# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Alan Welch' _publ_contact_author_address ; Department of Chemistry Heriot-Watt University Riccarton EDINBURGH EH14 4AS UNITED KINGDOM ; _publ_contact_author_email A.J.WELCH@HW.AC.UK _publ_section_title ; Unexpectedly facile isomerisation of [7,10-Ph2-7,10-nido-C2B10H10]2- to [7,9-Ph2-7,9-nido-C2B10H10]2- ; loop_ _publ_author_name A.Welch D.Ellis G.Rosair S.Zlatogorsky data_1x81270m _database_code_depnum_ccdc_archive 'CCDC 631512' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 B10' _chemical_formula_sum 'C14 H20 B10' _chemical_formula_weight 296.40 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.560(3) _cell_length_b 7.3833(17) _cell_length_c 19.199(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.339(12) _cell_angle_gamma 90.00 _cell_volume 1635.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3039 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 24.97 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.994 _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 'Bruker X8 Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26728 _diffrn_reflns_av_R_equivalents 0.1107 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3328 _reflns_number_gt 2169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1185P)^2^+5.6585P] 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 3328 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1445 _refine_ls_R_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.2973 _refine_ls_wR_factor_gt 0.2614 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 C1A C 0.5359(3) 0.9975(6) 0.0808(2) 0.0199(9) Uani 1 1 d . . . B2A B 0.4028(4) 0.9096(7) 0.0517(3) 0.0227(10) Uani 1 1 d . . . H2A H 0.343(4) 0.846(6) 0.086(2) 0.027 Uiso 1 1 d . . . B3A B 0.5341(4) 0.7966(7) 0.0354(3) 0.0221(10) Uani 1 1 d . . . H3A H 0.557(4) 0.673(6) 0.065(2) 0.027 Uiso 1 1 d . . . B4A B 0.6409(4) 0.9631(7) 0.0229(3) 0.0200(10) Uani 1 1 d . . . H4A H 0.731(4) 0.932(6) 0.039(2) 0.024 Uiso 1 1 d . . . B5A B 0.5765(4) 1.1804(7) 0.0312(3) 0.0221(10) Uani 1 1 d . . . H5A H 0.625(4) 1.291(6) 0.057(2) 0.026 Uiso 1 1 d . . . B6A B 0.4297(4) 1.1473(7) 0.0496(3) 0.0226(10) Uani 1 1 d . . . H6A H 0.385(4) 1.235(7) 0.084(2) 0.027 Uiso 1 1 d . . . C11A C 0.5714(3) 1.0001(5) 0.1575(2) 0.0201(9) Uani 1 1 d . . . C12A C 0.4995(4) 0.9389(6) 0.2069(2) 0.0220(9) Uani 1 1 d . . . H12A H 0.4269 0.8932 0.1926 0.026 Uiso 1 1 calc R . . C13A C 0.5323(4) 0.9438(6) 0.2775(2) 0.0247(10) Uani 1 1 d . . . H13A H 0.4816 0.9040 0.3101 0.030 Uiso 1 1 calc R . . C14A C 0.6421(4) 1.0090(6) 0.2993(2) 0.0253(10) Uani 1 1 d . . . H14A H 0.6660 1.0099 0.3464 0.030 Uiso 1 1 calc R . . C15A C 0.7141(4) 1.0714(6) 0.2505(2) 0.0253(10) Uani 1 1 d . . . H15A H 0.7865 1.1174 0.2649 0.030 Uiso 1 1 calc R . . C16A C 0.6814(4) 1.0674(6) 0.1802(2) 0.0235(9) Uani 1 1 d . . . H16A H 0.7319 1.1091 0.1478 0.028 Uiso 1 1 calc R . . C1B C 0.0445(3) 0.0002(6) 0.4241(2) 0.0189(9) Uani 1 1 d . . . B2B B 0.0769(4) -0.1837(7) 0.4776(3) 0.0221(10) Uani 1 1 d . . . H2B H 0.124(4) -0.298(7) 0.457(2) 0.026 Uiso 1 1 d . . . B3B B -0.0671(4) -0.1447(7) 0.4429(3) 0.0229(11) Uani 1 1 d . . . H3B H -0.106(4) -0.236(7) 0.403(2) 0.027 Uiso 1 1 d . . . B4B B -0.0894(4) 0.0942(7) 0.4370(3) 0.0218(10) Uani 1 1 d . . . H4B H -0.140(4) 0.155(6) 0.392(2) 0.026 Uiso 1 1 d . . . B5B B 0.0413(4) 0.2015(7) 0.4690(3) 0.0222(10) Uani 1 1 d . . . H5B H 0.069(4) 0.326(6) 0.443(2) 0.027 Uiso 1 1 d . . . B6B B 0.1429(4) 0.0305(7) 0.4935(3) 0.0214(10) Uani 1 1 d . . . H6B H 0.235(4) 0.056(6) 0.485(2) 0.026 Uiso 1 1 d . . . C11B C 0.0855(4) 0.0034(6) 0.3515(2) 0.0208(9) Uani 1 1 d . . . C12B C 0.0218(4) -0.0734(6) 0.2958(2) 0.0230(9) Uani 1 1 d . . . H12B H -0.0479 -0.1304 0.3038 0.028 Uiso 1 1 calc R . . C13B C 0.0589(4) -0.0680(6) 0.2286(2) 0.0271(10) Uani 1 1 d . . . H13B H 0.0140 -0.1196 0.1921 0.032 Uiso 1 1 calc R . . C14B C 0.1631(4) 0.0147(6) 0.2159(2) 0.0281(10) Uani 1 1 d . . . H14B H 0.1897 0.0168 0.1711 0.034 Uiso 1 1 calc R . . C15B C 0.2269(4) 0.0938(6) 0.2708(2) 0.0275(10) Uani 1 1 d . . . H15B H 0.2961 0.1518 0.2623 0.033 Uiso 1 1 calc R . . C16B C 0.1901(4) 0.0885(6) 0.3381(2) 0.0232(9) Uani 1 1 d . . . H16B H 0.2349 0.1414 0.3744 0.028 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 C1A 0.0135(19) 0.019(2) 0.027(2) -0.0021(17) -0.0004(16) -0.0008(16) B2A 0.015(2) 0.025(3) 0.028(3) 0.001(2) -0.0016(18) -0.0040(19) B3A 0.019(2) 0.021(3) 0.026(2) 0.002(2) -0.0019(18) 0.0052(19) B4A 0.013(2) 0.023(3) 0.023(2) -0.002(2) -0.0014(17) -0.0014(18) B5A 0.017(2) 0.021(3) 0.028(3) -0.001(2) -0.0007(18) -0.0026(19) B6A 0.016(2) 0.023(3) 0.028(3) -0.002(2) -0.0017(18) 0.0027(19) C11A 0.020(2) 0.014(2) 0.026(2) -0.0031(16) -0.0008(16) 0.0039(16) C12A 0.023(2) 0.019(2) 0.024(2) 0.0015(17) 0.0005(17) 0.0004(17) C13A 0.027(2) 0.021(2) 0.026(2) 0.0034(18) 0.0018(17) 0.0010(18) C14A 0.031(2) 0.022(2) 0.022(2) 0.0003(17) -0.0016(17) 0.0025(19) C15A 0.022(2) 0.021(2) 0.032(2) -0.0026(19) -0.0054(17) 0.0006(18) C16A 0.022(2) 0.021(2) 0.027(2) 0.0029(18) -0.0007(17) -0.0007(17) C1B 0.0150(19) 0.021(2) 0.021(2) -0.0028(17) -0.0009(15) -0.0015(16) B2B 0.020(2) 0.021(3) 0.025(2) -0.002(2) 0.0013(18) 0.0010(19) B3B 0.015(2) 0.028(3) 0.026(3) -0.005(2) 0.0031(18) -0.0070(19) B4B 0.013(2) 0.028(3) 0.025(2) -0.001(2) 0.0004(18) -0.0005(19) B5B 0.019(2) 0.021(3) 0.027(3) -0.005(2) 0.0038(18) -0.0023(19) B6B 0.015(2) 0.024(3) 0.024(2) -0.002(2) -0.0008(18) -0.0030(19) C11B 0.025(2) 0.018(2) 0.019(2) -0.0018(16) -0.0020(16) 0.0040(17) C12B 0.024(2) 0.024(2) 0.021(2) -0.0008(18) 0.0000(16) 0.0014(18) C13B 0.034(2) 0.026(2) 0.021(2) -0.0036(18) -0.0009(18) 0.004(2) C14B 0.033(3) 0.026(2) 0.025(2) -0.0010(19) 0.0051(19) 0.009(2) C15B 0.027(2) 0.026(2) 0.030(2) 0.0042(19) 0.0099(18) 0.0042(19) C16B 0.024(2) 0.026(2) 0.020(2) -0.0024(18) 0.0001(16) -0.0008(18) _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 C1A C11A 1.506(6) . ? C1A B4A 1.711(6) . ? C1A B3A 1.720(6) . ? C1A B5A 1.732(6) . ? C1A B2A 1.732(6) . ? C1A B6A 1.733(6) . ? B2A B5A 1.754(7) 3_675 ? B2A B4A 1.762(7) 3_675 ? B2A B3A 1.776(7) . ? B2A B6A 1.783(7) . ? B2A H2A 1.09(5) . ? B3A B6A 1.757(7) 3_675 ? B3A B5A 1.763(7) 3_675 ? B3A B4A 1.768(7) . ? B3A H3A 1.11(5) . ? B4A B2A 1.762(7) 3_675 ? B4A B6A 1.770(7) 3_675 ? B4A B5A 1.779(7) . ? B4A H4A 1.09(4) . ? B5A B2A 1.754(7) 3_675 ? B5A B3A 1.763(7) 3_675 ? B5A B6A 1.771(7) . ? B5A H5A 1.10(5) . ? B6A B3A 1.757(7) 3_675 ? B6A B4A 1.770(7) 3_675 ? B6A H6A 1.08(5) . ? C11A C12A 1.374(6) . ? C11A C16A 1.411(6) . ? C12A C13A 1.387(6) . ? C12A H12A 0.9300 . ? C13A C14A 1.399(6) . ? C13A H13A 0.9300 . ? C14A C15A 1.370(6) . ? C14A H14A 0.9300 . ? C15A C16A 1.380(6) . ? C15A H15A 0.9300 . ? C16A H16A 0.9300 . ? C1B C11B 1.497(6) . ? C1B B6B 1.716(6) . ? C1B B5B 1.720(6) . ? C1B B4B 1.727(6) . ? C1B B3B 1.730(6) . ? C1B B2B 1.730(6) . ? B2B B5B 1.761(6) 3_556 ? B2B B4B 1.766(7) 3_556 ? B2B B6B 1.775(7) . ? B2B B3B 1.780(7) . ? B2B H2B 1.09(5) . ? B3B B5B 1.751(7) 3_556 ? B3B B6B 1.758(7) 3_556 ? B3B B4B 1.785(7) . ? B3B H3B 1.10(5) . ? B4B B2B 1.766(7) 3_556 ? B4B B6B 1.763(7) 3_556 ? B4B B5B 1.783(7) . ? B4B H4B 1.12(4) . ? B5B B3B 1.751(7) 3_556 ? B5B B2B 1.761(7) 3_556 ? B5B B6B 1.770(7) . ? B5B H5B 1.10(5) . ? B6B B3B 1.758(7) 3_556 ? B6B B4B 1.763(7) 3_556 ? B6B H6B 1.11(4) . ? C11B C12B 1.384(6) . ? C11B C16B 1.400(6) . ? C12B C13B 1.383(6) . ? C12B H12B 0.9300 . ? C13B C14B 1.385(7) . ? C13B H13B 0.9300 . ? C14B C15B 1.379(6) . ? C14B H14B 0.9300 . ? C15B C16B 1.385(6) . ? C15B H15B 0.9300 . ? C16B H16B 0.9300 . ? 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 C11A C1A B4A 118.3(3) . . ? C11A C1A B3A 120.1(3) . . ? B4A C1A B3A 62.0(3) . . ? C11A C1A B5A 117.3(3) . . ? B4A C1A B5A 62.2(3) . . ? B3A C1A B5A 113.0(3) . . ? C11A C1A B2A 120.4(3) . . ? B4A C1A B2A 112.7(3) . . ? B3A C1A B2A 61.9(3) . . ? B5A C1A B2A 112.3(3) . . ? C11A C1A B6A 118.5(3) . . ? B4A C1A B6A 112.7(3) . . ? B3A C1A B6A 112.8(3) . . ? B5A C1A B6A 61.5(3) . . ? B2A C1A B6A 61.9(3) . . ? C1A B2A B5A 105.6(3) . 3_675 ? C1A B2A B4A 105.6(3) . 3_675 ? B5A B2A B4A 60.8(3) 3_675 3_675 ? C1A B2A B3A 58.7(3) . . ? B5A B2A B3A 59.9(3) 3_675 . ? B4A B2A B3A 108.3(3) 3_675 . ? C1A B2A B6A 59.1(3) . . ? B5A B2A B6A 108.6(3) 3_675 . ? B4A B2A B6A 59.9(3) 3_675 . ? B3A B2A B6A 107.9(3) . . ? C1A B2A H2A 123(2) . . ? B5A B2A H2A 121(2) 3_675 . ? B4A B2A H2A 124(2) 3_675 . ? B3A B2A H2A 119(2) . . ? B6A B2A H2A 124(3) . . ? C1A B3A B6A 105.7(3) . 3_675 ? C1A B3A B5A 105.7(3) . 3_675 ? B6A B3A B5A 60.4(3) 3_675 3_675 ? C1A B3A B4A 58.7(3) . . ? B6A B3A B4A 60.3(3) 3_675 . ? B5A B3A B4A 108.5(3) 3_675 . ? C1A B3A B2A 59.4(3) . . ? B6A B3A B2A 107.8(3) 3_675 . ? B5A B3A B2A 59.4(3) 3_675 . ? B4A B3A B2A 107.9(3) . . ? C1A B3A H3A 117(2) . . ? B6A B3A H3A 128(2) 3_675 . ? B5A B3A H3A 127(2) 3_675 . ? B4A B3A H3A 120(2) . . ? B2A B3A H3A 118(2) . . ? C1A B4A B2A 105.5(3) . 3_675 ? C1A B4A B6A 105.5(3) . 3_675 ? B2A B4A B6A 60.6(3) 3_675 3_675 ? C1A B4A B3A 59.2(3) . . ? B2A B4A B3A 108.2(3) 3_675 . ? B6A B4A B3A 59.5(3) 3_675 . ? C1A B4A B5A 59.5(3) . . ? B2A B4A B5A 59.4(3) 3_675 . ? B6A B4A B5A 108.1(3) 3_675 . ? B3A B4A B5A 108.4(3) . . ? C1A B4A H4A 124(2) . . ? B2A B4A H4A 124(2) 3_675 . ? B6A B4A H4A 121(2) 3_675 . ? B3A B4A H4A 119(2) . . ? B5A B4A H4A 124(2) . . ? C1A B5A B2A 105.0(3) . 3_675 ? C1A B5A B3A 105.3(3) . 3_675 ? B2A B5A B3A 60.6(3) 3_675 3_675 ? C1A B5A B6A 59.3(3) . . ? B2A B5A B6A 108.1(3) 3_675 . ? B3A B5A B6A 59.6(3) 3_675 . ? C1A B5A B4A 58.3(3) . . ? B2A B5A B4A 59.8(3) 3_675 . ? B3A B5A B4A 108.1(3) 3_675 . ? B6A B5A B4A 107.7(3) . . ? C1A B5A H5A 119(2) . . ? B2A B5A H5A 127(2) 3_675 . ? B3A B5A H5A 126(2) 3_675 . ? B6A B5A H5A 119(2) . . ? B4A B5A H5A 121(2) . . ? C1A B6A B3A 105.6(3) . 3_675 ? C1A B6A B4A 105.2(3) . 3_675 ? B3A B6A B4A 60.2(3) 3_675 3_675 ? C1A B6A B5A 59.2(3) . . ? B3A B6A B5A 60.0(3) 3_675 . ? B4A B6A B5A 108.1(3) 3_675 . ? C1A B6A B2A 59.0(3) . . ? B3A B6A B2A 107.7(3) 3_675 . ? B4A B6A B2A 59.5(3) 3_675 . ? B5A B6A B2A 108.1(3) . . ? C1A B6A H6A 122(2) . . ? B3A B6A H6A 125(3) 3_675 . ? B4A B6A H6A 123(2) 3_675 . ? B5A B6A H6A 122(2) . . ? B2A B6A H6A 119(3) . . ? C12A C11A C16A 118.3(4) . . ? C12A C11A C1A 121.9(4) . . ? C16A C11A C1A 119.8(4) . . ? C11A C12A C13A 121.6(4) . . ? C11A C12A H12A 119.2 . . ? C13A C12A H12A 119.2 . . ? C12A C13A C14A 119.6(4) . . ? C12A C13A H13A 120.2 . . ? C14A C13A H13A 120.2 . . ? C15A C14A C13A 119.2(4) . . ? C15A C14A H14A 120.4 . . ? C13A C14A H14A 120.4 . . ? C14A C15A C16A 121.3(4) . . ? C14A C15A H15A 119.4 . . ? C16A C15A H15A 119.4 . . ? C15A C16A C11A 120.1(4) . . ? C15A C16A H16A 120.0 . . ? C11A C16A H16A 120.0 . . ? C11B C1B B6B 119.3(3) . . ? C11B C1B B5B 118.0(3) . . ? B6B C1B B5B 62.0(3) . . ? C11B C1B B4B 117.5(3) . . ? B6B C1B B4B 113.3(3) . . ? B5B C1B B4B 62.3(3) . . ? C11B C1B B3B 119.0(3) . . ? B6B C1B B3B 112.8(3) . . ? B5B C1B B3B 113.0(3) . . ? B4B C1B B3B 62.1(3) . . ? C11B C1B B2B 119.7(3) . . ? B6B C1B B2B 62.0(3) . . ? B5B C1B B2B 113.0(3) . . ? B4B C1B B2B 113.3(3) . . ? B3B C1B B2B 61.9(3) . . ? C1B B2B B5B 104.9(3) . 3_556 ? C1B B2B B4B 105.1(3) . 3_556 ? B5B B2B B4B 60.7(3) 3_556 3_556 ? C1B B2B B6B 58.6(3) . . ? B5B B2B B6B 107.9(3) 3_556 . ? B4B B2B B6B 59.7(3) 3_556 . ? C1B B2B B3B 59.0(3) . . ? B5B B2B B3B 59.3(3) 3_556 . ? B4B B2B B3B 108.1(3) 3_556 . ? B6B B2B B3B 107.7(3) . . ? C1B B2B H2B 119(2) . . ? B5B B2B H2B 125(2) 3_556 . ? B4B B2B H2B 127(2) 3_556 . ? B6B B2B H2B 122(2) . . ? B3B B2B H2B 118(2) . . ? C1B B3B B5B 105.3(3) . 3_556 ? C1B B3B B6B 104.9(3) . 3_556 ? B5B B3B B6B 60.6(3) 3_556 3_556 ? C1B B3B B2B 59.0(3) . . ? B5B B3B B2B 59.8(3) 3_556 . ? B6B B3B B2B 108.1(3) 3_556 . ? C1B B3B B4B 58.9(3) . . ? B5B B3B B4B 108.3(3) 3_556 . ? B6B B3B B4B 59.7(3) 3_556 . ? B2B B3B B4B 108.2(3) . . ? C1B B3B H3B 121(2) . . ? B5B B3B H3B 124(2) 3_556 . ? B6B B3B H3B 125(2) 3_556 . ? B2B B3B H3B 120(2) . . ? B4B B3B H3B 121(3) . . ? C1B B4B B2B 105.0(3) . 3_556 ? C1B B4B B6B 104.8(3) . 3_556 ? B2B B4B B6B 60.4(3) 3_556 3_556 ? C1B B4B B5B 58.7(2) . . ? B2B B4B B5B 59.5(3) 3_556 . ? B6B B4B B5B 107.4(3) 3_556 . ? C1B B4B B3B 59.0(3) . . ? B2B B4B B3B 107.9(3) 3_556 . ? B6B B4B B3B 59.4(3) 3_556 . ? B5B B4B B3B 107.5(3) . . ? C1B B4B H4B 119(2) . . ? B2B B4B H4B 126(2) 3_556 . ? B6B B4B H4B 128(2) 3_556 . ? B5B B4B H4B 119(2) . . ? B3B B4B H4B 121(2) . . ? C1B B5B B3B 105.6(3) . 