Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Gibson, Vernon C.' 'Humphries, Martin J.' 'Tellmann, Kilian P.' 'White, Andrew J. P.' 'Williams, D.' _publ_contact_author_name 'Prof Vernon C. Gibson' _publ_contact_author_address ; Prof Vernon C. Gibson Chemistry Imperial College Exhibition Road London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email 'V.GIBSON@IC.AC.UK' _publ_section_title ;The Nature of the Active Species in Bis(imino)pyridyl Cobalt Ethylene Polymerisation Catalysts ; data_VG0014 _database_code_CSD 169303 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H43 N3 Cl Co' _chemical_formula_weight 576.08 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8194(14) _cell_length_b 23.121(2) _cell_length_c 15.744(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.076(13) _cell_angle_gamma 90.00 _cell_volume 3150.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 5.02 _cell_measurement_theta_max 12.51 _exptl_crystal_description 'platy rhombs' _exptl_crystal_colour Orange/brown _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.73 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method ? _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.28 _diffrn_reflns_number 4975 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.50 _reflns_number_total 4635 _reflns_number_observed 3253 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 452 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.2364P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4183 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_obs 0.0461 _refine_ls_wR_factor_all 0.1260 _refine_ls_wR_factor_obs 0.0995 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.075 _refine_ls_restrained_S_all 1.123 _refine_ls_restrained_S_obs 1.075 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co Co 0.85651(5) 0.20779(2) 0.78997(3) 0.03250(14) Uani 1 d . . Cl Cl 0.96140(13) 0.20721(5) 0.67533(6) 0.0558(3) Uani 1 d . . N1 N 0.7673(3) 0.20799(15) 0.8835(2) 0.0329(6) Uani 1 d . . C2 C 0.7391(4) 0.2594(2) 0.9211(2) 0.0373(8) Uani 1 d . . C3 C 0.6698(5) 0.2597(2) 0.9933(3) 0.0479(10) Uani 1 d . . H3A H 0.6506(5) 0.2945(2) 1.0190(3) 0.058 Uiso 1 calc R . C4 C 0.6296(5) 0.2077(2) 1.0268(2) 0.0510(9) Uani 1 d . . H4A H 0.5839(5) 0.2076(2) 1.0754(2) 0.061 Uiso 1 calc R . C5 C 0.6573(5) 0.1561(2) 0.9883(3) 0.0470(9) Uani 1 d . . H5A H 0.6297(5) 0.1212(2) 1.0105(3) 0.056 Uiso 1 calc R . C6 C 0.7268(4) 0.1566(2) 0.9161(2) 0.0357(8) Uani 1 d . . C7 C 0.7916(4) 0.3067(2) 0.8742(2) 0.0403(9) Uani 1 d . . N7 N 0.8543(3) 0.28958(14) 0.8091(2) 0.0365(6) Uani 1 d . . C8 C 0.7707(6) 0.3688(2) 0.8980(3) 0.0550(11) Uani 1 d . . H8A H 0.7208(6) 0.3704(2) 0.9471(3) 0.082 Uiso 1 d R . H8B H 0.7082(6) 0.3884(2) 0.8500(3) 0.082 Uiso 1 d R . H8C H 0.8699(6) 0.3873(2) 0.9123(3) 0.082 Uiso 1 d R . C9 C 0.7661(4) 0.1092(2) 0.8654(2) 0.0371(8) Uani 1 d . . N9 N 0.8291(3) 0.12618(13) 0.7999(2) 0.0342(6) Uani 1 d . . C10 C 0.7358(6) 0.0475(2) 0.8863(3) 0.0555(11) Uani 1 d . . H10A H 0.6267(6) 0.0418(2) 0.8817(3) 0.083 Uiso 1 d R . H10B H 0.7880(6) 0.0389(2) 0.9442(3) 0.083 Uiso 1 d R . H10C H 0.7733(6) 0.0224(2) 0.8463(3) 0.083 Uiso 1 d R . C11 C 0.9142(5) 0.3330(2) 0.7578(3) 0.0412(9) Uani 1 d . . C12 C 0.8170(5) 0.3546(2) 0.6849(3) 0.0513(10) Uani 1 d . . C13 C 0.8752(7) 0.3972(2) 0.6374(3) 0.0647(13) Uani 1 d . . H13A H 0.8116(7) 0.4128(2) 0.5889(3) 0.078 Uiso 1 calc R . C14 C 1.0239(7) 0.4166(2) 0.6609(4) 0.0684(14) Uani 1 d . . H14A H 1.0604(7) 0.4454(2) 0.6287(4) 0.082 Uiso 1 calc R . C15 C 1.1183(6) 0.3936(2) 0.7315(4) 0.0665(14) Uani 1 d . . H15A H 1.2198(6) 0.4066(2) 0.7463(4) 0.080 Uiso 1 calc R . C16 C 1.0667(5) 0.3509(2) 0.7827(3) 0.0532(11) Uani 1 d . . C17 C 0.6512(6) 0.3334(2) 0.6549(3) 0.0696(14) Uani 