# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Alan Welch' _publ_contact_author_name 'Alan Welch' _publ_contact_author_email a.j.welch@hw.ac.uk _publ_section_title ; The first supraicosahedral bis(heteroborane) ; # Attachment '3276--meso-.cif' data_3276 _database_code_depnum_ccdc_archive 'CCDC 784591' #TrackingRef '3276--meso-.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H32 B20 Co2, C H2 Cl2' _chemical_formula_sum 'C15 H34 B20 Cl2 Co2' _chemical_formula_weight 619.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.4896(13) _cell_length_b 9.1544(10) _cell_length_c 26.426(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.146(6) _cell_angle_gamma 90.00 _cell_volume 2757.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9922 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 31.28 _exptl_crystal_description NEEDLE _exptl_crystal_colour red _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4958 _exptl_absorpt_correction_T_max 0.9459 _exptl_absorpt_process_details 'SADABS (Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65593 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 32.01 _reflns_number_total 9467 _reflns_number_gt 6930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+1.5731P] 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 9467 _refine_ls_number_parameters 367 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 C1 C 0.00827(15) 0.3869(2) 0.12158(7) 0.0094(3) Uani 1 1 d . . . B2 B -0.00647(19) 0.3668(2) 0.06270(8) 0.0123(4) Uani 1 1 d . . . H2 H 0.0479 0.4462 0.0435 0.015 Uiso 1 1 calc R . . B3 B -0.07110(19) 0.3085(2) 0.15631(8) 0.0117(4) Uani 1 1 d . . . H3 H -0.0581 0.3464 0.1969 0.014 Uiso 1 1 calc R . . Co4 Co -0.16672(2) 0.43693(3) 0.093289(10) 0.01023(7) Uani 1 1 d . . . B5 B 0.03371(19) 0.1990(2) 0.10871(8) 0.0126(4) Uani 1 1 d . . . H5 H 0.125(2) 0.170(3) 0.1220(9) 0.015 Uiso 1 1 d . . . C6 C -0.13593(17) 0.2962(2) 0.03186(7) 0.0125(3) Uani 1 1 d . . . H6 H -0.1608 0.3508 -0.0059 0.015 Uiso 1 1 calc R . . B7 B -0.21212(19) 0.2359(2) 0.13039(8) 0.0137(4) Uani 1 1 d . . . H7 H -0.2819 0.2460 0.1563 0.016 Uiso 1 1 calc R . . B8 B -0.0905(2) 0.1169(2) 0.14103(8) 0.0137(4) Uani 1 1 d . . . H8 H -0.0723 0.0456 0.1756 0.016 Uiso 1 1 calc R . . B9 B -0.0197(2) 0.1815(2) 0.03922(8) 0.0134(4) Uani 1 1 d . . . H9 H 0.0395 0.1526 0.0101 0.016 Uiso 1 1 calc R . . B10 B -0.2509(2) 0.2430(2) 0.06188(8) 0.0140(4) Uani 1 1 d . . . H10 H -0.3438 0.2646 0.0453 0.017 Uiso 1 1 calc R . . B11 B -0.0563(2) 0.0497(2) 0.08286(9) 0.0147(4) Uani 1 1 d . . . H11 H -0.0152 -0.0613 0.0825 0.018 Uiso 1 1 calc R . . B12 B -0.1626(2) 0.1147(2) 0.03263(9) 0.0157(4) Uani 1 1 d . . . H12 H -0.1973 0.0482 -0.0015 0.019 Uiso 1 1 calc R . . B13 B -0.2069(2) 0.0757(2) 0.09348(9) 0.0153(4) Uani 1 1 d . . . H13 H -0.2695 -0.0160 0.0976 0.018 Uiso 1 1 calc R . . C41 C -0.24525(18) 0.5816(2) 0.13764(8) 0.0167(4) Uani 1 1 d . . . H41 H -0.2474 0.5735 0.1752 0.020 Uiso 1 1 calc R . . C42 C -0.15929(17) 0.6578(2) 0.11341(8) 0.0149(4) Uani 1 1 d . . . H42 H -0.0892 0.7095 0.1312 0.018 Uiso 1 1 calc R . . C43 C -0.18802(18) 0.6450(2) 0.05991(8) 0.0159(4) Uani 1 1 d . . . H43 H -0.1424 0.6860 0.0334 0.019 Uiso 1 1 calc R . . C44 C -0.29267(19) 0.5604(2) 0.05083(8) 0.0183(4) Uani 1 1 d . . . H44 H -0.3342 0.5335 0.0166 0.022 Uiso 1 1 calc R . . C45 C -0.32953(18) 0.5224(2) 0.09887(9) 0.0182(4) Uani 1 1 d . . . H45 H -0.4016 0.4662 0.1043 0.022 Uiso 1 1 calc R . . C1' C 0.11143(16) 0.4795(2) 0.14488(7) 0.0099(3) Uani 1 1 d . . . B2' B 0.09358(19) 0.5912(2) 0.18710(8) 0.0119(4) Uani 1 1 d . . . H2' H 0.0081 0.5792 0.2030 0.014 Uiso 1 1 calc R . . B3' B 0.23053(19) 0.4603(2) 0.12272(8) 0.0122(4) Uani 1 1 d . . . H3' H 0.2304 0.3646 0.0963 0.015 Uiso 1 1 calc R . . Co4' Co 0.23759(2) 0.43922(3) 0.207482(9) 0.00954(6) Uani 1 1 d . . . B5' B 0.14517(19) 0.6490(2) 0.11647(8) 0.0124(4) Uani 1 1 d . . . H5' H 0.079(2) 0.673(3) 0.0846(9) 0.015 Uiso 1 1 d . . . C6' C 0.21451(17) 0.6666(2) 0.22273(7) 0.0127(3) Uani 1 1 d . . . H6' H 0.1959 0.6869 0.2627 0.015 Uiso 1 1 calc R . . B7' B 0.36700(19) 0.5171(2) 0.15965(8) 0.0132(4) Uani 1 1 d . . . H7' H 0.4434 0.4422 0.1578 0.016 Uiso 1 1 calc R . . B8' B 0.30470(19) 0.6254(2) 0.10784(8) 0.0141(4) Uani 1 1 d . . . H8' H 0.3365 0.6254 0.0694 0.017 Uiso 1 1 calc R . . B9' B 0.15006(19) 0.7722(2) 0.17460(8) 0.0135(4) Uani 1 1 d . . . H9' H 0.0847 0.8619 0.1771 0.016 Uiso 1 1 calc R . . B10' B 0.35525(19) 0.6206(2) 0.21664(9) 0.0139(4) Uani 1 1 d . . . H10' H 0.4223 0.6057 0.2508 0.017 Uiso 1 1 calc R . . B11' B 0.2544(2) 0.7890(2) 0.13162(9) 0.0146(4) Uani 1 1 d . . . H11' H 0.2509 0.8882 0.1066 0.018 Uiso 1 1 calc R . . B12' B 0.2969(2) 0.7966(2) 0.19935(9) 0.0155(4) Uani 1 1 d . . . H12' H 0.3269 0.8987 0.2205 0.019 Uiso 1 1 calc R . . B13' B 0.3899(2) 0.7078(2) 0.15983(9) 0.0153(4) Uani 1 1 d . . . H13' H 0.4787 0.7542 0.1562 0.018 Uiso 1 1 calc R . . C41' C 0.29722(19) 0.2266(2) 0.21545(8) 0.0170(4) Uani 1 1 d . . . H41' H 0.3295 0.1669 0.1887 0.020 Uiso 1 1 calc R . . C42' C 0.36235(18) 0.3201(2) 0.25144(8) 0.0176(4) Uani 1 1 d . . . H42' H 0.4490 0.3370 0.2548 0.021 Uiso 1 1 calc R . . C43' C 0.28248(18) 0.3836(2) 0.28270(7) 0.0158(4) Uani 1 1 d . . . H43' H 0.3035 0.4532 0.3115 0.019 Uiso 1 1 calc R . . C44' C 0.16783(18) 0.3282(2) 0.26605(7) 0.0144(4) Uani 1 1 d . . . H44' H 0.0942 0.3540 0.2806 0.017 Uiso 1 1 calc R . . C45' C 0.17703(18) 0.2312(2) 0.22503(7) 0.0140(4) Uani 1 1 d . . . H45' H 0.1105 0.1775 0.2053 0.017 Uiso 1 1 calc R . . Cl1 Cl 0.48625(5) 0.09541(7) 0.12994(2) 0.02888(13) Uani 1 1 d D B . C1S C 0.4603(2) 0.0357(3) 0.06602(9) 0.0249(5) Uani 1 1 d D . . H1A H 0.4093 -0.0518 0.0640 0.030 Uiso 1 1 calc R A 1 H1B H 0.5357 0.0077 0.0542 0.030 Uiso 1 1 calc R A 