# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x81613o _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 B10 Co2' _chemical_formula_weight 392.26 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' Co Co 0.3494 0.9721 '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 14.9436(12) _cell_length_b 13.3925(10) _cell_length_c 16.7499(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3352.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9569 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.09 _exptl_crystal_description ? _exptl_crystal_colour purple _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3850 _exptl_absorpt_correction_T_max 0.7569 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_reflns_number 93508 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 28.26 _reflns_number_total 4134 _reflns_number_gt 3779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0000P)^2^+27.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4134 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 1.351 _refine_ls_restrained_S_all 1.351 _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 0.08059(4) 0.55595(5) 0.32028(4) 0.01221(15) Uani 1 1 d . . . C2 C 0.2125(3) 0.5486(3) 0.3697(3) 0.0140(8) Uani 1 1 d . . . H2C H 0.238(4) 0.480(4) 0.370(3) 0.017 Uiso 1 1 d . . . B3 B 0.2091(4) 0.5980(5) 0.2770(3) 0.0209(12) Uani 1 1 d . . . H3C H 0.236(4) 0.560(4) 0.228(3) 0.025 Uiso 1 1 d . . . B4 B 0.1241(4) 0.6816(5) 0.2502(4) 0.0309(15) Uani 1 1 d . . . H4C H 0.111(5) 0.696(5) 0.190(4) 0.037 Uiso 1 1 d . . . B5 B 0.0384(4) 0.7096(5) 0.3225(5) 0.0307(15) Uani 1 1 d . . . H5C H -0.026(4) 0.739(5) 0.304(4) 0.037 Uiso 1 1 d . . . B6 B 0.0451(4) 0.6531(4) 0.4172(4) 0.0238(12) Uani 1 1 d . . . H6C H -0.024(4) 0.637(5) 0.450(4) 0.029 Uiso 1 1 d . . . B7 B 0.1327(4) 0.5681(4) 0.4397(3) 0.0177(11) Uani 1 1 d . . . H7C H 0.108(4) 0.503(4) 0.477(3) 0.021 Uiso 1 1 d . . . B8 B 0.2798(4) 0.6502(4) 0.3531(3) 0.0163(10) Uani 1 1 d . . . H8C H 0.350(4) 0.646(4) 0.338(3) 0.020 Uiso 1 1 d . . . B9 B 0.2266(4) 0.7292(5) 0.2866(4) 0.0268(13) Uani 1 1 d . . . H9C H 0.265(4) 0.769(5) 0.246(4) 0.032 Uiso 1 1 d . . . C10 C 0.1307(4) 0.7809(4) 0.3097(5) 0.0366(16) Uani 1 1 d . . . H10C H 0.122(5) 0.836(6) 0.284(4) 0.044 Uiso 1 1 d . . . B11 B 0.0918(4) 0.7758(4) 0.4010(5) 0.0336(16) Uani 1 1 d . . . H11C H 0.067(5) 0.845(5) 0.421(4) 0.040 Uiso 1 1 d . . . B12 B 0.1396(4) 0.6955(5) 0.4722(4) 0.0231(12) Uani 1 1 d . . . H12C H 0.127(4) 0.716(5) 0.534(4) 0.028 Uiso 1 1 d . . . Co13 Co 0.25791(5) 0.62127(5) 0.46812(4) 0.01698(17) Uani 1 1 d . . . B14 B 0.2171(4) 0.7552(4) 0.3998(4) 0.0208(11) Uani 1 1 d . . . H14C H 0.254(4) 0.827(5) 0.414(3) 0.025 Uiso 1 1 d . . . C11 C 0.0596(3) 0.4015(4) 0.3221(4) 0.0246(11) Uani 1 1 d . . . H11 H 0.0963 0.3514 0.3519 0.029 Uiso 1 1 calc R . . C12 C -0.0166(4) 0.4531(4) 0.3521(3) 0.0245(11) Uani 1 1 d . . . H12 H -0.0439 0.4448 0.4062 0.029 Uiso 1 1 calc R . . C13 C -0.0476(3) 0.5168(4) 0.2905(4) 0.0276(12) Uani 1 1 d . . . H13 H -0.1013 0.5613 0.2933 0.033 Uiso 1 1 calc R . . C14 C 0.0090(4) 0.5050(5) 0.2240(3) 0.0304(13) Uani 1 1 d . . . H14 H 0.0026 0.5398 0.1715 0.036 Uiso 1 1 calc R . . C15 C 0.0743(4) 0.4337(4) 0.2432(4) 0.0302(12) Uani 1 1 d . . . H15 H 0.1234 0.4103 0.2073 0.036 Uiso 1 1 calc R . . C131 C 0.2668(6) 0.5966(6) 0.5895(4) 0.049(2) Uani 1 1 d . . . H131 H 0.2160 0.5940 0.6284 0.059 Uiso 1 1 calc R . . C132 C 0.3171(5) 0.6834(5) 0.5667(3) 0.0387(16) Uani 1 1 d . . . H132 H 0.3071 0.7528 0.5868 0.046 Uiso 1 1 calc R . . C133 C 0.3838(4) 0.6542(4) 0.5124(4) 0.0332(14) Uani 1 1 d . . . H133 H 0.4287 0.6994 0.4868 0.040 Uiso 1 1 calc R . . C134 C 0.3764(5) 0.5493(5) 0.4999(4) 0.0424(17) Uani 1 1 d . . . H134 H 0.4149 0.5078 0.4641 0.051 Uiso 1 1 calc R . . C135 C 0.3048(5) 0.5149(5) 0.5476(4) 0.046(2) Uani 1 1 d . . . H135 H 0.2836 0.4441 0.5507 0.055 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 0.0093(3) 0.0145(3) 0.0128(3) 0.0019(2) 0.0000(2) 0.0007(2) C2 0.016(2) 0.012(2) 0.014(2) -0.0035(16) -0.0050(17) 0.0035(17) B3 0.012(2) 0.041(3) 0.010(2) -0.003(2) 0.0007(19) -0.003(2) B4 0.020(3) 0.044(4) 0.029(3) 0.024(3) -0.010(2) -0.012(3) B5 0.010(2) 0.017(3) 0.065(5) 0.004(3) 0.000(3) 0.005(2) B6 0.018(3) 0.016(3) 0.037(3) -0.010(2) 0.011(2) -0.002(2) B7 0.030(3) 0.015(2) 0.008(2) -0.0027(19) 0.000(2) -0.005(2) B8 0.013(2) 0.022(3) 0.014(2) -0.002(2) 0.0018(19) 0.000(2) B9 0.021(3) 0.036(4) 0.023(3) 0.017(3) -0.002(2) -0.009(2) C10 0.020(3) 0.021(3) 0.069(5) 0.024(3) -0.010(3) -0.003(2) B11 0.017(3) 0.011(3) 0.072(5) -0.009(3) 0.008(3) -0.001(2) B12 0.021(3) 0.021(3) 0.027(3) -0.011(2) 0.010(2) -0.007(2) Co13 0.0257(4) 0.0133(3) 0.0119(3) 0.0003(2) -0.0061(3) -0.0061(3) B14 0.021(3) 0.010(2) 0.032(3) 0.003(2) 0.006(2) 0.000(2) C11 0.021(2) 0.012(2) 0.041(3) 0.002(2) -0.016(2) -0.0026(18) C12 0.022(2) 0.029(3) 0.022(2) -0.006(2) 0.005(2) -0.020(2) C13 0.012(2) 0.026(3) 0.045(3) -0.012(2) -0.009(2) 0.002(2) C14 0.043(3) 0.032(3) 0.017(2) -0.001(2) -0.012(2) -0.011(3) C15 0.027(3) 0.031(3) 0.032(3) -0.016(2) 0.010(2) -0.007(2) C131 0.075(5) 0.055(4) 0.018(3) 0.010(3) -0.020(3) -0.032(4) C132 0.066(5) 0.033(3) 0.017(3) 0.001(2) -0.016(3) -0.022(3) C133 0.037(3) 0.028(3) 0.034(3) 0.006(2) -0.025(3) -0.011(3) C134 0.048(4) 0.029(3) 0.050(4) 0.003(3) -0.037(3) 0.005(3) C135 0.068(5) 0.031(3) 0.038(3) 0.018(3) -0.044(4) -0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C13 2.047(5) . ? Co1 C14 2.052(5) . ? Co1 C12 2.071(5) . ? Co1 C15 2.087(5) . ? Co1 C11 2.092(5) . ? Co1 B3 2.128(5) . ? Co1 C2 2.140(5) . ? Co1 B6 2.148(6) . ? Co1 B5 2.153(6) . ? Co1 B4 2.153(6) . ? Co1 B7 2.153(5) . ? C2 B3 1.689(7) . ? C2 B7 1.693(7) . ? C2 B8 1.715(7) . ? C2 Co13 2.031(4) . ? C2 H2C 0.99(6) . ? B3 B4 1.752(9) . ? B3 B9 1.784(9) . ? B3 B8 1.798(8) . ? B3 H3C 1.04(6) . ? B4 C10 1.665(11) . ? B4 B9 1.768(9) . ? B4 B5 1.803(10) . ? B4 H4C 1.05(7) . ? B5 C10 1.692(8) . ? B5 B6 1.760(10) . ? B5 B11 1.775(11) . ? B5 H5C 1.08(7) . ? B6 B7 1.776(9) . ? B6 B12 1.778(9) . ? B6 B11 1.805(9) . ? B6 H6C 1.18(6) . ? B7 B12 1.793(8) . ? B7 Co13 2.058(6) . ? B7 H7C 1.14(6) . ? B8 B9 1.730(8) . ? B8 B14 1.862(8) . ? B8 Co13 1.992(5) . ? B8 H8C 1.08(6) . ? B9 C10 1.638(9) . ? B9 B14 1.932(9) . ? B9 H9C 1.04(7) . ? C10 B11 1.637(11) . ? C10 B14 2.015(9) . ? C10 H10C 0.86(7) . ? B11 B12 1.758(10) . ? B11 B14 1.893(9) . ? B11 H11C 1.06(7) . ? B12 B14 1.858(8) . ? B12 Co13 2.029(6) . ? B12 H12C 1.09(6) . ? Co13 C132 2.050(5) . ? Co13 C131 2.065(6) . ? Co13 C133 2.069(6) . ? Co13 C135 2.072(6) . ? Co13 C134 2.085(6) . ? Co13 B14 2.213(6) . ? B14 H14C 1.14(6) . ? C11 C15 1.407(8) . ? C11 C12 1.423(8) . ? C11 H11 1.0000 . ? C12 C13 1.417(8) . ? C12 H12 1.0000 . ? C13 C14 1.407(8) . ? C13 H13 1.0000 . ? C14 C15 1.403(9) . ? C14 H14 1.0000 . ? C15 H15 1.0000 . ? C131 C135 1.419(11) . ? C131 C132 1.437(9) . ? C131 H131 1.0000 . ? C132 C133 1.404(10) . ? C132 H132 1.0000 . ? C133 C134 1.424(9) . ? C133 H133 1.0000 . ? C134 C135 1.414(11) . ? C134 H134 1.0000 . ? C135 H135 1.0000 . ? 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 C13 Co1 C14 40.2(2) . . ? C13 Co1 C12 40.2(2) . . ? C14 Co1 C12 67.4(2) . . ? C13 Co1 C15 66.8(2) . . ? C14 Co1 C15 39.6(2) . . ? C12 Co1 C15 66.8(2) . . ? C13 Co1 C11 67.1(2) . . ? C14 Co1 C11 66.7(2) . . ? C12 Co1 C11 40.0(2) . . ? C15 Co1 C11 39.3(2) . . ? C13 Co1 B3 146.0(2) . . ? C14 Co1 B3 106.9(2) . . ? C12 Co1 B3 153.6(2) . . ? C15 Co1 B3 92.2(2) . . ? C11 Co1 B3 113.7(2) . . ? C13 Co1 C2 160.7(2) . . ? C14 Co1 C2 140.2(2) . . ? C12 Co1 C2 121.0(2) . . ? C15 Co1 C2 104.1(2) . . ? C11 Co1 C2 94.98(18) . . ? B3 Co1 C2 46.6(2) . . ? C13 Co1 B6 96.2(2) . . ? C14 Co1 B6 131.8(3) . . ? C12 Co1 B6 92.0(2) . . ? C15 Co1 B6 158.8(2) . . ? C11 Co1 B6 123.4(2) . . ? B3 Co1 B6 108.7(2) . . ? C2 Co1 B6 87.9(2) . . ? C13 Co1 B5 88.5(2) . . ? C14 Co1 B5 100.3(3) . . ? C12 Co1 B5 115.2(2) . . ? C15 Co1 B5 138.4(3) . . ? C11 Co1 B5 154.3(2) . . ? B3 Co1 B5 91.0(2) . . ? C2 Co1 B5 107.9(2) . . ? B6 Co1 B5 48.3(3) . . ? C13 Co1 B4 110.5(2) . . ? C14 Co1 B4 89.4(2) . . ? C12 Co1 B4 150.7(2) . . ? C15 Co1 B4 106.9(3) . . ? C11 Co1 B4 145.7(3) . . ? B3 Co1 B4 48.3(2) . . ? C2 Co1 B4 88.2(2) . . ? B6 Co1 B4 90.8(3) . . ? B5 Co1 B4 49.5(3) . . ? C13 Co1 B7 125.7(2) . . ? C14 Co1 B7 160.7(2) . . ? C12 Co1 B7 93.7(2) . . ? C15 Co1 B7 130.5(2) . . ? C11 Co1 B7 96.6(2) . . ? B3 Co1 B7 88.3(2) . . ? C2 Co1 B7 46.4(2) . . ? B6 Co1 B7 48.8(2) . . ? B5 Co1 B7 91.0(3) . . ? B4 Co1 B7 109.8(2) . . ? B3 C2 B7 123.7(4) . . ? B3 C2 B8 63.8(3) . . ? B7 C2 B8 113.7(4) . . ? B3 C2 Co13 124.6(3) . . ? B7 C2 Co13 66.4(2) . . ? B8 C2 Co13 63.6(2) . . ? B3 C2 Co1 66.3(2) . . ? B7 C2 Co1 67.2(2) . . ? B8 C2 Co1 116.2(3) . . ? Co13 C2 Co1 126.8(2) . . ? B3 C2 H2C 112(3) . . ? B7 C2 H2C 114(3) . . ? B8 C2 H2C 121(3) . . ? Co13 C2 H2C 108(3) . . ? Co1 C2 H2C 113(3) . . ? C2 B3 B4 120.6(4) . . ? C2 B3 B9 107.4(4) . . ? B4 B3 B9 60.0(4) . . ? C2 B3 B8 58.8(3) . . ? B4 B3 B8 111.1(5) . . ? B9 B3 B8 57.8(3) . . ? C2 B3 Co1 67.1(2) . . ? B4 B3 Co1 66.6(3) . . ? B9 B3 Co1 111.3(4) . . ? B8 B3 Co1 113.1(3) . . ? C2 B3 H3C 121(3) . . ? B4 B3 H3C 113(3) . . ? B9 B3 H3C 119(3) . . ? B8 B3 H3C 121(3) . . ? Co1 B3 H3C 119(3) . . ? C10 B4 B3 108.3(4) . . ? C10 B4 B9 56.9(4) . . ? B3 B4 B9 60.9(4) . . ? C10 B4 B5 58.2(4) . . ? B3 B4 B5 118.4(4) . . ? B9 B4 B5 108.0(5) . . ? C10 B4 Co1 108.4(4) . . ? B3 B4 Co1 65.1(3) . . ? B9 B4 Co1 110.8(3) . . ? B5 B4 Co1 65.2(3) . . ? C10 B4 H4C 116(4) . . ? B3 B4 H4C 120(4) . . ? B9 B4 H4C 115(4) . . ? B5 B4 H4C 119(4) . . ? Co1 B4 H4C 128(4) . . ? C10 B5 B6 108.0(5) . . ? C10 B5 B11 56.3(4) . . ? B6 B5 B11 61.4(4) . . ? C10 B5 B4 56.8(4) . . ? B6 B5 B4 118.4(4) . . ? B11 B5 B4 106.4(4) . . ? C10 B5 Co1 107.3(3) . . ? B6 B5 Co1 65.7(3) . . ? B11 B5 Co1 111.0(4) . . ? B4 B5 Co1 65.2(3) . . ? C10 B5 H5C 119(4) . . ? B6 B5 H5C 118(4) . . ? B11 B5 H5C 116(4) . . ? B4 B5 H5C 120(4) . . ? Co1 B5 H5C 127(4) . . ? B5 B6 B7 120.6(4) . . ? B5 B6 B12 112.0(4) . . ? B7 B6 B12 60.6(3) . . ? B5 B6 B11 59.7(4) . . ? B7 B6 B11 109.3(4) . . ? B12 B6 B11 58.8(4) . . ? B5 B6 Co1 66.0(3) . . ? B7 B6 Co1 65.8(2) . . ? B12 B6 Co1 112.9(3) . . ? B11 B6 Co1 110.0(4) . . ? B5 B6 H6C 117(3) . . ? B7 B6 H6C 115(3) . . ? B12 B6 H6C 120(3) . . ? B11 B6 H6C 125(3) . . ? Co1 B6 H6C 117(3) . . ? C2 B7 B6 118.1(4) . . ? C2 B7 B12 108.5(4) . . ? B6 B7 B12 59.8(3) . . ? C2 B7 Co13 64.7(3) . . ? B6 B7 Co13 119.8(3) . . ? B12 B7 Co13 63.2(3) . . ? C2 B7 Co1 66.4(2) . . ? B6 B7 Co1 65.5(3) . . ? B12 B7 Co1 112.0(3) . . ? Co13 B7 Co1 124.7(3) . . ? C2 B7 H7C 119(3) . . ? B6 B7 H7C 112(3) . . ? B12 B7 H7C 126(3) . . ? Co13 B7 H7C 116(3) . . ? Co1 B7 H7C 110(3) . . ? C2 B8 B9 108.7(4) . . ? C2 B8 B3 57.4(3) . . ? B9 B8 B3 60.7(4) . . ? C2 B8 B14 103.6(3) . . ? B9 B8 B14 65.0(4) . . ? B3 B8 B14 107.2(4) . . ? C2 B8 Co13 66.0(2) . . ? B9 B8 Co13 131.8(4) . . ? B3 B8 Co13 120.9(3) . . ? B14 B8 Co13 70.0(3) . . ? C2 B8 H8C 124(3) . . ? B9 B8 H8C 109(3) . . ? B3 B8 H8C 112(3) . . ? B14 B8 H8C 129(3) . . ? Co13 B8 H8C 112(3) . . ? C10 B9 B8 120.6(5) . . ? C10 B9 B4 58.4(4) . . ? B8 B9 B4 113.6(4) . . ? C10 B9 B3 108.0(4) . . ? B8 B9 B3 61.5(3) . . ? B4 B9 B3 59.1(4) . . ? C10 B9 B14 68.1(4) . . ? B8 B9 B14 60.8(3) . . ? B4 B9 B14 109.9(4) . . ? B3 B9 B14 104.8(4) . . ? C10 B9 H9C 115(4) . . ? B8 B9 H9C 119(4) . . ? B4 B9 H9C 116(4) . . ? B3 B9 H9C 122(4) . . ? B14 B9 H9C 126(4) . . ? B11 C10 B9 120.9(5) . . ? B11 C10 B4 120.3(5) . . ? B9 C10 B4 64.7(4) . . ? B11 C10 B5 64.4(4) . . ? B9 C10 B5 120.3(5) . . ? B4 C10 B5 64.9(4) . . ? B11 C10 B14 61.4(4) . . ? B9 C10 B14 62.9(3) . . ? B4 C10 B14 110.5(4) . . ? B5 C10 B14 109.3(4) . . ? B11 C10 H10C 117(5) . . ? B9 C10 H10C 112(5) . . ? B4 C10 H10C 112(5) . . ? B5 C10 H10C 115(5) . . ? B14 C10 H10C 128(5) . . ? C10 B11 B12 121.0(4) . . ? C10 B11 B5 59.3(4) . . ? B12 B11 B5 112.3(4) . . ? C10 B11 B6 108.4(5) . . ? B12 B11 B6 59.9(4) . . ? B5 B11 B6 58.9(4) . . ? C10 B11 B14 69.2(4) . . ? B12 B11 B14 61.1(3) . . ? B5 B11 B14 111.3(4) . . ? B6 B11 B14 104.6(4) . . ? C10 B11 H11C 112(4) . . ? B12 B11 H11C 118(4) . . ? B5 B11 H11C 121(4) . . ? B6 B11 H11C 129(4) . . ? B14 B11 H11C 119(4) . . ? B11 B12 B6 61.4(4) . . ? B11 B12 B7 110.7(4) . . ? B6 B12 B7 59.6(3) . . ? B11 B12 B14 63.1(4) . . ? B6 B12 B14 107.1(4) . . ? B7 B12 B14 104.3(4) . . ? B11 B12 Co13 129.1(4) . . ? B6 B12 Co13 121.2(4) . . ? B7 B12 Co13 64.8(3) . . ? B14 B12 Co13 69.2(3) . . ? B11 B12 H12C 115(3) . . ? B6 B12 H12C 116(3) . . ? B7 B12 