# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Colette Boskovic' 'Brendan F. Abrahams' 'Boujemaa Moubaraki' 'Yanyan Mulyana' 'Keith Murray' 'Giordano Poneti' 'Lorenzo Sorace' _publ_contact_author_name 'Colette Boskovic' _publ_contact_author_email C.BOSKOVIC@UNIMELB.EDU.AU _publ_section_title ; Solvation effects on the valence tautomeric transition of a cobalt complex in the solid state ; # Attachment 'Co_complete.cif' data_compound_1_py_130k _database_code_depnum_ccdc_archive 'CCDC 744065' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H105 Co2 N5 O8' _chemical_formula_weight 1394.63 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.710(2) _cell_length_b 18.689(2) _cell_length_c 12.537(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.425(2) _cell_angle_gamma 90.00 _cell_volume 3714.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 3.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2878 _exptl_absorpt_correction_T_max 0.5055 _exptl_absorpt_process_details SADABS _exptl_special_details ; Crystals were weakly diffracting and as a result data was only collected to a theta angle of 51.5. ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7679 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 51.47 _reflns_number_total 3968 _reflns_number_gt 2908 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The non-coordinated pyridine molecule is disordered across a centre of symmetry. Two opposing atoms in the pyridine molecule were tentatively assigned as N/C atoms (50% N, 50% C). No hydrogen atoms were assigned on the non-coordinated pyridine molecule. 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^)+(0.0916P)^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_number_reflns 3968 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 C40 C 0.5170(3) 0.0775(3) 0.9912(5) 0.0758(16) Uiso 0.50 1 d P . . N40 N 0.5170(3) 0.0775(3) 0.9912(5) 0.0758(16) Uiso 0.50 1 d P . . C39 C 0.5581(4) 0.0433(3) 1.0867(5) 0.0777(19) Uiso 1 1 d . . . C41 C 0.4580(4) 0.0367(4) 0.9019(6) 0.098(2) Uiso 1 1 d . . . Co1 Co 0.0000 0.0000 0.0000 0.0216(3) Uani 1 2 d S . . Co2 Co 0.5000 0.0000 0.5000 0.0252(3) Uani 1 2 d S . . O4 O 0.58063(17) 0.03997(14) 0.4411(2) 0.0268(7) Uani 1 1 d . . . O2 O 0.01297(16) 0.09191(14) -0.0568(2) 0.0248(7) Uani 1 1 d . . . O3 O 0.54344(16) -0.09022(14) 0.4809(2) 0.0265(7) Uani 1 1 d . . . O1 O -0.09033(16) 0.03950(15) 0.0418(2) 0.0268(7) Uani 1 1 d . . . N1 N 0.0796(2) 0.02686(18) 0.1458(3) 0.0246(9) Uani 1 1 d . . . C6 C -0.1794(3) 0.2190(2) -0.0149(3) 0.0276(11) Uani 1 1 d . . . C17 C 0.6435(2) -0.1414(2) 0.3970(3) 0.0240(11) Uani 1 1 d . . . C1 C -0.1020(2) 0.1072(2) 0.0090(3) 0.0230(11) Uani 1 1 d . . . C19 C 0.7294(3) -0.0539(2) 0.3335(3) 0.0262(11) Uani 1 1 d . . . C3 C 0.6018(2) -0.0831(2) 0.4310(3) 0.0238(10) Uani 1 1 d . . . C2 C -0.0466(3) 0.1365(2) -0.0459(3) 0.0242(11) Uani 1 1 d . . . C4 C 0.6235(3) -0.0118(2) 0.4116(3) 0.0240(11) Uani 1 1 d . . . C18 C 0.7058(2) -0.1244(2) 0.3500(3) 0.0264(11) Uani 1 1 d . . . H18 H 0.7344 -0.1626 0.3275 0.032 Uiso 1 1 calc R . . C8 C -0.0557(3) 0.2087(2) -0.0841(3) 0.0245(11) Uani 1 1 d . . . C25 C 0.8003(3) -0.0409(2) 0.2817(4) 0.0357(12) Uani 1 1 d . . . C13 C 0.0066(3) 0.2437(2) -0.1353(4) 0.0297(12) Uani 1 1 d . . . C9 C -0.2515(3) 0.2659(2) -0.0047(4) 0.0349(12) Uani 1 1 d . . . C5 C -0.1669(3) 0.1495(2) 0.0241(3) 0.0294(11) Uani 1 1 d . . . H5 H -0.2029 0.1299 0.0620 0.035 Uiso 1 1 calc R . . C33 C 0.1430(3) 0.0712(2) 0.1541(4) 0.0319(11) Uani 1 1 d . . . H33 H 0.1500 0.0898 0.0871 0.038 Uiso 1 1 calc R . . C7 C -0.1229(3) 0.2461(2) -0.0685(3) 0.0286(11) Uani 1 1 d . . . H7 H -0.1316 0.2938 -0.0960 0.034 Uiso 1 1 calc R . . C23 C 0.6348(3) -0.2330(2) 0.5383(4) 0.0416(13) Uani 1 1 d . . . H23A H 0.6190 -0.2824 0.5486 0.062 Uiso 1 1 calc R . . H23B H 0.6009 -0.2000 0.5671 0.062 Uiso 1 1 calc R . . H23C H 0.6947 -0.2258 0.5795 0.062 Uiso 1 1 calc R . . N2 N 0.5796(2) 0.00878(18) 0.6523(3) 0.0273(9) Uani 1 1 d . . . C21 C 0.6189(3) -0.2187(2) 0.4134(4) 0.0291(11) Uani 1 1 d . . . C15 C 0.0087(3) 0.2045(2) -0.2404(4) 0.0412(13) Uani 1 1 d . . . H15A H 0.0493 0.2277 -0.2709 0.062 Uiso 1 1 calc R . . H15B H -0.0475 0.2057 -0.2966 0.062 Uiso 1 1 calc R . . H15C H 0.0256 0.1546 -0.2215 0.062 Uiso 1 1 calc R . . C16 C -0.0148(3) 0.3221(2) -0.1669(4) 0.0417(13) Uani 1 1 d . . . H16A H 0.0268 0.3421 -0.1989 0.063 Uiso 1 1 calc R . . H16B H -0.0137 0.3493 -0.0996 0.063 Uiso 1 1 calc R . . H16C H -0.0711 0.3252 -0.2225 0.063 Uiso 1 1 calc R . . C32 C 0.1992(3) 0.0914(3) 0.2556(4) 0.0398(13) Uani 1 1 d . . . H32 H 0.2430 0.1245 0.2586 0.048 Uiso 1 1 calc R . . C31 C 0.1909(3) 0.0629(3) 0.3532(4) 0.0388(13) Uani 1 1 d . . . H31 H 0.2291 0.0755 0.4246 0.047 Uiso 1 1 calc R . . C38 C 0.6322(3) 0.0643(2) 0.6780(4) 0.0321(12) Uani 1 1 d . . . H38 H 0.6307 0.0983 0.6210 0.038 Uiso 1 1 calc R . . C10 C -0.3029(3) 0.2296(3) 0.0602(5) 0.0698(19) Uani 1 1 d . . . H10A H -0.3482 0.2616 0.0644 0.105 Uiso 1 1 calc R . . H10B H -0.2663 0.2184 0.1364 0.105 Uiso 1 1 calc R . . H10C H -0.3273 0.1853 0.0218 0.105 Uiso 1 1 calc R . . C20 C 0.6866(3) 0.0023(2) 0.3635(3) 0.0271(11) Uani 1 1 d . . . H20 H 0.7002 0.0503 0.3512 0.032 Uiso 1 1 calc R . . C11 C -0.2178(3) 0.3363(3) 0.0531(4) 0.0509(15) Uani 1 1 d . . . H11A H -0.2649 0.3657 0.0586 0.076 Uiso 1 1 calc R . . H11B H -0.1876 0.3619 0.0093 0.076 Uiso 1 1 calc R . . H11C H -0.1791 0.3267 0.1287 0.076 Uiso 1 1 calc R . . C28 C 0.8157(3) 0.0378(3) 0.2671(5) 0.0545(15) Uani 1 1 d . . . H28A H 0.8296 0.0619 0.3401 0.082 Uiso 1 1 calc R . . H28B H 0.7647 0.0593 0.2150 0.082 Uiso 1 1 calc R . . H28C H 0.8626 0.0432 0.2367 0.082 Uiso 1 1 calc R . . C12 C -0.3114(3) 0.2836(3) -0.1231(4) 0.0516(15) Uani 1 1 d . . . H12A H -0.3576 0.3138 -0.1168 0.077 Uiso 1 1 calc R . . H12B H -0.3344 0.2391 -0.1622 0.077 Uiso 1 1 calc R . . H12C H -0.2801 0.3091 -0.1657 0.077 Uiso 1 1 calc R . . C37 C 0.6885(3) 0.0745(3) 