3_556 ? C1B B5B B2B 105.5(3) . 3_556 ? B3B B5B B2B 60.9(3) 3_556 3_556 ? C1B B5B B6B 58.9(3) . . ? B3B B5B B6B 59.9(3) 3_556 . ? B2B B5B B6B 108.5(4) 3_556 . ? C1B B5B B4B 59.1(3) . . ? B3B B5B B4B 108.6(3) 3_556 . ? B2B B5B B4B 59.8(3) 3_556 . ? B6B B5B B4B 108.1(3) . . ? C1B B5B H5B 118(2) . . ? B3B B5B H5B 127(2) 3_556 . ? B2B B5B H5B 126(2) 3_556 . ? B6B B5B H5B 121(2) . . ? B4B B5B H5B 118(2) . . ? C1B B6B B3B 105.5(3) . 3_556 ? C1B B6B B4B 105.9(3) . 3_556 ? B3B B6B B4B 60.9(3) 3_556 3_556 ? C1B B6B B5B 59.1(3) . . ? B3B B6B B5B 59.5(3) 3_556 . ? B4B B6B B5B 108.5(3) 3_556 . ? C1B B6B B2B 59.4(3) . . ? B3B B6B B2B 108.7(3) 3_556 . ? B4B B6B B2B 59.9(3) 3_556 . ? B5B B6B B2B 108.5(3) . . ? C1B B6B H6B 120(2) . . ? B3B B6B H6B 123(2) 3_556 . ? B4B B6B H6B 126(2) 3_556 . ? B5B B6B H6B 118(2) . . ? B2B B6B H6B 122(2) . . ? C12B C11B C16B 117.9(4) . . ? C12B C11B C1B 122.0(4) . . ? C16B C11B C1B 120.1(4) . . ? C13B C12B C11B 121.9(4) . . ? C13B C12B H12B 119.0 . . ? C11B C12B H12B 119.0 . . ? C14B C13B C12B 119.8(4) . . ? C14B C13B H13B 120.1 . . ? C12B C13B H13B 120.1 . . ? C15B C14B C13B 119.0(4) . . ? C15B C14B H14B 120.5 . . ? C13B C14B H14B 120.5 . . ? C14B C15B C16B 121.4(4) . . ? C14B C15B H15B 119.3 . . ? C16B C15B H15B 119.3 . . ? C15B C16B C11B 120.0(4) . . ? C15B C16B H16B 120.0 . . ? C11B C16B H16B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.577 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.092 #===end data_3x81151 _database_code_depnum_ccdc_archive 'CCDC 631513' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H25 B10 Co' _chemical_formula_weight 420.42 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)/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 7.9865(15) _cell_length_b 16.119(3) _cell_length_c 15.593(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.559(7) _cell_angle_gamma 90.00 _cell_volume 1994.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 571 _cell_measurement_theta_min 2.5185 _cell_measurement_theta_max 20.87 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.901 _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22792 _diffrn_reflns_av_R_equivalents 0.1012 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.37 _reflns_number_total 2878 _reflns_number_gt 2063 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+1.6307P] 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 2878 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Co4 Co 0.21954(6) 0.72593(3) 0.84682(3) 0.02024(16) Uani 1 1 d . . . C1 C 0.2936(4) 0.8467(2) 0.8600(2) 0.0190(8) Uani 1 1 d . . . B2 B 0.4556(5) 0.7965(2) 0.8560(3) 0.0197(10) Uani 1 1 d . . . H2C H 0.559(4) 0.8038(17) 0.9098(19) 0.024 Uiso 1 1 d . . . B3 B 0.1433(5) 0.8457(3) 0.7874(2) 0.0217(10) Uani 1 1 d . . . H3C H 0.036(4) 0.8789(19) 0.8001(19) 0.026 Uiso 1 1 d . . . B5 B 0.3794(5) 0.8799(3) 0.7658(3) 0.0224(10) Uani 1 1 d . . . H5C H 0.420(4) 0.942(2) 0.7739(19) 0.027 Uiso 1 1 d . . . C6 C 0.4559(4) 0.7081(2) 0.7908(2) 0.0186(8) Uani 1 1 d . . . B7 B 0.1146(5) 0.7577(3) 0.7155(2) 0.0235(10) Uani 1 1 d . . . H7C H -0.017(4) 0.7395(18) 0.6992(19) 0.028 Uiso 1 1 d . . . B8 B 0.2020(5) 0.8494(3) 0.6801(3) 0.0265(11) Uani 1 1 d . . . H8C H 0.136(4) 0.8965(19) 0.641(2) 0.032 Uiso 1 1 d . . . B9 B 0.5442(5) 0.7962(2) 0.7555(2) 0.0210(10) Uani 1 1 d . . . H9C H 0.678(4) 0.8052(18) 0.7629(18) 0.025 Uiso 1 1 d . . . B10 B 0.2780(5) 0.6812(3) 0.7256(3) 0.0231(10) Uani 1 1 d . . . H10C H 0.253(4) 0.615(2) 0.7178(19) 0.028 Uiso 1 1 d . . . B11 B 0.4109(5) 0.8299(3) 0.6654(3) 0.0239(10) Uani 1 1 d . . . H11C H 0.474(4) 0.8666(19) 0.6207(19) 0.029 Uiso 1 1 d . . . B12 B 0.4583(5) 0.7238(3) 0.6826(2) 0.0241(10) Uani 1 1 d . . . H12C H 0.547(4) 0.6869(18) 0.6481(19) 0.029 Uiso 1 1 d . . . B13 B 0.2536(5) 0.7533(3) 0.6385(3) 0.0270(11) Uani 1 1 d . . . H13C H 0.212(4) 0.7342(19) 0.571(2) 0.032 Uiso 1 1 d . . . C11 C 0.2874(4) 0.9045(2) 0.9349(2) 0.0211(9) Uani 1 1 d . . . C12 C 0.3607(4) 0.8847(2) 1.0182(2) 0.0251(9) Uani 1 1 d . . . H12 H 0.4159 0.8328 1.0284 0.030 Uiso 1 1 calc R . . C13 C 0.3536(4) 0.9398(2) 1.0859(2) 0.0260(9) Uani 1 1 d . . . H13 H 0.4037 0.9254 1.1422 0.031 Uiso 1 1 calc R . . C14 C 0.2739(4) 1.0157(2) 1.0720(2) 0.0279(9) Uani 1 1 d . . . H14 H 0.2680 1.0531 1.1186 0.034 Uiso 1 1 calc R . . C15 C 0.2031(4) 1.0367(2) 0.9900(2) 0.0263(9) Uani 1 1 d . . . H15 H 0.1506 1.0892 0.9797 0.032 Uiso 1 1 calc R . . C16 C 0.2086(4) 0.9811(2) 0.9228(2) 0.0253(9) Uani 1 1 d . . . H16 H 0.1571 0.9957 0.8669 0.030 Uiso 1 1 calc R . . C41 C 0.0511(5) 0.6320(2) 0.8521(2) 0.0344(10) Uani 1 1 d . . . H41 H -0.0011 0.6019 0.8039 0.041 Uiso 1 1 calc R . . C42 C 0.2036(5) 0.6118(2) 0.9021(2) 0.0305(10) Uani 1 1 d . . . H42 H 0.2732 0.5657 0.8926 0.037 Uiso 1 1 calc R . . C43 C 0.2363(5) 0.6706(2) 0.9681(2) 0.0285(9) Uani 1 1 d . . . H43 H 0.3305 0.6712 1.0112 0.034 Uiso 1 1 calc R . . C44 C 0.1040(4) 0.7284(2) 0.9587(2) 0.0297(9) Uani 1 1 d . . . H44 H 0.0932 0.7751 0.9948 0.036 Uiso 1 1 calc R . . C45 C -0.0100(5) 0.7055(2) 0.8870(2) 0.0340(10) Uani 1 1 d . . . H45 H -0.1101 0.7343 0.8659 0.041 Uiso 1 1 calc R . . C61 C 0.5652(4) 0.6375(2) 0.8291(2) 0.0197(8) Uani 1 1 d . . . C62 C 0.6239(4) 0.6337(2) 0.9168(2) 0.0214(9) Uani 1 1 d . . . H62 H 0.5972 0.6775 0.9537 0.026 Uiso 1 1 calc R . . C63 C 0.7203(4) 0.5676(2) 0.9514(2) 0.0254(9) Uani 1 1 d . . . H63 H 0.7595 0.5666 1.0113 0.030 Uiso 1 1 calc R . . C64 C 0.7590(4) 0.5033(2) 0.8990(2) 0.0253(9) Uani 1 1 d . . . H64 H 0.8255 0.4580 0.9224 0.030 Uiso 1 1 calc R . . C65 C 0.7010(4) 0.5050(2) 0.8128(2) 0.0244(9) Uani 1 1 d . . . H65 H 0.7271 0.4606 0.7765 0.029 Uiso 1 1 calc R . . C66 C 0.6049(4) 0.5707(2) 0.7782(2) 0.0237(9) Uani 1 1 d . . . H66 H 0.5649 0.5705 0.7185 0.028 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 Co4 0.0205(3) 0.0228(3) 0.0176(3) 0.0017(2) 0.00268(19) -0.0041(3) C1 0.022(2) 0.019(2) 0.0162(19) 0.0033(16) 0.0006(16) -0.0015(16) B2 0.031(3) 0.011(2) 0.018(2) -0.0004(17) 0.003(2) -0.0050(18) B3 0.022(3) 0.027(3) 0.016(2) 0.0065(19) 0.0015(19) 0.003(2) B5 0.023(3) 0.023(3) 0.021(2) 0.008(2) 0.003(2) 0.000(2) C6 0.019(2) 0.022(2) 0.0150(18) -0.0006(15) 0.0019(15) -0.0035(16) B7 0.020(2) 0.028(3) 0.021(2) -0.0037(19) -0.0046(18) -0.004(2) B8 0.025(3) 0.036(3) 0.017(2) 0.005(2) -0.001(2) 0.002(2) B9 0.021(2) 0.022(3) 0.021(2) 0.0043(18) 0.0041(19) -0.0025(19) B10 0.022(2) 0.025(3) 0.022(2) 0.000(2) 0.0020(19) -0.009(2) B11 0.022(2) 0.031(3) 0.019(2) 0.002(2) 0.003(2) -0.002(2) B12 0.021(2) 0.032(3) 0.020(2) -0.002(2) 0.0050(18) -0.002(2) B13 0.032(3) 0.034(3) 0.014(2) 0.0017(19) -0.002(2) -0.003(2) C11 0.019(2) 0.021(2) 0.023(2) 0.0022(17) 0.0011(17) -0.0002(17) C12 0.028(2) 0.024(2) 0.022(2) 0.0030(18) 0.0016(17) 0.0045(18) C13 0.031(2) 0.030(2) 0.017(2) -0.0032(18) 0.0029(17) -0.0008(19) C14 0.033(2) 0.023(2) 0.029(2) -0.0061(18) 0.0081(19) -0.0030(19) C15 0.028(2) 0.020(2) 0.032(2) -0.0002(18) 0.0057(18) 0.0059(17) C16 0.024(2) 0.025(2) 0.026(2) 0.0036(18) 0.0019(17) -0.0011(18) C41 0.032(3) 0.042(3) 0.029(2) 0.000(2) 0.006(2) -0.018(2) C42 0.038(3) 0.024(2) 0.032(2) 0.0078(19) 0.012(2) -0.0048(19) C43 0.030(2) 0.036(3) 0.021(2) 0.0085(19) 0.0039(18) -0.006(2) C44 0.034(2) 0.032(2) 0.027(2) 0.004(2) 0.0179(18) -0.004(2) C45 0.021(2) 0.050(3) 0.033(2) 0.009(2) 0.0086(19) -0.006(2) C61 0.016(2) 0.022(2) 0.020(2) -0.0020(17) 0.0016(16) -0.0041(16) C62 0.021(2) 0.017(2) 0.026(2) -0.0004(17) 0.0044(17) -0.0017(16) C63 0.031(2) 0.025(2) 0.020(2) 0.0009(18) 0.0035(18) -0.0032(19) C64 0.029(2) 0.018(2) 0.030(2) 0.0048(18) 0.0064(18) 0.0006(18) C65 0.023(2) 0.019(2) 0.032(2) -0.0058(18) 0.0060(18) -0.0029(18) C66 0.024(2) 0.024(2) 0.023(2) -0.0030(18) 0.0004(17) -0.0035(18) _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 Co4 C45 2.031(4) . ? Co4 C41 2.033(4) . ? Co4 C1 2.038(3) . ? Co4 C42 2.042(4) . ? Co4 C44 2.066(3) . ? Co4 C43 2.082(3) . ? Co4 B10 2.124(4) . ? Co4 B7 2.183(4) . ? Co4 C6 2.188(3) . ? Co4 B2 2.192(4) . ? Co4 B3 2.197(4) . ? C1 C11 1.500(4) . ? C1 B2 1.533(5) . ? C1 B3 1.553(5) . ? C1 B5 1.772(5) . ? B2 C6 1.750(5) . ? B2 B9 1.792(6) . ? B2 B5 1.989(5) . ? B2 H2C 1.11(3) . ? B3 B8 1.789(6) . ? B3 B7 1.806(6) . ? B3 B5 2.029(6) . ? B3 H3C 1.05(3) . ? B5 B11 1.803(6) . ? B5 B8 1.898(6) . ? B5 B9 1.903(6) . ? B5 H5C 1.06(3) . ? C6 C61 1.516(4) . ? C6 B9 1.704(5) . ? C6 B10 1.706(5) . ? C6 B12 1.708(5) . ? B7 B13 1.727(6) . ? B7 B8 1.750(6) . ? B7 B10 1.789(6) . ? B7 H7C 1.09(3) . ? B8 B11 1.739(6) . ? B8 B13 1.747(6) . ? B8 H8C 1.08(3) . ? B9 B12 1.716(6) . ? B9 B11 1.748(6) . ? B9 H9C 1.07(3) . ? B10 B13 1.781(6) . ? B10 B12 1.793(6) . ? B10 H10C 1.09(3) . ? B11 B12 1.766(6) . ? B11 B13 1.778(6) . ? B11 H11C 1.08(3) . ? B12 B13 1.766(6) . ? B12 H12C 1.11(3) . ? B13 H13C 1.11(3) . ? C11 C16 1.389(4) . ? C11 C12 1.398(4) . ? C12 C13 1.386(5) . ? C12 H12 0.9500 . ? C13 C14 1.385(5) . ? C13 H13 0.9500 . ? C14 C15 1.380(5) . ? C14 H14 0.9500 . ? C15 C16 1.383(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C41 C42 1.407(5) . ? C41 C45 1.414(5) . ? C41 H41 0.9500 . ? C42 C43 1.402(5) . ? C42 H42 0.9500 . ? C43 C44 1.404(5) . ? C43 H43 0.9500 . ? C44 C45 1.408(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C61 C66 1.394(4) . ? C61 C62 1.395(4) . ? C62 C63 1.388(5) . ? C62 H62 0.9500 . ? C63 C64 1.378(5) . ? C63 H63 0.9500 . ? C64 C65 1.371(4) . ? C64 H64 0.9500 . ? C65 C66 1.382(5) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? 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 C45 Co4 C41 40.71(14) . . ? C45 Co4 C1 112.67(15) . . ? C41 Co4 C1 153.23(15) . . ? C45 Co4 C42 67.78(15) . . ? C41 Co4 C42 40.40(14) . . ? C1 Co4 C42 148.17(14) . . ? C45 Co4 C44 40.21(14) . . ? C41 Co4 C44 67.56(15) . . ? C1 Co4 C44 92.83(14) . . ? C42 Co4 C44 66.75(15) . . ? C45 Co4 C43 67.47(14) . . ? C41 Co4 C43 67.55(14) . . ? C1 Co4 C43 109.28(14) . . ? C42 Co4 C43 39.74(14) . . ? C44 Co4 C43 39.56(13) . . ? C45 Co4 B10 121.17(16) . . ? C41 Co4 B10 89.85(16) . . ? C1 Co4 B10 108.83(15) . . ? C42 Co4 B10 95.76(16) . . ? C44 Co4 B10 157.39(16) . . ? C43 Co4 B10 131.70(16) . . ? C45 Co4 B7 93.67(15) . . ? C41 Co4 B7 91.60(15) . . ? C1 Co4 B7 86.92(14) . . ? C42 Co4 B7 124.85(15) . . ? C44 Co4 B7 128.86(15) . . ? C43 Co4 B7 158.55(15) . . ? B10 Co4 B7 49.06(16) . . ? C45 Co4 C6 162.29(14) . . ? C41 Co4 C6 121.59(14) . . ? C1 Co4 C6 84.93(13) . . ? C42 Co4 C6 98.55(14) . . ? C44 Co4 C6 145.99(13) . . ? C43 Co4 C6 109.74(13) . . ? B10 Co4 C6 46.59(14) . . ? B7 Co4 C6 84.98(14) . . ? C45 Co4 B2 149.72(15) . . ? C41 Co4 B2 162.12(15) . . ? C1 Co4 B2 42.29(13) . . ? C42 Co4 B2 122.32(15) . . ? C44 Co4 B2 113.48(15) . . ? C43 Co4 B2 101.38(15) . . ? B10 Co4 B2 87.68(16) . . ? B7 Co4 B2 100.07(15) . . ? C6 Co4 B2 47.11(13) . . ? C45 Co4 B3 93.22(16) . . ? C41 Co4 B3 121.24(16) . . ? C1 Co4 B3 42.81(14) . . ? C42 Co4 B3 160.42(16) . . ? C44 Co4 B3 102.17(16) . . ? C43 Co4 B3 138.23(15) . . ? B10 Co4 B3 90.06(16) . . ? B7 Co4 B3 48.70(15) . . ? C6 Co4 B3 99.02(14) . . ? B2 Co4 B3 76.49(15) . . ? C11 C1 B2 117.5(3) . . ? C11 C1 B3 118.9(3) . . ? B2 C1 B3 123.4(3) . . ? C11 C1 B5 120.6(3) . . ? B2 C1 B5 73.6(2) . . ? B3 C1 B5 74.9(2) . . ? C11 C1 Co4 129.5(2) . . ? B2 C1 Co4 74.24(19) . . ? B3 C1 Co4 74.1(2) . . ? B5 C1 Co4 109.9(2) . . ? C1 B2 C6 120.7(3) . . ? C1 B2 B9 117.1(3) . . ? C6 B2 B9 57.5(2) . . ? C1 B2 B5 58.7(2) . . ? C6 B2 B5 99.2(2) . . ? B9 B2 B5 60.2(2) . . ? C1 B2 Co4 63.47(19) . . ? C6 B2 Co4 66.30(16) . . ? B9 B2 Co4 111.3(2) . . ? B5 B2 Co4 96.5(2) . . ? C1 B2 H2C 118.0(15) . . ? C6 B2 H2C 118.3(15) . . ? B9 B2 H2C 109.1(16) . . ? B5 B2 H2C 127.0(15) . . ? Co4 B2 H2C 131.4(15) . . ? C1 B3 B8 114.7(3) . . ? C1 B3 B7 119.6(3) . . ? B8 B3 B7 58.3(2) . . ? C1 B3 B5 57.5(2) . . ? B8 B3 B5 59.2(2) . . ? B7 B3 B5 99.5(3) . . ? C1 B3 Co4 63.14(18) . . ? B8 B3 Co4 109.5(3) . . ? B7 B3 Co4 65.26(18) . . ? B5 B3 Co4 95.2(2) . . ? C1 B3 H3C 115.8(17) . . ? B8 B3 H3C 117.8(17) . . ? B7 B3 H3C 118.1(17) . . ? B5 B3 H3C 133.3(17) . . ? Co4 B3 H3C 124.3(17) . . ? C1 B5 B11 133.6(3) . . ? C1 B5 