Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Bohumir Gruner' _publ_contact_author_email GRUNER@IIC.CAS.CZ _publ_section_title ; Boron substituted 8-nitrilium and 8-ammonium derivatives, versatile cobalt bis(1,2-dicarbollide) building blocks for synthetic purposes. ; loop_ _publ_author_name 'Bohumir Gruner' 'Ivana Cisarova' 'Magdalena Kvicalova' 'J Plesek' 'Vaclav Sicha' data_2 _database_code_depnum_ccdc_archive 'CCDC 698618' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H24 B18 Co N' _chemical_formula_sum 'C6 H24 B18 Co N' _chemical_formula_weight 363.77 _chemical_compound_source 'synthesized by the authors' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 22.05980(10) _cell_length_b 7.0999(2) _cell_length_c 11.5587(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1810.35(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2415 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.935 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '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 25157 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3943 _reflns_number_gt 3795 _reflns_threshold_expression I>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 ? _computing_publication_material ? _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. The crystal was refined as racemic twin, twin ration 0.54:0.46. ; _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^)+(0.0371P)^2^+0.5901P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(13) _refine_ls_number_reflns 3943 _refine_ls_number_parameters 273 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co3 Co 0.422893(8) 0.24021(2) 0.91204(4) 0.01233(7) Uani 1 1 d . . . C1 C 0.36433(8) 0.3067(3) 1.04327(15) 0.0173(3) Uani 1 1 d . . . H1 H 0.3842(9) 0.381(3) 1.0979(19) 0.022(5) Uiso 1 1 d . . . C2 C 0.38405(8) 0.0868(2) 1.04180(15) 0.0179(3) Uani 1 1 d . . . H2 H 0.4144(9) 0.048(3) 1.093(2) 0.019(5) Uiso 1 1 d . . . B4 B 0.33920(7) 0.3831(2) 0.9126(2) 0.0157(3) Uani 1 1 d . . . H4 H 0.3429(9) 0.520(3) 0.8893(19) 0.024(6) Uiso 1 1 d . . . B5 B 0.28851(9) 0.3335(3) 1.02955(18) 0.0207(4) Uani 1 1 d . . . H5 H 0.2617 0.4466 1.0698 0.025 Uiso 1 1 calc R . . B6 B 0.31850(9) 0.1484(3) 1.11407(18) 0.0211(4) Uani 1 1 d . . . H6 H 0.3117 0.1408 1.2082 0.025 Uiso 1 1 calc R . . B7 B 0.37432(8) -0.0131(2) 0.9082(2) 0.0177(3) Uani 1 1 d . . . H7 H 0.3981(10) -0.132(3) 0.8766(19) 0.025(6) Uiso 1 1 d . . . B8 B 0.34197(9) 0.1749(3) 0.82487(17) 0.0163(4) Uani 1 1 d . . . B9 B 0.27205(9) 0.2454(3) 0.88947(18) 0.0197(5) Uani 1 1 d . . . H9 H 0.2340 0.2997 0.8377 0.024 Uiso 1 1 calc R . . B10 B 0.25982(9) 0.1005(3) 1.01361(17) 0.0220(4) Uani 1 1 d . . . H10 H 0.2139 0.0606 1.0416 0.026 Uiso 1 1 calc R . . B11 B 0.32293(9) -0.0555(3) 1.02635(19) 0.0220(4) Uani 1 1 d . . . H11 H 0.3187 -0.1968 1.0645 0.026 Uiso 1 1 calc R . . B12 B 0.29371(9) 0.0014(3) 0.88742(16) 0.0212(4) Uani 1 1 d . . . H12 H 0.2696 -0.1031 0.8343 0.025 Uiso 1 1 calc R . . C1' C 0.50113(8) 0.3165(2) 0.99333(15) 0.0163(3) Uani 1 1 d . . . H1' H 0.4933(9) 0.321(3) 1.067(2) 0.013(5) Uiso 1 1 d . . . C2' C 0.47404(6) 0.47855(19) 0.90874(18) 0.0156(3) Uani 1 1 d . . . H2' H 0.4511(8) 0.578(3) 0.9436(15) 0.008(4) Uiso 1 1 d . . . B4' B 0.50714(8) 0.1044(2) 0.92436(18) 0.0163(3) Uani 1 1 d . . . H4' H 0.5058(9) -0.025(3) 0.9749(19) 0.019(5) Uiso 1 1 d . . . B5' B 0.57209(9) 0.2516(3) 0.9537(2) 0.0190(5) Uani 1 1 d . . . H5' H 0.6081 0.2066 1.0136 0.023 Uiso 1 1 calc R . . B6' B 0.54933(8) 0.4900(3) 0.94656(17) 0.0187(4) Uani 1 1 d . . . H6' H 0.5698 0.5992 1.0016 0.022 Uiso 1 1 calc R . . B7' B 0.45900(8) 0.3938(3) 0.77378(16) 0.0155(3) Uani 1 1 d . . . H7' H 0.4287(9) 0.467(3) 0.721(2) 0.027(6) Uiso 1 1 d . . . B8' B 0.48199(8) 0.1488(3) 0.77825(16) 0.0158(4) Uani 1 1 d . . . H8' H 0.4671(8) 0.042(3) 0.7193(16) 0.010(4) Uiso 1 1 d . . . B9' B 0.56150(9) 0.1489(3) 0.81503(17) 0.0192(4) Uani 1 1 d . . . H9' H 0.5915 0.0364 0.7834 0.023 Uiso 1 1 calc R . . B10' B 0.58792(9) 0.3864(3) 0.82779(18) 0.0208(4) Uani 1 1 d . . . H10' H 0.6343 0.4273 0.8036 0.025 Uiso 1 1 calc R . . B11' B 0.52443(9) 0.5374(3) 0.80468(17) 0.0192(4) Uani 1 1 d . . . H11' H 0.5294 0.6789 0.7670 0.023 Uiso 1 1 calc R . . B12' B 0.53186(9) 0.3264(3) 0.72216(16) 0.0181(4) Uani 1 1 d . . . H12' H 0.5425 0.3302 0.6292 0.022 Uiso 1 1 calc R . . N1 N 0.34117(7) 0.1754(2) 0.69449(14) 0.0189(3) Uani 1 1 d . . . C3 C 0.33764(8) 0.1731(3) 0.59612(16) 0.0188(3) Uani 1 1 d . . . C4 C 0.33273(9) 0.1684(3) 0.47097(16) 0.0240(4) Uani 1 1 d . . . H4A H 0.2994 0.0891 0.4491 0.036 Uiso 1 1 calc R . . H4B H 0.3696 0.1194 0.4386 0.036 Uiso 1 1 calc R . . H4C H 0.3260 0.2936 0.4424 0.036 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 Co3 0.01386(10) 0.01269(10) 0.01043(10) -0.00005(10) -0.00028(10) 0.00057(6) C1 0.0186(8) 0.0189(8) 0.0143(8) -0.0023(7) 0.0020(7) 0.0018(6) C2 0.0207(8) 0.0193(8) 0.0135(7) 0.0032(6) 0.0022(7) 0.0010(6) B4 0.0155(7) 0.0166(7) 0.0149(8) 0.0000(9) -0.0019(9) 0.0026(6) B5 0.0179(9) 0.0252(10) 0.0191(9) -0.0029(8) -0.0008(8) 0.0017(8) B6 0.0208(9) 0.0252(10) 0.0174(10) 0.0018(8) 0.0030(7) 0.0005(8) B7 0.0210(8) 0.0149(7) 0.0174(8) 0.0013(10) 0.0011(9) -0.0021(6) B8 0.0169(9) 0.0160(9) 0.0161(9) -0.0002(7) -0.0011(7) -0.0015(7) B9 0.0142(9) 0.0228(9) 0.0221(15) -0.0014(7) -0.0016(7) 0.0002(6) B10 0.0208(9) 0.0267(10) 0.0184(10) -0.0011(8) 0.0013(7) -0.0012(8) B11 0.0251(10) 0.0197(9) 0.0211(10) 0.0032(8) 0.0042(7) -0.0018(7) B12 0.0213(9) 0.0202(8) 0.0222(11) -0.0021(7) 0.0007(7) -0.0058(7) C1' 0.0189(8) 0.0194(8) 0.0104(7) -0.0008(6) -0.0009(6) 0.0003(6) C2' 0.0181(7) 0.0144(6) 0.0143(6) -0.0009(8) -0.0003(8) -0.0015(5) B4' 0.0174(8) 0.0161(7) 0.0154(9) 0.0001(8) -0.0010(7) 0.0042(6) B5' 0.0169(11) 0.0263(12) 0.0138(9) -0.0008(7) -0.0009(7) 0.0029(7) B6' 0.0184(9) 0.0215(9) 0.0160(9) -0.0021(7) -0.0006(7) -0.0027(7) B7' 0.0187(8) 0.0158(8) 0.0119(8) 0.0012(6) -0.0003(7) -0.0008(7) B8' 0.0199(9) 0.0161(9) 0.0114(9) -0.0003(7) 0.0008(7) 0.0035(6) B9' 0.0213(9) 0.0218(10) 0.0146(9) -0.0016(7) -0.0003(7) 0.0043(7) B10' 0.0199(9) 0.0264(10) 0.0162(9) 0.0006(8) 0.0005(7) -0.0003(8) B11' 0.0216(9) 0.0192(9) 0.0169(9) 0.0010(7) 0.0008(7) -0.0017(7) B12' 0.0191(9) 0.0209(9) 0.0144(9) 0.0011(7) 0.0016(7) 0.0000(7) N1 0.0179(7) 0.0198(8) 0.0189(8) -0.0016(6) -0.0025(6) -0.0016(6) C3 0.0170(7) 0.0199(8) 0.0194(9) -0.0021(7) -0.0012(6) -0.0019(6) C4 0.0299(10) 0.0276(10) 0.0146(9) -0.0013(7) -0.0013(7) -0.0028(7) _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' 2.0342(14) . ? Co3 C1' 2.0384(18) . ? Co3 C2 2.0421(17) . ? Co3 C1 2.0476(18) . ? Co3 B7' 2.0922(19) . ? Co3 B7 2.0941(16) . ? Co3 B4' 2.0987(17) . ? Co3 B8 2.1016(19) . ? Co3 B4 2.1066(16) . ? Co3 B8' 2.1240(18) . ? C1 C2 1.621(2) . ? C1 B5 1.691(3) . ? C1 B4 1.698(3) . ? C1 B6 1.719(3) . ? C1 H1 0.93(2) . ? C2 B11 1.694(3) . ? C2 B7 1.713(3) . ? C2 B6 1.726(3) . ? C2 H2 0.93(2) . ? B4 B5 1.789(3) . ? B4 B8 1.793(3) . ? B4 B9 1.795(3) . ? B4 H4 1.01(2) . ? B5 B6 1.767(3) . ? B5 B9 1.773(3) . ? B5 B10 1.781(3) . ? B5 H5 1.1000 . ? B6 B11 1.770(3) . ? B6 B10 1.772(3) . ? B6 H6 1.1000 . ? B7 B8 1.794(3) . ? B7 B12 1.797(3) . ? B7 B11 1.800(3) . ? B7 H7 1.06(2) . ? B8 N1 1.507(2) . ? B8 B12 1.782(3) . ? B8 B9 1.785(3) . ? B9 B10 1.786(3) . ? B9 B12 1.798(3) . ? B9 H9 1.1000 . ? B10 B12 1.784(3) . ? B10 B11 1.785(3) . ? B10 H10 1.1000 . ? B11 B12 1.777(3) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1' C2' 1.624(2) . ? C1' B5' 1.695(3) . ? C1' B4' 1.710(2) . ? C1' B6' 1.714(3) . ? C1' H1' 0.87(2) . ? C2' B11' 1.690(2) . ? C2' B7' 1.705(3) . ? C2' B6' 1.719(2) . ? C2' H2' 0.960(18) . ? B4' B9' 1.771(3) . ? B4' B8' 1.805(3) . ? B4' B5' 1.806(3) . ? B4' H4' 1.09(2) . ? B5' B6' 1.767(3) . ? B5' B9' 1.777(3) . ? B5' B10' 1.777(3) . ? B5' H5' 1.1000 . ? B6' B11' 1.762(3) . ? B6' B10' 1.775(3) . ? B6' H6' 1.1000 . ? B7' B12' 1.780(3) . ? B7' B11' 1.803(3) . ? B7' B8' 1.812(3) . ? B7' H7' 1.05(2) . ? B8' B12' 1.794(3) . ? B8' B9' 1.805(3) . ? B8' H8' 1.069(19) . ? B9' B12' 1.780(3) . ? B9' B10' 1.790(3) . ? B9' H9' 1.1000 . ? B10' B11' 1.784(3) . ? B10' B12' 1.789(3) . ? B10' H10' 1.1000 . ? B11' B12' 1.784(3) . ? B11' H11' 1.1000 . ? B12' H12' 1.1000 . ? N1 C3 1.140(2) . ? C3 C4 1.451(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? 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' 46.99(7) . . ? C2' Co3 C2 133.64(8) . . ? C1' Co3 C2 99.12(7) . . ? C2' Co3 C1 99.90(7) . . ? C1' Co3 C1 97.55(7) . . ? C2 Co3 C1 46.70(7) . . ? C2' Co3 B7' 48.77(8) . . ? C1' Co3 B7' 83.75(7) . . ? C2 Co3 B7' 177.12(8) . . ? C1 Co3 B7' 133.30(7) . . ? C2' Co3 B7 176.29(8) . . ? C1' Co3 B7 132.18(8) . . ? C2 Co3 B7 48.92(8) . . ? C1 Co3 B7 83.74(8) . . ? B7' Co3 B7 128.77(9) . . ? C2' Co3 B4' 83.83(6) . . ? C1' Co3 B4' 48.79(7) . . ? C2 Co3 B4' 94.39(7) . . ? C1 Co3 B4' 127.91(8) . . ? B7' Co3 B4' 87.38(7) . . ? B7 Co3 B4' 93.43(7) . . ? C2' Co3 B8 130.21(7) . . ? C1' Co3 B8 177.19(7) . . ? C2 Co3 B8 83.00(7) . . ? C1 Co3 B8 82.53(8) . . ? B7' Co3 B8 94.14(8) . . ? B7 Co3 B8 50.64(8) . . ? B4' Co3 B8 133.11(8) . . ? C2' Co3 B4 94.91(6) . . ? C1' Co3 B4 127.77(8) . . ? C2 Co3 B4 83.50(8) . . ? C1 Co3 B4 48.22(8) . . ? B7' Co3 B4 94.88(8) . . ? B7 Co3 B4 88.01(6) . . ? B4' Co3 B4 175.71(10) . . ? B8 Co3 B4 50.45(8) . . ? C2' Co3 B8' 84.26(7) . . ? C1' Co3 B8' 84.10(7) . . ? C2 Co3 B8' 129.00(7) . . ? C1 Co3 B8' 175.54(7) . . ? B7' Co3 B8' 50.91(7) . . ? B7 Co3 B8' 92.07(8) . . ? B4' Co3 B8' 50.62(8) . . ? B8 Co3 B8' 96.02(8) . . ? B4 Co3 B8' 133.41(9) . . ? C2 C1 B5 111.90(14) . . ? C2 C1 B4 112.71(13) . . ? B5 C1 B4 63.74(11) . . ? C2 C1 B6 62.15(12) . . ? B5 C1 B6 62.39(12) . . ? B4 C1 B6 116.12(14) . . ? C2 C1 Co3 66.47(8) . . ? B5 C1 Co3 125.49(12) . . ? B4 C1 Co3 67.71(8) . . ? B6 C1 Co3 124.95(12) . . ? C2 C1 H1 115.1(13) . . ? B5 C1 H1 117.7(12) . . ? B4 C1 H1 125.2(13) . . ? B6 C1 H1 108.9(13) . . ? Co3 C1 H1 109.6(13) . . ? C1 C2 B11 111.23(14) . . ? C1 C2 B7 112.01(13) . . ? B11 C2 B7 63.79(11) . . ? C1 C2 B6 61.73(12) . . ? B11 C2 B6 62.32(12) . . ? B7 C2 B6 115.86(14) . . ? C1 C2 Co3 66.83(8) . . ? B11 C2 Co3 125.07(12) . . ? B7 C2 Co3 67.12(8) . . ? B6 C2 Co3 124.89(12) . . ? C1 C2 H2 118.0(13) . . ? B11 C2 H2 117.6(13) . . ? B7 C2 H2 122.4(13) . . ? B6 C2 H2 111.8(13) . . ? Co3 C2 H2 108.5(13) . . ? C1 B4 B5 57.94(11) . . ? C1 B4 B8 103.22(12) . . ? B5 B4 B8 106.65(13) . . ? C1 B4 B9 103.19(13) . . ? B5 B4 B9 59.32(11) . . ? B8 B4 B9 59.67(10) . . ? C1 B4 Co3 64.07(8) . . ? B5 B4 Co3 117.09(12) . . ? B8 B4 Co3 64.63(8) . . ? B9 B4 Co3 117.43(10) . . ? C1 B4 H4 121.1(13) . . ? B5 B4 H4 116.2(12) . . ? B8 B4 H4 129.6(12) . . ? B9 B4 H4 123.4(12) . . ? Co3 B4 H4 113.0(12) . . ? C1 B5 B6 59.59(11) . . ? C1 B5 B9 104.38(14) . . ? B6 B5 B9 108.61(14) . . ? C1 B5 B10 104.87(14) . . ? B6 B5 B10 59.93(12) . . ? B9 B5 B10 60.33(11) . . ? C1 B5 B4 58.32(10) . . ? B6 B5 B4 109.28(13) . . ? B9 B5 B4 60.50(11) . . ? B10 B5 B4 109.06(14) . . ? C1 B5 H5 125.0 . . ? B6 B5 H5 120.7 . . ? B9 B5 H5 122.3 . . ? B10 B5 H5 122.1 . . ? B4 B5 H5 120.8 . . ? C1 B6 C2 56.12(10) . . ? C1 B6 B5 58.02(11) . . ? C2 B6 B5 103.56(14) . . ? C1 B6 B11 103.27(14) . . ? C2 B6 B11 57.96(11) . . ? B5 B6 B11 108.21(15) . . ? C1 B6 B10 104.06(14) . . ? C2 B6 B10 104.26(14) . . ? B5 B6 B10 60.44(12) . . ? B11 B6 B10 60.54(12) . . ? C1 B6 H6 125.6 . . ? C2 B6 H6 125.5 . . ? B5 B6 H6 122.2 . . ? B11 B6 H6 122.3 . . ? B10 B6 H6 122.7 . . ? C2 B7 B8 103.03(12) . . ? C2 B7 B12 102.74(14) . . ? B8 B7 B12 59.48(10) . . ? C2 B7 B11 57.59(12) . . ? B8 B7 B11 106.32(13) . . ? B12 B7 B11 59.19(11) . . ? C2 B7 Co3 63.96(8) . . ? B8 B7 Co3 64.90(8) . . ? B12 B7 Co3 117.38(10) . . ? B11 B7 Co3 116.72(13) . . ? C2 B7 H7 125.4(12) . . ? B8 B7 H7 127.2(12) . . ? B12 B7 H7 119.4(12) . . ? B11 B7 H7 116.2(12) . . ? Co3 B7 H7 116.0(12) . . ? N1 B8 B12 113.60(14) . . ? N1 B8 B9 114.05(15) . . ? B12 B8 B9 60.52(11) . . ? N1 B8 B4 124.28(16) . . ? B12 B8 B4 108.67(14) . . ? B9 B8 B4 60.20(10) . . ? N1 B8 B7 122.88(16) . . ? B12 B8 B7 60.34(11) . . ? B9 B8 B7 109.14(14) . . ? B4 B8 B7 108.87(14) . . ? N1 B8 Co3 119.26(13) . . ? B12 B8 Co3 117.74(12) . . ? B9 B8 Co3 118.14(12) . . ? B4 B8 Co3 64.92(8) . . ? B7 B8 Co3 64.47(8) . . ? B5 B9 B8 107.69(14) . . ? B5 B9 B10 60.04(12) . . ? B8 B9 B10 107.76(14) . . ? B5 B9 B4 60.19(12) . . ? B8 B9 B4 60.13(11) . . ? B10 B9 B4 108.58(14) . . ? B5 B9 B12 107.32(14) . . ? B8 B9 B12 59.65(11) . . ? B10 B9 B12 59.70(11) . . ? B4 B9 B12 107.92(13) . . ? B5 B9 H9 122.0 . . ? B8 B9 H9 122.0 . . ? B10 B9 H9 121.6 . . ? B4 B9 H9 121.3 . . ? B12 B9 H9 122.2 . . ? B6 B10 B5 59.63(12) . . ? B6 B10 B12 107.78(14) . . ? B5 B10 B12 107.60(14) . . ? B6 B10 B11 59.68(12) . . ? B5 B10 B11 106.90(15) . . ? B12 B10 B11 59.72(12) . . ? B6 B10 B9 107.80(14) . . ? B5 B10 B9 59.62(11) . . ? B12 