# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Ales Ruzicka' _publ_contact_author_email ales.ruzicka@upce.cz loop_ _publ_author_name 'Bohumir Gruner' 'Petr Svec' 'Vaclav Sicha' 'Zdenka Padelkova' data_Me3NH_3 _database_code_depnum_ccdc_archive 'CCDC 859798' #TrackingRef '- ESI-CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H26 B18 Co O, C3 H10 N' _chemical_formula_sum 'C9 H36 B18 Co N O' _chemical_formula_weight 427.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.907(2) _cell_length_b 12.982(3) _cell_length_c 15.032(5) _cell_angle_alpha 90 _cell_angle_beta 94.268(19) _cell_angle_gamma 90 _cell_volume 2317.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 18537 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.744 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.046 0 0 1 0.043 0 1 0 0.183 -1 -1 0 0.148 1 -1 0 0.162 1 1 0 0.238 -1 1 0 0.112 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 150(1) _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 Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18449 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 26.99 _reflns_number_total 4999 _reflns_number_gt 3451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0281P)^2^+4.0764P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4999 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 Co3 Co 0.24667(4) 0.29750(3) 0.25166(3) 0.02533(13) Uani 1 1 d . . . C2 C 0.2322(3) 0.1555(3) 0.3085(2) 0.0338(8) Uani 1 1 d . . . H2 H 0.3157 0.1188 0.3110 0.041 Uiso 1 1 d R . . O1 O 0.1669(2) -0.0048(2) 0.00641(17) 0.0429(7) Uani 1 1 d . . . H1 H 0.1646 0.0365 -0.0349 0.051 Uiso 1 1 d R . . B4 B 0.0755(3) 0.2721(3) 0.2133(3) 0.0303(8) Uani 1 1 d . . . H4 H 0.0503 0.3148 0.1519 0.036 Uiso 1 1 d R . . C2' C 0.2545(3) 0.4430(3) 0.2001(2) 0.0350(8) Uani 1 1 d . . . H2' H 0.1684 0.4744 0.1948 0.042 Uiso 1 1 d R . . C1 C 0.1547(3) 0.1639(3) 0.2131(2) 0.0279(7) Uani 1 1 d . . . B4' B 0.3931(3) 0.2763(3) 0.1838(3) 0.0310(9) Uani 1 1 d . . . H4' H 0.4049 0.1943 0.1686 0.037 Uiso 1 1 d R . . B8' B 0.4197(4) 0.3236(4) 0.2931(3) 0.0387(10) Uani 1 1 d . . . H8' H 0.4504 0.2748 0.3496 0.046 Uiso 1 1 d R . . C14 C 0.1148(3) 0.0385(3) 0.0797(2) 0.0351(8) Uani 1 1 d . . . H14A H 0.0937 -0.0156 0.1197 0.042 Uiso 1 1 d R . . H14B H 0.0471 0.0750 0.0582 0.042 Uiso 1 1 d R . . C13 C 0.1964(3) 0.1131(3) 0.1296(2) 0.0313(7) Uani 1 1 d . . . H13A H 0.2148 0.1672 0.0886 0.038 Uiso 1 1 d R . . H13B H 0.2654 0.0760 0.1466 0.038 Uiso 1 1 d R . . C1' C 0.2947(3) 0.3536(3) 0.1333(2) 0.0333(8) Uani 1 1 d . . . H1' H 0.2364 0.3206 0.0806 0.040 Uiso 1 1 d R . . B5 B 0.0139(4) 0.1496(3) 0.2313(3) 0.0352(9) Uani 1 1 d . . . H5 H -0.0494 0.1146 0.1835 0.042 Uiso 1 1 d R . . B11' B 0.3615(4) 0.5273(4) 0.2253(3) 0.0461(12) Uani 1 1 d . . . H11' H 0.3488 0.6094 0.2394 0.055 Uiso 1 1 d R . . B7' B 0.3264(4) 0.4305(3) 0.3036(3) 0.0364(9) Uani 1 1 d . . . H7' H 0.2949 0.4517 0.3681 0.044 Uiso 1 1 d R . . B6 B 0.1163(4) 0.0742(3) 0.2905(3) 0.0393(10) Uani 1 1 d . . . H6 H 0.1213 -0.0097 0.2809 0.047 Uiso 1 1 d R . . B7 B 0.2088(4) 0.2572(3) 0.3794(3) 0.0380(10) Uani 1 1 d . . . H7 H 0.2704 0.2895 0.4301 0.046 Uiso 1 1 d R . . B9 B -0.0182(4) 0.2554(4) 0.2976(3) 0.0435(11) Uani 1 1 d . . . H9 H -0.1026 0.2904 0.2926 0.052 Uiso 1 1 d R . . B8 B 0.1029(4) 0.3339(4) 0.3184(3) 0.0375(10) Uani 1 1 d . . . H8 H 0.0934 0.4173 0.3280 0.045 Uiso 1 1 d R . . B12 B 0.0635(4) 0.2445(4) 0.4004(3) 0.0478(12) Uani 1 1 d . . . H12 H 0.0325 0.2704 0.4638 0.057 Uiso 1 1 d R . . N18 N 0.7169(3) 0.1862(3) 0.0078(2) 0.0582(11) Uani 1 1 d . . . H18 H 0.7631 0.1304 0.0073 0.070 Uiso 1 1 d R . . B12' B 0.4684(4) 0.4538(4) 0.2822(3) 0.0460(12) Uani 1 1 d . . . H12' H 0.5276 0.4886 0.3332 0.055 Uiso 1 1 d R . . B5' B 0.4289(4) 0.3732(4) 0.1060(3) 0.0477(12) Uani 1 1 d . . . H5' H 0.4611 0.3533 0.0415 0.057 Uiso 1 1 d R . . B9' B 0.5103(4) 0.3577(4) 0.2085(3) 0.0483(12) Uani 1 1 d . . . H9' H 0.5973 0.3288 0.2109 0.058 Uiso 1 1 d R . . C17 C 0.7075(4) 0.2308(4) -0.0828(3) 0.0615(13) Uani 1 1 d . . . H17A H 0.6700 0.1820 -0.1229 0.074 Uiso 1 1 d R . . H17B H 0.7813 0.2448 -0.1017 0.074 Uiso 1 1 d R . . H17C H 0.6648 0.2935 -0.0832 0.074 Uiso 1 1 d R . . B11 B 0.1485(5) 0.1331(4) 0.3948(3) 0.0509(13) Uani 1 1 d . . . H11 H 0.1753 0.0866 0.4538 0.061 Uiso 1 1 d R . . C16 C 0.6034(5) 0.1497(4) 0.0323(4) 0.0734(16) Uani 1 1 d . . . H16A H 0.5492 0.2041 0.0225 0.088 Uiso 1 1 d R . . H16B H 0.6078 0.1298 0.0940 0.088 Uiso 1 1 d R . . H16C H 0.5809 0.0916 -0.0042 0.088 Uiso 1 1 d R . . B10 B 0.0083(5) 0.1322(4) 0.3475(3) 0.0505(13) Uani 1 1 d . . . H10 H -0.0582 0.0867 0.3760 0.061 Uiso 1 1 d R . . B6' B 0.3386(5) 0.4774(4) 0.1163(3) 0.0474(12) Uani 1 1 d . . . H6' H 0.3111 0.5263 0.0591 0.057 Uiso 1 1 d R . . B10' B 0.4756(5) 0.4836(4) 0.1676(3) 0.0551(14) Uani 1 1 d . . . H10' H 0.5398 0.5361 0.1445 0.066 Uiso 1 1 d R . . C15 C 0.7709(5) 0.2613(6) 0.0715(4) 0.101(2) Uani 1 1 d . . . H15A H 0.8466 0.2743 0.0566 0.121 Uiso 1 1 d R . . H15B H 0.7720 0.2342 0.1310 0.121 Uiso 1 1 d R . . H15C H 0.7287 0.3243 0.0680 0.121 Uiso 1 1 d 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 Co3 0.0269(2) 0.0224(2) 0.0264(2) -0.0024(2) -0.00005(15) 0.0004(2) C2 0.041(2) 0.0280(18) 0.0313(19) 0.0030(15) -0.0054(15) 0.0000(16) O1 0.0568(17) 0.0366(15) 0.0356(14) -0.0060(12) 0.0056(12) 0.0022(13) B4 0.0265(18) 0.030(2) 0.035(2) -0.0032(17) 0.0046(16) 0.0033(16) C2' 0.039(2) 0.0255(18) 0.040(2) -0.0032(16) 0.0014(16) 0.0019(16) C1 0.0291(17) 0.0255(16) 0.0285(17) -0.0019(14) -0.0002(14) 0.0015(14) B4' 0.0244(18) 0.033(2) 0.036(2) -0.0064(17) 0.0024(16) -0.0013(16) B8' 0.031(2) 0.045(3) 0.039(2) -0.004(2) -0.0045(18) -0.0013(19) C14 0.0381(19) 0.0328(19) 0.0343(19) -0.0081(16) 0.0024(16) -0.0021(16) C13 0.0312(17) 0.0286(18) 0.0346(18) -0.0057(15) 0.0047(14) 0.0019(15) C1' 0.0386(19) 0.0319(19) 0.0293(18) -0.0038(15) 0.0021(15) -0.0053(16) B5 0.033(2) 0.035(2) 0.038(2) -0.0037(18) 0.0041(17) -0.0071(18) B11' 0.065(3) 0.035(2) 0.039(2) -0.005(2) 0.002(2) -0.016(2) B7' 0.043(2) 0.030(2) 0.036(2) -0.0056(18) 0.0022(19) -0.0064(19) B6 0.055(3) 0.029(2) 0.033(2) 0.0025(18) -0.005(2) -0.009(2) B7 0.050(3) 0.031(2) 0.032(2) -0.0043(18) -0.0014(19) -0.013(2) B9 0.034(2) 0.049(3) 0.049(3) -0.017(2) 0.014(2) -0.006(2) B8 0.034(2) 0.033(2) 0.046(3) -0.012(2) 0.0085(19) 0.0016(18) B12 0.056(3) 0.050(3) 0.039(2) -0.013(2) 0.014(2) -0.016(2) N18 0.060(2) 0.070(3) 0.044(2) -0.0061(19) -0.0014(18) 0.037(2) B12' 0.043(3) 0.054(3) 0.040(3) -0.008(2) 0.001(2) -0.017(2) B5' 0.046(3) 0.059(3) 0.040(3) -0.009(2) 0.013(2) -0.019(2) B9' 0.033(2) 0.059(3) 0.052(3) -0.012(2) 0.001(2) -0.010(2) C17 0.055(3) 0.087(4) 0.043(2) 0.009(2) 0.010(2) -0.008(3) B11 0.082(4) 0.040(3) 0.029(2) 0.004(2) -0.002(2) -0.020(3) C16 0.086(4) 0.065(3) 0.073(3) 0.021(3) 0.035(3) 0.023(3) B10 0.065(3) 0.052(3) 0.036(2) -0.007(2) 0.015(2) -0.021(3) B6' 0.065(3) 0.041(3) 0.035(2) 0.003(2) 0.003(2) -0.019(2) B10' 0.063(3) 0.057(3) 0.046(3) -0.006(2) 0.011(2) -0.029(3) C15 0.091(4) 0.130(6) 0.078(4) -0.049(4) -0.026(3) 0.047(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co3 C2 2.044(4) . ? Co3 C1' 2.044(4) . ? Co3 C2' 2.046(4) . ? Co3 B7 2.073(4) . ? Co3 B7' 2.093(4) . ? Co3 B8 2.101(4) . ? Co3 B4 2.102(4) . ? Co3 B4' 2.103(4) . ? Co3 C1 2.109(3) . ? Co3 B8' 2.134(4) . ? C2 C1 1.649(5) . ? C2 B11 1.718(6) . ? C2 B7 1.733(6) . ? C2 B6 1.742(6) . ? C2 H2 1.1006 . ? O1 C14 1.421(4) . ? O1 H1 0.8199 . ? B4 C1 1.692(5) . ? B4 B9 1.764(6) . ? B4 B8 1.780(6) . ? B4 B5 1.780(6) . ? B4 H4 1.0991 . ? C2' C1' 1.629(5) . ? C2' B11' 1.702(6) . ? C2' B6' 1.724(6) . ? C2' B7' 1.726(6) . ? C2' H2' 1.1006 . ? C1 C13 1.534(5) . ? C1 B5 1.728(5) . ? C1 B6 1.731(5) . ? B4' C1' 1.681(5) . ? B4' B8' 1.761(6) . ? B4' B9' 1.767(6) . ? B4' B5' 1.791(6) . ? B4' H4' 1.1000 . ? B8' B9' 1.784(7) . ? B8' B7' 1.791(6) . ? B8' B12' 1.798(7) . ? B8' H8' 1.1001 . ? C14 C13 1.527(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C1' B5' 1.698(6) . ? C1' B6' 1.714(6) . ? C1' H1' 1.1005 . ? B5 B6 1.753(6) . ? B5 B9 1.756(6) . ? B5 B10 1.768(6) . ? B5 H5 1.1001 . ? B11' B10' 1.760(8) . ? B11' B12' 1.761(7) . ? B11' B6' 1.765(6) . ? B11' B7' 1.792(6) . ? B11' H11' 1.0993 . ? B7' B12' 1.770(6) . ? B7' H7' 1.1003 . ? B6 B11 1.761(6) . ? B6 B10 1.766(7) . ? B6 H6 1.1009 . ? B7 B11 1.786(6) . ? B7 B12 1.789(7) . ? B7 B8 1.803(7) . ? B7 H7 1.1006 . ? B9 B12 1.769(7) . ? B9 B8 1.775(6) . ? B9 B10 1.784(8) . ? B9 H9 1.1004 . ? B8 B12 1.782(7) . ? B8 H8 1.0992 . ? B12 B10 1.763(7) . ? B12 B11 1.771(8) . ? B12 H12 1.1000 . ? N18 C17 1.476(6) . ? N18 C15 1.479(7) . ? N18 C16 1.504(6) . ? N18 H18 0.9100 . ? B12' B9' 1.765(7) . ? B12' B10' 1.774(7) . ? B12' H12' 1.0992 . ? B5' B6' 1.742(8) . ? B5' B9' 1.770(7) . ? B5' B10' 1.773(7) . ? B5' H5' 1.0996 . ? B9' B10' 1.784(8) . ? B9' H9' 1.0998 . ? C17 H17A 0.9613 . ? C17 H17B 0.9608 . ? C17 H17C 0.9595 . ? B11 B10 1.766(8) . ? B11 H11 1.1003 . ? C16 H16A 0.9606 . ? C16 H16B 0.9604 . ? C16 H16C 0.9591 . ? B10 H10 1.1000 . ? B6' B10' 1.754(8) . ? B6' H6' 1.0989 . ? B10' H10' 1.0995 . ? C15 H15A 0.9598 . ? C15 H15B 0.9603 . ? C15 H15C 0.9593 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Co3 C1' 136.31(15) . . ? C2 Co3 C2' 176.52(15) . . ? C1' Co3 C2' 46.95(14) . . ? C2 Co3 B7 49.79(16) . . ? C1' Co3 B7 172.45(15) . . ? C2' Co3 B7 127.10(16) . . ? C2 Co3 B7' 129.65(16) . . ? C1' Co3 B7' 