1 Cl2 Cl 0.39260(6) 0.17366(7) 0.02573(3) 0.03204(15) Uani 0.95 1 d PD B 1 Cl2A Cl 0.502(2) -0.134(2) 0.0413(11) 0.094(8) Uani 0.05 1 d PDU B 2 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 C1 0.0080(8) 0.0089(7) 0.0107(8) 0.0005(6) -0.0011(6) 0.0014(6) B2 0.0136(10) 0.0121(9) 0.0106(9) -0.0001(7) -0.0009(7) 0.0001(7) B3 0.0123(9) 0.0117(9) 0.0106(9) 0.0004(7) -0.0004(7) -0.0009(7) Co4 0.00934(12) 0.01047(12) 0.01021(12) 0.00056(9) -0.00143(9) -0.00023(9) B5 0.0130(9) 0.0124(9) 0.0121(9) -0.0012(7) 0.0004(7) -0.0001(7) C6 0.0139(9) 0.0123(8) 0.0104(8) -0.0006(6) -0.0023(7) -0.0017(7) B7 0.0128(10) 0.0139(9) 0.0137(9) 0.0003(8) -0.0012(8) -0.0029(7) B8 0.0154(10) 0.0121(9) 0.0131(9) 0.0008(8) -0.0002(8) -0.0023(8) B9 0.0159(10) 0.0137(9) 0.0106(9) -0.0019(7) 0.0009(7) -0.0007(8) B10 0.0131(10) 0.0142(9) 0.0137(9) -0.0005(8) -0.0017(8) -0.0035(7) B11 0.0166(10) 0.0118(9) 0.0151(10) -0.0013(8) -0.0007(8) -0.0016(8) B12 0.0186(11) 0.0130(10) 0.0146(10) -0.0003(8) -0.0019(8) -0.0016(8) B13 0.0153(10) 0.0148(10) 0.0150(10) 0.0003(8) -0.0013(8) -0.0036(8) C41 0.0168(9) 0.0153(9) 0.0183(9) -0.0011(7) 0.0033(7) 0.0037(7) C42 0.0138(9) 0.0124(8) 0.0178(9) -0.0005(7) -0.0013(7) 0.0017(7) C43 0.0161(9) 0.0141(9) 0.0171(9) 0.0039(7) -0.0004(7) 0.0030(7) C44 0.0159(10) 0.0156(9) 0.0211(10) 0.0022(8) -0.0064(8) 0.0040(7) C45 0.0111(9) 0.0184(9) 0.0248(10) -0.0010(8) 0.0014(8) 0.0013(7) C1' 0.0092(8) 0.0109(8) 0.0088(7) 0.0015(6) -0.0025(6) -0.0007(6) B2' 0.0117(9) 0.0125(9) 0.0108(9) 0.0005(7) -0.0009(7) 0.0004(7) B3' 0.0122(9) 0.0139(9) 0.0099(9) 0.0009(7) -0.0008(7) -0.0009(7) Co4' 0.00938(12) 0.01006(12) 0.00857(11) 0.00085(9) -0.00134(9) 0.00039(9) B5' 0.0121(9) 0.0122(9) 0.0123(9) 0.0018(7) -0.0005(7) -0.0008(7) C6' 0.0139(9) 0.0115(8) 0.0119(8) -0.0001(7) -0.0013(7) -0.0011(6) B7' 0.0120(9) 0.0148(9) 0.0124(9) 0.0003(8) 0.0001(7) -0.0001(7) B8' 0.0120(10) 0.0181(10) 0.0118(9) 0.0025(8) -0.0002(7) -0.0030(8) B9' 0.0141(10) 0.0116(9) 0.0134(9) 0.0006(8) -0.0031(8) -0.0020(7) B10' 0.0131(10) 0.0133(9) 0.0142(9) 0.0012(8) -0.0024(8) -0.0014(8) B11' 0.0141(10) 0.0142(10) 0.0147(10) 0.0018(8) -0.0012(8) -0.0029(8) B12' 0.0162(10) 0.0132(10) 0.0161(10) 0.0001(8) -0.0025(8) -0.0039(8) B13' 0.0116(10) 0.0179(10) 0.0158(10) 0.0027(8) -0.0012(8) -0.0037(8) C41' 0.0202(10) 0.0129(9) 0.0173(9) 0.0021(7) 0.0008(8) 0.0051(7) C42' 0.0149(9) 0.0189(9) 0.0175(9) 0.0078(8) -0.0038(7) 0.0032(7) C43' 0.0196(10) 0.0158(9) 0.0105(8) 0.0036(7) -0.0049(7) -0.0008(7) C44' 0.0167(9) 0.0132(8) 0.0130(8) 0.0024(7) 0.0004(7) 0.0001(7) C45' 0.0173(9) 0.0117(8) 0.0121(8) 0.0036(7) -0.0018(7) 0.0006(7) Cl1 0.0231(3) 0.0373(3) 0.0266(3) -0.0056(2) 0.0045(2) -0.0020(2) C1S 0.0249(12) 0.0235(11) 0.0256(11) 0.0002(9) 0.0008(9) 0.0011(9) Cl2 0.0267(3) 0.0305(3) 0.0366(3) 0.0055(3) -0.0054(3) 0.0044(2) Cl2A 0.087(11) 0.096(11) 0.100(11) -0.006(9) 0.009(8) -0.001(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C1' 1.523(3) . ? C1 B3 1.548(3) . ? C1 B2 1.555(3) . ? C1 B5 1.785(3) . ? C1 Co4 2.1063(18) . ? B2 C6 1.730(3) . ? B2 B9 1.806(3) . ? B2 B5 1.978(3) . ? B2 Co4 2.197(2) . ? B3 B7 1.806(3) . ? B3 B8 1.808(3) . ? B3 B5 2.101(3) . ? B3 Co4 2.215(2) . ? Co4 C45 2.050(2) . ? Co4 C41 2.050(2) . ? Co4 C44 2.056(2) . ? Co4 C42 2.090(2) . ? Co4 C43 2.100(2) . ? Co4 C6 2.1360(19) . ? Co4 B10 2.139(2) . ? Co4 B7 2.179(2) . ? B5 B11 1.797(3) . ? B5 B9 1.869(3) . ? B5 B8 1.907(3) . ? C6 B12 1.691(3) . ? C6 B9 1.691(3) . ? C6 B10 1.695(3) . ? B7 B13 1.767(3) . ? B7 B8 1.767(3) . ? B7 B10 1.811(3) . ? B8 B11 1.745(3) . ? B8 B13 1.758(3) . ? B9 B12 1.741(3) . ? B9 B11 1.756(3) . ? B10 B13 1.787(3) . ? B10 B12 1.789(3) . ? B11 B12 1.790(3) . ? B11 B13 1.802(3) . ? B12 B13 1.782(3) . ? C41 C42 1.425(3) . ? C41 C45 1.426(3) . ? C42 C43 1.416(3) . ? C43 C44 1.425(3) . ? C44 C45 1.430(3) . ? C1' B2' 1.546(3) . ? C1' B3' 1.564(3) . ? C1' B5' 1.788(3) . ? C1' Co4' 2.0921(18) . ? B2' C6' 1.723(3) . ? B2' B9' 1.825(3) . ? B2' B5' 2.095(3) . ? B2' Co4' 2.178(2) . ? B3' B8' 1.803(3) . ? B3' B7' 1.817(3) . ? B3' B5' 1.983(3) . ? B3' Co4' 2.240(2) . ? Co4' C42' 2.0441(19) . ? Co4' C43' 2.0547(19) . ? Co4' C41' 2.065(2) . ? Co4' C44' 2.093(2) . ? Co4' C45' 2.099(2) . ? Co4' B10' 2.136(2) . ? Co4' C6' 2.1426(19) . ? Co4' B7' 2.187(2) . ? B5' B11' 1.804(3) . ? B5' B8' 1.887(3) . ? B5' B9' 1.901(3) . ? C6' B12' 1.685(3) . ? C6' B9' 1.693(3) . ? C6' B10' 1.698(3) . ? B7' B13' 1.766(3) . ? B7' B8' 1.768(3) . ? B7' B10' 1.798(3) . ? B8' B11' 1.750(3) . ? B8' B13' 1.755(3) . ? B9' B12' 1.746(3) . ? B9' B11' 1.758(3) . ? B10' B12' 1.783(3) . ? B10' B13' 1.788(3) . ? B11' B12' 1.797(3) . ? B11' B13' 1.801(3) . ? B12' B13' 1.781(3) . ? C41' C42' 1.421(3) . ? C41' C45' 1.435(3) . ? C42' C43' 1.432(3) . ? C43' C44' 1.429(3) . ? C44' C45' 1.416(3) . ? Cl1 C1S 1.765(2) . ? C1S Cl2 1.768(2) . ? C1S Cl2A 1.773(15) . ? 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' C1 B3 120.28(15) . . ? C1' C1 B2 116.93(16) . . ? B3 C1 B2 122.63(16) . . ? C1' C1 B5 118.39(14) . . ? B3 C1 B5 77.80(13) . . ? B2 C1 B5 72.25(13) . . ? C1' C1 Co4 133.07(13) . . ? B3 C1 Co4 72.82(10) . . ? B2 C1 Co4 71.96(10) . . ? B5 C1 Co4 108.28(11) . . ? C1 B2 C6 119.72(16) . . ? C1 B2 B9 116.69(16) . . ? C6 B2 B9 57.11(12) . . ? C1 B2 B5 59.26(11) . . ? C6 B2 B5 96.94(13) . . ? B9 B2 B5 59.00(11) . . ? C1 B2 Co4 65.73(10) . . ? C6 B2 Co4 64.63(10) . . ? B9 B2 Co4 111.26(13) . . ? B5 B2 Co4 98.23(11) . . ? C1 B3 B7 120.85(16) . . ? C1 B3 B8 112.51(16) . . ? B7 B3 B8 58.54(12) . . ? C1 B3 B5 56.13(11) . . ? B7 B3 B5 98.70(13) . . ? B8 B3 B5 57.80(11) . . ? C1 B3 Co4 65.29(10) . . ? B7 B3 Co4 64.70(10) . . ? B8 B3 Co4 108.14(12) . . ? B5 B3 Co4 94.06(10) . . ? C45 Co4 C41 40.71(8) . . ? C45 Co4 C44 40.77(9) . . ? C41 Co4 C44 