6) 0.048(3) Uani 1 1 d . . . H20A H 0.3313 0.1788 0.7359 0.058 Uiso 1 1 calc R . . B21A B 0.1346(10) 0.1507(2) 0.7634(7) 0.054(3) Uani 1 1 d . . . H21A H 0.1212 0.1661 0.8224 0.065 Uiso 1 1 calc R . . B22A B 0.1147(9) 0.1710(2) 0.6596(6) 0.049(3) Uani 1 1 d . . . H22A H 0.0874 0.2003 0.6503 0.059 Uiso 1 1 calc R . . Co1B Co 0.58364(12) 0.18324(3) 0.45027(7) 0.0504(4) Uani 1 1 d . . . Co2B Co 0.83137(11) 0.25346(3) 0.38262(7) 0.0509(4) Uani 1 1 d . . . Ni1B Ni 0.62839(10) 0.24138(2) 0.39169(6) 0.0444(3) Uani 1 1 d . . . S1B S 0.4395(2) 0.22557(5) 0.42447(14) 0.0484(6) Uani 1 1 d . . . S2B S 0.6031(2) 0.18872(5) 0.31178(14) 0.0459(6) Uani 1 1 d . . . S3B S 0.7606(2) 0.26787(5) 0.50189(13) 0.0510(7) Uani 1 1 d . . . S4B S 0.6897(2) 0.28913(5) 0.30962(13) 0.0492(7) Uani 1 1 d . . . C1B C 0.3637(8) 0.21227(19) 0.3179(5) 0.044(2) Uani 1 1 d . . . C2B C 0.4484(8) 0.19334(19) 0.2564(5) 0.043(2) Uani 1 1 d . . . C3B C 0.7276(8) 0.31792(18) 0.4848(5) 0.044(2) Uani 1 1 d . . . C4B C 0.6880(7) 0.32796(19) 0.3826(5) 0.039(2) Uani 1 1 d . . . C5B C 0.5736(19) 0.1677(6) 0.5730(9) 0.099(5) Uani 1 1 d . . . H5BA H 0.5148 0.1771 0.6074 0.119 Uiso 1 1 calc R . . C6B C 0.672(2) 0.1811(4) 0.5727(11) 0.137(9) Uani 1 1 d . . . H6BA H 0.7051 0.2026 0.6076 0.164 Uiso 1 1 calc R . . C7B C 0.7303(14) 0.1607(9) 0.5242(15) 0.171(13) Uani 1 1 d . . . H7BA H 0.8138 0.1643 0.5162 0.205 Uiso 1 1 calc R . . C8B C 0.655(3) 0.1346(5) 0.4857(12) 0.152(11) Uani 1 1 d . . . H8BA H 0.6734 0.1148 0.4467 0.182 Uiso 1 1 calc R . . C9B C 0.5580(18) 0.1375(5) 0.5209(12) 0.117(6) Uani 1 1 d . . . H9BA H 0.4881 0.1210 0.5114 0.140 Uiso 1 1 calc R . . C10B C 0.8959(10) 0.2267(3) 0.2851(7) 0.082(4) Uani 1 1 d . . . H10D H 0.8528 0.2217 0.2256 0.098 Uiso 1 1 calc R . . C11B C 0.9675(10) 0.2578(3) 0.3130(9) 0.078(4) Uani 1 1 d . . . H11D H 0.9801 0.2789 0.2757 0.093 Uiso 1 1 calc R . . C12B C 1.0145(9) 0.2547(3) 0.3991(9) 0.075(3) Uani 1 1 d . . . H12D H 1.0671 0.2727 0.4342 0.090 Uiso 1 1 calc R . . C13B C 0.9755(10) 0.2207(3) 0.4291(8) 0.085(4) Uani 1 1 d . . . H13D H 0.9962 0.2108 0.4889 0.102 Uiso 1 1 calc R . . C14B C 0.9047(10) 0.2032(3) 0.3587(9) 0.077(4) Uani 1 1 d . . . H14D H 0.8658 0.1790 0.3603 0.093 Uiso 1 1 calc R . . B3B B 0.3924(9) 0.2377(2) 0.2307(6) 0.045(3) Uani 1 1 d . . . H3B H 0.4456 0.2634 0.2366 0.054 Uiso 1 1 calc R . . B4B B 0.2484(10) 0.2366(3) 0.2561(6) 0.058(3) Uani 1 1 d . . . H4B H 0.2068 0.2615 0.2793 0.070 Uiso 1 1 calc R . . B5B B 0.2213(9) 0.1926(2) 0.2990(7) 0.053(3) Uani 1 1 d . . . H5B H 0.1645 0.1891 0.3496 0.064 Uiso 1 1 calc R . . B6B B 0.3496(10) 0.1646(2) 0.2977(7) 0.054(3) Uani 1 1 d . . . H6B H 0.3751 0.1427 0.3469 0.065 Uiso 1 1 calc R . . B7B B 0.4034(11) 0.2040(2) 0.1488(6) 0.061(3) Uani 1 1 d . . . H7B H 0.4655 0.2073 0.1018 0.073 Uiso 1 1 calc R . . B8B B 0.2721(10) 0.2315(3) 0.1471(7) 0.060(3) Uani 1 1 d . . . H8B H 0.2464 0.2532 0.0973 0.072 Uiso 1 1 calc R . . B9B B 0.1630(10) 0.2040(3) 0.1862(7) 0.062(3) Uani 1 1 d . . . H9B H 0.0662 0.2076 0.1625 0.074 Uiso 1 1 calc R . . B10B B 0.2268(10) 0.1598(3) 0.2115(7) 0.058(3) Uani 1 1 d . . . H10B H 0.1709 0.1347 0.2038 0.069 Uiso 1 1 calc R . . B11B B 0.3731(11) 0.1602(3) 0.1897(7) 0.068(4) Uani 1 1 d . . . H11B H 0.4153 0.1351 0.1686 0.082 Uiso 1 1 calc R . . B12B B 0.2591(10) 0.1840(3) 0.1194(8) 0.066(4) Uani 1 1 d . . . H12B H 0.2253 0.1747 0.0519 0.080 Uiso 1 1 calc R . . B13B B 0.8277(10) 0.3421(2) 0.4357(6) 0.046(3) Uani 1 1 d . . . H13B H 0.9132 0.3313 0.4212 0.055 Uiso 1 1 calc R . . B14B B 0.8091(11) 0.3522(2) 0.5437(6) 0.062(4) Uani 1 1 d . . . H14B H 0.8819 0.3482 0.6001 0.074 Uiso 1 1 calc R . . B15B B 0.6564(10) 0.3433(2) 0.5496(6) 0.048(3) Uani 1 1 d . . . H15B H 0.6309 0.3333 0.6110 0.057 Uiso 1 1 calc R . . B16B B 0.5828(9) 0.3277(2) 0.4464(6) 0.044(3) Uani 1 1 d . . . H16B H 0.5084 0.3077 0.4398 0.053 Uiso 1 1 calc R . . B17B B 0.7391(9) 0.3720(2) 0.3634(7) 0.051(3) Uani 1 1 d . . . H17B H 0.7674 0.3812 0.3022 0.062 Uiso 1 1 calc R . . B18B B 0.8109(10) 0.3880(2) 0.4667(6) 0.055(3) Uani 1 1 d . . . H18B H 0.8852 0.4081 0.4737 0.066 Uiso 1 1 calc R . . B19B B 0.7022(11) 0.3887(2) 0.5360(7) 0.060(3) Uani 1 1 d . . . H19B H 0.7050 0.4095 0.5885 0.072 Uiso 1 1 calc R . . B20B B 0.5671(11) 0.3735(2) 0.4775(7) 0.064(4) Uani 1 1 d . . . H20B H 0.4815 0.3843 0.4920 0.077 Uiso 1 1 calc R . . B21B B 0.5853(10) 0.3625(2) 0.3681(7) 0.056(3) Uani 1 1 d . . . H21B H 0.5141 0.3655 0.3103 0.067 Uiso 1 1 calc R . . B22B B 0.6607(10) 0.4003(3) 0.4253(7) 0.060(3) Uani 1 1 d . . . H22B H 0.6363 0.4289 0.4044 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1A 0.0573(10) 0.0356(6) 0.0446(8) -0.0003(6) 0.0063(7) 0.0034(7) Co2A 0.0602(10) 0.0392(7) 0.0418(8) 0.0054(6) 0.0068(7) -0.0015(7) Ni1A 0.0558(9) 0.0331(6) 0.0452(7) 0.0003(5) 0.0109(6) -0.0032(6) S1A 0.0590(19) 0.0460(13) 0.0427(15) 0.0070(11) 0.0102(13) 0.0057(13) S2A 0.0549(18) 0.0378(12) 0.0411(14) 0.0031(11) 0.0047(13) -0.0032(13) S3A 0.0528(18) 0.0343(12) 0.0495(14) 0.0000(11) 0.0164(13) 0.0011(12) S4A 0.0548(18) 0.0413(12) 0.0466(15) -0.0004(11) 0.0186(13) -0.0021(13) C1A 0.060(7) 0.038(5) 0.038(6) -0.001(4) 0.007(5) 0.004(5) C2A 0.050(7) 0.039(5) 0.033(5) -0.015(4) 0.004(5) -0.006(5) C3A 0.046(6) 0.025(4) 0.046(6) 0.003(4) 0.013(5) -0.003(4) C4A 0.043(6) 0.039(5) 0.042(6) 0.003(4) 0.021(5) 0.008(5) C5A 0.119(12) 0.092(9) 0.030(7) -0.022(7) 0.014(7) 0.037(8) C6A 0.072(10) 0.059(7) 0.119(11) -0.020(8) 0.059(9) 0.001(7) C7A 0.067(10) 0.101(10) 0.093(11) -0.009(8) 0.004(8) 0.019(8) C8A 0.116(13) 0.052(7) 0.091(11) 0.020(7) 0.045(9) 0.041(8) C9A 0.070(9) 0.029(6) 0.118(10) -0.004(7) 0.025(9) 0.005(6) C10A 0.094(10) 0.077(8) 0.050(7) 0.032(6) 0.034(6) 0.028(8) C11A 0.130(13) 0.051(7) 0.046(7) 0.016(5) -0.007(7) 0.008(8) C12A 0.067(9) 0.057(7) 0.074(8) 0.029(6) -0.013(7) -0.003(7) C13A 0.065(9) 0.059(7) 0.075(8) 0.024(6) 0.020(7) 0.008(6) C14A 0.085(10) 0.048(6) 0.060(7) 0.018(5) -0.006(7) -0.004(7) B3A 0.062(9) 0.029(5) 0.047(7) 0.001(5) -0.011(6) 0.005(6) B4A 0.075(10) 0.063(8) 0.060(8) -0.004(7) -0.014(8) 0.014(7) B5A 0.056(9) 0.039(6) 0.055(8) 0.013(5) -0.002(6) 0.017(6) B6A 0.055(8) 0.035(6) 0.042(7) 0.002(5) 0.010(6) 0.003(6) B7A 0.071(10) 0.040(6) 0.062(8) 0.005(6) 0.023(7) 0.001(7) B8A 0.060(10) 0.060(7) 0.060(8) -0.006(6) 0.000(7) -0.010(7) B9A 0.041(8) 0.072(8) 0.062(8) -0.011(6) -0.007(7) 0.006(7) B10A 0.057(9) 0.063(7) 0.052(8) -0.002(6) 0.002(7) 0.004(7) B11A 0.081(10) 0.060(7) 0.033(7) -0.006(6) 0.014(7) 0.019(7) B12A 0.042(8) 0.075(8) 0.062(8) -0.016(7) 0.011(6) -0.002(7) B13A 0.026(7) 0.049(6) 0.042(7) 0.008(5) -0.004(5) 0.013(5) B14A 0.049(8) 0.045(6) 0.031(6) 0.008(5) 0.005(6) 0.004(6) B15A 0.040(8) 0.046(6) 0.074(8) 0.010(6) 0.011(7) -0.006(6) B16A 0.034(7) 0.051(6) 0.041(6) -0.006(5) 0.012(6) -0.008(6) B17A 0.055(9) 0.018(5) 0.072(8) 0.008(5) 0.015(7) 0.016(5) B18A 0.049(8) 0.028(5) 0.058(7) 0.009(5) 0.011(6) 0.000(5) B19A 0.049(8) 0.045(6) 0.045(7) 0.006(5) 0.004(6) 0.006(6) B20A 0.055(9) 0.034(6) 0.057(7) -0.005(5) 0.013(6) -0.010(6) B21A 0.077(10) 0.020(5) 0.068(8) -0.005(5) 0.019(7) -0.004(6) B22A 0.045(8) 0.028(6) 0.068(8) -0.004(5) -0.008(6) 0.006(5) Co1B 0.0531(10) 0.0432(7) 0.0567(9) 0.0083(6) 0.0144(7) 0.0027(7) Co2B 0.0475(9) 0.0427(7) 0.0672(9) 0.0050(6) 0.0231(7) 0.0041(7) Ni1B 0.0454(9) 0.0380(6) 0.0523(7) 0.0016(6) 0.0159(6) -0.0001(6) S1B 0.0523(18) 0.0452(13) 0.0521(15) -0.0019(11) 0.0214(13) 0.0017(13) S2B 0.0404(17) 0.0410(13) 0.0580(16) -0.0034(11) 0.0135(13) 0.0049(12) S3B 0.0605(19) 0.0424(13) 0.0509(15) 0.0093(11) 0.0121(13) 0.0044(13) S4B 0.0559(19) 0.0419(13) 0.0523(15) 0.0035(11) 0.0166(13) 0.0015(13) C1B 0.063(7) 0.032(5) 0.039(5) 0.003(4) 0.012(5) 0.006(5) C2B 0.042(6) 0.037(5) 0.057(6) 