B10 B9 60.47(11) . . ? B11 B10 B9 107.81(14) . . ? B6 B10 H10 121.9 . . ? B5 B10 H10 122.4 . . ? B12 B10 H10 121.7 . . ? B11 B10 H10 122.3 . . ? B9 B10 H10 121.6 . . ? C2 B11 B6 59.72(11) . . ? C2 B11 B12 104.39(14) . . ? B6 B11 B12 108.17(15) . . ? C2 B11 B10 105.02(15) . . ? B6 B11 B10 59.79(12) . . ? B12 B11 B10 60.10(11) . . ? C2 B11 B7 58.62(10) . . ? B6 B11 B7 109.44(14) . . ? B12 B11 B7 60.32(11) . . ? B10 B11 B7 108.95(14) . . ? C2 B11 H11 124.7 . . ? B6 B11 H11 120.8 . . ? B12 B11 H11 122.6 . . ? B10 B11 H11 122.2 . . ? B7 B11 H11 120.7 . . ? B11 B12 B8 107.88(14) . . ? B11 B12 B10 60.19(11) . . ? B8 B12 B10 108.01(14) . . ? B11 B12 B7 60.49(12) . . ? B8 B12 B7 60.17(11) . . ? B10 B12 B7 109.15(14) . . ? B11 B12 B9 107.67(14) . . ? B8 B12 B9 59.83(11) . . ? B10 B12 B9 59.83(12) . . ? B7 B12 B9 108.44(13) . . ? B11 B12 H12 121.8 . . ? B8 B12 H12 121.9 . . ? B10 B12 H12 121.4 . . ? B7 B12 H12 120.9 . . ? B9 B12 H12 121.9 . . ? C2' C1' B5' 111.73(14) . . ? C2' C1' B4' 111.84(14) . . ? B5' C1' B4' 64.06(11) . . ? C2' C1' B6' 61.94(10) . . ? B5' C1' B6' 62.45(11) . . ? B4' C1' B6' 115.96(14) . . ? C2' C1' Co3 66.37(8) . . ? B5' C1' Co3 125.81(13) . . ? B4' C1' Co3 67.45(8) . . ? B6' C1' Co3 124.81(11) . . ? C2' C1' H1' 119.2(14) . . ? B5' C1' H1' 117.4(13) . . ? B4' C1' H1' 120.4(14) . . ? B6' C1' H1' 113.9(13) . . ? Co3 C1' H1' 107.0(13) . . ? C1' C2' B11' 111.20(12) . . ? C1' C2' B7' 111.88(12) . . ? B11' C2' B7' 64.15(12) . . ? C1' C2' B6' 61.62(11) . . ? B11' C2' B6' 62.23(11) . . ? B7' C2' B6' 115.94(13) . . ? C1' C2' Co3 66.64(8) . . ? B11' C2' Co3 125.72(12) . . ? B7' C2' Co3 67.39(8) . . ? B6' C2' Co3 124.76(10) . . ? C1' C2' H2' 117.7(11) . . ? B11' C2' H2' 117.5(11) . . ? B7' C2' H2' 122.8(10) . . ? B6' C2' H2' 111.6(10) . . ? Co3 C2' H2' 108.4(10) . . ? C1' B4' B9' 103.17(13) . . ? C1' B4' B8' 104.96(12) . . ? B9' B4' B8' 60.62(11) . . ? C1' B4' B5' 57.57(10) . . ? B9' B4' B5' 59.56(12) . . ? B8' B4' B5' 108.57(14) . . ? C1' B4' Co3 63.76(8) . . ? B9' B4' Co3 117.98(11) . . ? B8' B4' Co3 65.41(8) . . ? B5' B4' Co3 116.70(10) . . ? C1' B4' H4' 119.3(11) . . ? B9' B4' H4' 123.6(11) . . ? B8' B4' H4' 129.9(11) . . ? B5' B4' H4' 114.1(11) . . ? Co3 B4' H4' 113.5(11) . . ? C1' B5' B6' 59.31(11) . . ? C1' B5' B9' 103.53(14) . . ? B6' B5' B9' 108.25(15) . . ? C1' B5' B10' 104.84(14) . . ? B6' B5' B10' 60.10(11) . . ? B9' B5' B10' 60.49(13) . . ? C1' B5' B4' 58.37(10) . . ? B6' B5' B4' 108.67(13) . . ? B9' B5' B4' 59.24(12) . . ? B10' B5' B4' 108.28(16) . . ? C1' B5' H5' 125.1 . . ? B6' B5' H5' 120.8 . . ? B9' B5' H5' 122.9 . . ? B10' B5' H5' 122.0 . . ? B4' B5' H5' 121.5 . . ? C1' B6' C2' 56.44(10) . . ? C1' B6' B11' 103.73(13) . . ? C2' B6' B11' 58.07(11) . . ? C1' B6' B5' 58.24(11) . . ? C2' B6' B5' 103.96(13) . . ? B11' B6' B5' 108.38(15) . . ? C1' B6' B10' 104.11(14) . . ? C2' B6' B10' 104.30(13) . . ? B11' B6' B10' 60.58(11) . . ? B5' B6' B10' 60.21(13) . . ? C1' B6' H6' 125.4 . . ? C2' B6' H6' 125.2 . . ? B11' B6' H6' 122.1 . . ? B5' B6' H6' 122.1 . . ? B10' B6' H6' 122.8 . . ? C2' B7' B12' 103.06(13) . . ? C2' B7' B11' 57.54(10) . . ? B12' B7' B11' 59.71(11) . . ? C2' B7' B8' 104.96(12) . . ? B12' B7' B8' 59.92(11) . . ? B11' B7' B8' 108.24(13) . . ? C2' B7' Co3 63.84(8) . . ? B12' B7' Co3 117.36(11) . . ? B11' B7' Co3 116.63(11) . . ? B8' B7' Co3 65.45(8) . . ? C2' B7' H7' 118.9(12) . . ? B12' B7' H7' 121.0(12) . . ? B11' B7' H7' 110.2(12) . . ? B8' B7' H7' 132.4(13) . . ? Co3 B7' H7' 117.7(12) . . ? B12' B8' B9' 59.27(11) . . ? B12' B8' B4' 105.81(13) . . ? B9' B8' B4' 58.74(10) . . ? B12' B8' B7' 59.15(10) . . ? B9' B8' B7' 106.16(13) . . ? B4' B8' B7' 106.29(12) . . ? B12' B8' Co3 115.14(11) . . ? B9' B8' Co3 115.15(11) . . ? B4' B8' Co3 63.97(8) . . ? B7' B8' Co3 63.64(8) . . ? B12' B8' H8' 117.0(10) . . ? B9' B8' H8' 116.6(9) . . ? B4' B8' H8' 124.5(10) . . ? B7' B8' H8' 125.1(10) . . ? Co3 B8' H8' 119.5(10) . . ? B4' B9' B5' 61.20(11) . . ? B4' B9' B12' 107.95(13) . . ? B5' B9' B12' 107.59(14) . . ? B4' B9' B10' 109.27(13) . . ? B5' B9' B10' 59.77(11) . . ? B12' B9' B10' 60.17(11) . . ? B4' B9' B8' 60.65(11) . . ? B5' B9' B8' 109.90(14) . . ? B12' B9' B8' 60.07(11) . . ? B10' B9' B8' 109.64(14) . . ? B4' B9' H9' 121.0 . . ? B5' B9' H9' 121.2 . . ? B12' B9' H9' 122.3 . . ? B10' B9' H9' 121.0 . . ? B8' B9' H9' 120.4 . . ? B6' B10' B5' 59.68(11) . . ? B6' B10' B11' 59.35(11) . . ? B5' B10' B11' 106.99(14) . . ? B6' B10' B12' 107.16(14) . . ? B5' B10' B12' 107.16(15) . . ? B11' B10' B12' 59.89(11) . . ? B6' B10' B9' 107.33(14) . . ? B5' B10' B9' 59.75(12) . . ? B11' B10' B9' 107.36(15) . . ? B12' B10' B9' 59.64(12) . . ? B6' B10' H10' 122.3 . . ? B5' B10' H10' 122.3 . . ? B11' B10' H10' 122.2 . . ? B12' B10' H10' 122.1 . . ? B9' B10' H10' 122.0 . . ? C2' B11' B6' 59.70(10) . . ? C2' B11' B12' 103.49(13) . . ? B6' B11' B12' 107.96(14) . . ? C2' B11' B10' 105.13(13) . . ? B6' B11' B10' 60.06(11) . . ? B12' B11' B10' 60.20(11) . . ? C2' B11' B7' 58.31(10) . . ? B6' B11' B7' 109.02(14) . . ? B12' B11' B7' 59.51(11) . . ? B10' B11' B7' 108.56(14) . . ? C2' B11' H11' 125.0 . . ? B6' B11' H11' 120.8 . . ? B12' B11' H11' 123.1 . . ? B10' B11' H11' 121.9 . . ? B7' B11' H11' 121.2 . . ? B9' B12' B7' 108.66(14) . . ? B9' B12' B11' 107.81(13) . . ? B7' B12' B11' 60.78(11) . . ? B9' B12' B10' 60.20(12) . . ? B7' B12' B10' 109.34(14) . . ? B11' B12' B10' 59.91(11) . . ? B9' B12' B8' 60.66(11) . . ? B7' B12' B8' 60.93(11) . . ? B11' B12' B8' 109.90(13) . . ? B10' B12' B8' 110.14(14) . . ? B9' B12' H12' 121.9 . . ? B7' B12' H12' 120.9 . . ? B11' B12' H12' 121.4 . . ? B10' B12' H12' 120.9 . . ? B8' B12' H12' 120.1 . . ? C3 N1 B8 176.61(18) . . ? N1 C3 C4 179.4(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.324 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.045 data_6 _database_code_depnum_ccdc_archive 'CCDC 698619' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H35 B18 Co N2' _chemical_formula_sum 'C10 H35 B18 Co N2' _chemical_formula_weight 436.91 _chemical_compound_source 'synthesized by the authors' _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.0734(7) _cell_length_b 13.714(2) _cell_length_c 23.709(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2299.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8353 _cell_measurement_theta_min 1 _cell_measurement_theta_max 26.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3973 _exptl_crystal_size_mid 0.2425 _exptl_crystal_size_min 0.1231 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4 CCD' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 8.343 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16379 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.61 _reflns_number_total 4733 _reflns_number_gt 3491 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) ; _computing_cell_refinement ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) ; _computing_data_reduction ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) ; _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0490P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(17) _refine_ls_number_reflns 4733 _refine_ls_number_parameters 282 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 1.004 _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 0.74668(6) 0.17305(2) 0.133189(13) 0.01749(10) Uani 1 1 d . . . C1 C 0.5023(3) 0.09275(19) 0.13161(12) 0.0185(6) Uani 1 1 d . . . H1A H 0.3980 0.1337 0.1150 0.022 Uiso 1 1 d R . . C2 C 0.6704(4) 0.0466(2) 0.09438(13) 0.0206(7) Uani 1 1 d . . . H2A H 0.6699 0.0566 0.0530 0.025 Uiso 1 1 d R . . B4 B 0.5746(4) 0.1181(3) 0.19802(13) 0.0200(7) Uani 1 1 d . . . H4 H 0.5192 0.1771 0.2248 0.024 Uiso 1 1 calc R . . B5 B 0.4333(5) 0.0143(2) 0.18271(14) 0.0240(8) Uani 1 1 d . . . H5 H 0.2881 0.0082 0.1990 0.029 Uiso 1 1 calc R . . B6 B 0.4896(5) -0.0293(2) 0.11521(14) 0.0237(8) Uani 1 1 d . . . H6 H 0.3838 -0.0628 0.0873 0.028 Uiso 1 1 calc R . . B7 B 0.8773(4) 0.0367(2) 0.13102(15) 0.0200(7) Uani 1 1 d . . . H7 H 1.0210 0.0412 0.1135 0.024 Uiso 1 1 calc R . . B8 B 0.8165(5) 0.0791(3) 0.20084(13) 0.0208(8) Uani 1 1 d . . . B9 B 0.6308(5) 0.0027(2) 0.22693(14) 0.0215(8) Uani 1 1 d . . . H9 H 0.6156 -0.0119 0.2723 0.026 Uiso 1 1 calc R . . B10 B 0.5808(5) -0.0895(3) 0.17536(15) 0.0264(8) Uani 1 1 d . . . H10 H 0.5358 -0.1635 0.1872 0.032 Uiso 1 1 calc R . . B11 B 0.7283(5) -0.0668(2) 0.11640(13) 0.0226(8) Uani 1 1 d . . . H11 H 0.7776 -0.1261 0.0888 0.027 Uiso 1 1 calc R . . B12 B 0.8187(5) -0.0485(3) 0.18553(14) 0.0223(8) Uani 1 1 d . . . H12 H 0.9269 -0.0967 0.2038 0.027 Uiso 1 1 calc R . . C1' C 0.6825(4) 0.2703(2) 0.07088(12) 0.0214(7) Uani 1 1 d . . . H1A' H 0.5709 0.2527 0.0501 0.026 Uiso 1 1 d R . . C2' C 0.6376(4) 0.31032(19) 0.13362(13) 0.0230(7) Uani 1 1 d . . . H2A' H 0.5049 0.3090 0.1427 0.028 Uiso 1 1 d R . . B4' B 0.9041(5) 0.2260(3) 0.06503(14) 0.0219(8) Uani 1 1 d . . . H4' H 0.9495 0.1668 0.0368 0.026 Uiso 1 1 calc R . . B5' B 0.8394(5) 0.3420(3) 0.03680(15) 0.0270(8) Uani 1 1 d . . . H5' H 0.8416 0.3554 -0.0089 0.032 Uiso 1 1 calc R . . B6' B 0.6614(6) 0.3936(3) 0.07935(15) 0.0288(9) Uani 1 1 d . . . H6' H 0.5476 0.4393 0.0620 0.035 Uiso 1 1 calc R . . B7' B 0.8272(5) 0.2987(3) 0.17714(14) 0.0234(8) Uani 1 1 d . . . H7' H 0.8224 0.2879 0.2231 0.028 Uiso 1 1 calc R . . B8' B 1.0090(4) 0.2466(2) 0.13358(14) 0.0230(7) Uani 1 1 d . . . H8' H 1.1256 0.2023 0.1505 0.028 Uiso 1 1 calc R . . B9' B 1.0474(5) 0.3309(3) 0.07689(14) 0.0264(8) Uani 1 1 d . . . H9' H 1.1877 0.3378 0.0573 0.032 Uiso 1 1 calc R . . B10' B 0.8996(5) 0.4339(3) 0.08584(15) 0.0300(9) Uani 1 1 d . . . H10' H 0.9436 0.5075 0.0728 0.036 Uiso 1 1 calc R . . B11' B 0.7600(6) 0.4127(2) 0.14684(13) 0.0299(8) Uani 1 1 d . . . H11' H 0.7090 0.4729 0.1735 0.036 Uiso 1 1 calc R . . B12' B 1.0000(5) 0.3752(3) 0.14570(14) 0.0288(9) Uani 1 1 d . . . H12' H 1.1087 0.4115 0.1714 0.035 Uiso 1 1 calc R . . N1 N 0.9710(3) 0.11126(17) 0.24122(9) 0.0229(6) Uani 1 1 d . . . H1 H 1.0990 0.0961 0.2332 0.028 Uiso 1 1 d R . . C4 C 1.1407(4) 0.1731(2) 0.32223(12) 0.0256(7) Uani 1 1 d . . . H4A H 1.1353 0.2401 0.3340 0.038 Uiso 1 1 calc R . . H4B H 1.2456 0.1642 0.2971 0.038 Uiso 1 1 calc R . . H4C H 1.1565 0.1321 0.3547 0.038 Uiso 1 1 calc R . . N2 N 0.7994(3) 0.1596(2) 0.31860(10) 0.0343(7) Uani 1 1 d . . . H2 H 0.6938 0.1394 0.2947 0.041 Uiso 1 1 d R . . C3 C 0.9637(4) 0.1471(2) 0.29305(12) 0.0230(7) Uani 1 1 d . . . C5 C 0.7718(5) 0.1953(2) 0.37620(11) 0.0345(8) Uani 1 1 d . . . H5A H 0.7396 0.2641 0.3750 0.041 Uiso 1 1 calc R . . H5B H 0.8890 0.1886 0.3971 0.041 Uiso 1 1 calc R . . C6 C 0.6200(6) 0.1412(3) 0.40579(15) 0.0676(14) Uani 1 1 d . . . H6A H 0.6566 0.0733 0.4092 0.081 Uiso 1 1 calc R . . H6B H 0.5053 0.1440 0.3834 0.081 Uiso 1 1 calc R . . C7 C 0.5797(6) 0.1821(3) 0.46437(15) 0.0698(13) Uani 1 1 d D . . H7A H 0.6917 0.1750 0.4876 0.084 Uiso 1 1 calc R . . H7B H 0.5520 0.2512 0.4613 0.084 Uiso 1 1 calc R . . C8 C 0.4150(6) 0.1313(3) 0.49291(17) 0.0782(15) Uani 1 1 d D . . H8A H 0.3047 0.1363 0.4695 0.117 Uiso 1 1 calc R . . H8B H 0.3906 0.1615 0.5287 0.117 Uiso 1 1 calc R . . H8C H 0.4455 0.0638 0.4986 0.117 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 Co3 0.01460(17) 0.02230(18) 0.01557(16) -0.00209(16) 0.0006(2) 0.0002(2) C1 0.0128(13) 0.0226(15) 0.0201(14) -0.0004(14) 0.0002(13) 0.0028(12) C2 0.0158(14) 0.0274(18) 0.0186(15) -0.0046(13) 0.0011(13) 0.0018(13) B4 0.0164(18) 0.027(2) 0.0164(17) -0.0022(14) 0.0034(14) -0.0036(16) B5 0.0198(18) 0.0259(19) 0.0263(19) -0.0004(15) 0.0027(15) 0.0017(16) B6 0.0213(18) 0.0201(18) 0.030(2) -0.0020(15) -0.0029(15) -0.0041(15) B7 0.0186(16) 0.0237(18) 0.0176(16) -0.0044(16) -0.0074(16) 0.0040(14) B8 0.0166(17) 0.029(2) 0.0166(17) 0.0004(15) 0.0000(14) 0.0048(14) B9 0.0185(18) 0.026(2) 0.0205(17) 0.0010(16) 0.0006(14) 0.0036(15) B10 0.024(2) 0.028(2) 0.027(2) -0.0032(16) -0.0029(17) 0.0008(17) B11 0.023(2) 0.0198(16) 0.0254(16) -0.0022(12) -0.0020(17) 0.0038(17) B12 0.0209(18) 0.026(2) 0.0201(18) -0.0011(15) 0.0003(14) 0.0026(14) C1' 0.0172(16) 0.0287(18) 0.0182(15) 0.0015(13) -0.0021(12) 0.0009(13) C2' 0.0197(15) 0.0223(17) 0.0270(16) -0.0067(15) 0.0016(14) 0.0031(12) B4' 0.0181(18) 0.027(2) 0.0205(18) -0.0020(15) 0.0025(15) -0.0037(16) B5' 0.0271(18) 0.029(2) 0.0255(18) 0.0059(16) 0.0033(16) -0.0003(17) B6' 0.033(2) 0.022(2) 0.031(2) 0.0007(17) 0.0049(17) -0.0006(17) B7' 0.0223(16) 0.031(2) 0.0166(17) -0.0089(15) -0.0011(15) -0.0033(15) B8' 0.0179(16) 0.0317(19) 0.0193(16) -0.0056(17) 0.0008(17) -0.0031(15) B9' 0.0216(17) 0.030(2) 0.0273(18) -0.0024(17) 0.0044(14) -0.0090(18) B10' 0.038(2) 0.027(2) 0.025(2) 0.0018(17) 0.0060(18) -0.0050(18) B11' 0.0320(19) 0.0240(17) 0.0337(19) -0.0062(13) 0.002(2) -0.002(2) B12' 0.029(2) 0.031(2) 0.026(2) -0.0056(16) -0.0007(16) -0.0040(17) N1 