83.22(16) . . ? C2' Co3 B7' 49.29(16) . . ? B7 Co3 B7' 89.24(17) . . ? C2 Co3 B8 84.62(17) . . ? C1' Co3 B8 128.77(17) . . ? C2' Co3 B8 92.01(17) . . ? B7 Co3 B8 51.18(18) . . ? B7' Co3 B8 89.98(17) . . ? C2 Co3 B4 82.11(16) . . ? C1' Co3 B4 98.38(16) . . ? C2' Co3 B4 96.41(16) . . ? B7 Co3 B4 86.62(17) . . ? B7' Co3 B4 129.44(17) . . ? B8 Co3 B4 50.09(16) . . ? C2 Co3 B4' 100.59(16) . . ? C1' Co3 B4' 47.79(15) . . ? C2' Co3 B4' 82.75(16) . . ? B7 Co3 B4' 131.47(18) . . ? B7' Co3 B4' 85.36(17) . . ? B8 Co3 B4' 174.51(18) . . ? B4 Co3 B4' 131.95(15) . . ? C2 Co3 C1 46.76(13) . . ? C1' Co3 C1 103.13(14) . . ? C2' Co3 C1 133.81(14) . . ? B7 Co3 C1 84.42(15) . . ? B7' Co3 C1 173.01(15) . . ? B8 Co3 C1 83.76(15) . . ? B4 Co3 C1 47.38(14) . . ? B4' Co3 C1 101.04(14) . . ? C2 Co3 B8' 97.52(17) . . ? C1' Co3 B8' 82.60(17) . . ? C2' Co3 B8' 83.91(17) . . ? B7 Co3 B8' 92.37(18) . . ? B7' Co3 B8' 50.13(18) . . ? B8 Co3 B8' 128.89(17) . . ? B4 Co3 B8' 178.92(17) . . ? B4' Co3 B8' 49.10(16) . . ? C1 Co3 B8' 132.90(16) . . ? C1 C2 B11 110.5(3) . . ? C1 C2 B7 112.3(3) . . ? B11 C2 B7 62.3(2) . . ? C1 C2 B6 61.3(2) . . ? B11 C2 B6 61.2(2) . . ? B7 C2 B6 113.3(3) . . ? C1 C2 Co3 68.71(17) . . ? B11 C2 Co3 122.7(3) . . ? B7 C2 Co3 65.96(19) . . ? B6 C2 Co3 124.9(2) . . ? C1 C2 H2 120.2 . . ? B11 C2 H2 118.3 . . ? B7 C2 H2 119.7 . . ? B6 C2 H2 116.5 . . ? Co3 C2 H2 107.5 . . ? C14 O1 H1 109.7 . . ? C1 B4 B9 106.4(3) . . ? C1 B4 B8 108.1(3) . . ? B9 B4 B8 60.1(2) . . ? C1 B4 B5 59.6(2) . . ? B9 B4 B5 59.4(2) . . ? B8 B4 B5 108.6(3) . . ? C1 B4 Co3 66.53(17) . . ? B9 B4 Co3 118.3(3) . . ? B8 B4 Co3 64.92(19) . . ? B5 B4 Co3 120.0(3) . . ? C1 B4 H4 122.3 . . ? B9 B4 H4 121.2 . . ? B8 B4 H4 122.6 . . ? B5 B4 H4 119.2 . . ? Co3 B4 H4 110.5 . . ? C1' C2' B11' 110.3(3) . . ? C1' C2' B6' 61.4(2) . . ? B11' C2' B6' 62.0(3) . . ? C1' C2' B7' 109.9(3) . . ? B11' C2' B7' 63.0(2) . . ? B6' C2' B7' 114.0(3) . . ? C1' C2' Co3 66.45(18) . . ? B11' C2' Co3 124.3(3) . . ? B6' C2' Co3 124.1(3) . . ? B7' C2' Co3 66.75(19) . . ? C1' C2' H2' 122.3 . . ? B11' C2' H2' 117.1 . . ? B6' C2' H2' 116.1 . . ? B7' C2' H2' 119.8 . . ? Co3 C2' H2' 107.5 . . ? C13 C1 C2 119.3(3) . . ? C13 C1 B4 125.0(3) . . ? C2 C1 B4 109.2(3) . . ? C13 C1 B5 117.4(3) . . ? C2 C1 B5 110.0(3) . . ? B4 C1 B5 62.7(2) . . ? C13 C1 B6 112.3(3) . . ? C2 C1 B6 62.0(2) . . ? B4 C1 B6 112.4(3) . . ? B5 C1 B6 60.9(2) . . ? C13 C1 Co3 112.7(2) . . ? C2 C1 Co3 64.53(17) . . ? B4 C1 Co3 66.09(18) . . ? B5 C1 Co3 122.3(2) . . ? B6 C1 Co3 121.7(2) . . ? C1' B4' B8' 106.5(3) . . ? C1' B4' B9' 104.5(3) . . ? B8' B4' B9' 60.7(3) . . ? C1' B4' B5' 58.5(2) . . ? B8' B4' B5' 109.3(3) . . ? B9' B4' B5' 59.7(3) . . ? C1' B4' Co3 64.28(17) . . ? B8' B4' Co3 66.39(19) . . ? B9' B4' Co3 119.3(3) . . ? B5' B4' Co3 118.1(3) . . ? C1' B4' H4' 125.4 . . ? B8' B4' H4' 121.0 . . ? B9' B4' H4' 120.7 . . ? B5' B4' H4' 120.2 . . ? Co3 B4' H4' 110.5 . . ? B4' B8' B9' 59.8(2) . . ? B4' B8' B7' 106.4(3) . . ? B9' B8' B7' 106.4(3) . . ? B4' B8' B12' 106.2(3) . . ? B9' B8' B12' 59.0(3) . . ? B7' B8' B12' 59.1(3) . . ? B4' B8' Co3 64.51(18) . . ? B9' B8' Co3 116.9(3) . . ? B7' B8' Co3 63.73(19) . . ? B12' B8' Co3 115.7(3) . . ? B4' B8' H8' 123.1 . . ? B9' B8' H8' 120.6 . . ? B7' B8' H8' 123.4 . . ? B12' B8' H8' 121.4 . . ? Co3 B8' H8' 113.1 . . ? O1 C14 C13 109.5(3) . . ? O1 C14 H14A 110.0 . . ? C13 C14 H14A 109.8 . . ? O1 C14 H14B 109.6 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.3 . . ? C14 C13 C1 116.2(3) . . ? C14 C13 H13A 108.3 . . ? C1 C13 H13A 108.1 . . ? C14 C13 H13B 108.1 . . ? C1 C13 H13B 108.5 . . ? H13A C13 H13B 107.4 . . ? C2' C1' B4' 111.9(3) . . ? C2' C1' B5' 111.5(3) . . ? B4' C1' B5' 64.0(3) . . ? C2' C1' B6' 62.0(2) . . ? B4' C1' B6' 114.6(3) . . ? B5' C1' B6' 61.4(3) . . ? C2' C1' Co3 66.60(18) . . ? B4' C1' Co3 67.93(18) . . ? B5' C1' Co3 126.4(3) . . ? B6' C1' Co3 124.8(2) . . ? C2' C1' H1' 121.5 . . ? B4' C1' H1' 118.3 . . ? B5' C1' H1' 116.0 . . ? B6' C1' H1' 116.2 . . ? Co3 C1' H1' 106.6 . . ? C1 B5 B6 59.6(2) . . ? C1 B5 B9 105.1(3) . . ? B6 B5 B9 108.7(3) . . ? C1 B5 B10 106.2(3) . . ? B6 B5 B10 60.2(3) . . ? B9 B5 B10 60.8(3) . . ? C1 B5 B4 57.6(2) . . ? B6 B5 B4 107.3(3) . . ? B9 B5 B4 59.8(2) . . ? B10 B5 B4 108.0(3) . . ? C1 B5 H5 124.5 . . ? B6 B5 H5 121.2 . . ? B9 B5 H5 121.8 . . ? B10 B5 H5 121.2 . . ? B4 B5 H5 122.7 . . ? C2' B11' B10' 106.0(3) . . ? C2' B11' B12' 105.1(3) . . ? B10' B11' B12' 60.5(3) . . ? C2' B11' B6' 59.6(2) . . ? B10' B11' B6' 59.7(3) . . ? B12' B11' B6' 108.0(4) . . ? C2' B11' B7' 59.2(2) . . ? B10' B11' B7' 108.9(4) . . ? B12' B11' B7' 59.7(3) . . ? B6' B11' B7' 108.9(3) . . ? C2' B11' H11' 123.8 . . ? B10' B11' H11' 122.0 . . ? B12' B11' H11' 122.5 . . ? B6' B11' H11' 121.4 . . ? B7' B11' H11' 120.8 . . ? C2' B7' B12' 103.7(3) . . ? C2' B7' B8' 105.3(3) . . ? B12' B7' B8' 60.7(3) . . ? C2' B7' B11' 57.8(2) . . ? B12' B7' B11' 59.2(3) . . ? B8' B7' B11' 108.0(3) . . ? C2' B7' Co3 63.96(18) . . ? B12' B7' Co3 119.1(3) . . ? B8' B7' Co3 66.14(19) . . ? B11' B7' Co3 117.1(3) . . ? C2' B7' H7' 126.3 . . ? B12' B7' H7' 120.6 . . ? B8' B7' H7' 121.7 . . ? B11' B7' H7' 120.9 . . ? Co3 B7' H7' 111.1 . . ? C1 B6 C2 56.7(2) . . ? C1 B6 B5 59.5(2) . . ? C2 B6 B5 104.7(3) . . ? C1 B6 B11 104.8(3) . . ? C2 B6 B11 58.7(2) . . ? B5 B6 B11 107.9(3) . . ? C1 B6 B10 106.1(3) . . ? C2 B6 B10 105.3(3) . . ? B5 B6 B10 60.3(3) . . ? B11 B6 B10 60.1(3) . . ? C1 B6 H6 123.9 . . ? C2 B6 H6 124.7 . . ? B5 B6 H6 121.9 . . ? B11 B6 H6 122.4 . . ? B10 B6 H6 122.3 . . ? C2 B7 B11 58.4(2) . . ? C2 B7 B12 103.9(3) . . ? B11 B7 B12 59.4(3) . . ? C2 B7 B8 104.2(3) . . ? B11 B7 B8 107.0(3) . . ? B12 B7 B8 59.5(3) . . ? C2 B7 Co3 64.25(19) . . ? B11 B7 Co3 117.7(3) . . ? B12 B7 Co3 117.8(3) . . ? B8 B7 Co3 65.2(2) . . ? C2 B7 H7 126.0 . . ? B11 B7 H7 120.5 . . ? B12 B7 H7 121.1 . . ? B8 B7 H7 123.2 . . ? Co3 B7 H7 111.5 . . ? B5 B9 B4 60.8(2) . . ? B5 B9 B12 107.7(4) . . ? B4 B9 B12 107.5(3) . . ? B5 B9 B8 109.9(3) . . ? B4 B9 B8 60.4(2) . . ? B12 B9 B8 60.4(3) . . ? B5 B9 B10 59.9(3) . . ? B4 B9 B10 108.1(3) . . ? B12 B9 B10 59.5(3) . . ? B8 B9 B10 109.0(4) . . ? B5 B9 H9 121.4 . . ? B4 B9 H9 121.6 . . ? B12 B9 H9 122.2 . . ? B8 B9 H9 120.1 . . ? B10 B9 H9 122.1 . . ? B9 B8 B4 59.5(2) . . ? B9 B8 B12 59.7(3) . . ? B4 B8 B12 106.3(3) . . ? B9 B8 B7 107.5(3) . . ? B4 B8 B7 106.1(3) . . ? B12 B8 B7 59.9(3) . . ? B9 B8 Co3 117.9(3) . . ? B4 B8 Co3 64.98(18) . . ? B12 B8 Co3 116.7(3) . . ? B7 B8 Co3 63.6(2) . . ? B9 B8 H8 119.9 . . ? B4 B8 H8 123.1 . . ? B12 B8 H8 121.1 . . ? B7 B8 H8 123.5 . . ? Co3 B8 H8 112.3 . . ? B10 B12 B9 60.7(3) . . ? B10 B12 B11 59.9(3) . . ? B9 B12 B11 107.6(3) . . ? B10 B12 B8 109.6(3) . . ? B9 B12 B8 60.0(3) . . ? B11 B12 B8 108.6(3) . . ? B10 B12 B7 109.3(3) . . ? B9 B12 B7 108.4(3) . . ? B11 B12 B7 60.2(3) . . ? B8 B12 B7 60.7(3) . . ? B10 B12 H12 120.4 . . ? B9 B12 H12 122.3 . . ? B11 B12 H12 121.4 . . ? B8 B12 H12 121.5 . . ? B7 B12 H12 121.0 . . ? C17 N18 C15 109.8(5) . . ? C17 N18 C16 109.9(4) . . ? C15 N18 C16 113.9(4) . . ? C17 N18 H18 108.0 . . ? C15 N18 H18 107.2 . . ? C16 N18 H18 107.8 . . ? B11' B12' B9' 107.8(3) . . ? B11' B12' B7' 61.0(3) . . ? B9' B12' B7' 108.1(3) . . ? B11' B12' B10' 59.7(3) . . ? B9' B12' B10' 60.5(3) . . ? B7' B12' B10' 109.2(3) . . ? B11' B12' B8' 109.2(3) . . ? B9' B12' B8' 60.1(3) . . ? B7' B12' B8' 60.3(2) . . ? B10' B12' B8' 109.4(3) . . ? B11' B12' H12' 121.2 . . ? B9' B12' H12' 122.1 . . ? B7' B12' H12' 121.0 . . ? B10' B12' H12' 120.8 . . ? B8' B12' H12' 121.1 . . ? C1' B5' B6' 59.7(3) . . ? C1' B5' B9' 103.7(3) . . ? B6' B5' B9' 108.2(3) . . ? C1' B5' B10' 105.0(3) . . ? B6' B5' B10' 59.9(3) . . ? B9' B5' B10' 60.4(3) . . ? C1' B5' B4' 57.5(2) . . ? B6' B5' B4' 107.9(3) . . ? B9' B5' B4' 59.5(3) . . ? B10' B5' B4' 107.9(3) . . ? C1' B5' H5' 125.0 . . ? B6' B5' H5' 121.3 . . ? B9' B5' H5' 122.5 . . ? B10' B5' H5' 122.3 . . ? B4' B5' H5' 121.8 . . ? B12' B9' B4' 107.4(3) . . ? B12' B9' B5' 107.7(4) . . ? B4' B9' B5' 60.8(3) . . ? B12' B9' B10' 60.0(3) . . ? B4' B9' B10' 108.5(3) . . ? B5' B9' B10' 59.9(3) . . ? B12' B9' B8' 60.9(3) . . ? B4' B9' B8' 59.4(2) . . ? B5' B9' B8' 109.2(3) . . ? B10' B9' B8' 109.7(4) . . ? B12' B9' H9' 122.0 . . ? B4' B9' H9' 122.0 . . ? B5' B9' H9' 121.4 . . ? B10' B9' H9' 121.1 . . ? B8' B9' H9' 120.7 . . ? N18 C17 H17A 108.7 . . ? N18 C17 H17B 109.8 . . ? H17A C17 H17B 109.4 . . ? N18 C17 H17C 110.0 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C2 B11 B6 60.1(2) . . ? C2 B11 B10 106.3(3) . . ? B6 B11 B10 60.1(3) . . ? C2 B11 B12 105.3(3) . . ? B6 B11 B12 108.0(4) . . ? B10 B11 B12 59.8(3) . . ? C2 B11 B7 59.2(2) . . ? B6 B11 B7 109.8(3) . . ? B10 B11 B7 109.3(4) . . ? B12 B11 B7 60.4(3) . . ? C2 B11 H11 123.5 . . ? B6 B11 H11 120.7 . . ? B10 B11 H11 122.0 . . ? B12 B11 H11 122.8 . . ? B7 B11 H11 120.3 . . ? N18 C16 H16A 109.7 . . ? N18 C16 H16B 109.6 . . ? H16A C16 H16B 109.5 . . ? N18 C16 H16C 109.1 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? B12 B10 B11 60.2(3) . . ? B12 B10 B6 108.1(3) . . ? B11 B10 B6 59.8(3) . . ? B12 B10 B5 107.5(3) . . ? B11 B10 B5 107.0(3) . . ? B6 B10 B5 59.5(2) . . ? B12 B10 B9 59.8(3) . . ? B11 B10 B9 107.2(3) . . ? B6 B10 B9 106.9(3) . . ? B5 B10 B9 59.3(3) . . ? B12 B10 H10 121.5 . . ? B11 B10 H10 122.2 . . ? B6 B10 H10 122.1 . . ? B5 B10 H10 122.3 . . ? B9 B10 H10 122.3 . . ? C1' B6' C2' 56.6(2) . . ? C1' B6' B5' 58.8(3) . . ? C2' B6' B5' 105.1(3) . . ? C1' B6' B10' 105.2(4) . . ? C2' B6' B10' 105.2(3) . . ? B5' B6' B10' 60.9(3) . . ? C1' B6' B11' 103.6(3) . . ? C2' B6' B11' 58.4(2) . . ? B5' B6' B11' 108.3(4) . . ? B10' B6' B11' 60.0(3) . . ? C1' B6' H6' 125.5 . . ? C2' B6' H6' 124.4 . . ? B5' B6' H6' 121.9 . . ? B10' B6' H6' 122.1 . . ? B11' B6' H6' 122.1 . . ? B6' B10' B11' 60.3(3) . . ? B6' B10' B5' 59.2(3) . . ? B11' B10' B5' 107.2(3) . . ? B6' B10' B12' 107.8(3) . . ? B11' B10' B12' 59.8(3) . . ? B5' B10' B12' 107.2(4) . . ? B6' B10' B9' 107.0(3) . . ? B11' B10' B9' 107.1(3) . . ? B5' B10' B9' 59.7(3) . . ? B12' B10' B9' 59.5(3) . . ? B6' B10' H10' 122.4 . . ? B11' B10' H10' 122.4 . . ? B5' B10' H10' 122.3 . . ? B12' B10' H10' 121.8 . . ? B9' B10' H10' 121.9 . . ? N18 C15 H15A 109.6 . . ? N18 C15 H15B 109.7 . . ? H15A C15 H15B 109.5 . . ? N18 C15 H15C 109.0 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N18 H18 O1 0.91 1.85 2.748(4) 168.6 3_655 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.425 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.073 #END data_2Me3NH_6 _database_code_depnum_ccdc_archive 'CCDC 859799' #TrackingRef '- ESI-CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H49 B18 Co N2 O2' _chemical_formula_weight 531.