68.10(9) . . ? C45 Co4 C42 67.74(8) . . ? C41 Co4 C42 40.24(8) . . ? C44 Co4 C42 67.09(8) . . ? C45 Co4 C43 67.94(9) . . ? C41 Co4 C43 67.54(8) . . ? C44 Co4 C43 40.09(8) . . ? C42 Co4 C43 39.51(8) . . ? C45 Co4 C1 153.74(8) . . ? C41 Co4 C1 113.95(8) . . ? C44 Co4 C1 152.78(8) . . ? C42 Co4 C1 96.49(7) . . ? C43 Co4 C1 113.73(8) . . ? C45 Co4 C6 121.58(8) . . ? C41 Co4 C6 161.83(8) . . ? C44 Co4 C6 95.08(8) . . ? C42 Co4 C6 140.49(8) . . ? C43 Co4 C6 104.44(8) . . ? C1 Co4 C6 84.13(7) . . ? C45 Co4 B10 88.41(9) . . ? C41 Co4 B10 123.23(9) . . ? C44 Co4 B10 89.48(8) . . ? C42 Co4 B10 154.68(8) . . ? C43 Co4 B10 124.48(8) . . ? C1 Co4 B10 108.82(8) . . ? C6 Co4 B10 46.70(8) . . ? C45 Co4 B7 91.05(9) . . ? C41 Co4 B7 98.12(9) . . ? C44 Co4 B7 121.21(8) . . ? C42 Co4 B7 135.01(8) . . ? C43 Co4 B7 158.90(8) . . ? C1 Co4 B7 85.87(8) . . ? C6 Co4 B7 84.49(8) . . ? B10 Co4 B7 49.58(8) . . ? C45 Co4 B2 162.20(8) . . ? C41 Co4 B2 147.96(8) . . ? C44 Co4 B2 121.68(9) . . ? C42 Co4 B2 111.53(8) . . ? C43 Co4 B2 99.78(8) . . ? C1 Co4 B2 42.30(7) . . ? C6 Co4 B2 47.03(8) . . ? B10 Co4 B2 88.49(8) . . ? B7 Co4 B2 100.20(8) . . ? C45 Co4 B3 121.34(9) . . ? C41 Co4 B3 97.20(8) . . ? C44 Co4 B3 162.11(9) . . ? C42 Co4 B3 108.75(8) . . ? C43 Co4 B3 144.88(8) . . ? C1 Co4 B3 41.89(8) . . ? C6 Co4 B3 97.92(8) . . ? B10 Co4 B3 90.52(8) . . ? B7 Co4 B3 48.51(8) . . ? B2 Co4 B3 76.20(8) . . ? C1 B5 B11 134.87(16) . . ? C1 B5 B9 103.20(14) . . ? B11 B5 B9 57.20(12) . . ? C1 B5 B8 98.35(14) . . ? B11 B5 B8 56.14(12) . . ? B9 B5 B8 103.53(14) . . ? C1 B5 B2 48.49(10) . . ? B11 B5 B2 106.13(14) . . ? B9 B5 B2 55.91(11) . . ? B8 B5 B2 116.82(14) . . ? C1 B5 B3 46.07(10) . . ? B11 B5 B3 104.18(14) . . ? B9 B5 B3 119.12(14) . . ? B8 B5 B3 53.36(11) . . ? B2 B5 B3 83.69(12) . . ? B12 C6 B9 61.96(13) . . ? B12 C6 B10 63.81(13) . . ? B9 C6 B10 114.71(15) . . ? B12 C6 B2 120.53(15) . . ? B9 C6 B2 63.72(12) . . ? B10 C6 B2 124.16(15) . . ? B12 C6 Co4 122.44(13) . . ? B9 C6 Co4 119.36(12) . . ? B10 C6 Co4 66.76(10) . . ? B2 C6 Co4 68.33(10) . . ? B13 B7 B8 59.68(13) . . ? B13 B7 B3 115.12(16) . . ? B8 B7 B3 60.80(12) . . ? B13 B7 B10 59.91(12) . . ? B8 B7 B10 105.81(16) . . ? B3 B7 B10 117.61(16) . . ? B13 B7 Co4 115.23(14) . . ? B8 B7 Co4 111.33(13) . . ? B3 B7 Co4 66.79(10) . . ? B10 B7 Co4 64.07(10) . . ? B11 B8 B13 61.92(13) . . ? B11 B8 B7 109.72(16) . . ? B13 B8 B7 60.16(13) . . ? B11 B8 B3 120.24(16) . . ? B13 B8 B3 115.43(16) . . ? B7 B8 B3 60.66(12) . . ? B11 B8 B5 58.75(12) . . ? B13 B8 B5 108.02(15) . . ? B7 B8 B5 107.87(15) . . ? B3 B8 B5 68.84(12) . . ? C6 B9 B12 59.00(12) . . ? C6 B9 B11 104.58(16) . . ? B12 B9 B11 61.57(13) . . ? C6 B9 B2 59.18(12) . . ? B12 B9 B2 113.72(16) . . ? B11 B9 B2 115.88(15) . . ? C6 B9 B5 102.57(14) . . ? B12 B9 B5 108.57(15) . . ? B11 B9 B5 59.33(12) . . ? B2 B9 B5 65.08(12) . . ? C6 B10 B13 105.88(16) . . ? C6 B10 B12 57.99(12) . . ? B13 B10 B12 59.77(13) . . ? C6 B10 B7 111.67(15) . . ? B13 B10 B7 58.81(12) . . ? B12 B10 B7 109.04(16) . . ? C6 B10 Co4 66.54(10) . . ? B13 B10 Co4 116.24(13) . . ? B12 B10 Co4 117.35(13) . . ? B7 B10 Co4 66.35(10) . . ? B8 B11 B9 115.77(16) . . ? B8 B11 B12 109.16(16) . . ? B9 B11 B12 58.79(13) . . ? B8 B11 B5 65.10(13) . . ? B9 B11 B5 63.47(12) . . ? B12 B11 B5 109.66(15) . . ? B8 B11 B13 59.38(13) . . ? B9 B11 B13 108.94(16) . . ? B12 B11 B13 59.46(13) . . ? B5 B11 B13 111.00(16) . . ? C6 B12 B9 59.04(12) . . ? C6 B12 B13 106.28(16) . . ? B9 B12 B13 110.60(16) . . ? C6 B12 B10 58.20(12) . . ? B9 B12 B10 107.73(15) . . ? B13 B12 B10 60.06(13) . . ? C6 B12 B11 103.16(15) . . ? B9 B12 B11 59.63(13) . . ? B13 B12 B11 60.62(13) . . ? B10 B12 B11 105.61(16) . . ? B8 B13 B7 60.16(12) . . ? B8 B13 B12 108.97(16) . . ? B7 B13 B12 111.42(16) . . ? B8 B13 B10 107.22(15) . . ? B7 B13 B10 61.28(13) . . ? B12 B13 B10 60.17(13) . . ? B8 B13 B11 58.69(13) . . ? B7 B13 B11 107.16(15) . . ? B12 B13 B11 59.92(13) . . ? B10 B13 B11 105.17(15) . . ? C42 C41 C45 108.04(19) . . ? C42 C41 Co4 71.35(12) . . ? C45 C41 Co4 69.62(12) . . ? C43 C42 C41 108.64(18) . . ? C43 C42 Co4 70.65(11) . . ? C41 C42 Co4 68.40(11) . . ? C42 C43 C44 107.47(18) . . ? C42 C43 Co4 69.84(11) . . ? C44 C43 Co4 68.28(11) . . ? C43 C44 C45 108.63(18) . . ? C43 C44 Co4 71.63(11) . . ? C45 C44 Co4 69.39(11) . . ? C41 C45 C44 107.21(18) . . ? C41 C45 Co4 69.67(12) . . ? C44 C45 Co4 69.84(12) . . ? C1 C1' B2' 119.56(16) . . ? C1 C1' B3' 117.34(16) . . ? B2' C1' B3' 123.05(16) . . ? C1 C1' B5' 120.77(14) . . ? B2' C1' B5' 77.51(13) . . ? B3' C1' B5' 72.22(13) . . ? C1 C1' Co4' 130.51(13) . . ? B2' C1' Co4' 71.76(10) . . ? B3' C1' Co4' 73.97(10) . . ? B5' C1' Co4' 108.65(11) . . ? C1' B2' C6' 119.28(16) . . ? C1' B2' B9' 112.84(16) . . ? C6' B2' B9' 56.93(11) . . ? C1' B2' B5' 56.41(11) . . ? C6' B2' B5' 95.01(13) . . ? B9' B2' B5' 57.52(11) . . ? C1' B2' Co4' 65.85(10) . . ? C6' B2' Co4' 65.44(9) . . ? B9' B2' Co4' 110.40(12) . . ? B5' B2' Co4' 95.24(11) . . ? C1' B3' B8' 116.55(16) . . ? C1' B3' B7' 120.23(16) . . ? B8' B3' B7' 58.48(12) . . ? C1' B3' B5' 59.12(12) . . ? B8' B3' B5' 59.58(12) . . ? B7' B3' B5' 100.37(14) . . ? C1' B3' Co4' 63.87(10) . . ? B8' B3' Co4' 109.33(12) . . ? B7' B3' Co4' 64.27(10) . . ? B5' B3' Co4' 96.56(11) . . ? C42' Co4' C43' 40.90(9) . . ? C42' Co4' C41' 40.47(8) . . ? C43' Co4' C41' 68.13(8) . . ? C42' Co4' C1' 155.67(8) . . ? C43' Co4' C1' 150.98(8) . . ? C41' Co4' C1' 115.78(8) . . ? C42' Co4' C44' 68.09(8) . . ? C43' Co4' C44' 40.29(8) . . ? C41' Co4' C44' 67.65(8) . . ? C1' Co4' C44' 112.26(8) . . ? C42' Co4' C45' 67.60(8) . . ? C43' Co4' C45' 67.14(8) . . ? C41' Co4' C45' 40.31(8) . . ? C1' Co4' C45' 96.79(7) . . ? C44' Co4' C45' 39.47(8) . . ? C42' Co4' B10' 87.77(9) . . ? C43' Co4' B10' 90.23(8) . . ? C41' Co4' B10' 