H12C 121(3) . . ? B14 B12 H12C 128(3) . . ? Co13 B12 H12C 108(3) . . ? B8 Co13 B12 94.6(2) . . ? B8 Co13 C2 50.5(2) . . ? B12 Co13 C2 88.3(2) . . ? B8 Co13 C132 129.0(2) . . ? B12 Co13 C132 98.6(3) . . ? C2 Co13 C132 173.0(3) . . ? B8 Co13 B7 89.6(2) . . ? B12 Co13 B7 52.1(2) . . ? C2 Co13 B7 48.9(2) . . ? C132 Co13 B7 136.0(3) . . ? B8 Co13 C131 166.7(3) . . ? B12 Co13 C131 95.8(3) . . ? C2 Co13 C131 138.1(2) . . ? C132 Co13 C131 40.9(2) . . ? B7 Co13 C131 103.3(3) . . ? B8 Co13 C133 98.9(2) . . ? B12 Co13 C133 132.5(2) . . ? C2 Co13 C133 134.2(2) . . ? C132 Co13 C133 39.9(3) . . ? B7 Co13 C133 169.4(2) . . ? C131 Co13 C133 67.9(3) . . ? B8 Co13 C135 134.4(3) . . ? B12 Co13 C135 127.5(3) . . ? C2 Co13 C135 107.7(2) . . ? C132 Co13 C135 67.4(3) . . ? B7 Co13 C135 102.6(2) . . ? C131 Co13 C135 40.1(3) . . ? C133 Co13 C135 67.0(2) . . ? B8 Co13 C134 101.3(3) . . ? B12 Co13 C134 163.3(3) . . ? C2 Co13 C134 105.6(2) . . ? C132 Co13 C134 67.4(3) . . ? B7 Co13 C134 132.2(2) . . ? C131 Co13 C134 67.7(3) . . ? C133 Co13 C134 40.1(2) . . ? C135 Co13 C134 39.8(3) . . ? B8 Co13 B14 52.2(2) . . ? B12 Co13 B14 51.7(2) . . ? C2 Co13 B14 82.9(2) . . ? C132 Co13 B14 101.9(2) . . ? B7 Co13 B14 84.9(2) . . ? C131 Co13 B14 131.1(3) . . ? C133 Co13 B14 105.3(2) . . ? C135 Co13 B14 169.3(2) . . ? C134 Co13 B14 137.8(3) . . ? B12 B14 B8 105.2(4) . . ? B12 B14 B11 55.9(4) . . ? B8 B14 B11 127.8(4) . . ? B12 B14 B9 127.5(4) . . ? B8 B14 B9 54.2(3) . . ? B11 B14 B9 96.3(4) . . ? B12 B14 C10 99.4(4) . . ? B8 B14 C10 97.9(4) . . ? B11 B14 C10 49.4(4) . . ? B9 B14 C10 49.0(3) . . ? B12 B14 Co13 59.0(3) . . ? B8 B14 Co13 57.7(2) . . ? B11 B14 Co13 112.7(3) . . ? B9 B14 Co13 109.9(3) . . ? C10 B14 Co13 134.6(3) . . ? B12 B14 H14C 122(3) . . ? B8 B14 H14C 119(3) . . ? B11 B14 H14C 111(3) . . ? B9 B14 H14C 109(3) . . ? C10 B14 H14C 109(3) . . ? Co13 B14 H14C 116(3) . . ? C15 C11 C12 107.9(5) . . ? C15 C11 Co1 70.1(3) . . ? C12 C11 Co1 69.2(3) . . ? C15 C11 H11 126.0 . . ? C12 C11 H11 126.0 . . ? Co1 C11 H11 126.0 . . ? C13 C12 C11 107.3(5) . . ? C13 C12 Co1 69.0(3) . . ? C11 C12 Co1 70.8(3) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? Co1 C12 H12 126.4 . . ? C14 C13 C12 108.2(5) . . ? C14 C13 Co1 70.1(3) . . ? C12 C13 Co1 70.8(3) . . ? C14 C13 H13 125.9 . . ? C12 C13 H13 125.9 . . ? Co1 C13 H13 125.9 . . ? C15 C14 C13 108.2(5) . . ? C15 C14 Co1 71.5(3) . . ? C13 C14 Co1 69.8(3) . . ? C15 C14 H14 125.9 . . ? C13 C14 H14 125.9 . . ? Co1 C14 H14 125.9 . . ? C14 C15 C11 108.4(5) . . ? C14 C15 Co1 68.8(3) . . ? C11 C15 Co1 70.5(3) . . ? C14 C15 H15 125.8 . . ? C11 C15 H15 125.8 . . ? Co1 C15 H15 125.8 . . ? C135 C131 C132 106.4(7) . . ? C135 C131 Co13 70.2(3) . . ? C132 C131 Co13 69.0(3) . . ? C135 C131 H131 126.8 . . ? C132 C131 H131 126.8 . . ? Co13 C131 H131 126.8 . . ? C133 C132 C131 108.6(6) . . ? C133 C132 Co13 70.8(3) . . ? C131 C132 Co13 70.1(3) . . ? C133 C132 H132 125.7 . . ? C131 C132 H132 125.7 . . ? Co13 C132 H132 125.7 . . ? C132 C133 C134 108.4(6) . . ? C132 C133 Co13 69.3(3) . . ? C134 C133 Co13 70.6(3) . . ? C132 C133 H133 125.8 . . ? C134 C133 H133 125.8 . . ? Co13 C133 H133 125.8 . . ? C135 C134 C133 107.3(7) . . ? C135 C134 Co13 69.6(4) . . ? C133 C134 Co13 69.3(4) . . ? C135 C134 H134 126.4 . . ? C133 C134 H134 126.4 . . ? Co13 C134 H134 126.4 . . ? C134 C135 C131 109.3(6) . . ? C134 C135 Co13 70.6(3) . . ? C131 C135 Co13 69.7(4) . . ? C134 C135 H135 125.3 . . ? C131 C135 H135 125.3 . . ? Co13 C135 H135 125.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.637 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.128 _database_code_depnum_ccdc_archive 'CCDC 939752' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x82075 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H26 B10 Co2 O' _chemical_formula_weight 436.31 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.813(4) _cell_length_b 13.146(6) _cell_length_c 13.159(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.620(16) _cell_angle_gamma 90.00 _cell_volume 1858.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1911 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 18.58 _exptl_crystal_description NEEDLE _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 1.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5209 _exptl_absorpt_correction_T_max 0.9320 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_reflns_number 20203 _diffrn_reflns_av_R_equivalents 0.1138 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2651 _reflns_number_gt 1663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0418P)^2^+6.1556P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2651 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1153 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 0.94330(8) 0.61001(6) 0.21161(7) 0.0235(3) Uani 1 1 d . . . C2 C 0.7556(6) 0.5578(5) 0.1790(5) 0.0243(17) Uani 1 1 d . . . H2 H 0.750(6) 0.494(5) 0.191(5) 0.029 Uiso 1 1 d . . . B3 B 0.7695(7) 0.6352(5) 0.2797(6) 0.0211(18) Uani 1 1 d . . . B4 B 0.8658(7) 0.7442(6) 0.2688(7) 0.029(2) Uani 1 1 d . . . H4 H 0.906(5) 0.779(4) 0.345(5) 0.034 Uiso 1 1 d . . . B5 B 0.9432(8) 0.7643(6) 0.1582(7) 0.036(2) Uani 1 1 d . . . H5 H 1.027(6) 0.810(5) 0.180(5) 0.043 Uiso 1 1 d . . . B6 B 0.9249(8) 0.6780(6) 0.0591(6) 0.035(2) Uani 1 1 d . . . H6 H 1.011(6) 0.666(4) 0.013(5) 0.042 Uiso 1 1 d . . . B7 B 0.8338(7) 0.5676(6) 0.0752(6) 0.0247(19) Uani 1 1 d . . . H7 H 0.857(5) 0.500(4) 0.041(4) 0.030 Uiso 1 1 d . . . Co8 Co 0.59511(8) 0.63875(7) 0.19326(7) 0.0264(3) Uani 1 1 d . . . B9 B 0.7044(7) 0.7567(6) 0.2406(6) 0.029(2) Uani 1 1 d . . . H9 H 0.664(5) 0.810(5) 0.291(4) 0.035 Uiso 1 1 d . . . C10 C 0.8005(6) 0.8136(5) 0.1675(6) 0.0329(19) Uani 1 1 d . . . H10 H 0.794(6) 0.881(5) 0.173(5) 0.039 Uiso 1 1 d . . . B11 B 0.8301(9) 0.7846(7) 0.0511(7) 0.041(2) Uani 1 1 d . . . H11 H 0.839(6) 0.846(5) 0.005(5) 0.049 Uiso 1 1 d . . . B12 B 0.7698(8) 0.6721(6) 0.0016(7) 0.030(2) Uani 1 1 d . . . H12 H 0.742(5) 0.673(4) -0.079(5) 0.036 Uiso 1 1 d . . . B13 B 0.6710(7) 0.5984(6) 0.0678(6) 0.027(2) Uani 1 1 d . . . H13 H 0.620(6) 0.552(5) 0.031(5) 0.033 Uiso 1 1 d . . . B14 B 0.6741(8) 0.7452(6) 0.0898(6) 0.033(2) Uani 1 1 d . . . H14 H 0.600(6) 0.798(5) 0.060(5) 0.039 Uiso 1 1 d . . . C11 C 1.0030(6) 0.4889(5) 0.3052(6) 0.0337(18) Uani 1 1 d . . . H11A H 0.9486 0.4392 0.3366 0.040 Uiso 1 1 calc R . . C12 C 1.0486(6) 0.5795(6) 0.3483(5) 0.0369(19) Uani 1 1 d . . . H12A H 1.0329 0.6065 0.4166 0.044 Uiso 1 1 calc R . . C13 C 1.1223(6) 0.6275(6) 0.2791(6) 0.046(2) Uani 1 1 d . . . H13A H 1.1693 0.6928 0.2902 0.055 Uiso 1 1 calc R . . C14 C 1.1215(6) 0.5617(6) 0.1940(5) 0.0359(19) Uani 1 1 d . . . H14A H 1.1663 0.5730 0.1326 0.043 Uiso 1 1 calc R . . C15 C 1.0493(6) 0.4783(5) 0.2116(6) 0.0360(18) Uani 1 1 d . . . H15 H 1.0316 0.4198 0.1636 0.043 Uiso 1 1 calc R . . C31 C 0.7680(6) 0.6485(5) 0.4680(5) 0.0355(18) Uani 1 1 d . . . H31A H 0.7248 0.7141 0.4527 0.043 Uiso 1 1 calc R . . H31B H 0.8553 0.6630 0.4956 0.043 Uiso 1 1 calc R . . O31 O 0.7650(4) 0.5884(3) 0.3762(3) 0.0281(11) Uani 1 1 d . . . C32 C 0.7046(6) 0.5901(5) 0.5451(5) 0.0363(19) Uani 1 1 d . . . H32A H 0.7465 0.5246 0.5584 0.055 Uiso 1 1 calc R . . H32B H 0.6174 0.5785 0.5183 0.055 Uiso 1 1 calc R . . H32C H 0.7085 0.6291 0.6088 0.055 Uiso 1 1 calc R . . C81 C 0.4678(6) 0.6632(5) 0.2987(6) 0.0313(18) Uani 1 1 d . . . H81 H 0.4837 0.7029 0.3637 0.038 Uiso 1 1 calc R . . C82 C 0.4221(6) 0.7030(5) 0.2012(5) 0.0311(18) Uani 1 1 d . . . H82 H 0.3984 0.7753 0.1856 0.037 Uiso 1 1 calc R . . C83 C 0.4114(6) 0.6206(5) 0.1306(5) 0.0315(17) Uani 1 1 d . . . H83 H 0.3799 0.6254 0.0563 0.038 Uiso 1 1 calc R . . C84 C 0.4501(6) 0.5307(5) 0.1835(5) 0.0315(18) Uani 1 1 d . . . H84 H 0.4520 0.4609 0.1535 0.038 Uiso 1 1 calc R . . C85 C 0.4860(6) 0.5580(5) 0.2881(5) 0.0292(17) Uani 1 1 d . . . H85 H 0.5181 0.5102 0.3442 0.035 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 0.0241(5) 0.0211(5) 0.0268(5) -0.0038(4) 0.0092(4) -0.0015(4) C2 0.031(4) 0.014(4) 0.028(4) 0.003(3) 0.005(3) -0.006(3) B3 0.023(4) 0.015(4) 0.025(5) 0.003(4) 0.003(3) 0.004(3) B4 0.033(5) 0.020(5) 0.036(5) -0.001(4) 0.012(4) -0.002(4) B5 0.033(5) 0.030(5) 0.049(6) 0.003(4) 0.023(5) -0.004(4) B6 0.030(5) 0.036(5) 0.039(5) 0.002(4) 0.012(4) 0.002(4) B7 0.034(5) 0.014(4) 0.027(5) 0.004(4) 0.007(4) 0.010(4) Co8 0.0270(5) 0.0214(5) 0.0318(6) -0.0013(4) 0.0080(4) 0.0009(4) B9 0.028(5) 0.022(5) 0.039(5) -0.005(4) 0.013(4) 0.000(4) C10 0.041(5) 0.011(4) 0.051(5) -0.005(4) 0.022(4) 0.005(3) B11 0.058(6) 0.027(5) 0.042(6) 0.006(4) 0.026(5) 0.001(4) B12 0.037(5) 0.029(5) 0.028(5) 0.008(4) 0.015(4) 0.006(4) B13 0.026(5) 0.026(5) 0.031(5) 0.006(4) 0.008(4) 0.008(4) B14 0.039(5) 0.031(5) 0.030(5) 0.004(4) 0.015(4) 0.007(4) C11 0.028(4) 0.026(4) 0.048(5) 0.007(4) 0.006(4) 0.002(3) C12 0.039(5) 0.045(5) 0.027(4) -0.009(4) 0.009(4) 0.013(4) C13 0.029(4) 0.028(5) 0.078(6) -0.003(4) -0.010(4) -0.006(4) C14 0.026(4) 0.052(5) 0.031(5) 0.003(4) 0.008(4) 0.010(4) C15 0.033(4) 0.030(4) 0.043(5) -0.004(4) -0.003(4) 0.005(4) C31 0.039(4) 0.042(5) 0.026(4) -0.008(4) 0.007(3) -0.003(4) O31 0.036(3) 0.024(3) 0.026(3) -0.003(2) 0.009(2) -0.002(2) C32 0.039(4) 0.044(5) 0.025(4) -0.003(4) -0.001(3) -0.003(4) C81 0.031(4) 0.026(4) 0.039(5) -0.007(4) 0.017(4) -0.001(3) C82 0.025(4) 0.030(4) 0.040(5) 0.004(4) 0.012(4) -0.004(3) C83 0.022(4) 0.037(5) 0.036(4) -0.003(4) 0.004(3) -0.003(3) C84 0.036(4) 0.020(4) 0.040(5) -0.003(3) 0.009(4) -0.002(3) C85 0.031(4) 0.026(4) 0.032(5) 0.009(3) 0.011(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C13 2.048(7) . ? Co1 C12 2.054(7) . ? Co1 C14 2.067(7) . ? Co1 C11 2.070(7) . ? Co1 C15 2.077(7) . ? Co1 B7 2.108(8) . ? Co1 B4 2.127(8) . ? Co1 C2 2.138(7) . ? Co1 B5 2.146(8) . ? Co1 B6 2.185(8) . ? Co1 B3 2.199(7) . ? C2 B3 1.663(10) . ? C2 B7 1.693(9) . ? C2 B13 1.719(10) . ? C2 Co8 2.063(7) . ? C2 H2 0.85(6) . ? B3 O31 1.416(8) . ? B3 B4 1.787(10) . ? B3 B9 1.797(10) . ? B3 Co8 2.087(7) . ? B4 C10 1.700(11) . ? B4 B9 1.750(11) . ? B4 B5 1.780(11) . ? B4 H4 1.14(6) . ? B5 C10 1.691(10) . ? B5 B6 1.722(12) . ? B5 B11 1.777(13) . ? B5 H5 1.09(6) . ? B6 B11 1.733(12) . ? B6 B12 1.760(12) . ? B6 B7 1.780(11) . ? B6 H6 1.18(6) . ? B7 B12 1.775(11) . ? B7 B13 1.799(10) . ? B7 H7 1.04(6) . ? Co8 B13 1.998(8) . ? Co8 B9 2.005(8) . ? Co8 C82 2.067(7) . ? Co8 C83 2.075(7) . ? Co8 C81 2.089(6) . ? Co8 C85 2.102(6) . ? Co8 C84 2.109(7) . ? Co8 B14 2.192(8) . ? B9 C10 1.671(10) . ? B9 B14 1.979(12) . ? B9 H9 1.09(6) . ? C10 B11 1.646(11) . ? C10 B14 1.844(11) . ? C10 H10 0.89(6) . ? B11 B12 1.714(12) . ? B11 B14 1.890(12) . ? B11 H11 1.03(6) . ? B12 B13 1.747(11) . ? B12 B14 1.903(11) . ? B12 H12 1.07(6) . ? B13 B14 1.950(12) . ? B13 H13 0.92(6) . ? B14 H14 1.09(6) . ? C11 C12 1.385(9) . ? C11 C15 1.388(9) . ? C11 H11A 1.0000 . ? C12 C13 1.425(10) . ? C12 H12A 1.0000 . ? C13 C14 1.414(10) . ? C13 H13A 1.0000 . ? C14 C15 1.381(9) . ? C14 H14A 1.0000 . ? C15 H15 1.0000 . ? C31 O31 1.441(7) . ? C31 C32 1.499(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C81 C85 1.406(9) . ? C81 C82 1.421(9) . ? C81 H81 1.0000 . ? C82 C83 1.424(9) . ? C82 H82 1.0000 . ? C83 C84 1.410(9) . ? C83 H83 1.0000 . ? C84 C85 1.432(9) . ? C84 H84 1.0000 . ? C85 H85 1.0000 . ? 