1 d . . H17A H 0.6306(6) 0.3040(2) 0.6959(3) 0.084 Uiso 1 calc R . C18 C 0.6260(8) 0.3061(3) 0.5662(4) 0.096(2) Uani 1 d . . H18A H 0.5207(8) 0.2936(3) 0.5501(4) 0.145 Uiso 1 calc R . H18B H 0.6936(8) 0.2735(3) 0.5672(4) 0.145 Uiso 1 calc R . H18C H 0.6478(8) 0.3339(3) 0.5248(4) 0.145 Uiso 1 calc R . C19 C 0.5361(8) 0.3834(4) 0.6563(5) 0.102(2) Uani 1 d . . H19A H 0.5533(8) 0.4004(4) 0.7129(5) 0.154 Uiso 1 calc R . H19B H 0.4325(8) 0.3687(4) 0.6421(5) 0.154 Uiso 1 calc R . H19C H 0.5509(8) 0.4121(4) 0.6146(5) 0.154 Uiso 1 calc R . C20 C 1.1744(6) 0.3258(3) 0.8599(4) 0.080(2) Uani 1 d . . H20A H 1.1112(6) 0.3060(3) 0.8957(4) 0.096 Uiso 1 calc R . C21 C 1.2731(9) 0.3710(4) 0.9170(5) 0.111(2) Uani 1 d . . H21A H 1.3385(9) 0.3519(4) 0.9646(5) 0.166 Uiso 1 calc R . H21B H 1.2069(9) 0.3978(4) 0.9388(5) 0.166 Uiso 1 calc R . H21C H 1.3358(9) 0.3914(4) 0.8834(5) 0.166 Uiso 1 calc R . C22 C 1.2820(11) 0.2814(4) 0.8323(7) 0.160(5) Uani 1 d . . H22A H 1.3492(11) 0.2662(4) 0.8826(7) 0.240 Uiso 1 calc R . H22B H 1.3426(11) 0.2994(4) 0.7951(7) 0.240 Uiso 1 calc R . H22C H 1.2222(11) 0.2506(4) 0.8017(7) 0.240 Uiso 1 calc R . C23 C 0.8721(5) 0.0836(2) 0.7421(2) 0.0373(8) Uani 1 d . . C24 C 1.0272(5) 0.0667(2) 0.7533(3) 0.0473(9) Uani 1 d . . C25 C 1.0669(6) 0.0280(2) 0.6937(3) 0.0591(12) Uani 1 d . . H25A H 1.1687(6) 0.0155(2) 0.7005(3) 0.071 Uiso 1 calc R . C26 C 0.9605(6) 0.0078(2) 0.6253(3) 0.0612(12) Uani 1 d . . H26A H 0.9908(6) -0.0175(2) 0.5859(3) 0.073 Uiso 1 calc R . C27 C 0.8078(6) 0.0249(2) 0.6147(3) 0.0559(11) Uani 1 d . . H27A H 0.7364(6) 0.0110(2) 0.5680(3) 0.067 Uiso 1 calc R . C28 C 0.7593(5) 0.0629(2) 0.6733(3) 0.0451(9) Uani 1 d . . C29 C 1.1460(6) 0.0887(2) 0.8281(3) 0.0657(13) Uani 1 d . . H29A H 1.0998(6) 0.1216(2) 0.8529(3) 0.079 Uiso 1 calc R . C30 C 1.2923(7) 0.1107(4) 0.8001(5) 0.102(2) Uani 1 d . . H30A H 1.3641(7) 0.1241(4) 0.8499(5) 0.153 Uiso 1 calc R . H30B H 1.2663(7) 0.1419(4) 0.7597(5) 0.153 Uiso 1 calc R . H30C H 1.3385(7) 0.0798(4) 0.7732(5) 0.153 Uiso 1 calc R . C31 C 1.1828(9) 0.0428(4) 0.8988(4) 0.106(2) Uani 1 d . . H31A H 1.2586(9) 0.0576(4) 0.9458(4) 0.159 Uiso 1 calc R . H31B H 1.2226(9) 0.0089(4) 0.8757(4) 0.159 Uiso 1 calc R . H31C H 1.0904(9) 0.0331(4) 0.9194(4) 0.159 Uiso 1 calc R . C32 C 0.5914(6) 0.0822(2) 0.6619(3) 0.0574(11) Uani 1 d . . H32A H 0.5700(6) 0.0877(2) 0.7202(3) 0.069 Uiso 1 calc R . C33 C 0.5639(7) 0.1405(3) 0.6162(5) 0.093(2) Uani 1 d . . H33A H 0.6374(7) 0.1681(3) 0.6450(5) 0.139 Uiso 1 calc R . H33B H 0.4611(7) 0.1536(3) 0.6177(5) 0.139 Uiso 1 calc R . H33C H 0.5758(7) 0.1364(3) 0.5572(5) 0.139 Uiso 1 calc R . C34 C 0.4766(7) 0.0376(3) 0.6177(5) 0.096(2) Uani 1 d . . H34A H 0.3736(7) 0.0524(3) 0.6126(5) 0.143 Uiso 1 calc R . H34B H 0.4870(7) 0.0027(3) 0.6514(5) 0.143 Uiso 1 calc R . H34C H 0.4968(7) 0.0294(3) 0.5611(5) 0.143 Uiso 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 Co 0.0355(2) 0.0302(2) 0.0348(2) 0.0001(2) 0.0143(2) -0.0017(2) Cl 0.0792(7) 0.0448(5) 0.0550(5) 0.0008(5) 0.0422(5) -0.0067(5) N1 0.0313(13) 0.0345(14) 0.0342(14) 0.0021(14) 0.0096(11) 0.0020(14) C2 0.035(2) 0.038(2) 0.039(2) -0.003(2) 0.009(2) 0.003(2) C3 0.045(2) 0.056(3) 0.045(2) -0.007(2) 0.016(2) 0.008(2) C4 0.056(2) 0.061(2) 0.043(2) -0.002(2) 0.027(2) 0.003(2) C5 0.053(2) 0.049(2) 0.044(2) 0.003(2) 0.020(2) -0.001(2) C6 0.035(2) 0.039(2) 0.034(2) 0.0036(15) 0.0101(14) 0.0019(15) C7 0.040(2) 0.035(2) 0.044(2) -0.001(2) 0.004(2) 0.0008(15) N7 0.0349(14) 0.0338(14) 0.041(2) 0.0013(14) 0.0085(12) -0.0031(14) C8 0.065(3) 0.037(2) 0.064(3) -0.007(2) 0.015(2) 0.004(2) C9 0.041(2) 0.034(2) 0.037(2) 0.0036(15) 0.010(2) -0.003(2) N9 0.039(2) 0.0312(14) 0.0346(14) -0.0010(13) 0.0122(12) 0.0021(13) C10 0.078(3) 0.035(2) 0.061(3) 0.008(2) 0.033(2) 0.001(2) C11 