0.001(4) 0.028(5) 0.004(5) C3B 0.055(7) 0.031(5) 0.047(6) 0.006(4) 0.015(5) 0.001(5) C4B 0.041(6) 0.044(5) 0.032(5) -0.002(4) 0.008(5) -0.006(5) C5B 0.148(18) 0.096(12) 0.068(10) 0.046(10) 0.058(11) 0.045(11) C6B 0.20(3) 0.094(11) 0.107(15) 0.023(9) -0.009(14) -0.089(15) C7B 0.023(9) 0.36(4) 0.12(2) 0.16(2) 0.000(10) 0.023(14) C8B 0.24(3) 0.126(15) 0.099(14) 0.023(10) 0.043(17) 0.146(18) C9B 0.158(19) 0.052(9) 0.114(15) 0.057(9) -0.046(12) -0.049(10) C10B 0.088(10) 0.078(8) 0.094(9) -0.011(8) 0.056(8) 0.024(8) C11B 0.074(10) 0.050(7) 0.126(11) 0.026(8) 0.067(8) 0.015(7) C12B 0.052(8) 0.068(8) 0.112(10) 0.006(8) 0.031(8) 0.007(7) C13B 0.061(9) 0.081(9) 0.124(11) 0.038(8) 0.046(8) 0.039(7) C14B 0.072(10) 0.045(7) 0.124(11) -0.009(8) 0.039(8) 0.012(6) B3B 0.047(8) 0.045(6) 0.048(7) 0.012(5) 0.020(6) 0.010(6) B4B 0.044(8) 0.060(7) 0.073(8) 0.002(6) 0.015(7) 0.006(7) B5B 0.029(7) 0.054(7) 0.077(9) 0.005(6) 0.013(6) 0.007(6) B6B 0.057(9) 0.023(5) 0.087(9) 0.003(6) 0.027(7) 0.006(6) B7B 0.084(11) 0.060(7) 0.041(7) 0.002(6) 0.021(7) 0.018(7) B8B 0.065(10) 0.056(7) 0.057(8) -0.011(6) 0.006(7) -0.004(7) B9B 0.045(9) 0.066(8) 0.072(9) -0.002(6) 0.004(7) 0.010(7) B10B 0.034(8) 0.066(7) 0.077(9) -0.013(7) 0.022(7) -0.002(7) B11B 0.087(11) 0.034(6) 0.080(9) -0.003(6) 0.002(8) -0.008(7) B12B 0.047(9) 0.068(8) 0.081(9) -0.023(7) 0.003(7) 0.014(7) B13B 0.043(8) 0.056(7) 0.041(7) 0.010(5) 0.011(6) -0.010(6) B14B 0.091(11) 0.033(6) 0.051(8) -0.010(5) -0.016(7) -0.011(7) B15B 0.062(9) 0.034(6) 0.049(7) -0.003(5) 0.012(6) 0.004(6) B16B 0.020(7) 0.054(7) 0.060(7) 0.007(6) 0.015(6) 0.008(6) B17B 0.050(9) 0.036(6) 0.073(8) 0.009(6) 0.025(7) -0.007(6) B18B 0.070(10) 0.030(6) 0.066(8) -0.005(5) 0.015(7) -0.027(6) B19B 0.083(10) 0.031(6) 0.066(9) -0.007(6) 0.012(8) -0.011(7) B20B 0.077(11) 0.037(6) 0.086(9) -0.009(6) 0.033(8) 0.007(7) B21B 0.058(9) 0.032(6) 0.078(9) 0.019(6) 0.011(7) 0.014(6) B22B 0.053(9) 0.040(6) 0.087(9) -0.006(6) 0.007(7) -0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1A C5A 2.026(8) . ? Co1A C8A 2.035(9) . ? Co1A C9A 2.043(8) . ? Co1A C6A 2.046(10) . ? Co1A C7A 2.050(11) . ? Co1A S2A 2.208(2) . ? Co1A S1A 2.210(2) . ? Co1A Ni1A 2.3644(15) . ? Co2A C11A 1.987(9) . ? Co2A C10A 2.023(8) . ? Co2A C12A 2.027(10) . ? Co2A C13A 2.047(9) . ? Co2A C14A 2.054(8) . ? Co2A S3A 2.198(2) . ? Co2A S4A 2.209(3) . ? Co2A Ni1A 2.3710(17) . ? Ni1A S3A 2.239(3) . ? Ni1A S2A 2.240(2) . ? Ni1A S4A 2.333(2) . ? Ni1A S1A 2.348(2) . ? S1A C1A 1.782(9) . ? S2A C2A 1.780(8) . ? S3A C3A 1.825(6) . ? S4A C4A 1.813(7) . ? C1A C2A 1.629(9) . ? C1A B4A 1.688(13) . ? C1A B5A 1.719(12) . ? C1A B6A 1.751(11) . ? C1A B3A 1.756(11) . ? C2A B3A 1.696(10) . ? C2A B7A 1.707(12) . ? C2A B11A 1.737(12) . ? C2A B6A 1.749(11) . ? C3A C4A 1.639(10) . ? C3A B14A 1.682(10) . ? C3A B15A 1.686(11) . ? C3A B16A 1.708(11) . ? C3A B13A 1.721(12) . ? C4A B17A 1.680(11) . ? C4A B13A 1.691(11) . ? C4A B21A 1.694(10) . ? C4A B16A 1.707(12) . ? C5A C9A 1.376(12) . ? C5A C6A 1.418(12) . ? C5A H5AA 0.9800 . ? C6A C7A 1.357(12) . ? C6A H6AA 0.9800 . ? C7A C8A 1.407(13) . ? C7A H7AA 0.9800 . ? C8A C9A 1.390(12) . ? C8A H8AA 0.9800 . ? C9A H9AA 0.9800 . ? C10A C11A 1.347(12) . ? C10A C14A 1.372(11) . ? C10A H10C 0.9800 . ? C11A C12A 1.379(12) . ? C11A H11C 0.9800 . ? C12A C13A 1.371(11) . ? C12A H12C 0.9800 . ? C13A C14A 1.371(12) . ? C13A H13C 0.9800 . ? C14A H14C 0.9800 . ? B3A B8A 1.672(14) . ? B3A B7A 1.721(13) . ? B3A B4A 1.755(13) . ? B3A H3A 1.1000 . ? B4A B8A 1.727(14) . ? B4A B9A 1.741(14) . ? B4A B5A 1.750(13) . ? B4A H4A 1.1000 . ? B5A B10A 1.756(14) . ? B5A B9A 1.763(14) . ? B5A B6A 1.766(13) . ? B5A H5A 1.1000 . ? B6A B10A 1.715(14) . ? B6A B11A 1.722(13) . ? B6A H6A 1.1000 . ? B7A B8A 1.777(14) . ? B7A B12A 1.784(14) . ? B7A B11A 1.785(12) . ? B7A H7A 1.1000 . ? B8A B9A 1.774(13) . ? B8A B12A 1.789(13) . ? B8A H8A 1.1000 . ? B9A B12A 1.749(13) . ? B9A B10A 1.773(13) . ? B9A H9A 1.1000 . ? B10A B12A 1.745(13) . ? B10A B11A 1.749(13) . ? B10A H10A 1.1000 . ? B11A B12A 1.759(14) . ? B11A H11A 1.1000 . ? B12A H12A 1.1000 . ? B13A B17A 1.749(11) . ? B13A B14A 1.763(13) . ? B13A B18A 1.766(11) . ? B13A H13A 1.1000 . ? B14A B15A 1.758(13) . ? B14A B18A 1.777(12) . ? B14A B19A 1.788(12) . ? B14A H14A 1.1000 . ? B15A B19A 1.758(12) . ? B15A B16A 1.764(12) . ? B15A B20A 1.766(12) . ? B15A H15A 1.1000 . ? B16A B20A 1.762(11) . ? B16A B21A 1.769(13) . ? B16A H16A 1.1000 . ? B17A B22A 1.742(13) . ? B17A B21A 1.755(13) . ? B17A B18A 1.788(13) . ? B17A H17A 1.1000 . ? B18A B22A 1.759(12) . ? B18A B19A 1.772(13) . ? B18A H18A 1.1000 . ? B19A B20A 1.752(12) . ? B19A B22A 1.781(13) . ? B19A H19A 1.1000 . ? B20A B22A 1.776(14) . ? B20A B21A 1.780(13) . ? B20A H20A 1.1000 . ? B21A B22A 1.743(13) . ? B21A H21A 1.1000 . ? B22A H22A 1.1000 . ? Co1B C8B 1.967(13) . ? Co1B C6B 1.983(16) . ? Co1B C5B 1.999(10) . ? Co1B C7B 2.016(14) . ? Co1B C9B 2.025(10) . ? Co1B S2B 2.198(2) . ? Co1B S1B 2.217(2) . ? Co1B Ni1B 2.3712(15) . ? Co2B C10B 2.027(9) . ? Co2B C11B 2.029(9) . ? Co2B C13B 2.040(10) . ? Co2B C12B 2.040(10) . ? Co2B C14B 2.052(9) . ? Co2B S3B 2.194(2) . ? Co2B S4B 2.206(2) . ? Co2B Ni1B 2.3614(18) . ? Ni1B S2B 2.256(2) . ? Ni1B S3B 2.273(3) . ? Ni1B S4B 2.314(2) . ? Ni1B S1B 2.346(3) . ? S1B C1B 1.786(8) . ? S2B C2B 1.816(9) . ? S3B C3B 1.852(7) . ? S4B C4B 1.800(7) . ? C1B C2B 1.613(10) . ? C1B B3B 1.707(11) . ? C1B B4B 1.718(12) . ? C1B B5B 1.736(12) . ? C1B B6B 1.749(10) . ? C2B B7B 1.697(11) . ? C2B B11B 1.705(12) . ? C2B B6B 1.725(12) . ? C2B B3B 1.740(11) . ? C3B C4B 1.608(9) . ? C3B B15B 1.662(11) . ? C3B B16B 1.679(12) . ? C3B B13B 1.707(11) . ? C3B B14B 1.707(11) . ? C4B B16B 1.669(11) . ? C4B B21B 1.691(11) . ? C4B B13B 1.727(12) . ? C4B B17B 1.731(10) . ? C5B C6B 1.210(17) . ? C5B C9B 1.349(15) . ? C5B H5BA 0.9800 . ? C6B C7B 1.31(2) . ? C6B H6BA 0.9800 . ? C7B C8B 1.34(2) . ? C7B H7BA 0.9800 . ? C8B C9B 1.306(18) . ? C8B H8BA 0.9800 . ? C9B H9BA 0.9800 . ? C10B C11B 1.406(12) . ? C10B C14B 1.410(12) . ? C10B H10D 0.9800 . ? C11B C12B 1.350(11) . ? C11B H11D 0.9800 . ? C12B C13B 1.408(11) . ? C12B H12D 0.9800 . ? C13B C14B 1.386(12) . ? C13B H13D 0.9800 . ? C14B H14D 0.9800 . ? B3B B8B 1.722(14) . ? B3B B4B 1.739(14) . ? B3B B7B 1.774(12) . ? B3B H3B 1.1000 . ? B4B B8B 1.762(13) . ? B4B B9B 1.767(13) . ? B4B B5B 1.767(13) . ? B4B H4B 1.1000 . ? B5B B6B 1.769(13) . ? B5B B9B 1.803(13) . ? B5B B10B 1.804(13) . ? B5B H5B 1.1000 . ? B6B B11B 1.742(13) . ? B6B B10B 1.759(14) . ? B6B H6B 1.1000 . ? B7B B11B 1.755(13) . ? B7B B12B 1.770(15) . ? B7B B8B 1.779(14) . ? B7B H7B 1.1000 . ? B8B B12B 1.767(13) . ? B8B B9B 1.768(14) . ? B8B H8B 1.1000 . ? B9B B10B 1.762(13) . ? B9B B12B 1.775(14) . ? B9B H9B 1.1000 . ? B10B B11B 1.742(15) . ? B10B B12B 1.759(14) . ? B10B H10B 1.1000 . ? B11B B12B 1.757(14) . ? B11B H11B 1.1000 . ? B12B H12B 1.1000 . ? B13B B17B 1.738(12) . ? B13B B18B 1.741(12) . ? B13B B14B 1.757(13) . ? B13B H13B 1.1000 . ? B14B B18B 1.758(12) . ? B14B B15B 1.771(14) . ? B14B B19B 1.775(14) . ? B14B H14B 1.1000 . ? B15B B19B 1.740(12) . ? B15B B20B 1.749(13) . ? B15B B16B 1.759(13) . ? B15B H15B 1.1000 . ? B16B B20B 1.736(12) . ? B16B B21B 1.747(12) . ? B16B H16B 1.1000 . ? B17B B22B 1.742(13) . ? B17B B18B 1.760(13) . ? B17B B21B 1.784(14) . ? B17B H17B 1.1000 . ? B18B B19B 1.763(14) . ? B18B B22B 1.764(14) . ? B18B H18B 1.1000 . ? B19B B20B 1.724(15) . ? B19B B22B 1.745(13) . ? B19B H19B 1.1000 . ? B20B B22B 1.730(14) . ? B20B B21B 1.783(14) . ? B20B H20B 1.1000 . ? B21B B22B 1.761(13) . ? B21B H21B 1.1000 . ? B22B H22B 1.1000 . ? 