B8 100.2(3) . . ? B11 B5 B8 56.0(2) . . ? C1 B5 B9 101.1(3) . . ? B11 B5 B9 56.2(2) . . ? B8 B5 B9 103.0(3) . . ? C1 B5 B2 47.67(18) . . ? B11 B5 B2 104.5(3) . . ? B8 B5 B2 117.8(3) . . ? B9 B5 B2 54.8(2) . . ? C1 B5 B3 47.64(18) . . ? B11 B5 B3 104.3(3) . . ? B8 B5 B3 54.1(2) . . ? B9 B5 B3 119.1(3) . . ? B2 B5 B3 85.1(2) . . ? C1 B5 H5C 109.4(17) . . ? B11 B5 H5C 117.0(17) . . ? B8 B5 H5C 121.6(17) . . ? B9 B5 H5C 118.3(17) . . ? B2 B5 H5C 119.4(17) . . ? B3 B5 H5C 121.2(17) . . ? C61 C6 B9 120.8(3) . . ? C61 C6 B10 116.5(3) . . ? B9 C6 B10 111.5(3) . . ? C61 C6 B12 115.4(3) . . ? B9 C6 B12 60.4(2) . . ? B10 C6 B12 63.4(2) . . ? C61 C6 B2 114.9(3) . . ? B9 C6 B2 62.5(2) . . ? B10 C6 B2 119.8(3) . . ? B12 C6 B2 117.0(3) . . ? C61 C6 Co4 115.2(2) . . ? B9 C6 Co4 115.3(2) . . ? B10 C6 Co4 64.75(18) . . ? B12 C6 Co4 118.9(2) . . ? B2 C6 Co4 66.59(18) . . ? B13 B7 B8 60.3(2) . . ? B13 B7 B10 60.8(2) . . ? B8 B7 B10 107.2(3) . . ? B13 B7 B3 114.7(3) . . ? B8 B7 B3 60.4(2) . . ? B10 B7 B3 116.5(3) . . ? B13 B7 Co4 115.7(2) . . ? B8 B7 Co4 111.7(2) . . ? B10 B7 Co4 63.74(17) . . ? B3 B7 Co4 66.04(17) . . ? B13 B7 H7C 120.3(16) . . ? B8 B7 H7C 124.1(16) . . ? B10 B7 H7C 120.5(16) . . ? B3 B7 H7C 113.9(16) . . ? Co4 B7 H7C 114.3(16) . . ? B11 B8 B13 61.3(2) . . ? B11 B8 B7 108.2(3) . . ? B13 B8 B7 59.2(2) . . ? B11 B8 B3 118.3(3) . . ? B13 B8 B3 114.6(3) . . ? B7 B8 B3 61.4(2) . . ? B11 B8 B5 59.2(2) . . ? B13 B8 B5 107.6(3) . . ? B7 B8 B5 106.8(3) . . ? B3 B8 B5 66.7(2) . . ? B11 B8 H8C 117.8(17) . . ? B13 B8 H8C 122.3(17) . . ? B7 B8 H8C 126.1(17) . . ? B3 B8 H8C 113.3(17) . . ? B5 B8 H8C 119.8(17) . . ? C6 B9 B12 59.9(2) . . ? C6 B9 B11 106.4(3) . . ? B12 B9 B11 61.3(2) . . ? C6 B9 B2 60.0(2) . . ? B12 B9 B2 114.4(3) . . ? B11 B9 B2 115.9(3) . . ? C6 B9 B5 104.3(3) . . ? B12 B9 B5 108.1(3) . . ? B11 B9 B5 59.0(2) . . ? B2 B9 B5 65.0(2) . . ? C6 B9 H9C 121.5(16) . . ? B12 B9 H9C 118.8(16) . . ? B11 B9 H9C 123.5(16) . . ? B2 B9 H9C 113.2(16) . . ? B5 B9 H9C 125.8(16) . . ? C6 B10 B13 107.4(3) . . ? C6 B10 B7 115.3(3) . . ? B13 B10 B7 57.9(2) . . ? C6 B10 B12 58.4(2) . . ? B13 B10 B12 59.2(2) . . ? B7 B10 B12 108.2(3) . . ? C6 B10 Co4 68.66(18) . . ? B13 B10 Co4 116.2(3) . . ? B7 B10 Co4 67.20(19) . . ? B12 B10 Co4 118.1(3) . . ? C6 B10 H10C 116.6(16) . . ? B13 B10 H10C 123.4(16) . . ? B7 B10 H10C 122.7(17) . . ? B12 B10 H10C 118.7(17) . . ? Co4 B10 H10C 112.0(16) . . ? B8 B11 B9 117.1(3) . . ? B8 B11 B12 110.3(3) . . ? B9 B11 B12 58.5(2) . . ? B8 B11 B13 59.6(2) . . ? B9 B11 B13 108.8(3) . . ? B12 B11 B13 59.8(2) . . ? B8 B11 B5 64.8(2) . . ? B9 B11 B5 64.8(2) . . ? B12 B11 B5 110.5(3) . . ? B13 B11 B5 110.5(3) . . ? B8 B11 H11C 120.8(17) . . ? B9 B11 H11C 113.6(16) . . ? B12 B11 H11C 121.2(17) . . ? B13 B11 H11C 126.7(16) . . ? B5 B11 H11C 115.9(16) . . ? C6 B12 B9 59.7(2) . . ? C6 B12 B13 108.1(3) . . ? B9 B12 B13 110.9(3) . . ? C6 B12 B11 105.5(3) . . ? B9 B12 B11 60.3(2) . . ? B13 B12 B11 60.5(2) . . ? C6 B12 B10 58.3(2) . . ? B9 B12 B10 106.9(3) . . ? B13 B12 B10 60.0(2) . . ? B11 B12 B10 105.1(3) . . ? C6 B12 H12C 118.7(16) . . ? B9 B12 H12C 117.3(16) . . ? B13 B12 H12C 124.6(16) . . ? B11 B12 H12C 125.7(16) . . ? B10 B12 H12C 124.0(16) . . ? B7 B13 B8 60.5(2) . . ? B7 B13 B12 112.4(3) . . ? B8 B13 B12 110.0(3) . . ? B7 B13 B11 107.5(3) . . ? B8 B13 B11 59.1(2) . . ? B12 B13 B11 59.8(2) . . ? B7 B13 B10 61.3(2) . . ? B8 B13 B10 107.8(3) . . ? B12 B13 B10 60.7(2) . . ? B11 B13 B10 105.1(3) . . ? B7 B13 H13C 121.4(16) . . ? B8 B13 H13C 122.7(16) . . ? B12 B13 H13C 117.4(16) . . ? B11 B13 H13C 123.1(16) . . ? B10 B13 H13C 122.4(17) . . ? C16 C11 C12 117.7(3) . . ? C16 C11 C1 120.0(3) . . ? C12 C11 C1 122.3(3) . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 120.3(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 121.7(3) . . ? C15 C16 H16 119.1 . . ? C11 C16 H16 119.1 . . ? C42 C41 C45 107.3(3) . . ? C42 C41 Co4 70.1(2) . . ? C45 C41 Co4 69.6(2) . . ? C42 C41 H41 126.4 . . ? C45 C41 H41 126.4 . . ? Co4 C41 H41 125.5 . . ? C43 C42 C41 109.1(4) . . ? C43 C42 Co4 71.7(2) . . ? C41 C42 Co4 69.5(2) . . ? C43 C42 H42 125.5 . . ? C41 C42 H42 125.5 . . ? Co4 C42 H42 125.0 . . ? C42 C43 C44 107.3(3) . . ? C42 C43 Co4 68.6(2) . . ? C44 C43 Co4 69.6(2) . . ? C42 C43 H43 126.4 . . ? C44 C43 H43 126.4 . . ? Co4 C43 H43 127.0 . . ? C43 C44 C45 108.7(3) . . ? C43 C44 Co4 70.8(2) . . ? C45 C44 Co4 68.6(2) . . ? C43 C44 H44 125.7 . . ? C45 C44 H44 125.7 . . ? Co4 C44 H44 126.5 . . ? C44 C45 C41 107.7(3) . . ? C44 C45 Co4 71.2(2) . . ? C41 C45 Co4 69.7(2) . . ? C44 C45 H45 126.1 . . ? C41 C45 H45 126.1 . . ? Co4 C45 H45 124.5 . . ? C66 C61 C62 116.8(3) . . ? C66 C61 C6 120.9(3) . . ? C62 C61 C6 122.2(3) . . ? C63 C62 C61 121.6(3) . . ? C63 C62 H62 119.2 . . ? C61 C62 H62 119.2 . . ? C64 C63 C62 120.0(3) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C65 C64 C63 119.6(3) . . ? C65 C64 H64 120.2 . . ? C63 C64 H64 120.2 . . ? C64 C65 C66 120.5(3) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C65 C66 C61 121.5(3) . . ? C65 C66 H66 119.3 . . ? C61 C66 H66 119.3 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.267 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.063 #===end data_4x81178 _database_code_depnum_ccdc_archive 'CCDC 631514' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H25 B10 Co, 0.5(C6 H14)' _chemical_formula_sum 'C22 H32 B10 Co' _chemical_formula_weight 463.51 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.782(3) _cell_length_b 19.357(7) _cell_length_c 15.252(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.266(16) _cell_angle_gamma 90.00 _cell_volume 2543.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1428 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 20.36 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.572 _exptl_absorpt_correction_T_max 0.908 _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20710 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 20.68 _reflns_number_total 2566 _reflns_number_gt 2006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1117P)^2^+12.5635P] 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 2566 _refine_ls_number_parameters 345 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2278 _refine_ls_wR_factor_gt 0.2108 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.167 _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 Co4 Co 0.41208(13) 0.28212(6) 0.77485(7) 0.0282(5) Uani 1 1 d . . . C1 C 0.4047(9) 0.3122(4) 0.9033(5) 0.023(2) Uani 1 1 d U . . B2 B 0.3933(12) 0.2340(6) 0.9015(6) 0.029(3) Uani 1 1 d . . . H2C H 0.484(9) 0.203(4) 0.940(6) 0.035 Uiso 1 1 d . . . B3 B 0.2934(11) 0.3608(6) 0.8389(6) 0.022(2) Uani 1 1 d . . . H3C H 0.317(8) 0.414(4) 0.844(5) 0.027 Uiso 1 1 d . . . B5 B 0.2231(12) 0.2983(5) 0.9231(6) 0.028(3) Uani 1 1 d . . . H5C H 0.217(8) 0.326(4) 0.991(5) 0.034 Uiso 1 1 d . . . B6 B 0.2901(13) 0.1877(6) 0.8045(7) 0.033(3) Uani 1 1 d . . . H6C H 0.342(9) 0.136(4) 0.795(5) 0.040 Uiso 1 1 d . . . B7 B 0.1921(11) 0.3274(6) 0.7312(6) 0.026(3) Uani 1 1 d U . . H7C H 0.178(8) 0.367(4) 0.684(5) 0.032 Uiso 1 1 d . . . C8 C 0.1036(9) 0.3394(4) 0.8209(5) 0.023(2) Uani 1 1 d . . . B9 B 0.1978(13) 0.2045(6) 0.8940(7) 0.037(3) Uani 1 1 d . . . H9C H 0.187(10) 0.168(5) 0.934(6) 0.044 Uiso 1 1 d . . . B10 B 0.1916(12) 0.2384(6) 0.7123(7) 0.030(3) Uani 1 1 d . . . H10C H 0.191(9) 0.219(4) 0.647(6) 0.036 Uiso 1 1 d . . . B11 B 0.0476(12) 0.2618(5) 0.8593(6) 0.027(3) Uani 1 1 d . . . H11C H -0.054(9) 0.264(4) 0.886(5) 0.033 Uiso 1 1 d . . . B12 B 0.0308(13) 0.2787(5) 0.7417(7) 0.031(3) Uani 1 1 d . . . H12C H -0.078(10) 0.289(4) 0.705(6) 0.037 Uiso 1 1 d . . . B13 B 0.0878(13) 0.1962(6) 0.7868(7) 0.038(3) Uani 1 1 d . . . H13C H 0.009(9) 0.151(4) 0.766(5) 0.045 Uiso 1 1 d . . . C11 C 0.5264(9) 0.3464(4) 0.9752(5) 0.022(2) Uani 1 1 d . . . C12 C 0.6709(10) 0.3165(5) 1.0021(5) 0.030(2) Uani 1 1 d . . . H12 H 0.6967 0.2756 0.9738 0.036 Uiso 1 1 calc R . . C13 C 0.7804(10) 0.3469(5) 1.0722(5) 0.033(2) Uani 1 1 d . . . H13 H 0.8805 0.3270 1.0902 0.039 Uiso 1 1 calc R . . C14 C 0.7408(11) 0.4056(5) 1.1140(5) 0.034(2) Uani 1 1 d . . . H14 H 0.8140 0.4260 1.1609 0.041 Uiso 1 1 calc R . . C15 C 0.5963(11) 0.4347(5) 1.0883(5) 0.033(2) Uani 1 1 d . . . H15 H 0.5688 0.4746 1.1180 0.040 Uiso 1 1 calc R . . C16 C 0.4891(10) 0.4049(4) 1.0173(5) 0.025(2) Uani 1 1 d . . . H16 H 0.3899 0.4255 0.9986 0.030 Uiso 1 1 calc R . . C41 C 0.6314(11) 0.2449(5) 0.7693(6) 0.039(2) Uani 1 1 d . . . H41 H 0.6892 0.2117 0.8080 0.047 Uiso 1 1 calc R . . C42 C 0.6369(11) 0.3179(5) 0.7811(6) 0.042(3) Uani 1 1 d . . . H42 H 0.6997 0.3415 0.8297 0.050 Uiso 1 1 calc R . . C43 C 0.5360(10) 0.3494(5) 0.7102(5) 0.034(2) Uani 1 1 d . . . H43 H 0.5176 0.3976 0.7019 0.041 Uiso 1 1 calc R . . C44 C 0.4661(11) 0.2953(6) 0.6529(6) 0.041(3) Uani 1 1 d . . . H44 H 0.3925 0.3010 0.5988 0.049 Uiso 1 1 calc R . . C45 C 0.5256(11) 0.2311(5) 0.6907(6) 0.042(3) Uani 1 1 d . . . H45 H 0.4978 0.1867 0.6664 0.050 Uiso 1 1 calc R . . C81 C 0.0013(9) 0.4007(4) 0.8274(5) 0.028(2) Uani 1 1 d . . . C82 C -0.0543(10) 0.4424(5) 0.7512(6) 0.037(2) Uani 1 1 d . . . H82 H -0.0260 0.4314 0.6958 0.045 Uiso 1 1 calc R . . C83 C -0.1477(11) 0.4980(5) 0.7564(6) 0.041(3) Uani 1 1 d . . . H83 H -0.1827 0.5256 0.7049 0.049 Uiso 1 1 calc R . . C84 C -0.1923(11) 0.5147(5) 0.8372(6) 0.038(2) Uani 1 1 d . . . H84 H -0.2577 0.5532 0.8409 0.046 Uiso 1 1 calc R . . C85 C -0.1394(11) 0.4741(5) 0.9112(6) 0.038(2) Uani 1 1 d . . . H85 H -0.1706 0.4844 0.9660 0.046 Uiso 1 1 calc R . . C86 C -0.0423(10) 0.4188(5) 0.9071(5) 0.030(2) Uani 1 1 d . . . H86 H -0.0046 0.3927 0.9596 0.036 Uiso 1 1 calc R . . C1S C 0.157(3) 0.6156(14) 0.5088(15) 0.178(10) Uani 1 1 d . . . C2S C 0.382(7) 0.527(3) 0.568(3) 0.079(15) Uani 0.25 1 d PU . . C3S C 0.066(5) 0.506(3) 0.524(3) 0.073(14) Uani 0.25 1 d PU . . C4S C 0.292(5) 0.5419(13) 0.648(2) 0.29(2) Uani 1 1 d . . . C5S C 0.252(13) 0.546(6) 0.523(8) 0.19(4) Uiso 0.25 1 d P . . C6S C 0.519(11) 0.502(5) 0.470(5) 0.15(3) Uiso 0.25 1 d P . . 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 Co4 0.0309(8) 0.0404(9) 0.0132(8) -0.0095(6) 0.0036(5) -0.0018(6) C1 0.028(5) 0.032(5) 0.007(4) -0.010(4) 0.002(3) -0.005(4) B2 0.034(6) 0.038(7) 0.015(5) -0.007(5) 0.004(5) -0.002(5) B3 0.030(6) 0.033(7) 0.004(5) -0.004(5) 0.004(4) -0.001(5) B5 0.040(7) 0.034(7) 0.008(5) 0.004(5) 0.001(5) -0.002(5) B6 0.045(7) 0.028(6) 0.023(6) -0.007(5) -0.007(5) 0.006(5) B7 0.039(6) 0.035(6) 0.006(5) -0.002(4) 0.005(4) -0.002(5) C8 0.035(5) 0.028(5) 0.003(4) -0.002(4) -0.003(4) 0.000(4) B9 0.048(7) 0.034(7) 0.027(7) 0.001(5) 0.004(5) 0.005(6) B10 0.033(6) 0.044(7) 0.013(6) -0.008(5) 0.003(5) -0.001(5) B11 0.029(6) 0.039(7) 0.011(5) -0.005(5) -0.002(5) -0.005(5) B12 0.033(6) 0.035(7) 0.022(6) -0.009(5) 0.002(5) -0.001(5) B13 0.044(7) 0.042(7) 0.022(6) -0.002(5) -0.004(5) -0.007(6) C11 0.028(5) 0.026(5) 0.009(4) 0.004(4) -0.004(4) 0.001(4) C12 0.046(6) 0.030(5) 0.013(5) 0.001(4) 0.004(4) -0.003(5) C13 0.039(6) 0.045(6) 0.012(5) 0.010(5) 0.000(4) -0.002(5) C14 0.050(7) 0.038(6) 0.010(5) -0.001(5) -0.006(4) -0.009(5) C15 0.054(7) 0.029(5) 0.011(5) 0.002(4) -0.004(5) -0.001(5) C16 0.040(5) 0.024(5) 0.009(5) 0.005(4) 0.001(4) 0.002(4) C41 0.039(6) 0.049(7) 0.028(6) -0.016(5) 0.005(5) 0.002(5) C42 0.040(6) 0.060(8) 0.026(6) -0.004(5) 0.008(5) -0.007(5) C43 0.044(6) 0.044(6) 0.016(5) -0.001(5) 0.010(5) -0.002(5) C44 0.038(6) 0.075(8) 0.015(5) -0.008(6) 0.016(4) -0.006(6) C45 0.051(6) 0.051(7) 0.027(6) -0.032(6) 0.014(5) -0.008(5) C81 0.028(5) 0.032(5) 0.023(5) -0.004(4) 0.003(4) -0.002(4) C82 0.045(6) 0.042(6) 0.025(6) 0.004(5) 0.008(5) 0.007(5) C83 0.058(7) 0.040(6) 0.023(6) 0.003(5) 0.001(5) 0.014(6) C84 0.051(6) 0.044(6) 0.020(5) 0.003(5) 0.006(5) 0.010(5) C85 0.051(6) 0.043(6) 0.024(6) -0.005(5) 0.015(5) 0.001(5) C86 0.040(6) 0.038(6) 0.013(5) -0.003(4) 0.003(4) 0.006(5) C1S 0.155(19) 0.21(2) 0.146(19) -0.073(18) -0.012(15) 0.019(17) C2S 0.09(2) 0.09(2) 0.06(2) 0.013(17) 0.005(17) 0.003(18) C3S 0.07(2) 0.09(2) 0.06(2) 0.012(17) 0.021(17) 0.014(18) C4S 0.52(5) 0.14(2) 0.29(4) -0.08(2) 0.29(4) -0.12(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 Co4 C44 2.024(8) . ? Co4 C45 2.029(9) . ? Co4 C1 2.058(7) . ? Co4 C43 2.067(9) . ? Co4 C41 2.073(9) . ? Co4 C42 2.077(9) . ? Co4 B7 2.108(10) . ? Co4 B10 2.158(10) . ? Co4 B2 2.180(10) . ? Co4 B3 2.181(10) . ? Co4 B6 2.210(12) . ? C1 B2 1.518(14) . ? C1 C11 1.525(11) . ? C1 B3 1.559(13) . ? C1 B5 1.702(13) . ? B2 B9 1.791(16) . ? B2 B6 1.815(14) . ? B2 B5 2.021(14) . ? B2 H2C 1.08(8) . ? B3 C8 1.687(13) . ? B3 B7 1.826(12) . ? B3 B5 1.951(13) . ? B3 H3C 1.06(8) . ? B5 B11 1.798(14) . ? B5 B9 1.871(15) . ? B5 C8 1.877(12) . ? B5 H5C 1.18(8) . ? B6 B9 1.749(15) . ? B6 B13 1.751(16) . ? B6 B10 1.792(15) . ? B6 H6C 1.11(8) . ? B7 C8 1.716(12) . ? B7 B12 1.735(15) . ? B7 B10 1.748(15) . ? B7 H7C 1.05(8) . ? C8 C81 1.503(12) . ? C8 B12 1.717(13) . ? C8 B11 1.719(13) . ? B9 B11 1.724(15) . ? B9 B13 1.736(15) . ? B9 H9C 0.95(9) . ? B10 B12 1.747(15) . ? B10 B13 1.786(15) . ? B10 H10C 1.06(9) . ? B11 B13 1.765(15) . ? B11 B12 1.801(14) . ? B11 H11C 1.06(8) . ? B12 B13 1.772(16) . ? B12 H12C 1.03(8) . ? B13 H13C 1.12(9) . ? C11 C16 1.372(11) . ? C11 C12 1.382(11) . ? C12 C13 1.418(12) . ? C12 H12 0.9500 . ? C13 C14 1.380(12) . ? C13 H13 0.9500 . ? C14 C15 1.374(12) . ? C14 H14 0.9500 . ? C15 C16 1.412(11) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C41 C45 1.392(13) . ? C41 C42 1.424(13) . ? C41 H41 0.9500 . ? C42 C43 1.397(13) . ? C42 H42 0.9500 . ? C43 C44 1.424(13) . ? C43 H43 0.9500 . ? C44 C45 1.425(13) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C81 C86 1.389(12) . ? C81 C82 1.422(12) . ? C82 C83 1.365(12) . ? C82 H82 0.9500 . ? C83 C84 1.401(12) . ? C83 H83 0.9500 . ? C84 C85 1.379(12) . ? C84 H84 0.9500 . ? C85 C86 1.377(12) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? 