0.048(2) 0.026(2) 0.052(2) 0.000(2) 0.016(2) -0.003(2) C12 0.065(3) 0.035(2) 0.057(2) 0.001(2) 0.019(2) 0.002(2) C13 0.093(4) 0.042(2) 0.064(3) 0.008(2) 0.029(3) 0.001(2) C14 0.097(4) 0.039(2) 0.083(3) 0.008(2) 0.050(3) -0.008(2) C15 0.065(3) 0.047(3) 0.098(4) -0.012(3) 0.041(3) -0.020(2) C16 0.048(2) 0.043(2) 0.071(3) 0.000(2) 0.017(2) -0.008(2) C17 0.065(3) 0.068(3) 0.070(3) 0.024(3) -0.002(2) -0.002(2) C18 0.097(5) 0.085(5) 0.092(4) -0.005(3) -0.020(4) -0.005(3) C19 0.068(4) 0.134(6) 0.100(5) -0.003(4) 0.005(3) 0.019(4) C20 0.045(3) 0.082(4) 0.108(5) 0.018(3) 0.001(3) -0.016(3) C21 0.096(5) 0.125(6) 0.104(5) -0.029(5) 0.003(4) -0.019(5) C22 0.130(7) 0.096(6) 0.211(10) -0.040(6) -0.078(7) 0.044(5) C23 0.049(2) 0.029(2) 0.037(2) 0.0009(15) 0.017(2) 0.001(2) C24 0.055(2) 0.040(2) 0.050(2) 0.001(2) 0.019(2) 0.010(2) C25 0.067(3) 0.048(2) 0.069(3) -0.002(2) 0.031(2) 0.016(2) C26 0.085(3) 0.045(2) 0.061(3) -0.013(2) 0.031(3) 0.006(2) C27 0.075(3) 0.045(2) 0.051(2) -0.013(2) 0.019(2) -0.008(2) C28 0.059(2) 0.038(2) 0.042(2) -0.005(2) 0.018(2) -0.004(2) C29 0.051(3) 0.071(3) 0.074(3) -0.017(2) 0.010(2) 0.022(2) C30 0.055(3) 0.135(6) 0.113(5) -0.028(5) 0.012(3) -0.011(4) C31 0.120(6) 0.129(6) 0.061(3) 0.004(4) 0.001(4) 0.039(5) C32 0.059(3) 0.067(3) 0.045(2) -0.014(2) 0.009(2) -0.010(2) C33 0.056(3) 0.085(4) 0.130(6) 0.021(4) -0.003(3) 0.006(3) C34 0.069(4) 0.106(5) 0.113(5) -0.040(4) 0.021(3) -0.031(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 Co N1 1.797(3) . ? Co N9 1.912(3) . ? Co N7 1.916(3) . ? Co Cl 2.1807(10) . ? N1 C6 1.370(5) . ? N1 C2 1.373(5) . ? C2 C3 1.391(5) . ? C2 C7 1.444(5) . ? C3 C4 1.386(6) . ? C4 C5 1.383(6) . ? C5 C6 1.391(5) . ? C6 C9 1.435(5) . ? C7 N7 1.317(5) . ? C7 C8 1.504(5) . ? N7 C11 1.449(5) . ? C9 N9 1.322(5) . ? C9 C10 1.499(5) . ? N9 C23 1.440(5) . ? C11 C12 1.387(6) . ? C11 C16 1.391(6) . ? C12 C13 1.393(6) . ? C12 C17 1.528(7) . ? C13 C14 1.368(8) . ? C14 C15 1.363(8) . ? C15 C16 1.405(7) . ? C16 C20 1.507(8) . ? C17 C18 1.510(9) . ? C17 C19 1.540(9) . ? C20 C22 1.517(11) . ? C20 C21 1.534(9) . ? C23 C24 1.401(6) . ? C23 C28 1.407(6) . ? C24 C25 1.389(6) . ? C24 C29 1.506(7) . ? C25 C26 1.367(7) . ? C26 C27 1.382(7) . ? C27 C28 1.398(6) . ? C28 C32 1.524(7) . ? C29 C31 1.527(9) . ? C29 C30 1.529(8) . ? C32 C34 1.518(7) . ? C32 C33 1.525(8) . ? 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 N1 Co N9 81.58(14) . . ? N1 Co N7 81.35(14) . . ? N9 Co N7 162.92(12) . . ? N1 Co Cl 179.15(10) . . ? N9 Co Cl 98.17(9) . . ? N7 Co Cl 98.89(9) . . ? C6 N1 C2 120.6(3) . . ? C6 N1 Co 119.4(2) . . ? C2 N1 Co 120.0(3) . . ? N1 C2 C3 120.1(4) . . ? N1 C2 C7 109.5(3) . . ? C3 C2 C7 130.4(4) . . ? C4 C3 C2 119.5(4) . . ? C5 C4 C3 120.2(3) . . ? C4 C5 C6 119.6(4) . . ? N1 C6 C5 120.1(3) . . ? N1 C6 C9 110.2(3) . . ? C5 C6 C9 129.7(3) . . ? N7 C7 C2 113.2(3) . . ? N7 C7 C8 124.8(4) . . ? C2 C7 C8 121.9(4) . . ? C7 N7 C11 118.6(3) . . ? C7 N7 Co 116.0(2) . . ? C11 N7 Co 125.4(2) . . ? N9 C9 C6 113.0(3) . . ? N9 C9 C10 124.9(3) . . ? C6 C9 C10 122.1(3) . . ? C9 N9 C23 119.5(3) . . ? C9 N9 Co 115.8(2) . . ? C23 N9 Co 124.7(2) . . ? C12 C11 C16 122.5(4) . . ? C12 C11 N7 118.5(4) . . ? C16 C11 N7 119.0(4) . . ? C11 C12 C13 117.8(5) . . ? C11 C12 C17 122.9(4) . . ? C13 C12 C17 119.3(4) . . ? C14 C13 C12 121.3(5) . . ? C15 C14 C13 119.8(4) . . ? C14 C15 C16 121.8(5) . . ? C11 C16 C15 116.8(5) . . ? C11 C16 C20 122.6(4) . . ? C15 C16 C20 120.6(4) . . ? C18 C17 C12 112.4(5) . . ? C18 C17 C19 110.3(5) . . ? C12 C17 C19 110.5(5) . . ? C16 C20 C22 111.2(6) . . ? C16 C20 C21 114.2(5) . . ? C22 C20 C21 108.2(5) . . ? C24 C23 C28 122.1(3) . . ? C24 C23 N9 118.7(3) . . ? C28 C23 N9 119.1(3) . . ? C25 C24 C23 117.5(4) . . ? C25 C24 C29 121.2(4) . . ? C23 C24 C29 121.3(4) . . ? C26 C25 C24 121.9(5) . . ? C25 C26 C27 120.2(4) . . ? C26 C27 C28 121.0(4) . . ? C27 C28 C23 117.4(4) . . ? C27 C28 C32 121.4(4) . . ? C23 C28 C32 121.2(3) . . ? C24 C29 C31 110.8(5) . . ? C24 C29 C30 112.7(5) . . ? C31 C29 C30 111.6(5) . . ? C34 C32 C28 113.7(4) . . ? C34 C32 C33 110.7(5) . . ? C28 C32 C33 112.2(4) . . ? _refine_diff_density_max 0.324 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.052 data_VG0148 _database_code_CSD 169304 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H46 N5 B F15 Co' _chemical_formula_weight 1095.