0.7839(4) 0.0384(13) Uani 1 1 d . . . H37 H 0.7260 0.1141 0.7992 0.046 Uiso 1 1 calc R . . C30 C 0.1259(3) 0.0158(2) 0.3443(4) 0.0427(13) Uani 1 1 d . . . H30 H 0.1187 -0.0054 0.4096 0.051 Uiso 1 1 calc R . . C29 C 0.0720(3) 0.0000(2) 0.2404(4) 0.0330(12) Uani 1 1 d . . . H29 H 0.0267 -0.0319 0.2351 0.040 Uiso 1 1 calc R . . C34 C 0.5802(3) -0.0383(2) 0.7335(4) 0.0346(12) Uani 1 1 d . . . H34 H 0.5431 -0.0781 0.7158 0.042 Uiso 1 1 calc R . . C24 C 0.6704(3) -0.2728(2) 0.3698(4) 0.0428(13) Uani 1 1 d . . . H24A H 0.6529 -0.3215 0.3813 0.064 Uiso 1 1 calc R . . H24B H 0.7305 -0.2668 0.4109 0.064 Uiso 1 1 calc R . . H24C H 0.6605 -0.2647 0.2895 0.064 Uiso 1 1 calc R . . C35 C 0.6342(3) -0.0300(3) 0.8431(4) 0.0381(12) Uani 1 1 d . . . H35 H 0.6327 -0.0629 0.9002 0.046 Uiso 1 1 calc R . . C36 C 0.6894(3) 0.0263(3) 0.8671(4) 0.0419(13) Uani 1 1 d . . . H36 H 0.7281 0.0320 0.9406 0.050 Uiso 1 1 calc R . . C14 C 0.0953(3) 0.2417(2) -0.0484(4) 0.0405(13) Uani 1 1 d . . . H14A H 0.1357 0.2638 -0.0805 0.061 Uiso 1 1 calc R . . H14B H 0.1116 0.1920 -0.0282 0.061 Uiso 1 1 calc R . . H14C H 0.0950 0.2682 0.0190 0.061 Uiso 1 1 calc R . . C27 C 0.7789(3) -0.0774(3) 0.1669(4) 0.0517(15) Uani 1 1 d . . . H27A H 0.7691 -0.1285 0.1751 0.078 Uiso 1 1 calc R . . H27B H 0.8260 -0.0714 0.1369 0.078 Uiso 1 1 calc R . . H27C H 0.7280 -0.0557 0.1152 0.078 Uiso 1 1 calc R . . C26 C 0.8827(3) -0.0727(3) 0.3598(4) 0.0471(14) Uani 1 1 d . . . H26A H 0.8749 -0.1239 0.3703 0.071 Uiso 1 1 calc R . . H26B H 0.8979 -0.0484 0.4328 0.071 Uiso 1 1 calc R . . H26C H 0.9278 -0.0660 0.3263 0.071 Uiso 1 1 calc R . . C22 C 0.5248(3) -0.2302(3) 0.3468(4) 0.0491(14) Uani 1 1 d . . . H22A H 0.5088 -0.2795 0.3568 0.074 Uiso 1 1 calc R . . H22B H 0.5156 -0.2210 0.2669 0.074 Uiso 1 1 calc R . . H22C H 0.4903 -0.1971 0.3746 0.074 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 Co1 0.0253(6) 0.0172(6) 0.0234(6) 0.0003(5) 0.0094(4) 0.0007(4) Co2 0.0298(6) 0.0194(6) 0.0290(6) -0.0001(5) 0.0130(5) 0.0004(5) O4 0.0307(17) 0.0204(17) 0.0332(18) 0.0002(14) 0.0156(14) 0.0028(14) O2 0.0273(16) 0.0210(17) 0.0281(17) -0.0010(14) 0.0115(14) -0.0019(14) O3 0.0307(17) 0.0214(17) 0.0322(17) 0.0016(14) 0.0168(14) -0.0001(14) O1 0.0336(18) 0.0222(18) 0.0260(17) 0.0043(14) 0.0113(14) 0.0023(14) N1 0.029(2) 0.018(2) 0.028(2) -0.0008(18) 0.0103(18) 0.0017(19) C6 0.033(3) 0.025(3) 0.024(3) -0.005(2) 0.008(2) 0.002(2) C17 0.025(2) 0.022(3) 0.021(2) 0.000(2) 0.001(2) -0.005(2) C1 0.029(3) 0.020(3) 0.018(2) -0.003(2) 0.006(2) -0.002(2) C19 0.030(3) 0.027(3) 0.023(3) 0.001(2) 0.010(2) 0.002(2) C3 0.024(2) 0.023(3) 0.024(3) -0.002(2) 0.007(2) 0.000(2) C2 0.027(3) 0.023(3) 0.021(2) -0.003(2) 0.005(2) 0.003(2) C4 0.031(3) 0.019(3) 0.023(3) -0.001(2) 0.010(2) 0.000(2) C18 0.030(3) 0.021(3) 0.027(3) -0.003(2) 0.008(2) 0.002(2) C8 0.027(3) 0.022(3) 0.021(3) -0.004(2) 0.003(2) 0.004(2) C25 0.049(3) 0.029(3) 0.040(3) 0.004(2) 0.029(3) 0.006(2) C13 0.030(3) 0.022(3) 0.037(3) 0.000(2) 0.011(2) 0.001(2) C9 0.035(3) 0.029(3) 0.044(3) 0.004(2) 0.017(3) 0.009(2) C5 0.032(3) 0.027(3) 0.028(3) -0.002(2) 0.009(2) -0.001(2) C33 0.035(3) 0.033(3) 0.029(3) 0.001(2) 0.013(2) -0.005(3) C7 0.037(3) 0.018(3) 0.029(3) 0.002(2) 0.008(2) 0.004(2) C23 0.056(3) 0.023(3) 0.051(3) 0.006(2) 0.024(3) 0.000(2) N2 0.032(2) 0.020(2) 0.033(2) -0.0020(19) 0.0161(19) 0.0001(19) C21 0.033(3) 0.021(3) 0.033(3) -0.004(2) 0.010(2) -0.002(2) C15 0.053(3) 0.038(3) 0.043(3) 0.003(3) 0.030(3) -0.003(3) C16 0.044(3) 0.031(3) 0.055(3) 0.007(3) 0.022(3) 0.003(2) C32 0.031(3) 0.043(3) 0.043(3) -0.004(3) 0.007(3) -0.009(2) C31 0.038(3) 0.036(3) 0.034(3) -0.008(3) 0.000(2) 0.008(3) C38 0.038(3) 0.027(3) 0.032(3) 0.000(2) 0.013(2) -0.002(2) C10 0.074(4) 0.051(4) 0.112(5) 0.022(4) 0.069(4) 0.025(3) C20 0.043(3) 0.019(3) 0.023(3) 0.002(2) 0.016(2) 0.001(2) C11 0.049(3) 0.043(3) 0.064(4) -0.011(3) 0.022(3) 0.012(3) C28 0.064(4) 0.040(3) 0.081(4) 0.005(3) 0.054(3) -0.002(3) C12 0.040(3) 0.048(3) 0.065(4) -0.009(3) 0.013(3) 0.017(3) C37 0.044(3) 0.030(3) 0.040(3) -0.004(3) 0.011(3) -0.005(2) C30 0.069(4) 0.031(3) 0.026(3) 0.001(2) 0.011(3) 0.000(3) C29 0.049(3) 0.022(3) 0.028(3) -0.004(2) 0.013(3) -0.006(2) C34 0.043(3) 0.020(3) 0.043(3) 0.000(3) 0.017(3) 0.003(2) C24 0.051(3) 0.023(3) 0.059(4) -0.007(3) 0.023(3) -0.002(2) C35 0.054(3) 0.029(3) 0.031(3) 0.006(2) 0.014(3) 0.004(3) C36 0.048(3) 0.032(3) 0.038(3) -0.005(3) 0.002(3) 0.000(3) C14 0.034(3) 0.036(3) 0.051(3) 0.002(3) 0.012(3) -0.006(2) C27 0.066(4) 0.060(4) 0.039(3) -0.007(3) 0.032(3) -0.005(3) C26 0.045(3) 0.054(3) 0.051(3) 0.003(3) 0.027(3) 0.005(3) C22 0.042(3) 0.036(3) 0.066(4) -0.011(3) 0.012(3) -0.006(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 C40 C39 1.339(7) . ? C40 C41 1.452(8) . ? N40 C39 1.339(7) . ? N40 C41 1.452(8) . ? C39 C41 1.534(10) 3_657 ? C41 C39 1.534(10) 3_657 ? Co1 O1 1.897(3) . ? Co1 O1 1.897(3) 3 ? Co1 O2 1.898(3) . ? Co1 O2 1.898(3) 3 ? Co1 N1 1.956(3) 3 ? Co1 N1 1.956(3) . ? Co2 O3 1.881(3) 3_656 ? Co2 O3 1.881(3) . ? Co2 O4 1.883(3) . ? Co2 O4 1.883(3) 3_656 ? Co2 N2 1.958(3) 3_656 ? Co2 N2 1.958(3) . ? O4 C4 1.324(5) . ? O2 C2 1.338(5) . ? O3 C3 1.322(5) . ? O1 C1 1.326(5) . ? N1 C33 1.323(5) . ? N1 C29 1.330(5) . ? C6 C5 1.380(6) . ? C6 C7 1.415(6) . ? C6 C9 1.527(6) . ? C17 C18 1.385(5) . ? C17 C3 1.428(6) . ? C17 C21 1.534(6) . ? C1 C5 1.402(6) . ? C1 C2 1.425(6) . ? C19 C20 1.387(6) . ? C19 C18 1.410(6) . ? C19 C25 1.539(6) . ? C3 C4 1.423(6) . ? C2 C8 1.424(6) . ? C4 C20 1.395(6) . ? C8 C7 1.389(6) . ? C8 C13 1.531(6) . ? C25 C28 1.514(7) . ? C25 C27 1.529(6) . ? C25 C26 1.535(6) . ? C13 C15 1.518(6) . ? C13 C16 1.531(6) . ? C13 C14 1.537(6) . ? C9 C10 1.517(6) . ? C9 C11 1.522(6) . ? C9 C12 1.541(6) . ? C33 C32 1.374(6) . ? C23 C21 1.527(6) . ? N2 C38 1.332(5) . ? N2 C34 1.343(5) . ? C21 C24 1.536(6) . ? C21 C22 1.545(6) . ? C32 C31 1.381(6) . ? C31 C30 1.375(6) . ? C38 C37 1.376(6) . ? C37 C36 1.375(6) . ? C30 C29 1.362(6) . ? C34 C35 1.394(6) . ? C35 C36 1.369(7) . ? 