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 C5A Co1A C8A 67.1(4) . . ? C5A Co1A C9A 39.5(3) . . ? C8A Co1A C9A 39.8(3) . . ? C5A Co1A C6A 40.8(4) . . ? C8A Co1A C6A 66.0(4) . . ? C9A Co1A C6A 66.4(4) . . ? C5A Co1A C7A 67.6(4) . . ? C8A Co1A C7A 40.3(4) . . ? C9A Co1A C7A 67.2(4) . . ? C6A Co1A C7A 38.7(3) . . ? C5A Co1A S2A 162.8(5) . . ? C8A Co1A S2A 103.3(3) . . ? C9A Co1A S2A 124.2(4) . . ? C6A Co1A S2A 150.0(5) . . ? C7A Co1A S2A 115.0(4) . . ? C5A Co1A S1A 98.5(3) . . ? C8A Co1A S1A 161.1(5) . . ? C9A Co1A S1A 121.3(4) . . ? C6A Co1A S1A 111.7(4) . . ? C7A Co1A S1A 147.2(5) . . ? S2A Co1A S1A 87.26(9) . . ? C5A Co1A Ni1A 138.2(4) . . ? C8A Co1A Ni1A 137.3(5) . . ? C9A Co1A Ni1A 175.2(3) . . ? C6A Co1A Ni1A 109.2(3) . . ? C7A Co1A Ni1A 108.2(3) . . ? S2A Co1A Ni1A 58.55(6) . . ? S1A Co1A Ni1A 61.64(6) . . ? C11A Co2A C10A 39.3(4) . . ? C11A Co2A C12A 40.2(4) . . ? C10A Co2A C12A 66.5(4) . . ? C11A Co2A C13A 66.8(4) . . ? C10A Co2A C13A 66.8(4) . . ? C12A Co2A C13A 39.3(3) . . ? C11A Co2A C14A 65.4(4) . . ? C10A Co2A C14A 39.3(3) . . ? C12A Co2A C14A 65.2(4) . . ? C13A Co2A C14A 39.1(3) . . ? C11A Co2A S3A 144.6(4) . . ? C10A Co2A S3A 171.4(3) . . ? C12A Co2A S3A 112.2(3) . . ? C13A Co2A S3A 106.5(3) . . ? C14A Co2A S3A 132.1(3) . . ? C11A Co2A S4A 103.1(4) . . ? C10A Co2A S4A 98.6(3) . . ? C12A Co2A S4A 137.7(3) . . ? C13A Co2A S4A 165.3(3) . . ? C14A Co2A S4A 127.7(4) . . ? S3A Co2A S4A 87.90(8) . . ? C11A Co2A Ni1A 155.1(4) . . ? C10A Co2A Ni1A 119.8(4) . . ? C12A Co2A Ni1A 160.9(4) . . ? C13A Co2A Ni1A 123.8(3) . . ? C14A Co2A Ni1A 107.3(3) . . ? S3A Co2A Ni1A 58.54(7) . . ? S4A Co2A Ni1A 61.14(7) . . ? S3A Ni1A S2A 142.06(9) . . ? S3A Ni1A S4A 83.94(8) . . ? S2A Ni1A S4A 111.15(9) . . ? S3A Ni1A S1A 112.61(9) . . ? S2A Ni1A S1A 83.26(8) . . ? S4A Ni1A S1A 132.62(9) . . ? S3A Ni1A Co1A 102.03(7) . . ? S2A Ni1A Co1A 57.24(6) . . ? S4A Ni1A Co1A 166.92(7) . . ? S1A Ni1A Co1A 55.95(6) . . ? S3A Ni1A Co2A 56.87(7) . . ? S2A Ni1A Co2A 101.86(7) . . ? S4A Ni1A Co2A 56.00(7) . . ? S1A Ni1A Co2A 167.86(9) . . ? Co1A Ni1A Co2A 117.59(6) . . ? C1A S1A Co1A 102.7(3) . . ? C1A S1A Ni1A 100.5(3) . . ? Co1A S1A Ni1A 62.41(7) . . ? C2A S2A Co1A 102.0(3) . . ? C2A S2A Ni1A 101.4(3) . . ? Co1A S2A Ni1A 64.21(7) . . ? C3A S3A Co2A 102.1(2) . . ? C3A S3A Ni1A 101.0(3) . . ? Co2A S3A Ni1A 64.59(7) . . ? C4A S4A Co2A 102.2(3) . . ? C4A S4A Ni1A 100.9(2) . . ? Co2A S4A Ni1A 62.86(7) . . ? C2A C1A B4A 109.7(7) . . ? C2A C1A B5A 111.2(6) . . ? B4A C1A B5A 61.8(6) . . ? C2A C1A B6A 62.2(4) . . ? B4A C1A B6A 111.3(7) . . ? B5A C1A B6A 61.2(5) . . ? C2A C1A B3A 60.0(4) . . ? B4A C1A B3A 61.2(5) . . ? B5A C1A B3A 111.8(7) . . ? B6A C1A B3A 111.5(6) . . ? C2A C1A S1A 112.4(6) . . ? B4A C1A S1A 127.0(6) . . ? B5A C1A S1A 125.6(6) . . ? B6A C1A S1A 116.0(6) . . ? B3A C1A S1A 117.5(6) . . ? C1A C2A B3A 63.7(5) . . ? C1A C2A B7A 112.3(6) . . ? B3A C2A B7A 60.8(5) . . ? C1A C2A B11A 109.9(6) . . ? B3A C2A B11A 111.8(7) . . ? B7A C2A B11A 62.4(5) . . ? C1A C2A B6A 62.3(4) . . ? B3A C2A B6A 114.6(6) . . ? B7A C2A B6A 111.8(7) . . ? B11A C2A B6A 59.2(5) . . ? C1A C2A S2A 114.6(6) . . ? B3A C2A S2A 116.4(5) . . ? B7A C2A S2A 122.8(6) . . ? B11A C2A S2A 124.6(5) . . ? B6A C2A S2A 117.8(5) . . ? C4A C3A B14A 110.6(6) . . ? C4A C3A B15A 110.8(6) . . ? B14A C3A B15A 62.9(5) . . ? C4A C3A B16A 61.3(5) . . ? B14A C3A B16A 114.5(5) . . ? B15A C3A B16A 62.6(5) . . ? C4A C3A B13A 60.4(5) . . ? B14A C3A B13A 62.4(5) . . ? B15A C3A B13A 113.8(6) . . ? B16A C3A B13A 113.3(6) . . ? C4A C3A S3A 113.7(5) . . ? B14A C3A S3A 125.0(5) . . ? B15A C3A S3A 124.4(6) . . ? B16A C3A S3A 114.5(5) . . ? B13A C3A S3A 116.3(5) . . ? C3A C4A B17A 112.1(6) . . ? C3A C4A B13A 62.2(5) . . ? B17A C4A B13A 62.5(5) . . ? C3A C4A B21A 111.6(6) . . ? B17A C4A B21A 62.7(5) . . ? B13A C4A B21A 114.5(6) . . ? C3A C4A B16A 61.3(5) . . ? B17A C4A B16A 114.7(6) . . ? B13A C4A B16A 114.8(6) . . ? B21A C4A B16A 62.7(5) . . ? C3A C4A S4A 112.2(5) . . ? B17A C4A S4A 123.7(6) . . ? B13A C4A S4A 113.2(5) . . ? B21A C4A S4A 125.9(5) . . ? B16A C4A S4A 116.1(5) . . ? C9A C5A C6A 106.6(10) . . ? C9A C5A Co1A 70.9(5) . . ? C6A C5A Co1A 70.4(5) . . ? C9A C5A H5AA 126.7 . . ? C6A C5A H5AA 126.7 . . ? Co1A C5A H5AA 126.7 . . ? C7A C6A C5A 109.6(10) . . ? C7A C6A Co1A 70.8(6) . . ? C5A C6A Co1A 68.9(6) . . ? C7A C6A H6AA 125.2 . . ? C5A C6A H6AA 125.2 . . ? Co1A C6A H6AA 125.2 . . ? C6A C7A C8A 107.0(11) . . ? C6A C7A Co1A 70.5(7) . . ? C8A C7A Co1A 69.3(6) . . ? C6A C7A H7AA 126.5 . . ? C8A C7A H7AA 126.5 . . ? Co1A C7A H7AA 126.5 . . ? C9A C8A C7A 108.3(11) . . ? C9A C8A Co1A 70.4(6) . . ? C7A C8A Co1A 70.4(6) . . ? C9A C8A H8AA 125.9 . . ? C7A C8A H8AA 125.9 . . ? Co1A C8A H8AA 125.9 . . ? C5A C9A C8A 108.5(11) . . ? C5A C9A Co1A 69.6(5) . . ? C8A C9A Co1A 69.8(6) . . ? C5A C9A H9AA 125.8 . . ? C8A C9A H9AA 125.8 . . ? Co1A C9A H9AA 125.8 . . ? C11A C10A C14A 106.9(11) . . ? C11A C10A Co2A 68.9(6) . . ? C14A C10A Co2A 71.6(5) . . ? C11A C10A H10C 126.5 . . ? C14A C10A H10C 126.5 . . ? Co2A C10A H10C 126.5 . . ? C10A C11A C12A 109.2(10) . . ? C10A C11A Co2A 71.8(6) . . ? C12A C11A Co2A 71.5(6) . . ? C10A C11A H11C 125.4 . . ? C12A C11A H11C 125.4 . . ? Co2A C11A H11C 125.4 . . ? C13A C12A C11A 107.8(10) . . ? C13A C12A Co2A 71.1(6) . . ? C11A C12A Co2A 68.3(6) . . ? C13A C12A H12C 126.1 . . ? C11A C12A H12C 126.1 . . ? Co2A C12A H12C 126.1 . . ? C14A C13A C12A 106.6(9) . . ? C14A C13A Co2A 70.8(6) . . ? C12A C13A Co2A 69.6(5) . . ? C14A C13A H13C 126.7 . . ? C12A C13A H13C 126.7 . . ? Co2A C13A H13C 126.7 . . ? C13A C14A C10A 109.5(10) . . ? C13A C14A Co2A 70.2(5) . . ? C10A C14A Co2A 69.1(5) . . ? C13A C14A H14C 125.2 . . ? C10A C14A H14C 125.2 . . ? Co2A C14A H14C 125.2 . . ? B8A B3A C2A 108.2(7) . . ? B8A B3A B7A 63.1(6) . . ? C2A B3A B7A 59.9(5) . . ? B8A B3A B4A 60.5(6) . . ? C2A B3A B4A 103.6(6) . . ? B7A B3A B4A 109.8(8) . . ? B8A B3A C1A 105.8(7) . . ? C2A B3A C1A 56.3(4) . . ? B7A B3A C1A 105.6(6) . . ? B4A B3A C1A 57.5(5) . . ? B8A B3A H3A 120.4 . . ? C2A B3A H3A 124.2 . . ? B7A B3A H3A 120.0 . . ? B4A B3A H3A 122.8 . . ? C1A B3A H3A 125.2 . . ? C1A B4A B8A 106.4(7) . . ? C1A B4A B9A 107.2(7) . . ? B8A B4A B9A 61.5(6) . . ? C1A B4A B5A 60.0(5) . . ? B8A B4A B5A 110.2(8) . . ? B9A B4A B5A 60.7(6) . . ? C1A B4A B3A 61.3(5) . . ? B8A B4A B3A 57.4(6) . . ? B9A B4A B3A 107.8(8) . . ? B5A B4A B3A 110.4(7) . . ? C1A B4A H4A 122.5 . . ? B8A B4A H4A 122.1 . . ? B9A B4A H4A 121.5 . . ? B5A B4A H4A 119.8 . . ? B3A B4A H4A 121.5 . . ? C1A B5A B4A 58.2(5) . . ? C1A B5A B10A 105.1(7) . . ? B4A B5A B10A 107.3(7) . . ? C1A B5A B9A 104.8(6) . . ? B4A B5A B9A 59.4(6) . . ? B10A B5A B9A 60.5(6) . . ? C1A B5A B6A 60.3(5) . . ? B4A B5A B6A 107.8(7) . . ? B10A B5A B6A 58.3(5) . . ? B9A B5A B6A 107.2(7) . . ? C1A B5A H5A 123.9 . . ? B4A B5A H5A 122.1 . . ? B10A B5A H5A 122.8 . . ? B9A B5A H5A 122.5 . . ? B6A B5A H5A 121.8 . . ? B10A B6A B11A 61.2(6) . . ? B10A B6A C2A 106.2(7) . . ? B11A B6A C2A 60.0(5) . . ? B10A B6A C1A 105.5(7) . . ? B11A B6A C1A 105.0(6) . . ? C2A B6A C1A 55.5(4) . . ? B10A B6A B5A 60.6(6) . . ? B11A B6A B5A 109.2(8) . . ? C2A B6A B5A 103.6(6) . . ? C1A B6A B5A 58.5(5) . . ? B10A B6A H6A 121.7 . . ? B11A B6A H6A 120.9 . . ? C2A B6A H6A 124.8 . . ? C1A B6A H6A 125.1 . . ? B5A B6A H6A 122.2 . . ? C2A B7A B3A 59.3(5) . . ? C2A B7A B8A 103.1(7) . . ? B3A B7A B8A 57.1(5) . . ? C2A B7A B12A 104.3(6) . . ? B3A B7A B12A 106.1(7) . . ? B8A B7A B12A 60.3(6) . . ? C2A B7A B11A 59.6(5) . . ? B3A B7A B11A 108.3(7) . . ? B8A B7A B11A 107.1(7) . . ? B12A B7A B11A 59.1(5) . . ? C2A B7A H7A 124.5 . . ? B3A B7A H7A 122.5 . . ? B8A B7A H7A 123.9 . . ? B12A B7A H7A 123.1 . . ? B11A B7A H7A 121.2 . . ? B3A B8A B4A 62.2(6) . . ? B3A B8A B9A 110.0(8) . . ? B4A B8A B9A 59.6(6) . . ? B3A B8A B7A 59.8(6) . . ? B4A B8A B7A 108.6(8) . . ? B9A B8A B7A 108.0(7) . . ? B3A B8A B12A 