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7639(7) _cell_length_b 15.7966(8) _cell_length_c 15.8811(13) _cell_angle_alpha 100.546(5) _cell_angle_beta 102.862(5) _cell_angle_gamma 98.797(5) _cell_volume 2534.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.83 _cell_measurement_theta_max 24.97 _exptl_crystal_description 'blocky needles' _exptl_crystal_colour 'Ruby red' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method ? _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 3.510 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.4132 _exptl_absorpt_correction_T_max 0.6402 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8589 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 63.00 _reflns_number_total 8102 _reflns_number_observed 6057 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 396 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.3164P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7706 _refine_ls_number_parameters 668 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_obs 0.0554 _refine_ls_wR_factor_all 0.1445 _refine_ls_wR_factor_obs 0.1282 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.088 _refine_ls_restrained_S_all 1.048 _refine_ls_restrained_S_obs 1.088 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co Co 0.20530(6) 0.21491(4) 0.22502(4) 0.03111(15) Uani 1 d . . N1 N 0.2538(2) 0.3235(2) 0.2979(2) 0.0291(5) Uani 1 d . . C2 C 0.2574(3) 0.3952(2) 0.2621(2) 0.0324(6) Uani 1 d . . C3 C 0.2979(4) 0.4787(2) 0.3162(3) 0.0407(7) Uani 1 d . . H3A H 0.3019(4) 0.5291(2) 0.2914(3) 0.049 Uiso 1 calc R . C4 C 0.3326(4) 0.4877(2) 0.4077(3) 0.0437(8) Uani 1 d . . H4A H 0.3593(4) 0.5447(2) 0.4458(3) 0.052 Uiso 1 calc R . C5 C 0.3284(3) 0.4139(2) 0.4436(2) 0.0388(7) Uani 1 d . . H5A H 0.3527(3) 0.4198(2) 0.5060(2) 0.047 Uiso 1 calc R . C6 C 0.2881(3) 0.3310(2) 0.3867(2) 0.0324(6) Uani 1 d . . C7 C 0.2202(3) 0.3679(2) 0.1652(2) 0.0341(7) Uani 1 d . . N7 N 0.1935(3) 0.2828(2) 0.1363(2) 0.0328(6) Uani 1 d . . C8 C 0.2173(4) 0.4352(3) 0.1102(3) 0.0484(9) Uani 1 d . . H8A H 0.3050(4) 0.4705(3) 0.1220(3) 0.073 Uiso 1 d R . H8B H 0.1582(4) 0.4735(3) 0.1253(3) 0.073 Uiso 1 d R . H8C H 0.1867(4) 0.4057(3) 0.0473(3) 0.073 Uiso 1 d R . C9 C 0.2764(3) 0.2440(2) 0.4064(2) 0.0347(7) Uani 1 d . . N9 N 0.2353(3) 0.1803(2) 0.3356(2) 0.0325(6) Uani 1 d . . C10 C 0.3097(4) 0.2334(3) 0.5002(2) 0.0498(9) Uani 1 d . . H10A H 0.2543(4) 0.2621(3) 0.5327(2) 0.075 Uiso 1 d R . H10B H 0.4012(4) 0.2607(3) 0.5286(2) 0.075 Uiso 1 d R . H10C H 0.2954(4) 0.1708(3) 0.5006(2) 0.075 Uiso 1 d R . C11 C 0.1603(3) 0.2451(2) 0.0417(2) 0.0354(7) Uani 1 d . . C12 C 0.2602(4) 0.2183(3) 0.0066(3) 0.0488(9) Uani 1 d . . C13 C 0.2276(5) 0.1792(3) -0.0834(3) 0.0582(11) Uani 1 d . . H13A H 0.2933(5) 0.1612(3) -0.1097(3) 0.070 Uiso 1 calc R . C14 C 0.1036(5) 0.1662(3) -0.1349(3) 0.0557(11) Uani 1 d . . H14A H 0.0845(5) 0.1403(3) -0.1964(3) 0.067 Uiso 1 calc R . C15 C 0.0065(4) 0.1900(3) -0.0988(3) 0.0527(10) Uani 1 d . . H15A H -0.0799(4) 0.1793(3) -0.1351(3) 0.063 Uiso 1 calc R . C16 C 0.0335(4) 0.2298(3) -0.0091(2) 0.0438(8) Uani 1 d . . C17 C 0.3974(5) 0.2309(5) 0.0621(3) 0.073(2) Uani 1 d . . H17A H 0.3943(5) 0.2419(5) 