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 C39 C40 C41 118.1(6) . . ? C39 N40 C41 118.1(6) . . ? N40 C39 C41 119.5(6) . 3_657 ? C40 C39 C41 119.5(6) . 3_657 ? N40 C41 C39 122.4(6) . 3_657 ? C40 C41 C39 122.4(6) . 3_657 ? O1 Co1 O1 180.0(2) . 3 ? O1 Co1 O2 86.93(11) . . ? O1 Co1 O2 93.07(11) 3 . ? O1 Co1 O2 93.07(11) . 3 ? O1 Co1 O2 86.93(11) 3 3 ? O2 Co1 O2 180.00(7) . 3 ? O1 Co1 N1 89.57(13) . 3 ? O1 Co1 N1 90.43(13) 3 3 ? O2 Co1 N1 90.36(13) . 3 ? O2 Co1 N1 89.64(13) 3 3 ? O1 Co1 N1 90.43(13) . . ? O1 Co1 N1 89.57(13) 3 . ? O2 Co1 N1 89.64(13) . . ? O2 Co1 N1 90.36(13) 3 . ? N1 Co1 N1 180.0(3) 3 . ? O3 Co2 O3 180.0 3_656 . ? O3 Co2 O4 92.70(11) 3_656 . ? O3 Co2 O4 87.30(11) . . ? O3 Co2 O4 87.30(11) 3_656 3_656 ? O3 Co2 O4 92.70(11) . 3_656 ? O4 Co2 O4 180.00(17) . 3_656 ? O3 Co2 N2 91.65(13) 3_656 3_656 ? O3 Co2 N2 88.35(13) . 3_656 ? O4 Co2 N2 90.04(13) . 3_656 ? O4 Co2 N2 89.96(13) 3_656 3_656 ? O3 Co2 N2 88.35(13) 3_656 . ? O3 Co2 N2 91.65(13) . . ? O4 Co2 N2 89.96(13) . . ? O4 Co2 N2 90.04(13) 3_656 . ? N2 Co2 N2 180.0 3_656 . ? C4 O4 Co2 109.7(2) . . ? C2 O2 Co1 110.4(2) . . ? C3 O3 Co2 110.1(2) . . ? C1 O1 Co1 109.7(2) . . ? C33 N1 C29 117.8(4) . . ? C33 N1 Co1 121.7(3) . . ? C29 N1 Co1 120.5(3) . . ? C5 C6 C7 117.1(4) . . ? C5 C6 C9 123.1(4) . . ? C7 C6 C9 119.8(4) . . ? C18 C17 C3 117.0(4) . . ? C18 C17 C21 122.9(4) . . ? C3 C17 C21 120.1(4) . . ? O1 C1 C5 122.7(4) . . ? O1 C1 C2 117.5(4) . . ? C5 C1 C2 119.8(4) . . ? C20 C19 C18 118.3(4) . . ? C20 C19 C25 121.8(4) . . ? C18 C19 C25 119.9(4) . . ? O3 C3 C4 116.1(4) . . ? O3 C3 C17 124.6(4) . . ? C4 C3 C17 119.3(4) . . ? O2 C2 C8 124.0(4) . . ? O2 C2 C1 115.3(4) . . ? C8 C2 C1 120.7(4) . . ? O4 C4 C20 122.2(4) . . ? O4 C4 C3 116.6(4) . . ? C20 C4 C3 121.2(4) . . ? C17 C18 C19 124.1(4) . . ? C7 C8 C2 115.7(4) . . ? C7 C8 C13 122.1(4) . . ? C2 C8 C13 122.1(4) . . ? C28 C25 C27 108.6(4) . . ? C28 C25 C26 107.5(4) . . ? C27 C25 C26 108.9(4) . . ? C28 C25 C19 112.8(4) . . ? C27 C25 C19 110.2(4) . . ? C26 C25 C19 108.9(3) . . ? C15 C13 C8 111.3(3) . . ? C15 C13 C16 107.8(4) . . ? C8 C13 C16 112.6(4) . . ? C15 C13 C14 108.8(4) . . ? C8 C13 C14 108.8(4) . . ? C16 C13 C14 107.4(4) . . ? C10 C9 C11 108.6(4) . . ? C10 C9 C6 112.5(4) . . ? C11 C9 C6 110.7(3) . . ? C10 C9 C12 107.9(4) . . ? C11 C9 C12 107.7(4) . . ? C6 C9 C12 109.3(4) . . ? C6 C5 C1 121.3(4) . . ? N1 C33 C32 122.7(4) . . ? C8 C7 C6 125.3(4) . . ? C38 N2 C34 118.7(4) . . ? C38 N2 Co2 119.6(3) . . ? C34 N2 Co2 121.6(3) . . ? C23 C21 C17 109.6(3) . . ? C23 C21 C24 108.3(4) . . ? C17 C21 C24 111.6(4) . . ? C23 C21 C22 110.3(4) . . ? C17 C21 C22 109.1(3) . . ? C24 C21 C22 107.8(4) . . ? C33 C32 C31 119.0(4) . . ? C30 C31 C32 118.2(4) . . ? N2 C38 C37 122.6(4) . . ? C19 C20 C4 120.0(4) . . ? C36 C37 C38 118.8(4) . . ? C29 C30 C31 118.8(5) . . ? N1 C29 C30 123.5(4) . . ? N2 C34 C35 121.5(4) . . ? C36 C35 C34 118.9(4) . . ? C35 C36 C37 119.5(4) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 51.47 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.976 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.060 #===END data_compound_1_py_200k _database_code_depnum_ccdc_archive 'CCDC 744066' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H105 Co2 N5 O8' _chemical_formula_weight 1394.63 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.759(2) _cell_length_b 18.788(2) _cell_length_c 12.5700(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.2730(10) _cell_angle_gamma 90.00 _cell_volume 3758.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 3.904 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2909 _exptl_absorpt_correction_T_max 0.5090 _exptl_absorpt_process_details SADABS _exptl_special_details ; Crystals were weakly diffracting and as a result data was only collected to a theta angle of 51.5. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8936 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 51.47 _reflns_number_total 3997 _reflns_number_gt 2764 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The non-coordinated pyridine molecule is disordered across a centre of symmetry. Two opposing atoms in the pyridine molecule were tentatively assigned as N/C atoms (50% N, 50% C). No hydrogen atoms were assigned on the non-coordinated pyridine molecule. 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^)+(0.0932P)^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_number_reflns 3997 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 C40 C 0.0162(4) 0.0787(4) 0.4917(5) 0.110(2) Uiso 0.50 1 d P . . N40 N 0.0162(4) 0.0787(4) 0.4917(5) 0.110(2) Uiso 0.50 1 d P . . C39 C 0.0556(4) 0.0431(4) 0.5870(6) 0.116(2) Uiso 1 1 d . . . C41 C -0.0398(5) 0.0376(5) 0.3998(7) 0.134(3) Uiso 1 1 d . . . C16A C 0.2181(12) 0.2372(8) 0.5990(18) 0.056(6) Uiso 0.41(3) 1 d P A 1 H16A H 0.2674 0.2295 0.6649 0.084 Uiso 0.41(3) 1 calc PR A 1 H16B H 0.1869 0.1926 0.5787 0.084 Uiso 0.41(3) 1 calc PR A 1 H16C H 0.1818 0.2734 0.6161 0.084 Uiso 0.41(3) 1 calc PR A 1 C16B C 0.1877(9) 0.2252(5) 0.5443(14) 0.063(4) Uiso 0.59(3) 1 d P A 2 H16D H 0.2174 0.2098 0.6211 0.094 Uiso 0.59(3) 1 calc PR A 2 H16E H 0.1650 0.1835 0.4979 0.094 Uiso 0.59(3) 1 calc PR A 2 H16F H 0.1417 0.2572 0.5447 0.094 Uiso 0.59(3) 1 calc PR A 2 Co1 Co 0.5000 0.0000 0.5000 0.0302(3) Uani 1 2 d S . . Co2 Co 0.0000 0.0000 1.0000 0.0338(3) Uani 1 2 d S . . O4 O 0.04313(16) -0.09001(13) 0.9809(2) 0.0381(7) Uani 1 1 d . . . O1 O 0.51149(16) 0.09216(13) 0.4434(2) 0.0363(7) Uani 1 1 d . . . O3 O 0.07981(16) 0.03963(14) 0.9404(2) 0.0368(7) Uani 1 1 d . . . N1 N 0.5784(2) 0.02721(18) 0.6463(3) 0.0339(9) Uani 1 1 d . . . O2 O 0.40892(16) 0.03885(14) 0.5407(2) 0.0376(7) Uani 1 1 d . . . C2 C 0.3970(2) 0.1064(2) 0.5088(3) 0.0321(10) Uani 1 1 d . . . C8 C 0.4431(2) 0.2081(2) 0.4175(3) 0.0327(10) Uani 1 1 d . . . C6 C 0.3198(3) 0.2168(2) 0.4867(3) 0.0372(11) Uani 1 1 d . A . C3 