108.0(8) . . ? B4A B8A B12A 106.2(7) . . ? B9A B8A B12A 58.8(6) . . ? B7A B8A B12A 60.1(5) . . ? B3A B8A H8A 120.2 . . ? B4A B8A H8A 121.7 . . ? B9A B8A H8A 121.6 . . ? B7A B8A H8A 121.6 . . ? B12A B8A H8A 123.0 . . ? B4A B9A B12A 107.4(8) . . ? B4A B9A B5A 59.9(6) . . ? B12A B9A B5A 107.4(7) . . ? B4A B9A B10A 107.0(8) . . ? B12A B9A B10A 59.4(5) . . ? B5A B9A B10A 59.6(5) . . ? B4A B9A B8A 58.8(6) . . ? B12A B9A B8A 61.0(5) . . ? B5A B9A B8A 107.4(7) . . ? B10A B9A B8A 107.9(7) . . ? B4A B9A H9A 122.5 . . ? B12A B9A H9A 121.7 . . ? B5A B9A H9A 122.1 . . ? B10A B9A H9A 122.2 . . ? B8A B9A H9A 121.7 . . ? B6A B10A B12A 108.4(8) . . ? B6A B10A B11A 59.6(6) . . ? B12A B10A B11A 60.5(6) . . ? B6A B10A B5A 61.1(6) . . ? B12A B10A B5A 107.8(7) . . ? B11A B10A B5A 108.4(8) . . ? B6A B10A B9A 109.0(7) . . ? B12A B10A B9A 59.6(5) . . ? B11A B10A B9A 108.2(7) . . ? B5A B10A B9A 59.9(5) . . ? B6A B10A H10A 121.1 . . ? B12A B10A H10A 121.8 . . ? B11A B10A H10A 121.7 . . ? B5A B10A H10A 121.4 . . ? B9A B10A H10A 121.6 . . ? B6A B11A C2A 60.8(5) . . ? B6A B11A B10A 59.2(6) . . ? C2A B11A B10A 105.3(7) . . ? B6A B11A B12A 107.4(7) . . ? C2A B11A B12A 104.1(6) . . ? B10A B11A B12A 59.7(6) . . ? B6A B11A B7A 109.4(7) . . ? C2A B11A B7A 58.0(5) . . ? B10A B11A B7A 108.6(7) . . ? B12A B11A B7A 60.5(6) . . ? B6A B11A H11A 120.8 . . ? C2A B11A H11A 124.4 . . ? B10A B11A H11A 122.4 . . ? B12A B11A H11A 123.0 . . ? B7A B11A H11A 120.9 . . ? B10A B12A B9A 61.0(5) . . ? B10A B12A B11A 59.9(6) . . ? B9A B12A B11A 108.8(8) . . ? B10A B12A B7A 108.8(8) . . ? B9A B12A B7A 108.8(8) . . ? B11A B12A B7A 60.5(6) . . ? B10A B12A B8A 108.5(8) . . ? B9A B12A B8A 60.2(5) . . ? B11A B12A B8A 107.7(8) . . ? B7A B12A B8A 59.6(6) . . ? B10A B12A H12A 121.1 . . ? B9A B12A H12A 120.9 . . ? B11A B12A H12A 121.7 . . ? B7A B12A H12A 121.3 . . ? B8A B12A H12A 122.0 . . ? C4A B13A C3A 57.4(4) . . ? C4A B13A B17A 58.4(5) . . ? C3A B13A B17A 105.0(7) . . ? C4A B13A B14A 104.4(7) . . ? C3A B13A B14A 57.7(5) . . ? B17A B13A B14A 109.1(7) . . ? C4A B13A B18A 105.2(6) . . ? C3A B13A B18A 104.6(7) . . ? B17A B13A B18A 61.1(5) . . ? B14A B13A B18A 60.5(5) . . ? C4A B13A H13A 124.6 . . ? C3A B13A H13A 124.9 . . ? B17A B13A H13A 121.3 . . ? B14A B13A H13A 122.1 . . ? B18A B13A H13A 122.4 . . ? C3A B14A B15A 58.7(5) . . ? C3A B14A B13A 59.9(5) . . ? B15A B14A B13A 108.3(6) . . ? C3A B14A B18A 105.7(7) . . ? B15A B14A B18A 107.7(6) . . ? B13A B14A B18A 59.8(5) . . ? C3A B14A B19A 104.5(6) . . ? B15A B14A B19A 59.4(5) . . ? B13A B14A B19A 107.3(7) . . ? B18A B14A B19A 59.6(5) . . ? C3A B14A H14A 124.0 . . ? B15A B14A H14A 121.7 . . ? B13A B14A H14A 121.3 . . ? B18A B14A H14A 122.3 . . ? B19A B14A H14A 123.1 . . ? C3A B15A B14A 58.4(5) . . ? C3A B15A B19A 105.7(7) . . ? B14A B15A B19A 61.1(5) . . ? C3A B15A B16A 59.3(5) . . ? B14A B15A B16A 108.2(7) . . ? B19A B15A B16A 107.9(7) . . ? C3A B15A B20A 105.5(7) . . ? B14A B15A B20A 108.6(8) . . ? B19A B15A B20A 59.6(5) . . ? B16A B15A B20A 59.9(5) . . ? C3A B15A H15A 124.2 . . ? B14A B15A H15A 121.1 . . ? B19A B15A H15A 122.0 . . ? B16A B15A H15A 121.5 . . ? B20A B15A H15A 122.2 . . ? C4A B16A C3A 57.4(5) . . ? C4A B16A B20A 104.7(7) . . ? C3A B16A B20A 104.8(6) . . ? C4A B16A B15A 104.1(6) . . ? C3A B16A B15A 58.1(5) . . ? B20A B16A B15A 60.1(5) . . ? C4A B16A B21A 58.3(5) . . ? C3A B16A B21A 104.9(7) . . ? B20A B16A B21A 60.5(5) . . ? B15A B16A B21A 108.2(7) . . ? C4A B16A H16A 124.8 . . ? C3A B16A H16A 124.6 . . ? B20A B16A H16A 122.7 . . ? B15A B16A H16A 122.4 . . ? B21A B16A H16A 121.9 . . ? C4A B17A B22A 104.6(7) . . ? C4A B17A B13A 59.1(4) . . ? B22A B17A B13A 107.9(7) . . ? C4A B17A B21A 59.1(5) . . ? B22A B17A B21A 59.8(5) . . ? B13A B17A B21A 108.7(7) . . ? C4A B17A B18A 104.7(6) . . ? B22A B17A B18A 59.8(5) . . ? B13A B17A B18A 59.9(5) . . ? B21A B17A B18A 107.9(8) . . ? C4A B17A H17A 124.6 . . ? B22A B17A H17A 122.7 . . ? B13A B17A H17A 121.2 . . ? B21A B17A H17A 121.3 . . ? B18A B17A H17A 122.6 . . ? B22A B18A B13A 106.4(7) . . ? B22A B18A B19A 60.6(5) . . ? B13A B18A B19A 107.9(7) . . ? B22A B18A B14A 108.1(7) . . ? B13A B18A B14A 59.7(5) . . ? B19A B18A B14A 60.5(5) . . ? B22A B18A B17A 58.8(5) . . ? B13A B18A B17A 59.0(5) . . ? B19A B18A B17A 107.4(7) . . ? B14A B18A B17A 106.8(6) . . ? B22A B18A H18A 122.2 . . ? B13A B18A H18A 122.6 . . ? B19A B18A H18A 121.2 . . ? B14A B18A H18A 121.7 . . ? B17A B18A H18A 122.9 . . ? B20A B19A B15A 60.4(5) . . ? B20A B19A B18A 108.6(7) . . ? B15A B19A B18A 107.9(6) . . ? B20A B19A B22A 60.3(5) . . ? B15A B19A B22A 107.7(7) . . ? B18A B19A B22A 59.4(5) . . ? B20A B19A B14A 107.9(6) . . ? B15A B19A B14A 59.4(5) . . ? B18A B19A B14A 59.9(5) . . ? B22A B19A B14A 106.6(7) . . ? B20A B19A H19A 121.1 . . ? B15A B19A H19A 121.8 . . ? B18A B19A H19A 121.7 . . ? B22A B19A H19A 122.4 . . ? B14A B19A H19A 122.4 . . ? B19A B20A B16A 108.2(6) . . ? B19A B20A B15A 60.0(5) . . ? B16A B20A B15A 60.0(5) . . ? B19A B20A B22A 60.7(5) . . ? B16A B20A B22A 106.8(7) . . ? B15A B20A B22A 107.5(7) . . ? B19A B20A B21A 107.9(7) . . ? B16A B20A B21A 59.9(5) . . ? B15A B20A B21A 107.6(6) . . ? B22A B20A B21A 58.7(6) . . ? B19A B20A H20A 121.2 . . ? B16A B20A H20A 122.0 . . ? B15A B20A H20A 121.9 . . ? B22A B20A H20A 122.5 . . ? B21A B20A H20A 122.2 . . ? C4A B21A B22A 104.0(6) . . ? C4A B21A B17A 58.2(5) . . ? B22A B21A B17A 59.7(5) . . ? C4A B21A B16A 59.0(5) . . ? B22A B21A B16A 107.9(7) . . ? B17A B21A B16A 108.1(6) . . ? C4A B21A B20A 104.4(6) . . ? B22A B21A B20A 60.5(6) . . ? B17A B21A B20A 108.2(7) . . ? B16A B21A B20A 59.5(5) . . ? C4A B21A H21A 125.2 . . ? B22A B21A H21A 122.5 . . ? B17A B21A H21A 121.5 . . ? B16A B21A H21A 121.4 . . ? B20A B21A H21A 122.3 . . ? B17A B22A B21A 60.5(5) . . ? B17A B22A B18A 61.4(5) . . ? B21A B22A B18A 109.7(6) . . ? B17A B22A B20A 109.0(7) . . ? B21A B22A B20A 60.8(5) . . ? B18A B22A B20A 108.0(6) . . ? B17A B22A B19A 109.0(6) . . ? B21A B22A B19A 108.3(7) . . ? B18A B22A B19A 60.1(5) . . ? B20A B22A B19A 59.0(5) . . ? B17A B22A H22A 120.6 . . ? B21A B22A H22A 120.9 . . ? B18A B22A H22A 120.9 . . ? B20A B22A H22A 121.8 . . ? B19A B22A H22A 122.0 . . ? C8B Co1B C6B 65.5(8) . . ? C8B Co1B C5B 64.8(6) . . ? C6B Co1B C5B 35.4(5) . . ? C8B Co1B C7B 39.2(6) . . ? C6B Co1B C7B 38.2(6) . . ? C5B Co1B C7B 61.6(7) . . ? C8B Co1B C9B 38.2(5) . . ? C6B Co1B C9B 63.2(5) . . ? C5B Co1B C9B 39.1(4) . . ? C7B Co1B C9B 63.0(7) . . ? C8B Co1B S2B 104.3(6) . . ? C6B Co1B S2B 144.6(8) . . ? C5B Co1B S2B 168.7(5) . . ? C7B Co1B S2B 112.2(7) . . ? C9B Co1B S2B 130.2(7) . . ? C8B Co1B S1B 156.3(9) . . ? C6B Co1B S1B 115.6(7) . . ? C5B Co1B S1B 101.7(4) . . ? C7B Co1B S1B 152.4(10) . . ? C9B Co1B S1B 119.2(7) . . ? S2B Co1B S1B 87.50(9) . . ? C8B Co1B Ni1B 142.2(9) . . ? C6B Co1B Ni1B 107.1(5) . . ? C5B Co1B Ni1B 131.3(7) . . ? C7B Co1B Ni1B 111.4(7) . . ? C9B Co1B Ni1B 170.0(5) . . ? S2B Co1B Ni1B 59.02(6) . . ? S1B Co1B Ni1B 61.41(7) . . ? C10B Co2B C11B 40.6(3) . . ? C10B Co2B C13B 67.6(4) . . ? C11B Co2B C13B 66.4(4) . . ? C10B Co2B C12B 67.5(4) . . ? C11B Co2B C12B 38.7(3) . . ? C13B Co2B C12B 40.4(3) . . ? C10B Co2B C14B 40.4(3) . . ? C11B Co2B C14B 66.9(4) . . ? C13B Co2B C14B 39.6(3) . . ? C12B Co2B C14B 67.0(4) . . ? C10B Co2B S3B 165.2(4) . . ? C11B Co2B S3B 147.8(4) . . ? C13B Co2B S3B 103.0(3) . . ? C12B Co2B S3B 113.5(4) . . ? C14B Co2B S3B 125.2(4) . . ? C10B Co2B S4B 102.6(3) . . ? C11B Co2B S4B 103.5(3) . . ? C13B Co2B S4B 169.3(3) . . ? C12B Co2B S4B 133.0(4) . . ? C14B Co2B S4B 134.6(4) . . ? S3B Co2B S4B 87.41(9) . . ? C10B Co2B Ni1B 115.7(4) . . ? C11B Co2B Ni1B 151.4(4) . . ? C13B Co2B Ni1B 126.6(3) . . ? C12B Co2B Ni1B 166.0(4) . . ? C14B Co2B Ni1B 105.9(3) . . ? S3B Co2B Ni1B 59.74(7) . . ? S4B