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 C13 Co1 C12 40.6(3) . . ? C13 Co1 C14 40.2(3) . . ? C12 Co1 C14 66.9(3) . . ? C13 Co1 C11 67.3(3) . . ? C12 Co1 C11 39.2(3) . . ? C14 Co1 C11 66.4(3) . . ? C13 Co1 C15 66.4(3) . . ? C12 Co1 C15 65.6(3) . . ? C14 Co1 C15 38.9(3) . . ? C11 Co1 C15 39.1(3) . . ? C13 Co1 B7 144.0(3) . . ? C12 Co1 B7 153.4(3) . . ? C14 Co1 B7 105.2(3) . . ? C11 Co1 B7 114.1(3) . . ? C15 Co1 B7 92.0(3) . . ? C13 Co1 B4 98.3(3) . . ? C12 Co1 B4 93.1(3) . . ? C14 Co1 B4 134.8(3) . . ? C11 Co1 B4 122.4(3) . . ? C15 Co1 B4 158.6(3) . . ? B7 Co1 B4 108.4(3) . . ? C13 Co1 C2 162.0(3) . . ? C12 Co1 C2 122.0(3) . . ? C14 Co1 C2 139.0(3) . . ? C11 Co1 C2 95.5(3) . . ? C15 Co1 C2 104.1(3) . . ? B7 Co1 C2 47.0(3) . . ? B4 Co1 C2 86.2(3) . . ? C13 Co1 B5 90.0(3) . . ? C12 Co1 B5 116.8(3) . . ? C14 Co1 B5 102.6(3) . . ? C11 Co1 B5 155.5(3) . . ? C15 Co1 B5 140.1(3) . . ? B7 Co1 B5 89.5(3) . . ? B4 Co1 B5 49.2(3) . . ? C2 Co1 B5 105.8(3) . . ? C13 Co1 B6 109.5(3) . . ? C12 Co1 B6 150.0(3) . . ? C14 Co1 B6 90.6(3) . . ? C11 Co1 B6 148.2(3) . . ? C15 Co1 B6 109.4(3) . . ? B7 Co1 B6 49.0(3) . . ? B4 Co1 B6 89.3(3) . . ? C2 Co1 B6 87.9(3) . . ? B5 Co1 B6 46.9(3) . . ? C13 Co1 B3 128.1(3) . . ? C12 Co1 B3 95.0(3) . . ? C14 Co1 B3 160.7(3) . . ? C11 Co1 B3 95.5(3) . . ? C15 Co1 B3 128.6(3) . . ? B7 Co1 B3 88.0(3) . . ? B4 Co1 B3 48.7(3) . . ? C2 Co1 B3 45.1(3) . . ? B5 Co1 B3 91.3(3) . . ? B6 Co1 B3 108.7(3) . . ? B3 C2 B7 126.1(5) . . ? B3 C2 B13 118.6(5) . . ? B7 C2 B13 63.6(4) . . ? B3 C2 Co8 67.1(3) . . ? B7 C2 Co8 122.6(4) . . ? B13 C2 Co8 63.0(3) . . ? B3 C2 Co1 69.4(3) . . ? B7 C2 Co1 65.6(3) . . ? B13 C2 Co1 118.1(4) . . ? Co8 C2 Co1 127.3(3) . . ? B3 C2 H2 117(4) . . ? B7 C2 H2 106(4) . . ? B13 C2 H2 115(4) . . ? Co8 C2 H2 115(4) . . ? Co1 C2 H2 111(4) . . ? O31 B3 C2 116.0(5) . . ? O31 B3 B4 120.0(6) . . ? C2 B3 B4 115.2(5) . . ? O31 B3 B9 126.2(5) . . ? C2 B3 B9 108.6(5) . . ? B4 B3 B9 58.5(4) . . ? O31 B3 Co8 112.1(4) . . ? C2 B3 Co8 65.6(3) . . ? B4 B3 Co8 115.9(5) . . ? B9 B3 Co8 61.6(3) . . ? O31 B3 Co1 114.8(4) . . ? C2 B3 Co1 65.5(3) . . ? B4 B3 Co1 63.5(3) . . ? B9 B3 Co1 110.0(4) . . ? Co8 B3 Co1 122.8(3) . . ? C10 B4 B9 57.9(4) . . ? C10 B4 B5 58.1(4) . . ? B9 B4 B5 111.3(6) . . ? C10 B4 B3 107.5(6) . . ? B9 B4 B3 61.1(4) . . ? B5 B4 B3 121.2(6) . . ? C10 B4 Co1 108.2(5) . . ? B9 B4 Co1 115.3(5) . . ? B5 B4 Co1 65.9(4) . . ? B3 B4 Co1 67.7(3) . . ? C10 B4 H4 124(3) . . ? B9 B4 H4 115(3) . . ? B5 B4 H4 119(3) . . ? B3 B4 H4 115(3) . . ? Co1 B4 H4 121(3) . . ? C10 B5 B6 106.4(6) . . ? C10 B5 B11 56.6(5) . . ? B6 B5 B11 59.4(5) . . ? C10 B5 B4 58.6(4) . . ? B6 B5 B4 119.8(6) . . ? B11 B5 B4 109.0(6) . . ? C10 B5 Co1 107.7(5) . . ? B6 B5 Co1 67.8(4) . . ? B11 B5 Co1 112.1(5) . . ? B4 B5 Co1 64.8(4) . . ? C10 B5 H5 120(3) . . ? B6 B5 H5 125(3) . . ? B11 B5 H5 127(3) . . ? B4 B5 H5 108(3) . . ? Co1 B5 H5 117(3) . . ? B5 B6 B11 61.9(5) . . ? B5 B6 B12 112.0(6) . . ? B11 B6 B12 58.8(5) . . ? B5 B6 B7 117.6(6) . . ? B11 B6 B7 109.6(6) . . ? B12 B6 B7 60.2(4) . . ? B5 B6 Co1 65.4(4) . . ? B11 B6 Co1 112.1(5) . . ? B12 B6 Co1 111.0(5) . . ? B7 B6 Co1 63.3(4) . . ? B5 B6 H6 117(3) . . ? B11 B6 H6 125(3) . . ? B12 B6 H6 123(3) . . ? B7 B6 H6 115(3) . . ? Co1 B6 H6 115(3) . . ? C2 B7 B12 107.4(5) . . ? C2 B7 B6 119.5(6) . . ? B12 B7 B6 59.4(5) . . ? C2 B7 B13 58.9(4) . . ? B12 B7 B13 58.5(4) . . ? B6 B7 B13 111.2(5) . . ? C2 B7 Co1 67.4(3) . . ? B12 B7 Co1 113.9(5) . . ? B6 B7 Co1 67.8(4) . . ? B13 B7 Co1 115.9(5) . . ? C2 B7 H7 117(3) . . ? B12 B7 H7 122(3) . . ? B6 B7 H7 119(3) . . ? B13 B7 H7 117(3) . . ? Co1 B7 H7 117(3) . . ? B13 Co8 B9 100.3(3) . . ? B13 Co8 C2 50.1(3) . . ? B9 Co8 C2 87.4(3) . . ? B13 Co8 C82 127.7(3) . . ? B9 Co8 C82 99.9(3) . . ? C2 Co8 C82 172.6(3) . . ? B13 Co8 C83 96.1(3) . . ? B9 Co8 C83 135.7(3) . . ? C2 Co8 C83 133.0(3) . . ? C82 Co8 C83 40.2(2) . . ? B13 Co8 B3 90.7(3) . . ? B9 Co8 B3 52.1(3) . . ? C2 Co8 B3 47.3(3) . . ? C82 Co8 B3 138.4(3) . . ? C83 Co8 B3 167.8(3) . . ? B13 Co8 C81 162.7(3) . . ? B9 Co8 C81 94.8(3) . . ? C2 Co8 C81 139.9(3) . . ? C82 Co8 C81 40.0(2) . . ? C83 Co8 C81 66.9(3) . . ? B3 Co8 C81 105.3(3) . . ? B13 Co8 C85 132.0(3) . . ? B9 Co8 C85 123.9(3) . . ? C2 Co8 C85 109.2(3) . . ? C82 Co8 C85 66.6(3) . . ? C83 Co8 C85 66.5(3) . . ? B3 Co8 C85 101.5(3) . . ? C81 Co8 C85 39.2(2) . . ? B13 Co8 C84 98.3(3) . . ? B9 Co8 C84 161.3(3) . . ? C2 Co8 C84 105.9(3) . . ? C82 Co8 C84 66.9(3) . . ? C83 Co8 C84 39.4(2) . . ? B3 Co8 C84 129.5(3) . . ? C81 Co8 C84 66.5(3) . . ? C85 Co8 C84 39.8(2) . . ? B13 Co8 B14 55.2(3) . . ? B9 Co8 B14 56.0(3) . . ? C2 Co8 B14 83.2(3) . . ? C82 Co8 B14 101.0(3) . . ? C83 Co8 B14 104.5(3) . . ? B3 Co8 B14 87.7(3) . . ? C81 Co8 B14 130.4(3) . . ? C85 Co8 B14 167.6(3) . . ? C84 Co8 B14 137.1(3) . . ? C10 B9 B4 59.5(4) . . ? C10 B9 B3 108.2(5) . . ? B4 B9 B3 60.5(4) . . ? C10 B9 B14 60.0(4) . . ? B4 B9 B14 104.5(5) . . ? B3 B9 B14 103.5(5) . . ? C10 B9 Co8 123.4(5) . . ? B4 B9 Co8 122.0(5) . . ? B3 B9 Co8 66.3(4) . . ? B14 B9 Co8 66.8(4) . . ? C10 B9 H9 113(3) . . ? B4 B9 H9 113(3) . . ? B3 B9 H9 124(3) . . ? B14 B9 H9 129(3) . . ? Co8 B9 H9 115(3) . . ? B11 C10 B9 129.2(6) . . ? B11 C10 B5 64.3(5) . . ? B9 C10 B5 120.3(6) . . ? B11 C10 B4 119.9(6) . . ? B9 C10 B4 62.5(5) . . ? B5 C10 B4 63.4(5) . . ? B11 C10 B14 65.3(5) . . ? B9 C10 B14 68.3(5) . . ? B5 C10 B14 113.4(6) . . ? B4 C10 B14 112.8(5) . . ? B11 C10 H10 109(4) . . ? B9 C10 H10 109(4) . . ? B5 C10 H10 118(4) . . ? B4 C10 H10 120(4) . . ? B14 C10 H10 118(4) . . ? C10 B11 B12 116.6(6) . . ? C10 B11 B6 107.9(6) . . ? B12 B11 B6 61.4(5) . . ? C10 B11 B5 59.1(5) . . ? B12 B11 B5 111.6(6) . . ? B6 B11 B5 58.8(5) . . ? C10 B11 B14 62.4(4) . . ? B12 B11 B14 63.5(5) . . ? B6 B11 B14 107.6(6) . . ? B5 B11 B14 107.4(6) . . ? C10 B11 H11 114(4) . . ? B12 B11 H11 121(4) . . ? B6 B11 H11 125(4) . . ? B5 B11 H11 119(4) . . ? B14 B11 H11 122(4) . . ? B11 B12 B13 121.1(6) . . ? B11 B12 B6 59.8(5) . . ? B13 B12 B6 114.7(6) . . ? B11 B12 B7 110.7(6) . . ? B13 B12 B7 61.4(4) . . ? B6 B12 B7 60.5(5) . . ? B11 B12 B14 62.8(5) . . ? B13 B12 B14 64.4(4) . . ? B6 B12 B14 105.9(6) . . ? B7 B12 B14 105.3(5) . . ? B11 B12 H12 115(3) . . ? B13 B12 H12 113(3) . . ? B6 B12 H12 125(3) . . ? B7 B12 H12 127(3) . . ? B14 B12 H12 119(3) . . ? C2 B13 B12 107.5(6) . . ? C2 B13 B7 57.5(4) . . ? B12 B13 B7 60.0(4) . . ? C2 B13 B14 100.5(6) . . ? B12 B13 B14 61.6(4) . . ? B7 B13 B14 102.4(5) . . ? C2 B13 Co8 66.9(4) . . ? B12 B13 Co8 126.7(5) . . ? B7 B13 Co8 120.5(5) . . ? B14 B13 Co8 67.4(3) . . ? C2 B13 H13 118(4) . . ? B12 B13 H13 118(4) . . ? B7 B13 H13 114(4) . . ? B14 B13 H13 137(4) . . ? Co8 B13 H13 110(4) . . ? C10 B14 B11 52.3(4) . . ? C10 B14 B12 99.4(5) . . ? B11 B14 B12 53.7(4) . . ? C10 B14 B13 124.3(6) . . ? B11 B14 B13 103.4(5) . . ? B12 B14 B13 53.9(4) . . ? C10 B14 B9 51.7(4) . . ? B11 B14 B9 101.5(5) . . ? B12 B14 B9 127.7(6) . . ? B13 B14 B9 102.9(5) . . ? C10 B14 Co8 106.5(4) . . ? B11 B14 Co8 140.0(6) . . ? B12 B14 Co8 109.6(4) . . ? B13 B14 Co8 57.3(3) . . ? B9 B14 Co8 57.2(3) . . ? C10 B14 H14 111(3) . . ? B11 B14 H14 111(3) . . ? B12 B14 H14 121(3) . . ? B13 B14 H14 125(3) . . ? B9 B14 H14 110(3) . . ? Co8 B14 H14 108(3) . . ? C12 C11 C15 107.6(6) . . ? C12 C11 Co1 69.8(4) . . ? C15 C11 Co1 70.7(4) . . ? C12 C11 H11A 126.2 . . ? C15 C11 H11A 126.2 . . ? Co1 C11 H11A 126.2 . . ? C11 C12 C13 108.6(6) . . ? C11 C12 Co1 71.0(4) . . ? C13 C12 Co1 69.4(4) . . ? C11 C12 H12A 125.7 . . ? C13 C12 H12A 125.7 . . ? Co1 C12 H12A 125.7 . . ? C14 C13 C12 106.4(7) . . ? C14 C13 Co1 70.6(4) . . ? C12 C13 Co1 69.9(4) . . ? C14 C13 H13A 126.8 . . ? C12 C13 H13A 126.8 . . ? Co1 C13 H13A 126.8 . . ? C15 C14 C13 107.8(6) . . ? C15 C14 Co1 70.9(4) . . ? C13 C14 Co1 69.2(4) . . ? C15 C14 H14A 126.1 . . ? C13 C14 H14A 126.1 . . ? Co1 C14 H14A 126.1 . . ? C14 C15 C11 109.7(6) . . ? C14 C15 Co1 70.1(4) . . ? C11 C15 Co1 70.2(4) . . ? C14 C15 H15 125.1 . . ? C11 C15 H15 125.1 . . ? Co1 C15 H15 125.1 . . ? O31 C31 C32 108.6(5) . . ? O31 C31 H31A 110.0 . . ? C32 C31 H31A 110.0 . . ? O31 C31 H31B 110.0 . . ? C32 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? B3 O31 C31 120.9(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C85 C81 C82 108.1(6) . . ? C85 C81 Co8 70.9(4) . . ? C82 C81 Co8 69.2(4) . . ? C85 C81 H81 125.9 . . ? C82 C81 H81 125.9 . . ? Co8 C81 H81 125.9 . . ? C81 C82 C83 107.6(6) . . ? C81 C82 Co8 70.9(4) . . ? C83 C82 Co8 70.2(4) . . ? C81 C82 H82 126.2 . . ? C83 C82 H82 126.2 . . ? Co8 C82 H82 126.2 . . ? C84 C83 C82 108.6(6) . . ? C84 C83 Co8 71.6(4) . . ? C82 C83 Co8 69.6(4) . . ? C84 C83 H83 125.7 . . ? C82 C83 H83 125.7 . . ? Co8 C83 H83 125.7 . . ? C83 C84 C85 107.3(6) . . ? C83 C84 Co8 69.0(4) . . ? C85 C84 Co8 69.9(4) . . ? C83 C84 H84 126.4 . . ? C85 C84 H84 126.4 . . ? Co8 C84 H84 126.4 . . ? C81 C85 C84 108.4(6) . . ? C81 C85 Co8 69.9(4) . . ? C84 C85 Co8 70.4(4) . . ? C81 C85 H85 125.8 . . ? C84 C85 H85 125.8 . . ? Co8 C85 H85 125.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.480 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.102 _database_code_depnum_ccdc_archive 'CCDC 939753' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x83115 _audit_update_record ; 2013-05-03 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 B10 Co2' _chemical_formula_weight 392.26 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' Co Co 0.3494 0.9721 '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 7.4419(4) _cell_length_b 10.1756(6) _cell_length_c 12.2035(7) _cell_angle_alpha 90.288(3) _cell_angle_beta 103.174(3) _cell_angle_gamma 111.022(3) _cell_volume 836.07(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 522 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 22.08 _exptl_crystal_description BLOCK _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 1.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5214 _exptl_absorpt_correction_T_max 0.7699 _exptl_absorpt_process_details 'TWINABS (Bruker, 2008)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16116 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 29.97 _reflns_number_total 4740 _reflns_number_gt 4001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0331P)^2^+0.4370P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4740 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.44200(3) 0.60678(2) 0.744231(18) 0.01188(6) Uani 1 1 d . . . C2 C 0.4683(3) 0.81173(17) 0.80101(14) 0.0135(3) Uani 1 1 d . . . H2 H 0.348(3) 0.817(2) 0.8096(17) 0.016 Uiso 1 1 d . . . B3 B 0.5592(3) 0.7259(2) 0.90093(16) 0.0166(4) Uani 1 1 d . . . H3 H 0.497(3) 0.697(2) 0.9742(17) 0.020 Uiso 1 1 d . . . B4 B 0.7073(3) 0.6306(2) 0.87159(17) 0.0183(4) Uani 1 1 d . . . H4 H 0.717(3) 0.558(2) 0.9296(17) 0.022 Uiso 1 1 d . . . B5 B 0.7381(3) 0.6217(2) 0.73480(17) 0.0180(4) Uani 1 1 d . . . H5 H 0.761(3) 0.531(2) 0.7075(17) 0.022 Uiso 1 1 d . . . B6 B 0.6229(3) 0.7068(2) 0.62908(16) 0.0155(4) Uani 1 1 d . . . H6 H 0.581(3) 0.663(2) 0.5452(17) 0.019 Uiso 1 1 d . . . B7 B 0.4799(3) 0.80195(19) 0.66517(15) 0.0136(3) Uani 1 1 d . . . H7 H 0.347(3) 0.795(2) 0.6008(17) 0.016 Uiso 1 1 d . . . B8 B 0.6842(3) 0.9109(2) 0.89520(16) 0.0174(4) Uani 1 1 d . . . H8 H 0.694(3) 0.973(2) 0.9676(17) 0.021 Uiso 1 1 d . . . C9 C 0.8095(3) 0.80480(19) 0.92267(15) 0.0197(3) Uani 1 1 d . . . H9 H 0.893(3) 0.829(2) 1.0006(18) 0.024 Uiso 1 1 d . . . B10 B 0.9226(3) 0.7506(2) 0.83915(18) 0.0218(4) Uani 1 1 d . . . H10 H 1.068(3) 0.746(2) 0.8823(18) 0.026 Uiso 1 1 d . . . B11 B 0.8765(3) 0.7916(2) 0.70109(17) 0.0183(4) Uani 1 1 d . . . H11 H 0.996(3) 0.811(2) 0.6624(17) 0.022 Uiso 1 1 d . . . B12 B 0.7312(3) 0.8921(2) 0.65621(16) 0.0160(4) Uani 1 1 d . . . H12 H 0.773(3) 0.953(2) 0.5888(17) 0.019 Uiso 1 1 d . . . Co13 Co 0.63016(3) 0.99780(2) 0.754670(18) 0.01355(7) Uani 1 1 d . . . B14 B 0.8822(3) 0.9247(2) 0.80804(17) 0.0185(4) Uani 1 1 d . . . H14 H 1.024(3) 1.011(2) 0.8427(17) 0.022 Uiso 1 1 d . . . C11 C 0.1794(3) 0.49183(18) 0.78683(16) 0.0207(4) Uani 1 1 d . . . H11A H 0.1320 0.5181 0.8510 0.025 Uiso 1 1 calc R . . C12 C 0.2988(3) 0.40973(17) 0.79166(15) 0.0191(3) Uani 1 1 d . . . H12A H 0.3500 0.3672 0.8597 0.023 Uiso 1 1 calc R . . C13 C 0.3323(3) 0.39758(17) 0.68241(15) 0.0182(3) Uani 1 1 d . . . H13 H 0.4106 0.3446 0.6601 0.022 Uiso 1 1 calc R . . C14 C 0.2316(3) 0.47190(18) 0.61003(15) 0.0180(3) Uani 1 1 d . . . H14A H 0.2272 0.4812 0.5280 0.022 Uiso 1 1 calc R . . C15 C 0.1389(3) 0.53047(18) 0.67515(16) 0.0199(4) Uani 1 1 d . . . H15 H 0.0581 0.5890 0.6470 0.024 Uiso 1 1 calc R . . C131 C 0.4264(3) 1.09416(19) 0.70288(18) 0.0249(4) Uani 1 1 d . . . H131 H 0.2796 1.0444 0.6740 0.030 Uiso 1 1 calc R . . C132 C 0.5659(3) 1.13110(18) 0.63663(15) 0.0216(4) Uani 1 1 d . . . H132 H 0.5357 1.1123 0.5526 0.026 Uiso 1 1 calc R . . C133 C 0.7566(3) 1.19855(18) 0.70988(17) 0.0235(4) Uani 1 1 d . . . H133 H 0.8847 1.2371 0.6866 0.028 Uiso 1 1 calc R . . C134 C 0.7338(3) 1.2062(2) 0.82161(17) 0.0293(4) Uani 1 1 d . . . H134 H 0.8428 1.2504 0.8911 0.035 Uiso 1 1 calc R . . C135 C 0.5288(3) 1.1414(2) 0.81714(17) 0.0294(5) Uani 1 1 d . . . H135 H 0.4673 1.1309 0.8830 0.035 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 0.01324(12) 0.00982(11) 0.01455(11) 0.00040(8) 0.00548(8) 0.00533(9) C2 0.0170(8) 0.0104(7) 0.0154(7) 0.0013(6) 0.0072(6) 0.0060(6) B3 0.0202(9) 0.0157(9) 0.0148(8) 0.0016(7) 0.0050(7) 0.0072(8) B4 0.0192(9) 0.0176(9) 0.0204(9) 0.0021(7) 0.0038(7) 0.0102(8) B5 0.0173(9) 0.0189(10) 0.0221(9) 0.0021(7) 0.0083(8) 0.0098(8) B6 0.0177(9) 0.0148(9) 0.0164(8) 0.0002(7) 0.0086(7) 0.0061(7) B7 0.0168(9) 0.0105(8) 0.0147(8) -0.0002(6) 0.0057(7) 0.0056(7) B8 0.0214(10) 0.0157(9) 0.0147(8) -0.0002(7) 0.0045(7) 0.0062(8) C9 0.0217(9) 0.0193(9) 0.0163(8) -0.0004(6) 0.0020(7) 