121.59(9) . . ? C1' Co4' B10' 108.62(8) . . ? C44' Co4' B10' 126.09(8) . . ? C45' Co4' B10' 154.53(8) . . ? C42' Co4' C6' 120.37(8) . . ? C43' Co4' C6' 94.64(8) . . ? C41' Co4' C6' 160.63(8) . . ? C1' Co4' C6' 83.56(7) . . ? C44' Co4' C6' 105.36(8) . . ? C45' Co4' C6' 141.96(8) . . ? B10' Co4' C6' 46.76(8) . . ? C42' Co4' B2' 159.87(9) . . ? C43' Co4' B2' 119.29(8) . . ? C41' Co4' B2' 149.25(8) . . ? C1' Co4' B2' 42.39(8) . . ? C44' Co4' B2' 98.28(8) . . ? C45' Co4' B2' 111.82(8) . . ? B10' Co4' B2' 88.98(8) . . ? C6' Co4' B2' 46.99(8) . . ? C42' Co4' B7' 91.33(8) . . ? C43' Co4' B7' 122.21(8) . . ? C41' Co4' B7' 97.21(9) . . ? C1' Co4' B7' 86.54(8) . . ? C44' Co4' B7' 159.41(8) . . ? C45' Co4' B7' 133.73(8) . . ? B10' Co4' B7' 49.14(9) . . ? C6' Co4' B7' 84.31(8) . . ? B2' Co4' B7' 101.48(8) . . ? C42' Co4' B3' 123.36(9) . . ? C43' Co4' B3' 164.25(8) . . ? C41' Co4' B3' 98.82(8) . . ? C1' Co4' B3' 42.16(8) . . ? C44' Co4' B3' 144.29(8) . . ? C45' Co4' B3' 109.10(8) . . ? B10' Co4' B3' 89.43(8) . . ? C6' Co4' B3' 96.58(8) . . ? B2' Co4' B3' 76.45(8) . . ? B7' Co4' B3' 48.45(8) . . ? C1' B5' B11' 134.84(15) . . ? C1' B5' B8' 102.48(14) . . ? B11' B5' B8' 56.55(12) . . ? C1' B5' B9' 99.32(14) . . ? B11' B5' B9' 56.57(12) . . ? B8' B5' B9' 103.53(14) . . ? C1' B5' B3' 48.66(10) . . ? B11' B5' B3' 106.11(14) . . ? B8' B5' B3' 55.45(11) . . ? B9' B5' B3' 119.01(14) . . ? C1' B5' B2' 46.08(10) . . ? B11' B5' B2' 104.36(14) . . ? B8' B5' B2' 117.74(14) . . ? B9' B5' B2' 54.08(11) . . ? B3' B5' B2' 84.12(12) . . ? B12' C6' B9' 62.24(13) . . ? B12' C6' B10' 63.60(13) . . ? B9' C6' B10' 113.77(16) . . ? B12' C6' B2' 122.29(15) . . ? B9' C6' B2' 64.58(12) . . ? B10' C6' B2' 124.18(16) . . ? B12' C6' Co4' 121.94(14) . . ? B9' C6' Co4' 117.80(12) . . ? B10' C6' Co4' 66.41(10) . . ? B2' C6' Co4' 67.57(10) . . ? B13' B7' B8' 59.56(13) . . ? B13' B7' B10' 60.23(13) . . ? B8' B7' B10' 106.72(16) . . ? B13' B7' B3' 113.77(15) . . ? B8' B7' B3' 60.36(12) . . ? B10' B7' B3' 116.81(16) . . ? B13' B7' Co4' 115.63(14) . . ? B8' B7' Co4' 113.05(13) . . ? B10' B7' Co4' 63.94(10) . . ? B3' B7' Co4' 67.28(10) . . ? B11' B8' B13' 61.83(13) . . ? B11' B8' B7' 108.77(16) . . ? B13' B8' B7' 60.14(12) . . ? B11' B8' B3' 116.94(16) . . ? B13' B8' B3' 114.98(15) . . ? B7' B8' B3' 61.16(12) . . ? B11' B8' B5' 59.31(12) . . ? B13' B8' B5' 108.16(16) . . ? B7' B8' B5' 106.03(15) . . ? B3' B8' B5' 64.97(12) . . ? C6' B9' B12' 58.66(12) . . ? C6' B9' B11' 105.41(16) . . ? B12' B9' B11' 61.71(13) . . ? C6' B9' B2' 58.50(11) . . ? B12' B9' B2' 113.41(15) . . ? B11' B9' B2' 118.88(16) . . ? C6' B9' B5' 103.55(14) . . ? B12' B9' B5' 107.98(16) . . ? B11' B9' B5' 58.93(12) . . ? B2' B9' B5' 68.40(12) . . ? C6' B10' B12' 57.86(12) . . ? C6' B10' B13' 106.44(15) . . ? B12' B10' B13' 59.82(13) . . ? C6' B10' B7' 112.43(15) . . ? B12' B10' B7' 109.06(15) . . ? B13' B10' B7' 58.98(13) . . ? C6' B10' Co4' 66.83(10) . . ? B12' B10' Co4' 117.46(13) . . ? B13' B10' Co4' 117.13(13) . . ? B7' B10' Co4' 66.92(10) . . ? B8' B11' B9' 116.06(16) . . ? B8' B11' B12' 109.26(16) . . ? B9' B11' B12' 58.83(13) . . ? B8' B11' B13' 59.22(13) . . ? B9' B11' B13' 108.68(16) . . ? B12' B11' B13' 59.33(13) . . ? B8' B11' B5' 64.14(12) . . ? B9' B11' B5' 64.50(12) . . ? B12' B11' B5' 110.12(15) . . ? B13' B11' B5' 109.89(15) . . ? C6' B12' B9' 59.10(12) . . ? C6' B12' B13' 107.32(16) . . ? B9' B12' B13' 110.13(16) . . ? C6' B12' B10' 58.54(12) . . ? B9' B12' B10' 107.17(15) . . ? B13' B12' B10' 60.24(13) . . ? C6' B12' B11' 104.02(15) . . ? B9' B12' B11' 59.46(12) . . ? B13' B12' B11' 60.45(13) . . ? B10' B12' B11' 105.49(16) . . ? B8' B13' B7' 60.30(13) . . ? B8' B13' B12' 109.78(16) . . ? B7' B13' B12' 110.67(16) . . ? B8' B13' B10' 107.73(15) . . ? B7' B13' B10' 60.79(13) . . ? B12' B13' B10' 59.94(13) . . ? B8' B13' B11' 58.95(13) . . ? B7' B13' B11' 106.63(15) . . ? B12' B13' B11' 60.23(13) . . ? B10' B13' B11' 105.10(15) . . ? C42' C41' C45' 107.61(18) . . ? C42' C41' Co4' 68.96(11) . . ? C45' C41' Co4' 71.11(11) . . ? C41' C42' C43' 107.96(18) . . ? C41' C42' Co4' 70.58(11) . . ? C43' C42' Co4' 69.95(11) . . ? C44' C43' C42' 108.11(18) . . ? C44' C43' Co4' 71.29(11) . . ? C42' C43' Co4' 69.15(11) . . ? C45' C44' C43' 107.74(18) . . ? C45' C44' Co4' 70.51(11) . . ? C43' C44' Co4' 68.42(11) . . ? C44' C45' C41' 108.57(18) . . ? C44' C45' Co4' 70.02(11) . . ? C41' C45' Co4' 68.58(11) . . ? Cl1 C1S Cl2 111.36(13) . . ? Cl1 C1S Cl2A 127.1(10) . . ? Cl2 C1S Cl2A 121.5(10) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.829 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.095 # Attachment '3286--rac-.cif' data_x83286_0m _database_code_depnum_ccdc_archive 'CCDC 784592' #TrackingRef '3286--rac-.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H32 B20 Co2' _chemical_formula_weight 534.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.1973(8) _cell_length_b 11.6516(8) _cell_length_c 17.1287(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.279(3) _cell_angle_gamma 90.00 _cell_volume 2433.