C 0.1228(3) -0.0117(2) 0.9114(3) 0.0323(10) Uani 1 1 d . . . C1 C 0.4523(2) 0.1362(2) 0.4542(3) 0.0315(10) Uani 1 1 d . . . C17 C 0.1427(2) -0.1411(2) 0.8984(3) 0.0330(10) Uani 1 1 d . . . C4 C 0.1019(3) -0.0832(2) 0.9313(3) 0.0327(10) Uani 1 1 d . . . C21 C 0.2985(3) -0.0423(2) 0.7803(4) 0.0458(12) Uani 1 1 d . . . C9 C 0.5045(3) 0.2431(2) 0.3670(4) 0.0430(12) Uani 1 1 d . . . C5 C 0.3318(2) 0.1479(2) 0.5241(3) 0.0379(11) Uani 1 1 d . . . H5 H 0.2956 0.1280 0.5610 0.046 Uiso 1 1 calc R . . C19 C 0.2281(3) -0.0543(2) 0.8333(3) 0.0373(11) Uani 1 1 d . . . C18 C 0.2044(3) -0.1248(2) 0.8510(3) 0.0383(11) Uani 1 1 d . . . H18 H 0.2327 -0.1631 0.8289 0.046 Uiso 1 1 calc R . . C7 C 0.3759(3) 0.2449(2) 0.4338(3) 0.0416(11) Uani 1 1 d . . . H7 H 0.3670 0.2925 0.4073 0.050 Uiso 1 1 calc R . . N2 N 0.0797(2) 0.00830(18) 1.1506(3) 0.0360(9) Uani 1 1 d . . . C13 C 0.2478(3) 0.2635(2) 0.4973(4) 0.0507(13) Uani 1 1 d . . . C10 C 0.4827(3) 0.3213(2) 0.3356(4) 0.0639(15) Uani 1 1 d . . . H10A H 0.5241 0.3415 0.3037 0.096 Uiso 1 1 calc R . . H10B H 0.4834 0.3481 0.4027 0.096 Uiso 1 1 calc R . . H10C H 0.4266 0.3241 0.2802 0.096 Uiso 1 1 calc R . . C11 C 0.5057(3) 0.2045(3) 0.2603(4) 0.0630(14) Uani 1 1 d . . . H11A H 0.5460 0.2278 0.2295 0.094 Uiso 1 1 calc R . . H11B H 0.4495 0.2061 0.2049 0.094 Uiso 1 1 calc R . . H11C H 0.5224 0.1548 0.2780 0.094 Uiso 1 1 calc R . . C29 C 0.6413(3) 0.0722(3) 0.6552(4) 0.0505(12) Uani 1 1 d . . . H30 H 0.6485 0.0914 0.5889 0.061 Uiso 1 1 calc R . . C28 C 0.1341(3) -0.2318(2) 1.0406(4) 0.0615(14) Uani 1 1 d . . . H28A H 0.1186 -0.2810 1.0513 0.092 Uiso 1 1 calc R . . H28B H 0.1001 -0.1991 1.0691 0.092 Uiso 1 1 calc R . . H28C H 0.1937 -0.2244 1.0816 0.092 Uiso 1 1 calc R . . C20 C 0.1858(3) 0.0014(2) 0.8633(3) 0.0367(11) Uani 1 1 d . . . H20 H 0.1998 0.0491 0.8511 0.044 Uiso 1 1 calc R . . C25 C 0.1183(3) -0.2178(2) 0.9154(4) 0.0448(12) Uani 1 1 d . . . C34 C 0.0811(3) -0.0393(2) 1.2306(4) 0.0467(12) Uani 1 1 d . . . H40 H 0.0444 -0.0792 1.2128 0.056 Uiso 1 1 calc R . . C38 C 0.1323(3) 0.0639(2) 1.1765(4) 0.0428(11) Uani 1 1 d . . . H36 H 0.1306 0.0981 1.1201 0.051 Uiso 1 1 calc R . . C35 C 0.1353(3) -0.0314(3) 1.3387(4) 0.0572(14) Uani 1 1 d . . . H39 H 0.1343 -0.0647 1.3952 0.069 Uiso 1 1 calc R . . C30 C 0.6967(3) 0.0922(3) 0.7580(4) 0.0613(14) Uani 1 1 d . . . H31 H 0.7400 0.1256 0.7620 0.074 Uiso 1 1 calc R . . C15 C 0.2807(3) 0.3342(3) 0.5526(5) 0.0845(18) Uani 1 1 d . A . H15A H 0.3120 0.3585 0.5092 0.127 Uiso 1 1 calc R . . H15B H 0.3180 0.3257 0.6289 0.127 Uiso 1 1 calc R . . H15C H 0.2334 0.3641 0.5553 0.127 Uiso 1 1 calc R . . C31 C 0.6882(3) 0.0632(3) 0.8528(4) 0.0563(14) Uani 1 1 d . . . H32 H 0.7261 0.0755 0.9241 0.068 Uiso 1 1 calc R . . C36 C 0.1904(3) 0.0248(3) 1.3637(4) 0.0617(15) Uani 1 1 d . . . H38 H 0.2293 0.0299 1.4368 0.074 Uiso 1 1 calc R . . C22 C 0.3148(4) 0.0364(3) 0.7676(5) 0.0806(18) Uani 1 1 d . . . H22A H 0.3303 0.0595 0.8411 0.121 Uiso 1 1 calc R . . H22B H 0.2639 0.0587 0.7178 0.121 Uiso 1 1 calc R . . H22C H 0.3608 0.0418 0.7355 0.121 Uiso 1 1 calc R . . C37 C 0.1886(3) 0.0733(3) 1.2815(4) 0.0548(13) Uani 1 1 d . . . H37 H 0.2257 0.1129 1.2970 0.066 Uiso 1 1 calc R . . C33 C 0.5711(3) 0.0004(2) 0.7405(4) 0.0518(13) Uani 1 1 d . . . H34 H 0.5262 -0.0316 0.7355 0.062 Uiso 1 1 calc R . . C12 C 0.5927(3) 0.2413(3) 0.4510(4) 0.0617(14) Uani 1 1 d . . . H12A H 0.6322 0.2638 0.4180 0.093 Uiso 1 1 calc R . . H12B H 0.6095 0.1917 0.4700 0.093 Uiso 1 1 calc R . . H12C H 0.5932 0.2670 0.5190 0.093 Uiso 1 1 calc R . . C27 C 0.1700(3) -0.2718(2) 0.8738(4) 0.0654(15) Uani 1 1 d . . . H27A H 0.1526 -0.3201 0.8859 0.098 Uiso 1 1 calc R . . H27B H 0.2297 -0.2655 0.9151 0.098 Uiso 1 1 calc R . . H27C H 0.1608 -0.2643 0.7937 0.098 Uiso 1 1 calc R . . C32 C 0.6247(4) 0.0163(3) 0.8438(4) 0.0627(15) Uani 1 1 d . . . H33 H 0.6178 -0.0051 0.9089 0.075 Uiso 1 1 calc R . . C14 C 0.1881(3) 0.2810(3) 0.3810(5) 0.089(2) Uani 1 1 d . A . H14A H 0.2197 0.3035 0.3363 0.134 Uiso 1 1 calc R . . H14B H 0.1444 0.3136 0.3878 0.134 Uiso 1 1 calc R . . H14C H 0.1621 0.2370 0.3440 0.134 Uiso 1 1 calc R . . C23 C 0.2766(3) -0.0776(3) 0.6663(4) 0.0758(17) Uani 1 1 d . . . H23A H 0.2669 -0.1285 0.6740 0.114 Uiso 1 1 calc R . . H23B H 0.3230 -0.0713 0.6355 0.114 Uiso 1 1 calc R . . H23C H 0.2256 -0.0558 0.6158 0.114 Uiso 1 1 calc R . . C26 C 0.0254(3) -0.2299(3) 0.8494(4) 0.0689(16) Uani 1 1 d . . . H26A H 0.0099 -0.2791 0.8600 0.103 Uiso 1 1 calc R . . H26B H 0.0164 -0.2212 0.7696 0.103 Uiso 1 1 calc R . . H26C H -0.0094 -0.1971 0.8765 0.103 Uiso 1 1 calc R . . C24 C 0.3800(3) -0.0747(3) 0.8581(4) 0.0705(16) Uani 1 1 d . . . H24A H 0.3718 -0.1257 0.8673 0.106 Uiso 1 1 calc R . . H24B H 0.3950 -0.0512 0.9313 0.106 Uiso 1 1 calc R . . H24C H 0.4254 -0.0680 0.8252 0.106 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 Co1 0.0311(6) 0.0270(5) 0.0334(6) 0.0002(5) 0.0114(4) 0.0031(4) Co2 0.0370(6) 0.0280(6) 0.0399(6) -0.0002(5) 0.0169(5) -0.0004(5) O4 0.0453(18) 0.0279(16) 0.0463(17) 0.0012(14) 0.0217(16) -0.0033(14) O1 0.0358(17) 0.0345(16) 0.0411(17) -0.0023(14) 0.0156(14) -0.0003(14) O3 0.0407(18) 0.0273(16) 0.0471(17) -0.0009(14) 0.0207(15) 0.0019(14) N1 0.037(2) 0.032(2) 0.035(2) 0.0010(18) 0.0146(18) 0.0079(18) O2 0.0364(18) 0.0383(18) 0.0402(17) 0.0015(15) 0.0153(14) 0.0030(14) C2 0.033(3) 0.033(3) 0.028(2) -0.002(2) 0.005(2) 0.001(2) C8 0.030(3) 0.032(3) 0.036(2) -0.001(2) 0.010(2) 0.003(2) C6 0.035(3) 0.038(3) 0.039(3) -0.006(2) 0.013(2) 0.004(2) C3 0.036(3) 0.031(3) 0.031(2) 0.000(2) 0.011(2) -0.002(2) C1 0.028(3) 0.037(3) 0.029(2) -0.004(2) 0.009(2) 0.002(2) C17 0.036(3) 0.029(3) 0.033(2) -0.002(2) 0.009(2) -0.004(2) C4 0.035(3) 0.034(3) 0.030(2) 0.000(2) 0.011(2) -0.003(2) C21 0.055(3) 0.041(3) 0.053(3) 0.004(2) 0.035(3) 0.006(2) C9 0.041(3) 0.034(3) 0.055(3) 0.001(2) 0.017(2) 0.002(2) C5 0.033(3) 0.043(3) 0.041(3) -0.006(2) 0.015(2) 0.000(2) C19 0.044(3) 0.036(3) 0.034(3) 0.002(2) 