0.0072(7) B10 0.0174(10) 0.0238(11) 0.0253(10) 0.0019(8) 0.0044(8) 0.0096(8) B11 0.0166(9) 0.0184(10) 0.0218(9) -0.0004(7) 0.0082(8) 0.0065(8) B12 0.0172(9) 0.0159(9) 0.0158(8) 0.0006(7) 0.0069(7) 0.0055(7) Co13 0.01829(12) 0.00942(11) 0.01385(11) 0.00048(8) 0.00602(9) 0.00495(9) B14 0.0163(9) 0.0183(10) 0.0196(9) -0.0018(7) 0.0048(7) 0.0047(8) C11 0.0190(9) 0.0137(8) 0.0283(9) -0.0016(7) 0.0145(7) -0.0004(7) C12 0.0223(9) 0.0101(8) 0.0227(8) 0.0040(6) 0.0066(7) 0.0026(7) C13 0.0195(9) 0.0112(8) 0.0244(9) -0.0014(6) 0.0071(7) 0.0054(7) C14 0.0165(8) 0.0130(8) 0.0197(8) -0.0023(6) 0.0010(7) 0.0021(6) C15 0.0132(8) 0.0129(8) 0.0323(10) 0.0007(7) 0.0061(7) 0.0029(6) C131 0.0259(10) 0.0134(8) 0.0390(11) 0.0050(8) 0.0094(8) 0.0108(8) C132 0.0323(10) 0.0136(8) 0.0195(8) 0.0031(6) 0.0048(7) 0.0101(7) C133 0.0285(10) 0.0105(8) 0.0299(10) 0.0044(7) 0.0095(8) 0.0039(7) C134 0.0473(13) 0.0133(9) 0.0214(9) -0.0033(7) -0.0015(9) 0.0102(9) C135 0.0536(14) 0.0182(9) 0.0318(10) 0.0071(8) 0.0242(10) 0.0229(9) _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 C13 2.0551(17) . ? Co1 C12 2.0618(17) . ? Co1 C15 2.0665(18) . ? Co1 C14 2.0700(17) . ? Co1 C11 2.0703(17) . ? Co1 B3 2.0842(19) . ? Co1 C2 2.1210(16) . ? Co1 B4 2.151(2) . ? Co1 B7 2.1670(18) . ? Co1 B6 2.1719(18) . ? Co1 B5 2.1839(19) . ? C2 B3 1.664(2) . ? C2 B7 1.684(2) . ? C2 B8 1.704(3) . ? C2 Co13 2.0103(16) . ? C2 H2 0.95(2) . ? B3 C9 1.698(3) . ? B3 B8 1.786(3) . ? B3 B4 1.796(3) . ? B3 H3 1.09(2) . ? B4 C9 1.708(3) . ? B4 B5 1.742(3) . ? B4 B10 1.762(3) . ? B4 H4 1.04(2) . ? B5 B10 1.767(3) . ? B5 B11 1.773(3) . ? B5 B6 1.786(3) . ? B5 H5 1.06(2) . ? B6 B12 1.760(3) . ? B6 B11 1.774(3) . ? B6 B7 1.793(3) . ? B6 H6 1.05(2) . ? B7 B12 1.793(3) . ? B7 Co13 2.0585(18) . ? B7 H7 1.09(2) . ? B8 C9 1.653(3) . ? B8 Co13 1.9597(19) . ? B8 B14 1.973(3) . ? B8 H8 1.06(2) . ? C9 B10 1.664(3) . ? C9 B14 1.904(3) . ? C9 H9 0.99(2) . ? B10 B11 1.725(3) . ? B10 B14 1.925(3) . ? B10 H10 1.10(2) . ? B11 B12 1.744(3) . ? B11 B14 1.858(3) . ? B11 H11 1.06(2) . ? B12 B14 1.893(3) . ? B12 Co13 2.0360(19) . ? B12 H12 1.07(2) . ? Co13 C133 2.0551(18) . ? Co13 C134 2.0693(19) . ? Co13 C131 2.0727(18) . ? Co13 C132 2.0772(17) . ? Co13 C135 2.0798(18) . ? Co13 B14 2.224(2) . ? B14 H14 1.09(2) . ? C11 C12 1.414(3) . ? C11 C15 1.416(3) . ? C11 H11A 1.0000 . ? C12 C13 1.424(2) . ? C12 H12A 1.0000 . ? C13 C14 1.423(2) . ? C13 H13 1.0000 . ? C14 C15 1.415(2) . ? C14 H14A 1.0000 . ? C15 H15 1.0000 . ? C131 C132 1.407(3) . ? C131 C135 1.415(3) . ? C131 H131 1.0000 . ? C132 C133 1.415(3) . ? C132 H132 1.0000 . ? C133 C134 1.417(3) . ? C133 H133 1.0000 . ? C134 C135 1.416(3) . ? C134 H134 1.0000 . ? C135 H135 1.0000 . ? 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 C13 Co1 C12 40.47(7) . . ? C13 Co1 C15 67.52(7) . . ? C12 Co1 C15 67.36(7) . . ? C13 Co1 C14 40.37(7) . . ? C12 Co1 C14 67.72(7) . . ? C15 Co1 C14 40.00(7) . . ? C13 Co1 C11 67.62(7) . . ? C12 Co1 C11 40.03(7) . . ? C15 Co1 C11 40.04(7) . . ? C14 Co1 C11 67.43(7) . . ? C13 Co1 B3 137.98(7) . . ? C12 Co1 B3 100.68(7) . . ? C15 Co1 B3 119.71(7) . . ? C14 Co1 B3 158.70(8) . . ? C11 Co1 B3 92.08(8) . . ? C13 Co1 C2 163.71(7) . . ? C12 Co1 C2 131.67(7) . . ? C15 Co1 C2 96.52(7) . . ? C14 Co1 C2 127.84(7) . . ? C11 Co1 C2 98.29(7) . . ? B3 Co1 C2 46.60(7) . . ? C13 Co1 B4 104.06(7) . . ? C12 Co1 B4 90.58(8) . . ? C15 Co1 B4 154.73(8) . . ? C14 Co1 B4 143.02(7) . . ? C11 Co1 B4 114.80(8) . . ? B3 Co1 B4 50.15(7) . . ? C2 Co1 B4 89.06(7) . . ? C13 Co1 B7 133.52(7) . . ? C12 Co1 B7 158.83(7) . . ? C15 Co1 B7 91.50(7) . . ? C14 Co1 B7 97.20(7) . . ? C11 Co1 B7 121.43(7) . . ? B3 Co1 B7 88.49(7) . . ? C2 Co1 B7 46.23(6) . . ? B4 Co1 B7 109.72(8) . . ? C13 Co1 B6 101.89(7) . . ? C12 Co1 B6 140.74(7) . . ? C15 Co1 B6 115.17(7) . . ? C14 Co1 B6 89.61(7) . . ? C11 Co1 B6 154.84(8) . . ? B3 Co1 B6 109.24(8) . . ? C2 Co1 B6 87.59(7) . . ? B4 Co1 B6 89.61(8) . . ? B7 Co1 B6 48.80(7) . . ? C13 Co1 B5 89.36(7) . . ? C12 Co1 B5 108.06(7) . . ? C15 Co1 B5 149.54(8) . . ? C14 Co1 B5 109.63(7) . . ? C11 Co1 B5 147.80(8) . . ? B3 Co1 B5 90.72(8) . . ? C2 Co1 B5 106.75(7) . . ? B4 Co1 B5 47.38(8) . . ? B7 Co1 B5 90.70(7) . . ? B6 Co1 B5 48.41(7) . . ? B3 C2 B7 124.81(13) . . ? B3 C2 B8 64.04(11) . . ? B7 C2 B8 115.76(13) . . ? B3 C2 Co13 124.04(12) . . ? B7 C2 Co13 67.06(8) . . ? B8 C2 Co13 63.05(9) . . ? B3 C2 Co1 65.53(9) . . ? B7 C2 Co1 68.32(8) . . ? B8 C2 Co1 116.66(11) . . ? Co13 C2 Co1 127.44(8) . . ? B3 C2 H2 111.8(12) . . ? B7 C2 H2 113.4(12) . . ? B8 C2 H2 118.8(12) . . ? Co13 C2 H2 108.4(12) . . ? Co1 C2 H2 113.8(12) . . ? C2 B3 C9 104.53(14) . . ? C2 B3 B8 59.08(11) . . ? C9 B3 B8 56.57(11) . . ? C2 B3 B4 119.94(14) . . ? C9 B3 B4 58.44(11) . . ? B8 B3 B4 110.08(14) . . ? C2 B3 Co1 67.87(9) . . ? C9 B3 Co1 109.32(11) . . ? B8 B3 Co1 114.72(11) . . ? B4 B3 Co1 66.86(9) . . ? C2 B3 H3 122.0(11) . . ? C9 B3 H3 118.4(11) . . ? B8 B3 H3 115.7(11) . . ? B4 B3 H3 115.3(11) . . ? Co1 B3 H3 123.6(11) . . ? C9 B4 B5 107.12(14) . . ? C9 B4 B10 57.29(11) . . ? B5 B4 B10 60.55(12) . . ? C9 B4 B3 57.91(11) . . ? B5 B4 B3 118.30(14) . . ? B10 B4 B3 108.93(14) . . ? C9 B4 Co1 106.00(11) . . ? B5 B4 Co1 67.30(9) . . ? B10 B4 Co1 112.33(12) . . ? B3 B4 Co1 62.99(9) . . ? C9 B4 H4 116.9(12) . . ? B5 B4 H4 125.6(11) . . ? B10 B4 H4 120.9(11) . . ? B3 B4 H4 111.7(11) . . ? Co1 B4 H4 123.7(12) . . ? B4 B5 B10 60.29(12) . . ? B4 B5 B11 110.57(15) . . ? B10 B5 B11 58.34(12) . . ? B4 B5 B6 119.40(13) . . ? B10 B5 B6 109.45(14) . . ? B11 B5 B6 59.78(11) . . ? B4 B5 Co1 65.32(9) . . ? B10 B5 Co1 110.66(11) . . ? B11 B5 Co1 111.03(11) . . ? B6 B5 Co1 65.44(9) . . ? B4 B5 H5 116.8(11) . . ? B10 B5 H5 120.9(11) . . ? B11 B5 H5 120.4(11) . . ? B6 B5 H5 117.4(11) . . ? Co1 B5 H5 120.2(11) . . ? B12 B6 B11 59.16(11) . . ? B12 B6 B5 111.61(14) . . ? B11 B6 B5 59.74(11) . . ? B12 B6 B7 60.61(11) . . ? B11 B6 B7 110.11(13) . . ? B5 B6 B7 119.76(13) . . ? B12 B6 Co1 113.13(11) . . ? B11 B6 Co1 111.55(11) . . ? B5 B6 Co1 66.15(9) . . ? B7 B6 Co1 65.45(8) . . ? B12 B6 H6 118.4(11) . . ? B11 B6 H6 121.2(11) . . ? B5 B6 H6 117.5(11) . . ? B7 B6 H6 116.4(11) . . ? Co1 B6 H6 119.3(11) . . ? C2 B7 B6 117.41(13) . . ? C2 B7 B12 109.48(13) . . ? B6 B7 B12 58.79(10) . . ? C2 B7 Co13 64.07(8) . . ? B6 B7 Co13 118.07(12) . . ? B12 B7 Co13 63.39(9) . . ? C2 B7 Co1 65.45(8) . . ? B6 B7 Co1 65.74(8) . . ? B12 B7 Co1 111.98(11) . . ? Co13 B7 Co1 122.48(9) . . ? C2 B7 H7 116.9(10) . . ? B6 B7 H7 116.2(10) . . ? B12 B7 H7 125.7(10) . . ? Co13 B7 H7 114.1(10) . . ? Co1 B7 H7 112.0(10) . . ? C9 B8 C2 104.73(13) . . ? C9 B8 B3 59.02(11) . . ? C2 B8 B3 56.88(10) . . ? C9 B8 Co13 127.49(13) . . ? C2 B8 Co13 66.12(9) . . ? B3 B8 Co13 120.21(12) . . ? C9 B8 B14 62.64(11) . . ? C2 B8 B14 101.68(12) . . ? B3 B8 B14 105.22(13) . . ? Co13 B8 B14 68.88(9) . . ? C9 B8 H8 113.3(11) . . ? C2 B8 H8 124.7(11) . . ? B3 B8 H8 113.0(11) . . ? Co13 B8 H8 113.0(11) . . ? B14 B8 H8 130.8(11) . . ? B8 C9 B10 128.09(15) . . ? B8 C9 B3 64.41(12) . . ? B10 C9 B3 118.92(15) . . ? B8 C9 B4 121.75(14) . . ? B10 C9 B4 63.00(12) . . ? B3 C9 B4 63.66(11) . . ? B8 C9 B14 66.93(11) . . ? B10 C9 B14 64.90(11) . . ? B3 C9 B14 112.00(13) . . ? B4 C9 B14 111.64(13) . . ? B8 C9 H9 109.9(12) . . ? B10 C9 H9 110.0(12) . . ? B3 C9 H9 119.4(12) . . ? B4 C9 H9 117.2(12) . . ? B14 C9 H9 120.1(12) . . ? C9 B10 B11 115.71(15) . . ? C9 B10 B4 59.70(11) . . ? B11 B10 B4 111.88(15) . . ? C9 B10 B5 107.95(14) . . ? B11 B10 B5 61.01(12) . . ? B4 B10 B5 59.16(12) . . ? C9 B10 B14 63.59(11) . . ? B11 B10 B14 60.90(11) . . ? B4 B10 B14 108.28(13) . . ? B5 B10 B14 105.25(14) . . ? C9 B10 H10 114.9(11) . . ? B11 B10 H10 121.3(11) . . ? B4 B10 H10 118.2(11) . . ? B5 B10 H10 125.2(11) . . ? B14 B10 H10 123.3(11) . . ? B10 B11 B12 121.22(14) . . ? B10 B11 B5 60.65(12) . . ? B12 B11 B5 112.99(14) . . ? B10 B11 B6 111.97(14) . . ? B12 B11 B6 60.02(11) . . ? B5 B11 B6 60.47(11) . . ? B10 B11 B14 64.88(12) . . ? B12 B11 B14 63.31(11) . . ? B5 B11 B14 107.87(13) . . ? B6 B11 B14 105.59(13) . . ? B10 B11 H11 115.0(11) . . ? B12 B11 H11 114.1(11) . . ? B5 B11 H11 123.1(11) . . ? B6 B11 H11 124.0(11) . . ? B14 B11 H11 120.7(12) . . ? B11 B12 B6 60.82(11) . . ? B11 B12 B7 111.47(14) . . ? B6 B12 B7 60.60(11) . . ? B11 B12 B14 61.28(11) . . ? B6 B12 B14 104.69(13) . . ? B7 B12 B14 104.34(12) . . ? B11 B12 Co13 127.18(12) . . ? B6 B12 Co13 120.92(12) . . ? B7 B12 Co13 64.68(8) . . ? B14 B12 Co13 68.84(9) . . ? B11 B12 H12 113.0(11) . . ? B6 B12 H12 118.5(11) . . ? B7 B12 H12 124.3(11) . . ? B14 B12 H12 125.8(11) . . ? Co13 B12 H12 109.4(11) . . ? B8 Co13 C2 50.83(8) . . ? B8 Co13 B12 98.56(8) . . ? C2 Co13 B12 89.14(7) . . ? B8 Co13 C133 132.08(8) . . ? C2 Co13 C133 170.19(7) . . ? B12 Co13 C133 99.07(8) . . ? B8 Co13 B7 91.11(8) . . ? C2 Co13 B7 48.88(7) . . ? B12 Co13 B7 51.93(8) . . ? C133 Co13 B7 133.90(8) . . ? B8 Co13 C134 98.74(8) . . ? C2 Co13 C134 134.50(8) . . ? B12 Co13 C134 132.92(9) . . ? C133 Co13 C134 40.19(8) . . ? B7 Co13 C134 167.53(8) . . ? B8 Co13 C131 128.76(8) . . ? C2 Co13 C131 103.60(7) . . ? B12 Co13 C131 127.85(8) . . ? C133 Co13 C131 67.10(8) . . ? B7 Co13 C131 100.79(8) . . ? C134 Co13 C131 67.05(8) . . ? B8 Co13 C132 163.77(8) . . ? C2 Co13 C132 133.92(7) . . ? B12 Co13 C132 97.09(8) . . ? C133 Co13 C132 40.03(8) . . ? B7 Co13 C132 101.96(7) . . ? C134 Co13 C132 67.11(7) . . ? C131 Co13 C132 39.62(8) . . ? B8 Co13 C135 97.35(8) . . ? C2 Co13 C135 103.80(7) . . ? B12 Co13 C135 163.68(8) . . ? C133 Co13 C135 67.21(8) . . ? B7 Co13 C135 131.41(9) . . ? C134 Co13 C135 39.91(9) . . ? C131 Co13 C135 39.84(8) . . ? C132 Co13 C135 66.79(7) . . ? B8 Co13 B14 55.83(8) . . ? C2 Co13 B14 84.67(7) . . ? B12 Co13 B14 52.54(8) . . ? C133 Co13 B14 104.56(8) . . ? B7 Co13 B14 85.59(7) . . ? C134 Co13 B14 106.26(8) . . ? C131 Co13 B14 171.62(8) . . ? C132 Co13 B14 133.98(8) . . ? C135 Co13 B14 137.42(8) . . ? B11 B14 B12 55.41(10) . . ? B11 B14 C9 99.42(13) . . ? B12 B14 C9 123.98(14) . . ? B11 B14 B10 54.22(11) . . ? B12 B14 B10 104.69(13) . . ? C9 B14 B10 51.51(10) . . ? B11 B14 B8 128.37(14) . . ? B12 B14 B8 103.14(12) . . ? C9 B14 B8 50.43(9) . . ? B10 B14 B8 99.82(13) . . ? B11 B14 Co13 111.89(12) . . ? B12 B14 Co13 58.62(8) . . ? C9 B14 Co13 103.26(10) . . ? B10 B14 Co13 138.37(12) . . ? B8 B14 Co13 55.28(8) . . ? B11 B14 H14 117.4(11) . . ? B12 B14 H14 126.1(11) . . ? C9 B14 H14 109.9(11) . . ? B10 B14 H14 107.3(11) . . ? B8 B14 H14 112.6(11) . . ? Co13 B14 H14 113.0(11) . . ? C12 C11 C15 107.97(15) . . ? C12 C11 Co1 69.66(10) . . ? C15 C11 Co1 69.83(10) . . ? C12 C11 H11A 126.0 . . ? C15 C11 H11A 126.0 . . ? Co1 C11 H11A 126.0 . . ? C11 C12 C13 107.98(15) . . ? C11 C12 Co1 70.31(9) . . ? C13 C12 Co1 69.52(10) . . ? C11 C12 H12A 126.0 . . ? C13 C12 H12A 126.0 . . ? Co1 C12 H12A 126.0 . . ? C14 C13 C12 107.91(15) . . ? C14 C13 Co1 70.38(10) . . ? C12 C13 Co1 70.02(10) . . ? C14 C13 H13 126.0 . . ? C12 C13 H13 126.0 . . ? Co1 C13 H13 126.0 . . ? C15 C14 C13 107.62(16) . . ? C15 C14 Co1 69.87(10) . . ? C13 C14 Co1 69.25(10) . . ? C15 C14 H14A 126.2 . . ? C13 C14 H14A 126.2 . . ? Co1 C14 H14A 126.2 . . ? C14 C15 C11 108.52(16) . . ? C14 C15 Co1 70.13(10) . . ? C11 C15 Co1 70.12(10) . . ? C14 C15 H15 125.7 . . ? C11 C15 H15 125.7 . . ? Co1 C15 H15 125.7 . . ? C132 C131 C135 108.38(18) . . ? C132 C131 Co13 70.36(10) . . ? C135 C131 Co13 70.35(11) . . ? C132 C131 H131 125.8 . . ? C135 C131 H131 125.8 . . ? Co13 C131 H131 125.8 . . ? C131 C132 C133 107.93(17) . . ? C131 C132 Co13 70.01(10) . . ? C133 C132 Co13 69.14(10) . . ? C131 C132 H132 126.0 . . ? C133 C132 H132 126.0 . . ? Co13 C132 H132 126.0 . . ? C132 C133 C134 108.08(18) . . ? C132 C133 Co13 70.82(10) . . ? C134 C133 Co13 70.44(11) . . ? C132 C133 H133 125.9 . . ? C134 C133 H133 125.9 . . ? Co13 C133 H133 125.9 . . ? C135 C134 C133 107.76(18) . . ? C135 C134 Co13 70.44(11) . . ? C133 C134 Co13 69.37(10) . . ? C135 C134 H134 126.1 . . ? C133 C134 H134 126.1 . . ? Co13 C134 H134 126.1 . . ? C131 C135 C134 107.83(17) . . ? C131 C135 Co13 69.81(10) . . ? C134 C135 Co13 69.65(11) . . ? C131 C135 H135 126.1 . . ? C134 C135 H135 126.1 . . ? Co13 C135 H135 126.1 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.558 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.078 _database_code_depnum_ccdc_archive 'CCDC 939754' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x83090 _audit_update_record ; 2013-05-02 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H22 B10 Co2, C H2 Cl2' _chemical_formula_sum 