Co2B Ni1B 60.76(7) . . ? S2B Ni1B S3B 140.24(9) . . ? S2B Ni1B S4B 110.33(9) . . ? S3B Ni1B S4B 83.02(8) . . ? S2B Ni1B S1B 83.09(8) . . ? S3B Ni1B S1B 116.39(9) . . ? S4B Ni1B S1B 131.91(9) . . ? S2B Ni1B Co2B 98.95(7) . . ? S3B Ni1B Co2B 56.48(7) . . ? S4B Ni1B Co2B 56.30(7) . . ? S1B Ni1B Co2B 170.33(8) . . ? S2B Ni1B Co1B 56.66(7) . . ? S3B Ni1B Co1B 103.92(7) . . ? S4B Ni1B Co1B 165.99(7) . . ? S1B Ni1B Co1B 56.05(6) . . ? Co2B Ni1B Co1B 117.29(6) . . ? C1B S1B Co1B 101.7(3) . . ? C1B S1B Ni1B 100.1(3) . . ? Co1B S1B Ni1B 62.54(7) . . ? C2B S2B Co1B 102.6(3) . . ? C2B S2B Ni1B 101.7(2) . . ? Co1B S2B Ni1B 64.32(7) . . ? C3B S3B Co2B 101.8(3) . . ? C3B S3B Ni1B 102.3(3) . . ? Co2B S3B Ni1B 63.78(7) . . ? C4B S4B Co2B 102.6(3) . . ? C4B S4B Ni1B 101.4(2) . . ? Co2B S4B Ni1B 62.94(7) . . ? C2B C1B B3B 63.1(5) . . ? C2B C1B B4B 111.0(6) . . ? B3B C1B B4B 61.0(5) . . ? C2B C1B B5B 110.7(6) . . ? B3B C1B B5B 112.5(7) . . ? B4B C1B B5B 61.5(5) . . ? C2B C1B B6B 61.6(5) . . ? B3B C1B B6B 114.2(6) . . ? B4B C1B B6B 111.4(7) . . ? B5B C1B B6B 61.0(5) . . ? C2B C1B S1B 114.7(6) . . ? B3B C1B S1B 117.2(6) . . ? B4B C1B S1B 125.0(5) . . ? B5B C1B S1B 123.3(6) . . ? B6B C1B S1B 116.3(6) . . ? C1B C2B B7B 111.9(7) . . ? C1B C2B B11B 111.5(7) . . ? B7B C2B B11B 62.1(5) . . ? C1B C2B B6B 63.1(5) . . ? B7B C2B B6B 113.3(7) . . ? B11B C2B B6B 61.1(5) . . ? C1B C2B B3B 61.1(5) . . ? B7B C2B B3B 62.1(5) . . ? B11B C2B B3B 112.4(7) . . ? B6B C2B B3B 113.8(6) . . ? C1B C2B S2B 112.4(6) . . ? B7B C2B S2B 125.8(6) . . ? B11B C2B S2B 124.1(6) . . ? B6B C2B S2B 113.7(6) . . ? B3B C2B S2B 118.3(6) . . ? C4B C3B B15B 112.7(6) . . ? C4B C3B B16B 61.0(5) . . ? B15B C3B B16B 63.5(6) . . ? C4B C3B B13B 62.7(5) . . ? B15B C3B B13B 114.4(6) . . ? B16B C3B B13B 114.5(6) . . ? C4B C3B B14B 113.3(6) . . ? B15B C3B B14B 63.4(5) . . ? B16B C3B B14B 116.0(6) . . ? B13B C3B B14B 62.0(5) . . ? C4B C3B S3B 112.0(5) . . ? B15B C3B S3B 123.8(6) . . ? B16B C3B S3B 114.5(6) . . ? B13B C3B S3B 115.4(6) . . ? B14B C3B S3B 123.5(6) . . ? C3B C4B B16B 61.6(5) . . ? C3B C4B B21B 111.4(6) . . ? B16B C4B B21B 62.7(5) . . ? C3B C4B B13B 61.4(5) . . ? B16B C4B B13B 113.9(6) . . ? B21B C4B B13B 113.3(6) . . ? C3B C4B B17B 109.3(6) . . ? B16B C4B B17B 113.5(6) . . ? B21B C4B B17B 62.8(5) . . ? B13B C4B B17B 60.4(5) . . ? C3B C4B S4B 114.2(5) . . ? B16B C4B S4B 116.9(5) . . ? B21B C4B S4B 124.8(6) . . ? B13B C4B S4B 114.9(6) . . ? B17B C4B S4B 124.4(5) . . ? C6B C5B C9B 110.2(18) . . ? C6B C5B Co1B 71.6(10) . . ? C9B C5B Co1B 71.5(7) . . ? C6B C5B H5BA 124.9 . . ? C9B C5B H5BA 124.9 . . ? Co1B C5B H5BA 124.9 . . ? C5B C6B C7B 109(2) . . ? C5B C6B Co1B 73.0(11) . . ? C7B C6B Co1B 72.3(10) . . ? C5B C6B H6BA 125.2 . . ? C7B C6B H6BA 125.2 . . ? Co1B C6B H6BA 125.2 . . ? C6B C7B C8B 107.7(19) . . ? C6B C7B Co1B 69.6(11) . . ? C8B C7B Co1B 68.4(9) . . ? C6B C7B H7BA 126.1 . . ? C8B C7B H7BA 126.1 . . ? Co1B C7B H7BA 126.1 . . ? C9B C8B C7B 105.9(19) . . ? C9B C8B Co1B 73.3(8) . . ? C7B C8B Co1B 72.4(10) . . ? C9B C8B H8BA 126.7 . . ? C7B C8B H8BA 126.7 . . ? Co1B C8B H8BA 126.7 . . ? C8B C9B C5B 106.3(16) . . ? C8B C9B Co1B 68.5(8) . . ? C5B C9B Co1B 69.4(6) . . ? C8B C9B H9BA 126.9 . . ? C5B C9B H9BA 126.9 . . ? Co1B C9B H9BA 126.9 . . ? C11B C10B C14B 105.9(10) . . ? C11B C10B Co2B 69.8(5) . . ? C14B C10B Co2B 70.7(5) . . ? C11B C10B H10D 127.0 . . ? C14B C10B H10D 127.0 . . ? Co2B C10B H10D 127.0 . . ? C12B C11B C10B 110.1(10) . . ? C12B C11B Co2B 71.1(6) . . ? C10B C11B Co2B 69.7(5) . . ? C12B C11B H11D 124.9 . . ? C10B C11B H11D 124.9 . . ? Co2B C11B H11D 124.9 . . ? C11B C12B C13B 107.8(11) . . ? C11B C12B Co2B 70.2(6) . . ? C13B C12B Co2B 69.8(6) . . ? C11B C12B H12D 126.1 . . ? C13B C12B H12D 126.1 . . ? Co2B C12B H12D 126.1 . . ? C14B C13B C12B 107.9(11) . . ? C14B C13B Co2B 70.6(6) . . ? C12B C13B Co2B 69.8(6) . . ? C14B C13B H13D 126.0 . . ? C12B C13B H13D 126.0 . . ? Co2B C13B H13D 126.0 . . ? C13B C14B C10B 108.2(10) . . ? C13B C14B Co2B 69.8(5) . . ? C10B C14B Co2B 68.9(5) . . ? C13B C14B H14D 125.9 . . ? C10B C14B H14D 125.9 . . ? Co2B C14B H14D 125.9 . . ? C1B B3B B8B 106.9(8) . . ? C1B B3B B4B 59.8(5) . . ? B8B B3B B4B 61.2(6) . . ? C1B B3B C2B 55.8(4) . . ? B8B B3B C2B 105.1(7) . . ? B4B B3B C2B 104.2(6) . . ? C1B B3B B7B 104.0(6) . . ? B8B B3B B7B 61.2(6) . . ? B4B B3B B7B 109.2(8) . . ? C2B B3B B7B 57.8(5) . . ? C1B B3B H3B 124.3 . . ? B8B B3B H3B 121.3 . . ? B4B B3B H3B 121.3 . . ? C2B B3B H3B 125.8 . . ? B7B B3B H3B 122.1 . . ? C1B B4B B3B 59.2(5) . . ? C1B B4B B8B 104.7(7) . . ? B3B B4B B8B 58.9(6) . . ? C1B B4B B9B 106.4(7) . . ? B3B B4B B9B 108.1(7) . . ? B8B B4B B9B 60.1(5) . . ? C1B B4B B5B 59.7(5) . . ? B3B B4B B5B 109.5(7) . . ? B8B B4B B5B 109.3(7) . . ? B9B B4B B5B 61.4(5) . . ? C1B B4B H4B 124.0 . . ? B3B B4B H4B 121.5 . . ? B8B B4B H4B 122.7 . . ? B9B B4B H4B 121.6 . . ? B5B B4B H4B 119.9 . . ? C1B B5B B4B 58.7(5) . . ? C1B B5B B6B 59.9(5) . . ? B4B B5B B6B 108.2(8) . . ? C1B B5B B9B 104.1(7) . . ? B4B B5B B9B 59.3(5) . . ? B6B B5B B9B 106.4(7) . . ? C1B B5B B10B 104.1(7) . . ? B4B B5B B10B 106.0(7) . . ? B6B B5B B10B 59.0(5) . . ? B9B B5B B10B 58.5(5) . . ? C1B B5B H5B 124.3 . . ? B4B B5B H5B 121.9 . . ? B6B B5B H5B 121.4 . . ? B9B B5B H5B 123.6 . . ? B10B B5B H5B 123.9 . . ? C2B B6B B11B 58.9(5) . . ? C2B B6B C1B 55.3(4) . . ? B11B B6B C1B 103.6(6) . . ? C2B B6B B10B 104.7(7) . . ? B11B B6B B10B 59.7(6) . . ? C1B B6B B10B 105.5(7) . . ? C2B B6B B5B 104.2(6) . . ? B11B B6B B5B 108.8(8) . . ? C1B B6B B5B 59.1(5) . . ? B10B B6B B5B 61.5(6) . . ? C2B B6B H6B 125.3 . . ? B11B B6B H6B 122.3 . . ? C1B B6B H6B 125.2 . . ? B10B B6B H6B 122.2 . . ? B5B B6B H6B 121.3 . . ? C2B B7B B11B 59.2(5) . . ? C2B B7B B12B 105.5(7) . . ? B11B B7B B12B 59.8(6) . . ? C2B B7B B3B 60.1(5) . . ? B11B B7B B3B 108.4(7) . . ? B12B B7B B3B 106.8(8) . . ? C2B B7B B8B 104.5(7) . . ? B11B B7B B8B 107.0(9) . . ? B12B B7B B8B 59.7(6) . . ? B3B B7B B8B 58.0(5) . . ? C2B B7B H7B 123.7 . . ? B11B B7B H7B 121.5 . . ? B12B B7B H7B 122.6 . . ? B3B B7B H7B 121.9 . . ? B8B B7B H7B 123.6 . . ? B3B B8B B4B 59.9(5) . . ? B3B B8B B12B 109.3(8) . . ? B4B B8B B12B 108.2(7) . . ? B3B B8B B9B 108.8(7) . . ? B4B B8B B9B 60.1(6) . . ? B12B B8B B9B 60.3(6) . . ? B3B B8B B7B 60.9(6) . . ? B4B B8B B7B 107.9(7) . . ? B12B B8B B7B 59.9(6) . . ? B9B B8B B7B 108.1(7) . . ? B3B B8B H8B 120.8 . . ? B4B B8B H8B 122.0 . . ? B12B B8B H8B 121.3 . . ? B9B B8B H8B 121.5 . . ? B7B B8B H8B 121.7 . . ? B10B B9B B4B 107.8(7) . . ? B10B B9B B8B 107.5(8) . . ? B4B B9B B8B 59.8(6) . . ? B10B B9B B12B 59.7(6) . . ? B4B B9B B12B 107.6(8) . . ? B8B B9B B12B 59.8(6) . . ? B10B B9B B5B 60.8(5) . . ? B4B B9B B5B 59.3(5) . . ? B8B B9B B5B 107.4(8) . . ? B12B B9B B5B 108.2(8) . . ? B10B B9B H9B 121.7 . . ? B4B B9B H9B 122.1 . . ? B8B B9B H9B 122.2 . . ? B12B B9B H9B 121.8 . . ? B5B B9B H9B 121.7 . . ? B11B B10B B6B 59.7(6) . . ? B11B B10B B12B 60.2(6) . . ? B6B B10B B12B 108.6(8) . . ? B11B B10B B9B 108.3(8) . . ? B6B B10B B9B 108.6(7) . . ? B12B B10B B9B 60.5(6) . . ? B11B B10B B5B 107.2(8) . . ? B6B B10B B5B 59.5(5) . . ? B12B B10B B5B 108.8(7) . . ? B9B B10B B5B 60.7(5) . . ? B11B B10B H10B 122.1 . . ? B6B B10B H10B 121.7 . . ? B12B B10B H10B 121.0 . . ? B9B B10B H10B 121.0 . . ? B5B B10B H10B 121.8 . . ? C2B B11B B10B 106.3(7) . . ? C2B B11B B6B 60.0(5) . . ? B10B B11B B6B 60.6(6) . . ? C2B B11B B7B 58.7(5) . . ? B10B B11B B7B 109.1(8) . . ? B6B B11B B7B 109.6(7) . . ? C2B B11B B12B 105.7(7) . . ? B10B B11B B12B 60.4(7) . . ? B6B B11B B12B 109.5(9) . . ? B7B B11B B12B 60.5(6) . . ? C2B B11B H11B 124.0 . . ? B10B B11B H11B 121.6 . . ? B6B B11B H11B 120.2 . . ? B7B B11B H11B 120.9 . . ? B12B B11B H11B 121.8 . . ? B11B B12B B10B 