0.1255(3) 0.087 Uiso 1 calc R . C18 C 0.4550(7) 0.1486(6) 0.0439(6) 0.116(3) Uani 1 d . . H18A H 0.3971(7) 0.0979(6) 0.0516(6) 0.174 Uiso 1 calc R . H18B H 0.5406(7) 0.1575(6) 0.0855(6) 0.174 Uiso 1 calc R . H18C H 0.4640(7) 0.1376(6) -0.0170(6) 0.174 Uiso 1 calc R . C19 C 0.4824(6) 0.3092(5) 0.0510(5) 0.104(2) Uani 1 d . . H19A H 0.5708(6) 0.3155(5) 0.0880(5) 0.156 Uiso 1 calc R . H19B H 0.4484(6) 0.3619(5) 0.0691(5) 0.156 Uiso 1 calc R . H19C H 0.4842(6) 0.3020(5) -0.0113(5) 0.156 Uiso 1 calc R . C20 C -0.0759(4) 0.2547(4) 0.0301(3) 0.0632(13) Uani 1 d . . H20A H -0.0370(4) 0.2821(4) 0.0945(3) 0.076 Uiso 1 calc R . C21 C -0.1366(6) 0.3233(6) -0.0124(4) 0.099(2) Uani 1 d . . H21A H -0.2067(6) 0.3381(6) 0.0141(4) 0.148 Uiso 1 calc R . H21B H -0.1720(6) 0.2994(6) -0.0763(4) 0.148 Uiso 1 calc R . H21C H -0.0699(6) 0.3764(6) -0.0024(4) 0.148 Uiso 1 calc R . C22 C -0.1790(6) 0.1744(6) 0.0238(5) 0.108(3) Uani 1 d . . H22A H -0.2476(6) 0.1931(6) 0.0498(5) 0.162 Uiso 1 calc R . H22B H -0.1390(6) 0.1341(6) 0.0562(5) 0.162 Uiso 1 calc R . H22C H -0.2167(6) 0.1445(6) -0.0385(5) 0.162 Uiso 1 calc R . C23 C 0.2112(3) 0.0904(2) 0.3447(2) 0.0346(7) Uani 1 d . . C24 C 0.0878(4) 0.0539(2) 0.3501(2) 0.0368(7) Uani 1 d . . C25 C 0.0658(4) -0.0333(2) 0.3582(2) 0.0409(8) Uani 1 d . . H25A H -0.0168(4) -0.0595(2) 0.3634(2) 0.049 Uiso 1 calc R . C26 C 0.1608(4) -0.0819(3) 0.3586(3) 0.0500(9) Uani 1 d . . H26A H 0.1439(4) -0.1410(3) 0.3649(3) 0.060 Uiso 1 calc R . C27 C 0.2799(4) -0.0459(3) 0.3500(4) 0.0665(14) Uani 1 d . . H27A H 0.3443(4) -0.0808(3) 0.3488(4) 0.080 Uiso 1 calc R . C28 C 0.3086(4) 0.0412(3) 0.3429(4) 0.0558(11) Uani 1 d . . C29 C -0.0212(4) 0.1043(3) 0.3463(3) 0.0485(9) Uani 1 d . . H29A H 0.0132(4) 0.1646(3) 0.3399(3) 0.058 Uiso 1 calc R . C30 C -0.1359(4) 0.0616(3) 0.2660(3) 0.0583(11) Uani 1 d . . H30A H -0.2047(4) 0.0957(3) 0.2655(3) 0.087 Uiso 1 calc R . H30B H -0.1697(4) 0.0015(3) 0.2696(3) 0.087 Uiso 1 calc R . H30C H -0.1070(4) 0.0602(3) 0.2116(3) 0.087 Uiso 1 calc R . C31 C -0.0675(5) 0.1141(4) 0.4310(4) 0.080(2) Uani 1 d . . H31A H -0.1379(5) 0.1470(4) 0.4259(4) 0.121 Uiso 1 calc R . H31B H 0.0050(5) 0.1458(4) 0.4816(4) 0.121 Uiso 1 calc R . H31C H -0.0994(5) 0.0557(4) 0.4399(4) 0.121 Uiso 1 calc R . C32 C 0.4414(5) 0.0801(3) 0.3323(6) 0.087(2) Uani 1 d . . H32A H 0.4425(5) 0.1428(3) 0.3288(6) 0.104 Uiso 1 calc R . C33 C 0.5483(6) 0.0788(5) 0.4093(8) 0.133(4) Uani 1 d . . H33A H 0.6320(6) 0.1042(5) 0.4003(8) 0.200 Uiso 1 calc R . H33B H 0.5478(6) 0.0180(5) 0.4150(8) 0.200 Uiso 1 calc R . H33C H 0.5356(6) 0.1133(5) 0.4635(8) 0.200 Uiso 1 calc R . C34 C 0.4655(7) 0.0312(5) 0.2458(6) 0.102(3) Uani 1 d . . H34A H 0.3948(7) 0.0323(5) 0.1953(6) 0.153 Uiso 1 calc R . H34B H 0.4687(7) -0.0299(5) 0.2488(6) 0.153 Uiso 1 calc R . H34C H 0.5484(7) 0.0601(5) 0.2385(6) 0.153 Uiso 1 calc R . N35 N 0.1508(4) 0.1048(2) 0.1508(2) 0.0562(9) Uani 1 d . . N36 N 0.1102(7) 0.0396(3) 0.1044(3) 0.089(2) Uani 1 d . . B B 0.8332(4) 0.5831(3) 0.2343(2) 0.0348(8) Uani 1 d . . C40 C 0.8487(4) 0.5725(3) 0.1335(2) 0.0462(8) Uani 1 d . . H40A H 0.9114(4) 0.5350(3) 0.1249(2) 0.069 Uiso 1 calc R . H40B H 0.8799(4) 0.6306(3) 0.1235(2) 0.069 Uiso 1 calc R . H40C H 0.7642(4) 0.5457(3) 0.0915(2) 0.069 Uiso 1 calc R . C41 C 0.7844(3) 0.4850(2) 0.2535(2) 0.0338(7) Uani 1 d . . C42 C 0.6791(3) 0.4571(2) 0.2850(2) 0.0377(7) Uani 1 d . . F42 F 0.6032(2) 0.5136(2) 0.3100(2) 0.0521(6) Uani 1 d . . C43 C 0.6427(3) 0.3726(3) 0.2964(3) 0.0418(8) Uani 1 d . . F43 F 0.5371(2) 0.3512(2) 0.3262(2) 0.0602(7) Uani 1 d . . C44 C 0.7153(4) 0.3114(3) 0.2781(2) 0.0419(8) Uani 1 d . . F44 F 0.6823(3) 0.2295(2) 0.2891(2) 0.0577(6) Uani 1 d . . C45 C 0.8266(4) 0.3359(3) 0.2516(2) 0.0424(8) Uani 1 d . . F45 F 0.9042(3) 0.2781(2) 0.2394(2) 