'C13 H24 B10 Cl2 Co2' _chemical_formula_weight 477.18 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6842(8) _cell_length_b 11.0372(11) _cell_length_c 11.7319(12) _cell_angle_alpha 93.130(5) _cell_angle_beta 95.145(5) _cell_angle_gamma 98.582(5) _cell_volume 977.56(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5051 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 31.07 _exptl_crystal_description BLOCK _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 1.965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4924 _exptl_absorpt_correction_T_max 0.7186 _exptl_absorpt_process_details 'Bruker TWINABS' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31755 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.3952 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 31.29 _reflns_number_total 6087 _reflns_number_gt 4847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0496P)^2^+2.0381P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6087 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1294 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.182 _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 0.70215(7) 0.96972(5) 0.24525(4) 0.01114(12) Uani 1 1 d . . . C2 C 0.7622(5) 0.7880(4) 0.2194(3) 0.0118(7) Uani 1 1 d . . . H2 H 0.872(6) 0.790(5) 0.188(4) 0.014 Uiso 1 1 d . . . B3 B 0.7761(6) 0.8390(4) 0.3590(4) 0.0144(8) Uani 1 1 d . . . H3 H 0.898(7) 0.877(5) 0.411(4) 0.017 Uiso 1 1 d . . . C4 C 0.6066(5) 0.9087(4) 0.3990(3) 0.0145(7) Uani 1 1 d . . . H4 H 0.648(7) 0.960(5) 0.468(4) 0.017 Uiso 1 1 d . . . B5 B 0.4440(6) 0.9492(4) 0.3079(4) 0.0159(8) Uani 1 1 d . . . H5 H 0.389(7) 1.040(5) 0.337(4) 0.019 Uiso 1 1 d . . . B6 B 0.4387(6) 0.9020(4) 0.1617(4) 0.0162(8) Uani 1 1 d . . . H6 H 0.377(7) 0.962(5) 0.105(4) 0.019 Uiso 1 1 d . . . B7 B 0.6090(6) 0.8197(4) 0.1191(4) 0.0150(8) Uani 1 1 d . . . H7 H 0.653(7) 0.829(5) 0.038(4) 0.018 Uiso 1 1 d . . . Co8 Co 0.72162(7) 0.65247(5) 0.32791(4) 0.01228(12) Uani 1 1 d . . . B9 B 0.5931(6) 0.7578(4) 0.4253(4) 0.0150(8) Uani 1 1 d . . . H9 H 0.607(7) 0.735(5) 0.511(4) 0.018 Uiso 1 1 d . . . B10 B 0.4046(6) 0.8202(5) 0.3904(4) 0.0173(8) Uani 1 1 d . . . H10 H 0.320(7) 0.821(5) 0.461(4) 0.021 Uiso 1 1 d . . . C11 C 0.8424(6) 1.0636(4) 0.1276(4) 0.0185(8) Uani 1 1 d . . . H11A H 0.8581 1.0318 0.0483 0.022 Uiso 1 1 calc R . . B11 B 0.3070(6) 0.8136(4) 0.2512(4) 0.0173(8) Uani 1 1 d . . . H11 H 0.161(7) 0.819(5) 0.239(5) 0.021 Uiso 1 1 d . . . C12 C 0.9565(5) 1.0560(4) 0.2294(4) 0.0185(8) Uani 1 1 d . . . H12A H 1.0654 1.0161 0.2339 0.022 Uiso 1 1 calc R . . B12 B 0.4026(6) 0.7392(5) 0.1446(4) 0.0174(9) Uani 1 1 d . . . H12 H 0.323(7) 0.703(5) 0.087(5) 0.021 Uiso 1 1 d . . . C13 C 0.8885(6) 1.1141(4) 0.3228(4) 0.0219(8) Uani 1 1 d . . . H13A H 0.9404 1.1223 0.4046 0.026 Uiso 1 1 calc R . . B13 B 0.5914(6) 0.6747(4) 0.1766(4) 0.0142(8) Uani 1 1 d . . . H13 H 0.606(7) 0.591(5) 0.117(4) 0.017 Uiso 1 1 d . . . C14 C 0.7335(6) 1.1573(4) 0.2795(3) 0.0196(8) Uani 1 1 d . . . H14A H 0.6568 1.2020 0.3259 0.023 Uiso 1 1 calc R . . B14 B 0.4342(6) 0.6827(4) 0.2960(4) 0.0139(8) Uani 1 1 d . . . H14 H 0.343(7) 0.594(5) 0.305(4) 0.017 Uiso 1 1 d . . . C15 C 0.7049(6) 1.1280(4) 0.1597(3) 0.0171(7) Uani 1 1 d . . . H15A H 0.6059 1.1490 0.1068 0.021 Uiso 1 1 calc R . . C81 C 0.9117(6) 0.5472(5) 0.2849(4) 0.0247(9) Uani 1 1 d . . . H81 H 0.9799 0.5552 0.2163 0.030 Uiso 1 1 calc R . . C82 C 0.7490(7) 0.4701(4) 0.2903(5) 0.0270(10) Uani 1 1 d . . . H82 H 0.6816 0.4143 0.2261 0.032 Uiso 1 1 calc R . . C83 C 0.6968(6) 0.4865(5) 0.4028(5) 0.0277(10) Uani 1 1 d . . . H83 H 0.5875 0.4434 0.4320 0.033 Uiso 1 1 calc R . . C84 C 0.8309(6) 0.5719(4) 0.4672(4) 0.0230(9) Uani 1 1 d . . . H84 H 0.8319 0.6003 0.5497 0.028 Uiso 1 1 calc R . . C85 C 0.9622(5) 0.6104(4) 0.3943(4) 0.0217(9) Uani 1 1 d . . . H85 H 1.0726 0.6705 0.4163 0.026 Uiso 1 1 calc R . . Cl1S Cl 0.70365(16) 0.70606(13) 0.76790(10) 0.0324(3) Uani 1 1 d . . . C1S C 0.7424(6) 0.6148(4) 0.8840(4) 0.0217(8) Uani 1 1 d . . . H1S1 H 0.6522 0.6215 0.9382 0.026 Uiso 1 1 calc R . . H1S2 H 0.7298 0.5277 0.8548 0.026 Uiso 1 1 calc R . . Cl2S Cl 0.95465(14) 0.65942(11) 0.95730(10) 0.0253(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0124(2) 0.0095(2) 0.0112(2) 0.00297(18) -0.00016(17) 0.00081(17) C2 0.0116(15) 0.0099(16) 0.0149(16) 0.0061(12) 0.0016(12) 0.0027(12) B3 0.0141(18) 0.012(2) 0.0163(19) 0.0021(15) -0.0025(14) 0.0002(15) C4 0.0209(18) 0.0130(18) 0.0097(15) 0.0011(13) 0.0019(13) 0.0022(14) B5 0.0140(18) 0.017(2) 0.0177(19) 0.0039(16) 0.0022(15) 0.0048(16) B6 0.0145(18) 0.018(2) 0.0164(19) 0.0030(16) -0.0006(14) 0.0035(16) B7 0.0193(19) 0.014(2) 0.0115(17) 0.0035(15) 0.0003(14) 0.0032(16) Co8 0.0112(2) 0.0110(3) 0.0157(2) 0.00563(19) 0.00164(18) 0.00304(18) B9 0.0171(19) 0.014(2) 0.0134(17) 0.0020(15) 0.0007(14) 0.0017(16) B10 0.0141(19) 0.017(2) 0.022(2) 0.0055(17) 0.0045(15) 0.0021(16) C11 0.0196(18) 0.0147(19) 0.0220(18) 0.0103(15) 0.0057(15) 0.0001(15) B11 0.0132(18) 0.016(2) 0.022(2) 0.0039(17) 0.0006(16) 0.0012(16) C12 0.0141(17) 0.0120(18) 0.028(2) 0.0057(15) 0.0003(14) -0.0021(14) B12 0.0125(18) 0.021(2) 0.0171(19) 0.0041(17) -0.0041(15) 0.0006(16) C13 0.027(2) 0.0148(19) 0.0204(18) 0.0056(16) -0.0059(16) -0.0058(16) B13 0.0154(18) 0.0120(19) 0.0159(18) 0.0037(15) 0.0030(14) 0.0029(15) C14 0.034(2) 0.0035(17) 0.0224(19) 0.0061(14) 0.0034(17) 0.0037(16) B14 0.0120(17) 0.014(2) 0.0159(18) 0.0012(15) 0.0027(14) 0.0012(15) C15 0.0249(19) 0.0086(17) 0.0184(17) 0.0068(14) 0.0006(15) 0.0032(15) C81 0.022(2) 0.026(2) 0.030(2) 0.0080(18) 0.0088(16) 0.0126(19) C82 0.029(2) 0.010(2) 0.044(3) 0.0043(18) 0.0012(19) 0.0078(17) C83 0.0165(19) 0.021(2) 0.049(3) 0.023(2) 0.0083(18) 0.0062(17) C84 0.024(2) 0.024(2) 0.026(2) 0.0146(18) 0.0041(16) 0.0135(18) C85 0.0133(17) 0.022(2) 0.032(2) 0.0125(18) -0.0013(15) 0.0067(16) Cl1S 0.0284(5) 0.0364(7) 0.0292(6) 0.0148(5) -0.0040(4) -0.0057(5) C1S 0.025(2) 0.019(2) 0.0191(18) 0.0016(16) 0.0030(15) -0.0027(16) Cl2S 0.0246(5) 0.0248(5) 0.0253(5) 0.0041(4) -0.0007(4) 0.0012(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 C11 2.057(4) . ? Co1 C15 2.061(4) . ? Co1 C14 2.062(4) . ? Co1 C12 2.072(4) . ? Co1 C13 2.084(4) . ? Co1 C4 2.114(4) . ? Co1 B3 2.122(4) . ? Co1 C2 2.136(4) . ? Co1 B7 2.153(5) . ? Co1 B5 2.161(4) . ? Co1 B6 2.175(4) . ? C2 B7 1.677(6) . ? C2 B3 1.691(6) . ? C2 B13 1.691(6) . ? C2 Co8 2.023(4) . ? C2 H2 0.95(5) . ? B3 C4 1.696(6) . ? B3 B9 1.812(6) . ? B3 Co8 2.045(5) . ? B3 H3 1.09(5) . ? C4 B5 1.698(6) . ? C4 B10 1.697(6) . ? C4 B9 1.700(6) . ? C4 H4 0.96(5) . ? B5 B11 1.756(7) . ? B5 B6 1.760(6) . ? B5 B10 1.769(6) . ? B5 H5 1.19(5) . ? B6 B11 1.757(7) . ? B6 B12 1.774(7) . ? B6 B7 1.791(7) . ? B6 H6 1.09(5) . ? B7 B12 1.757(6) . ? B7 B13 1.762(6) . ? B7 H7 1.04(5) . ? Co8 B13 2.003(4) . ? Co8 B9 2.008(5) . ? Co8 C83 2.066(4) . ? Co8 C85 2.068(4) . ? Co8 C84 2.074(4) . ? Co8 C81 2.077(4) . ? Co8 C82 2.082(5) . ? Co8 B14 2.284(4) . ? B9 B10 1.721(7) . ? B9 B14 1.925(6) . ? B9 H9 1.05(5) . ? B10 B11 1.728(7) . ? B10 B14 1.883(7) . ? B10 H10 1.10(5) . ? C11 C15 1.425(6) . ? C11 C12 1.431(6) . ? C11 H11A 1.0000 . ? B11 B12 1.735(7) . ? B11 B14 1.931(6) . ? B11 H11 1.13(5) . ? C12 C13 1.418(7) . ? C12 H12A 1.0000 . ? B12 B13 1.730(6) . ? B12 B14 1.921(6) . ? B12 H12 0.90(5) . ? C13 C14 1.412(6) . ? C13 H13A 1.0000 . ? B13 B14 1.937(6) . ? B13 H13 1.15(5) . ? C14 C15 1.416(6) . ? C14 H14A 1.0000 . ? B14 H14 1.12(5) . ? C15 H15A 1.0000 . ? C81 C82 1.412(7) . ? C81 C85 1.420(7) . ? C81 H81 1.0000 . ? C82 C83 1.423(7) . ? C82 H82 1.0000 . ? C83 C84 1.419(7) . ? C83 H83 1.0000 . ? C84 C85 1.413(6) . ? C84 H84 1.0000 . ? C85 H85 1.0000 . ? Cl1S C1S 1.768(4) . ? C1S Cl2S 1.762(5) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? 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 C11 Co1 C15 40.50(17) . . ? C11 Co1 C14 67.78(17) . . ? C15 Co1 C14 40.17(16) . . ? C11 Co1 C12 40.56(16) . . ? C15 Co1 C12 67.63(17) . . ? C14 Co1 C12 67.10(18) . . ? C11 Co1 C13 67.82(18) . . ? C15 Co1 C13 67.40(17) . . ? C14 Co1 C13 39.81(17) . . ? C12 Co1 C13 39.91(18) . . ? C11 Co1 C4 163.81(16) . . ? C15 Co1 C4 135.15(17) . . ? C14 Co1 C4 100.53(16) . . ? C12 Co1 C4 125.47(16) . . ? C13 Co1 C4 96.01(16) . . ? C11 Co1 B3 130.30(17) . . ? C15 Co1 B3 161.61(17) . . ? C14 Co1 B3 126.55(16) . . ? C12 Co1 B3 96.25(16) . . ? C13 Co1 B3 94.66(17) . . ? C4 Co1 B3 47.21(17) . . ? C11 Co1 C2 102.61(16) . . ? C15 Co1 C2 139.44(16) . . ? C14 Co1 C2 161.11(16) . . ? C12 Co1 C2 94.87(16) . . ? C13 Co1 C2 122.09(16) . . ? C4 Co1 C2 85.12(15) . . ? B3 Co1 C2 46.80(16) . . ? C11 Co1 B7 90.70(17) . . ? C15 Co1 B7 106.27(16) . . ? C14 Co1 B7 145.43(16) . . ? C12 Co1 B7 113.92(17) . . ? C13 Co1 B7 153.83(18) . . ? C4 Co1 B7 104.69(16) . . ? B3 Co1 B7 88.02(17) . . ? C2 Co1 B7 46.04(15) . . ? C11 Co1 B5 140.27(17) . . ? C15 Co1 B5 101.92(17) . . ? C14 Co1 B5 90.68(18) . . ? C12 Co1 B5 155.83(18) . . ? C13 Co1 B5 116.34(19) . . ? C4 Co1 B5 46.78(16) . . ? B3 Co1 B5 89.42(17) . . ? C2 Co1 B5 105.95(16) . . ? B7 Co1 B5 89.67(18) . . ? C11 Co1 B6 107.24(17) . . ? C15 Co1 B6 89.51(17) . . ? C14 Co1 B6 110.29(18) . . ? C12 Co1 B6 147.48(17) . . ? C13 Co1 B6 150.03(18) . . ? C4 Co1 B6 87.05(16) . . ? B3 Co1 B6 108.76(17) . . ? C2 Co1 B6 87.86(16) . . ? B7 Co1 B6 48.90(18) . . ? B5 Co1 B6 47.89(17) . . ? B7 C2 B3 123.7(3) . . ? B7 C2 B13 63.1(2) . . ? B3 C2 B13 115.1(3) . . ? B7 C2 Co8 124.4(2) . . ? B3 C2 Co8 66.11(19) . . ? B13 C2 Co8 64.56(19) . . ? B7 C2 Co1 67.5(2) . . ? B3 C2 Co1 66.2(2) . . ? B13 C2 Co1 117.3(2) . . ? Co8 C2 Co1 125.90(18) . . ? B7 C2 H2 109(3) . . ? B3 C2 H2 115(3) . . ? B13 C2 H2 121(3) . . ? Co8 C2 H2 112(3) . . ? Co1 C2 H2 110(3) . . ? C2 B3 C4 116.1(3) . . ? C2 B3 B9 109.1(3) . . ? C4 B3 B9 57.9(2) . . ? C2 B3 Co8 64.8(2) . . ? C4 B3 Co8 115.9(3) . . ? B9 B3 Co8 62.4(2) . . ? C2 B3 Co1 67.03(19) . . ? C4 B3 Co1 66.12(19) . . ? B9 B3 Co1 113.9(3) . . ? Co8 B3 Co1 125.5(2) . . ? C2 B3 H3 125(3) . . ? C4 B3 H3 110(3) . . ? B9 B3 H3 120(3) . . ? Co8 B3 H3 118(3) . . ? Co1 B3 H3 110(3) . . ? B3 C4 B5 125.2(3) . . ? B3 C4 B10 116.7(3) . . ? B5 C4 B10 62.8(3) . . ? B3 C4 B9 64.5(3) . . ? B5 C4 B9 117.4(3) . . ? B10 C4 B9 60.9(3) . . ? B3 C4 Co1 66.66(19) . . ? B5 C4 Co1 68.09(19) . . ? B10 C4 Co1 118.1(2) . . ? B9 C4 Co1 119.6(3) . . ? B3 C4 H4 108(3) . . ? B5 C4 H4 119(3) . . ? B10 C4 H4 119(3) . . ? B9 C4 H4 111(3) . . ? Co1 C4 H4 116(3) . . ? C4 B5 B11 107.6(3) . . ? C4 B5 B6 117.3(3) . . ? B11 B5 B6 59.9(3) . . ? C4 B5 B10 58.6(2) . . ? B11 B5 B10 58.7(3) . . ? B6 B5 B10 110.5(3) . . ? C4 B5 Co1 65.13(19) . . ? B11 B5 Co1 112.7(3) . . ? B6 B5 Co1 66.5(2) . . ? B10 B5 Co1 112.5(3) . . ? C4 B5 H5 116(2) . . ? B11 B5 H5 123(3) . . ? B6 B5 H5 121(2) . . ? B10 B5 H5 118(3) . . ? Co1 B5 H5 118(3) . . ? B11 B6 B5 59.9(3) . . ? B11 B6 B12 58.9(3) . . ? B5 B6 B12 109.5(3) . . ? B11 B6 B7 109.5(3) . . ? B5 B6 B7 117.8(3) . . ? B12 B6 B7 59.0(3) . . ? B11 B6 Co1 112.0(3) . . ? B5 B6 Co1 65.6(2) . . ? B12 B6 Co1 110.7(3) . . ? B7 B6 Co1 64.9(2) . . ? B11 B6 H6 119(3) . . ? B5 B6 H6 113(3) . . ? B12 B6 H6 125(3) . . ? B7 B6 H6 122(3) . . ? Co1 B6 H6 118(3) . . ? C2 B7 B12 108.4(3) . . ? C2 B7 B13 58.9(2) . . ? B12 B7 B13 58.9(3) . . ? C2 B7 B6 119.1(3) . . ? B12 B7 B6 60.0(3) . . ? B13 B7 B6 111.2(3) . . ? C2 B7 Co1 66.5(2) . . ? B12 B7 Co1 112.4(3) . . ? B13 B7 Co1 113.3(3) . . ? B6 B7 Co1 66.2(2) . . ? C2 B7 H7 114(3) . . ? B12 B7 H7 124(3) . . ? B13 B7 H7 119(3) . . ? B6 B7 H7 120(3) . . ? Co1 B7 H7 117(3) . . ? B13 Co8 B9 97.17(18) . . ? B13 Co8 C2 49.67(17) . . ? B9 Co8 C2 90.19(17) . . ? B13 Co8 B3 89.66(18) . . ? B9 Co8 B3 53.09(18) . . ? C2 Co8 B3 49.13(17) . . ? B13 Co8 C83 122.6(2) . . ? B9 Co8 C83 104.2(2) . . ? C2 Co8 C83 164.94(19) . . ? B3 Co8 C83 144.7(2) . . ? B13 Co8 C85 140.00(18) . . ? B9 Co8 C85 118.88(19) . . ? C2 Co8 C85 109.65(16) . . ? B3 Co8 C85 98.22(18) . . ? C83 Co8 C85 67.37(18) . . ? B13 Co8 C84 161.9(2) . . ? B9 Co8 C84 93.61(18) . . ? C2 Co8 C84 145.04(17) . . ? B3 Co8 C84 108.41(19) . . ? C83 Co8 C84 40.1(2) . . ? C85 Co8 C84 39.89(17) . . ? B13 Co8 C81 103.84(19) . . ? B9 Co8 C81 158.68(19) . . ? C2 Co8 C81 100.57(17) . . ? B3 Co8 C81 122.64(19) . . ? C83 Co8 C81 67.32(18) . . ? C85 Co8 C81 40.08(19) . . ? C84 Co8 C81 67.09(18) . . ? B13 Co8 C82 95.9(2) . . ? B9 Co8 C82 141.94(19) . . ? C2 Co8 C82 124.80(18) . . ? B3 Co8 C82 162.30(19) . . ? C83 Co8 C82 40.1(2) . . ? C85 Co8 C82 66.99(19) . . ? C84 Co8 C82 67.0(2) . . ? C81 Co8 C82 39.68(19) . . ? B13 Co8 B14 