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 C44 Co4 C45 41.2(4) . . ? C44 Co4 C1 153.7(4) . . ? C45 Co4 C1 148.4(4) . . ? C44 Co4 C43 40.7(4) . . ? C45 Co4 C43 68.6(4) . . ? C1 Co4 C43 113.2(3) . . ? C44 Co4 C41 67.7(4) . . ? C45 Co4 C41 39.7(4) . . ? C1 Co4 C41 109.9(3) . . ? C43 Co4 C41 67.7(4) . . ? C44 Co4 C42 67.0(4) . . ? C45 Co4 C42 67.1(4) . . ? C1 Co4 C42 93.9(3) . . ? C43 Co4 C42 39.4(4) . . ? C41 Co4 C42 40.1(4) . . ? C44 Co4 B7 91.3(4) . . ? C45 Co4 B7 122.4(4) . . ? C1 Co4 B7 89.2(3) . . ? C43 Co4 B7 97.0(4) . . ? C41 Co4 B7 158.9(4) . . ? C42 Co4 B7 132.9(4) . . ? C44 Co4 B10 89.7(4) . . ? C45 Co4 B10 92.2(4) . . ? C1 Co4 B10 109.8(3) . . ? C43 Co4 B10 123.2(4) . . ? C41 Co4 B10 127.3(4) . . ? C42 Co4 B10 156.1(4) . . ? B7 Co4 B10 48.4(4) . . ? C44 Co4 B2 160.1(4) . . ? C45 Co4 B2 119.0(4) . . ? C1 Co4 B2 41.8(4) . . ? C43 Co4 B2 146.1(4) . . ? C41 Co4 B2 96.8(4) . . ? C42 Co4 B2 109.7(4) . . ? B7 Co4 B2 103.6(4) . . ? B10 Co4 B2 90.4(4) . . ? C44 Co4 B3 122.8(4) . . ? C45 Co4 B3 163.7(4) . . ? C1 Co4 B3 43.0(3) . . ? C43 Co4 B3 96.6(4) . . ? C41 Co4 B3 142.2(4) . . ? C42 Co4 B3 106.3(4) . . ? B7 Co4 B3 50.4(3) . . ? B10 Co4 B3 90.3(4) . . ? B2 Co4 B3 77.1(4) . . ? C44 Co4 B6 120.2(4) . . ? C45 Co4 B6 92.6(4) . . ? C1 Co4 B6 86.1(4) . . ? C43 Co4 B6 160.1(4) . . ? C41 Co4 B6 102.3(4) . . ? C42 Co4 B6 139.6(4) . . ? B7 Co4 B6 87.6(4) . . ? B10 Co4 B6 48.4(4) . . ? B2 Co4 B6 48.8(4) . . ? B3 Co4 B6 101.1(4) . . ? B2 C1 C11 118.7(7) . . ? B2 C1 B3 124.0(7) . . ? C11 C1 B3 117.2(7) . . ? B2 C1 B5 77.5(6) . . ? C11 C1 B5 119.4(6) . . ? B3 C1 B5 73.4(6) . . ? B2 C1 Co4 73.4(5) . . ? C11 C1 Co4 131.2(5) . . ? B3 C1 Co4 72.7(4) . . ? B5 C1 Co4 109.2(5) . . ? C1 B2 B9 112.2(8) . . ? C1 B2 B6 121.9(8) . . ? B9 B2 B6 58.0(6) . . ? C1 B2 B5 55.3(5) . . ? B9 B2 B5 58.4(5) . . ? B6 B2 B5 99.7(7) . . ? C1 B2 Co4 64.7(5) . . ? B9 B2 Co4 108.4(6) . . ? B6 B2 Co4 66.4(5) . . ? B5 B2 Co4 93.9(5) . . ? C1 B2 H2C 121(4) . . ? B9 B2 H2C 117(4) . . ? B6 B2 H2C 111(4) . . ? B5 B2 H2C 138(4) . . ? Co4 B2 H2C 123(4) . . ? C1 B3 C8 115.6(7) . . ? C1 B3 B7 119.3(8) . . ? C8 B3 B7 58.3(5) . . ? C1 B3 B5 56.7(5) . . ? C8 B3 B5 61.6(5) . . ? B7 B3 B5 102.2(7) . . ? C1 B3 Co4 64.3(4) . . ? C8 B3 Co4 107.4(6) . . ? B7 B3 Co4 62.7(4) . . ? B5 B3 Co4 95.9(5) . . ? C1 B3 H3C 117(4) . . ? C8 B3 H3C 115(4) . . ? B7 B3 H3C 118(4) . . ? B5 B3 H3C 130(4) . . ? Co4 B3 H3C 128(4) . . ? C1 B5 B11 134.4(7) . . ? C1 B5 B9 100.6(7) . . ? B11 B5 B9 56.0(6) . . ? C1 B5 C8 100.2(6) . . ? B11 B5 C8 55.7(5) . . ? B9 B5 C8 101.1(6) . . ? C1 B5 B3 50.0(5) . . ? B11 B5 B3 103.6(6) . . ? B9 B5 B3 118.9(7) . . ? C8 B5 B3 52.2(5) . . ? C1 B5 B2 47.2(5) . . ? B11 B5 B2 104.7(7) . . ? B9 B5 B2 54.6(5) . . ? C8 B5 B2 115.9(6) . . ? B3 B5 B2 86.3(6) . . ? C1 B5 H5C 107(4) . . ? B11 B5 H5C 118(4) . . ? B9 B5 H5C 129(4) . . ? C8 B5 H5C 115(4) . . ? B3 B5 H5C 112(4) . . ? B2 B5 H5C 126(4) . . ? B9 B6 B13 59.5(6) . . ? B9 B6 B10 106.5(8) . . ? B13 B6 B10 60.5(6) . . ? B9 B6 B2 60.3(6) . . ? B13 B6 B2 114.2(8) . . ? B10 B6 B2 117.2(8) . . ? B9 B6 Co4 108.8(7) . . ? B13 B6 Co4 114.1(7) . . ? B10 B6 Co4 64.3(5) . . ? B2 B6 Co4 64.7(5) . . ? B9 B6 H6C 122(4) . . ? B13 B6 H6C 119(4) . . ? B10 B6 H6C 122(4) . . ? B2 B6 H6C 113(4) . . ? Co4 B6 H6C 119(4) . . ? C8 B7 B12 59.7(5) . . ? C8 B7 B10 106.1(7) . . ? B12 B7 B10 60.2(6) . . ? C8 B7 B3 56.8(5) . . ? B12 B7 B3 111.9(7) . . ? B10 B7 B3 118.8(8) . . ? C8 B7 Co4 109.5(6) . . ? B12 B7 Co4 117.3(7) . . ? B10 B7 Co4 67.3(5) . . ? B3 B7 Co4 66.9(4) . . ? C8 B7 H7C 116(4) . . ? B12 B7 H7C 119(4) . . ? B10 B7 H7C 128(4) . . ? B3 B7 H7C 109(4) . . ? Co4 B7 H7C 120(4) . . ? C81 C8 B3 112.3(7) . . ? C81 C8 B7 121.9(7) . . ? B3 C8 B7 64.9(5) . . ? C81 C8 B12 116.2(7) . . ? B3 C8 B12 120.2(7) . . ? B7 C8 B12 60.7(6) . . ? C81 C8 B11 116.9(7) . . ? B3 C8 B11 119.9(7) . . ? B7 C8 B11 111.0(7) . . ? B12 C8 B11 63.2(5) . . ? C81 C8 B5 121.6(6) . . ? B3 C8 B5 66.1(5) . . ? B7 C8 B5 109.8(6) . . ? B12 C8 B5 111.4(6) . . ? B11 C8 B5 59.8(5) . . ? B11 B9 B13 61.3(6) . . ? B11 B9 B6 108.9(8) . . ? B13 B9 B6 60.3(6) . . ? B11 B9 B2 118.8(8) . . ? B13 B9 B2 116.1(8) . . ? B6 B9 B2 61.7(6) . . ? B11 B9 B5 59.9(6) . . ? B13 B9 B5 109.4(8) . . ? B6 B9 B5 108.4(8) . . ? B2 B9 B5 67.0(6) . . ? B11 B9 H9C 121(5) . . ? B13 B9 H9C 115(5) . . ? B6 B9 H9C 119(5) . . ? B2 B9 H9C 114(5) . . ? B5 B9 H9C 127(5) . . ? B12 B10 B7 59.5(6) . . ? B12 B10 B13 60.2(6) . . ? B7 B10 B13 109.3(7) . . ? B12 B10 B6 109.5(7) . . ? B7 B10 B6 115.2(7) . . ? B13 B10 B6 58.6(6) . . ? B12 B10 Co4 114.3(6) . . ? B7 B10 Co4 64.3(5) . . ? B13 B10 Co4 115.1(6) . . ? B6 B10 Co4 67.3(5) . . ? B12 B10 H10C 123(4) . . ? B7 B10 H10C 120(4) . . ? B13 B10 H10C 122(4) . . ? B6 B10 H10C 117(4) . . ? Co4 B10 H10C 113(4) . . ? C8 B11 B9 114.4(8) . . ? C8 B11 B13 108.1(7) . . ? B9 B11 B13 59.7(6) . . ? C8 B11 B5 64.5(5) . . ? B9 B11 B5 64.1(6) . . ? B13 B11 B5 111.5(8) . . ? C8 B11 B12 58.3(5) . . ? B9 B11 B12 109.3(8) . . ? B13 B11 B12 59.6(6) . . ? B5 B11 B12 111.3(7) . . ? C8 B11 H11C 114(4) . . ? B9 B11 H11C 125(4) . . ? B13 B11 H11C 125(4) . . ? B5 B11 H11C 118(4) . . ? B12 B11 H11C 118(4) . . ? C8 B12 B7 59.6(5) . . ? C8 B12 B10 106.1(7) . . ? B7 B12 B10 60.3(6) . . ? C8 B12 B13 107.8(7) . . ? B7 B12 B13 110.6(8) . . ? B10 B12 B13 61.0(6) . . ? C8 B12 B11 58.4(5) . . ? B7 B12 B11 106.3(7) . . ? B10 B12 B11 105.1(7) . . ? B13 B12 B11 59.2(6) . . ? C8 B12 H12C 115(4) . . ? B7 B12 H12C 122(5) . . ? B10 B12 H12C 131(5) . . ? B13 B12 H12C 123(4) . . ? B11 B12 H12C 118(5) . . ? B9 B13 B6 60.2(6) . . ? B9 B13 B11 59.0(6) . . ? B6 B13 B11 107.0(7) . . ? B9 B13 B12 110.1(8) . . ? B6 B13 B12 110.2(8) . . ? B11 B13 B12 61.2(6) . . ? B9 B13 B10 107.3(8) . . ? B6 B13 B10 60.9(6) . . ? B11 B13 B10 105.0(8) . . ? B12 B13 B10 58.8(6) . . ? B9 B13 H13C 123(4) . . ? B6 B13 H13C 122(4) . . ? B11 B13 H13C 123(4) . . ? B12 B13 H13C 118(4) . . ? B10 B13 H13C 122(4) . . ? C16 C11 C12 119.7(7) . . ? C16 C11 C1 119.8(7) . . ? C12 C11 C1 120.4(7) . . ? C11 C12 C13 119.9(8) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 119.6(8) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.5(8) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.4(8) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C11 C16 C15 120.8(8) . . ? C11 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C45 C41 C42 107.4(9) . . ? C45 C41 Co4 68.4(5) . . ? C42 C41 Co4 70.1(5) . . ? C45 C41 H41 126.3 . . ? C42 C41 H41 126.3 . . ? Co4 C41 H41 126.7 . . ? C43 C42 C41 109.6(8) . . ? C43 C42 Co4 69.9(5) . . ? C41 C42 Co4 69.8(5) . . ? C43 C42 H42 125.2 . . ? C41 C42 H42 125.2 . . ? Co4 C42 H42 126.7 . . ? C42 C43 C44 106.6(9) . . ? C42 C43 Co4 70.7(5) . . ? C44 C43 Co4 68.0(5) . . ? C42 C43 H43 126.7 . . ? C44 C43 H43 126.7 . . ? Co4 C43 H43 126.2 . . ? C43 C44 C45 108.2(8) . . ? C43 C44 Co4 71.3(5) . . ? C45 C44 Co4 69.6(5) . . ? C43 C44 H44 125.9 . . ? C45 C44 H44 125.9 . . ? Co4 C44 H44 124.8 . . ? C41 C45 C44 108.2(8) . . ? C41 C45 Co4 71.9(5) . . ? C44 C45 Co4 69.2(5) . . ? C41 C45 H45 125.9 . . ? C44 C45 H45 125.9 . . ? Co4 C45 H45 124.5 . . ? C86 C81 C82 117.5(8) . . ? C86 C81 C8 121.9(8) . . ? C82 C81 C8 120.6(7) . . ? C83 C82 C81 121.0(8) . . ? C83 C82 H82 119.5 . . ? C81 C82 H82 119.5 . . ? C82 C83 C84 120.5(8) . . ? C82 C83 H83 119.8 . . ? C84 C83 H83 119.8 . . ? C85 C84 C83 118.8(9) . . ? C85 C84 H84 120.6 . . ? C83 C84 H84 120.6 . . ? C86 C85 C84 121.2(8) . . ? C86 C85 H85 119.4 . . ? C84 C85 H85 119.4 . . ? C85 C86 C81 121.0(8) . . ? C85 C86 H86 119.5 . . ? C81 C86 H86 119.5 . . ? C5S C2S C6S 120(8) . 3_666 ? C5S C2S C4S 81(6) . . ? CC3S C3S C5S 143(7) 3_566 . ? C2S C5S C1S 136(9) . . ? C2S C5S C3S 126(9) . . ? C1S C5S C3S 85(6) . . ? C1S C5S C4S 100(6) . . ? C3S C5S C4S 88(5) . . ? C6S C6S C2S 139(10) 3_666 3_666 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 20.68 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.970 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.140 #===end data_5x81308 _database_code_depnum_ccdc_archive 'CCDC 631515' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H25 B10 Co' _chemical_formula_sum 'C19 H25 B10 Co' _chemical_formula_weight 420.42 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)/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 12.0447(8) _cell_length_b 12.6676(8) _cell_length_c 13.8241(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.129(4) _cell_angle_gamma 90.00 _cell_volume 2045.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3493 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 26.67 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.904 _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30880 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 30.73 _reflns_number_total 6327 _reflns_number_gt 3493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6327 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _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 Co4 Co 0.54600(3) 0.25061(3) 0.07990(2) 0.01500(10) Uani 1 1 d . . . C1 C 0.6554(2) 0.2983(2) 0.21268(16) 0.0155(5) Uani 1 1 d . . . B2 B 0.6290(3) 0.3965(2) 0.14426(19) 0.0164(6) Uani 1 1 d . . . H2C H 0.588(2) 0.4644(19) 0.1671(18) 0.020 Uiso 1 1 d . . . B3 B 0.7075(3) 0.1949(2) 0.1833(2) 0.0189(6) Uani 1 1 d . . . H3C H 0.719(2) 0.135(2) 0.234(2) 0.023 Uiso 1 1 d . . . B5 B 0.7872(3) 0.3376(2) 0.1874(2) 0.0185(6) Uani 1 1 d . . . H5C H 0.845(2) 0.367(2) 0.2564(19) 0.022 Uiso 1 1 d . . . B6 B 0.6046(3) 0.3823(2) 0.0113(2) 0.0152(6) Uani 1 1 d . . . H6C H 0.548(2) 0.4339(19) -0.0286(18) 0.018 Uiso 1 1 d . . . B7 B 0.6916(3) 0.1623(2) 0.0528(2) 0.0177(6) Uani 1 1 d . . . H7C H 0.679(2) 0.082(2) 0.0317(18) 0.021 Uiso 1 1 d . . . B8 B 0.8237(3) 0.2129(2) 0.1239(2) 0.0194(6) Uani 1 1 d . . . H8C H 0.896(2) 0.168(2) 0.1585(19) 0.023 Uiso 1 1 d . . . B9 B 0.7366(3) 0.4318(2) 0.0807(2) 0.0175(6) Uani 1 1 d . . . H9C H 0.757(2) 0.516(2) 0.0774(18) 0.021 Uiso 1 1 d . . . B10 B 0.6306(3) 0.2563(2) -0.03785(19) 0.0179(6) Uani 1 1 d . . . H10C H 0.582(2) 0.2333(19) -0.113(2) 0.022 Uiso 1 1 d . . . B11 B 0.8414(3) 0.3378(2) 0.0786(2) 0.0190(6) Uani 1 1 d . . . H11C H 0.927(2) 0.372(2) 0.0801(18) 0.023 Uiso 1 1 d . . . C12 C 0.7273(2) 0.35988(19) -0.02351(17) 0.0163(5) Uani 1 1 d . . . B13 B 0.7812(3) 0.2340(2) -0.0045(2) 0.0201(7) Uani 1 1 d . . . H13C H 0.825(2) 0.203(2) -0.0545(19) 0.024 Uiso 1 1 d . . . C11 C 0.6352(2) 0.3072(2) 0.31540(17) 0.0170(5) Uani 1 1 d . . . C12A C 0.6482(2) 0.4033(2) 0.36595(18) 0.0194(5) Uani 1 1 d . . . H12A H 0.6685 0.4643 0.3342 0.023 Uiso 1 1 calc R . . C13 C 0.6320(2) 0.4120(2) 0.46252(17) 