0.0598(7) Uani 1 d . . C46 C 0.8578(4) 0.4201(2) 0.2396(2) 0.0374(7) Uani 1 d . . F46 F 0.9693(2) 0.4389(2) 0.2155(2) 0.0508(5) Uani 1 d . . C47 C 0.9710(4) 0.6243(2) 0.3128(2) 0.0361(7) Uani 1 d . . C48 C 0.9714(4) 0.6305(3) 0.4012(2) 0.0432(8) Uani 1 d . . F48 F 0.8575(2) 0.6108(2) 0.4230(2) 0.0577(6) Uani 1 d . . C49 C 1.0804(5) 0.6572(3) 0.4716(3) 0.0522(10) Uani 1 d . . F49 F 1.0695(3) 0.6615(3) 0.5552(2) 0.0814(10) Uani 1 d . . C50 C 1.1999(4) 0.6808(3) 0.4555(3) 0.0519(10) Uani 1 d . . F50 F 1.3087(3) 0.7053(2) 0.5226(2) 0.0758(9) Uani 1 d . . C51 C 1.2064(4) 0.6777(3) 0.3698(3) 0.0475(9) Uani 1 d . . F51 F 1.3226(3) 0.6997(2) 0.3540(2) 0.0690(7) Uani 1 d . . C52 C 1.0939(4) 0.6498(2) 0.3014(3) 0.0407(7) Uani 1 d . . F52 F 1.1120(3) 0.6475(2) 0.2198(2) 0.0632(7) Uani 1 d . . C53 C 0.7259(4) 0.6473(2) 0.2408(2) 0.0388(7) Uani 1 d . . C54 C 0.7517(4) 0.7346(2) 0.2867(2) 0.0403(7) Uani 1 d . . F54 F 0.8717(2) 0.77432(14) 0.3385(2) 0.0489(5) Uani 1 d . . C55 C 0.6599(4) 0.7879(3) 0.2846(3) 0.0488(9) Uani 1 d . . F55 F 0.6943(3) 0.8718(2) 0.3316(2) 0.0666(7) Uani 1 d . . C56 C 0.5365(4) 0.7549(3) 0.2342(4) 0.0570(11) Uani 1 d . . F56 F 0.4443(3) 0.8050(2) 0.2304(3) 0.0854(11) Uani 1 d . . C57 C 0.5039(4) 0.6693(3) 0.1865(4) 0.0589(12) Uani 1 d . . F57 F 0.3818(3) 0.6354(2) 0.1360(3) 0.0874(11) Uani 1 d . . C58 C 0.5987(4) 0.6195(3) 0.1905(3) 0.0469(9) Uani 1 d . . F58 F 0.5586(3) 0.5360(2) 0.1400(2) 0.0608(7) Uani 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 Co 0.0383(3) 0.0322(3) 0.0256(3) 0.0089(2) 0.0098(2) 0.0101(2) N1 0.0266(12) 0.0351(13) 0.0300(13) 0.0129(10) 0.0101(10) 0.0086(10) C2 0.0302(15) 0.036(2) 0.035(2) 0.0123(13) 0.0117(13) 0.0091(12) C3 0.046(2) 0.033(2) 0.045(2) 0.0107(14) 0.012(2) 0.0091(14) C4 0.045(2) 0.039(2) 0.044(2) 0.0038(15) 0.011(2) 0.0075(15) C5 0.040(2) 0.045(2) 0.030(2) 0.0047(14) 0.0091(13) 0.0075(14) C6 0.0310(15) 0.039(2) 0.029(2) 0.0077(13) 0.0092(12) 0.0075(12) C7 0.033(2) 0.043(2) 0.031(2) 0.0147(13) 0.0105(12) 0.0097(13) N7 0.0323(13) 0.0406(15) 0.0285(14) 0.0098(11) 0.0095(10) 0.0111(11) C8 0.062(2) 0.051(2) 0.041(2) 0.025(2) 0.017(2) 0.014(2) C9 0.036(2) 0.041(2) 0.031(2) 0.0136(13) 0.0101(13) 0.0125(13) N9 0.0326(13) 0.0358(14) 0.0332(14) 0.0126(11) 0.0097(11) 0.0121(11) C10 0.065(2) 0.057(2) 0.030(2) 0.016(2) 0.010(2) 0.012(2) C11 0.039(2) 0.041(2) 0.028(2) 0.0119(13) 0.0097(13) 0.0076(14) C12 0.048(2) 0.073(3) 0.036(2) 0.018(2) 0.018(2) 0.024(2) C13 0.073(3) 0.076(3) 0.035(2) 0.012(2) 0.021(2) 0.032(2) C14 0.079(3) 0.057(2) 0.027(2) 0.004(2) 0.013(2) 0.010(2) C15 0.048(2) 0.070(3) 0.036(2) 0.016(2) 0.007(2) 0.001(2) C16 0.038(2) 0.064(2) 0.034(2) 0.019(2) 0.0112(15) 0.011(2) C17 0.046(2) 0.143(5) 0.037(2) 0.017(3) 0.017(2) 0.038(3) C18 0.074(4) 0.164(8) 0.142(7) 0.067(6) 0.036(4) 0.070(5) C19 0.051(3) 0.129(6) 0.099(5) -0.006(4) -0.009(3) 0.001(3) C20 0.038(2) 0.115(4) 0.045(2) 0.024(2) 0.014(2) 0.026(2) C21 0.072(4) 0.165(7) 0.077(4) 0.026(4) 0.021(3) 0.074(4) C22 0.051(3) 0.167(8) 0.117(6) 0.050(5) 0.037(3) 0.005(4) C23 0.039(2) 0.037(2) 0.032(2) 0.0144(13) 0.0107(13) 0.0116(13) C24 0.039(2) 0.036(2) 0.035(2) 0.0050(13) 0.0094(14) 0.0088(14) C25 0.039(2) 0.038(2) 0.043(2) 0.0099(14) 0.0101(15) 0.0022(14) C26 0.051(2) 0.039(2) 0.064(2) 0.024(2) 0.014(2) 0.009(2) C27 0.045(2) 0.050(2) 0.117(4) 0.042(3) 0.022(2) 0.018(2) C28 0.040(2) 0.046(2) 0.096(3) 0.036(2) 0.027(2) 0.016(2) C29 0.039(2) 0.037(2) 0.070(3) 0.008(2) 0.017(2) 0.0106(15) C30 0.045(2) 0.067(3) 0.066(3) 0.017(2) 0.012(2) 0.021(2) C31 0.062(3) 0.095(4) 0.074(3) -0.020(3) 0.022(3) 0.021(3) C32 0.054(3) 0.052(3) 0.180(7) 0.050(4) 0.054(4) 0.022(2) C33 0.040(3) 0.101(5) 0.252(13) 0.059(7) 0.014(5) 0.003(3) C34 0.083(4) 0.103(5) 0.160(8) 0.062(5) 0.075(5) 0.035(4) N35 