0.014(2) 0.003(2) C18 0.047(3) 0.033(3) 0.036(2) -0.005(2) 0.015(2) 0.006(2) C7 0.044(3) 0.033(3) 0.046(3) 0.005(2) 0.012(2) 0.005(2) N2 0.037(2) 0.031(2) 0.043(2) 0.0003(19) 0.0177(18) 0.0000(18) C13 0.042(3) 0.053(3) 0.061(3) -0.003(3) 0.023(3) 0.011(3) C10 0.060(3) 0.044(3) 0.095(4) 0.013(3) 0.035(3) 0.005(3) C11 0.080(4) 0.061(3) 0.062(3) 0.003(3) 0.043(3) -0.005(3) C29 0.043(3) 0.060(3) 0.050(3) 0.007(3) 0.016(3) -0.005(3) C28 0.085(4) 0.035(3) 0.072(4) 0.007(3) 0.036(3) -0.001(3) C20 0.049(3) 0.027(3) 0.037(3) 0.002(2) 0.018(2) -0.001(2) C25 0.048(3) 0.032(3) 0.055(3) -0.006(2) 0.017(2) -0.002(2) C34 0.054(3) 0.035(3) 0.050(3) 0.000(3) 0.015(3) -0.002(2) C38 0.045(3) 0.039(3) 0.045(3) 0.002(2) 0.016(3) -0.003(2) C35 0.077(4) 0.042(3) 0.048(3) 0.008(3) 0.013(3) 0.004(3) C30 0.042(3) 0.077(4) 0.055(3) -0.008(3) 0.001(3) -0.010(3) C15 0.075(4) 0.071(4) 0.115(5) -0.026(4) 0.042(4) 0.021(3) C31 0.057(4) 0.059(3) 0.044(3) -0.006(3) 0.002(3) 0.012(3) C36 0.069(4) 0.055(3) 0.048(3) -0.004(3) -0.002(3) 0.003(3) C22 0.098(5) 0.057(4) 0.120(5) 0.009(3) 0.083(4) -0.001(3) C37 0.054(3) 0.047(3) 0.058(3) -0.006(3) 0.010(3) -0.012(3) C33 0.073(4) 0.036(3) 0.045(3) -0.007(3) 0.017(3) -0.009(2) C12 0.042(3) 0.057(3) 0.083(4) 0.004(3) 0.015(3) -0.008(3) C27 0.074(4) 0.035(3) 0.093(4) -0.011(3) 0.035(3) -0.002(3) C32 0.098(5) 0.049(3) 0.036(3) 0.001(3) 0.014(3) -0.001(3) C14 0.061(4) 0.095(5) 0.102(5) -0.015(4) 0.011(4) 0.034(3) C23 0.089(4) 0.100(4) 0.055(3) -0.018(3) 0.046(3) -0.016(4) C26 0.056(4) 0.051(3) 0.097(4) -0.016(3) 0.020(3) -0.015(3) C24 0.058(4) 0.086(4) 0.080(4) 0.005(3) 0.040(3) 0.011(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 C40 C39 1.350(8) . ? C40 C41 1.460(9) . ? N40 C39 1.350(8) . ? N40 C41 1.460(9) . ? C39 C41 1.558(11) 3_556 ? C41 C39 1.558(11) 3_556 ? C16A C13 1.588(14) . ? C16B C13 1.501(9) . ? Co1 O2 1.901(3) . ? Co1 O2 1.901(3) 3_656 ? Co1 O1 1.904(2) . ? Co1 O1 1.904(2) 3_656 ? Co1 N1 1.963(3) 3_656 ? Co1 N1 1.963(3) . ? Co2 O3 1.880(3) 3_557 ? Co2 O3 1.880(3) . ? Co2 O4 1.884(3) 3_557 ? Co2 O4 1.884(3) . ? Co2 N2 1.951(3) 3_557 ? Co2 N2 1.951(3) . ? O4 C4 1.326(5) . ? O1 C1 1.331(4) . ? O3 C3 1.322(4) . ? N1 C33 1.326(5) . ? N1 C29 1.328(5) . ? O2 C2 1.327(5) . ? C2 C5 1.403(5) . ? C2 C1 1.429(5) . ? C8 C7 1.390(5) . ? C8 C1 1.421(5) . ? C8 C9 1.518(6) . ? C6 C5 1.371(6) . ? C6 C7 1.413(6) . ? C6 C13 1.531(5) . ? C3 C20 1.394(5) . ? C3 C4 1.429(5) . ? C17 C18 1.379(5) . ? C17 C4 1.415(5) . ? C17 C25 1.531(5) . ? C21 C23 1.516(6) . ? C21 C22 1.521(6) . ? C21 C24 1.535(6) . ? C21 C19 1.542(6) . ? C9 C12 1.525(6) . ? C9 C11 1.531(6) . ? C9 C10 1.534(6) . ? C19 C20 1.382(5) . ? C19 C18 1.421(6) . ? N2 C38 1.340(5) . ? N2 C34 1.341(5) . ? C13 C15 1.521(7) . ? C13 C14 1.526(6) . ? C29 C30 1.385(6) . ? C28 C25 1.535(6) . ? C25 C27 1.528(6) . ? C25 C26 1.534(6) . ? C34 C35 1.386(6) . ? C38 C37 1.371(6) . ? C35 C36 1.373(7) . ? C30 C31 1.357(6) . ? C31 C32 1.359(7) . ? C36 C37 1.371(6) . ? C33 C32 1.361(6) . ? 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 C39 C40 C41 117.0(7) . . ? C39 N40 C41 117.0(7) . . ? N40 C39 C41 121.6(6) . 3_556 ? C40 C39 C41 121.6(6) . 3_556 ? N40 C41 C39 121.3(6) . 3_556 ? C40 C41 C39 121.3(6) . 3_556 ? O2 Co1 O2 180.0 . 3_656 ? O2 Co1 O1 86.29(11) . . ? O2 Co1 O1 93.71(11) 3_656 . ? O2 Co1 O1 93.71(11) . 3_656 ? O2 Co1 O1 86.29(11) 3_656 3_656 ? O1 Co1 O1 180.00(6) . 3_656 ? O2 Co1 N1 89.69(12) . 3_656 ? O2 Co1 N1 90.31(12) 3_656 3_656 ? O1 Co1 N1 90.18(13) . 3_656 ? O1 Co1 N1 89.82(13) 3_656 3_656 ? O2 Co1 N1 90.31(12) . . ? O2 Co1 N1 89.69(12) 3_656 . ? O1 Co1 N1 89.82(13) . . ? O1 Co1 N1 90.18(13) 3_656 . ? N1 Co1 N1 180.0 3_656 . ? O3 Co2 O3 180.00(9) 3_557 . ? O3 Co2 O4 87.43(11) 3_557 3_557 ? O3 Co2 O4 92.57(11) . 3_557 ? O3 Co2 O4 92.57(11) 3_557 . ? O3 Co2 O4 87.43(11) . . ? O4 Co2 O4 180.000(1) 3_557 . ? O3 Co2 N2 89.95(13) 3_557 3_557 ? O3 Co2 N2 90.05(13) . 3_557 ? O4 Co2 N2 91.28(12) 3_557 3_557 ? O4 Co2 N2 88.72(12) . 3_557 ? O3 Co2 N2 90.05(13) 3_557 . ? O3 Co2 N2 89.95(13) . . ? O4 Co2 N2 88.72(12) 3_557 . ? O4 Co2 N2 91.28(12) . . ? N2 Co2 N2 180.000(1) 3_557 . ? C4 O4 Co2 110.2(2) . . ? C1 O1 Co1 111.2(2) . . ? C3 O3 Co2 109.7(2) . . ? C33 N1 C29 117.3(4) . . ? C33 N1 Co1 121.0(3) . . ? C29 N1 Co1 121.7(3) . . ? C2 O2 Co1 110.1(2) . . ? O2 C2 C5 122.7(4) . . ? O2 C2 C1 117.4(4) . . ? C5 C2 C1 119.9(4) . . ? C7 C8 C1 115.8(4) . . ? C7 C8 C9 122.2(4) . . ? C1 C8 C9 122.0(4) . . ? C5 C6 C7 117.7(4) . . ? C5 C6 C13 123.1(4) . . ? C7 C6 C13 119.1(4) . . ? O3 C3 C20 122.8(4) . . ? O3 C3 C4 117.0(4) . . ? C20 C3 C4 120.2(4) . . ? O1 C1 C8 124.5(4) . . ? O1 C1 C2 115.0(3) . . ? C8 C1 C2 120.5(4) . . ? C18 C17 C4 116.9(4) . . ? C18 C17 C25 122.6(4) . . ? C4 C17 C25 120.5(4) . . ? O4 C4 C17 124.2(4) . . ? O4 C4 C3 115.6(4) . . ? C17 C4 C3 120.2(4) . . ? C23 C21 C22 108.9(4) . . ? C23 C21 C24 109.3(4) . . ? C22 C21 C24 107.4(4) . . ? C23 C21 C19 110.6(4) . . ? C22 C21 C19 112.1(4) . . ? C24 C21 C19 108.4(3) . . ? C8 C9 C12 109.7(4) . . ? C8 C9 C11 111.0(3) . . ? C12 C9 C11 108.6(4) . . ? C8 C9 C10 112.6(4) . . ? C12 C9 C10 107.6(4) . . ? C11 C9 C10 107.2(4) . . ? C6 C5 C2 121.0(4) . . ? C20 C19 C18 118.1(4) . . ? C20 C19 C21 122.3(4) . . ? C18 C19 C21 119.6(4) . . ? C17 C18 C19 124.0(4) . . ? C8 C7 C6 125.0(4) . . ? C38 N2 C34 118.8(4) . . ? C38 N2 Co2 119.8(3) . . ? C34 N2 Co2 121.4(3) . . ? C16B C13 C15 115.6(7) . . ? C16B C13 C14 99.3(7) . . ? C15 C13 C14 106.6(4) . . ? C16B C13 C6 113.8(5) . . ? C15 C13 C6 110.9(4) . . ? C14 C13 C6 109.6(4) . . ? C15 C13 C16A 93.7(8) . . ? C14 C13 C16A 124.2(8) . . ? C6 C13 C16A 110.3(6) . . ? N1 C29 C30 122.2(4) . . ? C19 C20 C3 120.5(4) . . ? C27 C25 C17 111.8(4) . . ? C27 C25 C26 107.8(4) . . ? C17 C25 C26 109.5(4) . . ? C27 C25 C28 107.7(4) . . ? C17 C25 C28 109.7(3) . . ? C26 C25 C28 110.4(4) . . ? N2 C34 C35 121.1(4) . . ? N2 C38 C37 122.4(4) . . ? C36 C35 C34 119.6(5) . . ? C31 C30 C29 119.1(5) . . ? C30 C31 C32 118.8(5) . . ? C37 C36 C35 118.9(4) . . ? C36 C37 C38 119.1(4) . . ? N1 C33 C32 123.4(5) . . ? C31 C32 C33 119.1(5) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 51.47 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.814 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.055 #===END data_compound_1_py_250k _database_code_depnum_ccdc_archive 'CCDC 744067' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H105 Co2 N5 O8' _chemical_formula_weight 1394.63 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.817(5) _cell_length_b 18.941(5) _cell_length_c 12.596(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.818(4) _cell_angle_gamma 90.00 _cell_volume 3820(2) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 3.