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9419 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 26.15 _exptl_crystal_description BLOCK _exptl_crystal_colour red _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5840 _exptl_absorpt_correction_T_max 0.6241 _exptl_absorpt_process_details 'SADABS (Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33763 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.38 _reflns_number_total 4900 _reflns_number_gt 3557 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.0827P)^2^+4.8166P] 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 4900 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 C1 C 0.7171(3) 0.9573(4) 0.1242(2) 0.0183(9) Uani 1 1 d . . . B2 B 0.6003(4) 1.0019(4) 0.1057(3) 0.0206(10) Uani 1 1 d . . . H2 H 0.5539 0.9456 0.0636 0.025 Uiso 1 1 calc R . . B3 B 0.8044(4) 1.0294(5) 0.1706(3) 0.0219(11) Uani 1 1 d . . . H3 H 0.8882 0.9901 0.1721 0.026 Uiso 1 1 calc R . . Co4 Co 0.73016(5) 1.11448(5) 0.06536(3) 0.01787(18) Uani 1 1 d . . . B5 B 0.6568(4) 0.9827(5) 0.2162(3) 0.0221(11) Uani 1 1 d . . . H5 H 0.646(4) 0.906(4) 0.246(3) 0.027 Uiso 1 1 d . . . C6 C 0.5717(4) 1.1455(4) 0.1128(2) 0.0196(9) Uani 1 1 d . . . H6 H 0.5110 1.1722 0.0663 0.023 Uiso 1 1 calc R . . B7 B 0.7909(4) 1.1838(4) 0.1764(3) 0.0191(10) Uani 1 1 d . . . H7 H 0.8699 1.2324 0.1735 0.023 Uiso 1 1 calc R . . B8 B 0.7529(4) 1.0979(4) 0.2567(3) 0.0219(11) Uani 1 1 d . . . H8 H 0.8064 1.0838 0.3098 0.026 Uiso 1 1 calc R . . B9 B 0.5295(4) 1.0638(4) 0.1881(3) 0.0231(11) Uani 1 1 d . . . H9 H 0.4452 1.0291 0.1976 0.028 Uiso 1 1 calc R . . B10 B 0.6645(4) 1.2462(4) 0.1379(3) 0.0199(10) Uani 1 1 d . . . H10 H 0.6657 1.3316 0.1080 0.024 Uiso 1 1 calc R . . B11 B 0.6104(4) 1.1070(4) 0.2683(3) 0.0213(11) Uani 1 1 d . . . H11 H 0.5778 1.0951 0.3284 0.026 Uiso 1 1 calc R . . B12 B 0.5551(4) 1.2095(4) 0.2002(3) 0.0216(11) Uani 1 1 d . . . H12 H 0.4871 1.2703 0.2141 0.026 Uiso 1 1 calc R . . B13 B 0.6893(5) 1.2316(5) 0.2401(3) 0.0245(11) Uani 1 1 d . . . H13 H 0.7060 1.3069 0.2792 0.029 Uiso 1 1 calc R . . C41 C 0.8087(4) 1.2405(4) 0.0048(2) 0.0248(10) Uani 1 1 d . . . H41 H 0.8319 1.3170 0.0259 0.030 Uiso 1 1 calc R . . C42 C 0.7067(4) 1.2150(4) -0.0330(2) 0.0244(10) Uani 1 1 d . . . H42 H 0.6452 1.2705 -0.0420 0.029 Uiso 1 1 calc R . . C43 C 0.7068(4) 1.0988(4) -0.0565(2) 0.0224(10) Uani 1 1 d . . . H43 H 0.6455 1.0573 -0.0840 0.027 Uiso 1 1 calc R . . C44 C 0.8099(4) 1.0513(4) -0.0329(2) 0.0205(9) Uani 1 1 d . . . H44 H 0.8339 0.9702 -0.0411 0.025 Uiso 1 1 calc R . . C45 C 0.8721(4) 1.1390(4) 0.0063(2) 0.0234(10) Uani 1 1 d . . . H45 H 0.9483 1.1310 0.0284 0.028 Uiso 1 1 calc R . . C1' C 0.7426(4) 0.8354(4) 0.0983(2) 0.0182(9) Uani 1 1 d . . . B2' B 0.6521(4) 0.7436(4) 0.1073(3) 0.0204(10) Uani 1 1 d . . . H2' H 0.5846 0.7728 0.1458 0.025 Uiso 1 1 calc R . . B3' B 0.8536(4) 0.8095(4) 0.0593(3) 0.0197(10) Uani 1 1 d . . . H3' H 0.9147 0.8809 0.0655 0.024 Uiso 1 1 calc R . . Co4' Co 0.81202(5) 0.69359(5) 0.15595(3) 0.01904(19) Uani 1 1 d . . . B5' B 0.7038(4) 0.7916(5) 0.0017(3) 0.0210(11) Uani 1 1 d . . . H5' H 0.669(4) 0.866(4) -0.031(3) 0.025 Uiso 1 1 d . . . C6' C 0.6838(4) 0.6011(4) 0.0974(2) 0.0190(9) Uani 1 1 d . . . H6' H 0.6357 0.5482 0.1392 0.023 Uiso 1 1 calc R . . B7' B 0.9030(4) 0.6636(4) 0.0497(3) 0.0211(11) Uani 1 1 d . . . H7' H 0.9938 0.6526 0.0575 0.025 Uiso 1 1 calc R . . B8' B 0.8390(4) 0.7318(4) -0.0316(3) 0.0209(10) Uani 1 1 d . . . H8' H 0.8851 0.7726 -0.0801 0.025 Uiso 1 1 calc R . . B9' B 0.6184(4) 0.6613(4) 0.0202(3) 0.0211(11) Uani 1 1 d . . . H9' H 0.5288 0.6569 0.0050 0.025 Uiso 1 1 calc R . . B10' B 0.8107(4) 0.5498(4) 0.0791(3) 0.0215(11) Uani 1 1 d . . . H10' H 0.8437 0.4710 0.1088 0.026 Uiso 1 1 calc R . . B11' B 0.7156(4) 0.6616(4) -0.0539(3) 0.0207(10) Uani 1 1 d . . . H11' H 0.6858 0.6618 -0.1162 0.025 Uiso 1 1 calc R . . B12' B 0.7006(4) 0.5403(5) 0.0084(3) 0.0232(11) Uani 1 1 d . . . H12' H 0.6642 0.4565 -0.0110 0.028 Uiso 1 1 calc R . . B13' B 0.8337(4) 0.5813(4) -0.0222(3) 0.0216(11) Uani 1 1 d . . . H13' H 0.8810 0.5231 -0.0612 0.026 Uiso 1 1 calc R . . C41' C 0.8453(4) 0.7768(4) 0.2617(2) 0.0250(10) Uani 1 1 d . . . H41' H 0.8291 0.8592 0.2729 0.030 Uiso 1 1 calc R . . C42' C 0.7730(4) 0.6838(4) 0.2739(2) 0.0253(10) Uani 1 1 d . . . H42' H 0.6979 0.6883 0.2961 0.030 Uiso 1 1 calc R . . C43' C 0.8270(4) 0.5829(4) 0.2482(2) 0.0277(11) Uani 1 1 d . . . H43' H 0.7964 0.5034 0.2499 0.033 Uiso 1 1 calc R . . C44' C 0.9321(4) 0.6132(4) 0.2205(2) 0.0257(10) Uani 1 1 d . . . H44' H 0.9887 0.5593 0.2004 0.031 Uiso 1 1 calc R . . C45' C 0.9426(4) 0.7353(4) 0.2279(2) 0.0257(10) Uani 1 1 d . . . H45' H 1.0076 0.7823 0.2134 0.031 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 C1 0.027(2) 0.022(2) 0.0059(18) 0.0013(17) 0.0020(16) 0.0016(18) B2 0.030(3) 0.026(3) 0.006(2) 0.0013(19) 0.0029(18) 0.000(2) B3 0.024(3) 0.034(3) 0.008(2) -0.002(2) -0.0001(19) 0.001(2) Co4 0.0266(3) 0.0219(3) 0.0052(3) 0.0004(2) 0.0017(2) -0.0005(2) B5 0.031(3) 0.028(3) 0.008(2) 0.003(2) 0.0027(19) 0.001(2) C6 0.027(2) 0.024(2) 0.0079(19) -0.0001(17) 0.0035(16) 0.0033(18) B7 0.026(3) 0.023(3) 0.009(2) -0.0008(19) -0.0023(18) -0.002(2) B8 0.031(3) 0.027(3) 0.007(2) -0.0025(19) -0.0004(19) 0.002(2) B9 0.031(3) 0.026(3) 0.013(2) 0.004(2) 0.006(2) 0.004(2) B10 0.028(3) 0.019(3) 0.012(2) -0.0018(19) 0.0018(19) 0.003(2) B11 0.032(3) 0.022(3) 0.010(2) 0.0011(19) 0.005(2) 0.005(2) B12 0.030(3) 0.026(3) 0.009(2) 0.001(2) 0.0044(19) 0.003(2) B13 0.040(3) 0.024(3) 0.010(2) -0.002(2) 0.003(2) 0.001(2) C41 0.040(3) 0.023(2) 0.011(2) -0.0006(18) 0.0068(19) -0.005(2) C42 0.041(3) 0.029(3) 0.0037(19) 0.0048(17) 0.0062(18) 0.006(2) C43 0.035(3) 0.027(3) 0.0053(19) 0.0036(17) 0.0045(17) -0.0019(19) C44 0.032(2) 0.023(2) 0.0070(19) 0.0012(17) 0.0067(17) -0.0011(18) C45 0.029(2) 0.033(3) 0.009(2) -0.0015(18) 0.0080(17) -0.0056(19) C1' 0.029(2) 0.024(2) 0.0019(18) 0.0009(16) -0.0014(16) 0.0021(18) B2' 0.031(3) 0.021(3) 0.009(2) 0.0015(19) 0.0011(19) -0.003(2) B3' 0.028(3) 0.023(3) 0.008(2) 0.0029(19) 0.0010(19) -0.001(2) Co4' 0.0288(4) 0.0226(3) 0.0058(3) 0.0005(2) 0.0003(2) 0.0010(2) B5' 0.027(3) 0.028(3) 0.008(2) -0.002(2) 0.0019(19) -0.001(2) C6' 0.029(2) 0.020(2) 0.0082(19) -0.0010(16) -0.0016(17) -0.0005(17) B7' 0.031(3) 0.025(3) 0.007(2) -0.0012(19) 0.0034(19) 0.003(2) B8' 0.028(3) 0.026(3) 0.009(2) 0.000(2) -0.0006(19) 0.003(2) B9' 0.032(3) 0.023(3) 0.008(2) -0.0006(19) -0.0004(19) -0.002(2) B10' 