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 14.2370(9) _cell_length_b 13.7820(7) _cell_length_c 13.6790(10) _cell_angle_alpha 90 _cell_angle_beta 93.537(7) _cell_angle_gamma 90 _cell_volume 2678.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 18537 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.661 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.093 -1 0 0 0.099 0 -1 0 0.123 0 1 0 0.119 0 0 1 0.012 0 0 -1 0.088 -1 -1 0 0.122 1 -1 0 0.113 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.878 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 150(1) _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 Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19929 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10097 _reflns_number_gt 8609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0894P)^2^+6.6918P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 10097 _refine_ls_number_parameters 551 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1755 _refine_ls_wR_factor_gt 0.1654 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.004 _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 Co3 Co 0.97498(5) 0.53422(4) 0.33331(5) 0.01674(15) Uani 1 1 d . . . B7 B 0.8835(4) 0.6539(4) 0.3303(5) 0.0245(12) Uani 1 1 d . . . H7 H 0.8099 0.6292 0.3236 0.029 Uiso 1 1 d R . . C1 C 1.0666(4) 0.6365(4) 0.2749(4) 0.0209(10) Uani 1 1 d . . . B7' B 1.0668(5) 0.4177(4) 0.3500(5) 0.0246(14) Uani 1 1 d . . . H7' H 1.1396 0.4449 0.3517 0.029 Uiso 1 1 d R . . B4 B 1.0763(4) 0.6253(4) 0.4011(4) 0.0222(12) Uani 1 1 d . . . H4 H 1.1299 0.5825 0.4434 0.027 Uiso 1 1 d R . . B8 B 0.9584(4) 0.6427(4) 0.4408(4) 0.0221(12) Uani 1 1 d . . . H8 H 0.9363 0.6133 0.5105 0.027 Uiso 1 1 d R . . B5' B 0.8456(5) 0.3302(4) 0.3367(5) 0.0259(13) Uani 1 1 d . . . H5' H 0.7731 0.3025 0.3320 0.031 Uiso 1 1 d R . . C2' C 0.9926(4) 0.4122(4) 0.2468(4) 0.0223(10) Uani 1 1 d . . . H2' H 1.0182 0.4375 0.1769 0.027 Uiso 1 1 d R . . C1' C 0.8831(4) 0.4270(4) 0.2695(4) 0.0219(11) Uani 1 1 d . . . B12 B 0.9161(5) 0.7600(5) 0.3978(5) 0.0273(14) Uani 1 1 d . . . H12 H 0.8655 0.8015 0.4389 0.033 Uiso 1 1 d R . . B11 B 0.9141(4) 0.7605(4) 0.2694(5) 0.0243(12) Uani 1 1 d . . . H11 H 0.8609 0.8024 0.2255 0.029 Uiso 1 1 d R . . B5 B 1.1062(4) 0.7356(4) 0.3393(4) 0.0239(12) Uani 1 1 d . . . H5 H 1.1793 0.7617 0.3412 0.029 Uiso 1 1 d R . . B11' B 1.0367(4) 0.3053(4) 0.2905(4) 0.0224(12) Uani 1 1 d . . . H11' H 1.0902 0.2617 0.2557 0.027 Uiso 1 1 d R . . C2 C 0.9572(4) 0.6501(4) 0.2384(4) 0.0234(11) Uani 1 1 d . . . H2 H 0.9306 0.6199 0.1675 0.028 Uiso 1 1 d R . . B6 B 1.0295(5) 0.7487(4) 0.2335(5) 0.0250(13) Uani 1 1 d . . . H6 H 1.0525 0.7823 0.1661 0.030 Uiso 1 1 d R . . B12' B 1.0337(6) 0.3140(5) 0.4190(5) 0.0318(16) Uani 1 1 d . . . H12' H 1.0852 0.2753 0.4679 0.038 Uiso 1 1 d R . . B8' B 0.9912(5) 0.4335(4) 0.4489(5) 0.0267(13) Uani 1 1 d . . . H8' H 1.0149 0.4670 0.5192 0.032 Uiso 1 1 d R . . B6' B 0.9188(5) 0.3131(4) 0.2391(5) 0.0250(14) Uani 1 1 d . . . H6' H 0.8971 0.2751 0.1706 0.030 Uiso 1 1 d R . . B4' B 0.8746(4) 0.4447(4) 0.3935(5) 0.0241(12) Uani 1 1 d . . . H4' H 0.8202 0.4897 0.4250 0.029 Uiso 1 1 d R . . C13 C 1.1350(4) 0.5910(4) 0.2040(4) 0.0275(12) Uani 1 1 d . . . H13A H 1.1039 0.5927 0.1389 0.033 Uiso 1 1 d R . . H13B H 1.1451 0.5234 0.2213 0.033 Uiso 1 1 d R . . C15 C 1.0635(4) 1.0254(5) 0.5512(5) 0.0382(14) Uani 1 1 d . . . H15A H 1.0701 1.0889 0.5237 0.046 Uiso 1 1 d R . . H15B H 1.1194 1.0093 0.5907 0.046 Uiso 1 1 d R . . H15C H 1.0540 0.9788 0.4994 0.046 Uiso 1 1 d R . . C16 C 0.8975(4) 1.0578(5) 0.5562(5) 0.0378(14) Uani 1 1 d . . . H16A H 0.8851 1.0183 0.4991 0.045 Uiso 1 1 d R . . H16B H 0.8450 1.0545 0.5969 0.045 Uiso 1 1 d R . . H16C H 0.9069 1.1239 0.5367 0.045 Uiso 1 1 d R . . B10 B 1.0084(5) 0.8175(4) 0.3369(5) 0.0286(13) Uani 1 1 d . . . H10 H 1.0174 0.8968 0.3384 0.034 Uiso 1 1 d R . . B9 B 1.0362(4) 0.7425(4) 0.4412(5) 0.0244(12) Uani 1 1 d . . . H9 H 1.0643 0.7739 0.5110 0.029 Uiso 1 1 d R . . B10' B 0.9441(5) 0.2514(4) 0.3532(5) 0.0270(13) Uani 1 1 d . . . H10' H 0.9349 0.1725 0.3602 0.032 Uiso 1 1 d R . . B9' B 0.9126(5) 0.3327(4) 0.4463(5) 0.0329(15) Uani 1 1 d . . . H9' H 0.8832 0.3068 0.5141 0.040 Uiso 1 1 d R . . N18 N 0.9823(3) 1.0225(3) 0.6121(3) 0.0256(9) Uani 1 1 d . . . H18 H 0.9943 1.0637 0.6634 0.031 Uiso 1 1 calc . . . C17 C 0.9680(5) 0.9232(4) 0.6534(5) 0.0404(15) Uani 1 1 d . . . H17A H 0.9467 0.8809 0.6009 0.048 Uiso 1 1 d R . . H17B H 1.0275 0.9007 0.6816 0.048 Uiso 1 1 d R . . H17C H 0.9228 0.9236 0.7026 0.048 Uiso 1 1 d R . . C14 C 1.2282(6) 0.6363(7) 0.1977(7) 0.064(2) Uiso 1 1 d . . . H14A H 1.2614 0.6363 0.2618 0.076 Uiso 1 1 d R . . H14B H 1.2211 0.7027 0.1752 0.076 Uiso 1 1 d R . . N18' N 0.3436(5) 0.6294(4) 0.5804(5) 0.0553(17) Uani 1 1 d . . . H18' H 0.3253 0.5787 0.5410 0.066 Uiso 1 1 d R . . C13' C 0.8155(5) 0.4684(4) 0.1887(5) 0.0344(14) Uani 1 1 d . . . 13'A H 0.8539 0.4988 0.1412 0.041 Uiso 1 1 d R . . 13'B H 0.7797 0.5197 0.2177 0.041 Uiso 1 1 d R . . O1' O 0.6654(5) 0.4508(5) 0.0993(6) 0.088(2) Uiso 1 1 d . . . H1' H 0.6296 0.4115 0.0716 0.132 Uiso 1 1 calc R . . C14' C 0.7449(5) 0.4040(6) 0.1365(6) 0.0537(18) Uiso 1 1 d . . . 14'A H 0.7317 0.3488 0.1775 0.064 Uiso 1 1 d R . . 14'B H 0.7735 0.3796 0.0788 0.064 Uiso 1 1 d R . . C15' C 0.3295(7) 0.7192(6) 0.5235(7) 0.064(2) Uani 1 1 d . . . 15'A H 0.3608 0.7121 0.4637 0.076 Uiso 1 1 d R . . 15'B H 0.2636 0.7302 0.5085 0.076 Uiso 1 1 d R . . 15'C H 0.3558 0.7733 0.5599 0.076 Uiso 1 1 d R . . O1 O 1.2761(8) 0.5792(9) 0.1302(9) 0.146(4) Uiso 1 1 d . . . C17' C 0.2643(9) 0.6378(9) 0.6526(9) 0.094(3) Uiso 1 1 d . . . 17'A H 0.2502 0.7052 0.6616 0.113 Uiso 1 1 d R . . 17'B H 0.2079 0.6039 0.6308 0.113 Uiso 1 1 d R . . 17'C H 0.2889 0.6106 0.7135 0.113 Uiso 1 1 d R . . C16' C 0.4186(11) 0.6038(11) 0.6343(12) 0.126(5) Uiso 1 1 d . . . 16'A H 0.4223 0.6324 0.6985 0.152 Uiso 1 1 d R . . 16'B H 0.4217 0.5344 0.6402 0.152 Uiso 1 1 d R . . 16'C H 0.4702 0.6264 0.5985 0.152 Uiso 1 1 d R . . Co3A Co 1.47594(6) 1.01945(4) 0.32909(5) 0.02004(15) Uani 1 1 d . . . C1A C 1.3836(4) 1.1120(4) 0.4030(4) 0.0228(11) Uani 1 1 d . . . C2A C 1.3707(4) 0.9979(4) 0.4272(4) 0.0204(10) Uani 1 1 d . . . H2A H 1.4053 0.9665 0.4941 0.025 Uiso 1 1 d R . . C2'A C 1.5988(4) 1.0283(4) 0.4149(4) 0.0221(11) Uani 1 1 d . . . H2'A H 1.5800 1.0478 0.4892 0.027 Uiso 1 1 d R . . B11A B 1.2615(5) 0.9578(4) 0.3939(5) 0.0266(13) Uani 1 1 d . . . H11A H 1.2235 0.9023 0.4336 0.032 Uiso 1 1 d R . . B6'A B 1.6972(5) 0.9535(5) 0.4096(5) 0.0259(14) Uani 1 1 d . . . H6'A H 1.7393 0.9248 0.4732 0.031 Uiso 1 1 d R . . B22' B 1.6829(5) 1.0856(6) 0.2466(6) 0.0347(16) Uani 1 1 d . . . H22' H 1.7175 1.1419 0.2045 0.042 Uiso 1 1 d R . . B9A B 1.2667(4) 1.0927(5) 0.2351(5) 0.0285(13) Uani 1 1 d . . . H9A H 1.2315 1.1259 0.1695 0.034 Uiso 1 1 d R . . B7A B 1.3580(5) 0.9267(4) 0.3250(5) 0.0242(13) Uani 1 1 d . . . H7A H 1.3806 0.8507 0.3198 0.029 Uiso 1 1 d R . . C1'A C 1.5801(4) 0.9184(4) 0.3752(4) 0.0259(13) Uani 1 1 d . . . C13A C 1.4359(4) 1.1770(4) 0.4792(4) 0.0300(12) Uani 1 1 d . . . 13AA H 1.4886 1.2066 0.4487 0.036 Uiso 1 1 d R . . 13AB H 1.4621 1.1347 0.5305 0.036 Uiso 1 1 d R . . B4'A B 1.5552(5) 0.9228(5) 0.2515(5) 0.0291(14) Uani 1 1 d . . . H4'A H 1.5097 0.8701 0.2109 0.035 Uiso 1 1 d R . . B5A B 1.2835(4) 1.1570(5) 0.3455(5) 0.0296(13) Uani 1 1 d . . . H5A H 1.2588 1.2323 0.3519 0.035 Uiso 1 1 d R . . B12A B 1.2536(5) 0.9669(5) 0.2652(5) 0.0254(14) Uani 1 1 d . . . H12A H 1.2084 0.9175 0.2199 0.030 Uiso 1 1 d R . . B10A B 1.2032(5) 1.0587(5) 0.3373(5) 0.0283(13) Uani 1 1 d . . . H10A H 1.1267 1.0695 0.3382 0.034 Uiso 1 1 d R . . B4A B 1.3819(5) 1.1278(4) 0.2770(5) 0.0257(13) Uani 1 1 d . . . H4A H 1.4199 1.1853 0.2401 0.031 Uiso 1 1 d R . . B21' B 1.7014(4) 1.0762(5) 0.3766(5) 0.0296(14) Uani 1 1 d . . . H21' H 1.7472 1.1268 0.4195 0.035 Uiso 1 1 d R . . B7'A B 1.5879(5) 1.1139(5) 0.3231(5) 0.0273(13) Uani 1 1 d . . . H7'A H 1.5638 1.1892 0.3306 0.033 Uiso 1 1 d R . . B8A B 1.3623(5) 1.0082(5) 0.2235(5) 0.0249(13) Uani 1 1 d . . . H8A H 1.3853 0.9864 0.1514 0.030 Uiso 1 1 d R . . B8'A B 1.5644(5) 1.0468(6) 0.2147(5) 0.0319(14) Uani 1 1 d . . . H8'A H 1.5252 1.0765 0.1496 0.038 Uiso 1 1 d R . . B5'A B 1.6694(5) 0.8862(5) 0.3023(5) 0.0325(14) Uani 1 1 d . . . H5'A H 1.6946 0.8111 0.2959 0.039 Uiso 1 1 d R . . C23' C 1.5444(5) 0.8399(4) 0.4406(5) 0.0354(14) Uani 1 1 d . . . 