0.0206(6) Uani 1 1 d . . . H13 H 0.6398 0.4785 0.4953 0.025 Uiso 1 1 calc R . . C14 C 0.6047(2) 0.3232(2) 0.50973(19) 0.0249(6) Uani 1 1 d . . . H14 H 0.5941 0.3282 0.5754 0.030 Uiso 1 1 calc R . . C15 C 0.5928(2) 0.2263(2) 0.4609(2) 0.0233(6) Uani 1 1 d . . . H15 H 0.5748 0.1651 0.4937 0.028 Uiso 1 1 calc R . . C16 C 0.6069(2) 0.2185(2) 0.36532(18) 0.0194(6) Uani 1 1 d . . . H16 H 0.5974 0.1520 0.3326 0.023 Uiso 1 1 calc R . . C41 C 0.3804(2) 0.3014(2) 0.0708(2) 0.0241(6) Uani 1 1 d . . . H41 H 0.3563 0.3757 0.0795 0.029 Uiso 1 1 calc R . . C42 C 0.4112(2) 0.2251(2) 0.1467(2) 0.0246(7) Uani 1 1 d . . . H42 H 0.4137 0.2362 0.2188 0.030 Uiso 1 1 calc R . . C43 C 0.4397(2) 0.1305(2) 0.1040(2) 0.0242(6) Uani 1 1 d . . . H43 H 0.4645 0.0629 0.1402 0.029 Uiso 1 1 calc R . . C44 C 0.4259(2) 0.1485(2) 0.0008(2) 0.0252(6) Uani 1 1 d . . . H44 H 0.4380 0.0956 -0.0494 0.030 Uiso 1 1 calc R . . C45 C 0.3895(2) 0.2548(2) -0.01922(19) 0.0245(6) Uani 1 1 d . . . H45 H 0.3717 0.2899 -0.0861 0.029 Uiso 1 1 calc R . . C121 C 0.7427(2) 0.41921(19) -0.11427(17) 0.0181(5) Uani 1 1 d . . . C122 C 0.8484(2) 0.4618(2) -0.11768(19) 0.0239(6) Uani 1 1 d . . . H122 H 0.9129 0.4505 -0.0634 0.029 Uiso 1 1 calc R . . C123 C 0.8607(3) 0.5203(2) -0.19871(19) 0.0278(7) Uani 1 1 d . . . H123 H 0.9335 0.5483 -0.1999 0.033 Uiso 1 1 calc R . . C124 C 0.7681(3) 0.5385(2) -0.27782(19) 0.0284(7) Uani 1 1 d . . . H124 H 0.7771 0.5786 -0.3335 0.034 Uiso 1 1 calc R . . C125 C 0.6626(3) 0.4982(2) -0.27591(18) 0.0279(7) Uani 1 1 d . . . H125 H 0.5982 0.5125 -0.3294 0.034 Uiso 1 1 calc R . . C126 C 0.6498(2) 0.4367(2) -0.19597(18) 0.0242(6) Uani 1 1 d . . . H126 H 0.5774 0.4063 -0.1968 0.029 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 Co4 0.01466(17) 0.01479(16) 0.01407(14) -0.00156(14) 0.00064(11) -0.00093(15) C1 0.0126(13) 0.0183(13) 0.0141(11) -0.0010(9) 0.0002(9) -0.0030(10) B2 0.0178(16) 0.0173(15) 0.0120(12) -0.0029(10) -0.0001(11) -0.0004(12) B3 0.0188(16) 0.0169(15) 0.0196(14) 0.0023(11) 0.0023(12) 0.0019(12) B5 0.0209(16) 0.0156(14) 0.0171(13) 0.0007(11) 0.0011(12) -0.0028(12) B6 0.0151(15) 0.0138(14) 0.0153(12) 0.0013(10) 0.0008(11) 0.0011(11) B7 0.0202(16) 0.0146(14) 0.0184(13) -0.0023(11) 0.0046(11) 0.0009(12) B8 0.0188(16) 0.0202(14) 0.0187(13) 0.0003(11) 0.0038(12) 0.0059(12) B9 0.0213(16) 0.0151(14) 0.0149(12) -0.0013(10) 0.0020(11) -0.0007(12) B10 0.0183(14) 0.0192(14) 0.0156(11) -0.0031(12) 0.0029(10) -0.0004(13) B11 0.0181(16) 0.0222(16) 0.0154(13) -0.0010(11) 0.0016(11) -0.0011(12) C12 0.0173(13) 0.0169(13) 0.0138(11) -0.0002(9) 0.0018(10) -0.0018(10) B13 0.0199(16) 0.0205(18) 0.0189(13) -0.0037(11) 0.0030(11) 0.0020(12) C11 0.0146(13) 0.0184(13) 0.0163(11) 0.0019(10) 0.0005(10) 0.0003(10) C12A 0.0198(14) 0.0198(13) 0.0174(11) 0.0007(10) 0.0024(10) -0.0016(11) C13 0.0205(14) 0.0267(15) 0.0148(11) -0.0032(10) 0.0044(10) -0.0036(11) C14 0.0237(15) 0.0364(17) 0.0151(11) -0.0021(11) 0.0056(11) -0.0033(13) C15 0.0212(15) 0.0256(16) 0.0235(12) 0.0064(10) 0.0064(11) -0.0030(11) C16 0.0177(14) 0.0193(13) 0.0197(12) 0.0001(10) 0.0017(10) -0.0024(10) C41 0.0124(14) 0.0268(15) 0.0308(14) -0.0056(12) 0.0009(11) -0.0009(11) C42 0.0141(14) 0.0387(18) 0.0210(12) -0.0013(11) 0.0041(10) -0.0049(11) C43 0.0204(15) 0.0234(15) 0.0281(14) 0.0011(11) 0.0043(12) -0.0075(11) C44 0.0212(15) 0.0262(15) 0.0268(14) -0.0077(11) 0.0032(12) -0.0110(12) C45 0.0136(13) 0.0343(15) 0.0213(11) 0.0024(12) -0.0040(9) -0.0039(13) C121 0.0237(15) 0.0166(13) 0.0147(11) -0.0023(9) 0.0058(10) 0.0011(11) C122 0.0230(15) 0.0256(15) 0.0209(12) -0.0006(11) 0.0008(11) -0.0025(12) C123 0.0299(18) 0.0339(17) 0.0205(13) -0.0011(12) 0.0077(12) -0.0090(13) C124 0.0386(19) 0.0313(16) 0.0174(12) 0.0060(11) 0.0112(12) 0.0019(13) C125 0.0309(17) 0.0397(17) 0.0122(11) 0.0019(11) 0.0034(11) 0.0053(14) C126 0.0218(15) 0.0319(16) 0.0188(12) -0.0021(11) 0.0051(11) 0.0010(12) _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 Co4 C45 2.042(2) . ? Co4 C44 2.047(2) . ? Co4 C43 2.067(3) . ? Co4 C41 2.070(3) . ? Co4 C1 2.071(2) . ? Co4 C42 2.080(3) . ? Co4 B10 2.122(3) . ? Co4 B6 2.124(3) . ? Co4 B2 2.184(3) . ? Co4 B7 2.188(3) . ? Co4 B3 2.229(3) . ? C1 C11 1.502(3) . ? C1 B2 1.548(4) . ? C1 B3 1.548(4) . ? C1 B5 1.777(4) . ? B2 B9 1.791(4) . ? B2 B6 1.798(4) . ? B2 B5 1.997(4) . ? B2 H2C 1.08(2) . ? B3 B8 1.803(4) . ? B3 B7 1.816(4) . ? B3 B5 2.041(4) . ? B3 H3C 1.02(3) . ? B5 B11 1.781(4) . ? B5 B9 1.880(4) . ? B5 B8 1.910(4) . ? B5 H5C 1.10(3) . ? B6 C12 1.686(4) . ? B6 B9 1.759(4) . ? B6 B10 1.793(4) . ? B6 H6C 1.01(2) . ? B7 B13 1.742(4) . ? B7 B10 1.754(4) . ? B7 B8 1.773(4) . ? B7 H7C 1.05(3) . ? B8 B11 1.734(4) . ? B8 B13 1.744(4) . ? B8 H8C 1.06(3) . ? B9 C12 1.685(4) . ? B9 B11 1.742(4) . ? B9 H9C 1.09(3) . ? B10 C12 1.733(4) . ? B10 B13 1.781(4) . ? B10 H10C 1.09(3) . ? B11 C12 1.735(4) . ? B11 B13 1.779(4) . ? B11 H11C 1.11(3) . ? C12 C121 1.513(3) . ? C12 B13 1.717(4) . ? B13 H13C 1.04(3) . ? C11 C12A 1.394(3) . ? C11 C16 1.403(4) . ? C12A C13 1.400(3) . ? C12A H12A 0.9500 . ? C13 C14 1.380(4) . ? C13 H13 0.9500 . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 C16 1.376(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C41 C45 1.406(4) . ? C41 C42 1.408(4) . ? C41 H41 1.0000 . ? C42 C43 1.415(4) . ? C42 H42 1.0000 . ? C43 C44 1.414(4) . ? C43 H43 1.0000 . ? C44 C45 1.422(4) . ? C44 H44 1.0000 . ? C45 H45 1.0000 . ? C121 C122 1.394(4) . ? C121 C126 1.400(3) . ? C122 C123 1.381(4) . ? C122 H122 0.9500 . ? C123 C124 1.377(4) . ? C123 H123 0.9500 . ? C124 C125 1.375(4) . ? C124 H124 0.9500 . ? C125 C126 1.392(4) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? 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 C45 Co4 C44 40.71(11) . . ? C45 Co4 C43 67.73(11) . . ? C44 Co4 C43 40.22(10) . . ? C45 Co4 C41 39.97(10) . . ? C44 Co4 C41 67.62(11) . . ? C43 Co4 C41 67.24(11) . . ? C45 Co4 C1 150.49(11) . . ? C44 Co4 C1 150.66(11) . . ? C43 Co4 C1 110.90(10) . . ? C41 Co4 C1 110.99(10) . . ? C45 Co4 C42 67.01(11) . . ? C44 Co4 C42 67.22(11) . . ? C43 Co4 C42 39.90(10) . . ? C41 Co4 C42 39.67(11) . . ? C1 Co4 C42 92.78(10) . . ? C45 Co4 B10 91.26(11) . . ? C44 Co4 B10 91.18(11) . . ? C43 Co4 B10 125.51(11) . . ? C41 Co4 B10 125.38(11) . . ? C1 Co4 B10 110.43(10) . . ? C42 Co4 B10 156.80(11) . . ? C45 Co4 B6 91.87(11) . . ? C44 Co4 B6 121.76(11) . . ? C43 Co4 B6 159.52(11) . . ? C41 Co4 B6 98.57(11) . . ? C1 Co4 B6 87.59(10) . . ? C42 Co4 B6 134.51(11) . . ? B10 Co4 B6 49.95(11) . . ? C45 Co4 B2 120.44(11) . . ? C44 Co4 B2 161.03(11) . . ? C43 Co4 B2 142.83(11) . . ? C41 Co4 B2 95.74(11) . . ? C1 Co4 B2 42.56(10) . . ? C42 Co4 B2 106.24(11) . . ? B10 Co4 B2 91.49(11) . . ? B6 Co4 B2 49.33(10) . . ? C45 Co4 B7 123.04(11) . . ? C44 Co4 B7 94.40(11) . . ? C43 Co4 B7 101.83(12) . . ? C41 Co4 B7 161.63(11) . . ? C1 Co4 B7 86.44(10) . . ? C42 Co4 B7 137.89(11) . . ? B10 Co4 B7 47.99(11) . . ? B6 Co4 B7 87.57(11) . . ? B2 Co4 B7 101.32(11) . . ? C45 Co4 B3 163.04(11) . . ? C44 Co4 B3 122.35(11) . . ? C43 Co4 B3 98.12(11) . . ? C41 Co4 B3 144.51(11) . . ? C1 Co4 B3 42.00(10) . . ? C42 Co4 B3 108.62(11) . . ? B10 Co4 B3 89.74(11) . . ? B6 Co4 B3 101.67(11) . . ? B2 Co4 B3 76.45(11) . . ? B7 Co4 B3 48.54(11) . . ? C11 C1 B2 117.4(2) . . ? C11 C1 B3 118.7(2) . . ? B2 C1 B3 123.8(2) . . ? C11 C1 B5 121.56(19) . . ? B2 C1 B5 73.44(18) . . ? B3 C1 B5 75.37(18) . . ? C11 C1 Co4 130.14(17) . . ? B2 C1 Co4 72.61(13) . . ? B3 C1 Co4 74.45(14) . . ? B5 C1 Co4 108.22(14) . . ? C1 B2 B9 115.8(2) . . ? C1 B2 B6 120.2(2) . . ? B9 B2 B6 58.70(16) . . ? C1 B2 B5 58.57(16) . . ? B9 B2 B5 59.21(16) . . ? B6 B2 B5 100.01(19) . . ? C1 B2 Co4 64.82(13) . . ? B9 B2 Co4 109.00(16) . . ? B6 B2 Co4 63.59(12) . . ? B5 B2 Co4 96.55(15) . . ? C1 B2 H2C 120.2(13) . . ? B9 B2 H2C 112.5(13) . . ? B6 B2 H2C 114.0(13) . . ? B5 B2 H2C 133.2(14) . . ? Co4 B2 H2C 126.7(13) . . ? C1 B3 B8 115.0(2) . . ? C1 B3 B7 120.1(2) . . ? B8 B3 B7 58.69(17) . . ? C1 B3 B5 57.42(16) . . ? B8 B3 B5 59.22(16) . . ? B7 B3 B5 99.40(19) . . ? C1 B3 Co4 63.55(13) . . ? B8 B3 Co4 108.70(16) . . ? B7 B3 Co4 64.58(13) . . ? B5 B3 Co4 93.90(14) . . ? C1 B3 H3C 116.6(15) . . ? B8 B3 H3C 114.7(15) . . ? B7 B3 H3C 118.3(15) . . ? B5 B3 H3C 131.3(15) . . ? Co4 B3 H3C 128.7(15) . . ? C1 B5 B11 134.1(2) . . ? C1 B5 B9 101.44(19) . . ? B11 B5 B9 56.76(16) . . ? C1 B5 B8 100.11(18) . . ? B11 B5 B8 55.92(17) . . ? B9 B5 B8 103.39(18) . . ? C1 B5 B2 48.00(14) . . ? B11 B5 B2 105.52(18) . . ? B9 B5 B2 54.94(15) . . ? B8 B5 B2 118.80(18) . . ? C1 B5 B3 47.21(14) . . ? B11 B5 B3 104.20(19) . . ? B9 B5 B3 118.73(19) . . ? B8 B5 B3 54.17(15) . . ? B2 B5 B3 85.09(17) . . ? C1 B5 H5C 109.4(13) . . ? B11 B5 H5C 116.5(13) . . ? B9 B5 H5C 119.0(13) . . ? B8 B5 H5C 120.4(13) . . ? B2 B5 H5C 119.6(13) . . ? B3 B5 H5C 121.0(13) . . ? C12 B6 B9 58.51(16) . . ? C12 B6 B10 59.67(16) . . ? B9 B6 B10 107.8(2) . . ? C12 B6 B2 111.9(2) . . ? B9 B6 B2 60.44(16) . . ? B10 B6 B2 118.4(2) . . ? C12 B6 Co4 113.88(17) . . ? B9 B6 Co4 113.01(16) . . ? B10 B6 Co4 64.99(13) . . ? B2 B6 Co4 67.08(13) . . ? C12 B6 H6C 118.4(14) . . ? B9 B6 H6C 117.9(15) . . ? B10 B6 H6C 121.9(14) . . ? B2 B6 H6C 114.6(14) . . ? Co4 B6 H6C 120.1(14) . . ? B13 B7 B10 61.23(17) . . ? B13 B7 B8 59.48(17) . . ? B10 B7 B8 108.2(2) . . ? B13 B7 B3 114.0(2) . . ? B10 B7 B3 118.6(2) . . ? B8 B7 B3 60.28(16) . . ? B13 B7 Co4 114.97(18) . . ? B10 B7 Co4 64.03(13) . . ? B8 B7 Co4 111.61(17) . . ? B3 B7 Co4 66.89(13) . . ? B13 B7 H7C 115.9(14) . . ? B10 B7 H7C 116.7(14) . . ? B8 B7 H7C 123.1(14) . . ? B3 B7 H7C 117.8(13) . . ? Co4 B7 H7C 118.3(14) . . ? B11 B8 B13 61.54(16) . . ? B11 B8 B7 107.6(2) . . ? B13 B8 B7 59.37(17) . . ? B11 B8 B3 117.2(2) . . ? B13 B8 B3 114.6(2) . . ? B7 B8 B3 61.02(17) . . ? B11 B8 B5 58.25(16) . . ? B13 B8 B5 107.3(2) . . ? B7 B8 B5 106.1(2) . . ? B3 B8 B5 66.62(17) . . ? B11 B8 H8C 119.7(15) . . ? B13 B8 H8C 123.3(14) . . ? B7 B8 H8C 125.9(15) . . ? B3 B8 H8C 112.0(14) . . ? B5 B8 H8C 119.9(14) . . ? C12 B9 B11 60.82(16) . . ? C12 B9 B6 58.58(16) . . ? B11 B9 B6 108.0(2) . . ? C12 B9 B2 112.3(2) . . ? B11 B9 B2 116.8(2) . . ? B6 B9 B2 60.86(16) . . ? C12 B9 B5 105.56(19) . . ? B11 B9 B5 58.75(16) . . ? B6 B9 B5 106.2(2) . . ? B2 B9 B5 65.85(16) . . ? C12 B9 H9C 117.3(13) . . ? B11 B9 H9C 119.7(14) . . ? B6 B9 H9C 120.2(13) . . ? B2 B9 H9C 117.2(13) . . ? B5 B9 H9C 128.1(13) . . ? C12 B10 B7 106.26(19) . . ? C12 B10 B13 58.47(15) . . ? B7 B10 B13 59.05(17) . . ? C12 B10 B6 57.11(16) . . ? B7 B10 B6 114.56(19) . . ? B13 B10 B6 107.7(2) . . ? C12 B10 Co4 111.90(16) . . ? B7 B10 Co4 67.98(14) . . ? B13 B10 Co4 116.47(17) . . ? B6 B10 Co4 65.06(13) . . ? C12 B10 H10C 119.8(14) . . ? B7 B10 H10C 121.8(13) . . ? B13 B10 H10C 118.3(15) . . ? B6 B10 H10C 119.5(14) . . ? Co4 B10 H10C 118.1(14) . . ? B8 B11 C12 107.3(2) . . ? B8 B11 B9 117.7(2) . . ? C12 B11 B9 57.97(15) . . ? B8 B11 B13 59.51(16) . . ? C12 B11 B13 58.46(15) . . ? B9 B11 B13 109.4(2) . . ? B8 B11 B5 65.83(18) . . ? C12 B11 B5 107.8(2) . . ? B9 B11 B5 64.49(17) . . ? B13 B11 B5 111.6(2) . . ? B8 B11 H11C 122.6(13) . . ? C12 B11 H11C 120.1(13) . . ? B9 B11 H11C 114.3(13) . . ? B13 B11 H11C 121.7(13) . . ? B5 B11 H11C 121.0(13) . . ? C121 C12 B9 116.4(2) . . ? C121 C12 B6 116.5(2) . . ? B9 C12 B6 62.91(16) . . ? C121 C12 B13 118.0(2) . . ? B9 C12 B13 115.34(19) . . ? B6 C12 B13 116.0(2) . . ? C121 C12 B10 119.77(19) . . ? B9 C12 B10 114.2(2) . . ? B6 C12 B10 63.21(16) . . ? B13 C12 B10 62.14(17) . . ? C121 C12 B11 121.4(2) . . ? B9 C12 B11 61.21(16) . . ? B6 C12 B11 111.77(18) . . ? B13 C12 B11 62.05(16) . . ? B10 C12 B11 110.33(19) . . ? C12 B13 B7 107.5(2) . . ? C12 B13 B8 107.7(2) . . ? B7 B13 B8 61.15(17) . . ? C12 B13 B11 59.49(15) . . ? B7 B13 B11 107.0(2) . . ? B8 B13 B11 58.95(17) . . ? C12 B13 B10 59.39(16) . . ? B7 B13 B10 59.72(17) . . ? B8 B13 B10 108.4(2) . . ? B11 B13 B10 106.2(2) . . ? C12 B13 H13C 118.7(15) . . ? B7 B13 H13C 125.1(15) . . ? B8 B13 H13C 123.2(15) . . ? B11 B13 H13C 120.9(15) . . ? B10 B13 H13C 122.3(15) . . ? C12A C11 C16 117.7(2) . . ? C12A C11 C1 121.0(2) . . ? C16 C11 C1 121.3(2) . . ? C11 C12A C13 121.4(2) . . ? C11 C12A H12A 119.3 . . ? C13 C12A H12A 119.3 . . ? C14 C13 C12A 119.5(2) . . ? C14 C13 H13 120.3 . . ? C12A C13 H13 120.3 . . ? C13 C14 C15 119.9(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.5(2) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C11 121.1(2) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? C45 C41 C42 107.9(3) . . ? C45 C41 Co4 68.94(15) . . ? C42 C41 Co4 70.52(16) . . ? C45 C41 H41 126.0 . . ? C42 C41 H41 126.0 . . ? Co4 C41 H41 126.0 . . ? C41 C42 C43 108.5(2) . . ? C41 C42 Co4 69.82(15) . . ? C43 C42 Co4 69.56(15) . . ? C41 C42 H42 125.8 . . ? C43 C42 H42 125.8 . . ? Co4 C42 H42 125.8 . . ? C44 C43 C42 107.7(2) . . ? C44 C43 Co4 69.14(15) . . ? C42 C43 Co4 70.54(15) . . ? C44 C43 H43 126.2 . . ? C42 C43 H43 126.2 . . ? Co4 C43 H43 126.2 . . ? C43 C44 C45 107.7(2) . . ? C43 C44 Co4 70.65(15) . . ? C45 C44 Co4 69.48(14) . . ? C43 C44 H44 126.2 . . ? C45 C44 H44 126.2 . . ? Co4 C44 H44 126.2 . . ? C41 C45 C44 108.2(2) . . ? C41 C45 Co4 71.09(14) . . ? C44 C45 Co4 69.81(14) . . ? C41 C45 H45 125.9 . . ? C44 C45 H45 125.9 . . ? Co4 C45 H45 125.9 . . ? C122 C121 C126 117.9(2) . . ? C122 C121 C12 121.2(2) . . ? C126 C121 C12 120.8(2) . . ? C123 C122 C121 121.0(2) . . ? C123 C122 H122 119.5 . . ? C121 C122 H122 119.5 . . ? C124 C123 C122 120.5(3) . . ? C124 C123 H123 119.7 . . ? C122 C123 H123 119.7 . . ? C125 C124 C123 119.7(2) . . ? C125 C124 H124 120.2 . . ? C123 C124 H124 120.2 . . ? C124 C125 C126 120.3(2) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C125 C126 C121 120.5(3) . . ? C125 C126 H126 119.8 . . ? C121 C126 H126 119.8 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.602 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.089 #===end data_6x81317 _database_code_depnum_ccdc_archive 'CCDC 631516' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 B10 Ru' _chemical_formula_sum 'C24 H34 B10 Ru' _chemical_formula_weight 531.