0.0179(13) 0.0300(15) 0.0209(14) 0.0007(11) 0.0006(11) 0.0018(12) C4 0.0233(16) 0.0261(17) 0.0275(16) -0.0041(16) -0.0046(13) -0.0013(15) N2 0.0260(16) 0.0572(19) 0.0196(12) -0.0139(12) 0.0001(10) -0.0037(13) C3 0.0244(17) 0.0228(17) 0.0217(16) 0.0001(13) -0.0006(14) 0.0015(13) C5 0.0342(19) 0.049(2) 0.0204(15) -0.0085(12) 0.0019(16) 0.0016(17) C6 0.054(2) 0.115(4) 0.034(2) -0.012(2) 0.0024(19) -0.045(3) C7 0.081(3) 0.090(4) 0.039(2) 0.008(2) -0.008(2) -0.033(3) C8 0.079(3) 0.099(4) 0.057(3) -0.025(3) 0.008(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co3 C2' 2.035(3) . ? Co3 C2 2.036(3) . ? Co3 C1' 2.041(3) . ? Co3 C1 2.050(3) . ? Co3 B7 2.086(3) . ? Co3 B4' 2.093(3) . ? Co3 B7' 2.093(3) . ? Co3 B4 2.100(3) . ? Co3 B8' 2.113(3) . ? Co3 B8 2.116(3) . ? C1 C2 1.610(4) . ? C1 B4 1.692(4) . ? C1 B5 1.692(4) . ? C1 B6 1.720(4) . ? C1 H1A 1.0078 . ? C2 B11 1.691(4) . ? C2 B7 1.707(4) . ? C2 B6 1.721(4) . ? C2 H2A 0.9904 . ? B4 B9 1.770(5) . ? B4 B5 1.777(5) . ? B4 B8 1.794(5) . ? B4 H4 1.1000 . ? B5 B9 1.754(5) . ? B5 B6 1.754(5) . ? B5 B10 1.774(5) . ? B5 H5 1.1000 . ? B6 B11 1.766(5) . ? B6 B10 1.770(5) . ? B6 H6 1.1000 . ? B7 B12 1.791(5) . ? B7 B11 1.802(4) . ? B7 B8 1.806(5) . ? B7 H7 1.1000 . ? B8 N1 1.518(4) . ? B8 B12 1.788(5) . ? B8 B9 1.791(5) . ? B9 B10 1.794(5) . ? B9 B12 1.795(5) . ? B9 H9 1.1000 . ? B10 B11 1.772(5) . ? B10 B12 1.790(5) . ? B10 H10 1.1000 . ? B11 B12 1.777(4) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1' C2' 1.617(4) . ? C1' B4' 1.686(5) . ? C1' B5' 1.689(4) . ? C1' B6' 1.710(5) . ? C1' H1A' 0.9612 . ? C2' B11' 1.679(4) . ? C2' B7' 1.700(4) . ? C2' B6' 1.729(4) . ? C2' H2A' 0.9631 . ? B4' B9' 1.782(5) . ? B4' B5' 1.785(5) . ? B4' B8' 1.809(5) . ? B4' H4' 1.1000 . ? B5' B9' 1.758(5) . ? B5' B6' 1.762(5) . ? B5' B10' 1.767(5) . ? B5' H5' 1.1000 . ? B6' B11' 1.765(5) . ? B6' B10' 1.780(5) . ? B6' H6' 1.1000 . ? B7' B12' 1.775(5) . ? B7' B11' 1.785(5) . ? B7' B8' 1.798(5) . ? B7' H7' 1.1000 . ? B8' B12' 1.788(5) . ? B8' B9' 1.793(5) . ? B8' H8' 1.1000 . ? B9' B10' 1.771(5) . ? B9' B12' 1.773(5) . ? B9' H9' 1.1000 . ? B10' B11' 1.775(5) . ? B10' B12' 1.780(5) . ? B10' H10' 1.1000 . ? B11' B12' 1.774(5) . ? B11' H11' 1.1000 . ? B12' H12' 1.1000 . ? N1 C3 1.325(3) . ? N1 H1 0.9479 . ? C4 C3 1.474(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? N2 C3 1.322(3) . ? N2 C5 1.464(3) . ? N2 H2 0.9767 . ? C5 C6 1.482(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.525(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.517(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 133.62(11) . . ? C2' Co3 C1' 46.75(11) . . ? C2 Co3 C1' 99.81(12) . . ? C2' Co3 C1 100.22(11) . . ? C2 Co3 C1 46.42(10) . . ? C1' Co3 C1 98.63(11) . . ? C2' Co3 B7 175.84(12) . . ? C2 Co3 B7 48.91(12) . . ? C1' Co3 B7 131.77(13) . . ? C1 Co3 B7 83.76(11) . . ? C2' Co3 B4' 83.35(13) . . ? C2 Co3 B4' 95.04(13) . . ? C1' Co3 B4' 48.13(13) . . ? C1 Co3 B4' 128.40(12) . . ? B7 Co3 B4' 93.25(14) . . ? C2' Co3 B7' 48.61(12) . . ? C2 Co3 B7' 176.87(13) . . ? C1' Co3 B7' 83.28(14) . . ? C1 Co3 B7' 132.91(12) . . ? B7 Co3 B7' 129.04(13) . . ? B4' Co3 B7' 87.35(14) . . ? C2' Co3 B4 96.23(13) . . ? C2 Co3 B4 82.62(12) . . ? C1' Co3 B4 129.43(13) . . ? C1 Co3 B4 48.09(11) . . ? B7 Co3 B4 87.31(14) . . ? B4' Co3 B4 176.37(13) . . ? B7' Co3 B4 95.09(13) . . ? C2' Co3 B8' 83.75(12) . . ? C2 Co3 B8' 129.92(12) . . ? C1' Co3 B8' 83.49(13) . . ? C1 Co3 B8' 175.96(12) . . ? B7 Co3 B8' 92.25(13) . . ? B4' Co3 B8' 50.96(13) . . ? B7' Co3 B8' 50.61(13) . . ? B4 Co3 B8' 132.63(13) . . ? C2' Co3 B8 130.41(13) . . ? C2 Co3 B8 83.44(13) . . ? C1' Co3 B8 176.73(13) . . ? C1 Co3 B8 83.31(12) . . ? B7 Co3 B8 50.92(13) . . ? B4' Co3 B8 132.28(13) . . ? B7' Co3 B8 93.46(14) . . ? B4 Co3 B8 50.36(13) . . ? B8' Co3 B8 94.73(13) . . ? C2 C1 B4 111.6(2) . . ? C2 C1 B5 110.8(2) . . ? B4 C1 B5 63.34(18) . . ? C2 C1 B6 62.12(18) . . ? B4 C1 B6 115.2(2) . . ? B5 C1 B6 61.86(18) . . ? C2 C1 Co3 66.35(13) . . ? B4 C1 Co3 67.52(14) . . ? B5 C1 Co3 124.87(19) . . ? B6 C1 Co3 124.82(18) . . ? C2 C1 H1A 123.1 . . ? B4 C1 H1A 118.1 . . ? B5 C1 H1A 115.0 . . ? B6 C1 H1A 114.5 . . ? Co3 C1 H1A 109.0 . . ? C1 C2 B11 111.8(2) . . ? C1 C2 B7 112.6(2) . . ? B11 C2 B7 64.05(18) . . ? C1 C2 B6 62.08(17) . . ? B11 C2 B6 62.3(2) . . ? B7 C2 B6 116.3(2) . . ? C1 C2 Co3 67.23(14) . . ? B11 C2 Co3 125.4(2) . . ? B7 C2 Co3 67.07(15) . . ? B6 C2 Co3 125.60(19) . . ? C1 C2 H2A 119.1 . . ? B11 C2 H2A 115.7 . . ? B7 C2 H2A 121.2 . . ? B6 C2 H2A 111.4 . . ? Co3 C2 H2A 109.3 . . ? C1 B4 B9 104.2(2) . . ? C1 B4 B5 58.34(17) . . ? B9 B4 B5 59.28(18) . . ? C1 B4 B8 105.2(2) . . ? B9 B4 B8 60.32(19) . . ? B5 B4 B8 107.8(2) . . ? C1 B4 Co3 64.39(13) . . ? B9 B4 Co3 118.3(2) . . ? B5 B4 Co3 117.6(2) . . ? B8 B4 Co3 65.27(15) . . ? C1 B4 H4 125.4 . . ? B9 B4 H4 121.0 . . ? B5 B4 H4 120.4 . . ? B8 B4 H4 122.5 . . ? Co3 B4 H4 111.4 . . ? C1 B5 B9 104.8(2) . . ? C1 B5 B6 59.86(17) . . ? B9 B5 B6 109.5(2) . . ? C1 B5 B10 105.7(2) . . ? B9 B5 B10 61.12(19) . . ? B6 B5 B10 60.21(19) . . ? C1 B5 B4 58.31(17) . . ? B9 B5 B4 60.17(18) . . ? B6 B5 B4 109.4(2) . . ? B10 B5 B4 109.4(2) . . ? C1 B5 H5 124.7 . . ? B9 B5 H5 121.8 . . ? B6 B5 H5 120.4 . . ? B10 B5 H5 121.5 . . ? B4 B5 H5 121.0 . . ? C1 B6 C2 55.80(16) . . ? C1 B6 B5 58.28(18) . . ? C2 B6 B5 103.0(2) . . ? C1 B6 B11 103.3(2) . . ? C2 B6 B11 58.00(18) . . ? B5 B6 B11 107.6(2) . . ? C1 B6 B10 104.6(2) . . ? C2 B6 B10 104.0(2) . . ? B5 B6 B10 60.43(19) . . ? B11 B6 B10 60.15(19) . . ? C1 B6 H6 125.3 . . ? C2 B6 H6 125.8 . . ? B5 B6 H6 122.5 . . ? B11 B6 H6 122.6 . . ? B10 B6 H6 122.6 . . ? C2 B7 B12 102.7(2) . . ? C2 B7 B11 57.54(18) . . ? B12 B7 B11 59.28(18) . . ? C2 B7 B8 103.7(2) . . ? B12 B7 B8 59.59(19) . . ? B11 B7 B8 106.9(2) . . ? C2 B7 Co3 64.02(14) . . ? B12 B7 Co3 117.7(2) . . ? B11 B7 Co3 116.9(2) . . ? B8 B7 Co3 65.39(15) . . ? C2 B7 H7 126.6 . . ? B12 B7 H7 121.5 . . ? B11 B7 H7 120.8 . . ? B8 B7 H7 123.2 . . ? Co3 B7 H7 111.6 . . ? N1 B8 B12 114.0(2) . . ? N1 B8 B9 118.7(2) . . ? B12 B8 B9 60.22(19) . . ? N1 B8 B4 128.6(3) . . ? B12 B8 B4 107.0(2) . . ? B9 B8 B4 59.19(18) . . ? N1 B8 B7 120.0(2) . . ? B12 B8 B7 59.78(18) . . ? B9 B8 B7 107.6(2) . . ? B4 B8 B7 106.8(2) . . ? N1 B8 Co3 118.0(2) . . ? B12 B8 Co3 116.37(19) . . ? B9 B8 Co3 116.6(2) . . ? B4 B8 Co3 64.37(15) . . ? B7 B8 Co3 63.69(14) . . ? B5 B9 B4 60.55(18) . . ? B5 B9 B8 108.9(2) . . ? B4 B9 B8 60.50(18) . . ? B5 B9 B10 59.98(19) . . ? B4 B9 B10 108.8(2) . . ? B8 B9 B10 108.8(2) . . ? B5 B9 B12 107.4(2) . . ? B4 B9 B12 107.7(2) . . ? B8 B9 B12 59.81(19) . . ? B10 B9 B12 59.84(19) . . ? B5 B9 H9 121.6 . . ? B4 B9 H9 121.3 . . ? B8 B9 H9 121.1 . . ? B10 B9 H9 121.3 . . ? B12 B9 H9 122.4 . . ? B6 B10 B11 59.81(19) . . ? B6 B10 B5 59.35(19) . . ? B11 B10 B5 106.5(3) . . ? B6 B10 B12 107.8(2) . . ? B11 B10 B12 59.87(19) . . ? B5 B10 B12 106.7(2) . . ? B6 B10 B9 107.0(2) . . ? B11 B10 B9 107.4(2) . . ? B5 B10 B9 58.90(19) . . ? B12 B10 B9 60.12(18) . . ? B6 B10 H10 122.0 . . ? B11 B10 H10 122.2 . . ? B5 B10 H10 123.0 . . ? B12 B10 H10 121.8 . . ? B9 B10 H10 122.2 . . ? C2 B11 B6 59.68(18) . . ? C2 B11 B10 105.2(2) . . ? B6 B11 B10 60.04(19) . . ? C2 B11 B12 104.0(2) . . ? B6 B11 B12 108.5(2) . . ? B10 B11 B12 60.58(19) . . ? C2 B11 B7 58.41(17) . . ? B6 B11 B7 109.4(2) . . ? B10 B11 B7 109.3(2) . . ? B12 B11 B7 60.06(19) . . ? C2 B11 H11 125.0 . . ? B6 B11 H11 120.6 . . ? B10 B11 H11 121.7 . . ? B12 B11 H11 122.6 . . ? B7 B11 H11 120.8 . . ? B11 B12 B8 108.8(2) . . ? B11 B12 B10 59.56(19) . . ? B8 B12 B10 109.1(2) . . ? B11 B12 B7 60.66(18) . . ? B8 B12 B7 60.63(19) . . ? B10 B12 B7 109.0(2) . . ? B11 B12 B9 107.1(2) . . ? B8 B12 B9 59.97(18) . . ? B10 B12 B9 60.04(18) . . ? B7 B12 B9 108.1(2) . . ? B11 B12 H12 121.9 . . ? B8 B12 H12 120.9 . . ? B10 B12 H12 121.2 . . ? B7 B12 H12 121.0 . . ? B9 B12 H12 122.3 . . ? C2' C1' B4' 112.4(2) . . ? C2' C1' B5' 111.8(2) . . ? B4' C1' B5' 63.85(19) . . ? C2' C1' B6' 62.54(19) . . ? B4' C1' B6' 116.5(2) . . ? B5' C1' B6' 62.4(2) . . ? C2' C1' Co3 66.41(14) . . ? B4' C1' Co3 67.53(15) . . ? B5' C1' Co3 125.5(2) . . ? B6' C1' Co3 125.5(2) . . ? C2' C1' H1A' 113.3 . . ? B4' C1' H1A' 129.1 . . ? B5' C1' H1A' 116.1 . . ? B6' C1' H1A' 103.7 . . ? Co3 C1' H1A' 112.9 . . ? C1' C2' B11' 110.8(2) . . ? C1' C2' B7' 111.8(2) . . ? B11' C2' B7' 63.77(19) . . ? C1' C2' B6' 61.36(19) . . ? B11' C2' B6' 62.37(19) . . ? B7' C2' B6' 115.9(2) . . ? C1' C2' Co3 66.83(14) . . ? B11' C2' Co3 125.4(2) . . ? B7' C2' Co3 67.49(15) . . ? B6' C2' Co3 124.79(19) . . ? C1' C2' H2A' 113.0 . . ? B11' C2' H2A' 118.5 . . ? B7' C2' H2A' 129.1 . . ? B6' C2' H2A' 105.9 . . ? Co3 C2' H2A' 110.7 . . ? C1' B4' B9' 103.0(2) . . ? C1' B4' B5' 58.15(18) . . ? B9' B4' B5' 59.06(19) . . ? C1' B4' B8' 104.6(2) . . ? B9' B4' B8' 59.91(18) . . ? B5' B4' B8' 107.6(2) . . ? C1' B4' Co3 64.34(15) . . ? B9' B4' Co3 117.5(2) . . ? B5' B4' Co3 117.6(2) . . ? B8' B4' Co3 65.09(15) . . ? C1' B4' H4' 126.0 . . ? B9' B4' H4' 121.7 . . ? B5' B4' H4' 120.3 . . ? B8' B4' H4' 122.8 . . ? Co3 B4' H4' 111.6 . . ? C1' B5' B9' 103.9(2) . . ? C1' B5' B6' 59.35(19) . . ? B9' B5' B6' 108.9(3) . . ? C1' B5' B10' 105.0(2) . . ? B9' B5' B10' 60.3(2) . . ? B6' B5' B10' 60.6(2) . . ? C1' B5' B4' 58.00(18) . . ? B9' B5' B4' 60.4(2) . . ? B6' B5' B4' 109.0(2) . . ? B10' B5' B4' 109.1(2) . . ? C1' B5' H5' 125.3 . . ? B9' B5' H5' 122.4 . . ? B6' B5' H5' 120.5 . . ? B10' B5' H5' 121.7 . . ? B4' B5' H5' 121.0 . . ? C1' B6' C2' 56.11(17) . . ? C1' B6' B5' 58.21(19) . . ? C2' B6' B5' 103.3(2) . . ? C1' B6' B11' 102.6(3) . . ? C2' B6' B11' 57.44(18) . . ? B5' B6' B11' 107.2(3) . . ? C1' B6' B10' 103.6(2) . . ? C2' B6' B10' 103.5(3) . . ? B5' B6' B10' 59.86(19) . . ? B11' B6' B10' 60.1(2) . . ? C1' B6' H6' 125.7 . . ? C2' B6' H6' 125.7 . . ? B5' B6' H6' 122.5 . . ? B11' B6' H6' 123.0 . . ? B10' B6' H6' 123.2 . . ? C2' B7' B12' 103.5(2) . . ? C2' B7' B11' 57.55(18) . . ? B12' B7' B11' 59.8(2) . . ? C2' B7' B8' 104.7(2) . . ? B12' B7' B8' 60.04(19) . . ? B11' B7' B8' 107.9(2) . . ? C2' B7' Co3 63.91(14) . . ? B12' B7' Co3 117.7(2) . . ? B11' B7' Co3 116.6(2) . . ? B8' B7' Co3 65.26(15) . . ? C2' B7' H7' 126.2 . . ? B12' B7' H7' 121.1 . . ? B11' B7' H7' 120.6 . . ? B8' B7' H7' 122.5 . . ? Co3 B7' H7' 112.0 . . ? B12' B8' B9' 59.35(19) . . ? B12' B8' B7' 59.36(19) . . ? B9' B8' B7' 106.4(2) . . ? B12' B8' B4' 106.5(2) . . ? B9' B8' B4' 59.29(18) . . ? B7' B8' B4' 106.5(2) . . ? B12' B8' Co3 116.1(2) . . ? B9' B8' Co3 115.9(2) . . ? B7' B8' Co3 64.13(14) . . ? B4' B8' Co3 63.95(14) . . ? B12' B8' H8' 120.9 . . ? B9' B8' H8' 121.1 . . ? B7' B8' H8' 123.2 . . ? B4' B8' H8' 123.2 . . ? Co3 B8' H8' 113.3 . . ? B5' B9' B10' 60.1(2) . . ? B5' B9' B12' 108.1(3) . . ? B10' B9' B12' 60.3(2) . . ? B5' B9' B4' 60.57(19) . . ? B10' B9' B4' 109.1(2) . . ? B12' B9' B4' 108.3(2) . . ? B5' B9' B8' 109.6(2) . . ? B10' B9' B8' 109.6(2) . . ? B12' B9' B8' 60.18(19) . . ? B4' B9' B8' 60.80(18) . . ? B5' B9' H9' 121.3 . . ? B10' B9' H9' 121.0 . . ? B12' B9' H9' 121.9 . . ? B4' B9' H9' 121.1 . . ? B8' B9' H9' 120.5 . . ? B5' B10' B9' 59.6(2) . . ? B5' B10' B11' 106.6(3) . . ? B9' B10' B11' 107.2(3) . . ? B5' B10' B12' 107.3(3) . . ? B9' B10' B12' 59.92(19) . . ? B11' B10' B12' 59.9(2) . . ? B5' B10' B6' 59.56(19) . . ? B9' B10' B6' 107.5(2) . . ? B11' B10' B6' 59.5(2) . . ? B12' B10' B6' 107.8(3) . . ? B5' B10' H10' 122.5 . . ? B9' B10' H10' 122.1 . . ? B11' B10' H10' 122.5 . . ? B12' B10' H10' 121.7 . . ? B6' B10' H10' 121.9 . . ? C2' B11' B6' 60.19(19) . . ? C2' B11' B12' 104.4(2) . . ? B6' B11' B12' 108.7(2) . . ? C2' B11' B10' 105.8(2) . . ? B6' B11' B10' 60.4(2) . . ? B12' B11' B10' 60.2(2) . . ? C2' B11' B7' 58.68(17) . . ? B6' B11' B7' 109.9(2) . . ? B12' B11' B7' 59.8(2) . . ? B10' B11' B7' 108.9(3) . . ? C2' B11' H11' 124.4 . . ? B6' B11' H11' 120.2 . . ? B12' B11' H11' 122.7 . . ? B10' B11' H11' 121.8 . . ? B7' B11' H11' 120.9 . . ? B9' B12' B11' 107.1(2) . . ? B9' B12' B7' 108.3(2) . . ? B11' B12' B7' 60.38(19) . . ? B9' B12' B10' 59.8(2) . . ? B11' B12' B10' 59.93(19) . . ? B7' B12' B10' 109.1(3) . . ? B9' B12' B8' 60.5(2) . . ? B11' B12' B8' 108.8(2) . . ? B7' B12' B8' 60.60(19) . . ? B10' B12' B8' 109.4(3) . . ? B9' B12' H12' 122.2 . . ? B11' B12' H12' 122.0 . . ? B7' B12' H12' 121.1 . . ? B10' B12' H12' 121.1 . . ? B8' B12' H12' 120.7 . . ? C3 N1 B8 131.7(2) . . ? C3 N1 H1 107.7 . . ? B8 N1 H1 119.9 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 N2 C5 126.0(2) . . ? C3 N2 H2 111.7 . . ? C5 N2 H2 122.2 . . ? N2 C3 N1 120.5(3) . . ? N2 C3 C4 120.0(2) . . ? N1 C3 C4 119.5(3) . . ? N2 C5 C6 111.7(3) . . ? N2 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N2 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C5 C6 C7 112.5(3) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 112.4(3) . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.61 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.663 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.058 data_7 _database_code_depnum_ccdc_archive 'CCDC 698620' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H35 B18 Co N2' _chemical_formula_sum 'C10 H35 B18 Co N2' _chemical_formula_weight 436.91 _chemical_compound_source 'synthesized by the authors' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4127(2) _cell_length_b 12.1868(2) _cell_length_c 29.9491(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4530.43(12) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5708 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '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 44317 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5178 _reflns_number_gt 4476 _reflns_threshold_expression I>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 ? _computing_publication_material ? _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^)+(0.0356P)^2^+4.7024P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5178 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.490815(17) 0.202972(18) 0.158778(7) 0.01531(8) Uani 1 1 d . . . C1 C 0.48508(14) 0.33845(15) 0.19828(6) 0.0222(4) Uani 1 1 d . . . H1 H 0.4048 0.3751 0.1939 0.027 Uiso 1 1 calc R . . C2 C 0.50162(13) 0.22665(15) 0.22601(6) 0.0215(4) Uani 1 1 d . . . H2 H 0.4329 0.1834 0.2411 0.026 Uiso 1 1 calc R . . B4 B 0.57549(16) 0.35016(17) 0.15532(7) 0.0231(4) Uani 1 1 d . . . H4 H 0.5620 0.3920 0.1233 0.028 Uiso 1 1 calc R . . B5 B 0.58761(17) 0.42658(18) 0.20683(8) 0.0281(5) Uani 1 1 d . . . H5 H 0.5797 0.5165 0.2073 0.034 Uiso 1 1 calc R . . B6 B 0.53738(18) 0.34743(19) 0.25127(8) 0.0282(5) Uani 1 1 d . . . H6 H 0.4969 0.3845 0.2803 0.034 Uiso 1 1 calc R . . B7 B 0.60475(15) 0.14967(18) 0.20583(7) 0.0217(4) Uani 1 1 d . . . H7 H 0.6104 0.0596 0.2068 0.026 Uiso 1 1 calc R . . B8 B 0.66169(15) 0.22970(18) 0.16036(7) 0.0210(4) Uani 1 1 d . . . B9 B 0.70142(17) 0.35862(19) 0.18395(7) 0.0263(4) Uani 1 1 d . . . H9 H 0.7692 0.4048 0.1695 0.032 Uiso 1 1 calc R . . B10 B 0.67831(17) 0.35615(19) 0.24250(7) 0.0281(5) Uani 1 1 d . . . H10 H 0.7322 0.3995 0.2657 0.034 Uiso 1 1 calc R . . B11 B 0.61629(17) 0.22896(19) 0.25617(7) 0.0270(5) Uani 1 1 d . . . H11 H 0.6272 0.1893 0.2889 0.032 Uiso 1 1 calc R . . B12 B 0.71870(16) 0.23400(19) 0.21528(7) 0.0249(4) Uani 1 1 d . . . H12 H 0.7983 0.1975 0.2216 0.030 Uiso 1 1 calc R . . C1' C 0.39748(14) 0.06456(15) 0.16158(6) 0.0218(4) Uani 1 1 d . . . H1' H 0.4111 0.0270 0.1945 0.026 Uiso 1 1 calc R . . C2' C 0.32835(13) 0.17501(15) 0.15632(6) 0.0210(4) Uani 1 1 d . . . H2' H 0.2934 0.2160 0.1857 0.025 Uiso 1 1 calc R . . B4' B 0.49672(16) 0.05658(17) 0.12285(7) 0.0238(4) Uani 1 1 d . . . H4' H 0.5747 0.0151 0.1272 0.029 Uiso 1 1 calc R . . B5' B 0.37580(17) -0.02191(19) 0.11853(8) 0.0290(5) Uani 1 1 d . . . H5' H 0.3772 -0.1119 0.1210 0.035 Uiso 1 1 calc R . . B6' B 0.26827(16) 0.05325(18) 0.14120(7) 0.0250(4) Uani 1 1 d . . . H6' H 0.2004 0.0135 0.1584 0.030 Uiso 1 1 calc R . . B7' B 0.37193(16) 0.25480(18) 0.11356(7) 0.0236(4) Uani 1 1 d . . . H7' H 0.3671 0.3448 0.1119 0.028 Uiso 1 1 calc R . . B8' B 0.48077(16) 0.17890(19) 0.08906(7) 0.0242(4) Uani 1 1 d . . . H8' H 0.5471 0.2178 0.0706 0.029 Uiso 1 1 calc R . . B9' B 0.42582(17) 0.0497(2) 0.07121(8) 0.0301(5) Uani 1 1 d . . . H9' H 0.4597 0.0062 0.0423 0.036 Uiso 1 1 calc R . . B10' B 0.28507(17) 0.04861(18) 0.08240(7) 0.0258(4) Uani 1 1 d . . . H10' H 0.2281 0.0055 0.0604 0.031 Uiso 1 1 calc R . . B11' B 0.25225(16) 0.17344(18) 0.10961(7) 0.0246(4) Uani 1 1 d . . . H11' H 0.1724 0.2117 0.1064 0.029 Uiso 1 1 calc R . . B12' B 0.34778(17) 0.1729(2) 0.06572(7) 0.0285(5) Uani 1 1 d . . . H12' H 0.3301 0.2104 0.0331 0.034 Uiso 1 1 calc R . . N1 N 0.72313(12) 0.17851(14) 0.12164(5) 0.0259(3) Uani 1 1 d . . . C3 C 0.82638(14) 0.17146(16) 0.11021(6) 0.0251(4) Uani 1 1 d . . . C4 C 0.91270(15) 0.22218(18) 0.13821(7) 0.0310(4) Uani 1 1 d . . . H4A H 0.8808 0.2725 0.1591 0.046 Uiso 1 1 calc R . . H4B H 0.9623 0.2609 0.1194 0.046 Uiso 1 1 calc R . . H4C H 0.9504 0.1658 0.1542 0.046 Uiso 1 1 calc R . . N2 N 0.85516(12) 0.11870(15) 0.07307(5) 0.0299(4) Uani 1 1 d . . . C5 C 0.77663(16) 0.0715(2) 0.04176(6) 0.0348(5) Uani 1 1 d . . . H5A H 0.8067 0.0735 0.0119 0.042 Uiso 1 1 calc R . . H5B H 0.7122 0.1165 0.0418 0.042 Uiso 1 1 calc R . . C6 C 0.74567(19) -0.0461(2) 0.05292(8) 0.0458(6) Uani 1 1 d . . . H6A H 0.8089 -0.0914 0.0526 0.069 Uiso 1 1 calc R . . H6B H 0.6952 -0.0726 0.0312 0.069 Uiso 1 1 calc R . . H6C H 0.7134 -0.0484 0.0820 0.069 Uiso 1 1 calc R . . C7 C 0.96970(15) 0.0977(2) 0.06152(7) 0.0335(5) Uani 1 1 d . . . H7A H 0.9758 0.0255 0.0481 0.040 Uiso 1 1 calc R . . H7B H 1.0124 0.0979 0.0887 0.040 Uiso 1 1 calc R . . C8 C 1.01459(18) 0.1822(2) 0.02960(8) 0.0488(7) Uani 1 1 d . . . H8A H 0.9728 0.1823 0.0026 0.073 Uiso 1 1 calc R . . H8B H 1.0881 0.1646 0.0227 0.073 Uiso 1 1 calc R . . H8C H 1.0114 0.2535 0.0432 0.073 Uiso 1 1 calc R . . H1A H 0.675(2) 0.139(2) 0.1030(8) 0.050(7) 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 0.01254(12) 0.01649(12) 0.01691(13) -0.00228(8) -0.00131(8) -0.00022(8) C1 0.0194(8) 0.0218(9) 0.0253(9) -0.0069(7) 0.0007(7) -0.0002(7) C2 0.0200(8) 0.0264(9) 0.0180(8) -0.0020(7) -0.0002(6) -0.0027(7) B4 0.0211(9) 0.0220(10) 0.0261(10) 0.0009(8) 0.0003(8) -0.0052(8) B5 0.0254(10) 0.0236(10) 0.0353(12) -0.0075(9) -0.0016(9) -0.0044(8) B6 0.0246(10) 0.0336(11) 0.0263(10) -0.0107(9) 0.0016(8) -0.0040(9) B7 0.0188(9) 0.0248(10) 0.0216(10) -0.0008(8) -0.0029(7) 0.0005(8) B8 0.0139(8) 0.0282(10) 0.0210(9) -0.0044(8) 0.0008(7) -0.0010(7) B9 0.0219(10) 0.0315(11) 0.0256(11) -0.0057(9) 0.0007(8) -0.0078(8) B10 0.0222(10) 0.0350(12) 0.0271(11) -0.0124(9) -0.0013(8) -0.0046(9) B11 0.0215(10) 0.0381(12) 0.0213(10) -0.0035(9) -0.0026(8) -0.0032(9) B12 0.0190(9) 0.0332(12) 0.0224(10) -0.0054(9) -0.0035(8) -0.0014(8) C1' 0.0195(8) 0.0200(8) 0.0259(9) 0.0009(7) -0.0036(7) -0.0027(7) C2' 0.0142(8) 0.0257(9) 0.0230(9) -0.0028(7) -0.0003(6) -0.0022(6) B4' 0.0192(9) 0.0214(10) 0.0308(11) -0.0064(8) -0.0029(8) 0.0014(7) B5' 0.0247(10) 0.0233(10) 0.0391(13) -0.0081(9) -0.0054(9) -0.0017(8) B6' 0.0202(10) 0.0246(10) 0.0302(11) -0.0017(9) -0.0026(8) -0.0052(8) B7' 0.0202(9) 0.0216(10) 0.0290(11) 0.0017(8) -0.0066(8) 0.0009(8) B8' 0.0199(9) 0.0346(11) 0.0182(9) -0.0006(8) -0.0013(7) -0.0038(8) B9' 0.0216(10) 0.0402(13) 0.0284(11) -0.0149(10) -0.0018(8) 0.0001(9) B10' 0.0205(9) 0.0304(11) 0.0265(11) -0.0087(9) -0.0027(8) -0.0038(8) B11' 0.0163(9) 0.0275(11) 0.0299(11) -0.0027(9) -0.0039(8) -0.0007(8) B12' 0.0237(10) 0.0383(12) 0.0235(11) 0.0024(9) -0.0045(8) -0.0058(9) N1 0.0158(7) 0.0383(9) 0.0236(8) -0.0093(7) 0.0004(6) -0.0023(6) C3 0.0192(8) 0.0338(10) 0.0222(9) -0.0010(8) 0.0019(7) -0.0009(7) C4 0.0181(9) 0.0442(12) 0.0306(10) -0.0076(9) 0.0028(7) -0.0041(8) N2 0.0190(7) 0.0489(11) 0.0217(8) -0.0072(7) 0.0025(6) 0.0014(7) C5 0.0257(10) 0.0587(14) 0.0198(9) -0.0132(9) -0.0004(7) 0.0045(9) C6 0.0353(12) 0.0637(16) 0.0385(12) -0.0233(12) 0.0022(10) -0.0062(11) C7 0.0200(9) 0.0537(13) 0.0269(10) -0.0022(9) 0.0039(7) 0.0054(9) C8 0.0297(11) 0.0797(19) 0.0369(13) 0.0189(13) 0.0082(9) 0.0085(11) _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 C1 2.0324(18) . ? Co3 C2 2.0384(18) . ? Co3 C2' 2.0465(17) . ? Co3 C1' 2.0481(17) . ? Co3 B4 2.082(2) . ? Co3 B4' 2.085(2) . ? Co3 B7 2.0995(19) . ? Co3 B7' 2.100(2) . ? Co3 B8' 2.112(2) . ? Co3 B8 2.1464(19) . ? C1 C2 1.609(3) . ? C1 B5 1.685(3) . ? C1 B4 1.713(3) . ? C1 B6 1.718(3) . ? C1 H1 1.1000 . ? C2 B11 1.686(3) . ? C2 B7 1.698(3) . ? C2 B6 1.713(3) . ? C2 H2 1.1000 . ? B4 B9 1.786(3) . ? B4 B5 1.808(3) . ? B4 B8 1.823(3) . ? B4 H4 1.1000 . ? B5 B6 1.758(3) . ? B5 B10 1.774(3) . ? B5 B9 1.775(3) . ? B5 H5 1.1000 . ? B6 B11 1.751(3) . ? B6 B10 1.772(3) . ? B6 H6 1.1000 . ? B7 B12 1.771(3) . ? B7 B11 1.797(3) . ? B7 B8 1.818(3) . ? B7 H7 1.1000 . ? B8 N1 1.522(2) . ? B8 B12 1.791(3) . ? B8 B9 1.792(3) . ? B9 B10 1.777(3) . ? B9 B12 1.798(3) . ? B9 H9 1.1000 . ? B10 B12 1.770(3) . ? B10 B11 1.778(3) . ? B10 H10 1.1000 . ? B11 B12 1.766(3) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1' C2' 1.604(2) . ? C1' B5' 1.687(3) . ? C1' B4' 1.695(3) . ? C1' B6' 1.722(3) . ? C1' H1' 1.1000 . ? C2' B11' 1.688(3) . ? C2' B7' 1.696(3) . ? C2' B6' 1.721(3) . ? C2' H2' 1.1000 . ? B4' B9' 1.781(3) . ? B4' B5' 1.784(3) . ? B4' B8' 1.813(3) . ? B4' H4' 1.1000 . ? B5' B6' 1.755(3) . ? B5' B9' 1.777(3) . ? B5' B10' 1.783(3) . ? B5' H5' 1.1000 . ? B6' B11' 1.755(3) . ? B6' B10' 1.774(3) . ? B6' H6' 1.1000 . ? B7' B12' 1.772(3) . ? B7' B11' 1.790(3) . ? B7' B8' 1.794(3) . ? B7' H7' 1.1000 . ? B8' B12' 1.794(3) . ? B8' B9' 1.797(3) . ? B8' H8' 1.1000 . ? B9' B10' 1.779(3) . ? B9' B12' 1.794(3) . ? B9' H9' 1.1000 . ? B10' B11' 1.773(3) . ? B10' B12' 1.775(3) . ? B10' H10' 1.1000 . ? B11' B12' 1.770(3) . ? B11' H11' 1.1000 . ? B12' H12' 1.1000 . ? N1 C3 1.329(2) . ? N1 H1A 0.94(3) . ? C3 N2 1.334(2) . ? C3 C4 1.494(3) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? N2 C5 1.470(2) . ? N2 C7 1.485(2) . ? C5 C6 1.520(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.512(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 Co3 C2 46.55(7) . . ? C1 Co3 C2' 96.99(7) . . ? C2 Co3 C2' 97.12(7) . . ? C1 Co3 C1' 128.71(7) . . ? C2 Co3 C1' 96.51(7) . . ? C2' Co3 C1' 46.13(7) . . ? C1 Co3 B4 49.20(8) . . ? C2 Co3 B4 83.91(8) . . ? C2' Co3 B4 129.74(8) . . ? C1' Co3 B4 175.86(8) . . ? C1 Co3 B4' 175.47(8) . . ? C2 Co3 B4' 128.95(8) . . ? C2' Co3 B4' 82.73(8) . . ? C1' Co3 B4' 48.41(8) . . ? B4 Co3 B4' 133.95(8) . . ? C1 Co3 B7 83.35(8) . . ? C2 Co3 B7 48.43(7) . . ? C2' Co3 B7 129.52(8) . . ? C1' Co3 B7 95.66(8) . . ? B4 Co3 B7 87.70(8) . . ? B4' Co3 B7 93.32(8) . . ? C1 Co3 B7' 96.11(8) . . ? C2 Co3 B7' 129.84(8) . . ? C2' Co3 B7' 48.28(8) . . ? C1' Co3 B7' 82.91(8) . . ? B4 Co3 B7' 93.65(8) . . ? B4' Co3 B7' 87.09(8) . . ? B7 Co3 B7' 177.70(8) . . ? C1 Co3 B8' 133.33(8) . . ? C2 Co3 B8' 179.58(8) . . ? C2' Co3 B8' 83.29(7) . . ? C1' Co3 B8' 83.84(8) . . ? B4 Co3 B8' 95.76(8) . . ? B4' Co3 B8' 51.17(9) . . ? B7 Co3 B8' 131.32(8) . . ? B7' Co3 B8' 50.42(8) . . ? C1 Co3 B8 84.17(7) . . ? C2 Co3 B8 83.78(7) . . ? C2' Co3 B8 178.83(8) . . ? C1' Co3 B8 133.08(8) . . ? B4 Co3 B8 51.05(8) . . ? B4' Co3 B8 96.12(8) . . ? B7 Co3 B8 50.69(8) . . ? B7' Co3 B8 131.53(8) . . ? B8' Co3 B8 95.81(8) . . ? C2 C1 B5 111.41(14) . . ? C2 C1 B4 112.00(14) . . ? B5 C1 B4 64.29(12) . . ? C2 C1 B6 61.90(12) . . ? B5 C1 B6 62.20(12) . . ? B4 C1 B6 116.15(14) . . ? C2 C1 Co3 66.92(9) . . ? B5 C1 Co3 125.44(12) . . ? B4 C1 Co3 66.90(9) . . ? B6 C1 Co3 125.18(13) . . ? C2 C1 H1 121.4 . . ? B5 C1 H1 116.3 . . ? B4 C1 H1 118.0 . . ? B6 C1 H1 115.3 . . ? Co3 C1 H1 107.0 . . ? C1 C2 B11 111.73(14) . . ? C1 C2 B7 112.36(14) . . ? B11 C2 B7 64.12(12) . . ? C1 C2 B6 62.19(12) . . ? B11 C2 B6 61.99(13) . . ? B7 C2 B6 115.88(14) . . ? C1 C2 Co3 66.53(9) . . ? B11 C2 Co3 125.96(12) . . ? B7 C2 Co3 67.66(9) . . ? B6 C2 Co3 125.08(13) . . ? C1 C2 H2 121.3 . . ? B11 C2 H2 116.2 . . ? B7 C2 H2 117.8 . . ? B6 C2 H2 115.5 . . ? Co3 C2 H2 106.7 . . ? C1 B4 B9 102.57(14) . . ? C1 B4 B5 57.09(11) . . ? B9 B4 B5 59.20(12) . . ? C1 B4 B8 104.79(14) . . ? B9 B4 B8 59.53(12) . . ? B5 B4 B8 107.18(14) . . ? C1 B4 Co3 63.90(9) . . ? B9 B4 Co3 117.89(13) . . ? B5 B4 Co3 116.32(13) . . ? B8 B4 Co3 66.31(9) . . ? C1 B4 H4 126.5 . . ? B9 B4 H4 121.7 . . ? B5 B4 H4 121.2 . . ? B8 B4 H4 122.3 . . ? Co3 B4 H4 111.5 . . ? C1 B5 B6 59.82(12) . . ? C1 B5 B10 105.22(16) . . ? B6 B5 B10 60.24(13) . . ? C1 B5 B9 104.18(15) . . ? B6 B5 B9 108.57(16) . . ? B10 B5 B9 60.10(12) . . ? C1 B5 B4 58.61(11) . . ? B6 B5 B4 109.49(15) . . ? B10 B5 B4 108.51(15) . . ? B9 B5 B4 59.77(12) . . ? C1 B5 H5 124.7 . . ? B6 B5 H5 120.4 . . ? B10 B5 H5 122.1 . . ? B9 B5 H5 122.7 . . ? B4 B5 H5 121.0 . . ? C2 B6 C1 55.92(11) . . ? C2 B6 B11 58.24(12) . . ? C1 B6 B11 103.68(14) . . ? C2 B6 B5 103.24(15) . . ? C1 B6 B5 57.98(12) . . ? B11 B6 B5 108.52(15) . . ? C2 B6 B10 104.00(15) . . ? C1 B6 B10 103.89(15) . . ? B11 B6 B10 60.63(13) . . ? B5 B6 B10 60.32(13) . . ? C2 B6 H6 125.7 . . ? C1 B6 H6 125.6 . . ? B11 B6 H6 121.9 . . ? B5 B6 H6 122.3 . . ? B10 B6 H6 122.9 . . ? C2 B7 B12 102.98(14) . . ? C2 B7 B11 57.61(11) . . ? B12 B7 B11 59.34(12) . . ? C2 B7 B8 105.26(14) . . ? B12 B7 B8 59.86(11) . . ? B11 B7 B8 108.00(15) . . ? C2 B7 Co3 63.90(9) . . ? B12 B7 Co3 117.75(13) . . ? B11 B7 Co3 116.78(13) . . ? B8 B7 Co3 65.99(9) . . ? C2 B7 H7 126.1 . . ? B12 B7 H7 121.6 . . ? B11 B7 H7 120.6 . . ? B8 B7 H7 122.0 . . ? Co3 B7 H7 111.6 . . ? N1 B8 B12 120.91(15) . . ? N1 B8 B9 121.47(15) . . ? B12 B8 B9 60.24(12) . . ? N1 B8 B7 123.07(16) . . ? B12 