23'A H 1.4928 0.8066 0.4052 0.043 Uiso 1 1 d R . . 23'B H 1.5177 0.8732 0.4948 0.043 Uiso 1 1 d R . . B6A B 1.2784(5) 1.0737(5) 0.4432(5) 0.0270(14) Uani 1 1 d . . . H6A H 1.2524 1.0939 0.5146 0.032 Uiso 1 1 d R . . B9'A B 1.6605(5) 0.9654(5) 0.2015(5) 0.0341(15) Uani 1 1 d . . . H9'A H 1.6812 0.9434 0.1286 0.041 Uiso 1 1 d R . . B20' B 1.7453(5) 0.9864(5) 0.3000(5) 0.0344(15) Uani 1 1 d . . . H20' H 1.8211 0.9779 0.2905 0.041 Uiso 1 1 d R . . O1A O 1.4313(5) 1.3161(5) 0.5883(5) 0.0750(17) Uiso 1 1 d . . . H1A H 1.3983 1.3630 0.5997 0.112 Uiso 1 1 calc R . . C24' C 1.6112(6) 0.7680(6) 0.4905(8) 0.067(3) Uani 1 1 d . . . 24'A H 1.6446 0.7933 0.5490 0.080 Uiso 1 1 d R . . 24'B H 1.6575 0.7510 0.4441 0.080 Uiso 1 1 d R . . C14A C 1.3887(10) 1.2625(10) 0.5094(11) 0.112(4) Uiso 1 1 d . . . 14AA H 1.3421 1.2320 0.5482 0.134 Uiso 1 1 d R . . 14AB H 1.3544 1.2989 0.4580 0.134 Uiso 1 1 d R . . O1'A O 1.5650(11) 0.6774(12) 0.4924(11) 0.194(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co3 0.0193(3) 0.0154(2) 0.0153(3) -0.0015(3) -0.0012(2) -0.0007(3) B7 0.021(3) 0.020(3) 0.032(3) -0.002(2) 0.000(3) -0.001(2) C1 0.022(3) 0.018(2) 0.023(3) -0.0043(19) 0.003(2) -0.003(2) B7' 0.034(4) 0.020(3) 0.019(3) 0.000(2) -0.005(3) -0.003(3) B4 0.027(3) 0.022(3) 0.017(3) -0.004(2) -0.001(2) -0.001(2) B8 0.022(3) 0.021(3) 0.024(3) -0.008(2) 0.001(2) 0.002(2) B5' 0.032(3) 0.017(3) 0.030(3) -0.006(2) 0.011(3) -0.006(2) C2' 0.028(3) 0.020(2) 0.019(2) 0.0004(19) 0.002(2) 0.003(2) C1' 0.019(3) 0.021(2) 0.025(3) -0.001(2) -0.001(2) -0.003(2) B12 0.026(3) 0.022(3) 0.033(4) -0.009(2) -0.001(3) 0.003(3) B11 0.029(3) 0.018(3) 0.026(3) -0.006(2) -0.001(2) 0.006(2) B5 0.019(3) 0.023(3) 0.029(3) -0.005(2) -0.001(2) 0.000(2) B11' 0.028(3) 0.015(2) 0.025(3) -0.004(2) 0.000(2) 0.002(2) C2 0.024(3) 0.021(2) 0.024(3) -0.002(2) 0.001(2) 0.003(2) B6 0.027(3) 0.014(3) 0.034(3) 0.002(2) 0.002(3) -0.002(2) B12' 0.047(4) 0.029(4) 0.020(3) 0.005(3) 0.005(3) 0.001(3) B8' 0.037(4) 0.023(3) 0.020(3) 0.003(2) -0.003(3) 0.001(3) B6' 0.036(4) 0.009(3) 0.030(3) -0.002(2) -0.004(3) -0.005(3) B4' 0.026(3) 0.025(3) 0.023(3) -0.005(2) 0.008(2) -0.004(2) C13 0.032(3) 0.020(2) 0.030(3) -0.007(2) 0.003(2) 0.003(2) C15 0.029(3) 0.044(4) 0.042(4) -0.010(3) 0.008(3) -0.013(3) C16 0.019(3) 0.046(3) 0.048(4) 0.010(3) -0.005(3) 0.004(3) B10 0.034(3) 0.019(3) 0.033(3) -0.003(2) 0.001(3) 0.000(2) B9 0.024(3) 0.026(3) 0.024(3) -0.004(2) 0.001(2) -0.002(2) B10' 0.034(3) 0.022(3) 0.025(3) 0.007(2) 0.003(2) 0.002(2) B9' 0.056(4) 0.024(3) 0.019(3) 0.001(2) 0.008(3) 0.002(3) N18 0.032(2) 0.019(2) 0.026(2) 0.0000(16) -0.0053(19) -0.0016(18) C17 0.059(4) 0.024(3) 0.040(4) 0.013(2) 0.015(3) 0.004(3) N18' 0.070(4) 0.036(3) 0.058(4) -0.009(3) -0.018(3) 0.017(3) C13' 0.036(3) 0.026(3) 0.039(3) -0.003(2) -0.012(3) 0.002(2) C15' 0.078(6) 0.045(4) 0.066(5) 0.019(4) -0.012(4) -0.007(4) Co3A 0.0194(3) 0.0235(3) 0.0170(3) 0.0012(4) -0.0013(2) -0.0008(4) C1A 0.026(3) 0.021(2) 0.021(3) -0.001(2) -0.003(2) -0.003(2) C2A 0.024(3) 0.021(2) 0.016(2) 0.0014(19) 0.0015(19) -0.003(2) C2'A 0.021(3) 0.021(3) 0.024(3) -0.002(2) -0.004(2) 0.001(2) B11A 0.029(3) 0.027(3) 0.024(3) 0.004(2) 0.002(3) -0.001(3) B6'A 0.021(3) 0.026(3) 0.030(3) -0.006(2) -0.004(3) 0.006(3) B22' 0.024(3) 0.040(4) 0.041(4) 0.005(3) 0.012(3) -0.001(3) B9A 0.023(3) 0.031(3) 0.031(3) 0.013(3) -0.009(3) -0.007(3) B7A 0.025(3) 0.020(3) 0.026(3) 0.001(2) -0.003(3) 0.001(2) C1'A 0.026(3) 0.028(3) 0.024(3) -0.004(2) -0.003(2) 0.002(2) C13A 0.030(3) 0.027(3) 0.032(3) -0.005(2) -0.002(2) 0.003(2) B4'A 0.023(3) 0.040(4) 0.024(3) -0.009(3) 0.001(3) 0.001(3) B5A 0.024(3) 0.029(3) 0.035(3) 0.010(3) 0.000(3) -0.002(3) B12A 0.022(3) 0.032(3) 0.021(3) 0.005(2) -0.010(2) -0.010(3) B10A 0.025(3) 0.028(3) 0.031(3) 0.009(2) -0.004(3) -0.001(3) B4A 0.025(3) 0.022(3) 0.029(3) 0.010(2) -0.007(3) -0.003(2) B21' 0.017(3) 0.032(3) 0.040(4) -0.005(3) -0.004(3) 0.000(2) B7'A 0.024(3) 0.030(3) 0.027(3) 0.010(3) 0.002(3) -0.008(3) B8A 0.024(3) 0.032(3) 0.019(3) -0.007(2) -0.002(2) -0.006(3) B8'A 0.020(3) 0.045(4) 0.030(3) 0.002(3) -0.003(3) -0.003(3) B5'A 0.022(3) 0.038(4) 0.037(4) -0.006(3) 0.002(3) 0.002(3) C23' 0.041(3) 0.027(3) 0.040(3) 0.010(2) 0.010(3) 0.009(3) B6A 0.027(3) 0.028(3) 0.027(3) -0.002(2) 0.004(3) -0.002(3) B9'A 0.025(3) 0.053(4) 0.024(3) 0.003(3) 0.002(3) 0.002(3) B20' 0.025(3) 0.042(4) 0.036(4) -0.004(3) 0.000(3) -0.001(3) C24' 0.044(4) 0.041(4) 0.114(8) 0.032(4) -0.006(4) 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 Co3 C2 2.064(5) . ? Co3 B7' 2.075(7) . ? Co3 C2' 2.080(5) . ? Co3 B4 2.086(6) . ? Co3 B4' 2.094(6) . ? Co3 B7 2.101(6) . ? Co3 B8' 2.106(6) . ? Co3 C1 2.110(5) . ? Co3 B8 2.120(6) . ? Co3 C1' 2.125(5) . ? B7 C2 1.688(9) . ? B7 B11 1.757(9) . ? B7 B12 1.776(9) . ? B7 B8 1.803(9) . ? B7 H7 1.1002 . ? C1 C13 1.549(7) . ? C1 C2 1.617(7) . ? C1 B5 1.703(7) . ? C1 B6 1.719(8) . ? C1 B4 1.731(8) . ? B7' C2' 1.712(8) . ? B7' B11' 1.791(8) . ? B7' B12' 1.793(9) . ? B7' B8' 1.793(9) . ? B7' H7' 1.1010 . ? B4 B5 1.803(8) . ? B4 B9 1.809(8) . ? B4 B8 1.811(9) . ? B4 H4 1.1003 . ? B8 B9 1.766(9) . ? B8 B12 1.812(9) . ? B8 H8 1.0996 . ? B5' C1' 1.723(8) . ? B5' B9' 1.727(9) . ? B5' B6' 1.759(9) . ? B5' B10' 1.777(9) . ? B5' B4' 1.796(8) . ? B5' H5' 1.0987 . ? C2' C1' 1.621(8) . ? C2' B11' 1.696(7) . ? C2' B6' 1.723(8) . ? C2' H2' 1.1008 . ? C1' C13' 1.529(8) . ? C1' B6' 1.710(8) . ? C1' B4' 1.726(8) . ? B12 B11 1.755(9) . ? B12 B10 1.784(9) . ? B12 B9 1.792(9) . ? B12 H12 1.1010 . ? B11 C2 1.704(8) . ? B11 B6 1.752(9) . ? B11 B10 1.766(9) . ? B11 H11 1.1007 . ? B5 B9 1.765(9) . ? B5 B6 1.768(9) . ? B5 B10 1.791(8) . ? B5 H5 1.0999 . ? B11' B12' 1.766(9) . ? B11' B10' 1.779(9) . ? B11' B6' 1.783(9) . ? B11' H11' 1.1012 . ? C2 B6 1.708(8) . ? C2 H2 1.1010 . ? B6 B10 1.744(9) . ? B6 H6 1.0994 . ? B12' B10' 1.743(10) . ? B12' B9' 1.805(11) . ? B12' B8' 1.811(10) . ? B12' H12' 1.0996 . ? B8' B9' 1.783(9) . ? B8' B4' 1.789(9) . ? B8' H8' 1.1008 . ? B6' B10' 1.794(9) . ? B6' H6' 1.1009 . ? B4' B9' 1.775(9) . ? B4' H4' 1.1008 . ? C13 C14 1.474(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9698 . ? C15 N18 1.467(8) . ? C15 H15A 0.9595 . ? C15 H15B 0.9599 . ? C15 H15C 0.9597 . ? C16 N18 1.472(7) . ? C16 H16A 0.9595 . ? C16 H16B 0.9602 . ? C16 H16C 0.9609 . ? B10 B9 1.787(9) . ? B10 H10 1.1005 . ? B9 H9 1.1008 . ? B10' B9' 1.775(9) . ? B10' H10' 1.1001 . ? B9' H9' 1.0997 . ? N18 C17 1.499(7) . ? N18 H18 0.9100 . ? C17 H17A 0.9596 . ? C17 H17B 0.9602 . ? C17 H17C 0.9604 . ? C14 O1 1.420(14) . ? C14 H14A 0.9701 . ? C14 H14B 0.9689 . ? N18' C16' 1.308(15) . ? N18' C15' 1.469(9) . ? N18' C17' 1.550(14) . ? N18' H18' 0.9106 . ? C13' C14' 1.490(9) . ? C13' 13'A 0.9698 . ? C13' 13'B 0.9706 . ? O1' C14' 1.373(10) . ? O1' H1' 0.8200 . ? C14' 14'A 0.9704 . ? C14' 14'B 0.9703 . ? C15' 15'A 0.9603 . ? C15' 15'B 0.9600 . ? C15' 15'C 0.9597 . ? C17' 17'A 0.9599 . ? C17' 17'B 0.9605 . ? C17' 17'C 0.9598 . ? C16' 16'A 0.9611 . ? C16' 16'B 0.9607 . ? C16' 16'C 0.9597 . ? Co3A C2'A 2.050(5) . ? Co3A B7'A 2.063(6) . ? Co3A B4'A 2.079(6) . ? Co3A C2A 2.094(5) . ? Co3A B4A 2.101(6) . ? Co3A C1'A 2.103(6) . ? Co3A B8'A 2.103(7) . ? Co3A B8A 2.108(6) . ? Co3A B7A 2.108(7) . ? Co3A C1A 2.131(5) . ? C1A C13A 1.533(7) . ? C1A C2A 1.619(7) . ? C1A B5A 1.702(8) . ? C1A B6A 1.711(9) . ? C1A B4A 1.735(9) . ? C2A B11A 1.686(8) . ? C2A B6A 1.703(9) . ? C2A B7A 1.709(8) . ? C2A H2A 1.1008 . ? C2'A C1'A 1.625(8) . ? C2'A B21' 1.714(9) . ? C2'A B7'A 1.723(8) . ? C2'A B6'A 1.745(8) . ? C2'A H2'A 1.1002 . ? B11A B6A 1.745(9) . ? B11A B12A 1.761(9) . ? B11A B7A 1.766(9) . ? B11A B10A 1.773(9) . ? B11A H11A 1.0996 . ? B6'A B20' 1.746(10) . ? B6'A B21' 1.752(10) . ? B6'A B5'A 1.760(10) . ? B6'A C1'A 1.771(9) . ? B6'A H6'A 1.0991 . ? B22' B20' 1.765(11) . ? B22' B21' 1.786(11) . ? B22' B9'A 1.789(11) . ? B22' B8'A 1.797(10) . ? B22' B7'A 1.804(10) . ? B22' H22' 1.1000 . ? B9A B5A 1.755(10) . ? B9A B4A 1.771(9) . ? B9A B10A 1.775(9) . ? B9A B12A 1.795(9) . ? B9A B8A 1.805(10) . ? B9A H9A 1.1002 . ? B7A B12A 1.742(9) . ? B7A B8A 1.790(10) . ? B7A H7A 1.0994 . ? C1'A C23' 1.512(8) . ? C1'A B4'A 1.708(9) . ? C1'A B5'A 1.722(9) . ? C13A C14A 1.430(14) . ? C13A 13AA 0.9706 . ? C13A 13AB 0.9691 . ? B4'A B9'A 1.785(10) . ? B4'A B8'A 1.789(10) . ? B4'A B5'A 1.801(9) . ? B4'A H4'A 1.1006 . ? B5A B6A 1.766(9) . ? B5A B10A 1.772(9) . ? B5A B4A 1.779(10) . ? B5A H5A 1.1010 . ? B12A B8A 1.776(10) . ? B12A B10A 1.782(10) . ? B12A H12A 1.1012 . ? B10A B6A 1.760(9) . ? B10A H10A 1.0999 . ? B4A B8A 1.819(9) . ? B4A H4A 1.0996 . ? B21' B20' 1.761(10) . ? B21' B7'A 1.809(9) . ? B21' H21' 1.1000 . ? B7'A B8'A 1.762(10) . ? B7'A H7'A 1.0998 . ? B8A H8A 1.1000 . ? B8'A B9'A 1.787(10) . ? B8'A H8'A 1.1003 . ? B5'A B20' 1.755(10) . ? B5'A B9'A 1.757(10) . ? B5'A H5'A 1.1002 . ? C23' C24' 1.508(9) . ? C23' 23'A 0.9700 . ? C23' 23'B 0.9700 . ? B6A H6A 1.1008 . ? B9'A B20' 1.776(10) . ? B9'A H9'A 1.0998 . ? B20' H20' 1.1001 . ? O1A C14A 1.413(14) . ? O1A H1A 0.8200 . ? C24' O1'A 1.412(17) . ? C24' 24'A 0.9699 . ? C24' 24'B 0.9701 . ? C14A 14AA 0.9706 . ? C14A 14AB 0.9707 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Co3 