0.032(3) 0.022(3) 0.010(2) -0.005(2) 0.0005(19) 0.004(2) B11' 0.033(3) 0.021(3) 0.008(2) -0.0021(19) -0.0001(19) -0.003(2) B12' 0.038(3) 0.025(3) 0.006(2) 0.0003(19) -0.002(2) -0.004(2) B13' 0.033(3) 0.022(3) 0.010(2) 0.0002(19) 0.000(2) 0.004(2) C41' 0.040(3) 0.029(3) 0.0057(19) 0.0027(18) -0.0044(18) 0.000(2) C42' 0.035(3) 0.034(3) 0.007(2) 0.0020(18) -0.0011(18) -0.004(2) C43' 0.041(3) 0.030(3) 0.012(2) 0.0055(19) -0.0038(19) 0.003(2) C44' 0.034(3) 0.034(3) 0.009(2) 0.0015(18) -0.0026(18) 0.011(2) C45' 0.031(3) 0.037(3) 0.009(2) 0.0023(19) -0.0051(18) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C1' 1.521(6) . ? C1 B2 1.543(7) . ? C1 B3 1.560(6) . ? C1 B5 1.778(6) . ? C1 Co4 2.099(4) . ? B2 C6 1.714(7) . ? B2 B9 1.820(7) . ? B2 B5 2.012(7) . ? B2 Co4 2.181(5) . ? B2 H2 1.1200 . ? B3 B8 1.802(7) . ? B3 B7 1.809(7) . ? B3 B5 2.052(7) . ? B3 Co4 2.231(5) . ? B3 H3 1.1200 . ? Co4 C45 2.045(4) . ? Co4 C41 2.047(4) . ? Co4 C42 2.066(4) . ? Co4 C44 2.096(4) . ? Co4 C43 2.108(4) . ? Co4 B10 2.142(5) . ? Co4 C6 2.143(4) . ? Co4 B7 2.180(5) . ? B5 B11 1.799(7) . ? B5 B9 1.871(7) . ? B5 B8 1.902(7) . ? B5 H5 1.04(5) . ? C6 B10 1.679(7) . ? C6 B12 1.689(6) . ? C6 B9 1.693(6) . ? C6 H6 1.1200 . ? B7 B13 1.760(7) . ? B7 B8 1.771(7) . ? B7 B10 1.815(7) . ? B7 H7 1.1200 . ? B8 B11 1.758(7) . ? B8 B13 1.761(7) . ? B8 H8 1.1200 . ? B9 B12 1.737(7) . ? B9 B11 1.748(7) . ? B9 H9 1.1200 . ? B10 B13 1.778(7) . ? B10 B12 1.780(7) . ? B10 H10 1.1200 . ? B11 B12 1.790(7) . ? B11 B13 1.813(7) . ? B11 H11 1.1200 . ? B12 B13 1.778(8) . ? B12 H12 1.1200 . ? B13 H13 1.1200 . ? C41 C45 1.413(7) . ? C41 C42 1.421(7) . ? C41 H41 1.0000 . ? C42 C43 1.413(6) . ? C42 H42 1.0000 . ? C43 C44 1.423(6) . ? C43 H43 1.0000 . ? C44 C45 1.432(6) . ? C44 H44 1.0000 . ? C45 H45 1.0000 . ? C1' B2' 1.548(7) . ? C1' B3' 1.553(6) . ? C1' B5' 1.786(6) . ? C1' Co4' 2.094(4) . ? B2' C6' 1.713(7) . ? B2' B9' 1.812(7) . ? B2' B5' 2.009(7) . ? B2' Co4' 2.183(5) . ? B2' H2' 1.1200 . ? B3' B8' 1.807(7) . ? B3' B7' 1.813(7) . ? B3' B5' 2.069(7) . ? B3' Co4' 2.204(5) . ? B3' H3' 1.1200 . ? Co4' C44' 2.043(4) . ? Co4' C43' 2.044(4) . ? Co4' C45' 2.050(4) . ? Co4' C41' 2.086(4) . ? Co4' C42' 2.090(4) . ? Co4' B10' 2.131(5) . ? Co4' C6' 2.131(4) . ? Co4' B7' 2.181(5) . ? B5' B11' 1.796(7) . ? B5' B9' 1.872(7) . ? B5' B8' 1.890(7) . ? B5' H5' 1.11(5) . ? C6' B9' 1.682(6) . ? C6' B10' 1.696(7) . ? C6' B12' 1.698(6) . ? C6' H6' 1.1200 . ? B7' B13' 1.763(7) . ? B7' B8' 1.770(7) . ? B7' B10' 1.817(7) . ? B7' H7' 1.1200 . ? B8' B11' 1.748(7) . ? B8' B13' 1.762(7) . ? B8' H8' 1.1200 . ? B9' B12' 1.744(7) . ? B9' B11' 1.757(7) . ? B9' H9' 1.1200 . ? B10' B12' 1.792(7) . ? B10' B13' 1.802(7) . ? B10' H10' 1.1200 . ? B11' B12' 1.782(7) . ? B11' B13' 1.791(7) . ? B11' H11' 1.1200 . ? B12' B13' 1.782(7) . ? B12' H12' 1.1200 . ? B13' H13' 1.1200 . ? C41' C45' 1.416(7) . ? C41' C42' 1.416(6) . ? C41' H41' 1.0000 . ? C42' C43' 1.423(7) . ? C42' H42' 1.0000 . ? C43' C44' 1.422(7) . ? C43' H43' 1.0000 . ? C44' C45' 1.433(7) . ? C44' H44' 1.0000 . ? C45' H45' 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1' C1 B2 116.6(4) . . ? C1' C1 B3 120.6(4) . . ? B2 C1 B3 122.6(4) . . ? C1' C1 B5 120.3(3) . . ? B2 C1 B5 74.2(3) . . ? B3 C1 B5 75.5(3) . . ? C1' C1 Co4 131.0(3) . . ? B2 C1 Co4 71.7(2) . . ? B3 C1 Co4 73.5(2) . . ? B5 C1 Co4 108.5(3) . . ? C1 B2 C6 120.2(4) . . ? C1 B2 B9 115.2(3) . . ? C6 B2 B9 57.2(3) . . ? C1 B2 B5 58.3(3) . . ? C6 B2 B5 96.2(3) . . ? B9 B2 B5 58.2(3) . . ? C1 B2 Co4 66.1(2) . . ? C6 B2 Co4 65.5(2) . . ? B9 B2 Co4 111.6(3) . . ? B5 B2 Co4 97.4(3) . . ? C1 B2 H2 112.7 . . ? C6 B2 H2 121.2 . . ? B9 B2 H2 119.4 . . ? B5 B2 H2 134.3 . . ? Co4 B2 H2 120.6 . . ? C1 B3 B8 114.1(4) . . ? C1 B3 B7 120.1(4) . . ? B8 B3 B7 58.7(3) . . ? C1 B3 B5 57.1(3) . . ? B8 B3 B5 58.7(3) . . ? B7 B3 B5 99.2(3) . . ? C1 B3 Co4 64.4(2) . . ? B8 B3 Co4 108.8(3) . . ? B7 B3 Co4 64.3(2) . . ? B5 B3 Co4 94.7(2) . . ? C1 B3 H3 113.8 . . ? B8 B3 H3 119.7 . . ? B7 B3 H3 119.3 . . ? B5 B3 H3 133.7 . . ? Co4 B3 H3 123.7 . . ? C45 Co4 C41 40.39(18) . . ? C45 Co4 C42 67.71(18) . . ? C41 Co4 C42 40.40(19) . . ? C45 Co4 C44 40.43(17) . . ? C41 Co4 C44 67.33(17) . . ? C42 Co4 C44 66.60(17) . . ? C45 Co4 C1 115.72(18) . . ? C41 Co4 C1 155.58(18) . . ? C42 Co4 C1 151.13(17) . . ? C44 Co4 C1 96.93(16) . . ? C45 Co4 C43 67.63(18) . . ? C41 Co4 C43 67.36(17) . . ? C42 Co4 C43 39.56(17) . . ? C44 Co4 C43 39.58(17) . . ? C1 Co4 C43 112.93(16) . . ? C45 Co4 B10 121.23(19) . . ? C41 Co4 B10 88.01(19) . . ? C42 Co4 B10 91.16(18) . . ? C44 Co4 B10 154.69(18) . . ? C1 Co4 B10 108.27(17) . . ? C43 Co4 B10 126.38(18) . . ? C45 Co4 C6 160.79(18) . . ? C41 Co4 C6 120.45(18) . . ? C42 Co4 C6 95.96(17) . . ? C44 Co4 C6 143.32(17) . . ? C1 Co4 C6 83.48(16) . . ? C43 Co4 C6 106.69(17) . . ? B10 Co4 C6 46.15(18) . . ? C45 Co4 B7 96.01(18) . . ? C41 Co4 B7 91.30(18) . . ? C42 Co4 B7 122.64(18) . . ? C44 Co4 B7 132.51(18) . . ? C1 Co4 B7 86.11(17) . . ? C43 Co4 B7 158.65(18) . . ? B10 Co4 B7 49.64(18) . . ? C6 Co4 B7 84.17(18) . . ? C45 Co4 B2 150.46(19) . . ? C41 Co4 B2 160.56(19) . . ? C42 Co4 B2 120.72(19) . . ? C44 Co4 B2 113.36(18) . . ? C1 Co4 B2 42.22(18) . . ? C43 Co4 B2 100.29(18) . . ? B10 Co4 B2 87.91(19) . . ? C6 Co4 B2 46.69(17) . . ? B7 Co4 B2 100.45(18) . . ? C45 Co4 B3 97.40(18) . . ? C41 Co4 B3 122.80(19) . . ? C42 Co4 B3 163.06(19) . . ? C44 Co4 B3 107.77(18) . . ? C1 Co4 B3 42.10(17) . . ? C43 Co4 B3 143.56(18) . . ? B10 Co4 B3 89.99(18) . . ? C6 Co4 B3 97.00(17) . . ? B7 Co4 B3 48.40(18) . . ? B2 Co4 B3 76.20(18) . . ? C1 B5 B11 135.6(4) . . ? C1 B5 B9 102.3(3) . . ? B11 B5 B9 56.8(3) . . ? C1 B5 B8 100.2(3) . . ? B11 B5 B8 56.6(3) . . ? B9 B5 B8 103.8(3) . . ? C1 B5 B2 47.5(2) . . ? B11 