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2953 _exptl_absorpt_correction_T_max 0.5138 _exptl_absorpt_process_details SADABS _exptl_special_details ; Crystals were weakly diffracting and as a result data was only collected to a theta angle of 51.5. ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7662 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 51.42 _reflns_number_total 3938 _reflns_number_gt 2669 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The non-coordinated pyridine molecule is disordered across a centre of symmetry. Two opposing atoms in the pyridine molecule were tentatively assigned as N/C atoms (50% N, 50% C). No hydrogen atoms were assigned on the non-coordinated pyridine molecule. 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^)+(0.0640P)^2^+9.5244P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3938 _refine_ls_number_parameters 421 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1784 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.097 _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 C28 C 0.6881(6) 0.0341(5) 0.2373(9) 0.123(4) Uani 1 1 d . . . H28A H 0.6739 0.0573 0.1652 0.184 Uiso 1 1 calc R . . H28B H 0.7379 0.0556 0.2872 0.184 Uiso 1 1 calc R . . H28C H 0.6422 0.0392 0.2682 0.184 Uiso 1 1 calc R . . C40 C 0.9844(8) 0.0803(7) 0.5084(12) 0.162(4) Uiso 0.50 1 d P . . N40 N 0.9844(8) 0.0803(7) 0.5084(12) 0.162(4) Uiso 0.50 1 d P . . C41 C 1.0347(10) 0.0385(10) 0.6007(13) 0.188(6) Uiso 1 1 d . . . C39 C 0.9493(9) 0.0439(9) 0.4129(13) 0.169(5) Uiso 1 1 d . . . C14A C 0.8209(16) 0.2226(10) 0.469(3) 0.086(8) Uiso 0.51(4) 1 d P A 1 H14A H 0.8354 0.1795 0.5119 0.129 Uiso 0.51(4) 1 calc PR A 1 H14B H 0.8705 0.2515 0.4803 0.129 Uiso 0.51(4) 1 calc PR A 1 H14C H 0.7985 0.2108 0.3901 0.129 Uiso 0.51(4) 1 calc PR A 1 C14B C 0.7854(18) 0.2375(12) 0.410(2) 0.092(9) Uiso 0.49(4) 1 d PD A 2 H14D H 0.8095 0.1908 0.4280 0.138 Uiso 0.49(4) 1 calc PR A 2 H14E H 0.8272 0.2697 0.4001 0.138 Uiso 0.49(4) 1 calc PR A 2 H14F H 0.7386 0.2354 0.3425 0.138 Uiso 0.49(4) 1 calc PR A 2 Co1 Co 0.5000 0.0000 0.5000 0.0534(5) Uani 1 2 d S . . Co2 Co 1.0000 0.0000 0.0000 0.0584(5) Uani 1 2 d S . . O3 O 0.9583(3) -0.0895(2) 0.0209(4) 0.0626(13) Uani 1 1 d . . . O1 O 0.4905(3) 0.0953(2) 0.5588(4) 0.0631(13) Uani 1 1 d . . . O4 O 0.9207(3) 0.0385(2) 0.0616(4) 0.0614(13) Uani 1 1 d . . . N1 N 0.4203(4) 0.0289(3) 0.3485(5) 0.0609(16) Uani 1 1 d . . . O2 O 0.5944(3) 0.0417(3) 0.4619(4) 0.0640(13) Uani 1 1 d . . . C9 C 0.4977(5) 0.2452(4) 0.6351(7) 0.071(2) Uani 1 1 d . . . C3 C 0.8995(4) -0.0828(4) 0.0703(6) 0.0550(18) Uani 1 1 d . . . C2 C 0.6054(4) 0.1074(4) 0.4944(6) 0.0530(18) Uani 1 1 d . . . C8 C 0.5594(4) 0.2095(4) 0.5852(6) 0.0559(19) Uani 1 1 d . . . C4 C 0.8787(4) -0.0130(4) 0.0903(6) 0.0526(18) Uani 1 1 d . . . C20 C 0.8590(4) -0.1406(4) 0.1019(6) 0.0586(19) Uani 1 1 d . . . C1 C 0.5491(4) 0.1377(4) 0.5469(6) 0.0562(19) Uani 1 1 d . . . N2 N 0.9194(3) 0.0077(3) -0.1494(5) 0.0608(16) Uani 1 1 d . . . C5 C 0.6713(4) 0.1494(4) 0.4779(6) 0.064(2) Uani 1 1 d . . . H5 H 0.7067 0.1303 0.4402 0.077 Uiso 1 1 calc R . . C18 C 0.7744(4) -0.0550(4) 0.1703(6) 0.062(2) Uani 1 1 d . . . C19 C 0.7970(4) -0.1246(4) 0.1511(6) 0.062(2) Uani 1 1 d . . . H19 H 0.7689 -0.1623 0.1725 0.074 Uiso 1 1 calc R . . C6 C 0.6828(4) 0.2167(4) 0.5165(6) 0.063(2) Uani 1 1 d . A . C25 C 0.7040(5) -0.0432(5) 0.2234(7) 0.079(2) Uani 1 1 d . . . C7 C 0.6262(5) 0.2459(4) 0.5686(6) 0.069(2) Uani 1 1 d . . . H7 H 0.6346 0.2929 0.5934 0.082 Uiso 1 1 calc R . . C13 C 0.7553(5) 0.2635(4) 0.5055(8) 0.079(2) Uani 1 1 d D . . C17 C 0.8155(4) 0.0004(4) 0.1390(6) 0.0602(19) Uani 1 1 d . . . H17 H 0.8011 0.0472 0.1502 0.072 Uiso 1 1 calc R . . C29 C 0.3623(5) 0.0775(5) 0.3400(8) 0.085(3) Uani 1 1 d . . . H29 H 0.3587 0.0990 0.4055 0.103 Uiso 1 1 calc R . . C12 C 0.5196(5) 0.3218(4) 0.6656(8) 0.099(3) Uani 1 1 d . . . H12A H 0.4785 0.3421 0.6964 0.148 Uiso 1 1 calc R . . H12B H 0.5198 0.3478 0.5993 0.148 Uiso 1 1 calc R . . H12C H 0.5745 0.3244 0.7204 0.148 Uiso 1 1 calc R . . C35 C 0.8107(5) 0.0719(5) -0.2776(8) 0.081(2) Uani 1 1 d . . . H35 H 0.7747 0.1111 -0.2926 0.098 Uiso 1 1 calc R . . C11 C 0.4975(5) 0.2067(5) 0.7425(7) 0.094(3) Uani 1 1 d . . . H11A H 0.4582 0.2295 0.7740 0.140 Uiso 1 1 calc R . . H11B H 0.5530 0.2084 0.7959 0.140 Uiso 1 1 calc R . . H11C H 0.4812 0.1578 0.7254 0.140 Uiso 1 1 calc R . . C34 C 0.8684(5) 0.0634(4) -0.1743(7) 0.068(2) Uani 1 1 d . . . H34 H 0.8720 0.0979 -0.1194 0.081 Uiso 1 1 calc R . . C38 C 0.9158(5) -0.0410(4) -0.2274(8) 0.077(2) Uani 1 1 d . . . H38 H 0.9514 -0.0804 -0.2100 0.092 Uiso 1 1 calc R . . C31 C 0.3106(6) 0.0664(6) 0.1455(9) 0.096(3) Uani 1 1 d . . . H31 H 0.2732 0.0791 0.0760 0.115 Uiso 1 1 calc R . . C23 C 0.8691(6) -0.2301(4) -0.0392(7) 0.093(3) Uani 1 1 d . . . H23A H 0.8844 -0.2784 -0.0496 0.140 Uiso 1 1 calc R . . H23B H 0.9035 -0.1979 -0.0661 0.140 Uiso 1 1 calc R . . H23C H 0.8108 -0.2225 -0.0804 0.140 Uiso 1 1 calc R . . C15 C 0.8123(6) 0.2815(6) 0.6211(9) 0.132(4) Uani 1 1 d . A . H15A H 0.7800 0.3041 0.6636 0.199 Uiso 1 1 calc R . . H15B H 0.8559 0.3133 0.6150 0.199 Uiso 1 1 calc R . . H15C H 0.8373 0.2386 