53.24(16) . . ? B9 Co8 B14 52.83(17) . . ? C2 Co8 B14 82.83(15) . . ? B3 Co8 B14 85.02(17) . . ? C83 Co8 B14 102.24(17) . . ? C85 Co8 B14 165.97(17) . . ? C84 Co8 B14 126.14(17) . . ? C81 Co8 B14 146.31(19) . . ? C82 Co8 B14 111.72(18) . . ? C4 B9 B10 59.5(3) . . ? C4 B9 B3 57.7(2) . . ? B10 B9 B3 109.7(3) . . ? C4 B9 B14 100.9(3) . . ? B10 B9 B14 61.9(3) . . ? B3 B9 B14 103.3(3) . . ? C4 B9 Co8 117.7(3) . . ? B10 B9 Co8 129.8(3) . . ? B3 B9 Co8 64.5(2) . . ? B14 B9 Co8 71.0(2) . . ? C4 B9 H9 118(3) . . ? B10 B9 H9 113(3) . . ? B3 B9 H9 122(3) . . ? B14 B9 H9 131(3) . . ? Co8 B9 H9 110(3) . . ? C4 B10 B9 59.6(3) . . ? C4 B10 B11 108.9(3) . . ? B9 B10 B11 122.2(4) . . ? C4 B10 B5 58.6(2) . . ? B9 B10 B5 112.6(3) . . ? B11 B10 B5 60.3(3) . . ? C4 B10 B14 102.7(3) . . ? B9 B10 B14 64.4(3) . . ? B11 B10 B14 64.5(3) . . ? B5 B10 B14 106.4(3) . . ? C4 B10 H10 122(3) . . ? B9 B10 H10 113(3) . . ? B11 B10 H10 118(3) . . ? B5 B10 H10 121(3) . . ? B14 B10 H10 127(3) . . ? C15 C11 C12 107.2(4) . . ? C15 C11 Co1 69.9(2) . . ? C12 C11 Co1 70.3(2) . . ? C15 C11 H11A 126.4 . . ? C12 C11 H11A 126.4 . . ? Co1 C11 H11A 126.4 . . ? B10 B11 B12 118.1(3) . . ? B10 B11 B5 61.0(3) . . ? B12 B11 B5 111.5(3) . . ? B10 B11 B6 112.6(3) . . ? B12 B11 B6 61.1(3) . . ? B5 B11 B6 60.1(3) . . ? B10 B11 B14 61.6(3) . . ? B12 B11 B14 62.9(3) . . ? B5 B11 B14 104.9(3) . . ? B6 B11 B14 106.5(3) . . ? B10 B11 H11 118(3) . . ? B12 B11 H11 119(3) . . ? B5 B11 H11 116(3) . . ? B6 B11 H11 115(3) . . ? B14 B11 H11 132(3) . . ? C13 C12 C11 108.3(4) . . ? C13 C12 Co1 70.5(2) . . ? C11 C12 Co1 69.2(2) . . ? C13 C12 H12A 125.8 . . ? C11 C12 H12A 125.8 . . ? Co1 C12 H12A 125.8 . . ? B13 B12 B11 120.9(3) . . ? B13 B12 B7 60.7(3) . . ? B11 B12 B7 112.2(3) . . ? B13 B12 B6 113.6(3) . . ? B11 B12 B6 60.1(3) . . ? B7 B12 B6 61.0(3) . . ? B13 B12 B14 63.8(2) . . ? B11 B12 B14 63.5(3) . . ? B7 B12 B14 106.0(3) . . ? B6 B12 B14 106.2(3) . . ? B13 B12 H12 118(3) . . ? B11 B12 H12 113(3) . . ? B7 B12 H12 122(3) . . ? B6 B12 H12 118(4) . . ? B14 B12 H12 126(4) . . ? C14 C13 C12 107.6(4) . . ? C14 C13 Co1 69.2(2) . . ? C12 C13 Co1 69.6(2) . . ? C14 C13 H13A 126.2 . . ? C12 C13 H13A 126.2 . . ? Co1 C13 H13A 126.2 . . ? C2 B13 B12 109.0(3) . . ? C2 B13 B7 58.1(2) . . ? B12 B13 B7 60.4(3) . . ? C2 B13 B14 103.6(3) . . ? B12 B13 B14 62.9(2) . . ? B7 B13 B14 105.1(3) . . ? C2 B13 Co8 65.77(19) . . ? B12 B13 Co8 130.7(3) . . ? B7 B13 Co8 120.9(3) . . ? B14 B13 Co8 70.82(19) . . ? C2 B13 H13 123(3) . . ? B12 B13 H13 115(3) . . ? B7 B13 H13 118(3) . . ? B14 B13 H13 128(3) . . ? Co8 B13 H13 106(3) . . ? C13 C14 C15 108.9(4) . . ? C13 C14 Co1 71.0(2) . . ? C15 C14 Co1 69.9(2) . . ? C13 C14 H14A 125.6 . . ? C15 C14 H14A 125.6 . . ? Co1 C14 H14A 125.6 . . ? B10 B14 B12 102.7(3) . . ? B10 B14 B9 53.7(2) . . ? B12 B14 B9 128.4(3) . . ? B10 B14 B11 53.9(2) . . ? B12 B14 B11 53.5(2) . . ? B9 B14 B11 103.1(3) . . ? B10 B14 B13 128.4(3) . . ? B12 B14 B13 53.3(2) . . ? B9 B14 B13 102.3(3) . . ? B11 B14 B13 102.4(3) . . ? B10 B14 Co8 108.0(2) . . ? B12 B14 Co8 107.4(2) . . ? B9 B14 Co8 56.21(18) . . ? B11 B14 Co8 137.7(3) . . ? B13 B14 Co8 55.94(17) . . ? B10 B14 H14 117(3) . . ? B12 B14 H14 112(3) . . ? B9 B14 H14 120(3) . . ? B11 B14 H14 112(3) . . ? B13 B14 H14 114(3) . . ? Co8 B14 H14 110(3) . . ? C14 C15 C11 107.9(4) . . ? C14 C15 Co1 70.0(2) . . ? C11 C15 Co1 69.6(2) . . ? C14 C15 H15A 126.1 . . ? C11 C15 H15A 126.1 . . ? Co1 C15 H15A 126.1 . . ? C82 C81 C85 107.9(4) . . ? C82 C81 Co8 70.4(3) . . ? C85 C81 Co8 69.6(3) . . ? C82 C81 H81 126.0 . . ? C85 C81 H81 126.0 . . ? Co8 C81 H81 126.0 . . ? C81 C82 C83 108.1(4) . . ? C81 C82 Co8 69.9(3) . . ? C83 C82 Co8 69.3(3) . . ? C81 C82 H82 125.9 . . ? C83 C82 H82 125.9 . . ? Co8 C82 H82 125.9 . . ? C84 C83 C82 107.7(4) . . ? C84 C83 Co8 70.3(2) . . ? C82 C83 Co8 70.6(3) . . ? C84 C83 H83 126.2 . . ? C82 C83 H83 126.2 . . ? Co8 C83 H83 126.2 . . ? C85 C84 C83 108.1(4) . . ? C85 C84 Co8 69.8(2) . . ? C83 C84 Co8 69.6(3) . . ? C85 C84 H84 125.9 . . ? C83 C84 H84 125.9 . . ? Co8 C84 H84 125.9 . . ? C84 C85 C81 108.1(4) . . ? C84 C85 Co8 70.3(2) . . ? C81 C85 Co8 70.3(2) . . ? C84 C85 H85 125.9 . . ? C81 C85 H85 125.9 . . ? Co8 C85 H85 125.9 . . ? Cl2S C1S Cl1S 112.1(2) . . ? Cl2S C1S H1S1 109.2 . . ? Cl1S C1S H1S1 109.2 . . ? Cl2S C1S H1S2 109.2 . . ? Cl1S C1S H1S2 109.2 . . ? H1S1 C1S H1S2 107.9 . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.211 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.210 _database_code_depnum_ccdc_archive 'CCDC 939755' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3432 _audit_update_record ; 2013-05-10 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 B10 Co2' _chemical_formula_weight 392.26 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.7083(6) _cell_length_b 11.3413(9) _cell_length_c 9.9968(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.900(4) _cell_angle_gamma 90.00 _cell_volume 821.76(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6120 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 29.86 _exptl_crystal_description PLATE _exptl_crystal_colour purple _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 2.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3893 _exptl_absorpt_correction_T_max 0.9241 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16215 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 30.98 _reflns_number_total 4694 _reflns_number_gt 3857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0548P)^2^+0.7114P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(3) _refine_ls_number_reflns 4694 _refine_ls_number_parameters 254 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.29503(5) 0.37409(4) -0.03980(4) 0.01224(11) Uani 1 1 d . . . C2 C 0.4884(8) 0.3109(5) 0.1541(5) 0.0170(10) Uani 1 1 d . . . H2 H 0.603(6) 0.284(4) 0.144(5) 0.020 Uiso 1 1 d . . . B3 B 0.2976(9) 0.2241(4) 0.0882(6) 0.0234(12) Uani 1 1 d . . . H3 H 0.318(6) 0.135(4) 0.043(5) 0.028 Uiso 1 1 d . . . C4 C 0.0902(7) 0.2925(5) 0.0296(6) 0.0335(13) Uani 1 1 d . . . H4 H -0.004(7) 0.230(5) -0.028(6) 0.040 Uiso 1 1 d . . . B5 B 0.0658(8) 0.4400(6) 0.0135(7) 0.0294(13) Uani 1 1 d . . . H5 H -0.066(7) 0.474(5) -0.079(5) 0.035 Uiso 1 1 d . . . B6 B 0.2640(9) 0.5265(4) 0.0752(6) 0.0227(11) Uani 1 1 d . . . H6 H 0.252(6) 0.616(4) 0.035(5) 0.027 Uiso 1 1 d . . . B7 B 0.4822(9) 0.4578(6) 0.1479(7) 0.0193(12) Uani 1 1 d . . . H7 H 0.581(7) 0.506(4) 0.122(5) 0.023 Uiso 1 1 d . . . B8 B 0.3994(9) 0.2492(5) 0.2731(7) 0.0278(13) Uani 1 1 d . . . H8 H 0.464(7) 0.175(4) 0.331(5) 0.033 Uiso 1 1 d . . . B9 B 0.1622(9) 0.2392(5) 0.1991(6) 0.0271(12) Uani 1 1 d . . . H9 H 0.107(7) 0.156(4) 0.219(5) 0.033 Uiso 1 1 d . . . B10 B 0.0252(5) 0.3633(7) 0.1532(4) 0.0315(12) Uani 1 1 d . . . H10 H -0.124(6) 0.341(4) 0.156(4) 0.038 Uiso 1 1 d . . . B11 B 0.1274(9) 0.4982(5) 0.1836(7) 0.0289(13) Uani 1 1 d . . . H11 H 0.051(7) 0.561(4) 0.210(5) 0.035 Uiso 1 1 d . . . B12 B 0.3661(8) 0.5124(5) 0.2618(7) 0.0245(12) Uani 1 1 d . . . H12 H 0.389(6) 0.596(4) 0.311(5) 0.029 Uiso 1 1 d . . . Co13 Co 0.55663(6) 0.38898(7) 0.34922(5) 0.02425(17) Uani 1 1 d . . . B14 B 0.2499(5) 0.3759(6) 0.3100(4) 0.0179(7) Uani 1 1 d . . . H14 H 0.230(5) 0.362(4) 0.413(4) 0.021 Uiso 1 1 d . . . C101 C 0.4761(5) 0.3868(6) -0.1501(4) 0.0371(13) Uani 1 1 d . . . H101 H 0.6128 0.3970 -0.1073 0.044 Uiso 1 1 calc R . . C102 C 0.3460(9) 0.4775(4) -0.1907(6) 0.0332(13) Uani 1 1 d . . . H102 H 0.3734 0.5639 -0.1822 0.040 Uiso 1 1 calc R . . C103 C 0.1751(8) 0.4278(5) -0.2459(6) 0.0278(12) Uani 1 1 d . . . H103 H 0.0567 0.4727 -0.2837 0.033 Uiso 1 1 calc R . . C104 C 0.1901(10) 0.3041(5) -0.2415(7) 0.0357(16) Uani 1 1 d . . . H104 H 0.0872 0.2459 -0.2768 0.043 Uiso 1 1 calc R . . C105 C 0.3814(9) 0.2787(5) -0.1821(6) 0.0379(14) Uani 1 1 d . . . H105 H 0.4386 0.1985 -0.1658 0.045 Uiso 1 1 calc R . . C131 C 0.8317(6) 0.4443(5) 0.4261(6) 0.0355(14) Uani 1 1 d . . . H131 H 0.8983 0.4750 0.3632 0.043 Uiso 1 1 calc R . . C132 C 0.7307(6) 0.5162(5) 0.4861(4) 0.0324(10) Uani 1 1 d . . . H132 H 0.7179 0.6039 0.4782 0.039 Uiso 1 1 calc R . . C133 C 0.6555(9) 0.4417(6) 0.5614(7) 0.0363(15) Uani 1 1 d . . . H133 H 0.5757 0.4682 0.6164 0.044 Uiso 1 1 calc R . . C134 C 0.7012(10) 0.3245(7) 0.5473(7) 0.043(2) Uani 1 1 d . . . H134 H 0.6693 0.2541 0.5946 0.052 Uiso 1 1 calc R . . C135 C 0.8194(7) 0.3266(6) 0.4530(6) 0.0437(15) Uani 1 1 d . . . H135 H 0.8835 0.2591 0.4254 0.052 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 0.01048(18) 0.0150(2) 0.01128(19) -0.0002(3) 0.00370(14) 0.0000(2) C2 0.013(2) 0.030(2) 0.010(2) 0.0044(17) 0.0057(17) 0.0082(18) B3 0.044(3) 0.011(2) 0.021(3) -0.0005(19) 0.019(2) -0.001(2) C4 0.026(3) 0.050(3) 0.031(3) -0.015(2) 0.019(2) -0.024(2) B5 0.029(3) 0.046(3) 0.019(3) 0.015(2) 0.015(2) 0.020(2) B6 0.038(3) 0.012(2) 0.025(3) -0.002(2) 0.020(2) 0.003(2) B7 0.015(3) 0.024(3) 0.022(3) -0.009(2) 0.010(2) -0.005(2) B8 0.043(3) 0.025(3) 0.024(3) 0.006(2) 0.023(3) 0.015(2) B9 0.042(3) 0.025(3) 0.021(3) -0.003(2) 0.021(2) -0.016(2) B10 0.0144(17) 0.062(4) 0.0217(19) 0.005(3) 0.0110(15) 0.003(3) B11 0.040(3) 0.025(3) 0.029(3) 0.009(2) 0.021(3) 0.017(2) B12 0.037(3) 0.018(2) 0.022(3) -0.009(2) 0.015(2) -0.008(2) Co13 0.0110(2) 0.0503(4) 0.0111(2) -0.0013(3) 0.00333(16) -0.0003(3) B14 0.0177(16) 0.0207(17) 0.0174(16) -0.002(3) 0.0086(13) 0.003(2) C101 0.0187(16) 0.084(4) 0.0115(16) -0.004(3) 0.0085(13) -0.006(3) C102 0.065(4) 0.021(2) 0.023(3) -0.0080(19) 0.027(3) -0.018(2) C103 0.021(2) 0.047(3) 0.014(2) 0.007(2) 0.0031(18) 0.019(2) C104 0.057(4) 0.039(3) 0.016(3) -0.011(2) 0.018(3) -0.026(3) C105 0.065(4) 0.037(3) 0.021(3) 0.009(2) 0.028(3) 0.029(3) C131 0.010(2) 0.059(4) 0.029(3) -0.016(2) -0.0046(19) -0.001(2) C132 0.022(2) 0.055(3) 0.017(2) -0.009(2) 0.0015(17) -0.009(2) C133 0.034(3) 0.053(4) 0.016(2) -0.002(2) 0.000(2) -0.012(3) C134 0.056(4) 0.042(3) 0.013(3) 0.009(2) -0.014(3) -0.011(3) C135 0.021(3) 0.058(4) 0.040(3) 0.008(3) -0.006(2) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C103 2.044(6) . ? Co1 C102 2.052(5) . ? Co1 C101 2.057(3) . ? Co1 C104 2.059(6) . ? Co1 C105 2.069(5) . ? Co1 B3 2.125(5) . ? Co1 C2 2.127(5) . ? Co1 B6 2.134(5) . ? Co1 C4 2.139(5) . ? Co1 B5 2.146(5) . ? Co1 B7 2.159(6) . ? C2 B7 1.668(6) . ? C2 B3 1.705(8) . ? C2 B8 1.712(8) . ? C2 Co13 2.042(5) . ? C2 H2 0.97(5) . ? B3 C4 1.692(9) . ? B3 B8 1.768(9) . ? B3 B9 1.771(8) . ? B3 H3 1.14(5) . ? C4 B5 1.685(7) . ? C4 B10 1.686(7) . ? C4 B9 1.704(9) . ? C4 H4 1.04(5) . ? B5 B11 1.733(9) . ? B5 B6 1.742(9) . ? B5 B10 1.760(8) . ? B5 H5 1.18(5) . ? B6 B12 1.767(9) . ? B6 B7 1.769(9) . ? B6 B11 1.779(8) . ? B6 H6 1.09(5) . ? B7 B12 1.782(9) . ? B7 Co13 2.051(7) . ? B7 H7 1.04(5) . ? B8 B9 1.727(9) . ? B8 B14 1.954(7) . ? B8 Co13 1.983(7) . ? B8 H8 1.04(5) . ? B9 B10 1.726(9) . ? B9 B14 1.892(8) . ? B9 H9 1.08(5) . ? B10 B11 1.699(10) . ? B10 B14 1.905(5) . ? B10 H10 1.18(5) . ? B11 B12 1.744(9) . ? B11 B14 1.897(8) . ? B11 H11 1.01(5) . ? B12 B14 1.930(8) . ? B12 Co13 2.002(6) . ? B12 H12 1.06(5) . ? Co13 C134 2.048(6) . ? Co13 C135 2.061(5) . ? Co13 C133 2.083(6) . ? Co13 C131 2.090(5) . ? Co13 C132 2.122(5) . ? Co13 B14 2.266(3) . ? B14 H14 1.10(4) . ? C101 C102 1.397(8) . ? C101 C105 1.407(9) . ? C101 H101 1.0000 . ? C102 C103 1.365(8) . ? C102 H102 1.0000 . ? C103 C104 1.407(7) . ? C103 H103 1.0000 . ? C104 C105 1.419(9) . ? C104 H104 1.0000 . ? C105 H105 1.0000 . ? C131 C135 1.372(8) . ? C131 C132 1.396(7) . ? C131 H131 1.0000 . ? C132 C133 1.383(8) . ? C132 H132 1.0000 . ? C133 C134 1.395(9) . ? C133 H133 1.0000 . ? C134 C135 1.518(10) . ? C134 H134 1.0000 . ? C135 H135 1.0000 . ? 