B5 B2 105.8(3) . . ? B9 B5 B2 55.7(2) . . ? B8 B5 B2 117.4(3) . . ? C1 B5 B3 47.4(2) . . ? B11 B5 B3 105.3(3) . . ? B9 B5 B3 119.9(3) . . ? B8 B5 B3 54.1(2) . . ? B2 B5 B3 84.1(3) . . ? C1 B5 H5 111(3) . . ? B11 B5 H5 113(3) . . ? B9 B5 H5 116(3) . . ? B8 B5 H5 120(3) . . ? B2 B5 H5 121(3) . . ? B3 B5 H5 123(3) . . ? B10 C6 B12 63.8(3) . . ? B10 C6 B9 114.4(3) . . ? B12 C6 B9 61.8(3) . . ? B10 C6 B2 124.3(4) . . ? B12 C6 B2 121.5(3) . . ? B9 C6 B2 64.6(3) . . ? B10 C6 Co4 66.9(2) . . ? B12 C6 Co4 122.5(3) . . ? B9 C6 Co4 119.1(3) . . ? B2 C6 Co4 67.8(2) . . ? B10 C6 H6 114.8 . . ? B12 C6 H6 114.7 . . ? B9 C6 H6 119.4 . . ? B2 C6 H6 110.7 . . ? Co4 C6 H6 111.4 . . ? B13 B7 B8 59.8(3) . . ? B13 B7 B3 114.5(4) . . ? B8 B7 B3 60.4(3) . . ? B13 B7 B10 59.6(3) . . ? B8 B7 B10 105.9(3) . . ? B3 B7 B10 117.2(3) . . ? B13 B7 Co4 115.3(3) . . ? B8 B7 Co4 112.3(3) . . ? B3 B7 Co4 67.3(2) . . ? B10 B7 Co4 64.1(2) . . ? B13 B7 H7 119.1 . . ? B8 B7 H7 124.1 . . ? B3 B7 H7 114.9 . . ? B10 B7 H7 120.4 . . ? Co4 B7 H7 115.1 . . ? B11 B8 B13 62.0(3) . . ? B11 B8 B7 109.3(3) . . ? B13 B8 B7 59.8(3) . . ? B11 B8 B3 118.9(4) . . ? B13 B8 B3 114.8(3) . . ? B7 B8 B3 60.8(3) . . ? B11 B8 B5 58.7(3) . . ? B13 B8 B5 107.4(4) . . ? B7 B8 B5 106.6(3) . . ? B3 B8 B5 67.2(3) . . ? B11 B8 H8 118.4 . . ? B13 B8 H8 120.5 . . ? B7 B8 H8 123.9 . . ? B3 B8 H8 113.2 . . ? B5 B8 H8 122.4 . . ? C6 B9 B12 59.0(3) . . ? C6 B9 B11 105.1(4) . . ? B12 B9 B11 61.8(3) . . ? C6 B9 B2 58.3(3) . . ? B12 B9 B2 113.1(4) . . ? B11 B9 B2 117.0(4) . . ? C6 B9 B5 102.4(3) . . ? B12 B9 B5 108.5(4) . . ? B11 B9 B5 59.5(3) . . ? B2 B9 B5 66.1(3) . . ? C6 B9 H9 127.6 . . ? B12 B9 H9 119.9 . . ? B11 B9 H9 119.5 . . ? B2 B9 H9 115.0 . . ? B5 B9 H9 122.6 . . ? C6 B10 B13 106.5(4) . . ? C6 B10 B12 58.4(3) . . ? B13 B10 B12 60.0(3) . . ? C6 B10 B7 112.0(3) . . ? B13 B10 B7 58.7(3) . . ? B12 B10 B7 109.2(3) . . ? C6 B10 Co4 67.0(2) . . ? B13 B10 Co4 116.4(3) . . ? B12 B10 Co4 118.1(3) . . ? B7 B10 Co4 66.3(2) . . ? C6 B10 H10 121.2 . . ? B13 B10 H10 122.2 . . ? B12 B10 H10 120.4 . . ? B7 B10 H10 120.2 . . ? Co4 B10 H10 111.2 . . ? B9 B11 B8 115.8(3) . . ? B9 B11 B12 58.8(3) . . ? B8 B11 B12 109.0(4) . . ? B9 B11 B5 63.6(3) . . ? B8 B11 B5 64.6(3) . . ? B12 B11 B5 109.3(3) . . ? B9 B11 B13 108.3(3) . . ? B8 B11 B13 59.1(3) . . ? B12 B11 B13 59.2(3) . . ? B5 B11 B13 109.7(3) . . ? B9 B11 H11 118.7 . . ? B8 B11 H11 118.0 . . ? B12 B11 H11 123.0 . . ? B5 B11 H11 118.5 . . ? B13 B11 H11 123.1 . . ? C6 B12 B9 59.2(3) . . ? C6 B12 B13 106.1(3) . . ? B9 B12 B13 110.4(4) . . ? C6 B12 B10 57.8(3) . . ? B9 B12 B10 107.4(3) . . ? B13 B12 B10 60.0(3) . . ? C6 B12 B11 103.4(3) . . ? B9 B12 B11 59.4(3) . . ? B13 B12 B11 61.0(3) . . ? B10 B12 B11 105.9(4) . . ? C6 B12 H12 124.9 . . ? B9 B12 H12 120.8 . . ? B13 B12 H12 120.4 . . ? B10 B12 H12 122.9 . . ? B11 B12 H12 123.6 . . ? B7 B13 B8 60.4(3) . . ? B7 B13 B10 61.7(3) . . ? B8 B13 B10 107.9(3) . . ? B7 B13 B12 111.7(3) . . ? B8 B13 B12 109.4(4) . . ? B10 B13 B12 60.1(3) . . ? B7 B13 B11 107.3(4) . . ? B8 B13 B11 58.9(3) . . ? B10 B13 B11 105.1(4) . . ? B12 B13 B11 59.8(3) . . ? B7 B13 H13 119.8 . . ? B8 B13 H13 121.6 . . ? B10 B13 H13 122.5 . . ? B12 B13 H13 119.8 . . ? B11 B13 H13 124.0 . . ? C45 C41 C42 107.9(4) . . ? C45 C41 Co4 69.7(2) . . ? C42 C41 Co4 70.5(2) . . ? C45 C41 H41 126.0 . . ? C42 C41 H41 126.0 . . ? Co4 C41 H41 126.0 . . ? C43 C42 C41 108.9(4) . . ? C43 C42 Co4 71.8(2) . . ? C41 C42 Co4 69.1(2) . . ? C43 C42 H42 125.6 . . ? C41 C42 H42 125.6 . . ? Co4 C42 H42 125.6 . . ? C42 C43 C44 107.4(4) . . ? C42 C43 Co4 68.6(2) . . ? C44 C43 Co4 69.8(2) . . ? C42 C43 H43 126.3 . . ? C44 C43 H43 126.3 . . ? Co4 C43 H43 126.3 . . ? C43 C44 C45 108.1(4) . . ? C43 C44 Co4 70.7(2) . . ? C45 C44 Co4 67.9(2) . . ? C43 C44 H44 125.9 . . ? C45 C44 H44 125.9 . . ? Co4 C44 H44 125.9 . . ? C41 C45 C44 107.7(4) . . ? C41 C45 Co4 69.9(3) . . ? C44 C45 Co4 71.7(2) . . ? C41 C45 H45 126.1 . . ? C44 C45 H45 126.1 . . ? Co4 C45 H45 126.1 . . ? C1 C1' B2' 117.8(4) . . ? C1 C1' B3' 119.5(4) . . ? B2' C1' B3' 122.6(4) . . ? C1 C1' B5' 119.1(3) . . ? B2' C1' B5' 73.7(3) . . ? B3' C1' B5' 76.2(3) . . ? C1 C1' Co4' 133.0(3) . . ? B2' C1' Co4' 71.9(3) . . ? B3' C1' Co4' 72.6(2) . . ? B5' C1' Co4' 107.9(3) . . ? C1' B2' C6' 119.8(4) . . ? C1' B2' B9' 115.7(4) . . ? C6' B2' B9' 56.9(3) . . ? C1' B2' B5' 58.6(3) . . ? C6' B2' B5' 96.0(3) . . ? B9' B2' B5' 58.4(3) . . ? C1' B2' Co4' 65.8(2) . . ? C6' B2' Co4' 65.0(2) . . ? B9' B2' Co4' 110.9(3) . . ? B5' B2' Co4' 97.0(3) . . ? C1' B2' H2' 112.5 . . ? C6' B2' H2' 121.5 . . ? B9' B2' H2' 119.3 . . ? B5' B2' H2' 134.1 . . ? Co4' B2' H2' 121.2 . . ? C1' B3' B8' 113.4(4) . . ? C1' B3' B7' 121.1(4) . . ? B8' B3' B7' 58.5(3) . . ? C1' B3' B5' 57.0(3) . . ? B8' B3' B5' 57.9(3) . . ? B7' B3' B5' 98.8(3) . . ? C1' B3' Co4' 65.1(2) . . ? B8' B3' Co4' 108.7(3) . . ? B7' B3' Co4' 64.9(2) . . ? B5' B3' Co4' 94.6(2) . . ? C1' B3' H3' 113.5 . . ? B8' B3' H3' 120.4 . . ? B7' B3' H3' 119.0 . . ? B5' B3' H3' 134.3 . . ? Co4' B3' H3' 123.2 . . ? C44' Co4' C43' 40.71(19) . . ? C44' Co4' C45' 41.00(19) . . ? C43' Co4' C45' 68.32(19) . . ? C44' Co4' C41' 67.65(18) . . ? C43' Co4' C41' 67.07(19) . . ? C45' Co4' C41' 40.04(18) . . ? C44' Co4' C42' 68.15(18) . . ? C43' Co4' C42' 40.26(19) . . ? C45' Co4' C42' 67.83(18) . . ? C41' Co4' C42' 39.66(18) . . ? C44' Co4' C1' 153.43(19) . . ? C43' Co4' C1' 152.92(18) . . ? C45' Co4' C1' 113.37(18) . . ? C41' Co4' C1' 96.38(17) . . ? C42' Co4' C1' 113.59(17) . . ? C44' Co4' B10' 88.25(19) . . ? C43' Co4' B10' 88.89(19) . . ? C45' Co4' B10' 123.6(2) . . ? C41' Co4' B10' 154.23(19) . . ? C42' Co4' B10' 123.79(19) . . ? C1' Co4' B10' 109.39(17) . . ? C44' Co4' C6' 122.19(18) . . ? C43' Co4' C6' 95.53(18) . . ? C45' Co4' C6' 