0.6588 0.199 Uiso 1 1 calc R . . C30 C 0.3069(5) 0.0981(6) 0.2395(9) 0.099(3) Uani 1 1 d . . . H30 H 0.2673 0.1336 0.2367 0.118 Uiso 1 1 calc R . . C36 C 0.8066(6) 0.0226(5) -0.3580(8) 0.091(3) Uani 1 1 d . . . H36 H 0.7676 0.0274 -0.4292 0.109 Uiso 1 1 calc R . . C33 C 0.4231(6) -0.0008(4) 0.2549(8) 0.091(3) Uani 1 1 d . . . H33 H 0.4643 -0.0351 0.2588 0.109 Uiso 1 1 calc R . . C10 C 0.4097(5) 0.2425(5) 0.5520(7) 0.092(3) Uani 1 1 d . . . H10A H 0.3709 0.2655 0.5841 0.138 Uiso 1 1 calc R . . H10B H 0.3932 0.1937 0.5353 0.138 Uiso 1 1 calc R . . H10C H 0.4093 0.2667 0.4839 0.138 Uiso 1 1 calc R . . C21 C 0.8828(5) -0.2165(4) 0.0852(7) 0.069(2) Uani 1 1 d . . . C37 C 0.8601(6) -0.0341(5) -0.3339(8) 0.094(3) Uani 1 1 d . . . H37 H 0.8590 -0.0678 -0.3891 0.112 Uiso 1 1 calc R . . C16 C 0.7224(6) 0.3337(5) 0.4520(9) 0.128(4) Uani 1 1 d . A . H16A H 0.6912 0.3569 0.4954 0.191 Uiso 1 1 calc R . . H16B H 0.6860 0.3257 0.3767 0.191 Uiso 1 1 calc R . . H16C H 0.7688 0.3633 0.4496 0.191 Uiso 1 1 calc R . . C32 C 0.3691(8) 0.0159(5) 0.1524(8) 0.109(4) Uani 1 1 d . . . H32 H 0.3724 -0.0073 0.0880 0.131 Uiso 1 1 calc R . . C22 C 0.8312(6) -0.2706(4) 0.1252(8) 0.101(3) Uani 1 1 d . . . H22A H 0.8491 -0.3178 0.1134 0.152 Uiso 1 1 calc R . . H22B H 0.7726 -0.2648 0.0837 0.152 Uiso 1 1 calc R . . H22C H 0.8389 -0.2636 0.2040 0.152 Uiso 1 1 calc R . . C24 C 0.9757(5) -0.2290(5) 0.1503(8) 0.102(3) Uani 1 1 d . . . H24A H 0.9905 -0.2774 0.1399 0.153 Uiso 1 1 calc R . . H24B H 0.9847 -0.2202 0.2290 0.153 Uiso 1 1 calc R . . H24C H 1.0101 -0.1971 0.1229 0.153 Uiso 1 1 calc R . . C27 C 0.7259(6) -0.0792(6) 0.3354(8) 0.123(4) Uani 1 1 d . . . H27A H 0.7350 -0.1291 0.3265 0.184 Uiso 1 1 calc R . . H27B H 0.6804 -0.0733 0.3669 0.184 Uiso 1 1 calc R . . H27C H 0.7763 -0.0583 0.3850 0.184 Uiso 1 1 calc R . . C26 C 0.6227(5) -0.0751(6) 0.1473(8) 0.117(4) Uani 1 1 d . . . H26A H 0.6073 -0.0515 0.0756 0.175 Uiso 1 1 calc R . . H26B H 0.5786 -0.0689 0.1813 0.175 Uiso 1 1 calc R . . H26C H 0.6307 -0.1250 0.1370 0.175 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 C28 0.148(9) 0.079(7) 0.192(11) -0.014(7) 0.126(9) 0.004(6) Co1 0.0552(10) 0.0467(10) 0.0598(11) 0.0009(9) 0.0200(8) -0.0037(8) Co2 0.0608(10) 0.0501(10) 0.0706(12) 0.0002(9) 0.0291(9) 0.0016(8) O3 0.066(3) 0.055(3) 0.076(3) -0.004(3) 0.035(3) 0.004(2) O1 0.059(3) 0.067(3) 0.070(3) 0.005(3) 0.029(3) -0.002(3) O4 0.068(3) 0.047(3) 0.077(3) 0.002(3) 0.034(3) 0.002(2) N1 0.070(4) 0.049(4) 0.071(5) -0.003(4) 0.031(3) -0.010(3) O2 0.065(3) 0.065(4) 0.067(3) 0.002(3) 0.029(3) 0.004(3) C9 0.067(5) 0.062(5) 0.088(6) 0.002(5) 0.030(5) 0.002(4) C3 0.061(5) 0.045(5) 0.060(5) 0.003(4) 0.018(4) 0.002(4) C2 0.065(5) 0.045(5) 0.051(5) 0.013(4) 0.020(4) 0.001(4) C8 0.062(5) 0.046(5) 0.060(5) 0.008(4) 0.020(4) 0.000(4) C4 0.061(4) 0.047(5) 0.055(5) 0.004(4) 0.025(4) -0.002(4) C20 0.062(5) 0.046(5) 0.066(5) 0.001(4) 0.018(4) 0.001(4) C1 0.050(4) 0.071(6) 0.049(5) 0.014(4) 0.017(4) 0.003(4) N2 0.063(4) 0.045(4) 0.081(5) 0.005(4) 0.032(3) 0.003(3) C5 0.068(5) 0.069(6) 0.063(5) 0.012(4) 0.029(4) 0.001(4) C18 0.071(5) 0.055(5) 0.066(5) -0.002(4) 0.027(4) -0.002(4) C19 0.072(5) 0.061(6) 0.057(5) 0.004(4) 0.024(4) -0.010(4) C6 0.067(5) 0.072(6) 0.055(5) 0.015(4) 0.025(4) -0.002(4) C25 0.088(6) 0.078(6) 0.089(7) -0.009(5) 0.053(5) -0.014(5) C7 0.071(5) 0.061(5) 0.078(6) -0.001(4) 0.028(5) -0.007(4) C13 0.076(6) 0.073(6) 0.096(7) 0.008(5) 0.039(5) -0.017(5) C17 0.073(5) 0.052(5) 0.060(5) 0.002(4) 0.027(4) 0.000(4) C29 0.074(6) 0.105(7) 0.074(7) -0.013(5) 0.018(5) 0.014(5) C12 0.097(6) 0.066(6) 0.150(9) -0.020(6) 0.062(6) -0.008(5) C35 0.086(6) 0.068(6) 0.086(7) 0.003(6) 0.020(6) 0.013(5) C11 0.103(7) 0.095(7) 0.096(7) -0.006(6) 0.051(5) 0.006(5) C34 0.078(6) 0.060(6) 0.069(6) -0.003(4) 0.029(5) 0.005(4) C38 0.086(6) 0.042(5) 0.100(7) -0.005(5) 0.024(6) 0.004(4) C31 0.098(7) 0.088(8) 0.086(8) 0.007(6) 0.007(6) -0.017(6) C23 0.129(8) 0.048(5) 0.112(8) -0.011(5) 0.051(6) -0.003(5) C15 0.088(7) 0.147(10) 0.150(10) 0.022(8) 0.018(7) -0.050(7) C30 0.073(6) 0.127(9) 0.088(8) -0.006(7) 0.013(6) 0.021(6) C36 0.092(7) 0.081(7) 0.081(7) 0.003(6) -0.001(5) 0.002(5) C33 0.153(9) 0.052(5) 0.077(7) 0.000(6) 0.049(7) 0.015(5) C10 0.068(6) 0.086(6) 0.119(8) -0.003(6) 0.024(5) 0.012(5) C21 0.080(6) 0.049(5) 0.080(6) 0.005(4) 0.028(5) 0.002(4) C37 0.109(7) 0.062(6) 0.094(8) -0.009(6) 0.007(6) 0.000(6) C16 0.112(8) 0.111(9) 0.173(11) 0.041(8) 0.063(8) -0.025(7) C32 0.193(12) 0.071(7) 0.061(7) -0.001(6) 0.037(7) 0.002(7) C22 0.115(7) 0.048(5) 0.153(9) 0.014(6) 0.059(7) 0.002(5) C24 0.086(7) 0.075(6) 0.137(9) 0.015(6) 0.022(6) 0.017(5) C27 0.147(9) 0.148(10) 0.101(8) 0.026(7) 0.079(7) 0.035(8) C26 0.087(7) 0.148(10) 0.136(9) -0.012(7) 0.063(7) -0.014(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 C28 C25 1.509(11) . ? C40 C39 1.355(16) . ? C40 C41 1.447(17) . ? N40 C39 1.355(16) . ? N40 C41 1.447(17) . ? C41 C39 1.601(19) 3_756 ? C39 C41 1.601(19) 3_756 ? C14A C13 1.534(19) . ? C14B C13 1.518(14) . ? Co1 O2 1.960(5) . ? Co1 O2 1.960(5) 3_656 ? Co1 O1 1.976(5) . ? Co1 O1 1.976(5) 3_656 ? Co1 N1 2.043(6) 3_656 ? Co1 N1 2.043(6) . ? Co2 O4 1.882(4) . ? Co2 O4 1.882(4) 3_755 ? Co2 O3 1.883(5) 3_755 ? Co2 O3 1.883(5) . ? Co2 N2 1.959(6) 3_755 ? Co2 N2 1.959(6) . ? O3 C3 1.325(8) . ? O1 C1 1.315(8) . ? O4 C4 1.318(7) . ? N1 C33 1.320(9) . ? N1 C29 1.320(9) . ? O2 C2 1.307(8) . ? C9 C12 1.517(10) . ? C9 C8 1.526(10) . ? C9 C10 1.530(10) . ? C9 C11 1.538(11) . ? C3 C20 1.409(9) . ? C3 C4 1.411(9) . ? C2 C5 1.429(9) . ? C2 C1 1.431(9) . ? C8 C7 1.386(9) . ? C8 C1 1.436(10) . ? C4 C17 1.404(9) . ? C20 C19 1.398(9) . ? C20 C21 1.525(10) . ? N2 C38 1.335(9) . ? N2 C34 1.337(9) . ? C5 C6 1.357(10) . ? C18 C17 1.379(9) . ? C18 C19 1.415(10) . ? C18 C25 1.543(10) . ? C6 C7 1.423(10) . ? C6 C13 1.548(10) . ? C25 C27 1.508(12) . ? C25 C26 1.532(12) . ? C13 C16 1.516(12) . ? C13 C15 1.517(12) . ? C29 C30 1.378(11) . ? C35 C36 1.363(11) . ? C35 C34 1.374(10) . ? C38 C37 1.388(11) . ? C31 C30 1.345(12) . ? C31 C32 1.355(12) . ? C23 C21 1.534(10) . ? C36 C37 1.374(11) . ? C33 C32 1.369(12) . ? C21 C22 1.525(10) . ? C21 C24 1.543(10) . ? 