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 C103 Co1 C102 38.9(2) . . ? C103 Co1 C101 66.1(2) . . ? C102 Co1 C101 39.8(2) . . ? C103 Co1 C104 40.1(2) . . ? C102 Co1 C104 67.0(2) . . ? C101 Co1 C104 67.3(2) . . ? C103 Co1 C105 66.7(2) . . ? C102 Co1 C105 66.83(16) . . ? C101 Co1 C105 39.9(2) . . ? C104 Co1 C105 40.2(3) . . ? C103 Co1 B3 139.0(2) . . ? C102 Co1 B3 159.3(2) . . ? C101 Co1 B3 120.7(2) . . ? C104 Co1 B3 101.6(2) . . ? C105 Co1 B3 93.2(2) . . ? C103 Co1 C2 162.8(2) . . ? C102 Co1 C2 127.8(2) . . ? C101 Co1 C2 96.84(19) . . ? C104 Co1 C2 133.0(3) . . ? C105 Co1 C2 99.2(2) . . ? B3 Co1 C2 47.3(2) . . ? C103 Co1 B6 101.9(2) . . ? C102 Co1 B6 91.0(2) . . ? C101 Co1 B6 116.9(2) . . ? C104 Co1 B6 139.6(3) . . ? C105 Co1 B6 156.2(2) . . ? B3 Co1 B6 107.70(15) . . ? C2 Co1 B6 87.4(2) . . ? C103 Co1 C4 109.0(2) . . ? C102 Co1 C4 146.4(2) . . ? C101 Co1 C4 156.1(2) . . ? C104 Co1 C4 93.7(2) . . ? C105 Co1 C4 116.3(2) . . ? B3 Co1 C4 46.8(2) . . ? C2 Co1 C4 85.7(2) . . ? B6 Co1 C4 86.9(2) . . ? C103 Co1 B5 91.1(2) . . ? C102 Co1 B5 111.3(2) . . ? C101 Co1 B5 151.0(2) . . ? C104 Co1 B5 107.2(3) . . ? C105 Co1 B5 146.9(3) . . ? B3 Co1 B5 88.2(2) . . ? C2 Co1 B5 105.8(2) . . ? B6 Co1 B5 48.0(3) . . ? C4 Co1 B5 46.31(19) . . ? C103 Co1 B7 133.2(3) . . ? C102 Co1 B7 98.6(2) . . ? C101 Co1 B7 93.4(2) . . ? C104 Co1 B7 160.7(2) . . ? C105 Co1 B7 123.4(3) . . ? B3 Co1 B7 87.9(2) . . ? C2 Co1 B7 45.80(17) . . ? B6 Co1 B7 48.7(2) . . ? C4 Co1 B7 104.9(2) . . ? B5 Co1 B7 89.7(3) . . ? B7 C2 B3 123.5(5) . . ? B7 C2 B8 114.9(5) . . ? B3 C2 B8 62.3(3) . . ? B7 C2 Co13 66.2(3) . . ? B3 C2 Co13 121.8(3) . . ? B8 C2 Co13 63.1(3) . . ? B7 C2 Co1 68.1(3) . . ? B3 C2 Co1 66.3(3) . . ? B8 C2 Co1 116.6(4) . . ? Co13 C2 Co1 126.7(3) . . ? B7 C2 H2 109(3) . . ? B3 C2 H2 118(3) . . ? B8 C2 H2 123(3) . . ? Co13 C2 H2 107(3) . . ? Co1 C2 H2 113(3) . . ? C4 B3 C2 117.3(4) . . ? C4 B3 B8 108.6(4) . . ? C2 B3 B8 59.0(3) . . ? C4 B3 B9 58.9(3) . . ? C2 B3 B9 108.5(4) . . ? B8 B3 B9 58.4(3) . . ? C4 B3 Co1 67.1(3) . . ? C2 B3 Co1 66.4(2) . . ? B8 B3 Co1 114.2(3) . . ? B9 B3 Co1 114.4(3) . . ? C4 B3 H3 121(2) . . ? C2 B3 H3 117(2) . . ? B8 B3 H3 119(3) . . ? B9 B3 H3 122(2) . . ? Co1 B3 H3 116(3) . . ? B5 C4 B10 63.0(4) . . ? B5 C4 B3 123.4(4) . . ? B10 C4 B3 116.5(4) . . ? B5 C4 B9 115.8(5) . . ? B10 C4 B9 61.2(4) . . ? B3 C4 B9 62.9(4) . . ? B5 C4 Co1 67.1(3) . . ? B10 C4 Co1 117.9(3) . . ? B3 C4 Co1 66.2(2) . . ? B9 C4 Co1 116.7(3) . . ? B5 C4 H4 126(3) . . ? B10 C4 H4 114(3) . . ? B3 C4 H4 106(3) . . ? B9 C4 H4 104(3) . . ? Co1 C4 H4 125(3) . . ? C4 B5 B11 107.5(5) . . ? C4 B5 B6 118.0(5) . . ? B11 B5 B6 61.6(4) . . ? C4 B5 B10 58.6(4) . . ? B11 B5 B10 58.2(4) . . ? B6 B5 B10 111.6(4) . . ? C4 B5 Co1 66.6(3) . . ? B11 B5 Co1 113.7(4) . . ? B6 B5 Co1 65.6(3) . . ? B10 B5 Co1 114.1(3) . . ? C4 B5 H5 116(3) . . ? B11 B5 H5 121(3) . . ? B6 B5 H5 120(3) . . ? B10 B5 H5 117(3) . . ? Co1 B5 H5 119(2) . . ? B5 B6 B12 110.1(4) . . ? B5 B6 B7 119.6(4) . . ? B12 B6 B7 60.5(4) . . ? B5 B6 B11 59.0(3) . . ? B12 B6 B11 58.9(3) . . ? B7 B6 B11 110.3(4) . . ? B5 B6 Co1 66.3(3) . . ? B12 B6 Co1 113.8(3) . . ? B7 B6 Co1 66.4(3) . . ? B11 B6 Co1 112.3(3) . . ? B5 B6 H6 116(2) . . ? B12 B6 H6 115(3) . . ? B7 B6 H6 121(2) . . ? B11 B6 H6 114(2) . . ? Co1 B6 H6 125(3) . . ? C2 B7 B6 117.8(5) . . ? C2 B7 B12 109.7(5) . . ? B6 B7 B12 59.7(3) . . ? C2 B7 Co13 65.7(4) . . ? B6 B7 Co13 118.7(4) . . ? B12 B7 Co13 62.5(3) . . ? C2 B7 Co1 66.1(3) . . ? B6 B7 Co1 64.9(3) . . ? B12 B7 Co1 112.1(4) . . ? Co13 B7 Co1 124.5(3) . . ? C2 B7 H7 122(3) . . ? B6 B7 H7 110(2) . . ? B12 B7 H7 123(3) . . ? Co13 B7 H7 118(3) . . ? Co1 B7 H7 110(3) . . ? C2 B8 B9 110.2(4) . . ? C2 B8 B3 58.6(3) . . ? B9 B8 B3 60.9(4) . . ? C2 B8 B14 103.4(4) . . ? B9 B8 B14 61.5(3) . . ? B3 B8 B14 103.6(4) . . ? C2 B8 Co13 66.6(3) . . ? B9 B8 Co13 129.5(4) . . ? B3 B8 Co13 121.7(4) . . ? B14 B8 Co13 70.3(2) . . ? C2 B8 H8 119(3) . . ? B9 B8 H8 115(3) . . ? B3 B8 H8 114(3) . . ? B14 B8 H8 134(3) . . ? Co13 B8 H8 108(3) . . ? C4 B9 B10 58.9(3) . . ? C4 B9 B8 110.0(4) . . ? B10 B9 B8 121.5(4) . . ? C4 B9 B3 58.2(3) . . ? B10 B9 B3 110.5(4) . . ? B8 B9 B3 60.7(3) . . ? C4 B9 B14 102.8(4) . . ? B10 B9 B14 63.3(3) . . ? B8 B9 B14 65.2(3) . . ? B3 B9 B14 106.1(3) . . ? C4 B9 H9 118(3) . . ? B10 B9 H9 121(3) . . ? B8 B9 H9 114(3) . . ? B3 B9 H9 112(3) . . ? B14 B9 H9 134(3) . . ? C4 B10 B11 109.0(4) . . ? C4 B10 B9 59.9(4) . . ? B11 B10 B9 118.8(3) . . ? C4 B10 B5 58.5(3) . . ? B11 B10 B5 60.1(4) . . ? B9 B10 B5 110.9(4) . . ? C4 B10 B14 103.0(3) . . ? B11 B10 B14 63.2(3) . . ? B9 B10 B14 62.6(3) . . ? B5 B10 B14 105.0(4) . . ? C4 B10 H10 117(2) . . ? B11 B10 H10 125(2) . . ? B9 B10 H10 109(2) . . ? B5 B10 H10 124(2) . . ? B14 B10 H10 128(2) . . ? B10 B11 B5 61.7(3) . . ? B10 B11 B12 121.2(4) . . ? B5 B11 B12 111.7(4) . . ? B10 B11 B6 112.8(4) . . ? B5 B11 B6 59.5(3) . . ? B12 B11 B6 60.2(4) . . ? B10 B11 B14 63.7(3) . . ? B5 B11 B14 106.4(4) . . ? B12 B11 B14 63.9(3) . . ? B6 B11 B14 105.9(4) . . ? B10 B11 H11 114(3) . . ? B5 B11 H11 122(3) . . ? B12 B11 H11 116(3) . . ? B6 B11 H11 123(3) . . ? B14 B11 H11 123(3) . . ? B11 B12 B6 60.9(4) . . ? B11 B12 B7 111.4(4) . . ? B6 B12 B7 59.8(3) . . ? B11 B12 B14 61.9(3) . . ? B6 B12 B14 105.0(3) . . ? B7 B12 B14 104.9(4) . . ? B11 B12 Co13 129.5(3) . . ? B6 B12 Co13 121.4(3) . . ? B7 B12 Co13 65.3(3) . . ? B14 B12 Co13 70.4(2) . . ? B11 B12 H12 106(2) . . ? B6 B12 H12 111(3) . . ? B7 B12 H12 125(3) . . ? B14 B12 H12 128(3) . . ? Co13 B12 H12 116(3) . . ? B8 Co13 B12 97.45(18) . . ? B8 Co13 C2 50.3(2) . . ? B12 Co13 C2 88.5(2) . . ? B8 Co13 C134 98.4(3) . . ? B12 Co13 C134 138.5(3) . . ? C2 Co13 C134 130.3(3) . . ? B8 Co13 B7 89.9(2) . . ? B12 Co13 B7 52.2(2) . . ? C2 Co13 B7 48.11(17) . . ? C134 Co13 B7 164.4(3) . . ? B8 Co13 C135 106.6(3) . . ? B12 Co13 C135 155.4(2) . . ? C2 Co13 C135 102.8(2) . . ? C134 Co13 C135 43.3(3) . . ? B7 Co13 C135 121.6(2) . . ? B8 Co13 C133 125.8(2) . . ? B12 Co13 C133 101.8(3) . . ? C2 Co13 C133 169.6(3) . . ? C134 Co13 C133 39.5(2) . . ? B7 Co13 C133 140.7(3) . . ? C135 Co13 C133 68.3(3) . . ? B8 Co13 C131 142.4(2) . . ? B12 Co13 C131 116.9(2) . . ? C2 Co13 C131 112.4(2) . . ? C134 Co13 C131 66.5(3) . . ? B7 Co13 C131 99.0(3) . . ? C135 Co13 C131 38.6(2) . . ? C133 Co13 C131 64.3(2) . . ? B8 Co13 C132 163.8(2) . . ? B12 Co13 C132 90.9(2) . . ? C2 Co13 C132 144.3(2) . . ? C134 Co13 C132 66.6(3) . . ? B7 Co13 C132 106.2(2) . . ? C135 Co13 C132 67.1(2) . . ? C133 Co13 C132 38.4(2) . . ? C131 Co13 C132 38.70(19) . . ? B8 Co13 B14 54.3(2) . . ? B12 Co13 B14 53.3(2) . . ? C2 Co13 B14 83.81(18) . . ? C134 Co13 B14 109.6(2) . . ? B7 Co13 B14 85.9(2) . . ? C135 Co13 B14 148.6(2) . . ? C133 Co13 B14 101.2(2) . . ? C131 Co13 B14 162.0(2) . . ? C132 Co13 B14 123.33(18) . . ? B9 B14 B11 102.2(3) . . ? B9 B14 B10 54.1(3) . . ? B11 B14 B10 53.1(3) . . ? B9 B14 B12 127.9(3) . . ? B11 B14 B12 54.2(3) . . ? B10 B14 B12 102.9(3) . . ? B9 B14 B8 53.3(3) . . ? B11 B14 B8 127.1(3) . . ? B10 B14 B8 102.6(4) . . ? B12 B14 B8 100.9(3) . . ? B9 B14 Co13 107.4(3) . . ? B11 B14 Co13 108.7(3) . . ? B10 B14 Co13 138.6(2) . . ? B12 B14 Co13 56.3(2) . . ? B8 B14 Co13 55.5(2) . . ? B9 B14 H14 107(3) . . ? B11 B14 H14 122(2) . . ? B10 B14 H14 112.4(18) . . ? B12 B14 H14 125(3) . . ? B8 B14 H14 110(2) . . ? Co13 B14 H14 108.5(18) . . ? C102 C101 C105 108.1(3) . . ? C102 C101 Co1 69.9(3) . . ? C105 C101 Co1 70.5(3) . . ? C102 C101 H101 126.0 . . ? C105 C101 H101 126.0 . . ? Co1 C101 H101 126.0 . . ? C103 C102 C101 108.2(4) . . ? C103 C102 Co1 70.2(3) . . ? C101 C102 Co1 70.3(3) . . ? C103 C102 H102 125.9 . . ? C101 C102 H102 125.9 . . ? Co1 C102 H102 125.9 . . ? C102 C103 C104 109.9(6) . . ? C102 C103 Co1 70.9(3) . . ? C104 C103 Co1 70.5(4) . . ? C102 C103 H103 125.0 . . ? C104 C103 H103 125.0 . . ? Co1 C103 H103 125.0 . . ? C103 C104 C105 106.2(6) . . ? C103 C104 Co1 69.4(4) . . ? C105 C104 Co1 70.3(3) . . ? C103 C104 H104 126.9 . . ? C105 C104 H104 126.9 . . ? Co1 C104 H104 126.9 . . ? C101 C105 C104 107.6(4) . . ? C101 C105 Co1 69.6(3) . . ? C104 C105 Co1 69.5(3) . . ? C101 C105 H105 126.2 . . ? C104 C105 H105 126.2 . . ? Co1 C105 H105 126.2 . . ? C135 C131 C132 113.5(6) . . ? C135 C131 Co13 69.6(4) . . ? C132 C131 Co13 71.9(3) . . ? C135 C131 H131 123.2 . . ? C132 C131 H131 123.2 . . ? Co13 C131 H131 123.2 . . ? C133 C132 C131 106.0(5) . . ? C133 C132 Co13 69.3(3) . . ? C131 C132 Co13 69.4(3) . . ? C133 C132 H132 127.0 . . ? C131 C132 H132 127.0 . . ? Co13 C132 H132 127.0 . . ? C132 C133 C134 111.1(6) . . ? C132 C133 Co13 72.3(3) . . ? C134 C133 Co13 68.9(4) . . ? C132 C133 H133 124.4 . . ? C134 C133 H133 124.4 . . ? Co13 C133 H133 124.4 . . ? C133 C134 C135 105.9(6) . . ? C133 C134 Co13 71.6(4) . . ? C135 C134 Co13 68.8(3) . . ? C133 C134 H134 127.0 . . ? C135 C134 H134 127.0 . . ? Co13 C134 H134 127.0 . . ? C131 C135 C134 103.5(5) . . ? C131 C135 Co13 71.9(3) . . ? C134 C135 Co13 67.9(3) . . ? C131 C135 H135 128.1 . . ? C134 C135 H135 128.1 . . ? Co13 C135 H135 128.1 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.122 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 939756' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4958 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H22 B10 Co2' _chemical_formula_sum 'C12 H22 B10 Co2' _chemical_formula_weight 392.26 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' Co Co 0.3494 0.9721 '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 14.8157(18) _cell_length_b 13.3179(18) _cell_length_c 16.818(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3318.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9830 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 34.93 _exptl_crystal_description block _exptl_crystal_colour Red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4307 _exptl_absorpt_correction_T_max 0.6472 _exptl_absorpt_process_details 'SADABS (Bruker, 2010)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 98827 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 35.17 _reflns_number_total 7274 _reflns_number_gt 6076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0377P)^2^+3.2709P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7274 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.085803(11) 0.057783(13) 0.318709(10) 0.01054(4) Uani 1 1 d . . . C2 C 0.21207(8) 0.04211(10) 0.37927(8) 0.0129(2) Uani 1 1 d . . . H2 H 0.2325(13) -0.0283(15) 0.3826(12) 0.016 Uiso 1 1 d . . . B3 B 0.12701(11) 0.07004(12) 0.44133(9) 0.0151(3) Uani 1 1 d . . . H3 H 0.0988(14) 0.0094(16) 0.4800(12) 0.018 Uiso 1 1 d . . . B4 B 0.04754(10) 0.16335(13) 0.40742(11) 0.0192(3) Uani 1 1 d . . . H4 H -0.0194(14) 0.1597(16) 0.4287(13) 0.023 Uiso 1 1 d . . . C5 C 0.06647(10) 0.21642(11) 0.31688(10) 0.0216(3) Uani 1 1 d . . . H5 H 0.0055(15) 0.2430(16) 0.2958(14) 0.026 Uiso 1 1 d . . . B6 B 0.14466(12) 0.17894(14) 0.25219(11) 0.0207(3) Uani 1 1 d . . . H6 H 0.1274(15) 0.1891(17) 0.1885(13) 0.025 Uiso 1 1 d . . . B7 B 0.22206(10) 0.08509(13) 0.28596(9) 0.0166(3) Uani 1 1 d . . . H7 H 0.2536(14) 0.0324(16) 0.2430(13) 0.020 Uiso 1 1 d . . . Co8 Co 0.251770(12) 0.119150(14) 0.477149(11) 0.01358(5) Uani 1 1 d . . . B9 B 0.13589(11) 0.19942(13) 0.47155(10) 0.0188(3) Uani 1 1 d . . . H9 H 0.1174(14) 0.2257(16) 0.5324(13) 0.023 Uiso 1 1 d . . . B10 B 0.10259(11) 0.28189(13) 0.39678(12) 0.0224(3) Uani 1 1 d . . . H10 H 0.0670(15) 0.3492(17) 0.4146(14) 0.027 Uiso 1 1 d . . . B11 B 0.15920(13) 0.29059(13) 0.30793(12) 0.0242(3) Uani 1 1 d . . . H11 H 0.1509(16) 0.3638(17) 0.2825(14) 0.029 Uiso 1 1 d . . . B12 B 0.25062(11) 0.21390(14) 0.29136(10) 0.0201(3) Uani 1 1 d . . . H12 H 0.3025(14) 0.2464(16) 0.2544(14) 0.024 Uiso 1 1 d . . . B13 B 0.28958(10) 0.13422(12) 0.36443(9) 0.0156(3) Uani 1 1 d . . . H13 H 0.3606(14) 0.1183(15) 0.3606(13) 0.019 Uiso 1 1 d . . . B14 B 0.22711(10) 0.25375(12) 0.40017(11) 0.0169(3) Uani 1 1 d . . . H14 H 0.2697(14) 0.3131(16) 0.4226(13) 0.020 Uiso 1 1 d . . . C81 C 0.37807(11) 0.14266(14) 0.52658(10) 0.0243(3) Uani 1 1 d . . . H81 H 0.4295 0.1795 0.5014 0.029 Uiso 1 1 calc R . . C82 C 0.30922(11) 0.18518(13) 0.57484(9) 0.0230(3) Uani 1 1 d . . . H82 H 0.3041 0.2578 0.5894 0.028 Uiso 1 1 calc R . . C83 C 0.25030(13) 0.10808(16) 0.60048(10) 0.0306(4) Uani 1 1 d . . . H83 H 0.1965 0.1163 0.6358 0.037 Uiso 1 1 calc R . . C84 C 0.28160(16) 0.01712(15) 0.56683(12) 0.0377(5) Uani 1 1 d . . . H84 H 0.2533 -0.0505 0.5739 0.045 Uiso 1 1 calc R . . C85 C 0.36093(15) 0.03840(15) 0.52129(12) 0.0344(4) Uani 1 1 d . . . H85 H 0.3978 -0.0116 0.4911 0.041 Uiso 1 1 calc R . . C11 C -0.04338(9) 0.02691(12) 0.28107(10) 0.0204(3) Uani 1 1 d . . . H11A H -0.0947 0.0756 0.2792 0.025 Uiso 1 1 calc R . . C12 C -0.02073(10) -0.03617(12) 0.34615(9) 0.0197(3) Uani 1 1 d . . . H12A H -0.0531 -0.0398 0.3983 0.024 Uiso 1 1 calc R . . C13 C 0.05617(10) -0.09359(11) 0.32366(10) 0.0198(3) Uani 1 1 d . . . H13A H 0.0876 -0.1446 0.3573 0.024 Uiso 1 1 calc R . . C14 C 0.07991(10) -0.06638(11) 0.24461(10) 0.0210(3) Uani 1 1 d . . . H14A H 0.1313 -0.0947 0.2132 0.025 Uiso 1 1 calc R . . C15 C 0.01893(11) 0.00744(12) 0.21831(9) 0.0211(3) Uani 1 1 d . . . H15 H 0.0193 0.0405 0.1649 0.025 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 0.00873(7) 0.01237(8) 0.01052(7) 0.00047(6) -0.00072(5) -0.00022(5) C2 0.0132(5) 0.0124(5) 0.0133(5) -0.0016(4) -0.0032(4) 0.0008(4) B3 