B7' 136.1(2) . . ? C2 Co3 C2' 106.4(2) . . ? B7' Co3 C2' 48.7(2) . . ? C2 Co3 B4 82.4(2) . . ? B7' Co3 B4 90.2(2) . . ? C2' Co3 B4 129.4(2) . . ? C2 Co3 B4' 130.0(2) . . ? B7' Co3 B4' 86.7(3) . . ? C2' Co3 B4' 81.8(2) . . ? B4 Co3 B4' 130.5(2) . . ? C2 Co3 B7 47.8(2) . . ? B7' Co3 B7 174.8(3) . . ? C2' Co3 B7 136.1(2) . . ? B4 Co3 B7 87.0(2) . . ? B4' Co3 B7 91.9(2) . . ? C2 Co3 B8' 170.3(2) . . ? B7' Co3 B8' 50.8(3) . . ? C2' Co3 B8' 83.3(2) . . ? B4 Co3 B8' 91.3(3) . . ? B4' Co3 B8' 50.4(3) . . ? B7 Co3 B8' 124.8(3) . . ? C2 Co3 C1 45.6(2) . . ? B7' Co3 C1 99.1(2) . . ? C2' Co3 C1 103.0(2) . . ? B4 Co3 C1 48.7(2) . . ? B4' Co3 C1 174.1(2) . . ? B7 Co3 C1 82.3(2) . . ? B8' Co3 C1 133.0(2) . . ? C2 Co3 B8 82.9(2) . . ? B7' Co3 B8 124.4(2) . . ? C2' Co3 B8 170.7(2) . . ? B4 Co3 B8 51.0(2) . . ? B4' Co3 B8 92.0(2) . . ? B7 Co3 B8 50.6(2) . . ? B8' Co3 B8 87.4(2) . . ? C1 Co3 B8 83.7(2) . . ? C2 Co3 C1' 103.4(2) . . ? B7' Co3 C1' 82.8(2) . . ? C2' Co3 C1' 45.3(2) . . ? B4 Co3 C1' 172.9(2) . . ? B4' Co3 C1' 48.3(2) . . ? B7 Co3 C1' 99.9(2) . . ? B8' Co3 C1' 83.5(2) . . ? C1 Co3 C1' 133.5(2) . . ? B8 Co3 C1' 133.1(2) . . ? C2 B7 B11 59.2(3) . . ? C2 B7 B12 104.9(4) . . ? B11 B7 B12 59.5(4) . . ? C2 B7 B8 105.0(4) . . ? B11 B7 B8 108.5(4) . . ? B12 B7 B8 60.8(3) . . ? C2 B7 Co3 65.0(3) . . ? B11 B7 Co3 119.6(4) . . ? B12 B7 Co3 119.6(4) . . ? B8 B7 Co3 65.3(3) . . ? C2 B7 H7 124.2 . . ? B11 B7 H7 118.8 . . ? B12 B7 H7 121.0 . . ? B8 B7 H7 123.7 . . ? Co3 B7 H7 110.2 . . ? C13 C1 C2 119.0(4) . . ? C13 C1 B5 116.6(4) . . ? C2 C1 B5 110.4(4) . . ? C13 C1 B6 110.5(4) . . ? C2 C1 B6 61.5(3) . . ? B5 C1 B6 62.2(3) . . ? C13 C1 B4 125.1(4) . . ? C2 C1 B4 109.5(4) . . ? B5 C1 B4 63.3(3) . . ? B6 C1 B4 114.3(4) . . ? C13 C1 Co3 113.2(3) . . ? C2 C1 Co3 65.7(3) . . ? B5 C1 Co3 122.2(4) . . ? B6 C1 Co3 122.8(4) . . ? B4 C1 Co3 64.9(3) . . ? C2' B7' B11' 57.9(3) . . ? C2' B7' B12' 103.3(4) . . ? B11' B7' B12' 59.1(4) . . ? C2' B7' B8' 105.0(5) . . ? B11' B7' B8' 108.1(5) . . ? B12' B7' B8' 60.7(4) . . ? C2' B7' Co3 65.8(3) . . ? B11' B7' Co3 119.2(4) . . ? B12' B7' Co3 119.4(5) . . ? B8' B7' Co3 65.5(3) . . ? C2' B7' H7' 124.4 . . ? B11' B7' H7' 120.2 . . ? B12' B7' H7' 122.6 . . ? B8' B7' H7' 123.4 . . ? Co3 B7' H7' 109.0 . . ? C1 B4 B5 57.6(3) . . ? C1 B4 B9 102.5(4) . . ? B5 B4 B9 58.5(3) . . ? C1 B4 B8 105.6(4) . . ? B5 B4 B8 106.2(4) . . ? B9 B4 B8 58.4(3) . . ? C1 B4 Co3 66.4(3) . . ? B5 B4 Co3 118.4(4) . . ? B9 B4 Co3 116.7(4) . . ? B8 B4 Co3 65.5(3) . . ? C1 B4 H4 125.6 . . ? B5 B4 H4 121.5 . . ? B9 B4 H4 122.7 . . ? B8 B4 H4 122.6 . . ? Co3 B4 H4 110.4 . . ? B9 B8 B7 105.9(4) . . ? B9 B8 B4 60.7(3) . . ? B7 B8 B4 105.7(4) . . ? B9 B8 B12 60.1(4) . . ? B7 B8 B12 58.9(3) . . ? B4 B8 B12 108.4(4) . . ? B9 B8 Co3 117.1(4) . . ? B7 B8 Co3 64.2(3) . . ? B4 B8 Co3 63.5(3) . . ? B12 B8 Co3 116.9(4) . . ? B9 B8 H8 119.8 . . ? B7 B8 H8 124.9 . . ? B4 B8 H8 122.1 . . ? B12 B8 H8 120.2 . . ? Co3 B8 H8 113.1 . . ? C1' B5' B9' 106.0(4) . . ? C1' B5' B6' 58.8(3) . . ? B9' B5' B6' 109.9(5) . . ? C1' B5' B10' 105.9(4) . . ? B9' B5' B10' 60.8(4) . . ? B6' B5' B10' 61.0(4) . . ? C1' B5' B4' 58.7(3) . . ? B9' B5' B4' 60.4(4) . . ? B6' B5' B4' 108.4(4) . . ? B10' B5' B4' 108.9(4) . . ? C1' B5' H5' 123.9 . . ? B9' B5' H5' 121.6 . . ? B6' B5' H5' 120.5 . . ? B10' B5' H5' 121.8 . . ? B4' B5' H5' 121.4 . . ? C1' C2' B11' 112.4(4) . . ? C1' C2' B7' 112.9(4) . . ? B11' C2' B7' 63.4(3) . . ? C1' C2' B6' 61.4(3) . . ? B11' C2' B6' 62.8(4) . . ? B7' C2' B6' 115.4(4) . . ? C1' C2' Co3 68.8(3) . . ? B11' C2' Co3 123.9(3) . . ? B7' C2' Co3 65.5(3) . . ? B6' C2' Co3 125.6(4) . . ? C1' C2' H2' 120.0 . . ? B11' C2' H2' 116.5 . . ? B7' C2' H2' 118.8 . . ? B6' C2' H2' 115.6 . . ? Co3 C2' H2' 107.2 . . ? C13' C1' C2' 118.6(5) . . ? C13' C1' B6' 110.5(5) . . ? C2' C1' B6' 62.2(3) . . ? C13' C1' B5' 118.2(5) . . ? C2' C1' B5' 109.7(4) . . ? B6' C1' B5' 61.6(4) . . ? C13' C1' B4' 125.3(5) . . ? C2' C1' B4' 109.4(4) . . ? B6' C1' B4' 114.1(4) . . ? B5' C1' B4' 62.8(3) . . ? C13' C1' Co3 112.4(4) . . ? C2' C1' Co3 65.8(3) . . ? B6' C1' Co3 123.6(4) . . ? B5' C1' Co3 121.5(4) . . ? B4' C1' Co3 64.9(3) . . ? B11 B12 B7 59.7(4) . . ? B11 B12 B10 59.9(4) . . ? B7 B12 B10 107.4(4) . . ? B11 B12 B9 106.8(5) . . ? B7 B12 B9 106.0(4) . . ? B10 B12 B9 60.0(4) . . ? B11 B12 B8 108.2(4) . . ? B7 B12 B8 60.3(3) . . ? B10 B12 B8 108.0(4) . . ? B9 B12 B8 58.7(3) . . ? B11 B12 H12 122.6 . . ? B7 B12 H12 122.3 . . ? B10 B12 H12 122.1 . . ? B9 B12 H12 122.8 . . ? B8 B12 H12 120.9 . . ? C2 B11 B6 59.2(3) . . ? C2 B11 B12 105.2(4) . . ? B6 B11 B12 108.8(5) . . ? C2 B11 B7 58.4(3) . . ? B6 B11 B7 108.7(4) . . ? B12 B11 B7 60.8(4) . . ? C2 B11 B10 104.7(4) . . ? B6 B11 B10 59.4(4) . . ? B12 B11 B10 60.9(4) . . ? B7 B11 B10 109.1(4) . . ? C2 B11 H11 125.4 . . ? B6 B11 H11 121.4 . . ? B12 B11 H11 121.1 . . ? B7 B11 H11 121.0 . . ? B10 B11 H11 121.8 . . ? C1 B5 B9 105.5(4) . . ? C1 B5 B6 59.3(3) . . ? B9 B5 B6 106.9(4) . . ? C1 B5 B10 105.3(4) . . ? B9 B5 B10 60.3(4) . . ? B6 B5 B10 58.7(3) . . ? C1 B5 B4 59.1(3) . . ? B9 B5 B4 60.9(3) . . ? B6 B5 B4 108.5(4) . . ? B10 B5 B4 109.5(4) . . ? C1 B5 H5 123.9 . . ? B9 B5 H5 122.9 . . ? B6 B5 H5 121.4 . . ? B10 B5 H5 121.9 . . ? B4 B5 H5 121.0 . . ? C2' B11' B12' 105.1(4) . . ? C2' B11' B10' 105.2(4) . . ? B12' B11' B10' 58.9(4) . . ? C2' B11' B6' 59.3(3) . . ? B12' B11' B6' 107.9(5) . . ? B10' B11' B6' 60.5(4) . . ? C2' B11' B7' 58.7(3) . . ? B12' B11' B7' 60.5(4) . . ? B10' B11' B7' 107.8(4) . . ? B6' B11' B7' 108.7(4) . . ? C2' B11' H11' 125.0 . . ? B12' B11' H11' 121.9 . . ? B10' B11' H11' 122.3 . . ? B6' B11' H11' 121.5 . . ? B7' B11' H11' 121.1 . . ? C1 C2 B7 113.9(4) . . ? C1 C2 B11 112.5(4) . . ? B7 C2 B11 62.4(4) . . ? C1 C2 B6 62.2(3) . . ? B7 C2 B6 114.1(4) . . ? B11 C2 B6 61.8(4) . . ? C1 C2 Co3 68.7(3) . . ? B7 C2 Co3 67.2(3) . . ? B11 C2 Co3 124.5(4) . . ? B6 C2 Co3 126.1(4) . . ? C1 C2 H2 120.0 . . ? B7 C2 H2 118.2 . . ? B11 C2 H2 116.6 . . ? B6 C2 H2 116.2 . . ? Co3 C2 H2 106.5 . . ? C2 B6 C1 56.3(3) . . ? C2 B6 B10 105.4(4) . . ? C1 B6 B10 106.7(4) . . ? C2 B6 B11 59.0(3) . . ? C1 B6 B11 105.4(4) . . ? B10 B6 B11 60.7(4) . . ? C2 B6 B5 103.3(4) . . ? C1 B6 B5 58.5(3) . . ? B10 B6 B5 61.3(4) . . ? B11 B6 B5 108.8(5) . . ? C2 B6 H6 125.4 . . ? C1 B6 H6 123.6 . . ? B10 B6 H6 121.8 . . ? B11 B6 H6 122.0 . . ? B5 B6 H6 121.9 . . ? B10' B12' B11' 60.9(4) . . ? B10' B12' B7' 109.3(5) . . ? B11' B12' B7' 60.4(3) . . ? B10' B12' B9' 60.0(4) . . ? B11' B12' B9' 107.4(5) . . ? B7' B12' B9' 106.3(5) . . ? B10' B12' B8' 108.8(5) . . ? B11' B12' B8' 108.4(5) . . ? B7' B12' B8' 59.7(4) . . ? B9' B12' B8' 59.1(4) . . ? B10' B12' H12' 120.9 . . ? B11' B12' H12' 121.1 . . ? B7' B12' H12' 121.3 . . ? B9' B12' H12' 123.6 . . ? B8' B12' H12' 121.6 . . ? B9' B8' B4' 59.6(4) . . ? B9' B8' B7' 107.2(4) . . ? B4' B8' B7' 106.0(4) . . ? B9' B8' B12' 60.3(4) . . ? B4' B8' B12' 107.3(5) . . ? B7' B8' B12' 59.6(4) . . ? B9' B8' Co3 117.3(4) . . ? B4' B8' Co3 64.4(3) . . ? B7' B8' Co3 63.7(3) . . ? B12' B8' Co3 116.9(4) . . ? B9' B8' H8' 120.2 . . ? B4' B8' H8' 124.1 . . ? B7' B8' H8' 123.0 . . ? B12' B8' H8' 119.4 . . ? Co3 B8' H8' 113.2 . . ? C1' B6' C2' 56.4(3) . . ? C1' B6' B5' 59.6(4) . . ? C2' B6' B5' 103.6(4) . . ? C1' B6' B11' 104.3(4) . . ? C2' B6' B11' 57.9(3) . . ? B5' B6' B11' 107.3(5) . . ? C1' B6' B10' 105.7(5) . . ? C2' B6' B10' 103.5(4) . . ? B5' B6' B10' 60.0(4) . . ? B11' B6' B10' 59.7(4) . . ? C1' B6' H6' 124.9 . . ? C2' B6' H6' 124.6 . . ? B5' B6' H6' 124.1 . . ? B11' B6' H6' 121.0 . . ? B10' B6' H6' 123.1 . . ? C1' B4' B9' 103.8(4) . . ? C1' B4' B8' 106.6(4) . . ? B9' B4' B8' 60.1(4) . . ? C1' B4' B5' 58.5(3) . . ? B9' B4' B5' 57.8(4) . . ? B8' B4' B5' 106.8(4) . . ? C1' B4' Co3 66.8(3) . . ? B9' B4' Co3 118.3(4) . . ? B8' B4' Co3 65.1(3) . . ? B5' B4' Co3 119.4(4) . . ? C1' B4' H4' 123.9 . . ? B9' B4' H4' 122.3 . . ? B8' B4' H4' 122.7 . . ? B5' B4' H4' 121.1 . . ? Co3 B4' H4' 109.6 . . ? C14 C13 C1 117.9(5) . . ? C14 C13 H13A 107.3 . . ? C1 C13 H13A 107.2 . . ? C14 C13 H13B 107.5 . . ? C1 C13 H13B 109.0 . . ? H13A C13 H13B 107.4 . . ? N18 C15 H15A 110.3 . . ? N18 C15 H15B 109.2 . . ? H15A C15 H15B 109.5 . . ? N18 C15 H15C 108.7 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.6 . . ? N18 C16 H16A 109.8 . . ? N18 C16 H16B 109.0 . . ? H16A C16 H16B 109.5 . . ? N18 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.4 . . ? B6 B10 B11 59.9(4) . . ? B6 B10 B12 107.8(4) . . ? B11 B10 B12 59.2(4) . . ? B6 B10 B9 107.0(4) . . ? B11 B10 B9 106.5(4) . . ? B12 B10 B9 60.2(4) . . ? B6 B10 B5 60.0(4) . . ? B11 B10 B5 107.2(4) . . ? B12 B10 B5 107.8(4) . . ? B9 B10 B5 59.1(3) . . ? B6 B10 H10 122.0 . . ? B11 B10 H10 122.4 . . ? B12 B10 H10 121.4 . . ? B9 B10 H10 122.7 . . ? B5 B10 H10 122.4 . . ? B5 B9 B8 109.9(4) . . ? B5 B9 B10 60.6(3) . . ? B8 B9 B10 109.9(4) . . ? B5 B9 B12 108.6(4) . . ? B8 B9 B12 61.2(4) . . ? B10 B9 B12 59.8(4) . . ? B5 B9 B4 60.6(3) . . ? B8 B9 B4 60.9(3) . . ? B10 B9 B4 109.4(4) . . ? B12 B9 B4 109.4(4) . . ? B5 B9 H9 120.9 . . ? B8 B9 H9 120.2 . . ? B10 B9 H9 121.1 . . ? B12 B9 H9 121.5 . . ? B4 B9 H9 120.6 . . ? B12' B10' B9' 61.7(4) . . ? B12' B10' B5' 108.1(5) . . ? B9' B10' B5' 58.2(4) . . ? B12' B10' B11' 60.2(4) . . ? B9' B10' B11' 108.1(4) . . ? B5' B10' B11' 106.6(4) . . ? B12' B10' B6' 108.4(4) . . ? B9' B10' B6' 106.2(4) . . ? B5' B10' B6' 59.0(4) . . ? B11' B10' B6' 59.8(4) . . ? B12' B10' H10' 122.1 . . ? B9' B10' H10' 121.7 . . ? B5' B10' H10' 121.2 . . ? B11' B10' H10' 123.4 . . ? B6' B10' H10' 121.7 . . ? B5' B9' B10' 61.0(3) . . ? B5' B9' B4' 61.7(4) . . ? B10' B9' B4' 110.0(4) . . ? B5' B9' B8' 110.2(4) . . ? B10' B9' B8' 108.7(5) . . ? B4' B9' B8' 60.4(3) . . ? B5' B9' B12' 107.5(5) . . ? B10' B9' B12' 58.3(4) . . ? B4' B9' B12' 108.1(5) . . ? B8' B9' B12' 60.6(4) . . ? B5' B9' H9' 120.5 . . ? B10' B9' H9' 121.8 . . ? B4' B9' H9' 120.3 . . ? B8' B9' H9' 120.4 . . ? B12' B9' H9' 123.0 . . ? C15 N18 C16 110.2(5) . . ? C15 N18 C17 111.6(5) . . ? C16 N18 C17 111.8(5) . . ? C15 N18 H18 107.7 . . ? C16 N18 H18 107.7 . . ? C17 N18 H18 107.7 . . ? N18 C17 H17A 108.5 . . ? N18 C17 H17B 108.0 . . ? H17A C17 H17B 109.5 . . ? N18 C17 H17C 111.8 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.4 . . ? O1 C14 C13 105.8(8) . . ? O1 C14 H14A 111.2 . . ? C13 C14 H14A 109.7 . . ? O1 C14 H14B 111.2 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.8 . . ? C16' N18' C15' 127.3(10) . . ? C16' N18' C17' 105.2(10) . . ? C15' N18' C17' 101.2(7) . . ? C16' N18' H18' 108.7 . . ? C15' N18' H18' 108.0 . . ? C17' N18' H18' 104.0 . . ? C14' C13' C1' 120.0(5) . . ? C14' C13' 13'A 109.1 . . ? C1' C13' 13'A 106.8 . . ? C14' C13' 13'B 105.9 . . ? C1' C13' 13'B 107.4 . . ? 