162.68(18) . . ? C41' Co4' C6' 140.36(18) . . ? C42' Co4' C6' 104.27(17) . . ? C1' Co4' C6' 83.83(16) . . ? B10' Co4' C6' 46.89(18) . . ? C44' Co4' B7' 90.33(18) . . ? C43' Co4' B7' 120.34(19) . . ? C45' Co4' B7' 97.83(19) . . ? C41' Co4' B7' 134.89(19) . . ? C42' Co4' B7' 158.35(19) . . ? C1' Co4' B7' 86.64(17) . . ? B10' Co4' B7' 49.85(19) . . ? C6' Co4' B7' 84.75(18) . . ? C44' Co4' B2' 162.32(19) . . ? C43' Co4' B2' 121.80(19) . . ? C45' Co4' B2' 147.32(19) . . ? C41' Co4' B2' 111.26(19) . . ? C42' Co4' B2' 99.36(18) . . ? C1' Co4' B2' 42.36(17) . . ? B10' Co4' B2' 88.83(19) . . ? C6' Co4' B2' 46.78(17) . . ? B7' Co4' B2' 101.03(19) . . ? C44' Co4' B3' 120.85(19) . . ? C43' Co4' B3' 161.56(19) . . ? C45' Co4' B3' 96.72(18) . . ? C41' Co4' B3' 108.85(18) . . ? C42' Co4' B3' 145.16(18) . . ? C1' Co4' B3' 42.27(17) . . ? B10' Co4' B3' 90.95(19) . . ? C6' Co4' B3' 97.80(17) . . ? B7' Co4' B3' 48.83(18) . . ? B2' Co4' B3' 76.63(18) . . ? C1' B5' B11' 135.2(4) . . ? C1' B5' B9' 102.2(3) . . ? B11' B5' B9' 57.2(3) . . ? C1' B5' B8' 99.8(3) . . ? B11' B5' B8' 56.5(3) . . ? B9' B5' B8' 104.2(3) . . ? C1' B5' B2' 47.7(2) . . ? B11' B5' B2' 105.8(3) . . ? B9' B5' B2' 55.5(2) . . ? B8' B5' B2' 117.5(3) . . ? C1' B5' B3' 46.8(2) . . ? B11' B5' B3' 104.9(3) . . ? B9' B5' B3' 119.3(3) . . ? B8' B5' B3' 54.1(2) . . ? B2' B5' B3' 83.7(3) . . ? C1' B5' H5' 110(2) . . ? B11' B5' H5' 115(2) . . ? B9' B5' H5' 120(2) . . ? B8' B5' H5' 118(2) . . ? B2' B5' H5' 123(2) . . ? B3' B5' H5' 119(2) . . ? B9' C6' B10' 114.8(3) . . ? B9' C6' B12' 62.1(3) . . ? B10' C6' B12' 63.7(3) . . ? B9' C6' B2' 64.5(3) . . ? B10' C6' B2' 124.7(4) . . ? B12' C6' B2' 121.6(3) . . ? B9' C6' Co4' 119.3(3) . . ? B10' C6' Co4' 66.5(2) . . ? B12' C6' Co4' 122.1(3) . . ? B2' C6' Co4' 68.2(2) . . ? B9' C6' H6' 119.0 . . ? B10' C6' H6' 114.7 . . ? B12' C6' H6' 114.8 . . ? B2' C6' H6' 110.3 . . ? Co4' C6' H6' 111.6 . . ? B13' B7' B8' 59.8(3) . . ? B13' B7' B3' 114.7(4) . . ? B8' B7' B3' 60.6(3) . . ? B13' B7' B10' 60.4(3) . . ? B8' B7' B10' 106.3(4) . . ? B3' B7' B10' 116.7(4) . . ? B13' B7' Co4' 115.2(3) . . ? B8' B7' Co4' 111.2(3) . . ? B3' B7' Co4' 66.3(2) . . ? B10' B7' Co4' 63.6(2) . . ? B13' B7' H7' 118.6 . . ? B8' B7' H7' 124.2 . . ? B3' B7' H7' 115.2 . . ? B10' B7' H7' 120.1 . . ? Co4' B7' H7' 116.1 . . ? B11' B8' B13' 61.4(3) . . ? B11' B8' B7' 108.9(4) . . ? B13' B8' B7' 59.9(3) . . ? B11' B8' B3' 119.4(4) . . ? B13' B8' B3' 115.1(3) . . ? B7' B8' B3' 60.9(3) . . ? B11' B8' B5' 59.0(3) . . ? B13' B8' B5' 107.8(3) . . ? B7' B8' B5' 107.5(3) . . ? B3' B8' B5' 68.0(3) . . ? B11' B8' H8' 118.7 . . ? B13' B8' H8' 120.7 . . ? B7' B8' H8' 123.7 . . ? B3' B8' H8' 112.7 . . ? B5' B8' H8' 121.5 . . ? C6' B9' B12' 59.4(3) . . ? C6' B9' B11' 104.7(4) . . ? B12' B9' B11' 61.2(3) . . ? C6' B9' B2' 58.6(3) . . ? B12' B9' B2' 113.8(4) . . ? B11' B9' B2' 116.7(4) . . ? C6' B9' B5' 102.5(3) . . ? B12' B9' B5' 108.2(4) . . ? B11' B9' B5' 59.2(3) . . ? B2' B9' B5' 66.1(3) . . ? C6' B9' H9' 127.4 . . ? B12' B9' H9' 119.8 . . ? B11' B9' H9' 120.2 . . ? B2' B9' H9' 114.7 . . ? B5' B9' H9' 122.8 . . ? C6' B10' B12' 58.2(3) . . ? C6' B10' B13' 105.6(3) . . ? B12' B10' B13' 59.4(3) . . ? C6' B10' B7' 111.6(3) . . ? B12' B10' B7' 108.5(3) . . ? B13' B10' B7' 58.3(3) . . ? C6' B10' Co4' 66.6(2) . . ? B12' B10' Co4' 117.5(3) . . ? B13' B10' Co4' 115.8(3) . . ? B7' B10' Co4' 66.5(2) . . ? C6' B10' H10' 121.7 . . ? B12' B10' H10' 120.8 . . ? B13' B10' H10' 122.8 . . ? B7' B10' H10' 120.3 . . ? Co4' B10' H10' 111.5 . . ? B8' B11' B9' 115.7(3) . . ? B8' B11' B12' 109.8(4) . . ? B9' B11' B12' 59.1(3) . . ? B8' B11' B13' 59.7(3) . . ? B9' B11' B13' 109.3(3) . . ? B12' B11' B13' 59.8(3) . . ? B8' B11' B5' 64.4(3) . . ? B9' B11' B5' 63.6(3) . . ? B12' B11' B5' 109.9(3) . . ? B13' B11' B5' 110.7(3) . . ? B8' B11' H11' 117.8 . . ? B9' B11' H11' 118.7 . . ? B12' B11' H11' 122.5 . . ? B13' B11' H11' 122.1 . . ? B5' B11' H11' 118.4 . . ? C6' B12' B9' 58.5(3) . . ? C6' B12' B13' 106.4(3) . . ? B9' B12' B13' 110.3(4) . . ? C6' B12' B11' 102.9(3) . . ? B9' B12' B11' 59.7(3) . . ? B13' B12' B11' 60.3(3) . . ? C6' B12' B10' 58.1(3) . . ? B9' B12' B10' 107.2(3) . . ? B13' B12' B10' 60.6(3) . . ? B11' B12' B10' 105.7(4) . . ? C6' B12' H12' 125.1 . . ? B9' B12' H12' 120.9 . . ? B13' B12' H12' 120.3 . . ? B11' B12' H12' 124.0 . . ? B10' B12' H12' 122.7 . . ? B8' B13' B7' 60.3(3) . . ? B8' B13' B12' 109.2(4) . . ? B7' B13' B12' 111.5(3) . . ? B8' B13' B11' 58.9(3) . . ? B7' B13' B11' 107.3(3) . . ? B12' B13' B11' 59.8(3) . . ? B8' B13' B10' 107.3(3) . . ? B7' B13' B10' 61.3(3) . . ? B12' B13' B10' 60.0(3) . . ? B11' B13' B10' 104.9(3) . . ? B8' B13' H13' 121.8 . . ? B7' B13' H13' 120.0 . . ? B12' B13' H13' 119.9 . . ? B11' B13' H13' 123.9 . . ? B10' B13' H13' 122.9 . . ? C45' C41' C42' 109.3(4) . . ? C45' C41' Co4' 68.6(2) . . ? C42' C41' Co4' 70.3(2) . . ? C45' C41' H41' 125.3 . . ? C42' C41' H41' 125.3 . . ? Co4' C41' H41' 125.3 . . ? C41' C42' C43' 106.9(4) . . ? C41' C42' Co4' 70.0(2) . . ? C43' C42' Co4' 68.1(2) . . ? C41' C42' H42' 126.5 . . ? C43' C42' H42' 126.5 . . ? Co4' C42' H42' 126.5 . . ? C44' C43' C42' 109.0(4) . . ? C44' C43' Co4' 69.6(2) . . ? C42' C43' Co4' 71.6(3) . . ? C44' C43' H43' 125.5 . . ? C42' C43' H43' 125.5 . . ? Co4' C43' H43' 125.5 . . ? C43' C44' C45' 107.2(4) . . ? C43' C44' Co4' 69.7(3) . . ? C45' C44' Co4' 69.8(2) . . ? C43' C44' H44' 126.4 . . ? C45' C44' H44' 126.4 . . ? Co4' C44' H44' 126.4 . . ? C41' C45' C44' 107.5(4) . . ? C41' C45' Co4' 71.4(3) . . ? C44' C45' Co4' 69.2(3) . . ? C41' C45' H45' 126.2 . . ? C44' C45' H45' 126.2 . . ? Co4' C45' H45' 126.2 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.992 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.125