0.096(3) 0.038(2) 0.036(2) 0.0090(15) 0.018(2) 0.014(2) N36 0.149(5) 0.047(2) 0.058(3) 0.000(2) 0.024(3) 0.006(3) B 0.037(2) 0.040(2) 0.030(2) 0.0125(14) 0.0100(15) 0.0084(15) C40 0.060(2) 0.048(2) 0.032(2) 0.0136(15) 0.012(2) 0.009(2) C41 0.035(2) 0.039(2) 0.0295(15) 0.0120(13) 0.0075(13) 0.0099(13) C42 0.034(2) 0.044(2) 0.043(2) 0.0172(14) 0.0138(14) 0.0143(14) F42 0.0454(12) 0.0566(13) 0.075(2) 0.0336(12) 0.0314(11) 0.0261(10) C43 0.033(2) 0.051(2) 0.047(2) 0.022(2) 0.0120(15) 0.0082(15) F43 0.0416(12) 0.0646(15) 0.092(2) 0.0435(14) 0.0283(12) 0.0144(11) C44 0.047(2) 0.041(2) 0.040(2) 0.0186(14) 0.010(2) 0.0071(15) F44 0.073(2) 0.0414(12) 0.069(2) 0.0260(11) 0.0247(13) 0.0139(11) C45 0.051(2) 0.047(2) 0.038(2) 0.0151(15) 0.018(2) 0.021(2) F45 0.084(2) 0.0566(14) 0.065(2) 0.0286(12) 0.0430(14) 0.0410(13) C46 0.040(2) 0.044(2) 0.036(2) 0.0147(14) 0.0159(14) 0.0145(14) F46 0.0514(13) 0.0584(13) 0.0586(14) 0.0227(11) 0.0322(11) 0.0209(11) C47 0.040(2) 0.038(2) 0.033(2) 0.0108(13) 0.0111(14) 0.0097(14) C48 0.044(2) 0.052(2) 0.035(2) 0.013(2) 0.010(2) 0.011(2) F48 0.0504(13) 0.087(2) 0.0382(12) 0.0136(11) 0.0203(10) 0.0095(12) C49 0.060(3) 0.060(2) 0.032(2) 0.006(2) 0.005(2) 0.014(2) F49 0.085(2) 0.118(3) 0.0321(13) 0.0137(14) 0.0043(13) 0.013(2) C50 0.048(2) 0.047(2) 0.050(2) 0.003(2) -0.003(2) 0.012(2) F50 0.056(2) 0.082(2) 0.065(2) 0.0047(15) -0.0173(14) 0.0064(14) C51 0.037(2) 0.042(2) 0.062(2) 0.010(2) 0.010(2) 0.0076(15) F51 0.0415(13) 0.071(2) 0.089(2) 0.0126(15) 0.0174(13) 0.0000(12) C52 0.042(2) 0.043(2) 0.041(2) 0.0108(14) 0.0149(15) 0.0099(15) F52 0.0521(14) 0.090(2) 0.0518(14) 0.0221(13) 0.0253(11) 0.0035(13) C53 0.045(2) 0.041(2) 0.036(2) 0.0185(14) 0.0109(14) 0.0112(15) C54 0.045(2) 0.042(2) 0.039(2) 0.0173(15) 0.0140(15) 0.0101(15) F54 0.0509(13) 0.0415(11) 0.0501(12) 0.0087(9) 0.0075(10) 0.0073(9) C55 0.062(2) 0.040(2) 0.055(2) 0.021(2) 0.024(2) 0.016(2) F55 0.086(2) 0.0415(12) 0.081(2) 0.0163(12) 0.030(2) 0.0243(13) C56 0.054(2) 0.053(2) 0.082(3) 0.037(2) 0.025(2) 0.026(2) F56 0.064(2) 0.074(2) 0.141(3) 0.050(2) 0.031(2) 0.042(2) C57 0.041(2) 0.057(2) 0.083(3) 0.037(2) 0.005(2) 0.013(2) F57 0.0462(15) 0.069(2) 0.138(3) 0.041(2) -0.012(2) 0.0148(13) C58 0.047(2) 0.036(2) 0.055(2) 0.018(2) 0.001(2) 0.008(2) F58 0.0535(14) 0.0471(13) 0.068(2) 0.0125(11) -0.0110(12) 0.0084(10) _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 Co N1 1.812(3) . ? Co N35 1.841(3) . ? Co N9 1.908(3) . ? Co N7 1.915(3) . ? N1 C6 1.354(4) . ? N1 C2 1.356(4) . ? C2 C3 1.383(5) . ? C2 C7 1.465(5) . ? C3 C4 1.392(6) . ? C4 C5 1.388(6) . ? C5 C6 1.391(5) . ? C6 C9 1.459(5) . ? C7 N7 1.303(5) . ? C7 C8 1.493(5) . ? N7 C11 1.452(4) . ? C9 N9 1.303(5) . ? C9 C10 1.499(5) . ? N9 C23 1.444(4) . ? C11 C16 1.383(5) . ? C11 C12 1.402(5) . ? C12 C13 1.392(6) . ? C12 C17 1.504(6) . ? C13 C14 1.365(7) . ? C14 C15 1.368(7) . ? C15 C16 1.393(6) . ? C16 C20 1.519(5) . ? C17 C19 1.484(10) . ? C17 C18 1.532(9) . ? C20 C22 1.523(9) . ? C20 C21 1.533(8) . ? C23 C24 1.393(5) . ? C23 C28 1.399(5) . ? C24 C25 1.396(5) . ? C24 C29 1.512(5) . ? C25 C26 1.369(6) . ? C26 C27 1.368(6) . ? C27 C28 1.394(6) . ? C28 C32 1.524(6) . ? C29 C31 1.526(7) . ? C29 C30 1.528(6) . ? C32 C33 1.487(11) . ? C32 C34 1.543(10) . ? N35 N36 1.112(6) . ? B C40 1.627(5) . ? B C53 1.657(5) . ? B C47 1.662(5) . ? B C41 1.663(5) . ? C41 C42 1.382(5) . ? C41 C46 1.403(5) . ? C42 F42 1.364(4) . ? C42 C43 1.389(5) . ? C43 F43 1.346(4) . ? C43 C44 1.363(6) . ? C44 F44 1.342(4) . ? C44 C45 1.380(6) . ? C45 F45 1.345(4) . ? C45 C46 1.379(5) . ? C46 F46 1.347(4) . ? C47 C52 1.384(5) . ? C47 C48 1.388(5) . ? C48 F48 1.354(5) . ? C48 C49 1.377(6) . ? C49 F49 1.348(5) . ? C49 C50 1.375(7) . ? C50 F50 1.346(5) . ? C50 C51 1.371(7) . ? C51 F51 1.336(5) . ? C51 C52 1.384(6) . ? C52 F52 1.348(5) . ? C53 C58 1.381(6) . ? C53 C54 1.392(5) . ? C54 F54 1.352(5) . ? C54 C55 1.392(6) . ? C55 F55 1.348(5) . ? C55 C56 1.355(7) . ? C56 F56 1.359(5) . ? C56 C57 1.374(7) . ? C57 F57 1.347(5) . ? C57 C58 1.379(6) . ? C58 F58 1.361(5) . ? 