13'A C13' 13'B 106.9 . . ? C14' O1' H1' 109.5 . . ? O1' C14' C13' 114.4(7) . . ? O1' C14' 14'A 113.5 . . ? C13' C14' 14'A 109.8 . . ? O1' C14' 14'B 103.9 . . ? C13' C14' 14'B 107.0 . . ? 14'A C14' 14'B 107.7 . . ? N18' C15' 15'A 108.1 . . ? N18' C15' 15'B 110.2 . . ? 15'A C15' 15'B 109.4 . . ? N18' C15' 15'C 110.1 . . ? 15'A C15' 15'C 109.5 . . ? 15'B C15' 15'C 109.5 . . ? N18' C17' 17'A 108.7 . . ? N18' C17' 17'B 113.2 . . ? 17'A C17' 17'B 109.4 . . ? N18' C17' 17'C 106.4 . . ? 17'A C17' 17'C 109.6 . . ? 17'B C17' 17'C 109.4 . . ? N18' C16' 16'A 113.6 . . ? N18' C16' 16'B 110.4 . . ? 16'A C16' 16'B 109.4 . . ? N18' C16' 16'C 104.4 . . ? 16'A C16' 16'C 109.4 . . ? 16'B C16' 16'C 109.5 . . ? C2'A Co3A B7'A 49.5(2) . . ? C2'A Co3A B4'A 81.9(2) . . ? B7'A Co3A B4'A 86.5(3) . . ? C2'A Co3A C2A 105.1(2) . . ? B7'A Co3A C2A 134.4(3) . . ? B4'A Co3A C2A 132.0(2) . . ? C2'A Co3A B4A 131.0(2) . . ? B7'A Co3A B4A 90.9(3) . . ? B4'A Co3A B4A 129.6(3) . . ? C2A Co3A B4A 81.5(2) . . ? C2'A Co3A C1'A 46.1(2) . . ? B7'A Co3A C1'A 84.1(3) . . ? B4'A Co3A C1'A 48.2(2) . . ? C2A Co3A C1'A 103.5(2) . . ? B4A Co3A C1'A 174.6(3) . . ? C2'A Co3A B8'A 83.5(2) . . ? B7'A Co3A B8'A 50.0(3) . . ? B4'A Co3A B8'A 50.6(3) . . ? C2A Co3A B8'A 171.1(2) . . ? B4A Co3A B8'A 91.1(3) . . ? C1'A Co3A B8'A 84.1(3) . . ? C2'A Co3A B8A 171.6(3) . . ? B7'A Co3A B8A 125.6(3) . . ? B4'A Co3A B8A 91.2(3) . . ? C2A Co3A B8A 83.1(2) . . ? B4A Co3A B8A 51.2(3) . . ? C1'A Co3A B8A 130.9(2) . . ? B8'A Co3A B8A 88.5(3) . . ? C2'A Co3A B7A 134.6(2) . . ? B7'A Co3A B7A 175.8(3) . . ? B4'A Co3A B7A 93.1(3) . . ? C2A Co3A B7A 48.0(2) . . ? B4A Co3A B7A 86.1(2) . . ? C1'A Co3A B7A 98.8(2) . . ? B8'A Co3A B7A 127.0(3) . . ? B8A Co3A B7A 50.2(3) . . ? C2'A Co3A C1A 102.9(2) . . ? B7'A Co3A C1A 98.2(2) . . ? B4'A Co3A C1A 174.8(2) . . ? C2A Co3A C1A 45.05(19) . . ? B4A Co3A C1A 48.4(2) . . ? C1'A Co3A C1A 134.3(2) . . ? B8'A Co3A C1A 131.4(3) . . ? B8A Co3A C1A 84.2(2) . . ? B7A Co3A C1A 82.0(2) . . ? C13A C1A C2A 119.0(4) . . ? C13A C1A B5A 117.3(4) . . ? C2A C1A B5A 110.3(4) . . ? C13A C1A B6A 111.1(5) . . ? C2A C1A B6A 61.5(3) . . ? B5A C1A B6A 62.3(4) . . ? C13A C1A B4A 125.3(5) . . ? C2A C1A B4A 109.3(4) . . ? B5A C1A B4A 62.3(4) . . ? B6A C1A B4A 113.5(4) . . ? C13A C1A Co3A 112.6(4) . . ? C2A C1A Co3A 66.3(3) . . ? B5A C1A Co3A 121.6(4) . . ? B6A C1A Co3A 123.1(3) . . ? B4A C1A Co3A 64.9(3) . . ? C1A C2A B11A 112.2(4) . . ? C1A C2A B6A 61.9(4) . . ? B11A C2A B6A 62.0(4) . . ? C1A C2A B7A 113.4(4) . . ? B11A C2A B7A 62.7(4) . . ? B6A C2A B7A 114.5(4) . . ? C1A C2A Co3A 68.7(3) . . ? B11A C2A Co3A 123.9(3) . . ? B6A C2A Co3A 125.7(4) . . ? B7A C2A Co3A 66.4(3) . . ? C1A C2A H2A 120.1 . . ? B11A C2A H2A 117.0 . . ? B6A C2A H2A 116.3 . . ? B7A C2A H2A 118.3 . . ? Co3A C2A H2A 106.7 . . ? C1'A C2'A B21' 112.4(5) . . ? C1'A C2'A B7'A 112.9(4) . . ? B21' C2'A B7'A 63.5(4) . . ? C1'A C2'A B6'A 63.3(4) . . ? B21' C2'A B6'A 60.9(4) . . ? B7'A C2'A B6'A 114.3(5) . . ? C1'A C2'A Co3A 68.7(3) . . ? B21' C2'A Co3A 124.1(4) . . ? B7'A C2'A Co3A 65.6(3) . . ? B6'A C2'A Co3A 126.9(4) . . ? C1'A C2'A H2'A 119.5 . . ? B21' C2'A H2'A 116.7 . . ? B7'A C2'A H2'A 119.3 . . ? B6'A C2'A H2'A 115.1 . . ? Co3A C2'A H2'A 107.2 . . ? C2A B11A B6A 59.5(4) . . ? C2A B11A B12A 104.3(4) . . ? B6A B11A B12A 108.6(4) . . ? C2A B11A B7A 59.3(3) . . ? B6A B11A B7A 109.6(5) . . ? B12A B11A B7A 59.2(4) . . ? C2A B11A B10A 105.0(4) . . ? B6A B11A B10A 60.0(4) . . ? B12A B11A B10A 60.5(4) . . ? B7A B11A B10A 108.4(4) . . ? C2A B11A H11A 124.6 . . ? B6A B11A H11A 120.4 . . ? B12A B11A H11A 122.7 . . ? B7A B11A H11A 121.2 . . ? B10A B11A H11A 122.0 . . ? C2'A B6'A B20' 104.0(5) . . ? C2'A B6'A B21' 58.7(3) . . ? B20' B6'A B21' 60.5(4) . . ? C2'A B6'A B5'A 101.9(4) . . ? B20' B6'A B5'A 60.1(4) . . ? B21' B6'A B5'A 107.7(5) . . ? C2'A B6'A C1'A 55.1(3) . . ? B20' B6'A C1'A 104.8(5) . . ? B21' B6'A C1'A 103.9(4) . . ? B5'A B6'A C1'A 58.4(4) . . ? C2'A B6'A H6'A 125.4 . . ? B20' B6'A H6'A 123.3 . . ? B21' B6'A H6'A 121.7 . . ? B5'A B6'A H6'A 123.6 . . ? C1'A B6'A H6'A 124.8 . . ? B20' B22' B21' 59.5(4) . . ? B20' B22' B9'A 59.9(4) . . ? B21' B22' B9'A 106.7(5) . . ? B20' B22' B8'A 108.1(5) . . ? B21' B22' B8'A 107.4(5) . . ? B9'A B22' B8'A 59.7(4) . . ? B20' B22' B7'A 107.7(5) . . ? B21' B22' B7'A 60.5(4) . . ? B9'A B22' B7'A 106.0(5) . . ? B8'A B22' B7'A 58.6(4) . . ? B20' B22' H22' 122.1 . . ? B21' B22' H22' 122.0 . . ? B9'A B22' H22' 123.2 . . ? B8'A B22' H22' 121.8 . . ? B7'A B22' H22' 121.9 . . ? B5A B9A B4A 60.6(4) . . ? B5A B9A B10A 60.3(4) . . ? B4A B9A B10A 108.9(5) . . ? B5A B9A B12A 107.5(4) . . ? B4A B9A B12A 107.3(4) . . ? B10A B9A B12A 59.9(4) . . ? B5A B9A B8A 109.8(4) . . ? B4A B9A B8A 61.1(3) . . ? B10A B9A B8A 108.8(4) . . ? B12A B9A B8A 59.1(4) . . ? B5A B9A H9A 121.5 . . ? B4A B9A H9A 121.1 . . ? B10A B9A H9A 121.6 . . ? B12A B9A H9A 122.7 . . ? B8A B9A H9A 120.3 . . ? C2A B7A B12A 104.2(5) . . ? C2A B7A B11A 58.0(3) . . ? B12A B7A B11A 60.3(4) . . ? C2A B7A B8A 105.5(4) . . ? B12A B7A B8A 60.4(4) . . ? B11A B7A B8A 109.1(4) . . ? C2A B7A Co3A 65.6(3) . . ? B12A B7A Co3A 118.4(4) . . ? B11A B7A Co3A 118.9(4) . . ? B8A B7A Co3A 64.9(3) . . ? C2A B7A H7A 125.7 . . ? B12A B7A H7A 121.1 . . ? B11A B7A H7A 120.4 . . ? B8A B7A H7A 121.6 . . ? Co3A B7A H7A 110.1 . . ? C23' C1'A C2'A 121.5(5) . . ? C23' C1'A B4'A 123.7(5) . . ? C2'A C1'A B4'A 108.5(5) . . ? C23' C1'A B5'A 116.4(5) . . ? C2'A C1'A B5'A 108.8(5) . . ? B4'A C1'A B5'A 63.3(4) . . ? C23' C1'A B6'A 112.6(5) . . ? C2'A C1'A B6'A 61.6(4) . . ? B4'A C1'A B6'A 112.8(5) . . ? B5'A C1'A B6'A 60.5(4) . . ? C23' C1'A Co3A 113.2(4) . . ? C2'A C1'A Co3A 65.2(3) . . ? B4'A C1'A Co3A 65.2(3) . . ? B5'A C1'A Co3A 122.0(4) . . ? B6'A C1'A Co3A 122.3(4) . . ? C14A C13A C1A 117.5(7) . . ? C14A C13A 13AA 99.6 . . ? C1A C13A 13AA 108.0 . . ? C14A C13A 13AB 116.9 . . ? C1A C13A 13AB 106.9 . . ? 13AA C13A 13AB 106.9 . . ? C1'A B4'A B9'A 105.3(5) . . ? C1'A B4'A B8'A 107.4(5) . . ? B9'A B4'A B8'A 60.0(4) . . ? C1'A B4'A B5'A 58.7(4) . . ? B9'A B4'A B5'A 58.7(4) . . ? B8'A B4'A B5'A 107.3(5) . . ? C1'A B4'A Co3A 66.6(3) . . ? B9'A B4'A Co3A 118.7(4) . . ? B8'A B4'A Co3A 65.4(3) . . ? B5'A B4'A Co3A 119.2(4) . . ? C1'A B4'A H4'A 123.8 . . ? B9'A B4'A H4'A 120.4 . . ? B8'A B4'A H4'A 122.6 . . ? B5'A B4'A H4'A 119.9 . . ? Co3A B4'A H4'A 111.0 . . ? C1A B5A B9A 106.2(5) . . ? C1A B5A B6A 59.1(4) . . ? B9A B5A B6A 108.3(4) . . ? C1A B5A B10A 105.6(4) . . ? B9A B5A B10A 60.4(4) . . ? B6A B5A B10A 59.7(4) . . ? C1A B5A B4A 59.7(3) . . ? B9A B5A B4A 60.1(4) . . ? B6A B5A B4A 108.8(5) . . ? B10A B5A B4A 108.6(5) . . ? C1A B5A H5A 124.7 . . ? B9A B5A H5A 121.1 . . ? B6A B5A H5A 121.6 . . ? B10A B5A H5A 121.2 . . ? B4A B5A H5A 121.4 . . ? B7A B12A B11A 60.5(4) . . ? B7A B12A B8A 61.2(4) . . ? B11A B12A B8A 109.9(4) . . ? B7A B12A B10A 109.1(5) . . ? B11A B12A B10A 60.1(4) . . ? B8A B12A B10A 109.8(5) . . ? B7A B12A B9A 108.5(4) . . ? B11A B12A B9A 107.3(5) . . ? B8A B12A B9A 60.7(4) . . ? B10A B12A B9A 59.5(4) . . ? B7A B12A H12A 121.3 . . ? B11A B12A H12A 121.2 . . ? B8A B12A H12A 120.5 . . ? B10A B12A H12A 120.6 . . ? B9A B12A H12A 122.3 . . ? B6A B10A B5A 60.0(4) . . ? B6A B10A B11A 59.2(4) . . ? B5A B10A B11A 106.8(4) . . ? B6A B10A B9A 107.7(5) . . ? B5A B10A B9A 59.3(4) . . ? B11A B10A B9A 107.7(5) . . ? B6A B10A B12A 107.1(5) . . ? B5A B10A B12A 107.3(5) . . ? B11A B10A B12A 59.4(4) . . ? B9A B10A B12A 60.6(4) . . ? B6A B10A H10A 121.8 . . ? B5A B10A H10A 122.1 . . ? B11A B10A H10A 122.6 . . ? B9A B10A H10A 121.8 . . ? B12A B10A H10A 122.4 . . ? C1A B4A B9A 104.1(4) . . ? C1A B4A B5A 57.9(4) . . ? B9A B4A B5A 59.3(4) . . ? C1A B4A B8A 106.1(4) . . ? B9A B4A B8A 60.4(4) . . ? B5A B4A B8A 108.1(4) . . ? C1A B4A Co3A 66.7(3) . . ? B9A B4A Co3A 118.3(4) . . ? B5A B4A Co3A 119.2(4) . . ? B8A B4A Co3A 64.6(3) . . ? C1A B4A H4A 124.7 . . ? B9A B4A H4A 121.3 . . ? B5A B4A H4A 120.3 . . ? B8A B4A H4A 122.4 . . ? Co3A B4A H4A 110.3 . . ? C2'A B21' B6'A 60.4(4) . . ? C2'A B21' B20' 104.6(4) . . ? B6'A B21' B20' 59.6(4) . . ? C2'A B21' B22' 