0.0195(6) 0.0155(6) 0.0104(6) -0.0014(5) 0.0017(5) -0.0045(5) B4 0.0139(6) 0.0183(7) 0.0255(8) -0.0073(6) 0.0027(5) 0.0008(5) C5 0.0199(6) 0.0155(6) 0.0293(8) 0.0018(5) -0.0075(5) 0.0022(5) B6 0.0217(7) 0.0228(7) 0.0175(7) 0.0074(6) -0.0051(6) -0.0040(6) B7 0.0134(5) 0.0241(7) 0.0123(6) -0.0019(5) 0.0006(5) -0.0031(5) Co8 0.01731(8) 0.01345(8) 0.00999(8) 0.00037(6) -0.00344(6) -0.00385(6) B9 0.0192(6) 0.0190(7) 0.0183(7) -0.0070(6) 0.0042(5) -0.0030(5) B10 0.0195(7) 0.0142(7) 0.0333(9) -0.0051(6) -0.0029(6) 0.0027(5) B11 0.0275(8) 0.0155(7) 0.0295(9) 0.0076(6) -0.0077(7) -0.0026(6) B12 0.0208(7) 0.0235(7) 0.0161(7) 0.0047(6) -0.0011(5) -0.0079(6) B13 0.0123(5) 0.0214(7) 0.0130(6) -0.0021(5) 0.0002(5) -0.0024(5) B14 0.0166(6) 0.0117(6) 0.0224(7) 0.0018(5) -0.0005(5) -0.0013(5) C81 0.0214(6) 0.0318(8) 0.0197(7) -0.0014(6) -0.0084(5) -0.0030(6) C82 0.0286(7) 0.0267(7) 0.0136(6) -0.0026(5) -0.0064(5) -0.0066(6) C83 0.0322(8) 0.0472(11) 0.0123(6) 0.0055(6) -0.0065(6) -0.0156(8) C84 0.0586(12) 0.0265(8) 0.0281(9) 0.0131(7) -0.0269(9) -0.0164(8) C85 0.0435(10) 0.0293(9) 0.0303(9) -0.0066(7) -0.0236(8) 0.0132(7) C11 0.0117(5) 0.0252(7) 0.0244(7) -0.0059(6) -0.0057(5) -0.0004(5) C12 0.0162(5) 0.0269(7) 0.0160(6) -0.0045(5) 0.0021(5) -0.0107(5) C13 0.0209(6) 0.0147(6) 0.0239(7) 0.0001(5) -0.0066(5) -0.0052(5) C14 0.0189(6) 0.0205(6) 0.0236(7) -0.0074(5) 0.0022(5) -0.0025(5) C15 0.0248(6) 0.0248(7) 0.0136(6) -0.0023(5) -0.0039(5) -0.0053(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 Co1 C11 2.0574(14) . ? Co1 C13 2.0650(15) . ? Co1 C12 2.0663(14) . ? Co1 C15 2.0693(14) . ? Co1 C14 2.0724(15) . ? Co1 B7 2.1238(15) . ? Co1 B4 2.1269(17) . ? Co1 C5 2.1323(15) . ? Co1 C2 2.1403(13) . ? Co1 B6 2.1484(17) . ? Co1 B3 2.1569(16) . ? C2 B7 1.677(2) . ? C2 B3 1.678(2) . ? C2 B13 1.699(2) . ? C2 Co8 2.0269(13) . ? C2 H2 0.99(2) . ? B3 B9 1.801(2) . ? B3 B4 1.804(2) . ? B3 Co8 2.0511(16) . ? B3 H3 1.12(2) . ? B4 C5 1.702(3) . ? B4 B9 1.763(2) . ? B4 B10 1.786(2) . ? B4 H4 1.06(2) . ? C5 B6 1.666(3) . ? C5 B10 1.689(2) . ? C5 B11 1.699(2) . ? C5 H5 1.03(2) . ? B6 B12 1.765(2) . ? B6 B11 1.771(3) . ? B6 B7 1.789(2) . ? B6 H6 1.11(2) . ? B7 B12 1.769(2) . ? B7 B13 1.781(2) . ? B7 H7 1.11(2) . ? Co8 B13 1.9869(16) . ? Co8 B9 2.0247(18) . ? Co8 C82 2.0487(15) . ? Co8 C81 2.0713(15) . ? Co8 C84 2.0776(17) . ? Co8 C85 2.0792(18) . ? Co8 C83 2.0794(17) . ? Co8 B14 2.2412(16) . ? B9 B10 1.741(3) . ? B9 B14 1.947(2) . ? B9 H9 1.12(2) . ? B10 B11 1.718(3) . ? B10 B14 1.883(2) . ? B10 H10 1.08(2) . ? B11 B12 1.719(3) . ? B11 B14 1.913(2) . ? B11 H11 1.07(2) . ? B12 B13 1.723(2) . ? B12 B14 1.937(3) . ? B12 H12 1.08(2) . ? B13 B14 1.937(2) . ? B13 H13 1.07(2) . ? B14 H14 1.08(2) . ? C81 C85 1.414(3) . ? C81 C82 1.421(2) . ? C81 H81 1.0000 . ? C82 C83 1.415(2) . ? C82 H82 1.0000 . ? C83 C84 1.415(3) . ? C83 H83 1.0000 . ? C84 C85 1.431(3) . ? C84 H84 1.0000 . ? C85 H85 1.0000 . ? C11 C12 1.420(2) . ? C11 C15 1.426(2) . ? C11 H11A 1.0000 . ? C12 C13 1.423(2) . ? C12 H12A 1.0000 . ? C13 C14 1.422(2) . ? C13 H13A 1.0000 . ? C14 C15 1.406(2) . ? C14 H14A 1.0000 . ? C15 H15 1.0000 . ? 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 C11 Co1 C13 67.64(6) . . ? C11 Co1 C12 40.28(7) . . ? C13 Co1 C12 40.31(6) . . ? C11 Co1 C15 40.43(6) . . ? C13 Co1 C15 67.34(6) . . ? C12 Co1 C15 67.69(6) . . ? C11 Co1 C14 67.44(6) . . ? C13 Co1 C14 40.21(6) . . ? C12 Co1 C14 67.60(6) . . ? C15 Co1 C14 39.70(6) . . ? C11 Co1 B7 147.00(6) . . ? C13 Co1 B7 112.32(7) . . ? C12 Co1 B7 152.58(7) . . ? C15 Co1 B7 107.39(6) . . ? C14 Co1 B7 91.19(6) . . ? C11 Co1 B4 95.74(6) . . ? C13 Co1 B4 124.08(7) . . ? C12 Co1 B4 92.29(6) . . ? C15 Co1 B4 131.22(7) . . ? C14 Co1 B4 159.72(6) . . ? B7 Co1 B4 108.78(6) . . ? C11 Co1 C5 93.94(6) . . ? C13 Co1 C5 159.95(6) . . ? C12 Co1 C5 120.04(6) . . ? C15 Co1 C5 104.18(6) . . ? C14 Co1 C5 140.92(7) . . ? B7 Co1 C5 87.38(6) . . ? B4 Co1 C5 47.10(7) . . ? C11 Co1 C2 160.06(6) . . ? C13 Co1 C2 94.10(5) . . ? C12 Co1 C2 120.15(6) . . ? C15 Co1 C2 140.82(6) . . ? C14 Co1 C2 104.19(6) . . ? B7 Co1 C2 46.31(6) . . ? B4 Co1 C2 87.91(6) . . ? C5 Co1 C2 102.76(5) . . ? C11 Co1 B6 111.56(7) . . ? C13 Co1 B6 147.20(7) . . ? C12 Co1 B6 151.78(6) . . ? C15 Co1 B6 90.73(7) . . ? C14 Co1 B6 107.65(7) . . ? B7 Co1 B6 49.50(7) . . ? B4 Co1 B6 88.68(7) . . ? C5 Co1 B6 45.80(7) . . ? C2 Co1 B6 88.07(6) . . ? C11 Co1 B3 124.94(6) . . ? C13 Co1 B3 95.48(6) . . ? C12 Co1 B3 92.78(6) . . ? C15 Co1 B3 160.09(6) . . ? C14 Co1 B3 130.33(6) . . ? B7 Co1 B3 88.05(6) . . ? B4 Co1 B3 49.82(7) . . ? C5 Co1 B3 88.67(6) . . ? C2 Co1 B3 45.97(6) . . ? B6 Co1 B3 109.04(6) . . ? B7 C2 B3 124.93(11) . . ? B7 C2 B13 63.66(9) . . ? B3 C2 B13 116.04(10) . . ? B7 C2 Co8 124.17(9) . . ? B3 C2 Co8 66.46(7) . . ? B13 C2 Co8 63.74(7) . . ? B7 C2 Co1 66.33(7) . . ? B3 C2 Co1 67.54(7) . . ? B13 C2 Co1 116.78(9) . . ? Co8 C2 Co1 126.21(6) . . ? B7 C2 H2 110.5(12) . . ? B3 C2 H2 113.9(12) . . ? B13 C2 H2 119.1(12) . . ? Co8 C2 H2 110.2(12) . . ? Co1 C2 H2 112.9(12) . . ? C2 B3 B9 109.43(11) . . ? C2 B3 B4 116.50(11) . . ? B9 B3 B4 58.53(9) . . ? C2 B3 Co8 64.95(7) . . ? B9 B3 Co8 63.02(7) . . ? B4 B3 Co8 117.46(9) . . ? C2 B3 Co1 66.49(7) . . ? B9 B3 Co1 111.27(10) . . ? B4 B3 Co1 64.23(7) . . ? Co8 B3 Co1 124.06(7) . . ? C2 B3 H3 118.9(11) . . ? B9 B3 H3 123.6(11) . . ? B4 B3 H3 115.9(11) . . ? Co8 B3 H3 113.4(11) . . ? Co1 B3 H3 113.3(11) . . ? C5 B4 B9 108.17(12) . . ? C5 B4 B10 57.86(10) . . ? B9 B4 B10 58.76(10) . . ? C5 B4 B3 117.47(11) . . ? B9 B4 B3 60.65(9) . . ? B10 B4 B3 110.03(11) . . ? C5 B4 Co1 66.61(8) . . ? B9 B4 Co1 114.29(9) . . ? B10 B4 Co1 113.10(11) . . ? B3 B4 Co1 65.95(7) . . ? C5 B4 H4 118.5(12) . . ? B9 B4 H4 120.2(12) . . ? B10 B4 H4 120.2(12) . . ? B3 B4 H4 118.3(12) . . ? Co1 B4 H4 117.3(12) . . ? B6 C5 B10 117.00(12) . . ? B6 C5 B11 63.51(11) . . ? B10 C5 B11 60.93(11) . . ? B6 C5 B4 125.07(12) . . ? B10 C5 B4 63.56(11) . . ? B11 C5 B4 117.00(12) . . ? B6 C5 Co1 67.61(8) . . ? B10 C5 Co1 117.23(10) . . ? B11 C5 Co1 117.95(10) . . ? B4 C5 Co1 66.28(7) . . ? B6 C5 H5 119.1(13) . . ? B10 C5 H5 111.9(13) . . ? B11 C5 H5 118.5(12) . . ? B4 C5 H5 107.8(13) . . ? Co1 C5 H5 117.5(12) . . ? C5 B6 B12 107.20(13) . . ? C5 B6 B11 59.15(11) . . ? B12 B6 B11 58.18(10) . . ? C5 B6 B7 116.60(12) . . ? B12 B6 B7 59.71(10) . . ? B11 B6 B7 109.91(12) . . ? C5 B6 Co1 66.59(8) . . ? B12 B6 Co1 111.39(10) . . ? B11 B6 Co1 113.85(11) . . ? B7 B6 Co1 64.53(7) . . ? C5 B6 H6 115.7(11) . . ? B12 B6 H6 122.2(11) . . ? B11 B6 H6 115.9(12) . . ? B7 B6 H6 122.6(12) . . ? Co1 B6 H6 120.1(12) . . ? C2 B7 B12 107.70(11) . . ? C2 B7 B13 58.76(8) . . ? B12 B7 B13 58.08(9) . . ? C2 B7 B6 118.63(12) . . ? B12 B7 B6 59.48(10) . . ? B13 B7 B6 109.80(12) . . ? C2 B7 Co1 67.36(7) . . ? B12 B7 Co1 112.34(10) . . ? B13 B7 Co1 113.88(9) . . ? B6 B7 Co1 65.96(7) . . ? C2 B7 H7 115.5(11) . . ? B12 B7 H7 123.1(11) . . ? B13 B7 H7 118.5(11) . . ? B6 B7 H7 120.4(11) . . ? Co1 B7 H7 117.4(11) . . ? B13 Co8 B9 98.12(7) . . ? B13 Co8 C2 50.07(6) . . ? B9 Co8 C2 89.05(6) . . ? B13 Co8 C82 127.21(6) . . ? B9 Co8 C82 99.38(7) . . ? C2 Co8 C82 171.55(6) . . ? B13 Co8 B3 90.35(6) . . ? B9 Co8 B3 52.45(6) . . ? C2 Co8 B3 48.59(6) . . ? C82 Co8 B3 138.32(6) . . ? B13 Co8 C81 96.49(7) . . ? B9 Co8 C81 134.82(7) . . ? C2 Co8 C81 131.65(6) . . ? C82 Co8 C81 40.35(7) . . ? B3 Co8 C81 168.56(7) . . ? B13 Co8 C84 134.32(9) . . ? B9 Co8 C84 124.02(9) . . ? C2 Co8 C84 108.68(7) . . ? C82 Co8 C84 67.06(7) . . ? B3 Co8 C84 101.32(7) . . ? C81 Co8 C84 67.38(8) . . ? B13 Co8 C85 99.99(8) . . ? B9 Co8 C85 161.68(8) . . ? C2 Co8 C85 104.70(6) . . ? C82 Co8 C85 67.20(7) . . ? B3 Co8 C85 129.86(8) . . ? C81 Co8 C85 39.84(8) . . ? C84 Co8 C85 40.28(10) . . ? B13 Co8 C83 164.10(7) . . ? B9 Co8 C83 94.30(8) . . ? C2 Co8 C83 140.46(7) . . ? C82 Co8 C83 40.08(7) . . ? B3 Co8 C83 105.13(6) . . ? C81 Co8 C83 67.66(7) . . ? C84 Co8 C83 39.81(9) . . ? C85 Co8 C83 67.38(9) . . ? B13 Co8 B14 54.13(6) . . ? B9 Co8 B14 54.03(6) . . ? C2 Co8 B14 83.59(6) . . ? C82 Co8 B14 100.82(7) . . ? B3 Co8 B14 86.47(6) . . ? C81 Co8 B14 104.97(7) . . ? C84 Co8 B14 167.73(7) . . ? C85 Co8 B14 138.31(8) . . ? C83 Co8 B14 129.14(8) . . ? B10 B9 B4 61.29(10) . . ? B10 B9 B3 112.27(12) . . ? B4 B9 B3 60.83(9) . . ? B10 B9 B14 61.12(9) . . ? B4 B9 B14 103.85(11) . . ? B3 B9 B14 103.43(10) . . ? B10 B9 Co8 127.37(11) . . ? B4 B9 Co8 120.95(10) . . ? B3 B9 Co8 64.53(8) . . ? B14 B9 Co8 68.67(7) . . ? B10 B9 H9 113.3(11) . . ? B4 B9 H9 117.7(11) . . ? B3 B9 H9 122.7(11) . . ? B14 B9 H9 128.3(11) . . ? Co8 B9 H9 109.3(11) . . ? C5 B10 B11 59.82(11) . . ? C5 B10 B9 109.80(12) . . ? B11 B10 B9 122.18(13) . . ? C5 B10 B4 58.58(10) . . ? B11 B10 B4 111.71(13) . . ? B9 B10 B4 59.96(10) . . ? C5 B10 B14 103.40(12) . . ? B11 B10 B14 63.98(10) . . ? B9 B10 B14 64.85(9) . . ? B4 B10 B14 105.57(11) . . ? C5 B10 H10 119.6(12) . . ? B11 B10 H10 115.0(13) . . ? B9 B10 H10 117.4(13) . . ? B4 B10 H10 118.8(12) . . ? B14 B10 H10 129.3(12) . . ? C5 B11 B10 59.25(10) . . ? C5 B11 B12 107.83(12) . . ? B10 B11 B12 119.06(13) . . ? C5 B11 B6 57.34(10) . . ? B10 B11 B6 110.15(13) . . ? B12 B11 B6 60.74(10) . . ? C5 B11 B14 101.79(12) . . ? B10 B11 B14 62.23(10) . . ? B12 B11 B14 64.19(10) . . ? B6 B11 B14 106.14(11) . . ? C5 B11 H11 118.1(13) . . ? B10 B11 H11 110.6(13) . . ? B12 B11 H11 124.5(13) . . ? B6 B11 H11 122.6(13) . . ? B14 B11 H11 128.1(13) . . ? B11 B12 B13 120.95(13) . . ? B11 B12 B6 61.08(11) . . ? B13 B12 B6 113.68(12) . . ? B11 B12 B7 113.32(12) . . ? B13 B12 B7 61.29(9) . . ? B6 B12 B7 60.81(10) . . ? B11 B12 B14 62.77(10) . . ? B13 B12 B14 63.59(9) . . ? B6 B12 B14 105.37(11) . . ? B7 B12 B14 105.73(11) . . ? B11 B12 H12 114.6(11) . . ? B13 B12 H12 114.8(12) . . ? B6 B12 H12 121.6(12) . . ? B7 B12 H12 122.0(12) . . ? B14 B12 H12 124.2(12) . . ? C2 B13 B12 108.85(11) . . ? C2 B13 B7 57.57(8) . . ? B12 B13 B7 60.63(10) . . ? C2 B13 B14 103.00(10) . . ? B12 B13 B14 63.58(10) . . ? B7 B13 B14 105.28(11) . . ? C2 B13 Co8 66.19(7) . . ? B12 B13 Co8 130.40(11) . . ? B7 B13 Co8 120.77(9) . . ? B14 B13 Co8 69.65(7) . . ? C2 B13 H13 121.9(11) . . ? B12 B13 H13 114.0(11) . . ? B7 B13 H13 115.7(11) . . ? B14 B13 H13 130.4(11) . . ? Co8 B13 H13 108.2(12) . . ? B10 B14 B11 53.79(10) . . ? B10 B14 B12 101.66(11) . . ? B11 B14 B12 53.04(10) . . ? B10 B14 B13 128.47(11) . . ? B11 B14 B13 102.15(11) . . ? B12 B14 B13 52.83(8) . . ? B10 B14 B9 54.03(9) . . ? B11 B14 B9 103.31(11) . . ? B12 B14 B9 127.26(11) . . ? B13 B14 B9 102.56(10) . . ? B10 B14 Co8 109.65(9) . . ? B11 B14 Co8 139.40(10) . . ? B12 B14 Co8 107.30(9) . . ? B13 B14 Co8 56.22(6) . . ? B9 B14 Co8 57.30(7) . . ? B10 B14 H14 115.9(11) . . ? B11 B14 H14 113.8(11) . . ? B12 B14 H14 115.2(11) . . ? B13 B14 H14 115.5(11) . . ? B9 B14 H14 117.5(11) . . ? Co8 B14 H14 106.8(11) . . ? C85 C81 C82 107.36(17) . . ? C85 C81 Co8 70.38(10) . . ? C82 C81 Co8 68.97(9) . . ? C85 C81 H81 126.3 . . ? C82 C81 H81 126.3 . . ? Co8 C81 H81 126.3 . . ? C83 C82 C81 109.12(16) . . ? C83 C82 Co8 71.13(9) . . ? C81 C82 Co8 70.68(9) . . ? C83 C82 H82 125.4 . . ? C81 C82 H82 125.4 . . ? Co8 C82 H82 125.4 . . ? C82 C83 C84 107.29(17) . . ? C82 C83 Co8 68.79(9) . . ? C84 C83 Co8 70.03(10) . . ? C82 C83 H83 126.4 . . ? C84 C83 H83 126.4 . . ? Co8 C83 H83 126.4 . . ? C83 C84 C85 108.27(16) . . ? C83 C84 Co8 70.16(10) . . ? C85 C84 Co8 69.92(10) . . ? C83 C84 H84 125.9 . . ? C85 C84 H84 125.9 . . ? Co8 C84 H84 125.9 . . ? C81 C85 C84 107.95(18) . . ? C81 C85 Co8 69.78(10) . . ? C84 C85 Co8 69.80(11) . . ? C81 C85 H85 126.0 . . ? C84 C85 H85 126.0 . . ? Co8 C85 H85 126.0 . . ? C12 C11 C15 108.06(13) . . ? C12 C11 Co1 70.20(8) . . ? C15 C11 Co1 70.24(8) . . ? C12 C11 H11A 126.0 . . ? C15 C11 H11A 126.0 . . ? Co1 C11 H11A 126.0 . . ? C11 C12 C13 107.59(13) . . ? C11 C12 Co1 69.52(8) . . ? C13 C12 Co1 69.80(8) . . ? C11 C12 H12A 126.2 . . ? C13 C12 H12A 126.2 . . ? Co1 C12 H12A 126.2 . . ? C14 C13 C12 108.02(13) . . ? C14 C13 Co1 70.18(8) . . ? C12 C13 Co1 69.90(8) . . ? C14 C13 H13A 126.0 . . ? C12 C13 H13A 126.0 . . ? Co1 C13 H13A 126.0 . . ? C15 C14 C13 108.26(13) . . ? C15 C14 Co1 70.03(8) . . ? C13 C14 Co1 69.61(9) . . ? C15 C14 H14A 125.9 . . ? C13 C14 H14A 125.9 . . ? Co1 C14 H14A 125.9 . . ? C14 C15 C11 108.07(14) . . ? C14 C15 Co1 70.27(9) . . ? C11 C15 Co1 69.33(8) . . ? C14 C15 H15 126.0 . . ? C11 C15 H15 126.0 . . ? Co1 C15 H15 126.0 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.906 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 939818'