59.4(6) . . ? B11B B12B B8B 107.5(8) . . ? B10B B12B B8B 107.7(7) . . ? B11B B12B B7B 59.7(6) . . ? B10B B12B B7B 107.7(8) . . ? B8B B12B B7B 60.4(6) . . ? B11B B12B B9B 107.1(8) . . ? B10B B12B B9B 59.8(6) . . ? B8B B12B B9B 59.9(5) . . ? B7B B12B B9B 108.2(7) . . ? B11B B12B H12B 122.4 . . ? B10B B12B H12B 122.1 . . ? B8B B12B H12B 121.7 . . ? B7B B12B H12B 121.5 . . ? B9B B12B H12B 121.9 . . ? C3B B13B C4B 55.8(5) . . ? C3B B13B B17B 104.5(7) . . ? C4B B13B B17B 59.9(5) . . ? C3B B13B B18B 104.5(7) . . ? C4B B13B B18B 106.1(7) . . ? B17B B13B B18B 60.8(5) . . ? C3B B13B B14B 59.0(5) . . ? C4B B13B B14B 105.3(7) . . ? B17B B13B B14B 109.5(7) . . ? B18B B13B B14B 60.3(5) . . ? C3B B13B H13B 125.5 . . ? C4B B13B H13B 124.1 . . ? B17B B13B H13B 121.2 . . ? B18B B13B H13B 122.4 . . ? B14B B13B H13B 121.4 . . ? C3B B14B B13B 59.0(5) . . ? C3B B14B B18B 103.7(7) . . ? B13B B14B B18B 59.4(5) . . ? C3B B14B B15B 57.0(5) . . ? B13B B14B B15B 106.7(7) . . ? B18B B14B B15B 107.0(8) . . ? C3B B14B B19B 101.7(7) . . ? B13B B14B B19B 106.3(7) . . ? B18B B14B B19B 59.9(5) . . ? B15B B14B B19B 58.8(6) . . ? C3B B14B H14B 126.0 . . ? B13B B14B H14B 122.0 . . ? B18B B14B H14B 122.6 . . ? B15B B14B H14B 122.6 . . ? B19B B14B H14B 123.9 . . ? C3B B15B B19B 105.1(7) . . ? C3B B15B B20B 104.2(7) . . ? B19B B15B B20B 59.2(6) . . ? C3B B15B B16B 58.7(5) . . ? B19B B15B B16B 107.2(7) . . ? B20B B15B B16B 59.3(5) . . ? C3B B15B B14B 59.6(5) . . ? B19B B15B B14B 60.7(6) . . ? B20B B15B B14B 108.3(7) . . ? B16B B15B B14B 108.9(7) . . ? C3B B15B H15B 124.5 . . ? B19B B15B H15B 122.6 . . ? B20B B15B H15B 123.0 . . ? B16B B15B H15B 121.7 . . ? B14B B15B H15B 120.4 . . ? C4B B16B C3B 57.4(5) . . ? C4B B16B B20B 106.0(7) . . ? C3B B16B B20B 104.0(8) . . ? C4B B16B B21B 59.3(5) . . ? C3B B16B B21B 105.4(7) . . ? B20B B16B B21B 61.6(5) . . ? C4B B16B B15B 105.1(7) . . ? C3B B16B B15B 57.8(5) . . ? B20B B16B B15B 60.1(5) . . ? B21B B16B B15B 109.8(7) . . ? C4B B16B H16B 123.9 . . ? C3B B16B H16B 125.2 . . ? B20B B16B H16B 122.5 . . ? B21B B16B H16B 120.7 . . ? B15B B16B H16B 121.9 . . ? C4B B17B B13B 59.7(5) . . ? C4B B17B B22B 103.1(7) . . ? B13B B17B B22B 107.5(7) . . ? C4B B17B B18B 105.1(6) . . ? B13B B17B B18B 59.7(5) . . ? B22B B17B B18B 60.5(6) . . ? C4B B17B B21B 57.5(5) . . ? B13B B17B B21B 108.3(6) . . ? B22B B17B B21B 59.9(6) . . ? B18B B17B B21B 109.0(7) . . ? C4B B17B H17B 125.3 . . ? B13B B17B H17B 121.3 . . ? B22B B17B H17B 123.1 . . ? B18B B17B H17B 121.7 . . ? B21B B17B H17B 121.4 . . ? B13B B18B B14B 60.3(5) . . ? B13B B18B B17B 59.5(5) . . ? B14B B18B B17B 108.5(6) . . ? B13B B18B B19B 107.6(7) . . ? B14B B18B B19B 60.5(6) . . ? B17B B18B B19B 107.2(8) . . ? B13B B18B B22B 106.4(7) . . ? B14B B18B B22B 107.9(8) . . ? B17B B18B B22B 59.3(6) . . ? B19B B18B B22B 59.3(6) . . ? B13B B18B H18B 122.4 . . ? B14B B18B H18B 121.0 . . ? B17B B18B H18B 122.0 . . ? B19B B18B H18B 122.0 . . ? B22B B18B H18B 122.7 . . ? B20B B19B B15B 60.6(5) . . ? B20B B19B B22B 59.8(6) . . ? B15B B19B B22B 107.9(7) . . ? B20B B19B B18B 108.8(8) . . ? B15B B19B B18B 108.2(7) . . ? B22B B19B B18B 60.4(6) . . ? B20B B19B B14B 109.3(7) . . ? B15B B19B B14B 60.5(5) . . ? B22B B19B B14B 107.9(7) . . ? B18B B19B B14B 59.6(6) . . ? B20B B19B H19B 120.9 . . ? B15B B19B H19B 121.5 . . ? B22B B19B H19B 122.0 . . ? B18B B19B H19B 121.6 . . ? B14B B19B H19B 121.4 . . ? B19B B20B B22B 60.7(6) . . ? B19B B20B B16B 108.9(8) . . ? B22B B20B B16B 107.5(7) . . ? B19B B20B B15B 60.1(6) . . ? B22B B20B B15B 108.2(9) . . ? B16B B20B B15B 60.6(5) . . ? B19B B20B B21B 109.4(8) . . ? B22B B20B B21B 60.2(6) . . ? B16B B20B B21B 59.5(5) . . ? B15B B20B B21B 108.6(7) . . ? B19B B20B H20B 120.7 . . ? B22B B20B H20B 121.8 . . ? B16B B20B H20B 121.8 . . ? B15B B20B H20B 121.4 . . ? B21B B20B H20B 121.3 . . ? C4B B21B B16B 58.1(5) . . ? C4B B21B B22B 104.0(7) . . ? B16B B21B B22B 105.7(8) . . ? C4B B21B B20B 103.0(7) . . ? B16B B21B B20B 58.9(5) . . ? B22B B21B B20B 58.4(6) . . ? C4B B21B B17B 59.7(5) . . ? B16B B21B B17B 107.2(7) . . ? B22B B21B B17B 58.9(6) . . ? B20B B21B B17B 105.5(8) . . ? C4B B21B H21B 124.7 . . ? B16B B21B H21B 122.5 . . ? B22B B21B H21B 123.7 . . ? B20B B21B H21B 124.2 . . ? B17B B21B H21B 122.0 . . ? B20B B22B B17B 109.8(7) . . ? B20B B22B B19B 59.5(6) . . ? B17B B22B B19B 108.8(8) . . ? B20B B22B B21B 61.4(6) . . ? B17B B22B B21B 61.2(5) . . ? B19B B22B B21B 109.5(7) . . ? B20B B22B B18B 108.5(8) . . ? B17B B22B B18B 60.3(6) . . ? B19B B22B B18B 60.3(6) . . ? B21B B22B B18B 109.9(7) . . ? B20B B22B H22B 121.1 . . ? B17B B22B H22B 120.8 . . ? B19B B22B H22B 121.6 . . ? B21B B22B H22B 120.0 . . ? B18B B22B H22B 121.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.564 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.083 # Attachment '12_bi_CpSCN4Phcarbs_f41219a.cif' data_f41219a _database_code_depnum_ccdc_archive 'CCDC 621989' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 B9 Co2 N8 S4' _chemical_formula_weight 773.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.789(12) _cell_length_b 9.574(3) _cell_length_c 23.449(8) _cell_angle_alpha 90.00 _cell_angle_beta 117.630(5) _cell_angle_gamma 90.00 _cell_volume 7118(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 915 _cell_measurement_theta_min 2.305 _cell_measurement_theta_max 27.184 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8896 _exptl_absorpt_correction_T_max 0.9425 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.83 _diffrn_reflns_number 14278 _diffrn_reflns_av_R_equivalents 0.1044 _diffrn_reflns_av_sigmaI/netI 0.1399 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6246 _reflns_number_gt 3207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0758P)^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 6246 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1522 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.1863 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.20368(3) 0.46076(9) 0.02952(5) 0.0469(3) Uani 1 1 d . . . Co3 Co 0.14675(3) 0.17869(10) 0.05387(5) 0.0457(3) Uani 1 1 d . . . N1 N 0.14000(19) 0.1459(6) -0.0324(3) 0.0476(15) Uani 1 1 d . . . N2 N 0.1272(2) 0.0184(7) -0.0613(3) 0.0620(18) Uani 1 1 d . . . N3 N 0.1201(2) 0.0265(7) -0.1208(3) 0.068(2) Uani 1 1 d . . . N4 N 0.1276(2) 0.1607(7) -0.1318(3) 0.0596(18) Uani 1 1 d . . . N5 N 0.0867(2) 0.1941(7) 0.0181(3) 0.0543(17) Uani 1 1 d . . . N6 N 0.0551(2) 0.1771(7) -0.0428(3) 0.0645(19) Uani 1 1 d . . . N7 N 0.0191(2) 0.2057(8) -0.0447(4) 0.072(2) Uani 1 1 d . . . N8 N 0.0273(2) 0.2478(7) 0.0157(3) 0.0593(18) Uani 1 1 d . . . S1 S 0.23276(6) 0.24872(18) 0.05400(9) 0.0470(5) Uani 1 1 d . . . S2 S 0.16271(6) 0.42060(18) 0.07554(9) 0.0482(5) Uani 1 1 d . . . S3 S 0.15108(7) 0.4091(2) -0.07048(10) 0.0592(6) Uani 1 1 d . . . S4 S 0.09750(7) 0.2735(3) 0.13441(11) 0.0661(6) Uani 1 1 d . . . B4 B 0.1469(3) 0.1898(9) 0.1417(5) 0.050(2) Uani 1 1 d . . . B5 B 0.1952(3) 0.2445(9) 0.2058(4) 0.050(2) Uani 1 1 d . . . H5 H 0.1963 0.3222 0.2411 0.061 Uiso 1 1 calc R . . B6 B 0.2350(3) 0.2367(9) 0.1797(4) 0.046(2) Uani 1 1 d . . . H6 H 0.2618 0.3097 0.1985 0.055 Uiso 1 1 calc R . . B7 B 0.2394(3) 0.0603(8) 0.1583(4) 0.047(2) Uani 1 1 d . . . H7 H 0.2696 0.0179 0.1644 0.057 Uiso 1 1 calc R . . B8 B 0.1888(3) 0.0128(9) 0.0915(4) 0.053(2) Uani 1 1 d . . . H8 H 0.1863 -0.0626 0.0545 0.064 Uiso 1 1 calc R . . B9 B 0.1504(3) 0.0136(9) 0.1185(4) 0.057(3) Uani 1 1 d . . . H9 H 0.1240 -0.0609 0.0999 0.069 Uiso 1 1 calc R . . B10 B 0.1759(3) 0.0691(9) 0.2014(4) 0.055(2) Uani 1 1 d . . . H10 H 0.1652 0.0316 0.2358 0.066 Uiso 1 1 calc R . . B11 B 0.2300(3) 0.0968(9) 0.2255(4) 0.052(2) Uani 1 1 d . . . H11 H 0.2541 0.0769 0.2752 0.063 Uiso 1 1 calc R . . B12 B 0.2022(3) -0.0421(9) 0.1708(4) 0.055(2) Uani 1 1 d . . . H12 H 0.2087 -0.1525 0.1851 0.066 Uiso 1 1 calc R . . C1 C 0.1846(2) 0.2819(7) 0.1292(3) 0.0422(18) Uani 1 1 d . . . C2 C 0.2101(2) 0.1755(7) 0.1000(3) 0.0474(19) Uani 1 1 d . . . C3 C 0.2193(3) 0.6552(8) 0.0734(5) 0.073(3) Uani 1 1 d . . . H3A H 0.2083 0.6959 0.1010 0.088 Uiso 1 1 calc R . . C4 C 0.2545(3) 0.5718(9) 0.0938(4) 0.068(2) Uani 1 1 d . . . H4A H 0.2731 0.5447 0.1385 0.082 Uiso 1 1 calc R . . C5 C 0.2607(3) 0.5388(8) 0.0408(5) 0.066(2) Uani 1 1 d . . . H5A H 0.2840 0.4828 0.0421 0.080 Uiso 1 1 calc R . . C6 C 0.2279(3) 0.5930(9) -0.0140(5) 0.071(3) Uani 1 1 d . . . H6A H 0.2242 0.5842 -0.0579 0.085 Uiso 1 1 calc R . . C7 C 0.2010(3) 0.6698(8) 0.0049(5) 0.079(3) Uani 1 1 d . . . H7A H 0.1758 0.7235 -0.0231 0.095 Uiso 1 1 calc R . . C8 C 0.1402(2) 0.2345(8) -0.0762(4) 0.051(2) Uani 1 1 d . . . C9 C 0.1201(3) 0.2050(9) -0.1951(4) 0.063(2) Uani 1 1 d . . . C10 C 0.1510(3) 0.2710(10) -0.2027(4) 0.074(3) Uani 1 1 d . . . H10A H 0.1772 0.2873 -0.1676 0.089 Uiso 1 1 calc R . . C11 C 0.1428(4) 0.3133(11) -0.2636(5) 0.089(3) Uani 1 1 d . . . H11A H 0.1635 0.3599 -0.2698 0.107 Uiso 1 1 calc R . . C12 C 0.1049(5) 0.2872(13) -0.3143(5) 0.106(4) Uani 1 1 d . . . H12A H 0.0999 0.3149 -0.3553 0.127 Uiso 1 1 calc R . . C13 C 0.0738(4) 0.2210(16) -0.3065(5) 0.131(5) Uani 1 1 d . . . H13A H 0.0476 0.2044 -0.3416 0.157 Uiso 1 1 calc R . . C14 C 0.0822(3) 0.1789(13) -0.2446(5) 0.108(4) Uani 1 1 d . . . H14A H 0.0616 0.1331 -0.2380 0.129 Uiso 1 1 calc R . . C15 C 0.0687(3) 0.2390(8) 0.0534(4) 0.058(2) Uani 1 1 d . . . C16 C -0.0057(3) 0.2869(9) 0.0295(4) 0.062(2) Uani 1 1 d . . . C17 C -0.0418(3) 0.2086(11) 0.0071(5) 0.088(3) Uani 1 1 d . . . H17A H -0.0442 0.1289 -0.0170 0.106 Uiso 1 1 calc R . . C18 C -0.0738(4) 0.2436(14) 0.0190(6) 0.111(4) Uani 1 1 d . . . H18A H -0.0977 0.1877 0.0039 0.133 Uiso 1 1 calc R . . C19 C -0.0710(4) 0.3627(15) 0.0535(6) 0.110(4) Uani 1 1 d . . . H19A H -0.0930 0.3879 0.0620 0.131 Uiso 1 1 calc R . . C20 C -0.0359(4) 0.4431(11) 0.0751(5) 0.093(3) Uani 1 1 d . . . H20A H -0.0342 0.5237 0.0983 0.112 Uiso 1 1 calc R . . C21 C -0.0027(3) 0.4084(10) 0.0636(5) 0.085(3) Uani 1 1 d . . . H21A H 0.0212 0.4649 0.0783 0.102 Uiso 1 1 calc R . . C23 C 0.959(2) 0.241(5) 0.239(2) 0.52(5) Uani 1 1 d . . . C25 C 0.880(3) 0.321(7) 0.194(4) 0.38(6) Uani 0.50 1 d P . . C24 C 0.931(3) 0.376(7) 0.227(2) 0.79(9) Uani 1 1 d . . . C22 C 1.0000 0.328(5) 0.2500 0.34(4) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0725(8) 0.0261(5) 0.0540(6) -0.0017(5) 0.0393(6) -0.0024(5) Co3 0.0596(7) 0.0362(5) 0.0450(6) -0.0023(5) 0.0273(5) -0.0053(5) N1 0.066(4) 0.037(3) 0.047(4) -0.006(3) 0.032(3) -0.010(3) N2 0.081(5) 0.051(4) 0.055(4) -0.010(3) 0.032(4) -0.017(4) N3 0.097(6) 0.056(5) 0.052(4) -0.014(4) 0.034(4) -0.022(4) N4 0.078(5) 0.048(4) 0.051(4) -0.005(3) 0.029(4) -0.006(4) N5 0.066(5) 0.052(4) 0.042(4) -0.006(3) 0.023(4) -0.006(4) N6 0.061(5) 0.065(5) 0.066(5) -0.007(4) 0.028(4) -0.003(4) N7 0.061(5) 0.077(5) 0.077(5) 0.001(4) 0.030(4) -0.002(4) N8 0.059(5) 0.061(4) 0.060(4) 0.002(4) 0.030(4) -0.001(4) S1 0.0667(13) 0.0324(10) 0.0541(11) -0.0002(9) 0.0384(11) 0.0019(10) S2 0.0640(13) 0.0335(10) 0.0559(11) 0.0009(9) 0.0351(10) 0.0031(9) S3 0.0847(16) 0.0410(11) 0.0521(12) 0.0029(9) 0.0320(12) 0.0012(11) S4 0.0658(15) 0.0785(16) 0.0640(14) -0.0076(12) 0.0386(13) -0.0017(13) B4 0.043(5) 0.050(5) 0.065(6) -0.006(5) 0.031(5) -0.016(5) B5 0.073(6) 0.043(5) 0.043(5) 0.009(4) 0.033(5) 0.004(5) B6 0.056(6) 0.040(5) 0.046(5) -0.006(4) 0.028(5) -0.008(4) B7 0.062(6) 0.034(5) 0.051(5) -0.004(4) 0.030(5) 0.003(4) B8 0.080(7) 0.036(5) 0.047(5) 0.001(4) 0.032(5) -0.004(5) B9 0.085(7) 0.042(5) 0.047(5) 0.000(4) 0.032(5) -0.010(5) B10 0.069(7) 0.043(5) 0.060(6) 0.002(4) 0.037(5) -0.012(5) B11 0.073(7) 0.039(5) 0.046(5) 0.007(4) 0.029(5) 0.002(5) B12 0.084(7) 0.040(5) 0.046(5) 0.004(4) 0.034(5) -0.006(5) C1 0.058(5) 0.027(4) 0.048(4) -0.005(3) 0.030(4) -0.007(3) C2 0.078(6) 0.028(4) 0.043(4) -0.006(3) 0.034(4) -0.001(4) C3 0.118(8) 0.039(5) 0.093(7) -0.026(5) 0.075(7) -0.017(5) C4 0.091(7) 0.046(5) 0.075(6) -0.007(5) 0.045(6) -0.016(5) C5 0.075(6) 0.041(5) 0.106(7) -0.011(5) 0.061(6) -0.016(5) C6 0.099(8) 0.056(6) 0.071(6) -0.012(5) 0.051(6) -0.025(6) C7 0.105(8) 0.030(4) 0.104(8) 0.006(5) 0.050(7) -0.005(5) C8 0.060(5) 0.041(4) 0.053(5) -0.005(4) 0.026(4) -0.003(4) C9 0.075(6) 0.064(6) 0.045(5) -0.006(4) 0.025(5) -0.003(5) C10 0.089(7) 0.083(7) 0.053(5) 0.007(5) 0.035(5) 0.010(6) C11 0.126(9) 0.087(8) 0.065(6) 0.007(6) 0.054(7) 0.001(7) C12 0.147(12) 0.110(10) 0.053(7) 0.005(6) 0.041(8) 0.032(9) C13 0.111(10) 0.187(15) 0.054(7) -0.006(8) 0.003(7) -0.026(10) C14 0.083(8) 0.144(11) 0.072(7) 0.001(7) 0.016(6) -0.030(8) C15 0.049(5) 0.055(5) 0.053(5) 0.002(4) 0.009(5) -0.009(4) C16 0.045(5) 0.069(6) 0.071(6) 0.003(5) 0.027(5) -0.003(5) C17 0.071(7) 0.089(8) 0.113(8) -0.006(6) 0.050(7) 0.000(6) C18 0.087(9) 0.117(10) 0.144(11) -0.035(9) 0.066(8) -0.021(8) C19 0.072(8) 0.137(12) 0.131(11) -0.003(9) 0.057(8) 0.008(8) C20 0.107(9) 0.074(7) 0.112(9) 0.002(6) 0.063(8) 0.018(7) C21 0.082(7) 0.062(6) 0.120(9) -0.008(6) 0.056(7) -0.005(6) C23 0.86(13) 0.41(7) 0.46(7) -0.23(6) 0.45(9) -0.35(8) C25 0.71(17) 0.19(5) 0.35(10) 0.19(6) 0.33(11) 0.17(7) C24 1.4(2) 0.80(12) 0.22(4) 0.20(6) 0.45(10) 0.73(13) C22 0.61(11) 0.17(4) 0.17(3) 0.000 0.12(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C4 2.042(9) . ? Co1 C6 2.052(8) . ? Co1 C5 2.071(8) . ? Co1 C7 2.073(8) . ? Co1 C3 2.075(8) . ? Co1 S2 2.220(2) . ? Co1 S1 2.232(2) . ? Co1 S3 2.279(2) . ? Co3 N5 1.914(7) . ? Co3 C1 1.926(7) . ? Co3 N1 1.947(6) . ? Co3 C2 2.009(8) . ? Co3 B4 2.059(9) . ? Co3 B8 2.082(9) . ? Co3 B9 2.151(9) . ? Co3 S2 2.383(2) . ? N1 C8 1.335(9) . ? N1 N2 1.369(8) . ? N2 N3 1.300(8) . ? N3 N4 1.361(9) . ? N4 C8 1.363(9) . ? N4 C9 1.443(10) . ? N5 C15 1.335(10) . ? N5 N6 1.360(8) . ? N6 N7 1.298(9) . ? N7 N8 1.366(9) . ? N8 C15 1.331(9) . ? N8 C16 1.410(10) . ? S1 C2 1.767(7) . ? S2 C1 1.745(7) . ? S3 C8 1.707(8) . ? S4 C15 1.722(8) . ? S4 B4 1.874(9) . ? B4 B10 1.740(13) . ? B4 C1 1.746(10) . ? B4 B5 1.765(13) . ? B4 B9 1.795(12) . ? B5 C1 1.693(10) . ? B5 B6 1.793(12) . ? B5 B11 1.797(12) . ? B5 B10 1.801(12) . ? B5 H5 1.1000 . ? B6 C1 1.692(11) . ? B6 C2 1.757(10) . ? B6 B11 1.777(12) . ? B6 B7 1.789(11) . ? B6 H6 1.1000 . ? B7 C2 1.690(11) . ? B7 B12 1.784(12) . ? B7 B11 1.790(12) . ? B7 B8 1.818(13) . ? B7 H7 1.1000 . ? B8 C2 1.704(11) . ? B8 B9 1.760(13) . ? B8 B12 1.770(11) . ? B8 H8 1.1000 . ? B9 B12 1.765(13) . ? B9 B10 1.804(12) . ? B9 H9 1.1000 . ? B10 B11 1.769(13) . ? B10 B12 1.779(13) . ? B10 H10 1.1000 . ? B11 B12 1.795(12) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1 C2 1.709(9) . ? C3 C4 1.377(12) . ? C3 C7 1.434(12) . ? C3 H3A 0.9800 . ? C4 C5 1.394(11) . ? C4 H4A 0.9800 . ? C5 C6 1.378(12) . ? C5 H5A 0.9800 . ? C6 C7 1.433(12) . ? C6 H6A 0.9800 . ? C7 H7A 0.9800 . ? C9 C14 1.339(12) . ? C9 C10 1.357(11) . ? C10 C11 1.378(12) . ? C10 H10A 0.9300 . ? C11 C12 1.349(14) . ? C11 H11A 0.9300 . ? C12 C13 1.365(16) . ? C12 H12A 0.9300 . ? C13 C14 1.398(15) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C16 C17 1.372(12) . ? C16 C21 1.388(12) . ? C17 C18 1.338(13) . ? C17 H17A 0.9300 . ? C18 C19 1.376(15) . ? C18 H18A 0.9300 . ? C19 C20 1.355(14) . ? C19 H19A 0.9300 . ? C20 C21 1.377(12) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C23 C24 1.57(9) . ? C23 C22 1.61(4) . ? C25 C24 1.70(17) . ? C22 C23 1.61(4) 2_755 ? 