104.9(4) . . ? B6'A B21' B22' 108.8(5) . . ? B20' B21' B22' 59.7(4) . . ? C2'A B21' B7'A 58.5(3) . . ? B6'A B21' B7'A 109.8(4) . . ? B20' B21' B7'A 107.6(5) . . ? B22' B21' B7'A 60.2(4) . . ? C2'A B21' H21' 124.7 . . ? B6'A B21' H21' 120.2 . . ? B20' B21' H21' 122.9 . . ? B22' B21' H21' 122.1 . . ? B7'A B21' H21' 121.3 . . ? C2'A B7'A B8'A 105.0(5) . . ? C2'A B7'A B22' 103.7(5) . . ? B8'A B7'A B22' 60.5(4) . . ? C2'A B7'A B21' 58.0(4) . . ? B8'A B7'A B21' 107.9(5) . . ? B22' B7'A B21' 59.3(4) . . ? C2'A B7'A Co3A 64.8(3) . . ? B8'A B7'A Co3A 66.2(3) . . ? B22' B7'A Co3A 119.7(4) . . ? B21' B7'A Co3A 118.4(4) . . ? C2'A B7'A H7'A 126.4 . . ? B8'A B7'A H7'A 122.0 . . ? B22' B7'A H7'A 120.5 . . ? B21' B7'A H7'A 120.6 . . ? Co3A B7'A H7'A 110.2 . . ? B12A B8A B7A 58.5(4) . . ? B12A B8A B9A 60.2(4) . . ? B7A B8A B9A 106.0(4) . . ? B12A B8A B4A 106.1(5) . . ? B7A B8A B4A 105.6(4) . . ? B9A B8A B4A 58.5(4) . . ? B12A B8A Co3A 116.8(4) . . ? B7A B8A Co3A 64.9(3) . . ? B9A B8A Co3A 116.3(4) . . ? B4A B8A Co3A 64.2(3) . . ? B12A B8A H8A 120.9 . . ? B7A B8A H8A 123.4 . . ? B9A B8A H8A 121.5 . . ? B4A B8A H8A 124.2 . . ? Co3A B8A H8A 112.1 . . ? B7'A B8'A B9'A 107.9(5) . . ? B7'A B8'A B4'A 106.1(5) . . ? B9'A B8'A B4'A 59.9(4) . . ? B7'A B8'A B22' 60.9(4) . . ? B9'A B8'A B22' 59.9(4) . . ? B4'A B8'A B22' 107.5(5) . . ? B7'A B8'A Co3A 63.8(3) . . ? B9'A B8'A Co3A 117.4(4) . . ? B4'A B8'A Co3A 64.0(3) . . ? B22' B8'A Co3A 118.0(4) . . ? B7'A B8'A H8'A 123.1 . . ? B9'A B8'A H8'A 120.4 . . ? B4'A B8'A H8'A 122.8 . . ? B22' B8'A H8'A 120.5 . . ? Co3A B8'A H8'A 111.8 . . ? C1'A B5'A B20' 106.5(5) . . ? C1'A B5'A B9'A 105.9(5) . . ? B20' B5'A B9'A 60.8(4) . . ? C1'A B5'A B6'A 61.1(4) . . ? B20' B5'A B6'A 59.6(4) . . ? B9'A B5'A B6'A 109.1(5) . . ? C1'A B5'A B4'A 58.0(3) . . ? B20' B5'A B4'A 108.3(5) . . ? B9'A B5'A B4'A 60.2(4) . . ? B6'A B5'A B4'A 109.0(5) . . ? C1'A B5'A H5'A 123.0 . . ? B20' B5'A H5'A 122.4 . . ? B9'A B5'A H5'A 122.0 . . ? B6'A B5'A H5'A 120.3 . . ? B4'A B5'A H5'A 121.5 . . ? C24' C23' C1'A 120.8(6) . . ? C24' C23' 23'A 110.6 . . ? C1'A C23' 23'A 108.4 . . ? C24' C23' 23'B 103.3 . . ? C1'A C23' 23'B 106.0 . . ? 23'A C23' 23'B 106.6 . . ? C2A B6A C1A 56.6(3) . . ? C2A B6A B11A 58.5(4) . . ? C1A B6A B11A 105.1(5) . . ? C2A B6A B10A 104.9(5) . . ? C1A B6A B10A 105.8(5) . . ? B11A B6A B10A 60.8(4) . . ? C2A B6A B5A 103.5(5) . . ? C1A B6A B5A 58.6(3) . . ? B11A B6A B5A 108.3(5) . . ? B10A B6A B5A 60.3(4) . . ? C2A B6A H6A 124.9 . . ? C1A B6A H6A 123.7 . . ? B11A B6A H6A 121.9 . . ? B10A B6A H6A 122.7 . . ? B5A B6A H6A 122.6 . . ? B5'A B9'A B20' 59.6(4) . . ? B5'A B9'A B4'A 61.1(4) . . ? B20' B9'A B4'A 108.1(5) . . ? B5'A B9'A B8'A 109.3(5) . . ? B20' B9'A B8'A 108.1(5) . . ? B4'A B9'A B8'A 60.1(4) . . ? B5'A B9'A B22' 107.6(5) . . ? B20' B9'A B22' 59.4(4) . . ? B4'A B9'A B22' 108.0(5) . . ? B8'A B9'A B22' 60.3(4) . . ? B5'A B9'A H9'A 122.0 . . ? B20' B9'A H9'A 121.6 . . ? B4'A B9'A H9'A 122.3 . . ? B8'A B9'A H9'A 120.9 . . ? B22' B9'A H9'A 121.0 . . ? B6'A B20' B5'A 60.4(4) . . ? B6'A B20' B21' 59.9(4) . . ? B5'A B20' B21' 107.5(5) . . ? B6'A B20' B22' 110.0(5) . . ? B5'A B20' B22' 108.8(5) . . ? B21' B20' B22' 60.9(4) . . ? B6'A B20' B9'A 108.9(5) . . ? B5'A B20' B9'A 59.7(4) . . ? B21' B20' B9'A 108.4(5) . . ? B22' B20' B9'A 60.7(4) . . ? B6'A B20' H20' 120.8 . . ? B5'A B20' H20' 121.9 . . ? B21' B20' H20' 122.1 . . ? B22' B20' H20' 120.4 . . ? B9'A B20' H20' 121.3 . . ? C14A O1A H1A 109.5 . . ? O1'A C24' C23' 107.9(9) . . ? O1'A C24' 24'A 120.5 . . ? C23' C24' 24'A 113.6 . . ? O1'A C24' 24'B 97.8 . . ? C23' C24' 24'B 107.3 . . ? 24'A C24' 24'B 107.9 . . ? O1A C14A C13A 117.7(10) . . ? O1A C14A 14AA 94.9 . . ? C13A C14A 14AA 98.7 . . ? O1A C14A 14AB 117.1 . . ? C13A C14A 14AB 116.1 . . ? 14AA C14A 14AB 106.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N18' H18' O1 0.91 2.61 3.120(14) 116.0 2_465 O1' H1' O1'A 0.82 1.84 2.655(17) 169.6 2_464 O1A H1A O1 0.82 1.98 2.730(14) 151.4 2_575 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.560 0.500 0.020 379.3 103.9 _platon_squeeze_details ; ; _vrf_CHEMW03_2Me3NH_6 ; ALERT_2_A The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 RESPONSE: The disordered Me3NH cations were removed from data using SQUEEZE procedure, but were retained in formula, moiety and other strings causing several alerts ; _vrf_PLAT043_2Me3NH_6 ; ALERT_1_A Check Reported Molecular Weight ................ 531.06 RESPONSE: The disordered Me3NH cations were removed from data using SQUEEZE procedure, but were retained in formula, moiety and other strings causing this alert with MW ; _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.213 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.098 #END data_Cs_5 _database_code_depnum_ccdc_archive 'CCDC 859800' #TrackingRef '- ESI-CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H26 B18 Co Cs O2' _chemical_formula_sum 'C6 H26 B18 Co Cs O2' _chemical_formula_weight 516.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cs Cs -0.3680 2.1192 '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 19.534(8) _cell_length_b 7.441(6) _cell_length_c 15.702(9) _cell_angle_alpha 90.00 _cell_angle_beta 122.39(12) _cell_angle_gamma 90.00 _cell_volume 1927(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 9684 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.172 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 2.752 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.026 0 1 0 0.086 -1 0 0 0.073 1 0 0 0.085 -1 0 1 0.106 1 0 -1 0.207 0 0 -1 0.205 1 0 1 0.101 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.484 _exptl_absorpt_correction_T_max 0.731 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 150(1) _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 Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9038 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 26.37 _reflns_number_total 1952 _reflns_number_gt 1800 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0186P)^2^+2.9572P] 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 1952 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0540 _refine_ls_wR_factor_gt 0.0522 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 Co3 Co 0.0000 -0.05553(5) 0.2500 0.00976(9) Uani 1 2 d S . . Cs1 Cs -0.01434(3) 0.47122(7) 0.49089(5) 0.03001(15) Uani 0.50 1 d P . . B11 B 0.13389(12) 0.0515(3) 0.18795(16) 0.0149(4) Uani 1 1 d . . . H11 H 0.1397 0.1270 0.1319 0.018 Uiso 1 1 d R . . C1 C 0.11460(10) 0.0579(2) 0.34944(13) 0.0121(4) Uani 1 1 d . . . B8 B 0.06838(12) -0.2582(3) 0.23396(15) 0.0137(4) Uani 1 1 d . . . H8 H 0.0361 -0.3873 0.2091 0.016 Uiso 1 1 d R . . C13 C 0.11937(11) 0.1895(3) 0.42795(13) 0.0157(4) Uani 1 1 d . . . H13A H 0.0967 0.1322 0.4630 0.019 Uiso 1 1 d R . . H13B H 0.1760 0.2148 0.4773 0.019 Uiso 1 1 d R . . B5 B 0.20324(12) -0.0551(3) 0.39247(16) 0.0144(4) Uani 1 1 d . . . H5 H 0.2552 -0.0503 0.4709 0.017 Uiso 1 1 d R . . B10 B 0.21672(12) -0.0659(3) 0.28963(16) 0.0155(4) Uani 1 1 d . . . H10 H 0.2781 -0.0710 0.3002 0.019 Uiso 1 1 calc R . . B9 B 0.17586(12) -0.2528(3) 0.31948(15) 0.0145(4) Uani 1 1 d . . . H9 H 0.2101 -0.3787 0.3498 0.017 Uiso 1 1 d R . . B4 B 0.11151(12) -0.1702(3) 0.35970(15) 0.0135(4) Uani 1 1 d . . . H4 H 0.1062 -0.2399 0.4177 0.016 Uiso 1 1 d R . . B7 B 0.04281(12) -0.0663(3) 0.15372(15) 0.0141(4) Uani 1 1 d . . . H7 H -0.0079 -0.0671 0.0744 0.017 Uiso 1 1 d R . . B6 B 0.17855(12) 0.1314(3) 0.31182(15) 0.0148(4) Uani 1 1 d . . . H6 H 0.2132 0.2578 0.3359 0.018 Uiso 1 1 d R . . O1 O 0.07789(9) 0.3542(2) 0.38678(11) 0.0213(3) Uani 1 1 d . . . C2 C 0.07443(10) 0.1152(3) 0.23266(13) 0.0130(4) Uani 1 1 d . . . H2 H 0.0414 0.2431 0.2054 0.016 Uiso 1 1 d R . . B12 B 0.13292(12) -0.1851(3) 0.19174(16) 0.0150(4) Uani 1 1 d . . . H12 H 0.1395 -0.2662 0.1380 0.018 Uiso 1 1 d R . . H199 H 0.104(2) 0.419(5) 0.376(2) 0.048(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co3 0.00968(16) 0.01096(18) 0.00881(16) 0.000 0.00507(13) 0.000 Cs1 0.0434(4) 0.0312(4) 0.0217(2) 0.0111(2) 0.0216(3) 0.0221(2) B11 0.0146(9) 0.0167(11) 0.0161(10) -0.0001(8) 0.0099(8) -0.0009(8) C1 0.0104(8) 0.0125(9) 0.0114(8) 0.0002(7) 0.0045(7) 0.0008(7) B8 0.0143(9) 0.0135(10) 0.0152(9) -0.0009(8) 0.0092(8) 0.0007(8) C13 0.0159(8) 0.0148(10) 0.0147(9) -0.0035(7) 0.0070(7) -0.0002(7) B5 0.0127(9) 0.0147(10) 0.0149(9) 0.0004(8) 0.0067(8) 0.0015(8) B10 0.0140(9) 0.0150(10) 0.0185(10) -0.0008(8) 0.0094(8) 0.0004(8) B9 0.0139(9) 0.0143(11) 0.0149(9) 0.0002(8) 0.0075(8) 0.0017(8) B4 0.0135(9) 0.0139(10) 0.0134(9) 0.0002(8) 0.0073(8) 0.0020(8) B7 0.0131(9) 0.0169(11) 0.0122(9) -0.0001(8) 0.0067(8) -0.0011(8) B6 0.0118(9) 0.0156(11) 0.0156(9) -0.0013(8) 0.0063(8) -0.0015(8) O1 0.0232(7) 0.0133(7) 0.0271(7) -0.0029(6) 0.0133(6) 0.0019(6) C2 0.0116(8) 0.0154(9) 0.0117(8) 0.0006(7) 0.0060(7) -0.0010(7) B12 0.0152(9) 0.0167(11) 0.0160(9) -0.0020(8) 0.0103(8) -0.0013(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Co3 C2 2.0557(18) 2 ? Co3 C2 2.0557(18) . ? Co3 B7 2.085(2) 2 ? Co3 B7 2.085(2) . ? Co3 C1 2.1017(17) . ? Co3 C1 2.1017(17) 2 ? Co3 B4 2.102(2) 2 ? Co3 B4 2.102(2) . ? Co3 B8 2.117(2) 2 ? Co3 B8 2.117(2) . ? Cs1 Cs1 0.6383(6) 5_566 ? Cs1 O1 3.0779(16) 5_566 ? Cs1 O1 3.1355(17) . ? Cs1 B12 3.608(2) 2_565 ? Cs1 B12 3.611(2) 6_556 ? Cs1 B8 3.617(2) 6_556 ? Cs1 B8 3.693(2) 2_565 ? Cs1 B7 3.716(2) 6_556 ? Cs1 C13 3.867(2) . ? Cs1 C13 3.874(2) 5_566 ? B11 C2 1.715(3) . ? B11 B6 1.755(3) . ? B11 B12 1.762(3) . ? B11 B10 1.779(3) . ? B11 B7 1.788(3) . ? B11 H11 1.1001 . ? C1 C13 1.538(2) . ? C1 C2 1.618(2) . ? C1 B5 1.706(3) . ? C1 B4 1.709(3) . ? C1 B6 1.732(3) . ? B8 B9 1.787(3) . ? B8 B7 1.790(3) . ? B8 B12 1.795(3) . ? B8 B4 1.804(3) . ? B8 Cs1 3.617(2) 6 ? B8 Cs1 3.693(2) 2_545 ? B8 H8 1.1001 . ? C13 O1 1.419(2) . ? C13 Cs1 3.874(2) 5_566 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? B5 B9 1.762(3) . ? B5 B6 1.763(3) . ? B5 B10 1.772(3) . ? B5 B4 1.795(3) . ? B5 H5 1.0999 . ? B10 B6 1.764(3) . ? B10 B12 1.770(3) . ? B10 B9 1.786(3) . ? B10 H10 1.1200 . ? B9 B12 1.783(3) . ? B9 B4 1.791(3) . ? B9 H9 1.0999 . ? B4 H4 1.1000 . ? B7 C2 1.709(3) . ? B7 B12 1.764(3) . ? B7 Cs1 3.716(2) 6 ? B7 H7 1.1000 . ? B6 C2 1.729(3) . ? B6 H6 1.0999 . ? O1 Cs1 3.0779(16) 5_566 ? O1 H199 0.78(4) . ? C2 H2 1.0999 . ? B12 Cs1 3.608(2) 2_545 ? B12 Cs1 3.611(2) 6 ? B12 H12 1.1001 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Co3 C2 103.66(11) 2 . ? C2 Co3 B7 48.76(8) 2 2 ? C2 Co3 B7 134.96(8) . 