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 N1 Co N35 178.3(2) . . ? N1 Co N9 81.68(12) . . ? N35 Co N9 98.44(14) . . ? N1 Co N7 81.67(12) . . ? N35 Co N7 98.23(14) . . ? N9 Co N7 163.31(12) . . ? C6 N1 C2 121.6(3) . . ? C6 N1 Co 119.2(2) . . ? C2 N1 Co 119.2(2) . . ? N1 C2 C3 120.3(3) . . ? N1 C2 C7 110.0(3) . . ? C3 C2 C7 129.6(3) . . ? C2 C3 C4 118.8(3) . . ? C5 C4 C3 120.4(3) . . ? C4 C5 C6 118.9(3) . . ? N1 C6 C5 120.0(3) . . ? N1 C6 C9 109.9(3) . . ? C5 C6 C9 130.1(3) . . ? N7 C7 C2 112.9(3) . . ? N7 C7 C8 126.7(3) . . ? C2 C7 C8 120.3(3) . . ? C7 N7 C11 119.9(3) . . ? C7 N7 Co 116.1(2) . . ? C11 N7 Co 124.0(2) . . ? N9 C9 C6 113.2(3) . . ? N9 C9 C10 125.9(3) . . ? C6 C9 C10 120.9(3) . . ? C9 N9 C23 119.5(3) . . ? C9 N9 Co 116.0(2) . . ? C23 N9 Co 124.4(2) . . ? C16 C11 C12 122.0(3) . . ? C16 C11 N7 121.0(3) . . ? C12 C11 N7 116.8(3) . . ? C13 C12 C11 117.0(4) . . ? C13 C12 C17 120.4(4) . . ? C11 C12 C17 122.6(4) . . ? C14 C13 C12 121.5(4) . . ? C13 C14 C15 120.7(4) . . ? C14 C15 C16 120.4(4) . . ? C11 C16 C15 118.4(4) . . ? C11 C16 C20 121.9(3) . . ? C15 C16 C20 119.7(4) . . ? C19 C17 C12 111.6(5) . . ? C19 C17 C18 111.1(5) . . ? C12 C17 C18 112.2(5) . . ? C16 C20 C22 111.9(5) . . ? C16 C20 C21 111.3(4) . . ? C22 C20 C21 111.2(5) . . ? C24 C23 C28 122.0(3) . . ? C24 C23 N9 118.2(3) . . ? C28 C23 N9 119.8(3) . . ? C23 C24 C25 117.5(3) . . ? C23 C24 C29 122.7(3) . . ? C25 C24 C29 119.8(3) . . ? C26 C25 C24 121.4(4) . . ? C27 C26 C25 120.2(4) . . ? C26 C27 C28 121.2(4) . . ? C27 C28 C23 117.7(4) . . ? C27 C28 C32 120.5(4) . . ? C23 C28 C32 121.8(4) . . ? C24 C29 C31 112.0(4) . . ? C24 C29 C30 111.5(3) . . ? C31 C29 C30 109.9(4) . . ? C33 C32 C28 111.7(6) . . ? C33 C32 C34 109.9(6) . . ? C28 C32 C34 111.2(5) . . ? N36 N35 Co 175.4(5) . . ? C40 B C53 104.9(3) . . ? C40 B C47 114.6(3) . . ? C53 B C47 111.2(3) . . ? C40 B C41 110.2(3) . . ? C53 B C41 112.7(3) . . ? C47 B C41 103.5(3) . . ? C42 C41 C46 112.7(3) . . ? C42 C41 B 128.4(3) . . ? C46 C41 B 118.8(3) . . ? F42 C42 C41 121.1(3) . . ? F42 C42 C43 114.3(3) . . ? C41 C42 C43 124.6(3) . . ? F43 C43 C44 120.0(3) . . ? F43 C43 C42 120.3(3) . . ? C44 C43 C42 119.7(3) . . ? F44 C44 C43 120.7(4) . . ? F44 C44 C45 120.2(4) . . ? C43 C44 C45 119.0(3) . . ? F45 C45 C46 120.9(4) . . ? F45 C45 C44 119.8(4) . . ? C46 C45 C44 119.3(3) . . ? F46 C46 C45 115.4(3) . . ? F46 C46 C41 120.1(3) . . ? C45 C46 C41 124.5(3) . . ? C52 C47 C48 112.7(3) . . ? C52 C47 B 127.4(3) . . ? C48 C47 B 119.7(3) . . ? F48 C48 C49 115.3(4) . . ? F48 C48 C47 119.5(3) . . ? C49 C48 C47 125.2(4) . . ? F49 C49 C50 120.6(4) . . ? F49 C49 C48 120.3(4) . . ? C50 C49 C48 119.1(4) . . ? F50 C50 C51 120.5(4) . . ? F50 C50 C49 120.6(4) . . ? C51 C50 C49 118.8(4) . . ? F51 C51 C50 118.9(4) . . ? F51 C51 C52 121.4(4) . . ? C50 C51 C52 119.7(4) . . ? F52 C52 C47 120.9(3) . . ? F52 C52 C51 114.7(3) . . ? C47 C52 C51 124.4(4) . . ? C58 C53 C54 112.3(3) . . ? C58 C53 B 120.8(3) . . ? C54 C53 B 126.6(3) . . ? F54 C54 C55 114.5(3) . . ? F54 C54 C53 121.1(3) . . ? C55 C54 C53 124.4(4) . . ? F55 C55 C56 120.6(4) . . ? F55 C55 C54 120.0(4) . . ? C56 C55 C54 119.4(4) . . ? C55 C56 F56 121.1(4) . . ? C55 C56 C57 119.6(4) . . ? F56 C56 C57 119.4(4) . . ? F57 C57 C56 120.4(4) . . ? F57 C57 C58 120.9(5) . . ? C56 C57 C58 118.7(4) . . ? F58 C58 C57 114.8(4) . . ? F58 C58 C53 119.6(4) . . ? C57 C58 C53 125.6(4) . . ? _refine_diff_density_max 0.484 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.056