B8 B7 58.77(11) . . ? B9 B8 B7 106.39(14) . . ? N1 B8 B4 124.14(16) . . ? B12 B8 B4 106.52(14) . . ? B9 B8 B4 59.21(12) . . ? B7 B8 B4 105.42(13) . . ? N1 B8 Co3 114.59(12) . . ? B12 B8 Co3 114.53(12) . . ? B9 B8 Co3 114.44(12) . . ? B7 B8 Co3 63.32(9) . . ? B4 B8 Co3 62.64(9) . . ? B5 B9 B10 59.91(13) . . ? B5 B9 B4 61.03(12) . . ? B10 B9 B4 109.36(15) . . ? B5 B9 B8 110.01(14) . . ? B10 B9 B8 109.25(15) . . ? B4 B9 B8 61.26(11) . . ? B5 B9 B12 106.72(15) . . ? B10 B9 B12 59.34(12) . . ? B4 B9 B12 107.83(14) . . ? B8 B9 B12 59.86(12) . . ? B5 B9 H9 121.4 . . ? B10 B9 H9 121.3 . . ? B4 B9 H9 120.7 . . ? B8 B9 H9 120.3 . . ? B12 B9 H9 123.0 . . ? B12 B10 B6 107.30(15) . . ? B12 B10 B5 108.02(15) . . ? B6 B10 B5 59.44(13) . . ? B12 B10 B9 60.92(12) . . ? B6 B10 B9 107.85(15) . . ? B5 B10 B9 59.99(13) . . ? B12 B10 B11 59.71(12) . . ? B6 B10 B11 59.09(13) . . ? B5 B10 B11 106.60(15) . . ? B9 B10 B11 108.17(15) . . ? B12 B10 H10 121.5 . . ? B6 B10 H10 122.4 . . ? B5 B10 H10 122.3 . . ? B9 B10 H10 121.1 . . ? B11 B10 H10 122.5 . . ? C2 B11 B6 59.77(12) . . ? C2 B11 B12 103.68(14) . . ? B6 B11 B12 108.40(16) . . ? C2 B11 B10 104.87(16) . . ? B6 B11 B10 60.27(13) . . ? B12 B11 B10 59.90(12) . . ? C2 B11 B7 58.26(11) . . ? B6 B11 B7 109.17(15) . . ? B12 B11 B7 59.61(11) . . ? B10 B11 B7 108.07(15) . . ? C2 B11 H11 125.0 . . ? B6 B11 H11 120.4 . . ? B12 B11 H11 122.9 . . ? B10 B11 H11 122.3 . . ? B7 B11 H11 121.4 . . ? B11 B12 B10 60.39(13) . . ? B11 B12 B7 61.04(12) . . ? B10 B12 B7 109.60(14) . . ? B11 B12 B8 110.57(14) . . ? B10 B12 B8 109.62(15) . . ? B7 B12 B8 61.37(11) . . ? B11 B12 B9 107.78(15) . . ? B10 B12 B9 59.74(13) . . ? B7 B12 B9 108.15(14) . . ? B8 B12 B9 59.90(12) . . ? B11 B12 H12 120.8 . . ? B10 B12 H12 121.0 . . ? B7 B12 H12 120.7 . . ? B8 B12 H12 120.1 . . ? B9 B12 H12 122.6 . . ? C2' C1' B5' 111.33(14) . . ? C2' C1' B4' 111.70(14) . . ? B5' C1' B4' 63.70(12) . . ? C2' C1' B6' 62.22(11) . . ? B5' C1' B6' 61.99(12) . . ? B4' C1' B6' 115.46(14) . . ? C2' C1' Co3 66.89(9) . . ? B5' C1' Co3 124.99(13) . . ? B4' C1' Co3 66.93(9) . . ? B6' C1' Co3 125.34(12) . . ? C2' C1' H1' 121.3 . . ? B5' C1' H1' 116.8 . . ? B4' C1' H1' 118.5 . . ? B6' C1' H1' 115.3 . . ? Co3 C1' H1' 107.0 . . ? C1' C2' B11' 111.79(14) . . ? C1' C2' B7' 112.62(14) . . ? B11' C2' B7' 63.86(12) . . ? C1' C2' B6' 62.24(11) . . ? B11' C2' B6' 61.95(12) . . ? B7' C2' B6' 115.70(14) . . ? C1' C2' Co3 66.99(9) . . ? B11' C2' Co3 125.68(12) . . ? B7' C2' Co3 67.51(9) . . ? B6' C2' Co3 125.44(12) . . ? C1' C2' H2' 120.9 . . ? B11' C2' H2' 116.5 . . ? B7' C2' H2' 118.0 . . ? B6' C2' H2' 115.5 . . ? Co3 C2' H2' 106.5 . . ? C1' B4' B9' 103.76(14) . . ? C1' B4' B5' 57.93(11) . . ? B9' B4' B5' 59.77(13) . . ? C1' B4' B8' 104.80(14) . . ? B9' B4' B8' 59.99(13) . . ? B5' B4' B8' 107.97(15) . . ? C1' B4' Co3 64.67(9) . . ? B9' B4' Co3 118.08(13) . . ? B5' B4' Co3 117.81(13) . . ? B8' B4' Co3 65.20(10) . . ? C1' B4' H4' 125.8 . . ? B9' B4' H4' 121.1 . . ? B5' B4' H4' 120.2 . . ? B8' B4' H4' 122.7 . . ? Co3 B4' H4' 111.3 . . ? C1' B5' B6' 59.98(12) . . ? C1' B5' B9' 104.30(15) . . ? B6' B5' B9' 108.53(16) . . ? C1' B5' B10' 105.29(15) . . ? B6' B5' B10' 60.19(12) . . ? B9' B5' B10' 59.98(13) . . ? C1' B5' B4' 58.37(11) . . ? B6' B5' B4' 109.38(15) . . ? B9' B5' B4' 60.03(12) . . ? B10' B5' B4' 108.48(16) . . ? C1' B5' H5' 124.7 . . ? B6' B5' H5' 120.4 . . ? B9' B5' H5' 122.6 . . ? B10' B5' H5' 122.2 . . ? B4' B5' H5' 121.1 . . ? C2' B6' C1' 55.54(10) . . ? C2' B6' B11' 58.09(11) . . ? C1' B6' B11' 103.29(14) . . ? C2' B6' B5' 102.83(14) . . ? C1' B6' B5' 58.03(11) . . ? B11' B6' B5' 108.26(16) . . ? C2' B6' B10' 103.75(15) . . ? C1' B6' B10' 104.18(14) . . ? B11' B6' B10' 60.33(12) . . ? B5' B6' B10' 60.68(13) . . ? C2' B6' H6' 126.0 . . ? C1' B6' H6' 125.7 . . ? B11' B6' H6' 122.2 . . ? B5' B6' H6' 122.3 . . ? B10' B6' H6' 122.7 . . ? C2' B7' B12' 103.51(15) . . ? C2' B7' B11' 57.84(11) . . ? B12' B7' B11' 59.61(12) . . ? C2' B7' B8' 104.67(14) . . ? B12' B7' B8' 60.41(12) . . ? B11' B7' B8' 108.20(15) . . ? C2' B7' Co3 64.21(9) . . ? B12' B7' Co3 118.09(13) . . ? B11' B7' Co3 117.33(13) . . ? B8' B7' Co3 65.14(9) . . ? C2' B7' H7' 126.1 . . ? B12' B7' H7' 121.0 . . ? B11' B7' H7' 120.3 . . ? B8' B7' H7' 122.5 . . ? Co3 B7' H7' 111.6 . . ? B12' B8' B7' 59.17(12) . . ? B12' B8' B9' 59.95(12) . . ? B7' B8' B9' 106.71(14) . . ? B12' B8' B4' 106.53(15) . . ? B7' B8' B4' 106.14(14) . . ? B9' B8' B4' 59.14(12) . . ? B12' B8' Co3 116.43(13) . . ? B7' B8' Co3 64.44(9) . . ? B9' B8' Co3 115.99(13) . . ? B4' B8' Co3 63.63(9) . . ? B12' B8' H8' 120.7 . . ? B7' B8' H8' 123.2 . . ? B9' B8' H8' 120.8 . . ? B4' B8' H8' 123.6 . . ? Co3 B8' H8' 113.2 . . ? B5' B9' B10' 60.18(13) . . ? B5' B9' B4' 60.20(12) . . ? B10' B9' B4' 108.79(15) . . ? B5' B9' B12' 107.20(15) . . ? B10' B9' B12' 59.56(12) . . ? B4' B9' B12' 107.89(15) . . ? B5' B9' B8' 109.02(15) . . ? B10' B9' B8' 108.87(15) . . ? B4' B9' B8' 60.87(12) . . ? B12' B9' B8' 59.95(12) . . ? B5' B9' H9' 121.7 . . ? B10' B9' H9' 121.3 . . ? B4' B9' H9' 121.2 . . ? B12' B9' H9' 122.5 . . ? B8' B9' H9' 120.8 . . ? B11' B10' B6' 59.30(12) . . ? B11' B10' B12' 59.87(12) . . ? B6' B10' B12' 107.68(15) . . ? B11' B10' B9' 107.79(15) . . ? B6' B10' B9' 107.58(15) . . ? B12' B10' B9' 60.64(13) . . ? B11' B10' B5' 106.24(14) . . ? B6' B10' B5' 59.14(12) . . ? B12' B10' B5' 107.77(15) . . ? B9' B10' B5' 59.84(13) . . ? B11' B10' H10' 122.5 . . ? B6' B10' H10' 122.3 . . ? B12' B10' H10' 121.4 . . ? B9' B10' H10' 121.5 . . ? B5' B10' H10' 122.6 . . ? C2' B11' B6' 59.96(12) . . ? C2' B11' B12' 103.91(14) . . ? B6' B11' B12' 108.74(16) . . ? C2' B11' B10' 105.19(15) . . ? B6' B11' B10' 60.38(12) . . ? B12' B11' B10' 60.11(13) . . ? C2' B11' B7' 58.30(11) . . ? B6' B11' B7' 109.43(14) . . ? B12' B11' B7' 59.68(12) . . ? B10' B11' B7' 108.35(15) . . ? C2' B11' H11' 124.9 . . ? B6' B11' H11' 120.2 . . ? B12' B11' H11' 122.7 . . ? B10' B11' H11' 122.1 . . ? B7' B11' H11' 121.2 . . ? B11' B12' B7' 60.71(12) . . ? B11' B12' B10' 60.02(12) . . ? B7' B12' B10' 109.11(15) . . ? B11' B12' B9' 107.26(16) . . ? B7' B12' B9' 107.81(15) . . ? B10' B12' B9' 59.80(13) . . ? B11' B12' B8' 109.07(15) . . ? B7' B12' B8' 60.41(12) . . ? B10' B12' B8' 109.19(16) . . ? B9' B12' B8' 60.10(12) . . ? B11' B12' H12' 121.6 . . ? B7' B12' H12' 121.2 . . ? B10' B12' H12' 121.1 . . ? B9' B12' H12' 122.5 . . ? B8' B12' H12' 120.8 . . ? C3 N1 B8 134.90(16) . . ? C3 N1 H1A 114.8(16) . . ? B8 N1 H1A 110.1(16) . . ? N1 C3 N2 120.28(17) . . ? N1 C3 C4 121.33(17) . . ? N2 C3 C4 118.39(16) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 N2 C5 122.90(16) . . ? C3 N2 C7 122.26(16) . . ? C5 N2 C7 114.75(15) . . ? N2 C5 C6 113.34(18) . . ? N2 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 112.50(18) . . ? N2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.379 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.054 data_11 _database_code_depnum_ccdc_archive 'CCDC 698621' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H36 B18 Co N' _chemical_formula_sum 'C18 H36 B18 Co N' _chemical_formula_weight 519.99 _chemical_compound_source 'synthesized by the authors' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.6244(2) _cell_length_b 12.4912(2) _cell_length_c 16.4535(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.3098(10) _cell_angle_gamma 90.00 _cell_volume 2687.45(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5519 _cell_measurement_theta_min 1 _cell_measurement_theta_max 26.0 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '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 38101 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.07 _reflns_number_total 10583 _reflns_number_gt 10184 _reflns_threshold_expression I>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 ? _computing_publication_material ? _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^)+(0.0349P)^2^+2.0205P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(10) _refine_ls_number_reflns 10583 _refine_ls_number_parameters 694 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.064 _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 Co13 Co -0.02134(2) -0.44298(3) -0.15698(2) 0.01691(8) Uani 1 1 d . . . C11 C -0.1069(2) -0.5796(2) -0.17573(18) 0.0219(6) Uani 1 1 d . . . H11 H -0.0996 -0.6139 -0.1127 0.026 Uiso 1 1 calc R . . C12 C -0.0125(2) -0.5839(2) -0.21761(17) 0.0221(6) Uani 1 1 d . . . H12 H 0.0612 -0.6211 -0.1849 0.026 Uiso 1 1 calc R . . B14 B -0.1803(2) -0.4672(2) -0.20403(19) 0.0215(6) Uani 1 1 d . . . H14 H -0.2227 -0.4248 -0.1659 0.026 Uiso 1 1 calc R . . B15 B -0.2204(2) -0.5963(3) -0.2482(2) 0.0242(6) Uani 1 1 d . . . H15 H -0.2869 -0.6362 -0.2361 0.029 Uiso 1 1 calc R . . B16 B -0.1134(3) -0.6712(2) -0.2544(2) 0.0239(7) Uani 1 1 d . . . H16 H -0.1096 -0.7587 -0.2463 0.029 Uiso 1 1 calc R . . B17 B -0.0120(3) -0.4741(2) -0.27961(19) 0.0209(6) Uani 1 1 d . . . H17 H 0.0556 -0.4361 -0.2912 0.025 Uiso 1 1 calc R . . B18 B -0.1233(2) -0.3993(2) -0.27549(19) 0.0193(6) Uani 1 1 d . . . B19 B -0.2334(2) -0.4842(3) -0.3156(2) 0.0248(7) Uani 1 1 d . . . H19 H -0.3087 -0.4510 -0.3490 0.030 Uiso 1 1 calc R . . B110 B -0.1909(3) -0.6088(3) -0.3464(2) 0.0246(6) Uani 1 1 d . . . H110 H -0.2383 -0.6554 -0.3999 0.030 Uiso 1 1 calc R . . B111 B -0.0550(3) -0.6035(3) -0.3233(2) 0.0264(7) Uani 1 1 d . . . H111 H -0.0130 -0.6477 -0.3608 0.032 Uiso 1 1 calc R . . B112 B -0.1294(3) -0.4882(3) -0.3620(2) 0.0238(7) Uani 1 1 d . . . H112 H -0.1371 -0.4571 -0.4260 0.029 Uiso 1 1 calc R . . C21 C 0.0763(2) -0.4834(2) -0.04202(17) 0.0214(6) Uani 1 1 d . . . H21 H 0.0763 -0.5713 -0.0379 0.026 Uiso 1 1 calc R . . C22 C -0.0213(2) -0.4134(2) -0.03493(16) 0.0214(6) Uani 1 1 d . . . H22 H -0.0902 -0.4514 -0.0257 0.026 Uiso 1 1 calc R . . B24 B 0.1379(2) -0.4258(2) -0.10783(19) 0.0218(6) Uani 1 1 d . . . H24 H 0.1795 -0.4681 -0.1466 0.026 Uiso 1 1 calc R . . B25 B 0.1884(2) -0.4222(3) 0.0052(2) 0.0255(7) Uani 1 1 d . . . H25 H 0.2600 -0.4637 0.0375 0.031 Uiso 1 1 calc R . . B26 B 0.0856(3) -0.4171(3) 0.0515(2) 0.0266(7) Uani 1 1 d . . . H26 H 0.0897 -0.4548 0.1128 0.032 Uiso 1 1 calc R . . B27 B -0.0357(2) -0.3004(2) -0.09481(19) 0.0219(6) Uani 1 1 d . . . H27 H -0.1086 -0.2600 -0.1250 0.026 Uiso 1 1 calc R . . B28 B 0.0693(2) -0.3024(2) -0.1415(2) 0.0215(6) Uani 1 1 d . . . H28 H 0.0666 -0.2623 -0.2016 0.026 Uiso 1 1 calc R . . B29 B 0.1852(2) -0.3033(2) -0.0559(2) 0.0238(6) Uani 1 1 d . . . H29 H 0.2554 -0.2661 -0.0630 0.029 Uiso 1 1 calc R . . B210 B 0.1531(3) -0.2982(3) 0.0417(2) 0.0259(7) Uani 1 1 d . . . H210 H 0.2026 -0.2569 0.0972 0.031 Uiso 1 1 calc R . . B211 B 0.0169(3) -0.2975(3) 0.0177(2) 0.0265(7) Uani 1 1 d . . . H211 H -0.0234 -0.2571 0.0584 0.032 Uiso 1 1 calc R . . B212 B 0.0774(2) -0.2260(3) -0.0475(2) 0.0242(6) Uani 1 1 d . . . H212 H 0.0773 -0.1380 -0.0488 0.029 Uiso 1 1 calc R . . N1 N -0.13460(17) -0.2742(2) -0.29684(14) 0.0219(5) Uani 1 1 d . . . C1A C -0.2460(2) -0.2393(2) -0.3196(2) 0.0292(7) Uani 1 1 d . . . H1A1 H -0.2812 -0.2696 -0.3743 0.035 Uiso 1 1 calc R . . H1A2 H -0.2769 -0.2694 -0.2783 0.035 Uiso 1 1 calc R . . C2A C -0.2639(2) -0.1204(2) -0.32337(18) 0.0250(6) Uani 1 1 d . . . C3A C -0.2590(2) -0.0622(2) -0.25019(19) 0.0299(7) Uani 1 1 d . . . H3A H -0.2444 -0.0967 -0.1981 0.036 Uiso 1 1 calc R . . C4A C -0.2759(2) 0.0471(3) -0.2550(2) 0.0352(7) Uani 1 1 d . . . H4A H -0.2715 0.0859 -0.2059 0.042 Uiso 1 1 calc R . . C5A C -0.2992(2) 0.0991(2) -0.3323(2) 0.0359(7) Uani 1 1 d . . . H5A H -0.3112 0.1725 -0.3353 0.043 Uiso 1 1 calc R . . C6A C -0.3047(2) 0.0414(3) -0.4047(2) 0.0350(7) Uani 1 1 d . . . H6A H -0.3197 0.0762 -0.4567 0.042 Uiso 1 1 calc R . . C7A C -0.2879(2) -0.0682(2) -0.40073(19) 0.0301(7) Uani 1 1 d . . . H7A H -0.2927 -0.1067 -0.4501 0.036 Uiso 1 1 calc R . . C1B C -0.0808(2) -0.2430(2) -0.36206(19) 0.0274(6) Uani 1 1 d . . . H1B1 H -0.1233 -0.2652 -0.4172 0.033 Uiso 1 1 calc R . . H1B2 H -0.0176 -0.2833 -0.3506 0.033 Uiso 1 1 calc R . . C2B C -0.0555(2) -0.1252(2) -0.36718(19) 0.0267(6) Uani 1 1 d . . . C3B C -0.0223(2) -0.0601(2) -0.2970(2) 0.0308(7) Uani 1 1 d . . . H3B H -0.0175 -0.0874 -0.2434 0.037 Uiso 1 1 calc R . . C4B C 0.0040(2) 0.0461(3) -0.3060(2) 0.0393(8) Uani 1 1 d . . . H4B H 0.0252 0.0899 -0.2586 0.047 Uiso 1 1 calc R . . C5B C -0.0014(3) 0.0865(2) -0.3854(3) 0.0431(9) Uani 1 1 d . . . H5B H 0.0154 0.1576 -0.3916 0.052 Uiso 1 1 calc R . . C6B C -0.0318(3) 0.0209(3) -0.4551(3) 0.0430(9) Uani 1 1 d . . . H6B H -0.0338 0.0475 -0.5084 0.052 Uiso 1 1 calc R . . C7B C -0.0593(2) -0.0840(2) -0.4466(2) 0.0320(7) Uani 1 1 d . . . H7B H -0.0805 -0.1274 -0.4943 0.038 Uiso 1 1 calc R . . Co23 Co 0.38502(2) 0.22591(3) -0.14808(2) 0.01743(8) Uani 1 1 d . . . C31 C 0.4421(2) 0.3633(2) -0.18378(17) 