2 ? C2 Co3 B7 134.96(8) 2 . ? C2 Co3 B7 48.76(8) . . ? B7 Co3 B7 175.61(13) 2 . ? C2 Co3 C1 101.58(7) 2 . ? C2 Co3 C1 45.80(7) . . ? B7 Co3 C1 99.09(7) 2 . ? B7 Co3 C1 82.69(7) . . ? C2 Co3 C1 45.80(7) 2 2 ? C2 Co3 C1 101.58(7) . 2 ? B7 Co3 C1 82.69(7) 2 2 ? B7 Co3 C1 99.09(7) . 2 ? C1 Co3 C1 132.64(10) . 2 ? C2 Co3 B4 82.15(8) 2 2 ? C2 Co3 B4 129.66(7) . 2 ? B7 Co3 B4 86.37(8) 2 2 ? B7 Co3 B4 91.85(8) . 2 ? C1 Co3 B4 174.54(7) . 2 ? C1 Co3 B4 47.97(8) 2 2 ? C2 Co3 B4 129.66(7) 2 . ? C2 Co3 B4 82.15(8) . . ? B7 Co3 B4 91.85(8) 2 . ? B7 Co3 B4 86.37(8) . . ? C1 Co3 B4 47.97(8) . . ? C1 Co3 B4 174.54(7) 2 . ? B4 Co3 B4 132.11(12) 2 . ? C2 Co3 B8 83.60(8) 2 2 ? C2 Co3 B8 172.75(8) . 2 ? B7 Co3 B8 50.41(8) 2 2 ? B7 Co3 B8 125.64(9) . 2 ? C1 Co3 B8 133.35(7) . 2 ? C1 Co3 B8 83.43(7) 2 2 ? B4 Co3 B8 50.62(8) 2 2 ? B4 Co3 B8 93.23(8) . 2 ? C2 Co3 B8 172.75(8) 2 . ? C2 Co3 B8 83.60(8) . . ? B7 Co3 B8 125.64(9) 2 . ? B7 Co3 B8 50.41(8) . . ? C1 Co3 B8 83.43(7) . . ? C1 Co3 B8 133.35(7) 2 . ? B4 Co3 B8 93.23(8) 2 . ? B4 Co3 B8 50.62(8) . . ? B8 Co3 B8 89.15(12) 2 . ? Cs1 Cs1 O1 89.28(12) 5_566 5_566 ? Cs1 Cs1 O1 78.98(12) 5_566 . ? O1 Cs1 O1 168.255(13) 5_566 . ? Cs1 Cs1 B12 85.19(12) 5_566 2_565 ? O1 Cs1 B12 83.97(5) 5_566 2_565 ? O1 Cs1 B12 94.94(5) . 2_565 ? Cs1 Cs1 B12 84.66(12) 5_566 6_556 ? O1 Cs1 B12 95.90(5) 5_566 6_556 ? O1 Cs1 B12 83.12(5) . 6_556 ? B12 Cs1 B12 169.854(12) 2_565 6_556 ? Cs1 Cs1 B8 91.85(12) 5_566 6_556 ? O1 Cs1 B8 68.16(5) 5_566 6_556 ? O1 Cs1 B8 111.83(5) . 6_556 ? B12 Cs1 B8 152.02(5) 2_565 6_556 ? B12 Cs1 B8 28.75(5) 6_556 6_556 ? Cs1 Cs1 B8 78.20(12) 5_566 2_565 ? O1 Cs1 B8 111.23(5) 5_566 2_565 ? O1 Cs1 B8 66.60(4) . 2_565 ? B12 Cs1 B8 28.43(5) 2_565 2_565 ? B12 Cs1 B8 147.41(5) 6_556 2_565 ? B8 Cs1 B8 170.053(11) 6_556 2_565 ? Cs1 Cs1 B7 111.58(12) 5_566 6_556 ? O1 Cs1 B7 89.19(5) 5_566 6_556 ? O1 Cs1 B7 95.09(5) . 6_556 ? B12 Cs1 B7 161.85(5) 2_565 6_556 ? B12 Cs1 B7 27.81(5) 6_556 6_556 ? B8 Cs1 B7 28.21(5) 6_556 6_556 ? B8 Cs1 B7 157.91(5) 2_565 6_556 ? Cs1 Cs1 C13 85.85(12) 5_566 . ? O1 Cs1 C13 160.32(4) 5_566 . ? O1 Cs1 C13 20.11(4) . . ? B12 Cs1 C13 114.52(5) 2_565 . ? B12 Cs1 C13 64.69(4) 6_556 . ? B8 Cs1 C13 92.93(5) 6_556 . ? B8 Cs1 C13 86.42(5) 2_565 . ? B7 Cs1 C13 75.00(4) 6_556 . ? Cs1 Cs1 C13 84.69(12) 5_566 5_566 ? O1 Cs1 C13 19.59(4) 5_566 5_566 ? O1 Cs1 C13 154.95(4) . 5_566 ? B12 Cs1 C13 64.65(4) 2_565 5_566 ? B12 Cs1 C13 114.30(5) 6_556 5_566 ? B8 Cs1 C13 87.38(5) 6_556 5_566 ? B8 Cs1 C13 91.64(5) 2_565 5_566 ? B7 Cs1 C13 108.60(5) 6_556 5_566 ? C13 Cs1 C13 170.541(10) . 5_566 ? C2 B11 B6 59.75(11) . . ? C2 B11 B12 103.90(14) . . ? B6 B11 B12 108.00(15) . . ? C2 B11 B10 104.97(14) . . ? B6 B11 B10 59.90(12) . . ? B12 B11 B10 59.98(12) . . ? C2 B11 B7 58.36(11) . . ? B6 B11 B7 108.85(14) . . ? B12 B11 B7 59.57(12) . . ? B10 B11 B7 108.01(15) . . ? C2 B11 H11 124.7 . . ? B6 B11 H11 120.7 . . ? B12 B11 H11 123.0 . . ? B10 B11 H11 122.3 . . ? B7 B11 H11 121.5 . . ? C13 C1 C2 121.66(15) . . ? C13 C1 B5 112.57(14) . . ? C2 C1 B5 110.61(14) . . ? C13 C1 B4 123.17(15) . . ? C2 C1 B4 110.38(14) . . ? B5 C1 B4 63.41(12) . . ? C13 C1 B6 109.09(15) . . ? C2 C1 B6 62.02(11) . . ? B5 C1 B6 61.72(12) . . ? B4 C1 B6 114.47(14) . . ? C13 C1 Co3 115.75(12) . . ? C2 C1 Co3 65.60(9) . . ? B5 C1 Co3 123.20(12) . . ? B4 C1 Co3 66.04(9) . . ? B6 C1 Co3 123.32(11) . . ? B9 B8 B7 106.48(14) . . ? B9 B8 B12 59.71(11) . . ? B7 B8 B12 58.95(12) . . ? B9 B8 B4 59.83(11) . . ? B7 B8 B4 105.75(14) . . ? B12 B8 B4 106.59(14) . . ? B9 B8 Co3 117.18(12) . . ? B7 B8 Co3 63.85(9) . . ? B12 B8 Co3 116.15(13) . . ? B4 B8 Co3 64.27(9) . . ? B9 B8 Cs1 118.93(11) . 6 ? B7 B8 Cs1 78.95(9) . 6 ? B12 B8 Cs1 75.42(9) . 6 ? B4 B8 Cs1 175.29(12) . 6 ? Co3 B8 Cs1 118.94(7) . 6 ? B9 B8 Cs1 110.47(11) . 2_545 ? B7 B8 Cs1 86.16(10) . 2_545 ? B12 B8 Cs1 73.13(9) . 2_545 ? B4 B8 Cs1 166.13(12) . 2_545 ? Co3 B8 Cs1 128.79(8) . 2_545 ? Cs1 B8 Cs1 9.947(11) 6 2_545 ? B9 B8 H8 120.4 . . ? B7 B8 H8 123.8 . . ? B12 B8 H8 121.2 . . ? B4 B8 H8 123.2 . . ? Co3 B8 H8 112.7 . . ? Cs1 B8 H8 52.9 6 . ? Cs1 B8 H8 50.9 2_545 . ? O1 C13 C1 114.21(15) . . ? O1 C13 Cs1 49.44(9) . . ? C1 C13 Cs1 142.27(11) . . ? O1 C13 Cs1 46.66(9) . 5_566 ? C1 C13 Cs1 149.71(11) . 5_566 ? Cs1 C13 Cs1 9.459(10) . 5_566 ? O1 C13 H13A 108.4 . . ? C1 C13 H13A 108.9 . . ? Cs1 C13 H13A 61.2 . . ? Cs1 C13 H13A 67.5 5_566 . ? O1 C13 H13B 109.0 . . ? C1 C13 H13B 108.5 . . ? Cs1 C13 H13B 109.1 . . ? Cs1 C13 H13B 100.9 5_566 . ? H13A C13 H13B 107.6 . . ? C1 B5 B9 105.30(14) . . ? C1 B5 B6 59.88(11) . . ? B9 B5 B6 108.60(14) . . ? C1 B5 B10 106.04(14) . . ? B9 B5 B10 60.72(12) . . ? B6 B5 B10 59.88(12) . . ? C1 B5 B4 58.39(11) . . ? B9 B5 B4 60.45(12) . . ? B6 B5 B4 108.83(14) . . ? B10 B5 B4 109.27(14) . . ? C1 B5 H5 124.0 . . ? B9 B5 H5 122.2 . . ? B6 B5 H5 120.8 . . ? B10 B5 H5 121.6 . . ? B4 B5 H5 121.2 . . ? B6 B10 B12 107.24(14) . . ? B6 B10 B5 59.82(12) . . ? B12 B10 B5 107.12(15) . . ? B6 B10 B11 59.38(12) . . ? B12 B10 B11 59.54(12) . . ? B5 B10 B11 106.74(15) . . ? B6 B10 B9 107.49(15) . . ? B12 B10 B9 60.17(12) . . ? B5 B10 B9 59.38(12) . . ? B11 B10 B9 107.37(14) . . ? B6 B10 H10 122.1 . . ? B12 B10 H10 122.1 . . ? B5 B10 H10 122.5 . . ? B11 B10 H10 122.5 . . ? B9 B10 H10 121.9 . . ? B5 B9 B12 106.96(15) . . ? B5 B9 B10 59.90(12) . . ? B12 B9 B10 59.46(12) . . ? B5 B9 B8 109.43(14) . . ? B12 B9 B8 60.36(11) . . ? B10 B9 B8 109.31(14) . . ? B5 B9 B4 60.67(12) . . ? B12 B9 B4 107.67(14) . . ? B10 B9 B4 108.79(15) . . ? B8 B9 B4 60.56(11) . . ? B5 B9 H9 121.8 . . ? B12 B9 H9 122.5 . . ? B10 B9 H9 121.5 . . ? B8 B9 H9 120.2 . . ? B4 B9 H9 121.2 . . ? C1 B4 B9 103.93(14) . . ? C1 B4 B5 58.20(11) . . ? B9 B4 B5 58.89(11) . . ? C1 B4 B8 106.07(14) . . ? B9 B4 B8 59.61(11) . . ? B5 B4 B8 107.24(14) . . ? C1 B4 Co3 65.99(9) . . ? B9 B4 Co3 117.73(12) . . ? B5 B4 Co3 118.59(13) . . ? B8 B4 Co3 65.11(9) . . ? C1 B4 H4 124.7 . . ? B9 B4 H4 121.7 . . ? B5 B4 H4 120.6 . . ? B8 B4 H4 122.6 . . ? Co3 B4 H4 110.8 . . ? C2 B7 B12 104.07(14) . . ? C2 B7 B11 58.66(11) . . ? B12 B7 B11 59.47(12) . . ? C2 B7 B8 105.29(14) . . ? B12 B7 B8 60.66(12) . . ? B11 B7 B8 108.78(14) . . ? C2 B7 Co3 64.74(9) . . ? B12 B7 Co3 119.27(13) . . ? B11 B7 Co3 118.96(13) . . ? B8 B7 Co3 65.74(9) . . ? C2 B7 Cs1 176.80(12) . 6 ? B12 B7 Cs1 72.78(10) . 6 ? B11 B7 Cs1 119.22(11) . 6 ? B8 B7 Cs1 72.84(9) . 6 ? Co3 B7 Cs1 116.15(8) . 6 ? C2 B7 H7 125.6 . . ? B12 B7 H7 120.7 . . ? B11 B7 H7 119.4 . . ? B8 B7 H7 122.3 . . ? Co3 B7 H7 110.7 . . ? Cs1 B7 H7 57.3 6 . ? C2 B6 C1 55.76(10) . . ? C2 B6 B11 58.96(11) . . ? C1 B6 B11 104.46(14) . . ? C2 B6 B5 103.02(14) . . ? C1 B6 B5 58.40(11) . . ? B11 B6 B5 108.16(15) . . ? C2 B6 B10 105.00(14) . . ? C1 B6 B10 105.23(15) . . ? B11 B6 B10 60.72(12) . . ? B5 B6 B10 60.30(12) . . ? C2 B6 H6 125.2 . . ? C1 B6 H6 125.1 . . ? B11 B6 H6 121.3 . . ? B5 B6 H6 123.0 . . ? B10 B6 H6 122.2 . . ? C13 O1 Cs1 113.75(11) . 5_566 ? C13 O1 Cs1 110.45(11) . . ? Cs1 O1 Cs1 11.745(13) 5_566 . ? C13 O1 H199 111(3) . . ? Cs1 O1 H199 113(3) 5_566 . ? Cs1 O1 H199 124(3) . . ? C1 C2 B7 112.41(15) . . ? C1 C2 B11 111.56(14) . . ? B7 C2 B11 62.98(12) . . ? C1 C2 B6 62.22(11) . . ? B7 C2 B6 113.93(14) . . ? B11 C2 B6 61.29(11) . . ? C1 C2 Co3 68.60(9) . . ? B7 C2 Co3 66.50(9) . . ? B11 C2 Co3 124.45(13) . . ? B6 C2 Co3 126.24(12) . . ? C1 C2 H2 119.8 . . ? B7 C2 H2 119.5 . . ? B11 C2 H2 117.7 . . ? B6 C2 H2 116.0 . . ? Co3 C2 H2 106.1 . . ? B11 B12 B7 60.96(12) . . ? B11 B12 B10 60.48(12) . . ? B7 B12 B10 109.52(15) . . ? B11 B12 B9 108.27(15) . . ? B7 B12 B9 107.78(14) . . ? B10 B12 B9 60.37(12) . . ? B11 B12 B8 109.75(15) . . ? B7 B12 B8 60.38(12) . . ? B10 B12 B8 109.70(14) . . ? B9 B12 B8 59.93(11) . . ? B11 B12 Cs1 134.06(12) . 2_545 ? B7 B12 Cs1 89.25(10) . 2_545 ? B10 B12 Cs1 161.22(12) . 2_545 ? B9 B12 Cs1 114.12(12) . 2_545 ? B8 B12 Cs1 78.44(10) . 2_545 ? B11 B12 Cs1 125.29(11) . 6 ? B7 B12 Cs1 79.41(10) . 6 ? B10 B12 Cs1 170.92(12) . 6 ? B9 B12 Cs1 119.38(12) . 6 ? B8 B12 Cs1 75.83(9) . 6 ? Cs1 B12 Cs1 10.146(12) 2_545 6 ? B11 B12 H12 121.0 . . ? B7 B12 H12 121.4 . . ? B10 B12 H12 120.5 . . ? B9 B12 H12 122.0 . . ? B8 B12 H12 120.7 . . ? Cs1 B12 H12 44.8 2_545 . ? Cs1 B12 H12 51.1 6 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.315 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.063 #END#