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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 9.3596(8) _cell_length_b 8.7670(9) _cell_length_c 15.4785(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.803(5) _cell_angle_gamma 90.00 _cell_volume 1261.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6532 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 23.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 0.938 _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20080 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 24.43 _reflns_number_total 3972 _reflns_number_gt 3370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.9076P] 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 -0.02(5) _refine_ls_number_reflns 3972 _refine_ls_number_parameters 349 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.056 _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 Ru4 Ru 0.45244(4) 0.89023(7) 0.18006(2) 0.01906(14) Uani 1 1 d . . . C1 C 0.5298(6) 0.8142(7) 0.3105(4) 0.0191(13) Uani 1 1 d . . . B2 B 0.5250(7) 0.6691(9) 0.2536(4) 0.0197(15) Uani 1 1 d D . . H2C H 0.460(5) 0.575(5) 0.274(4) 0.024 Uiso 1 1 d D . . B3 B 0.6184(8) 0.9609(9) 0.2928(5) 0.0218(16) Uani 1 1 d D . . H3C H 0.610(7) 1.062(4) 0.334(3) 0.026 Uiso 1 1 d D . . B5 B 0.7080(8) 0.7602(9) 0.3185(4) 0.0224(16) Uani 1 1 d D . . H5C H 0.756(6) 0.733(6) 0.3851(19) 0.027 Uiso 1 1 d D . . B6 B 0.5739(7) 0.6744(9) 0.1444(4) 0.0190(15) Uani 1 1 d D . . H6C H 0.515(5) 0.587(5) 0.103(3) 0.023 Uiso 1 1 d D . . B7 B 0.6694(7) 0.9992(9) 0.1814(4) 0.0238(17) Uani 1 1 d D . . H7C H 0.674(7) 1.126(3) 0.173(4) 0.029 Uiso 1 1 d D . . C8 C 0.7897(6) 0.9265(8) 0.2646(4) 0.028(2) Uani 1 1 d . . . B9 B 0.7030(7) 0.6121(9) 0.2308(5) 0.0242(16) Uani 1 1 d D . . H9C H 0.724(6) 0.491(3) 0.241(4) 0.029 Uiso 1 1 d D . . B10 B 0.6404(7) 0.8494(9) 0.1032(5) 0.027(2) Uani 1 1 d D . . H10C H 0.621(5) 0.888(10) 0.035(2) 0.032 Uiso 1 1 d D . . B11 B 0.8426(7) 0.7454(9) 0.2438(5) 0.0260(17) Uani 1 1 d D . . H11C H 0.953(3) 0.721(7) 0.273(4) 0.031 Uiso 1 1 d D . . B12 B 0.7597(7) 0.6948(9) 0.1385(4) 0.0247(17) Uani 1 1 d D . . H12C H 0.818(6) 0.623(6) 0.097(3) 0.030 Uiso 1 1 d D . . B13 B 0.8140(6) 0.8855(18) 0.1599(3) 0.0265(14) Uani 1 1 d D . . H13C H 0.903(4) 0.942(6) 0.133(3) 0.032 Uiso 1 1 d D . . C11 C 0.4503(6) 0.8177(7) 0.3901(4) 0.0226(14) Uani 1 1 d . . . C12 C 0.3260(7) 0.7313(8) 0.3929(4) 0.0289(15) Uani 1 1 d . . . H12 H 0.2890 0.6727 0.3437 0.035 Uiso 1 1 calc R . . C13 C 0.2552(8) 0.7299(8) 0.4676(4) 0.0355(17) Uani 1 1 d . . . H13 H 0.1694 0.6722 0.4683 0.043 Uiso 1 1 calc R . . C14 C 0.3096(8) 0.8121(9) 0.5401(5) 0.0415(19) Uani 1 1 d . . . H14 H 0.2623 0.8090 0.5911 0.050 Uiso 1 1 calc R . . C15 C 0.4334(7) 0.8995(14) 0.5390(3) 0.0370(15) Uani 1 1 d . . . H15 H 0.4698 0.9581 0.5884 0.044 Uiso 1 1 calc R . . C16 C 0.5037(6) 0.8999(14) 0.4640(3) 0.0294(14) Uani 1 1 d . . . H16 H 0.5897 0.9574 0.4635 0.035 Uiso 1 1 calc R . . C40 C 0.2479(6) 0.8316(7) 0.0898(4) 0.0267(17) Uani 1 1 d . . . C41 C 0.2125(5) 0.8538(8) 0.1773(4) 0.023(2) Uani 1 1 d . . . H41 H 0.1773 0.7649 0.2093 0.028 Uiso 1 1 calc R . . C42 C 0.2501(6) 0.9910(8) 0.2237(4) 0.0259(15) Uani 1 1 d . . . H42 H 0.2409 0.9948 0.2873 0.031 Uiso 1 1 calc R . . C43 C 0.3253(6) 1.1096(8) 0.1866(4) 0.0294(16) Uani 1 1 d . . . C44 C 0.3631(6) 1.0851(8) 0.1012(4) 0.0305(17) Uani 1 1 d . . . H44 H 0.4312 1.1579 0.0777 0.037 Uiso 1 1 calc R . . C45 C 0.3240(7) 0.9536(8) 0.0542(4) 0.0290(17) Uani 1 1 d . . . H45 H 0.3669 0.9350 -0.0010 0.035 Uiso 1 1 calc R . . C46 C 0.3648(7) 1.2511(8) 0.2367(5) 0.0411(18) Uani 1 1 d . . . H46A H 0.2855 1.3245 0.2272 0.062 Uiso 1 1 calc R . . H46B H 0.4514 1.2955 0.2170 0.062 Uiso 1 1 calc R . . H46C H 0.3834 1.2267 0.2988 0.062 Uiso 1 1 calc R . . C47 C 0.2030(6) 0.6961(8) 0.0360(4) 0.0309(16) Uani 1 1 d . . . H47 H 0.2819 0.6713 0.0000 0.037 Uiso 1 1 calc R . . C48 C 0.1774(7) 0.5553(8) 0.0907(5) 0.0372(17) Uani 1 1 d . . . H48A H 0.2609 0.5390 0.1342 0.056 Uiso 1 1 calc R . . H48B H 0.1634 0.4657 0.0528 0.056 Uiso 1 1 calc R . . H48C H 0.0915 0.5712 0.1201 0.056 Uiso 1 1 calc R . . C49 C 0.0690(7) 0.7371(9) -0.0257(4) 0.0381(18) Uani 1 1 d . . . H49A H -0.0089 0.7654 0.0083 0.057 Uiso 1 1 calc R . . H49B H 0.0393 0.6490 -0.0625 0.057 Uiso 1 1 calc R . . H49C H 0.0906 0.8231 -0.0624 0.057 Uiso 1 1 calc R . . C81 C 0.8996(6) 1.0335(7) 0.3134(4) 0.0215(14) Uani 1 1 d . . . C82 C 0.9230(6) 1.1764(8) 0.2830(4) 0.0299(15) Uani 1 1 d . . . H82 H 0.8711 1.2086 0.2296 0.036 Uiso 1 1 calc R . . C83 C 1.0215(7) 1.2772(9) 0.3284(5) 0.0379(18) Uani 1 1 d . . . H83 H 1.0360 1.3763 0.3063 0.045 Uiso 1 1 calc R . . C84 C 1.0983(7) 1.2285(9) 0.4072(4) 0.0370(18) Uani 1 1 d . . . H84 H 1.1651 1.2949 0.4393 0.044 Uiso 1 1 calc R . . C85 C 1.0763(6) 1.0871(8) 0.4367(4) 0.0320(17) Uani 1 1 d . . . H85 H 1.1299 1.0548 0.4895 0.038 Uiso 1 1 calc R . . C86 C 0.9785(6) 0.9867(8) 0.3932(4) 0.0266(15) Uani 1 1 d . . . H86 H 0.9644 0.8882 0.4163 0.032 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 Ru4 0.00914(19) 0.0322(2) 0.0157(2) 0.0030(4) 0.00088(13) 0.0002(4) C1 0.012(3) 0.028(3) 0.016(3) 0.002(3) 0.001(3) 0.005(3) B2 0.012(3) 0.032(4) 0.014(3) 0.000(3) -0.004(3) 0.002(3) B3 0.016(4) 0.031(4) 0.017(4) 0.000(3) 0.000(3) -0.003(3) B5 0.015(4) 0.037(5) 0.014(3) 0.001(3) -0.003(3) 0.006(3) B6 0.013(3) 0.030(4) 0.014(3) -0.005(3) 0.001(3) 0.000(3) B7 0.008(3) 0.039(5) 0.023(4) 0.003(3) -0.003(3) 0.002(3) C8 0.012(3) 0.054(8) 0.017(3) 0.000(3) 0.000(2) -0.002(3) B9 0.014(3) 0.030(4) 0.028(4) -0.002(3) -0.001(3) 0.003(3) B10 0.010(3) 0.046(7) 0.023(3) 0.000(3) -0.001(3) -0.002(3) B11 0.009(3) 0.046(5) 0.023(4) -0.010(3) 0.003(3) -0.003(3) B12 0.010(3) 0.049(5) 0.015(3) -0.003(3) -0.002(3) 0.001(3) B13 0.013(3) 0.051(4) 0.015(3) -0.012(6) 0.002(2) -0.003(6) C11 0.017(3) 0.031(3) 0.021(3) 0.012(3) 0.007(3) 0.005(3) C12 0.022(3) 0.034(4) 0.033(4) 0.005(3) 0.011(3) 0.008(3) C13 0.035(4) 0.034(4) 0.041(4) 0.012(3) 0.019(3) 0.001(3) C14 0.050(5) 0.050(4) 0.030(4) 0.013(3) 0.027(4) 0.017(4) C15 0.051(4) 0.038(4) 0.024(3) -0.002(6) 0.011(3) 0.007(6) C16 0.026(3) 0.040(4) 0.022(3) -0.009(5) 0.004(2) 0.006(5) C40 0.011(3) 0.051(5) 0.017(3) -0.001(3) -0.006(3) 0.006(3) C41 0.003(2) 0.046(7) 0.020(3) 0.004(3) 0.002(2) 0.005(3) C42 0.011(3) 0.042(4) 0.025(4) 0.002(3) 0.002(3) 0.006(3) C43 0.016(3) 0.034(4) 0.039(4) 0.007(3) 0.003(3) 0.006(3) C44 0.016(3) 0.039(4) 0.036(4) 0.020(3) 0.003(3) 0.002(3) C45 0.014(3) 0.047(5) 0.026(4) 0.011(3) 0.001(3) 0.005(3) C46 0.026(4) 0.039(4) 0.058(5) 0.004(4) 0.001(3) 0.009(3) C47 0.018(3) 0.046(5) 0.028(4) -0.007(3) 0.003(3) -0.001(3) C48 0.024(4) 0.043(4) 0.044(4) -0.015(4) 0.000(3) -0.005(3) C49 0.027(4) 0.053(5) 0.033(4) -0.015(4) -0.002(3) 0.006(3) C81 0.009(3) 0.034(4) 0.020(3) -0.003(3) 0.000(3) 0.005(3) C82 0.019(3) 0.043(4) 0.025(3) -0.002(3) -0.005(3) 0.001(3) C83 0.021(4) 0.044(5) 0.049(5) -0.003(4) 0.002(3) -0.002(3) C84 0.021(4) 0.051(5) 0.037(4) -0.018(4) -0.002(3) -0.002(3) C85 0.018(3) 0.055(5) 0.022(3) -0.011(3) -0.006(3) 0.008(3) C86 0.015(3) 0.039(4) 0.026(3) 0.000(3) 0.003(3) 0.004(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 Ru4 C1 2.168(6) . ? Ru4 C44 2.206(6) . ? Ru4 C45 2.235(6) . ? Ru4 B7 2.242(7) . ? Ru4 C42 2.264(6) . ? Ru4 C41 2.264(5) . ? Ru4 B10 2.266(7) . ? Ru4 C43 2.270(6) . ? Ru4 B3 2.280(7) . ? Ru4 C40 2.290(6) . ? Ru4 B6 2.308(7) . ? Ru4 B2 2.309(7) . ? C1 C11 1.512(8) . ? C1 B2 1.545(10) . ? C1 B3 1.573(9) . ? C1 B5 1.724(9) . ? B2 B6 1.804(9) . ? B2 B9 1.813(9) . ? B2 B5 2.042(10) . ? B2 H2C 1.10(2) . ? B3 C8 1.737(9) . ? B3 B7 1.873(10) . ? B3 B5 1.969(11) . ? B3 H3C 1.10(2) . ? B5 B11 1.814(10) . ? B5 B9 1.876(10) . ? B5 C8 1.887(10) . ? B5 H5C 1.10(2) . ? B6 B12 1.761(9) . ? B6 B9 1.778(9) . ? B6 B10 1.801(10) . ? B6 H6C 1.10(2) . ? B7 C8 1.729(9) . ? B7 B13 1.745(12) . ? B7 B10 1.785(10) . ? B7 H7C 1.12(2) . ? C8 C81 1.525(8) . ? C8 B13 1.702(8) . ? C8 B11 1.705(11) . ? B9 B12 1.739(10) . ? B9 B11 1.747(10) . ? B9 H9C 1.09(2) . ? B10 B13 1.782(8) . ? B10 B12 1.799(10) . ? B10 H10C 1.11(2) . ? B11 B12 1.776(9) . ? B11 B13 1.785(14) . ? B11 H11C 1.10(2) . ? B12 B13 1.767(17) . ? B12 H12C 1.09(2) . ? B13 H13C 1.09(2) . ? C11 C12 1.394(9) . ? C11 C16 1.395(10) . ? C12 C13 1.398(9) . ? C12 H12 0.9500 . ? C13 C14 1.380(10) . ? C13 H13 0.9500 . ? C14 C15 1.391(11) . ? C14 H14 0.9500 . ? C15 C16 1.400(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C40 C45 1.431(9) . ? C40 C41 1.446(9) . ? C40 C47 1.483(9) . ? C41 C42 1.423(9) . ? C41 H41 1.0000 . ? C42 C43 1.415(9) . ? C42 H42 1.0000 . ? C43 C44 1.425(9) . ? C43 C46 1.486(10) . ? C44 C45 1.389(9) . ? C44 H44 1.0000 . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C49 1.527(9) . ? C47 C48 1.532(10) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C81 C82 1.365(10) . ? C81 C86 1.422(8) . ? C82 C83 1.404(9) . ? C82 H82 0.9500 . ? C83 C84 1.407(10) . ? C83 H83 0.9500 . ? C84 C85 1.346(10) . ? C84 H84 0.9500 . ? C85 C86 1.385(9) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru4 C44 144.7(2) . . ? C1 Ru4 C45 167.0(2) . . ? C44 Ru4 C45 36.4(2) . . ? C1 Ru4 B7 85.4(2) . . ? C44 Ru4 B7 87.6(2) . . ? C45 Ru4 B7 107.2(2) . . ? C1 Ru4 C42 92.3(2) . . ? C44 Ru4 C42 65.6(2) . . ? C45 Ru4 C42 77.3(2) . . ? B7 Ru4 C42 128.3(3) . . ? C1 Ru4 C41 101.2(2) . . ? C44 Ru4 C41 77.8(2) . . ? C45 Ru4 C41 65.7(2) . . ? B7 Ru4 C41 162.9(2) . . ? C42 Ru4 C41 36.6(2) . . ? C1 Ru4 B10 104.3(2) . . ? C44 Ru4 B10 95.7(2) . . ? C45 Ru4 B10 87.3(2) . . ? B7 Ru4 B10 46.7(3) . . ? C42 Ru4 B10 161.3(2) . . ? C41 Ru4 B10 142.9(2) . . ? C1 Ru4 C43 109.7(2) . . ? C44 Ru4 C43 37.1(2) . . ? C45 Ru4 C43 66.3(2) . . ? B7 Ru4 C43 96.7(2) . . ? C42 Ru4 C43 36.4(2) . . ? C41 Ru4 C43 66.2(2) . . ? B10 Ru4 C43 126.9(3) . . ? C1 Ru4 B3 41.3(2) . . ? C44 Ru4 B3 113.1(3) . . ? C45 Ru4 B3 147.9(3) . . ? B7 Ru4 B3 48.9(3) . . ? C42 Ru4 B3 100.6(3) . . ? C41 Ru4 B3 129.6(2) . . ? B10 Ru4 B3 86.8(3) . . ? C43 Ru4 B3 92.8(3) . . ? C1 Ru4 C40 131.4(2) . . ? C44 Ru4 C40 66.5(2) . . ? C45 Ru4 C40 36.8(2) . . ? B7 Ru4 C40 142.3(2) . . ? C42 Ru4 C40 66.5(2) . . ? C41 Ru4 C40 37.0(2) . . ? B10 Ru4 C40 106.8(2) . . ? C43 Ru4 C40 79.2(2) . . ? B3 Ru4 C40 166.4(2) . . ? C1 Ru4 B6 81.4(2) . . ? C44 Ru4 B6 131.9(2) . . ? C45 Ru4 B6 103.0(2) . . ? B7 Ru4 B6 83.1(3) . . ? C42 Ru4 B6 147.6(2) . . ? C41 Ru4 B6 113.3(2) . . ? B10 Ru4 B6 46.3(3) . . ? C43 Ru4 B6 168.8(2) . . ? B3 Ru4 B6 95.5(3) . . ? C40 Ru4 B6 94.0(2) . . ? C1 Ru4 B2 40.2(2) . . ? C44 Ru4 B2 173.2(3) . . ? C45 Ru4 B2 137.3(2) . . ? B7 Ru4 B2 98.0(2) . . ? C42 Ru4 B2 112.8(2) . . ? C41 Ru4 B2 97.1(2) . . ? B10 Ru4 B2 85.7(3) . . ? C43 Ru4 B2 144.5(2) . . ? B3 Ru4 B2 73.6(3) . . ? C40 Ru4 B2 106.7(2) . . ? B6 Ru4 B2 46.0(2) . . ? C11 C1 B2 119.9(6) . . ? C11 C1 B3 116.5(5) . . ? B2 C1 B3 123.6(5) . . ? C11 C1 B5 120.8(5) . . ? B2 C1 B5 77.1(4) . . ? B3 C1 B5 73.2(4) . . ? C11 C1 Ru4 127.6(4) . . ? B2 C1 Ru4 74.8(3) . . ? B3 C1 Ru4 73.2(4) . . ? B5 C1 Ru4 111.4(4) . . ? C1 B2 B6 121.4(6) . . ? C1 B2 B9 111.9(5) . . ? B6 B2 B9 58.9(4) . . ? C1 B2 B5 55.4(4) . . ? B6 B2 B5 99.2(4) . . ? B9 B2 B5 57.9(4) . . ? C1 B2 Ru4 65.0(3) . . ? B6 B2 Ru4 67.0(3) . . ? B9 B2 Ru4 111.0(4) . . ? B5 B2 Ru4 95.4(4) . . ? C1 B2 H2C 116(3) . . ? B6 B2 H2C 120(3) . . ? B9 B2 H2C 114(3) . . ? B5 B2 H2C 128(3) . . ? Ru4 B2 H2C 129(3) . . ? C1 B3 C8 115.1(5) . . ? C1 B3 B7 120.3(5) . . ? C8 B3 B7 57.1(4) . . ? C1 B3 B5 56.9(4) . . ? C8 B3 B5 60.8(4) . . ? B7 B3 B5 101.4(5) . . ? C1 B3 Ru4 65.5(3) . . ? C8 B3 Ru4 109.0(4) . . ? B7 B3 Ru4 64.5(3) . . ? B5 B3 Ru4 98.5(4) . . ? C1 B3 H3C 119(3) . . ? C8 B3 H3C 115(4) . . ? B7 B3 H3C 115(3) . . ? B5 B3 H3C 132(3) . . ? Ru4 B3 H3C 125(3) . . ? C1 B5 B11 135.5(5) . . ? C1 B5 B9 101.4(4) . . ? B11 B5 B9 56.5(4) . . ? C1 B5 C8 101.3(5) . . ? B11 B5 C8 54.8(4) . . ? B9 B5 C8 101.0(4) . . ? C1 B5 B3 49.9(3) . . ? B11 B5 B3 104.2(5) . . ? B9 B5 B3 119.9(5) . . ? C8 B5 B3 53.5(4) . . ? C1 B5 B2 47.5(3) . . ? B11 B5 B2 105.3(4) . . ? B9 B5 B2 54.9(3) . . ? C8 B5 B2 116.4(4) . . ? B3 B5 B2 86.4(4) . . ? C1 B5 H5C 114(3) . . ? B11 B5 H5C 110(3) . . ? B9 B5 H5C 120(3) . . ? C8 B5 H5C 116(3) . . ? B3 B5 H5C 120(3) . . ? B2 B5 H5C 127(3) . . ? B12 B6 B9 58.9(4) . . ? B12 B6 B10 60.7(4) . . ? B9 B6 B10 107.2(5) . . ? B12 B6 B2 114.4(5) . . ? B9 B6 B2 60.8(4) . . ? B10 B6 B2 119.4(5) . . ? B12 B6 Ru4 116.5(4) . . ? B9 B6 Ru4 112.4(4) . . ? B10 B6 Ru4 65.6(3) . . ? B2 B6 Ru4 67.0(3) . . ? B12 B6 H6C 118(3) . . ? B9 B6 H6C 118(3) . . ? B10 B6 H6C 124(3) . . ? B2 B6 H6C 111(3) . . ? Ru4 B6 H6C 119(3) . . ? C8 B7 B13 58.7(3) . . ? C8 B7 B10 105.5(5) . . ? B13 B7 B10 60.6(4) . . ? C8 B7 B3 57.5(4) . . ? B13 B7 B3 111.2(5) . . ? B10 B7 B3 117.2(5) . . ? C8 B7 Ru4 111.0(4) . . ? B13 B7 Ru4 118.5(6) . . ? B10 B7 Ru4 67.4(3) . . ? B3 B7 Ru4 66.6(3) . . ? C8 B7 H7C 115(4) . . ? B13 B7 H7C 120(3) . . ? B10 B7 H7C 131(3) . . ? B3 B7 H7C 108(3) . . ? Ru4 B7 H7C 118(3) . . ? C81 C8 B13 116.3(5) . . ? C81 C8 B11 118.2(5) . . ? B13 C8 B11 63.2(6) . . ? C81 C8 B7 119.0(6) . . ? B13 C8 B7 61.1(4) . . ? B11 C8 B7 112.4(5) . . ? C81 C8 B3 110.9(5) . . ? B13 C8 B3 120.5(4) . . ? B11 C8 B3 120.4(5) . . ? B7 C8 B3 65.4(4) . . ? C81 C8 B5 122.8(5) . . ? B13 C8 B5 111.4(6) . . ? B11 C8 B5 60.4(4) . . ? B7 C8 B5 110.6(4) . . ? B3 C8 B5 65.7(4) . . ? B12 B9 B11 61.2(4) . . ? B12 B9 B6 60.1(4) . . ? B11 B9 B6 108.3(5) . . ? B12 B9 B2 115.0(5) . . ? B11 B9 B2 119.0(5) . . ? B6 B9 B2 60.3(4) . . ? B12 B9 B5 108.8(5) . . ? B11 B9 B5 60.0(4) . . ? B6 B9 B5 106.8(5) . . ? B2 B9 B5 67.2(4) . . ? B12 B9 H9C 118(3) . . ? B11 B9 H9C 121(3) . . ? B6 B9 H9C 120(3) . . ? B2 B9 H9C 113(3) . . ? B5 B9 H9C 125(3) . . ? B13 B10 B7 58.6(5) . . ? B13 B10 B12 59.1(6) . . ? B7 B10 B12 108.0(5) . . ? B13 B10 B6 108.1(6) . . ? B7 B10 B6 114.7(5) . . ? B12 B10 B6 58.6(4) . . ? B13 B10 Ru4 115.6(4) . . ? B7 B10 Ru4 65.9(3) . . ? B12 B10 Ru4 116.8(4) . . ? B6 B10 Ru4 68.1(3) . . ? B13 B10 H10C 117(3) . . ? B7 B10 H10C 115(5) . . ? B12 B10 H10C 123(4) . . ? B6 B10 H10C 125(4) . . ? Ru4 B10 H10C 114(3) . . ? C8 B11 B9 114.5(5) . . ? C8 B11 B12 107.5(5) . . ? B9 B11 B12 59.2(4) . . ? C8 B11 B13 58.3(5) . . ? B9 B11 B13 109.3(5) . . ? B12 B11 B13 59.5(5) . . ? C8 B11 B5 64.8(4) . . ? B9 B11 B5 63.5(4) . . ? B12 B11 B5 110.0(5) . . ? B13 B11 B5 111.1(5) . . ? C8 B11 H11C 112(4) . . ? B9 B11 H11C 125(4) . . ? B12 B11 H11C 128(3) . . ? B13 B11 H11C 119(3) . . ? B5 B11 H11C 116(3) . . ? B9 B12 B6 61.1(4) . . ? B9 B12 B13 110.5(5) . . ? B6 B12 B13 110.5(5) . . ? B9 B12 B11 59.6(4) . . ? B6 B12 B11 107.8(5) . . ? B13 B12 B11 60.5(4) . . ? B9 B12 B10 109.0(5) . . ? B6 B12 B10 60.8(4) . . ? B13 B12 B10 59.9(4) . . ? B11 B12 B10 106.2(5) . . ? B9 B12 H12C 118(3) . . ? B6 B12 H12C 123(3) . . ? B13 B12 H12C 120(3) . . ? B11 B12 H12C 119(3) . . ? B10 B12 H12C 126(3) . . ? C8 B13 B7 60.2(4) . . ? C8 B13 B12 108.0(7) . . ? B7 B13 B12 111.3(5) . . ? C8 B13 B10 106.8(4) . . ? B7 B13 B10 60.8(4) . . ? B12 B13 B10 60.9(5) . . ? C8 B13 B11 58.5(4) . . ? B7 B13 B11 107.9(4) . . ? B12 B13 B11 60.0(6) . . ? B10 B13 B11 106.6(7) . . ? C8 B13 H13C 118(3) . . ? B7 B13 H13C 117(3) . . ? B12 B13 H13C 125(3) . . ? B10 B13 H13C 126(3) . . ? B11 B13 H13C 122(3) . . ? C12 C11 C16 118.3(6) . . ? C12 C11 C1 120.5(6) . . ? C16 C11 C1 121.0(6) . . ? C11 C12 C13 120.7(6) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 120.1(7) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.4(6) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 119.0(8) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C11 C16 C15 121.4(8) . . ? C11 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C45 C40 C41 116.1(6) . . ? C45 C40 C47 120.2(6) . . ? C41 C40 C47 123.5(6) . . ? C45 C40 Ru4 69.5(3) . . ? C41 C40 Ru4 70.5(3) . . ? C47 C40 Ru4 133.1(4) . . ? C42 C41 C40 121.0(6) . . ? C42 C41 Ru4 71.7(3) . . ? C40 C41 Ru4 72.5(3) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? Ru4 C41 H41 119.0 . . ? C43 C42 C41 121.5(6) . . ? C43 C42 Ru4 72.1(4) . . ? C41 C42 Ru4 71.7(3) . . ? C43 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? Ru4 C42 H42 118.7 . . ? C42 C43 C44 117.1(6) . . ? C42 C43 C46 120.5(6) . . ? C44 C43 C46 122.4(6) . . ? C42 C43 Ru4 71.6(4) . . ? C44 C43 Ru4 69.0(4) . . ? C46 C43 Ru4 129.2(4) . . ? C45 C44 C43 122.2(6) . . ? C45 C44 Ru4 72.9(4) . . ? C43 C44 Ru4 73.9(4) . . ? C45 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? Ru4 C44 H44 118.6 . . ? C44 C45 C40 122.1(6) . . ? C44 C45 Ru4 70.6(4) . . ? C40 C45 Ru4 73.7(3) . . ? C44 C45 H45 118.4 . . ? C40 C45 H45 118.4 . . ? Ru4 C45 H45 118.4 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C40 C47 C49 108.6(5) . . ? C40 C47 C48 112.8(5) . . ? C49 C47 C48 111.4(5) . . ? C40 C47 H47 107.9 . . ? C49 C47 H47 107.9 . . ? C48 C47 H47 107.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C82 C81 C86 118.5(6) . . ? C82 C81 C8 121.3(6) . . ? C86 C81 C8 120.2(6) . . ? C81 C82 C83 121.8(6) . . ? C81 C82 H82 119.1 . . ? C83 C82 H82 119.1 . . ? C82 C83 C84 118.8(7) . . ? C82 C83 H83 120.6 . . ? C84 C83 H83 120.6 . . ? C85 C84 C83 119.4(6) . . ? C85 C84 H84 120.3 . . ? C83 C84 H84 120.3 . . ? C84 C85 C86 122.6(6) . . ? C84 C85 H85 118.7 . . ? C86 C85 H85 118.7 . . ? C85 C86 C81 119.0(6) . . ? C85 C86 H86 120.5 . . ? C81 C86 H86 120.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.43 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.389 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.095 #===end data_7x81268 _database_code_depnum_ccdc_archive 'CCDC 631517' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 B10 Ru' _chemical_formula_sum 'C24 H34 B10 Ru' _chemical_formula_weight 531.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.144(4) _cell_length_b 13.209(2) _cell_length_c 18.065(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.439(8) _cell_angle_gamma 90.00 _cell_volume 4961.6(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2242 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 21.93 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 0.962 _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27682 _diffrn_reflns_av_R_equivalents 0.1297 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 23.34 _reflns_number_total 3583 _reflns_number_gt 2223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3583 _refine_ls_number_parameters 349 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.962 _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 Ru4 Ru 0.32625(2) 0.50491(4) 0.23389(2) 0.01402(18) Uani 1 1 d . . . C1 C 0.2596(3) 0.4725(4) 0.1292(3) 0.0163(15) Uani 1 1 d . . . B2 B 0.2511(4) 0.5860(5) 0.1469(4) 0.0149(16) Uani 1 1 d . . . H2 H 0.210(3) 0.611(4) 0.154(3) 0.018 Uiso 1 1 d . . . B3 B 0.3253(4) 0.4266(6) 0.1195(4) 0.0211(18) Uani 1 1 d . . . H3 H 0.325(3) 0.352(4) 0.115(3) 0.025 Uiso 1 1 d . . . B5 B 0.2816(4) 0.5391(5) 0.0518(4) 0.0183(17) Uani 1 1 d . . . H5 H 0.243(3) 0.520(4) -0.002(3) 0.022 Uiso 1 1 d . . . B6 B 0.3184(3) 0.6629(5) 0.1874(4) 0.0160(16) Uani 1 1 d . . . H6 H 0.309(2) 0.723(4) 0.221(3) 0.019 Uiso 1 1 d . . . B7 B 0.4003(3) 0.4887(6) 0.1572(4) 0.0202(16) Uani 1 1 d . . . H7 H 0.440(3) 0.440(4) 0.176(3) 0.024 Uiso 1 1 d . . . B8 B 0.3684(3) 0.4988(6) 0.0599(4) 0.0191(15) Uani 1 1 d . . . H8 H 0.387(2) 0.451(4) 0.013(3) 0.023 Uiso 1 1 d . . . B9 B 0.2870(3) 0.6723(5) 0.0902(4) 0.0159(16) Uani 1 1 d . . . H9 H 0.256(2) 0.737(4) 0.063(3) 0.019 Uiso 1 1 d . . . B10 B 0.3976(4) 0.6111(5) 0.1969(4) 0.0205(17) Uani 1 1 d . . . H10 H 0.432(3) 0.644(4) 0.236(3) 0.025 Uiso 1 1 d . . . B11 B 0.3443(3) 0.6222(6) 0.0409(4) 0.0210(18) Uani 1 1 d . . . H11 H 0.343(3) 0.656(4) -0.016(3) 0.025 Uiso 1 1 d . . . C12 C 0.3658(3) 0.6906(4) 0.1237(3) 0.0173(14) Uani 1 1 d . . . B13 B 0.4164(4) 0.5943(5) 0.1053(4) 0.0215(18) Uani 1 1 d . . . H13C H 0.462(3) 0.619(4) 0.094(3) 0.026 Uiso 1 1 d . . . C11 C 0.1991(3) 0.4090(4) 0.1121(3) 0.0162(14) Uani 1 1 d . . . C12C C 0.1465(3) 0.4254(4) 0.1468(3) 0.0204(15) Uani 1 1 d . . . H12 H 0.1501 0.4712 0.1879 0.024 Uiso 1 1 calc R . . C13 C 0.0886(3) 0.3754(5) 0.1221(3) 0.0247(16) Uani 1 1 d . . . H13 H 0.0525 0.3895 0.1449 0.030 Uiso 1 1 calc R . . C14 C 0.0833(3) 0.3046(4) 0.0637(3) 0.0255(16) Uani 1 1 d . . . H14 H 0.0443 0.2685 0.0480 0.031 Uiso 1 1 calc R . . C15 C 0.1357(3) 0.2879(5) 0.0295(3) 0.0253(16) Uani 1 1 d . . . H15 H 0.1322 0.2413 -0.0111 0.030 Uiso 1 1 calc R . . C16 C 0.1929(3) 0.3378(4) 0.0533(3) 0.0195(15) Uani 1 1 d . . . H16 H 0.2286 0.3240 0.0297 0.023 Uiso 1 1 calc R . . C40 C 0.3796(3) 0.3905(4) 0.3199(3) 0.0174(15) Uani 1 1 d . . . C41 C 0.3946(3) 0.4914(5) 0.3419(3) 0.0181(14) Uani 1 1 d . . . H4 H 0.4397 0.5160 0.3448 0.022 Uiso 1 1 calc R . . C42 C 0.3463(3) 0.5618(5) 0.3496(3) 0.0238(16) Uani 1 1 d . . . H42 H 0.3584 0.6346 0.3583 0.029 Uiso 1 1 calc R . . C43 C 0.2811(3) 0.5358(4) 0.3375(3) 0.0174(15) Uani 1 1 d U . . C44 C 0.2650(3) 0.4360(4) 0.3126(3) 0.0164(15) Uani 1 1 d . . . H44 H 0.2190 0.4191 0.2923 0.020 Uiso 1 1 calc R . . C45 C 0.3132(3) 0.3661(4) 0.3033(3) 0.0193(15) Uani 1 1 d . . . H45 H 0.3000 0.3012 0.2764 0.023 Uiso 1 1 calc R . . C46 C 0.2301(3) 0.6098(4) 0.3479(3) 0.0236(16) Uani 1 1 d . . . H46A H 0.1901 0.5932 0.3135 0.035 Uiso 1 1 calc R . . H46B H 0.2438 0.6783 0.3372 0.035 Uiso 1 1 calc R . . H46C H 0.2229 0.6065 0.3999 0.035 Uiso 1 1 calc R . . C47 C 0.4332(3) 0.3174(5) 0.3156(3) 0.0250(16) Uani 1 1 d . . . H47 H 0.4659 0.3539 0.2919 0.030 Uiso 1 1 calc R . . C48 C 0.4656(3) 0.2897(5) 0.3963(3) 0.0348(18) Uani 1 1 d . . . H48A H 0.4782 0.3517 0.4249 0.052 Uiso 1 1 calc R . . H48B H 0.5038 0.2484 0.3947 0.052 Uiso 1 1 calc R . . H48C H 0.4353 0.2513 0.4206 0.052 Uiso 1 1 calc R . . C49 C 0.4125(3) 0.2243(5) 0.2680(4) 0.0285(17) Uani 1 1 d . . . H49A H 0.3821 0.1847 0.2913 0.043 Uiso 1 1 calc R . . H49B H 0.4502 0.1828 0.2646 0.043 Uiso 1 1 calc R . . H49C H 0.3916 0.2453 0.2174 0.043 Uiso 1 1 calc R . . C121 C 0.3889(3) 0.7989(4) 0.1206(3) 0.0187(15) Uani 1 1 d . . . C122 C 0.4120(3) 0.8520(5) 0.1858(4) 0.0250(16) Uani 1 1 d . . . H122 H 0.4168 0.8182 0.2329 0.030 Uiso 1 1 calc R . . C123 C 0.4283(3) 0.9539(5) 0.1839(4) 0.0279(17) Uani 1 1 d . . . H123 H 0.4420 0.9897 0.2296 0.033 Uiso 1 1 calc R . . C124 C 0.4249(3) 1.0027(5) 0.1169(4) 0.0279(15) Uani 1 1 d . . . H124 H 0.4377 1.0716 0.1157 0.033 Uiso 1 1 calc R . . C125 C 0.4025(3) 0.9510(5) 0.0499(4) 0.0273(16) Uani 1 1 d . . . H125 H 0.3996 0.9847 0.0030 0.033 Uiso 1 1 calc R . . C126 C 0.3845(3) 0.8503(4) 0.0520(3) 0.0253(16) Uani 1 1 d . . . H126 H 0.3689 0.8156 0.0063 0.030 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 Ru4 0.0170(3) 0.0156(3) 0.0096(3) 0.0001(3) 0.00291(18) 0.0004(3) C1 0.025(4) 0.015(4) 0.010(3) 0.005(2) 