0.0216(6) Uani 1 1 d . . . H31 H 0.4942 0.3977 -0.1261 0.026 Uiso 1 1 calc R . . C32 C 0.3196(2) 0.3653(2) -0.20025(18) 0.0229(6) Uani 1 1 d . . . H32 H 0.2842 0.4017 -0.1545 0.028 Uiso 1 1 calc R . . B34 B 0.4830(2) 0.2522(2) -0.22498(19) 0.0219(6) Uani 1 1 d . . . H34 H 0.5569 0.2112 -0.2003 0.026 Uiso 1 1 calc R . . B35 B 0.4755(3) 0.3834(3) -0.2742(2) 0.0253(7) Uani 1 1 d . . . H35 H 0.5446 0.4257 -0.2788 0.030 Uiso 1 1 calc R . . B36 B 0.3722(3) 0.4541(3) -0.2551(2) 0.0260(7) Uani 1 1 d . . . H36 H 0.3740 0.5416 -0.2467 0.031 Uiso 1 1 calc R . . B37 B 0.2624(3) 0.2539(2) -0.2549(2) 0.0241(7) Uani 1 1 d . . . H37 H 0.1922 0.2143 -0.2500 0.029 Uiso 1 1 calc R . . B38 B 0.3672(3) 0.1816(3) -0.27615(19) 0.0221(6) Uani 1 1 d . . . B39 B 0.4254(3) 0.2688(3) -0.3366(2) 0.0265(7) Uani 1 1 d . . . H39 H 0.4618 0.2365 -0.3832 0.032 Uiso 1 1 calc R . . B310 B 0.3574(3) 0.3923(3) -0.3539(2) 0.0280(7) Uani 1 1 d . . . H310 H 0.3491 0.4394 -0.4120 0.034 Uiso 1 1 calc R . . B311 B 0.2581(3) 0.3845(3) -0.3036(2) 0.0282(7) Uani 1 1 d . . . H311 H 0.1852 0.4274 -0.3277 0.034 Uiso 1 1 calc R . . B312 B 0.2900(3) 0.2695(3) -0.3550(2) 0.0279(7) Uani 1 1 d . . . H312 H 0.2380 0.2376 -0.4137 0.034 Uiso 1 1 calc R . . C41 C 0.4045(2) 0.2674(2) -0.02411(17) 0.0247(6) Uani 1 1 d . . . H41 H 0.4095 0.3553 -0.0208 0.030 Uiso 1 1 calc R . . C42 C 0.4977(2) 0.1961(2) -0.03832(17) 0.0214(6) Uani 1 1 d . . . H42 H 0.5685 0.2329 -0.0448 0.026 Uiso 1 1 calc R . . B44 B 0.2884(2) 0.2118(3) -0.0693(2) 0.0257(7) Uani 1 1 d . . . H44 H 0.2162 0.2554 -0.0950 0.031 Uiso 1 1 calc R . . B45 B 0.3475(3) 0.2081(3) 0.0422(2) 0.0288(7) Uani 1 1 d . . . H45 H 0.3140 0.2508 0.0865 0.035 Uiso 1 1 calc R . . B46 B 0.4813(3) 0.2008(3) 0.0619(2) 0.0274(7) Uani 1 1 d . . . H46 H 0.5346 0.2381 0.1176 0.033 Uiso 1 1 calc R . . B47 B 0.4535(2) 0.0829(2) -0.09480(19) 0.0216(6) Uani 1 1 d . . . H47 H 0.4906 0.0413 -0.1372 0.026 Uiso 1 1 calc R . . B48 B 0.3162(2) 0.0877(2) -0.1140(2) 0.0232(6) Uani 1 1 d . . . H48 H 0.2623 0.0482 -0.1683 0.028 Uiso 1 1 calc R . . B49 B 0.2922(3) 0.0909(3) -0.0125(2) 0.0282(7) Uani 1 1 d . . . H49 H 0.2221 0.0556 -0.0033 0.034 Uiso 1 1 calc R . . B410 B 0.4103(3) 0.0834(3) 0.0677(2) 0.0269(7) Uani 1 1 d . . . H410 H 0.4167 0.0426 0.1282 0.032 Uiso 1 1 calc R . . B411 B 0.5098(3) 0.0798(3) 0.0174(2) 0.0241(7) Uani 1 1 d . . . H411 H 0.5824 0.0380 0.0454 0.029 Uiso 1 1 calc R . . B412 B 0.3937(3) 0.0105(3) -0.0284(2) 0.0244(7) Uani 1 1 d . . . H412 H 0.3904 -0.0775 -0.0298 0.029 Uiso 1 1 calc R . . N2 N 0.36208(17) 0.0571(2) -0.29825(14) 0.0219(4) Uani 1 1 d . . . C1C C 0.4409(3) 0.0270(2) -0.3441(2) 0.0325(7) Uani 1 1 d . . . H1C1 H 0.4211 0.0603 -0.3996 0.039 Uiso 1 1 calc R . . H1C2 H 0.5061 0.0576 -0.3131 0.039 Uiso 1 1 calc R . . C2C C 0.4564(2) -0.0906(2) -0.35572(19) 0.0266(6) Uani 1 1 d . . . C3C C 0.4438(2) -0.1306(3) -0.4369(2) 0.0356(7) Uani 1 1 d . . . H3C H 0.4234 -0.0851 -0.4834 0.043 Uiso 1 1 calc R . . C4C C 0.4616(3) -0.2379(3) -0.4489(2) 0.0403(8) Uani 1 1 d . . . H4C H 0.4531 -0.2639 -0.5034 0.048 Uiso 1 1 calc R . . C5C C 0.4916(3) -0.3065(3) -0.3806(2) 0.0407(8) Uani 1 1 d . . . H5C H 0.5023 -0.3787 -0.3889 0.049 Uiso 1 1 calc R . . C6C C 0.5058(2) -0.2669(3) -0.2995(2) 0.0375(7) Uani 1 1 d . . . H6C H 0.5264 -0.3126 -0.2532 0.045 Uiso 1 1 calc R . . C7C C 0.4894(2) -0.1600(2) -0.2871(2) 0.0328(7) Uani 1 1 d . . . H7C H 0.5006 -0.1338 -0.2324 0.039 Uiso 1 1 calc R . . C1D C 0.2539(2) 0.0221(2) -0.34392(19) 0.0284(6) Uani 1 1 d . . . H1D1 H 0.2074 0.0544 -0.3158 0.034 Uiso 1 1 calc R . . H1D2 H 0.2364 0.0499 -0.4013 0.034 Uiso 1 1 calc R . . C2D C 0.2365(2) -0.0974(2) -0.34803(18) 0.0247(6) Uani 1 1 d . . . C3D C 0.2056(2) -0.1462(2) -0.42599(19) 0.0299(7) Uani 1 1 d . . . H3D H 0.1954 -0.1048 -0.4746 0.036 Uiso 1 1 calc R . . C4D C 0.1893(2) -0.2555(2) -0.4336(2) 0.0354(7) Uani 1 1 d . . . H4D H 0.1680 -0.2875 -0.4867 0.042 Uiso 1 1 calc R . . C5D C 0.2051(2) -0.3162(2) -0.3609(2) 0.0347(7) Uani 1 1 d . . . H5D H 0.1966 -0.3901 -0.3652 0.042 Uiso 1 1 calc R . . C6D C 0.2332(2) -0.2690(3) -0.2827(2) 0.0324(6) Uani 1 1 d . . . H6D H 0.2423 -0.3107 -0.2343 0.039 Uiso 1 1 calc R . . C7D C 0.2479(2) -0.1596(2) -0.2753(2) 0.0311(7) Uani 1 1 d . . . H7D H 0.2654 -0.1274 -0.2222 0.037 Uiso 1 1 calc R . . H1 H -0.103(3) -0.242(3) -0.250(2) 0.033(9) Uiso 1 1 d . . . H2 H 0.372(3) 0.020(3) -0.251(2) 0.038(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 Co13 0.01697(16) 0.01564(16) 0.01764(16) -0.00062(14) 0.00408(12) -0.00007(14) C11 0.0226(13) 0.0185(13) 0.0239(14) 0.0001(11) 0.0052(11) -0.0037(11) C12 0.0233(13) 0.0174(13) 0.0254(14) -0.0006(11) 0.0066(11) 0.0000(11) B14 0.0207(14) 0.0199(15) 0.0215(14) 0.0009(11) 0.0022(11) -0.0021(11) B15 0.0231(15) 0.0222(16) 0.0250(16) 0.0026(12) 0.0029(12) -0.0041(13) B16 0.0262(16) 0.0161(15) 0.0275(16) -0.0008(12) 0.0045(13) -0.0049(12) B17 0.0268(16) 0.0176(15) 0.0189(14) -0.0017(11) 0.0077(12) -0.0009(12) B18 0.0230(15) 0.0143(13) 0.0189(14) -0.0002(11) 0.0029(12) -0.0014(12) B19 0.0220(15) 0.0219(15) 0.0255(16) 0.0020(12) -0.0016(13) -0.0040(12) B110 0.0264(16) 0.0207(14) 0.0248(15) 0.0010(12) 0.0039(12) -0.0066(12) B111 0.0346(18) 0.0188(15) 0.0278(17) -0.0041(13) 0.0119(14) -0.0046(14) B112 0.0311(17) 0.0189(14) 0.0217(16) -0.0014(12) 0.0080(13) -0.0073(13) C21 0.0196(13) 0.0217(13) 0.0205(13) -0.0002(10) 0.0021(11) 0.0031(10) C22 0.0210(13) 0.0252(15) 0.0186(13) 0.0005(10) 0.0067(10) 0.0019(11) B24 0.0188(14) 0.0223(16) 0.0226(14) -0.0021(12) 0.0034(11) 0.0030(12) B25 0.0237(15) 0.0234(17) 0.0274(16) 0.0000(13) 0.0037(12) 0.0039(13) B26 0.0251(16) 0.0316(19) 0.0206(15) -0.0032(13) 0.0023(12) -0.0007(13) B27 0.0210(15) 0.0214(16) 0.0219(15) -0.0024(12) 0.0033(12) -0.0001(12) B28 0.0200(14) 0.0191(15) 0.0251(15) -0.0015(12) 0.0058(12) -0.0017(11) B29 0.0212(15) 0.0235(16) 0.0248(15) -0.0026(12) 0.0036(12) -0.0001(12) B210 0.0291(16) 0.0238(17) 0.0223(15) -0.0061(12) 0.0028(13) 0.0007(13) B211 0.0241(16) 0.0321(19) 0.0238(16) -0.0085(13) 0.0078(12) 0.0012(13) B212 0.0245(16) 0.0202(14) 0.0256(16) -0.0045(12) 0.0036(13) 0.0007(13) N1 0.0246(11) 0.0185(11) 0.0213(11) 0.0003(10) 0.0046(9) -0.0006(11) C1A 0.0233(14) 0.0250(15) 0.0352(16) 0.0046(12) 0.0014(12) 0.0001(11) C2A 0.0209(13) 0.0211(14) 0.0303(15) 0.0013(11) 0.0029(11) 0.0003(11) C3A 0.0283(15) 0.0310(16) 0.0276(15) 0.0019(12) 0.0033(12) 0.0034(12) C4A 0.0286(15) 0.0326(16) 0.0372(16) -0.0115(15) -0.0024(12) 0.0014(14) C5A 0.0289(16) 0.0210(14) 0.054(2) 0.0013(14) 0.0045(14) 0.0011(12) C6A 0.0350(16) 0.0296(17) 0.0403(17) 0.0116(14) 0.0104(13) 0.0038(14) C7A 0.0335(16) 0.0287(15) 0.0265(15) -0.0016(12) 0.0058(12) 0.0062(13) C1B 0.0357(16) 0.0207(14) 0.0289(15) 0.0030(11) 0.0144(13) -0.0020(11) C2B 0.0226(13) 0.0211(14) 0.0363(16) 0.0043(12) 0.0083(12) -0.0006(11) C3B 0.0292(16) 0.0233(15) 0.0386(17) 0.0030(12) 0.0076(13) 0.0001(12) C4B 0.0267(15) 0.0252(16) 0.064(2) -0.0069(16) 0.0084(14) -0.0037(14) C5B 0.0306(17) 0.0179(15) 0.082(3) 0.0160(16) 0.0175(17) 0.0025(12) C6B 0.0363(18) 0.0355(18) 0.061(2) 0.0240(17) 0.0206(17) 0.0068(14) C7B 0.0299(16) 0.0277(16) 0.0395(17) 0.0068(13) 0.0116(13) 0.0001(13) Co23 0.01757(16) 0.01612(17) 0.01863(16) 0.00062(14) 0.00510(13) 0.00174(14) C31 0.0236(14) 0.0191(13) 0.0220(14) 0.0025(11) 0.0064(11) -0.0002(11) C32 0.0214(14) 0.0195(13) 0.0269(14) 0.0024(11) 0.0052(11) 0.0048(11) B34 0.0238(15) 0.0223(16) 0.0214(15) 0.0012(11) 0.0094(12) 0.0024(12) B35 0.0292(16) 0.0230(16) 0.0249(16) 0.0015(13) 0.0097(13) -0.0004(13) B36 0.0286(17) 0.0194(15) 0.0284(17) 0.0020(13) 0.0055(13) 0.0006(13) B37 0.0231(15) 0.0179(16) 0.0278(17) 0.0002(12) 0.0016(13) 0.0026(12) B38 0.0271(16) 0.0194(15) 0.0190(15) 0.0009(12) 0.0050(12) -0.0002(12) B39 0.0352(18) 0.0213(15) 0.0239(16) 0.0002(12) 0.0101(14) -0.0003(13) B310 0.0352(18) 0.0235(16) 0.0244(17) 0.0025(13) 0.0068(14) -0.0007(15) B311 0.0274(17) 0.0193(15) 0.0332(19) 0.0023(14) 0.0007(14) 0.0000(14) B312 0.0333(18) 0.0208(15) 0.0251(17) 0.0018(13) 0.0006(14) 0.0025(14) C41 0.0330(16) 0.0232(13) 0.0205(14) -0.0007(11) 0.0117(12) 0.0048(12) C42 0.0214(13) 0.0214(14) 0.0205(13) 0.0009(10) 0.0048(10) 0.0027(11) B44 0.0254(15) 0.0261(17) 0.0281(16) 0.0040(13) 0.0117(12) 0.0021(14) B45 0.0339(17) 0.0274(18) 0.0294(16) 0.0039(14) 0.0159(14) 0.0052(15) B46 0.0337(17) 0.0287(19) 0.0197(15) 0.0003(13) 0.0074(13) 0.0017(14) B47 0.0243(15) 0.0168(15) 0.0234(15) 0.0040(11) 0.0061(12) 0.0017(11) B48 0.0208(15) 0.0225(16) 0.0279(16) 0.0020(12) 0.0096(12) -0.0013(12) B49 0.0250(16) 0.0311(17) 0.0318(17) 0.0046(14) 0.0134(14) 0.0014(13) B410 0.0335(17) 0.0262(18) 0.0255(16) 0.0056(13) 0.0158(13) 0.0037(13) B411 0.0281(16) 0.0226(17) 0.0217(15) 0.0060(12) 0.0072(13) 0.0035(13) B412 0.0284(16) 0.0217(15) 0.0250(16) 0.0025(13) 0.0106(13) -0.0008(13) N2 0.0254(11) 0.0177(11) 0.0215(11) -0.0008(11) 0.0051(9) 0.0007(11) C1C 0.0353(17) 0.0263(16) 0.0395(17) -0.0013(13) 0.0167(14) -0.0015(12) C2C 0.0247(14) 0.0242(14) 0.0349(16) -0.0050(12) 0.0151(12) -0.0009(12) C3C 0.0330(16) 0.0439(19) 0.0313(16) -0.0038(14) 0.0113(13) 0.0028(14) C4C 0.0402(19) 0.0414(19) 0.0420(19) -0.0188(15) 0.0160(15) -0.0068(15) C5C 0.0316(17) 0.0276(16) 0.069(2) -0.0117(16) 0.0246(17) -0.0023(13) C6C 0.0324(16) 0.0316(16) 0.0533(19) 0.0039(16) 0.0196(14) 0.0003(15) C7C 0.0339(17) 0.0312(16) 0.0348(17) -0.0027(13) 0.0119(14) 0.0010(13) C1D 0.0281(15) 0.0221(14) 0.0296(15) -0.0023(11) -0.0006(12) 0.0001(11) C2D 0.0258(14) 0.0181(13) 0.0298(15) 0.0017(11) 0.0074(11) -0.0002(11) C3D 0.0351(16) 0.0229(15) 0.0280(15) 0.0025(12) 0.0027(13) -0.0008(12) C4D 0.0395(17) 0.0242(16) 0.0378(17) -0.0071(13) 0.0034(14) -0.0050(13) C5D 0.0322(17) 0.0173(13) 0.056(2) 0.0027(13) 0.0142(15) -0.0023(12) C6D 0.0342(16) 0.0261(14) 0.0426(17) 0.0113(14) 0.0199(13) 0.0034(14) C7D 0.0347(17) 0.0310(16) 0.0292(16) 0.0014(13) 0.0114(13) 0.0037(13) _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 Co13 C11 2.041(3) . ? Co13 C22 2.042(3) . ? Co13 C12 2.043(3) . ? Co13 C21 2.047(3) . ? Co13 B27 2.090(3) . ? Co13 B17 2.093(3) . ? Co13 B24 2.103(3) . ? Co13 B14 2.107(3) . ? Co13 B28 2.121(3) . ? Co13 B18 2.123(3) . ? C11 C12 1.621(4) . ? C11 B15 1.680(4) . ? C11 B16 1.711(4) . ? C11 B14 1.711(4) . ? C11 H11 1.1000 . ? C12 B111 1.690(4) . ? C12 B17 1.711(4) . ? C12 B16 1.725(4) . ? C12 H12 1.1000 . ? B14 B19 1.787(4) . ? B14 B15 1.791(4) . ? B14 B18 1.794(4) . ? B14 H14 1.1000 . ? B15 B16 1.759(5) . ? B15 B19 1.765(4) . ? B15 B110 1.778(5) . ? B15 H15 1.1000 . ? B16 B110 1.766(5) . ? B16 B111 1.773(5) . ? B16 H16 1.1000 . ? B17 B112 1.790(4) . ? B17 B18 1.798(4) . ? B17 B111 1.799(4) . ? B17 H17 1.1000 . ? B18 N1 1.599(4) . ? B18 B112 1.788(4) . ? B18 B19 1.803(4) . ? B19 B110 1.783(5) . ? B19 B112 1.788(5) . ? B19 H19 1.1000 . ? B110 B112 1.777(5) . ? B110 B111 1.784(5) . ? B110 H110 1.1000 . ? B111 B112 1.774(5) . ? B111 H111 1.1000 . ? B112 H112 1.1000 . ? C21 C22 1.623(4) . ? C21 B25 1.689(4) . ? C21 B24 1.704(4) . ? C21 B26 1.720(4) . ? C21 H21 1.1000 . ? C22 B211 1.692(4) . ? C22 B27 1.701(4) . ? C22 B26 1.727(4) . ? C22 H22 1.1000 . ? B24 B29 1.782(4) . ? B24 B25 1.793(4) . ? B24 B28 1.808(4) . ? B24 H24 1.1000 . ? B25 B26 1.773(5) . ? B25 B210 1.777(4) . ? B25 B29 1.787(4) . ? B25 H25 1.1000 . ? B26 B211 1.768(5) . ? B26 B210 1.778(5) . ? B26 H26 1.1000 . ? B27 B212 1.781(4) . ? B27 B211 1.788(4) . ? B27 B28 1.804(4) . ? B27 H27 1.1000 . ? B28 B212 1.794(4) . ? B28 B29 1.797(4) . ? B28 H28 1.1000 . ? B29 B210 1.779(4) . ? B29 B212 1.795(4) . ? B29 H29 1.1000 . ? B210 B212 1.782(4) . ? B210 B211 1.785(5) . ? B210 H210 1.1000 . ? B211 B212 1.767(5) . ? B211 H211 1.1000 . ? B212 H212 1.1000 . ? N1 C1B 1.511(3) . ? N1 C1A 1.522(4) . ? N1 H1 0.87(4) . ? C1A C2A 1.503(4) . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A C7A 1.385(4) . ? C2A C3A 1.392(4) . ? C3A C4A 1.382(5) . ? C3A H3A 0.9300 . ? C4A C5A 1.383(5) . ? C4A H4A 0.9300 . ? C5A C6A 1.377(5) . ? C5A H5A 0.9300 . ? C6A C7A 1.387(4) . ? C6A H6A 0.9300 . ? C7A H7A 0.9300 . ? C1B C2B 1.519(4) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C2B C3B 1.380(4) . ? C2B C7B 1.392(4) . ? C3B C4B 1.393(4) . ? C3B H3B 0.9300 . ? C4B C5B 1.382(5) . ? C4B H4B 0.9300 . ? C5B C6B 1.375(5) . ? C5B H5B 0.9300 . ? C6B C7B 1.382(4) . ? C6B H6B 0.9300 . ? C7B H7B 0.9300 . ? Co23 C32 2.032(3) . ? Co23 C31 2.038(3) . ? Co23 C41 2.048(3) . ? Co23 C42 2.050(3) . ? Co23 B37 2.086(3) . ? Co23 B47 2.090(3) . ? Co23 B44 2.098(3) . ? Co23 B34 2.107(3) . ? Co23 B48 2.114(3) . ? Co23 B38 2.126(3) . ? C31 C32 1.614(4) . ? C31 B35 1.692(4) . ? C31 B34 1.706(4) . ? C31 B36 1.715(4) . ? C31 H31 1.1000 . ? C32 B311 1.689(4) . ? C32 B36 1.709(4) . ? C32 B37 1.719(4) . ? C32 H32 1.1000 . ? B34 B39 1.795(4) . ? B34 B38 1.797(4) . ? B34 B35 1.819(4) . ? B34 H34 1.1000 . ? B35 B36 1.763(5) . ? B35 B310 1.771(5) . ? B35 B39 1.783(5) . ? B35 H35 1.1000 . ? B36 B310 1.760(5) . ? B36 B311 1.764(5) . ? B36 H36 1.1000 . ? B37 B312 1.799(5) . ? B37 B38 1.805(5) . ? B37 B311 1.811(4) . ? B37 H37 1.1000 . ? B38 N2 1.594(4) . ? B38 B312 1.796(4) . ? B38 B39 1.802(4) . ? B39 B310 1.782(5) . ? B39 B312 1.784(5) . ? B39 H39 1.1000 . ? B310 B311 1.775(5) . ? B310 B312 1.785(5) . ? B310 H310 1.1000 . ? B311 B312 1.782(5) . ? B311 H311 1.1000 . ? B312 H312 1.1000 . ? C41 C42 1.622(4) . ? C41 B45 1.679(4) . ? C41 B44 1.696(4) . ? C41 B46 1.720(4) . ? C41 H41 1.1000 . ? C42 B411 1.700(4) . ? C42 B47 1.706(4) . ? C42 B46 1.726(4) . ? C42 H42 1.1000 . ? B44 B49 1.769(5) . ? B44 B45 1.785(5) . ? B44 B48 1.801(5) . ? B44 H44 1.1000 . ? B45 B46 1.762(5) . ? B45 B410 1.770(5) . ? B45 B49 1.772(5) . ? B45 H45 1.1000 . ? B46 B411 1.769(5) . ? B46 B410 1.774(5) . ? B46 H46 1.1000 . ? B47 B412 1.782(4) . ? B47 B411 1.790(4) . ? B47 B48 1.809(4) . ? B47 H47 1.1000 . ? B48 B412 1.788(4) . ? B48 B49 1.790(5) . ? B48 H48 1.1000 . ? B49 B410 1.773(5) . ? B49 B412 1.787(5) . ? B49 H49 1.1000 . ? B410 B411 1.776(5) . ? B410 B412 1.783(4) . ? B410 H410 1.1000 . ? B411 B412 1.774(5) . ? B411 H411 1.1000 . ? B412 H412 1.1000 . ? N2 C1D 1.519(4) . ? N2 C1C 1.523(4) . ? N2 H2 0.89(4) . ? C1C C2C 1.503(4) . ? C1C H1C1 0.9700 . ? C1C H1C2 0.9700 . ? C2C C3C 1.391(4) . ? C2C C7C 1.394(4) . ? C3C C4C 1.386(5) . ? C3C H3C 0.9300 . ? C4C C5C 1.381(5) . ? C4C H4C 0.9300 . ? C5C C6C 1.384(5) . ? C5C H5C 0.9300 . ? C6C C7C 1.379(5) . ? C6C H6C 0.9300 . ? C7C H7C 0.9300 . ? C1D C2D 1.511(4) . ? C1D H1D1 0.9700 . ? C1D H1D2 0.9700 . ? C2D C3D 1.375(4) . ? C2D C7D 1.398(4) . ? C3D C4D 1.384(4) . ? C3D H3D 0.9300 . ? C4D C5D 1.381(5) . ? C4D H4D 0.9300 . ? C5D C6D 1.369(5) . ? C5D H5D 0.9300 . ? C6D C7D 1.382(5) . ? C6D H6D 0.9300 . ? C7D H7D 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Co13 C22 98.20(11) . . ? C11 Co13 C12 46.77(11) . . ? C22 Co13 C12 130.71(11) . . ? C11 Co13 C21 97.40(11) . . ? C22 Co13 C21 46.78(11) . . ? C12 Co13 C21 97.26(11) . . ? C11 Co13 B27 131.18(12) . . ? C22 Co13 B27 48.59(11) . . ? C12 Co13 B27 177.90(12) . . ? C21 Co13 B27 83.34(11) . . ? C11 Co13 B17 83.44(12) . . ? C22 Co13 B17 176.63(12) . . ? C12 Co13 B17 48.84(11) . . ? C21 Co13 B17 130.18(12) . . ? B27 Co13 B17 132.01(12) . . ? C11 Co13 B24 128.86(12) . . ? C22 Co13 B24 83.56(11) . . ? C12 Co13 B24 94.59(11) . . ? C21 Co13 B24 48.47(11) . . ? B27 Co13 B24 87.31(12) . . ? B17 Co13 B24 93.12(12) . . ? C11 Co13 B14 48.70(11) . . ? C22 Co13 B14 95.96(11) . . ? C12 Co13 B14 83.82(11) . . ? C21 Co13 B14 129.68(12) . . ? B27 Co13 B14 94.24(12) . . ? B17 Co13 B14 87.34(13) . . ? B24 Co13 B14 177.46(12) . . ? C11 Co13 B28 177.90(12) . . ? C22 Co13 B28 83.83(12) . . ? C12 Co13 B28 131.31(11) . . ? C21 Co13 B28 83.57(12) . . ? B27 Co13 B28 50.72(12) . . ? B17 Co13 B28 94.51(12) . . ? B24 Co13 B28 50.68(12) . . ? B14 Co13 B28 131.79(11) . . ? C11 Co13 B18 82.96(11) . . ? C22 Co13 B18 132.54(12) . . ? C12 Co13 B18 83.46(11) . . ? C21 Co13 B18 179.26(12) . . ? B27 Co13 B18 95.93(12) . . ? B17 Co13 B18 50.48(12) . . ? B24 Co13 B18 131.70(12) . . ? B14 Co13 B18 50.17(12) . . ? B28 Co13 B18 96.09(12) . . ? C12 C11 B15 112.1(2) . . ? C12 C11 B16 62.28(18) . . ? B15 C11 B16 62.51(18) . . ? C12 C11 B14 112.6(2) . . ? B15 C11 B14 63.74(18) . . ? B16 C11 B14 116.2(2) . . ? C12 C11 Co13 66.69(13) . . ? B15 C11 Co13 125.73(19) . . ? B16 C11 Co13 125.41(19) . . ? B14 C11 Co13 67.66(13) . . ? C12 C11 H11 121.0 . . ? B15 C11 H11 116.2 . . ? B16 C11 H11 115.1 . . ? B14 C11 H11 117.8 . . ? Co13 C11 H11 106.7 . . ? C11 C12 B111 111.1(2) . . ? C11 C12 B17 111.3(2) . . ? B111 C12 B17 63.89(17) . . ? C11 C12 B16 61.40(17) . . ? B111 C12 B16 62.54(18) . . ? B17 C12 B16 115.7(2) . . ? C11 C12 Co13 66.53(13) . . ? B111 C12 Co13 125.26(18) . . ? B17 C12 Co13 67.10(13) . . ? B16 C12 Co13 124.44(19) . . ? C11 C12 H12 122.0 . . ? B111 C12 H12 116.3 . . ? B17 C12 H12 118.3 . . ? B16 C12 H12 115.6 . . ? Co13 C12 H12 107.2 . . ? C11 B14 B19 102.6(2) . . ? C11 B14 B15 57.27(16) . . ? B19 B14 B15 59.10(17) . . ? C11 B14 B18 103.8(2) . . ? B19 B14 B18 60.47(17) . . ? B15 B14 B18 107.4(2) . . ? C11 B14 Co13 63.63(13) . . ? B19 B14 Co13 118.2(2) . . ? B15 B14 Co13 116.31(19) . . ? B18 B14 Co13 65.39(14) . . ? C11 B14 H14 126.9 . . ? B19 B14 H14 121.1 . . ? B15 B14 H14 121.1 . . ? B18 B14 H14 122.6 . . ? Co13 B14 H14 111.8 . . ? C11 B15 B16 59.61(17) . . ? C11 B15 B19 104.9(2) . . ? B16 B15 B19 108.9(2) . . ? C11 B15 B110 105.0(2) . . ? B16 B15 B110 59.91(19) . . ? B19 B15 B110 60.43(19) . . ? C11 B15 B14 58.99(16) . . ? B16 B15 B14 109.8(2) . . ? B19 B15 B14 60.35(17) . . ? B110 B15 B14 109.1(2) . . ? C11 B15 H15 124.7 . . ? B16 B15 H15 120.5 . . ? B19 B15 H15 122.1 . . ? B110 B15 H15 122.2 . . ? B14 B15 H15 120.5 . . ? C11 B16 C12 56.31(16) . . ? C11 B16 B15 57.88(17) . . ? C12 B16 B15 103.6(2) . . ? C11 B16 B110 104.2(2) . . ? C12 B16 B110 104.3(2) . . ? B15 B16 B110 60.58(19) . . ? C11 B16 B111 103.2(2) . . ? C12 B16 B111 57.77(17) . . ? B15 B16 B111 108.2(2) . . ? B110 B16 B111 60.55(19) . . ? C11 B16 H16 125.6 . . ? C12 B16 H16 125.4 . . ? B15 B16 H16 122.2 . . ? B110 B16 H16 122.6 . . ? B111 B16 H16 122.4 . . ? C12 B17 B112 102.7(2) . . ? C12 B17 B18 104.5(2) . . ? B112 B17 B18 59.77(18) . . ? C12 B17 B111 57.49(16) . . ? B112 B17 B111 59.22(18) . . ? B18 B17 B111 107.4(2) . . ? C12 B17 Co13 64.06(13) . . ? B112 B17 Co13 117.7(2) . . ? B18 B17 Co13 65.63(14) . . ? B111 B17 Co13 116.83(19) . . ? C12 B17 H17 126.4 . . ? B112 B17 H17 121.6 . . ? B18 B17 H17 122.6 . . ? B111 B17 H17 120.8 . . ? Co13 B17 H17 111.6 . . ? N1 B18 B112 116.8(2) . . ? N1 B18 B14 125.0(2) . . ? B112 B18 B14 107.2(2) . . ? N1 B18 B17 122.0(2) . . ? B112 B18 B17 59.90(17) . . ? B14 B18 B17 107.7(2) . . ? N1 B18 B19 118.4(2) . . ? B112 B18 B19 59.73(18) . . ? B14 B18 B19 59.58(17) . . ? B17 B18 B19 107.7(2) . . ? N1 B18 Co13 116.77(18) . . ? B112 B18 Co13 116.30(19) . . ? B14 B18 Co13 64.44(13) . . ? B17 B18 Co13 63.88(14) . . ? B19 B18 Co13 116.58(18) . . ? B15 B19 B110 60.17(18) . . ? B15 B19 B14 60.55(17) . . ? B110 B19 B14 109.0(2) . . ? B15 B19 B112 107.1(2) . . ? B110 B19 B112 59.69(18) . . ? B14 B19 B112 107.5(2) . . ? B15 B19 B18 108.1(2) . . ? B110 B19 B18 108.3(2) . . ? B14 B19 B18 59.94(17) . . ? B112 B19 B18 59.72(17) . . ? B15 B19 H19 121.8 . . ? B110 B19 H19 121.2 . . ? B14 B19 H19 121.3 . . ? B112 B19 H19 122.5 . . ? B18 B19 H19 121.7 . . ? B16 B110 B112 107.7(2) . . ? B16 B110 B15 59.51(19) . . ? B112 B110 B15 107.0(2) . . ? B16 B110 B19 107.8(2) . . ? B112 B110 B19 60.30(19) . . ? B15 B110 B19 59.40(19) . . ? B16 B110 B111 59.90(19) . . ? B112 B110 B111 59.74(19) . . ? B15 B110 B111 106.8(2) . . ? B19 B110 B111 107.9(2) . . ? B16 B110 H110 121.8 . . ? B112 B110 H110 121.9 . . ? B15 B110 H110 122.7 . . ? B19 B110 H110 121.6 . . ? B111 B110 H110 122.1 . . ? C12 B111 B16 59.69(17) . . ? C12 B111 B112 104.3(2) . . ? B16 B111 B112 107.6(2) . . ? C12 B111 B110 105.0(2) . . ? B16 B111 B110 59.55(19) . . ? B112 B111 B110 59.93(19) . . ? C12 B111 B17 58.62(17) . . ? B16 B111 B17 109.1(2) . . ? B112 B111 B17 60.14(18) . . ? B110 B111 B17 108.6(2) . . ? C12 B111 H111 124.6 . . ? B16 B111 H111 121.1 . . ? B112 B111 H111 122.8 . . ? B110 B111 H111 122.3 . . ? B17 B111 H111 120.9 . . ? B111 B112 B110 60.33(19) . . ? B111 B112 B18 109.0(2) . . ? B110 B112 B18 109.3(2) . . ? B111 B112 B19 108.1(2) . . ? B110 B112 B19 60.01(19) . . ? B18 B112 B19 60.55(18) . . ? B111 B112 B17 60.64(18) . . ? B110 B112 B17 109.4(2) . . ? B18 B112 B17 60.34(17) . . ? B19 B112 B17 108.7(2) . . ? B111 B112 H112 121.4 . . ? B110 B112 H112 121.0 . . ? B18 B112 H112 120.9 . . ? B19 B112 H112 121.7 . . ? B17 B112 H112 121.0 . . ? C22 C21 B25 112.1(2) . . ? C22 C21 B24 112.2(2) . . ? B25 C21 B24 63.79(18) . . ? C22 C21 B26 62.12(17) . . ? B25 C21 B26 62.66(18) . . ? B24 C21 B26 116.0(2) . . ? C22 C21 Co13 66.43(13) . . ? B25 C21 Co13 125.62(19) . . ? B24 C21 Co13 67.48(13) . . ? B26 C21 Co13 124.96(18) . . ? C22 C21 H21 121.3 . . ? B25 C21 H21 116.0 . . ? B24 C21 H21 118.0 . . ? B26 C21 H21 115.2 . . ? Co13 C21 H21 107.0 . . ? C21 C22 B211 111.0(2) . . ? C21 C22 B27 111.7(2) . . ? B211 C22 B27 63.61(18) . . ? C21 C22 B26 61.70(17) . . ? B211 C22 B26 62.28(18) . . ? B27 C22 B26 115.7(2) . . ? C21 C22 Co13 66.79(13) . . ? B211 C22 Co13 124.99(18) . . ? B27 C22 Co13 67.19(14) . . ? B26 C22 Co13 124.91(18) . . ? C21 C22 H22 121.7 . . ? B211 C22 H22 116.8 . . ? B27 C22 H22 118.3 . . ? B26 C22 H22 115.5 . . ? Co13 C22 H22 107.0 . . ? C21 B24 B29 103.5(2) . . ? C21 B24 B25 57.69(17) . . ? B29 B24 B25 59.98(17) . . ? C21 B24 B28 104.5(2) . . ? B29 B24 B28 60.07(17) . . ? B25 B24 B28 108.2(2) . . ? C21 B24 Co13 64.05(13) . . ? B29 B24 Co13 117.83(18) . . ? B25 B24 Co13 117.09(19) . . ? B28 B24 Co13 65.16(13) . . ? C21 B24 H24 126.2 . . ? B29 B24 H24 121.0 . . ? B25 B24 H24 120.2 . . ? B28 B24 H24 122.6 . . ? Co13 B24 H24 111.8 . . ? C21 B25 B26 59.53(17) . . ? C21 B25 B210 104.7(2) . . ? B26 B25 B210 60.13(18) . . ? C21 B25 B29 103.9(2) . . ? B26 B25 B29 108.3(2) . . ? B210 B25 B29 59.91(18) . . ? C21 B25 B24 58.52(17) . . ? B26 B25 B24 109.1(2) . . ? B210 B25 B24 108.1(2) . . ? B29 B25 B24 59.70(17) . . ? C21 B25 H25 124.9 . . ? B26 B25 H25 120.6 . . ? B210 B25 H25 122.4 . . ? B29 B25 H25 122.8 . . ? B24 B25 H25 121.3 . . ? C21 B26 C22 56.18(16) . . ? C21 B26 B211 103.1(2) . . ? C22 B26 B211 57.88(17) . . ? C21 B26 B25 57.81(17) . . ? C22 B26 B25 103.5(2) . . ? B211 B26 B25 107.9(2) . . ? C21 B26 B210 103.4(2) . . ? C22 B26 B210 103.9(2) . . ? B211 B26 B210 60.45(19) . . ? B25 B26 B210 60.03(18) . . ? C21 B26 H26 125.9 . . ? C22 B26 H26 125.5 . . ? B211 B26 H26 122.4 . . ? B25 B26 H26 122.4 . . ? B210 B26 H26 123.1 . . ? C22 B27 B212 103.6(2) . . ? C22 B27 B211 57.96(17) . . ? B212 B27 B211 59.37(18) . . ? C22 B27 B28 105.0(2) . . ? B212 B27 B28 60.07(17) . . ? B211 B27 B28 107.8(2) . . ? C22 B27 Co13 64.21(13) . . ? B212 B27 Co13 118.05(19) . . ? B211 B27 Co13 117.29(19) . . ? B28 B27 Co13 65.52(13) . . ? C22 B27 H27 125.8 . . ? B212 B27 H27 121.2 . . ? B211 B27 H27 120.5 . . ? B28 B27 H27 122.4 . . ? Co13 B27 H27 111.5 . . ? B212 B28 B29 59.98(17) . . ? B212 B28 B27 59.33(17) . . ? B29 B28 B27 107.1(2) . . ? B212 B28 B24 106.7(2) . . ? B29 B28 B24 59.25(16) . . ? B27 B28 B24 106.6(2) . . ? B212 B28 Co13 115.89(19) . . ? B29 B28 Co13 116.25(18) . . ? B27 B28 Co13 63.76(13) . . ? B24 B28 Co13 64.16(13) . . ? B212 B28 H28 120.8 . . ? B29 B28 H28 120.5 . . ? B27 B28 H28 123.2 . . ? B24 B28 H28 123.2 . . ? Co13 B28 H28 113.4 . . ? B210 B29 B24 108.5(2) . . ? B210 B29 B25 59.76(18) . . ? B24 B29 B25 60.32(17) . . ? B210 B29 B212 59.81(18) . . ? B24 B29 B212 107.8(2) . . ? B25 B29 B212 107.2(2) . . ? B210 B29 B28 108.8(2) . . ? B24 B29 B28 60.68(16) . . ? B25 B29 B28 108.9(2) . . ? B212 B29 B28 59.94(17) . . ? B210 B29 H29 121.5 . . ? B24 B29 H29 121.4 . . ? B25 B29 H29 121.8 . . ? B212 B29 H29 122.4 . . ? B28 B29 H29 120.9 . . ? B25 B210 B26 59.84(18) . . ? B25 B210 B29 60.34(18) . . ? B26 B210 B29 108.4(2) . . ? B25 B210 B212 108.2(2) . . ? B26 B210 B212 107.6(2) . . ? B29 B210 B212 60.53(18) . . ? B25 B210 B211 107.0(2) . . ? B26 B210 B211 59.50(19) . . ? B29 B210 B211 107.7(2) . . ? B212 B210 B211 59.39(18) . . ? B25 B210 H210 121.9 . . ? B26 B210 H210 121.8 . . ? B29 B210 H210 121.2 . . ? B212 B210 H210 121.7 . . ? B211 B210 H210 122.6 . . ? C22 B211 B212 104.5(2) . . ? C22 B211 B26 59.84(17) . . ? B212 B211 B26 108.8(2) . . ? C22 B211 B210 105.1(2) . . ? B212 B211 B210 60.22(18) . . ? B26 B211 B210 60.05(18) . . ? C22 B211 B27 58.44(16) . . ? B212 B211 B27 60.12(18) . . ? B26 B211 B27 109.4(2) . . ? B210 B211 B27 108.6(2) . . ? C22 B211 H211 124.7 . . ? B212 B211 H211 122.3 . . ? B26 B211 H211 120.5 . . ? B210 B211 H211 122.2 . . ? B27 B211 H211 121.0 . . ? B211 B212 B27 60.51(18) . . ? B211 B212 B210 60.39(19) . . ? B27 B212 B210 109.0(2) . . ? B211 B212 B28 109.2(2) . . ? B27 B212 B28 60.60(17) . . ? B210 B212 B28 108.8(2) . . ? B211 B212 B29 107.8(2) . . ? B27 B212 B29 108.2(2) . . ? B210 B212 B29 59.65(18) . . ? B28 B212 B29 60.09(17) . . ? B211 B212 H212 121.3 . . ? B27 B212 H212 121.1 . . ? B210 B212 H212 121.3 . . ? B28 B212 H212 121.0 . . ? B29 B212 H212 122.2 . . ? C1B N1 C1A 113.6(2) . . ? C1B N1 B18 111.9(2) . . ? C1A N1 B18 111.2(2) . . ? C1B N1 H1 107(2) . . ? C1A N1 H1 107(2) . . ? B18 N1 H1 105(2) . . ? C2A C1A N1 115.6(2) . . ? C2A C1A H1A1 108.4 . . ? N1 C1A H1A1 108.4 . . ? C2A C1A H1A2 108.4 . . ? N1 C1A H1A2 108.4 . . ? H1A1 C1A H1A2 107.4 . . ? C7A C2A C3A 119.3(3) . . ? C7A C2A C1A 119.8(3) . . ? C3A C2A C1A 120.9(3) . . ? C4A C3A C2A 120.0(3) . . ? C4A C3A H3A 120.0 . . ? C2A C3A H3A 120.0 . . ? C3A C4A