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 C4 Co1 C6 67.0(3) . . ? C4 Co1 C5 39.6(3) . . ? C6 Co1 C5 39.0(3) . . ? C4 Co1 C7 67.3(4) . . ? C6 Co1 C7 40.7(3) . . ? C5 Co1 C7 66.6(4) . . ? C4 Co1 C3 39.1(3) . . ? C6 Co1 C3 67.3(3) . . ? C5 Co1 C3 65.8(3) . . ? C7 Co1 C3 40.5(3) . . ? C4 Co1 S2 107.1(3) . . ? C6 Co1 S2 150.9(3) . . ? C5 Co1 S2 146.5(3) . . ? C7 Co1 S2 110.3(3) . . ? C3 Co1 S2 90.1(3) . . ? C4 Co1 S1 97.7(3) . . ? C6 Co1 S1 115.8(3) . . ? C5 Co1 S1 88.9(3) . . ? C7 Co1 S1 154.9(3) . . ? C3 Co1 S1 134.6(3) . . ? S2 Co1 S1 92.96(7) . . ? C4 Co1 S3 154.3(3) . . ? C6 Co1 S3 87.7(3) . . ? C5 Co1 S3 120.3(3) . . ? C7 Co1 S3 90.8(3) . . ? C3 Co1 S3 127.6(3) . . ? S2 Co1 S3 92.64(9) . . ? S1 Co1 S3 97.55(8) . . ? N5 Co3 C1 122.0(3) . . ? N5 Co3 N1 89.1(3) . . ? C1 Co3 N1 137.0(3) . . ? N5 Co3 C2 173.4(3) . . ? C1 Co3 C2 51.5(3) . . ? N1 Co3 C2 97.0(3) . . ? N5 Co3 B4 85.2(3) . . ? C1 Co3 B4 51.8(3) . . ? N1 Co3 B4 171.1(3) . . ? C2 Co3 B4 89.1(3) . . ? N5 Co3 B8 133.5(3) . . ? C1 Co3 B8 86.5(3) . . ? N1 Co3 B8 92.0(3) . . ? C2 Co3 B8 49.2(3) . . ? B4 Co3 B8 87.1(4) . . ? N5 Co3 B9 93.1(3) . . ? C1 Co3 B9 86.8(3) . . ? N1 Co3 B9 123.4(3) . . ? C2 Co3 B9 85.7(3) . . ? B4 Co3 B9 50.4(3) . . ? B8 Co3 B9 49.1(4) . . ? N5 Co3 S2 97.3(2) . . ? C1 Co3 S2 46.3(2) . . ? N1 Co3 S2 106.25(18) . . ? C2 Co3 S2 78.5(2) . . ? B4 Co3 S2 81.2(2) . . ? B8 Co3 S2 126.6(3) . . ? B9 Co3 S2 129.3(2) . . ? C8 N1 N2 107.7(6) . . ? C8 N1 Co3 130.9(5) . . ? N2 N1 Co3 120.7(5) . . ? N3 N2 N1 109.4(6) . . ? N2 N3 N4 107.6(6) . . ? N3 N4 C8 108.4(6) . . ? N3 N4 C9 120.8(6) . . ? C8 N4 C9 130.7(7) . . ? C15 N5 N6 106.4(6) . . ? C15 N5 Co3 121.3(5) . . ? N6 N5 Co3 132.1(6) . . ? N7 N6 N5 109.9(7) . . ? N6 N7 N8 107.1(7) . . ? C15 N8 N7 107.9(7) . . ? C15 N8 C16 131.0(8) . . ? N7 N8 C16 121.0(7) . . ? C2 S1 Co1 103.1(2) . . ? C1 S2 Co1 107.8(2) . . ? C1 S2 Co3 52.9(2) . . ? Co1 S2 Co3 102.22(8) . . ? C8 S3 Co1 110.1(3) . . ? C15 S4 B4 94.3(4) . . ? B10 B4 C1 104.6(6) . . ? B10 B4 B5 61.8(5) . . ? C1 B4 B5 57.6(4) . . ? B10 B4 B9 61.3(5) . . ? C1 B4 B9 104.8(6) . . ? B5 B4 B9 111.0(7) . . ? B10 B4 S4 122.8(6) . . ? C1 B4 S4 122.5(6) . . ? B5 B4 S4 117.4(6) . . ? B9 B4 S4 124.8(6) . . ? B10 B4 Co3 119.7(6) . . ? C1 B4 Co3 60.1(4) . . ? B5 B4 Co3 114.5(5) . . ? B9 B4 Co3 67.5(4) . . ? S4 B4 Co3 111.5(5) . . ? C1 B5 B4 60.6(5) . . ? C1 B5 B6 58.0(4) . . ? B4 B5 B6 108.4(6) . . ? C1 B5 B11 103.1(6) . . ? B4 B5 B11 105.9(6) . . ? B6 B5 B11 59.3(5) . . ? C1 B5 B10 104.2(6) . . ? B4 B5 B10 58.4(5) . . ? B6 B5 B10 106.7(6) . . ? B11 B5 B10 58.9(5) . . ? C1 B5 H5 124.6 . . ? B4 B5 H5 121.5 . . ? B6 B5 H5 121.8 . . ? B11 B5 H5 124.0 . . ? B10 B5 H5 123.5 . . ? C1 B6 C2 59.4(4) . . ? C1 B6 B11 104.0(6) . . ? C2 B6 B11 104.4(6) . . ? C1 B6 B7 104.4(6) . . ? C2 B6 B7 56.9(4) . . ? B11 B6 B7 60.3(5) . . ? C1 B6 B5 58.0(5) . . ? C2 B6 B5 106.6(6) . . ? B11 B6 B5 60.4(5) . . ? B7 B6 B5 108.8(6) . . ? C1 B6 H6 124.5 . . ? C2 B6 H6 123.8 . . ? B11 B6 H6 123.3 . . ? B7 B6 H6 122.6 . . ? B5 B6 H6 121.2 . . ? C2 B7 B12 105.2(6) . . ? C2 B7 B6 60.6(4) . . ? B12 B7 B6 107.7(6) . . ? C2 B7 B11 106.6(6) . . ? B12 B7 B11 60.3(5) . . ? B6 B7 B11 59.5(5) . . ? C2 B7 B8 58.0(4) . . ? B12 B7 B8 58.9(5) . . ? B6 B7 B8 107.2(6) . . ? B11 B7 B8 106.8(6) . . ? C2 B7 H7 123.3 . . ? B12 B7 H7 122.6 . . ? B6 B7 H7 121.4 . . ? B11 B7 H7 122.1 . . ? B8 B7 H7 123.0 . . ? C2 B8 B9 109.6(6) . . ? C2 B8 B12 105.1(6) . . ? B9 B8 B12 60.0(5) . . ? C2 B8 B7 57.3(4) . . ? B9 B8 B7 108.7(6) . . ? B12 B8 B7 59.6(5) . . ? C2 B8 Co3 63.2(4) . . ? B9 B8 Co3 67.5(4) . . ? B12 B8 Co3 117.5(6) . . ? B7 B8 Co3 114.2(5) . . ? C2 B8 H8 124.1 . . ? B9 B8 H8 119.5 . . ? B12 B8 H8 121.1 . . ? B7 B8 H8 122.0 . . ? Co3 B8 H8 112.8 . . ? B8 B9 B12 60.3(5) . . ? B8 B9 B4 106.8(6) . . ? B12 B9 B4 105.8(6) . . ? B8 B9 B10 107.5(7) . . ? B12 B9 B10 59.8(5) . . ? B4 B9 B10 57.8(5) . . ? B8 B9 Co3 63.4(4) . . ? B12 B9 Co3 114.4(6) . . ? B4 B9 Co3 62.1(4) . . ? B10 B9 Co3 112.2(5) . . ? B8 B9 H9 121.8 . . ? B12 B9 H9 120.8 . . ? B4 B9 H9 124.1 . . ? B10 B9 H9 121.9 . . ? Co3 B9 H9 116.0 . . ? B4 B10 B11 108.2(6) . . ? B4 B10 B12 107.6(6) . . ? B11 B10 B12 60.8(5) . . ? B4 B10 B5 59.8(5) . . ? B11 B10 B5 60.4(5) . . ? B12 B10 B5 108.6(6) . . ? B4 B10 B9 60.8(5) . . ? B11 B10 B9 108.6(7) . . ? B12 B10 B9 59.0(5) . . ? B5 B10 B9 109.0(6) . . ? B4 B10 H10 121.8 . . ? B11 B10 H10 121.1 . . ? B12 B10 H10 121.9 . . ? B5 B10 H10 121.2 . . ? B9 B10 H10 121.4 . . ? B10 B11 B6 108.8(6) . . ? B10 B11 B7 108.4(6) . . ? B6 B11 B7 60.2(5) . . ? B10 B11 B12 59.9(5) . . ? B6 B11 B12 107.7(6) . . ? B7 B11 B12 59.7(5) . . ? B10 B11 B5 60.7(5) . . ? B6 B11 B5 60.2(5) . . ? B7 B11 B5 108.6(6) . . ? B12 B11 B5 108.1(7) . . ? B10 B11 H11 121.2 . . ? B6 B11 H11 121.5 . . ? B7 B11 H11 121.6 . . ? B12 B11 H11 122.1 . . ? B5 B11 H11 121.3 . . ? B9 B12 B8 59.7(5) . . ? B9 B12 B10 61.2(5) . . ? B8 B12 B10 108.1(7) . . ? B9 B12 B7 110.1(6) . . ? B8 B12 B7 61.5(5) . . ? B10 B12 B7 108.2(6) . . ? B9 B12 B11 109.2(6) . . ? B8 B12 B11 108.7(6) . . ? B10 B12 B11 59.3(5) . . ? B7 B12 B11 60.0(5) . . ? B9 B12 H12 120.5 . . ? B8 B12 H12 121.4 . . ? B10 B12 H12 121.9 . . ? B7 B12 H12 120.6 . . ? B11 B12 H12 121.7 . . ? B6 C1 B5 64.0(5) . . ? B6 C1 C2 62.2(4) . . ? B5 C1 C2 113.6(6) . . ? B6 C1 S2 132.4(5) . . ? B5 C1 S2 137.0(5) . . ? C2 C1 S2 108.0(4) . . ? B6 C1 B4 114.2(6) . . ? B5 C1 B4 61.7(5) . . ? C2 C1 B4 111.4(5) . . ? S2 C1 B4 112.5(5) . . ? B6 C1 Co3 125.3(5) . . ? B5 C1 Co3 125.5(5) . . ? C2 C1 Co3 66.8(3) . . ? S2 C1 Co3 80.8(3) . . ? B4 C1 Co3 68.0(4) . . ? B7 C2 B8 64.8(5) . . ? B7 C2 C1 108.1(5) . . ? B8 C2 C1 107.3(6) . . ? B7 C2 B6 62.5(4) . . ? B8 C2 B6 114.0(6) . . ? C1 C2 B6 58.4(4) . . ? B7 C2 S1 117.7(5) . . ? B8 C2 S1 126.8(5) . . ? C1 C2 S1 119.3(4) . . ? B6 C2 S1 111.5(5) . . ? B7 C2 Co3 124.6(5) . . ? B8 C2 Co3 67.7(4) . . ? C1 C2 Co3 61.8(3) . . ? B6 C2 Co3 117.1(5) . . ? S1 C2 Co3 112.9(4) . . ? C4 C3 C7 108.3(8) . . ? C4 C3 Co1 69.2(5) . . ? C7 C3 Co1 69.7(5) . . ? C4 C3 H3A 125.8 . . ? C7 C3 H3A 125.8 . . ? Co1 C3 H3A 125.8 . . ? C3 C4 C5 108.6(9) . . ? C3 C4 Co1 71.7(5) . . ? C5 C4 Co1 71.3(5) . . ? C3 C4 H4A 125.6 . . ? C5 C4 H4A 125.6 . . ? Co1 C4 H4A 125.6 . . ? C6 C5 C4 109.1(8) . . ? C6 C5 Co1 69.8(5) . . ? C4 C5 Co1 69.1(5) . . ? C6 C5 H5A 125.4 . . ? C4 C5 H5A 125.4 . . ? Co1 C5 H5A 125.4 . . ? C5 C6 C7 108.0(8) . . ? C5 C6 Co1 71.2(5) . . ? C7 C6 Co1 70.4(5) . . ? C5 C6 H6A 126.0 . . ? C7 C6 H6A 126.0 . . ? Co1 C6 H6A 126.0 . . ? C6 C7 C3 105.8(9) . . ? C6 C7 Co1 68.9(5) . . ? C3 C7 Co1 69.9(5) . . ? C6 C7 H7A 127.1 . . ? C3 C7 H7A 127.1 . . ? Co1 C7 H7A 127.1 . . ? N1 C8 N4 106.9(6) . . ? N1 C8 S3 130.1(6) . . ? N4 C8 S3 123.0(6) . . ? C14 C9 C10 122.2(9) . . ? C14 C9 N4 117.9(9) . . ? C10 C9 N4 119.9(8) . . ? C9 C10 C11 118.7(10) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? C12 C11 C10 120.1(11) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 121.1(11) . . ? C11 C12 H12A 119.4 . . ? C13 C12 H12A 119.4 . . ? C12 C13 C14 118.5(11) . . ? C12 C13 H13A 120.7 . . ? C14 C13 H13A 120.7 . . ? C9 C14 C13 119.4(11) . . ? C9 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? N8 C15 N5 108.6(7) . . ? N8 C15 S4 129.3(7) . . ? N5 C15 S4 122.1(6) . . ? C17 C16 C21 119.1(9) . . ? C17 C16 N8 120.5(9) . . ? C21 C16 N8 120.4(8) . . ? C18 C17 C16 121.9(11) . . ? C18 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? C17 C18 C19 119.7(11) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C20 C19 C18 119.5(11) . . ? C20 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? C19 C20 C21 121.7(11) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C20 C21 C16 118.2(9) . . ? C20 C21 H21A 120.9 . . ? C16 C21 H21A 120.9 . . ? C24 C23 C22 93(5) . . ? C23 C24 C25 106(7) . . ? C23 C22 C23 117(6) . 2_755 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.837 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.104