0.006(3) -0.001(3) B2 0.019(4) 0.016(4) 0.011(4) 0.004(3) 0.005(3) 0.006(3) B3 0.025(5) 0.023(4) 0.014(4) -0.004(3) 0.001(3) -0.001(4) B5 0.022(4) 0.017(4) 0.015(4) -0.001(3) 0.003(3) 0.003(3) B6 0.016(4) 0.024(4) 0.008(4) 0.001(3) 0.002(3) 0.003(3) B7 0.021(4) 0.021(4) 0.020(4) 0.002(4) 0.006(3) 0.001(4) B8 0.020(4) 0.020(4) 0.018(4) -0.003(4) 0.006(3) 0.000(4) B9 0.020(4) 0.018(4) 0.010(4) 0.001(3) 0.004(3) 0.002(3) B10 0.028(5) 0.018(4) 0.016(4) -0.001(3) 0.004(4) 0.000(4) B11 0.022(5) 0.025(4) 0.016(4) 0.003(3) 0.002(4) -0.006(3) C12 0.025(4) 0.014(3) 0.013(3) 0.000(3) 0.005(3) 0.000(3) B13 0.026(5) 0.021(4) 0.018(4) -0.002(3) 0.007(4) 0.002(4) C11 0.018(4) 0.018(3) 0.012(3) 0.002(3) 0.000(3) -0.004(3) C12C 0.025(4) 0.024(4) 0.012(3) 0.000(3) 0.002(3) 0.000(3) C13 0.027(4) 0.026(4) 0.022(4) 0.007(3) 0.008(3) 0.000(3) C14 0.030(4) 0.019(4) 0.026(4) 0.004(3) -0.001(3) -0.007(3) C15 0.035(5) 0.019(4) 0.022(4) 0.000(3) 0.006(3) -0.001(3) C16 0.026(4) 0.016(3) 0.019(4) -0.001(3) 0.009(3) 0.001(3) C40 0.025(4) 0.021(4) 0.007(3) 0.005(3) 0.003(3) -0.001(3) C41 0.016(3) 0.023(4) 0.014(3) 0.003(3) 0.000(2) -0.005(3) C42 0.042(5) 0.019(4) 0.009(3) 0.002(3) 0.001(3) -0.001(3) C43 0.023(4) 0.027(4) 0.002(3) 0.002(3) 0.003(3) 0.004(3) C44 0.015(4) 0.023(4) 0.011(3) 0.003(3) 0.003(3) 0.005(3) C45 0.026(4) 0.021(4) 0.011(3) 0.001(3) 0.004(3) -0.005(3) C46 0.034(4) 0.024(4) 0.015(3) 0.000(3) 0.009(3) 0.006(3) C47 0.021(4) 0.032(4) 0.023(4) 0.003(3) 0.007(3) 0.002(3) C48 0.030(4) 0.048(5) 0.028(4) 0.015(4) 0.008(3) 0.018(4) C49 0.020(4) 0.022(4) 0.047(5) 0.000(3) 0.015(3) 0.005(3) C121 0.014(4) 0.022(4) 0.022(4) 0.002(3) 0.008(3) 0.006(3) C122 0.029(4) 0.023(4) 0.023(4) 0.003(3) 0.003(3) -0.008(3) C123 0.035(5) 0.027(4) 0.022(4) -0.010(3) 0.003(3) -0.008(3) C124 0.025(4) 0.018(3) 0.040(4) 0.008(4) 0.005(3) 0.001(4) C125 0.033(4) 0.023(4) 0.026(4) 0.009(3) 0.004(3) 0.000(3) C126 0.037(4) 0.018(4) 0.020(4) 0.001(3) 0.002(3) 0.005(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 Ru4 C1 2.186(6) . ? Ru4 C42 2.190(6) . ? Ru4 C41 2.215(5) . ? Ru4 B6 2.245(7) . ? Ru4 B10 2.247(7) . ? Ru4 C45 2.266(6) . ? Ru4 C44 2.278(6) . ? Ru4 B7 2.281(7) . ? Ru4 C43 2.286(5) . ? Ru4 B2 2.288(7) . ? Ru4 B3 2.307(7) . ? Ru4 C40 2.310(6) . ? C1 C11 1.514(8) . ? C1 B2 1.549(9) . ? C1 B3 1.553(9) . ? C1 B5 1.784(9) . ? B2 B9 1.791(9) . ? B2 B6 1.794(10) . ? B2 B5 2.037(9) . ? B2 H2 0.97(5) . ? B3 B8 1.804(10) . ? B3 B7 1.806(10) . ? B3 B5 2.037(10) . ? B3 H3 0.98(5) . ? B5 B11 1.760(10) . ? B5 B9 1.886(9) . ? B5 B8 1.891(10) . ? B5 H5 1.18(6) . ? B6 C12 1.697(9) . ? B6 B9 1.766(9) . ? B6 B10 1.787(10) . ? B6 H6 1.04(5) . ? B7 B13 1.748(10) . ? B7 B8 1.769(10) . ? B7 B10 1.774(10) . ? B7 H7 1.07(6) . ? B8 B11 1.724(10) . ? B8 B13 1.731(10) . ? B8 H8 1.17(5) . ? B9 C12 1.684(9) . ? B9 B11 1.758(10) . ? B9 H9 1.13(5) . ? B10 C12 1.727(9) . ? B10 B13 1.785(10) . ? B10 H10 1.01(5) . ? B11 C12 1.735(9) . ? B11 B13 1.781(10) . ? B11 H11 1.11(5) . ? C12 C121 1.516(8) . ? C12 B13 1.733(9) . ? B13 H13C 1.08(5) . ? C11 C12C 1.390(8) . ? C11 C16 1.408(8) . ? C12C C13 1.391(8) . ? C12C H12 0.9500 . ? C13 C14 1.398(8) . ? C13 H13 0.9500 . ? C14 C15 1.381(8) . ? C14 H14 0.9500 . ? C15 C16 1.375(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C40 C41 1.410(8) . ? C40 C45 1.420(8) . ? C40 C47 1.501(8) . ? C41 C42 1.406(8) . ? C41 H4 1.0000 . ? C42 C43 1.399(8) . ? C42 H42 1.0000 . ? C43 C44 1.413(8) . ? C43 C46 1.493(8) . ? C44 C45 1.407(8) . ? C44 H44 1.0000 . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C49 1.520(8) . ? C47 C48 1.537(8) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C121 C122 1.381(8) . ? C121 C126 1.401(8) . ? C122 C123 1.392(8) . ? C122 H122 0.9500 . ? C123 C124 1.361(8) . ? C123 H123 0.9500 . ? C124 C125 1.395(9) . ? C124 H124 0.9500 . ? C125 C126 1.387(8) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru4 C42 151.2(2) . . ? C1 Ru4 C41 164.1(2) . . ? C42 Ru4 C41 37.2(2) . . ? C1 Ru4 B6 82.3(2) . . ? C42 Ru4 B6 91.5(2) . . ? C41 Ru4 B6 113.4(2) . . ? C1 Ru4 B10 103.1(2) . . ? C42 Ru4 B10 92.6(3) . . ? C41 Ru4 B10 86.9(2) . . ? B6 Ru4 B10 46.9(3) . . ? C1 Ru4 C45 101.3(2) . . ? C42 Ru4 C45 76.8(2) . . ? C41 Ru4 C45 64.7(2) . . ? B6 Ru4 C45 162.0(2) . . ? B10 Ru4 C45 145.6(3) . . ? C1 Ru4 C44 96.4(2) . . ? C42 Ru4 C44 64.8(2) . . ? C41 Ru4 C44 76.8(2) . . ? B6 Ru4 C44 126.4(2) . . ? B10 Ru4 C44 157.3(2) . . ? C45 Ru4 C44 36.1(2) . . ? C1 Ru4 B7 82.1(2) . . ? C42 Ru4 B7 125.3(3) . . ? C41 Ru4 B7 96.8(2) . . ? B6 Ru4 B7 82.6(3) . . ? B10 Ru4 B7 46.1(3) . . ? C45 Ru4 B7 115.2(2) . . ? C44 Ru4 B7 150.7(2) . . ? C1 Ru4 C43 116.3(2) . . ? C42 Ru4 C43 36.3(2) . . ? C41 Ru4 C43 66.1(2) . . ? B6 Ru4 C43 97.3(2) . . ? B10 Ru4 C43 122.3(2) . . ? C45 Ru4 C43 65.2(2) . . ? C44 Ru4 C43 36.1(2) . . ? B7 Ru4 C43 161.5(2) . . ? C1 Ru4 B2 40.4(2) . . ? C42 Ru4 B2 119.0(2) . . ? C41 Ru4 B2 154.6(2) . . ? B6 Ru4 B2 46.6(2) . . ? B10 Ru4 B2 85.6(3) . . ? C45 Ru4 B2 128.3(2) . . ? C44 Ru4 B2 102.3(2) . . ? B7 Ru4 B2 95.4(3) . . ? C43 Ru4 B2 97.9(2) . . ? C1 Ru4 B3 40.3(2) . . ? C42 Ru4 B3 167.9(3) . . ? C41 Ru4 B3 130.7(2) . . ? B6 Ru4 B3 95.4(3) . . ? B10 Ru4 B3 84.9(3) . . ? C45 Ru4 B3 98.7(2) . . ? C44 Ru4 B3 117.8(2) . . ? B7 Ru4 B3 46.3(3) . . ? C43 Ru4 B3 151.1(3) . . ? B2 Ru4 B3 72.7(3) . . ? C1 Ru4 C40 127.9(2) . . ? C42 Ru4 C40 66.2(2) . . ? C41 Ru4 C40 36.2(2) . . ? B6 Ru4 C40 148.6(2) . . ? B10 Ru4 C40 109.6(2) . . ? C45 Ru4 C40 36.1(2) . . ? C44 Ru4 C40 65.3(2) . . ? B7 Ru4 C40 92.4(2) . . ? C43 Ru4 C40 78.0(2) . . ? B2 Ru4 C40 164.1(2) . . ? B3 Ru4 C40 103.5(2) . . ? C11 C1 B2 116.9(5) . . ? C11 C1 B3 120.0(5) . . ? B2 C1 B3 122.7(6) . . ? C11 C1 B5 116.4(5) . . ? B2 C1 B5 75.0(4) . . ? B3 C1 B5 74.9(4) . . ? C11 C1 Ru4 132.3(4) . . ? B2 C1 Ru4 73.4(3) . . ? B3 C1 Ru4 74.0(4) . . ? B5 C1 Ru4 111.3(4) . . ? C1 B2 B9 114.9(5) . . ? C1 B2 B6 121.2(5) . . ? B9 B2 B6 59.0(4) . . ? C1 B2 B5 57.7(3) . . ? B9 B2 B5 58.6(3) . . ? B6 B2 B5 99.6(4) . . ? C1 B2 Ru4 66.2(3) . . ? B9 B2 Ru4 112.2(4) . . ? B6 B2 Ru4 65.4(3) . . ? B5 B2 Ru4 98.7(3) . . ? C1 B2 H2 120(3) . . ? B9 B2 H2 110(3) . . ? B6 B2 H2 115(3) . . ? B5 B2 H2 131(3) . . ? Ru4 B2 H2 127(3) . . ? C1 B3 B8 114.8(5) . . ? C1 B3 B7 121.5(5) . . ? B8 B3 B7 58.7(4) . . ? C1 B3 B5 57.7(4) . . ? B8 B3 B5 58.6(4) . . ? B7 B3 B5 99.6(5) . . ? C1 B3 Ru4 65.6(3) . . ? B8 B3 Ru4 112.0(4) . . ? B7 B3 Ru4 66.1(3) . . ? B5 B3 Ru4 98.1(4) . . ? C1 B3 H3 114(3) . . ? B8 B3 H3 118(3) . . ? B7 B3 H3 118(3) . . ? B5 B3 H3 133(3) . . ? Ru4 B3 H3 122(3) . . ? B11 B5 C1 134.7(5) . . ? B11 B5 B9 57.5(4) . . ? C1 B5 B9 100.3(4) . . ? B11 B5 B8 56.2(4) . . ? C1 B5 B8 100.8(4) . . ? B9 B5 B8 103.9(5) . . ? B11 B5 B3 104.7(5) . . ? C1 B5 B3 47.4(3) . . ? B9 B5 B3 118.0(5) . . ? B8 B5 B3 54.5(3) . . ? B11 B5 B2 105.4(5) . . ? C1 B5 B2 47.3(3) . . ? B9 B5 B2 54.2(3) . . ? B8 B5 B2 118.1(5) . . ? B3 B5 B2 83.9(4) . . ? B11 B5 H5 118(3) . . ? C1 B5 H5 107(3) . . ? B9 B5 H5 119(2) . . ? B8 B5 H5 121(3) . . ? B3 B5 H5 121(2) . . ? B2 B5 H5 119(3) . . ? C12 B6 B9 58.2(4) . . ? C12 B6 B10 59.4(4) . . ? B9 B6 B10 107.5(5) . . ? C12 B6 B2 111.6(5) . . ? B9 B6 B2 60.4(4) . . ? B10 B6 B2 118.8(5) . . ? C12 B6 Ru4 116.2(4) . . ? B9 B6 Ru4 115.3(4) . . ? B10 B6 Ru4 66.6(3) . . ? B2 B6 Ru4 68.0(3) . . ? C12 B6 H6 116(3) . . ? B9 B6 H6 117(3) . . ? B10 B6 H6 121(3) . . ? B2 B6 H6 117(3) . . ? Ru4 B6 H6 120(3) . . ? B13 B7 B8 59.0(4) . . ? B13 B7 B10 60.9(4) . . ? B8 B7 B10 107.4(5) . . ? B13 B7 B3 113.8(5) . . ? B8 B7 B3 60.6(4) . . ? B10 B7 B3 118.4(5) . . ? B13 B7 Ru4 118.2(4) . . ? B8 B7 Ru4 114.6(4) . . ? B10 B7 Ru4 65.9(3) . . ? B3 B7 Ru4 67.6(3) . . ? B13 B7 H7 116(3) . . ? B8 B7 H7 120(3) . . ? B10 B7 H7 120(3) . . ? B3 B7 H7 116(3) . . ? Ru4 B7 H7 117(3) . . ? B11 B8 B13 62.1(4) . . ? B11 B8 B7 108.3(5) . . ? B13 B8 B7 59.9(4) . . ? B11 B8 B3 117.1(5) . . ? B13 B8 B3 114.8(5) . . ? B7 B8 B3 60.7(4) . . ? B11 B8 B5 58.0(4) . . ? B13 B8 B5 108.0(5) . . ? B7 B8 B5 106.8(5) . . ? B3 B8 B5 66.9(4) . . ? B11 B8 H8 119(3) . . ? B13 B8 H8 119(3) . . ? B7 B8 H8 124(3) . . ? B3 B8 H8 115(3) . . ? B5 B8 H8 123(3) . . ? C12 B9 B11 60.5(4) . . ? C12 B9 B6 58.9(4) . . ? B11 B9 B6 107.9(5) . . ? C12 B9 B2 112.3(5) . . ? B11 B9 B2 116.9(5) . . ? B6 B9 B2 60.6(4) . . ? C12 B9 B5 104.8(5) . . ? B11 B9 B5 57.6(4) . . ? B6 B9 B5 106.7(5) . . ? B2 B9 B5 67.2(4) . . ? C12 B9 H9 120(3) . . ? B11 B9 H9 118(3) . . ? B6 B9 H9 124(3) . . ? B2 B9 H9 117(3) . . ? B5 B9 H9 124(3) . . ? C12 B10 B7 106.3(5) . . ? C12 B10 B13 59.1(4) . . ? B7 B10 B13 58.8(4) . . ? C12 B10 B6 57.7(4) . . ? B7 B10 B6 114.1(5) . . ? B13 B10 B6 108.7(5) . . ? C12 B10 Ru4 114.7(4) . . ? B7 B10 Ru4 68.0(3) . . ? B13 B10 Ru4 118.2(4) . . ? B6 B10 Ru4 66.5(3) . . ? C12 B10 H10 113(3) . . ? B7 B10 H10 127(3) . . ? B13 B10 H10 116(3) . . ? B6 B10 H10 116(3) . . ? Ru4 B10 H10 120(3) . . ? B8 B11 C12 107.4(5) . . ? B8 B11 B9 117.4(5) . . ? C12 B11 B9 57.6(4) . . ? B8 B11 B5 65.8(4) . . ? C12 B11 B5 108.3(5) . . ? B9 B11 B5 64.9(4) . . ? B8 B11 B13 59.1(4) . . ? C12 B11 B13 59.0(4) . . ? B9 B11 B13 109.5(5) . . ? B5 B11 B13 111.8(5) . . ? B8 B11 H11 121(3) . . ? C12 B11 H11 123(3) . . ? B9 B11 H11 114(3) . . ? B5 B11 H11 118(3) . . ? B13 B11 H11 123(3) . . ? C121 C12 B9 115.2(5) . . ? C121 C12 B6 117.5(5) . . ? B9 C12 B6 63.0(4) . . ? C121 C12 B10 121.2(5) . . ? B9 C12 B10 114.2(5) . . ? B6 C12 B10 62.9(4) . . ? C121 C12 B13 118.2(5) . . ? B9 C12 B13 115.6(5) . . ? B6 C12 B13 115.6(5) . . ? B10 C12 B13 62.1(4) . . ? C121 C12 B11 119.7(5) . . ? B9 C12 B11 61.9(4) . . ? B6 C12 B11 112.2(5) . . ? B10 C12 B11 110.4(5) . . ? B13 C12 B11 61.8(4) . . ? B8 B13 C12 107.2(5) . . ? B8 B13 B7 61.1(4) . . ? C12 B13 B7 107.2(5) . . ? B8 B13 B11 58.8(4) . . ? C12 B13 B11 59.2(4) . . ? B7 B13 B11 106.7(5) . . ? B8 B13 B10 108.6(5) . . ? C12 B13 B10 58.8(4) . . ? B7 B13 B10 60.3(4) . . ? B11 B13 B10 105.7(5) . . ? B8 B13 H13C 127(3) . . ? C12 B13 H13C 115(3) . . ? B7 B13 H13C 128(3) . . ? B11 B13 H13C 120(3) . . ? B10 B13 H13C 120(3) . . ? C12C C11 C16 118.1(5) . . ? C12C C11 C1 122.5(5) . . ? C16 C11 C1 119.0(5) . . ? C11 C12C C13 120.7(6) . . ? C11 C12C H12 119.6 . . ? C13 C12C H12 119.6 . . ? C12C C13 C14 120.4(6) . . ? C12C C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 118.9(6) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C16 C15 C14 121.0(6) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C11 120.9(6) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? C41 C40 C45 115.9(5) . . ? C41 C40 C47 119.3(5) . . ? C45 C40 C47 124.8(5) . . ? C41 C40 Ru4 68.2(3) . . ? C45 C40 Ru4 70.3(3) . . ? C47 C40 Ru4 131.9(4) . . ? C42 C41 C40 121.5(6) . . ? C42 C41 Ru4 70.4(3) . . ? C40 C41 Ru4 75.5(3) . . ? C42 C41 H4 118.9 . . ? C40 C41 H4 118.9 . . ? Ru4 C41 H4 118.9 . . ? C43 C42 C41 122.3(6) . . ? C43 C42 Ru4 75.6(3) . . ? C41 C42 Ru4 72.4(3) . . ? C43 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? Ru4 C42 H42 118.7 . . ? C42 C43 C44 116.9(5) . . ? C42 C43 C46 122.2(5) . . ? C44 C43 C46 120.9(6) . . ? C42 C43 Ru4 68.1(3) . . ? C44 C43 Ru4 71.7(3) . . ? C46 C43 Ru4 129.7(4) . . ? C45 C44 C43 120.8(6) . . ? C45 C44 Ru4 71.5(3) . . ? C43 C44 Ru4 72.3(3) . . ? C45 C44 H44 119.1 . . ? C43 C44 H44 119.1 . . ? Ru4 C44 H44 119.1 . . ? C44 C45 C40 122.4(6) . . ? C44 C45 Ru4 72.4(3) . . ? C40 C45 Ru4 73.6(3) . . ? C44 C45 H45 118.4 . . ? C40 C45 H45 118.4 . . ? Ru4 C45 H45 118.4 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C40 C47 C49 114.0(5) . . ? C40 C47 C48 108.3(5) . . ? C49 C47 C48 112.2(5) . . ? C40 C47 H47 107.3 . . ? C49 C47 H47 107.3 . . ? C48 C47 H47 107.3 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C122 C121 C126 117.7(6) . . ? C122 C121 C12 121.0(5) . . ? C126 C121 C12 121.2(5) . . ? C121 C122 C123 121.4(6) . . ? C121 C122 H122 119.3 . . ? C123 C122 H122 119.3 . . ? C124 C123 C122 120.5(6) . . ? C124 C123 H123 119.8 . . ? C122 C123 H123 119.8 . . ? C123 C124 C125 119.6(6) . . ? C123 C124 H124 120.2 . . ? C125 C124 H124 120.2 . . ? C126 C125 C124 119.9(6) . . ? C126 C125 H125 120.1 . . ? C124 C125 H125 120.1 . . ? C125 C126 C121 121.0(6) . . ? C125 C126 H126 119.5 . . ? C121 C126 H126 119.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.474 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.113