C5A 120.6(3) . . ? C3A C4A H4A 119.7 . . ? C5A C4A H4A 119.7 . . ? C6A C5A C4A 119.5(3) . . ? C6A C5A H5A 120.3 . . ? C4A C5A H5A 120.3 . . ? C5A C6A C7A 120.5(3) . . ? C5A C6A H6A 119.7 . . ? C7A C6A H6A 119.7 . . ? C2A C7A C6A 120.1(3) . . ? C2A C7A H7A 119.9 . . ? C6A C7A H7A 119.9 . . ? N1 C1B C2B 116.9(2) . . ? N1 C1B H1B1 108.1 . . ? C2B C1B H1B1 108.1 . . ? N1 C1B H1B2 108.1 . . ? C2B C1B H1B2 108.1 . . ? H1B1 C1B H1B2 107.3 . . ? C3B C2B C7B 119.0(3) . . ? C3B C2B C1B 123.4(3) . . ? C7B C2B C1B 117.4(3) . . ? C2B C3B C4B 120.4(3) . . ? C2B C3B H3B 119.8 . . ? C4B C3B H3B 119.8 . . ? C5B C4B C3B 120.1(3) . . ? C5B C4B H4B 120.0 . . ? C3B C4B H4B 120.0 . . ? C6B C5B C4B 119.6(3) . . ? C6B C5B H5B 120.2 . . ? C4B C5B H5B 120.2 . . ? C5B C6B C7B 120.5(3) . . ? C5B C6B H6B 119.8 . . ? C7B C6B H6B 119.8 . . ? C6B C7B C2B 120.4(3) . . ? C6B C7B H7B 119.8 . . ? C2B C7B H7B 119.8 . . ? C32 Co23 C31 46.72(11) . . ? C32 Co23 C41 97.03(11) . . ? C31 Co23 C41 96.92(11) . . ? C32 Co23 C42 131.23(11) . . ? C31 Co23 C42 98.92(11) . . ? C41 Co23 C42 46.63(11) . . ? C32 Co23 B37 49.32(11) . . ? C31 Co23 B37 84.02(12) . . ? C41 Co23 B37 130.21(13) . . ? C42 Co23 B37 175.78(13) . . ? C32 Co23 B47 179.47(13) . . ? C31 Co23 B47 132.78(12) . . ? C41 Co23 B47 83.17(12) . . ? C42 Co23 B47 48.65(11) . . ? B37 Co23 B47 130.85(12) . . ? C32 Co23 B44 93.21(12) . . ? C31 Co23 B44 127.24(12) . . ? C41 Co23 B44 48.28(12) . . ? C42 Co23 B44 83.42(12) . . ? B37 Co23 B44 92.39(13) . . ? B47 Co23 B44 87.29(13) . . ? C32 Co23 B34 83.67(12) . . ? C31 Co23 B34 48.58(11) . . ? C41 Co23 B34 129.18(12) . . ? C42 Co23 B34 96.49(12) . . ? B37 Co23 B34 87.72(13) . . ? B47 Co23 B34 95.82(12) . . ? B44 Co23 B34 175.78(13) . . ? C32 Co23 B48 129.55(12) . . ? C31 Co23 B48 176.27(12) . . ? C41 Co23 B48 83.45(12) . . ? C42 Co23 B48 84.05(12) . . ? B37 Co23 B48 92.90(13) . . ? B47 Co23 B48 50.95(12) . . ? B44 Co23 B48 50.63(12) . . ? B34 Co23 B48 133.58(12) . . ? C32 Co23 B38 83.68(12) . . ? C31 Co23 B38 83.12(12) . . ? C41 Co23 B38 179.07(13) . . ? C42 Co23 B38 132.44(12) . . ? B37 Co23 B38 50.73(13) . . ? B47 Co23 B38 96.11(12) . . ? B44 Co23 B38 132.35(13) . . ? B34 Co23 B38 50.24(12) . . ? B48 Co23 B38 96.57(12) . . ? C32 C31 B35 111.8(2) . . ? C32 C31 B34 112.5(2) . . ? B35 C31 B34 64.73(18) . . ? C32 C31 B36 61.70(18) . . ? B35 C31 B36 62.32(18) . . ? B34 C31 B36 116.6(2) . . ? C32 C31 Co23 66.46(14) . . ? B35 C31 Co23 126.66(19) . . ? B34 C31 Co23 67.82(14) . . ? B36 C31 Co23 124.79(19) . . ? C32 C31 H31 121.7 . . ? B35 C31 H31 115.7 . . ? B34 C31 H31 117.2 . . ? B36 C31 H31 115.6 . . ? Co23 C31 H31 106.6 . . ? C31 C32 B311 111.6(2) . . ? C31 C32 B36 62.07(18) . . ? B311 C32 B36 62.55(19) . . ? C31 C32 B37 111.8(2) . . ? B311 C32 B37 64.20(18) . . ? B36 C32 B37 116.4(2) . . ? C31 C32 Co23 66.82(13) . . ? B311 C32 Co23 125.60(19) . . ? B36 C32 Co23 125.46(19) . . ? B37 C32 Co23 66.97(14) . . ? C31 C32 H32 121.5 . . ? B311 C32 H32 116.2 . . ? B36 C32 H32 114.9 . . ? B37 C32 H32 118.1 . . ? Co23 C32 H32 106.9 . . ? C31 B34 B39 102.4(2) . . ? C31 B34 B38 104.1(2) . . ? B39 B34 B38 60.23(18) . . ? C31 B34 B35 57.25(16) . . ? B39 B34 B35 59.12(17) . . ? B38 B34 B35 107.5(2) . . ? C31 B34 Co23 63.60(13) . . ? B39 B34 Co23 117.6(2) . . ? B38 B34 Co23 65.42(14) . . ? B35 B34 Co23 116.20(18) . . ? C31 B34 H34 126.8 . . ? B39 B34 H34 121.5 . . ? B38 B34 H34 122.5 . . ? B35 B34 H34 121.0 . . ? Co23 B34 H34 112.0 . . ? C31 B35 B36 59.50(17) . . ? C31 B35 B310 104.4(2) . . ? B36 B35 B310 59.75(19) . . ? C31 B35 B39 103.5(2) . . ? B36 B35 B39 108.1(2) . . ? B310 B35 B39 60.17(19) . . ? C31 B35 B34 58.01(16) . . ? B36 B35 B34 108.7(2) . . ? B310 B35 B34 108.2(2) . . ? B39 B35 B34 59.77(17) . . ? C31 B35 H35 125.3 . . ? B36 B35 H35 120.9 . . ? B310 B35 H35 122.4 . . ? B39 B35 H35 122.8 . . ? B34 B35 H35 121.4 . . ? C32 B36 C31 56.24(16) . . ? C32 B36 B310 104.2(2) . . ? C31 B36 B310 103.8(2) . . ? C32 B36 B35 104.0(2) . . ? C31 B36 B35 58.18(17) . . ? B310 B36 B35 60.36(19) . . ? C32 B36 B311 58.16(18) . . ? C31 B36 B311 103.5(2) . . ? B310 B36 B311 60.5(2) . . ? B35 B36 B311 108.5(2) . . ? C32 B36 H36 125.2 . . ? C31 B36 H36 125.6 . . ? B310 B36 H36 122.9 . . ? B35 B36 H36 121.9 . . ? B311 B36 H36 122.1 . . ? C32 B37 B312 102.2(2) . . ? C32 B37 B38 103.9(2) . . ? B312 B37 B38 59.79(18) . . ? C32 B37 B311 57.10(17) . . ? B312 B37 B311 59.14(19) . . ? B38 B37 B311 107.1(2) . . ? C32 B37 Co23 63.71(14) . . ? B312 B37 Co23 117.7(2) . . ? B38 B37 Co23 65.77(14) . . ? B311 B37 Co23 116.29(19) . . ? C32 B37 H37 127.0 . . ? B312 B37 H37 121.6 . . ? B38 B37 H37 122.7 . . ? B311 B37 H37 121.1 . . ? Co23 B37 H37 111.7 . . ? N2 B38 B312 116.9(2) . . ? N2 B38 B34 124.2(2) . . ? B312 B38 B34 107.3(2) . . ? N2 B38 B39 117.5(2) . . ? B312 B38 B39 59.43(19) . . ? B34 B38 B39 59.83(18) . . ? N2 B38 B37 123.1(2) . . ? B312 B38 B37 59.96(19) . . ? B34 B38 B37 107.6(2) . . ? B39 B38 B37 107.4(2) . . ? N2 B38 Co23 117.76(19) . . ? B312 B38 Co23 115.9(2) . . ? B34 B38 Co23 64.33(14) . . ? B39 B38 Co23 116.37(19) . . ? B37 B38 Co23 63.50(14) . . ? B310 B39 B35 59.59(18) . . ? B310 B39 B312 60.10(19) . . ? B35 B39 B312 107.7(2) . . ? B310 B39 B34 108.8(2) . . ? B35 B39 B34 61.12(18) . . ? B312 B39 B34 107.9(2) . . ? B310 B39 B38 108.8(2) . . ? B35 B39 B38 108.9(2) . . ? B312 B39 B38 60.12(18) . . ? B34 B39 B38 59.95(17) . . ? B310 B39 H39 121.4 . . ? B35 B39 H39 121.4 . . ? B312 B39 H39 122.0 . . ? B34 B39 H39 121.2 . . ? B38 B39 H39 121.2 . . ? B36 B310 B35 59.89(19) . . ? B36 B310 B311 59.87(19) . . ? B35 B310 B311 107.7(2) . . ? B36 B310 B39 108.2(2) . . ? B35 B310 B39 60.24(19) . . ? B311 B310 B39 108.0(2) . . ? B36 B310 B312 108.1(2) . . ? B35 B310 B312 108.1(2) . . ? B311 B310 B312 60.05(19) . . ? B39 B310 B312 60.01(19) . . ? B36 B310 H310 121.7 . . ? B35 B310 H310 121.8 . . ? B311 B310 H310 121.9 . . ? B39 B310 H310 121.6 . . ? B312 B310 H310 121.6 . . ? C32 B311 B36 59.29(18) . . ? C32 B311 B310 104.5(2) . . ? B36 B311 B310 59.65(19) . . ? C32 B311 B312 104.1(2) . . ? B36 B311 B312 108.1(2) . . ? B310 B311 B312 60.3(2) . . ? C32 B311 B37 58.71(17) . . ? B36 B311 B37 109.2(2) . . ? B310 B311 B37 108.7(2) . . ? B312 B311 B37 60.10(19) . . ? C32 B311 H311 125.1 . . ? B36 B311 H311 121.0 . . ? B310 B311 H311 122.3 . . ? B312 B311 H311 122.6 . . ? B37 B311 H311 120.8 . . ? B311 B312 B39 107.6(2) . . ? B311 B312 B310 59.7(2) . . ? B39 B312 B310 59.89(19) . . ? B311 B312 B38 108.8(2) . . ? B39 B312 B38 60.45(18) . . ? B310 B312 B38 108.9(2) . . ? B311 B312 B37 60.76(19) . . ? B39 B312 B37 108.4(2) . . ? B310 B312 B37 108.8(2) . . ? B38 B312 B37 60.25(18) . . ? B311 B312 H312 121.7 . . ? B39 B312 H312 121.9 . . ? B310 B312 H312 121.5 . . ? B38 B312 H312 121.0 . . ? B37 B312 H312 121.1 . . ? C42 C41 B45 112.0(2) . . ? C42 C41 B44 112.5(2) . . ? B45 C41 B44 63.86(19) . . ? C42 C41 B46 62.12(18) . . ? B45 C41 B46 62.45(19) . . ? B44 C41 B46 116.1(2) . . ? C42 C41 Co23 66.73(14) . . ? B45 C41 Co23 125.5(2) . . ? B44 C41 Co23 67.40(14) . . ? B46 C41 Co23 125.13(19) . . ? C42 C41 H41 121.0 . . ? B45 C41 H41 116.2 . . ? B44 C41 H41 117.9 . . ? B46 C41 H41 115.3 . . ? Co23 C41 H41 106.9 . . ? C41 C42 B411 110.6(2) . . ? C41 C42 B47 111.3(2) . . ? B411 C42 B47 63.40(17) . . ? C41 C42 B46 61.73(18) . . ? B411 C42 B46 62.16(18) . . ? B47 C42 B46 115.3(2) . . ? C41 C42 Co23 66.64(14) . . ? B411 C42 Co23 124.43(18) . . ? B47 C42 Co23 66.92(13) . . ? B46 C42 Co23 124.69(19) . . ? C41 C42 H42 121.8 . . ? B411 C42 H42 117.1 . . ? B47 C42 H42 118.6 . . ? B46 C42 H42 115.5 . . ? Co23 C42 H42 107.4 . . ? C41 B44 B49 103.4(2) . . ? C41 B44 B45 57.60(17) . . ? B49 B44 B45 59.79(19) . . ? C41 B44 B48 104.7(2) . . ? B49 B44 B48 60.19(18) . . ? B45 B44 B48 108.2(2) . . ? C41 B44 Co23 64.33(14) . . ? B49 B44 Co23 117.9(2) . . ? B45 B44 Co23 117.19(19) . . ? B48 B44 Co23 65.14(14) . . ? C41 B44 H44 126.1 . . ? B49 B44 H44 121.1 . . ? B45 B44 H44 120.3 . . ? B48 B44 H44 122.5 . . ? Co23 B44 H44 111.7 . . ? C41 B45 B46 59.91(18) . . ? C41 B45 B410 105.1(2) . . ? B46 B45 B410 60.28(19) . . ? C41 B45 B49 104.0(2) . . ? B46 B45 B49 108.7(2) . . ? B410 B45 B49 60.10(19) . . ? C41 B45 B44 58.54(18) . . ? B46 B45 B44 109.6(2) . . ? B410 B45 B44 108.3(2) . . ? B49 B45 B44 59.65(19) . . ? C41 B45 H45 124.8 . . ? B46 B45 H45 120.2 . . ? B410 B45 H45 122.2 . . ? B49 B45 H45 122.7 . . ? B44 B45 H45 121.1 . . ? C41 B46 C42 56.16(16) . . ? C41 B46 B45 57.64(18) . . ? C42 B46 B45 103.4(2) . . ? C41 B46 B411 103.1(2) . . ? C42 B46 B411 58.20(17) . . ? B45 B46 B411 107.7(2) . . ? C41 B46 B410 103.3(2) . . ? C42 B46 B410 104.0(2) . . ? B45 B46 B410 60.07(19) . . ? B411 B46 B410 60.16(18) . . ? C41 B46 H46 126.0 . . ? C42 B46 H46 125.3 . . ? B45 B46 H46 122.5 . . ? B411 B46 H46 122.4 . . ? B410 B46 H46 123.2 . . ? C42 B47 B412 103.8(2) . . ? C42 B47 B411 58.15(16) . . ? B412 B47 B411 59.56(18) . . ? C42 B47 B48 104.9(2) . . ? B412 B47 B48 59.73(17) . . ? B411 B47 B48 107.7(2) . . ? C42 B47 Co23 64.43(13) . . ? B412 B47 Co23 117.65(19) . . ? B411 B47 Co23 117.55(18) . . ? B48 B47 Co23 65.19(14) . . ? C42 B47 H47 125.6 . . ? B412 B47 H47 121.3 . . ? B411 B47 H47 120.3 . . ? B48 B47 H47 122.8 . . ? Co23 B47 H47 111.6 . . ? B412 B48 B49 59.92(18) . . ? B412 B48 B44 106.7(2) . . ? B49 B48 B44 59.02(17) . . ? B412 B48 B47 59.40(17) . . ? B49 B48 B47 106.8(2) . . ? B44 B48 B47 106.4(2) . . ? B412 B48 Co23 116.20(19) . . ? B49 B48 Co23 116.10(19) . . ? B44 B48 Co23 64.24(14) . . ? B47 B48 Co23 63.86(13) . . ? B412 B48 H48 120.6 . . ? B49 B48 H48 120.8 . . ? B44 B48 H48 123.3 . . ? B47 B48 H48 123.3 . . ? Co23 B48 H48 113.3 . . ? B44 B49 B45 60.56(18) . . ? B44 B49 B410 108.9(2) . . ? B45 B49 B410 59.90(19) . . ? B44 B49 B412 108.2(2) . . ? B45 B49 B412 107.6(2) . . ? B410 B49 B412 60.09(18) . . ? B44 B49 B48 60.79(17) . . ? B45 B49 B48 109.2(2) . . ? B410 B49 B48 109.1(2) . . ? B412 B49 B48 59.98(18) . . ? B44 B49 H49 121.1 . . ? B45 B49 H49 121.5 . . ? B410 B49 H49 121.2 . . ? B412 B49 H49 122.2 . . ? B48 B49 H49 120.8 . . ? B45 B410 B49 60.00(19) . . ? B45 B410 B46 59.65(19) . . ? B49 B410 B46 108.1(2) . . ? B45 B410 B411 107.1(2) . . ? B49 B410 B411 107.8(2) . . ? B46 B410 B411 59.79(18) . . ? B45 B410 B412 107.9(2) . . ? B49 B410 B412 60.34(19) . . ? B46 B410 B412 108.1(2) . . ? B411 B410 B412 59.81(18) . . ? B45 B410 H410 122.2 . . ? B49 B410 H410 121.5 . . ? B46 B410 H410 121.7 . . ? B411 B410 H410 122.2 . . ? B412 B410 H410 121.6 . . ? C42 B411 B46 59.64(17) . . ? C42 B411 B412 104.4(2) . . ? B46 B411 B412 108.7(2) . . ? C42 B411 B410 105.0(2) . . ? B46 B411 B410 60.05(18) . . ? B412 B411 B410 60.29(18) . . ? C42 B411 B47 58.46(16) . . ? B46 B411 B47 109.2(2) . . ? B412 B411 B47 60.00(17) . . ? B410 B411 B47 108.5(2) . . ? C42 B411 H411 124.8 . . ? B46 B411 H411 120.6 . . ? B412 B411 H411 122.4 . . ? B410 B411 H411 122.1 . . ? B47 B411 H411 121.1 . . ? B411 B412 B47 60.43(18) . . ? B411 B412 B410 59.90(18) . . ? B47 B412 B410 108.6(2) . . ? B411 B412 B49 107.3(2) . . ? B47 B412 B49 108.1(2) . . ? B410 B412 B49 59.57(19) . . ? B411 B412 B48 109.3(2) . . ? B47 B412 B48 60.87(17) . . ? B410 B412 B48 108.8(2) . . ? B49 B412 B48 60.10(18) . . ? B411 B412 H412 121.6 . . ? B47 B412 H412 121.2 . . ? B410 B412 H412 121.6 . . ? B49 B412 H412 122.4 . . ? B48 B412 H412 120.7 . . ? C1D N2 C1C 113.9(2) . . ? C1D N2 B38 111.6(2) . . ? C1C N2 B38 111.2(2) . . ? C1D N2 H2 100(2) . . ? C1C N2 H2 111(2) . . ? B38 N2 H2 109(2) . . ? C2C C1C N2 116.6(2) . . ? C2C C1C H1C1 108.1 . . ? N2 C1C H1C1 108.1 . . ? C2C C1C H1C2 108.1 . . ? N2 C1C H1C2 108.1 . . ? H1C1 C1C H1C2 107.3 . . ? C3C C2C C7C 118.6(3) . . ? C3C C2C C1C 119.3(3) . . ? C7C C2C C1C 122.0(3) . . ? C4C C3C C2C 120.3(3) . . ? C4C C3C H3C 119.8 . . ? C2C C3C H3C 119.8 . . ? C5C C4C C3C 120.5(3) . . ? C5C C4C H4C 119.7 . . ? C3C C4C H4C 119.7 . . ? C4C C5C C6C 119.5(3) . . ? C4C C5C H5C 120.3 . . ? C6C C5C H5C 120.3 . . ? C7C C6C C5C 120.2(3) . . ? C7C C6C H6C 119.9 . . ? C5C C6C H6C 119.9 . . ? C6C C7C C2C 120.8(3) . . ? C6C C7C H7C 119.6 . . ? C2C C7C H7C 119.6 . . ? C2D C1D N2 115.1(2) . . ? C2D C1D H1D1 108.5 . . ? N2 C1D H1D1 108.5 . . ? C2D C1D H1D2 108.5 . . ? N2 C1D H1D2 108.5 . . ? H1D1 C1D H1D2 107.5 . . ? C3D C2D C7D 118.9(3) . . ? C3D C2D C1D 118.9(3) . . ? C7D C2D C1D 122.2(3) . . ? C2D C3D C4D 121.4(3) . . ? C2D C3D H3D 119.3 . . ? C4D C3D H3D 119.3 . . ? C5D C4D C3D 118.8(3) . . ? C5D C4D H4D 120.6 . . ? C3D C4D H4D 120.6 . . ? C6D C5D C4D 120.7(3) . . ? C6D C5D H5D 119.6 . . ? C4D C5D H5D 119.6 . . ? C5D C6D C7D 120.3(3) . . ? C5D C6D H6D 119.8 . . ? C7D C6D H6D 119.8 . . ? C6D C7D C2D 119.7(3) . . ? C6D C7D H7D 120.2 . . ? C2D C7D H7D 120.2 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.482 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.049 #===END