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 C39 C40 C41 115.0(13) . . ? C39 N40 C41 115.0(13) . . ? N40 C41 C39 121.6(13) . 3_756 ? C40 C41 C39 121.6(13) . 3_756 ? N40 C39 C41 123.3(13) . 3_756 ? C40 C39 C41 123.3(13) . 3_756 ? O2 Co1 O2 180.0(3) . 3_656 ? O2 Co1 O1 83.6(2) . . ? O2 Co1 O1 96.4(2) 3_656 . ? O2 Co1 O1 96.39(19) . 3_656 ? O2 Co1 O1 83.6(2) 3_656 3_656 ? O1 Co1 O1 180.0 . 3_656 ? O2 Co1 N1 89.3(2) . 3_656 ? O2 Co1 N1 90.7(2) 3_656 3_656 ? O1 Co1 N1 90.0(2) . 3_656 ? O1 Co1 N1 90.0(2) 3_656 3_656 ? O2 Co1 N1 90.7(2) . . ? O2 Co1 N1 89.3(2) 3_656 . ? O1 Co1 N1 90.0(2) . . ? O1 Co1 N1 90.0(2) 3_656 . ? N1 Co1 N1 180.000(1) 3_656 . ? O4 Co2 O4 180.0(3) . 3_755 ? O4 Co2 O3 92.87(19) . 3_755 ? O4 Co2 O3 87.13(19) 3_755 3_755 ? O4 Co2 O3 87.13(19) . . ? O4 Co2 O3 92.87(19) 3_755 . ? O3 Co2 O3 180.0(3) 3_755 . ? O4 Co2 N2 90.1(2) . 3_755 ? O4 Co2 N2 89.9(2) 3_755 3_755 ? O3 Co2 N2 91.3(2) 3_755 3_755 ? O3 Co2 N2 88.7(2) . 3_755 ? O4 Co2 N2 89.9(2) . . ? O4 Co2 N2 90.1(2) 3_755 . ? O3 Co2 N2 88.7(2) 3_755 . ? O3 Co2 N2 91.3(2) . . ? N2 Co2 N2 180.0(6) 3_755 . ? C3 O3 Co2 110.1(4) . . ? C1 O1 Co1 111.5(4) . . ? C4 O4 Co2 109.4(4) . . ? C33 N1 C29 116.9(8) . . ? C33 N1 Co1 121.8(6) . . ? C29 N1 Co1 121.3(6) . . ? C2 O2 Co1 110.8(4) . . ? C12 C9 C8 112.6(6) . . ? C12 C9 C10 108.3(7) . . ? C8 C9 C10 109.9(7) . . ? C12 C9 C11 107.3(7) . . ? C8 C9 C11 109.7(6) . . ? C10 C9 C11 108.9(7) . . ? O3 C3 C20 123.6(6) . . ? O3 C3 C4 115.7(6) . . ? C20 C3 C4 120.7(6) . . ? O2 C2 C5 121.7(7) . . ? O2 C2 C1 118.5(6) . . ? C5 C2 C1 119.8(7) . . ? C7 C8 C1 116.1(7) . . ? C7 C8 C9 121.7(7) . . ? C1 C8 C9 122.0(6) . . ? O4 C4 C17 121.8(6) . . ? O4 C4 C3 117.5(6) . . ? C17 C4 C3 120.6(7) . . ? C19 C20 C3 116.6(6) . . ? C19 C20 C21 121.9(7) . . ? C3 C20 C21 121.6(6) . . ? O1 C1 C2 115.6(7) . . ? O1 C1 C8 124.0(6) . . ? C2 C1 C8 120.4(7) . . ? C38 N2 C34 119.4(7) . . ? C38 N2 Co2 121.2(5) . . ? C34 N2 Co2 119.3(6) . . ? C6 C5 C2 120.1(7) . . ? C17 C18 C19 118.4(7) . . ? C17 C18 C25 122.2(7) . . ? C19 C18 C25 119.4(7) . . ? C20 C19 C18 123.7(7) . . ? C5 C6 C7 119.3(7) . . ? C5 C6 C13 122.4(7) . . ? C7 C6 C13 118.3(7) . . ? C27 C25 C28 109.3(8) . . ? C27 C25 C26 108.8(8) . . ? C28 C25 C26 107.4(8) . . ? C27 C25 C18 109.9(7) . . ? C28 C25 C18 112.1(7) . . ? C26 C25 C18 109.2(7) . . ? C8 C7 C6 124.2(7) . . ? C16 C13 C15 105.5(8) . . ? C16 C13 C14B 95.6(13) . . ? C15 C13 C14B 124.4(14) . . ? C16 C13 C14A 120.5(12) . . ? C15 C13 C14A 95.9(13) . . ? C16 C13 C6 110.6(7) . . ? C15 C13 C6 109.0(7) . . ? C14B C13 C6 110.3(10) . . ? C14A C13 C6 113.4(9) . . ? C18 C17 C4 120.0(7) . . ? N1 C29 C30 123.1(8) . . ? C36 C35 C34 118.9(8) . . ? N2 C34 C35 122.1(7) . . ? N2 C38 C37 120.8(8) . . ? C30 C31 C32 119.1(10) . . ? C31 C30 C29 118.8(9) . . ? C35 C36 C37 119.4(9) . . ? N1 C33 C32 123.2(9) . . ? C20 C21 C22 112.8(6) . . ? C20 C21 C23 109.6(6) . . ? C22 C21 C23 107.6(7) . . ? C20 C21 C24 109.7(6) . . ? C22 C21 C24 108.0(7) . . ? C23 C21 C24 109.2(7) . . ? C36 C37 C38 119.3(9) . . ? C31 C32 C33 118.9(9) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 51.42 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.542 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.051 #===END data_compound_1_py_273k _database_code_depnum_ccdc_archive 'CCDC 744068' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H105 Co2 N5 O8' _chemical_formula_weight 1394.63 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.829(4) _cell_length_b 19.017(3) _cell_length_c 12.603(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.581(2) _cell_angle_gamma 90.00 _cell_volume 3845.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 3.816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2971 _exptl_absorpt_correction_T_max 0.5158 _exptl_absorpt_process_details SADABS _exptl_special_details ; Crystals were weakly diffracting and as a result data was only collected to a theta angle of 51.5. ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8474 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 51.44 _reflns_number_total 4036 _reflns_number_gt 2730 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The non-coordinated pyridine molecule is disordered across a centre of symmetry. Two opposing atoms in the pyridine molecule were tentatively assigned as N/C atoms (50% N, 50% C). No hydrogen atoms were assigned on the non-coordinated pyridine molecule. 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^)+(0.0527P)^2^+8.0463P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4036 _refine_ls_number_parameters 422 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1756 _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_restrained_S_all 1.245 _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 C40 C 0.4844(8) 0.9188(7) 0.0076(13) 0.162(5) Uiso 0.50 1 d P . . N3 N 0.4844(8) 0.9188(7) 0.0076(13) 0.162(5) Uiso 0.50 1 d P . . C41 C 0.4519(9) 0.9568(10) -0.0878(14) 0.172(6) Uiso 1 1 d . . . C39 C 0.5324(10) 0.9601(10) 0.1011(14) 0.186(6) Uiso 1 1 d . . . C10A C -0.2881(17) 0.2392(12) 0.084(2) 0.078(9) Uiso 0.49(4) 1 d PD A 1 H10A H -0.2417 0.2312 0.1491 0.118 Uiso 0.49(4) 1 calc PR A 1 H10B H -0.3186 0.1962 0.0622 0.118 Uiso 0.49(4) 1 calc PR A 1 H10C H -0.3241 0.2742 0.0997 0.118 Uiso 0.49(4) 1 calc PR A 1 C10B C -0.3235(16) 0.2226(11) 0.026(3) 0.079(8) Uiso 0.51(4) 1 d P A 2 H10D H -0.2999 0.2056 0.1007 0.118 Uiso 0.51(4) 1 calc PR A 2 H10E H -0.3421 0.1836 -0.0235 0.118 Uiso 0.51(4) 1 calc PR A 2 H10F H -0.3700 0.2527 0.0229 0.118 Uiso 0.51(4) 1 calc PR A 2 C22 C 0.8112(7) 0.0329(5) 0.2605(10) 0.120(4) Uani 1 1 d . B 3 H22A H 0.8246 0.0558 0.3317 0.180 Uiso 1 1 calc R B 3 H22B H 0.7627 0.0545 0.2105 0.180 Uiso 1 1 calc R B 3 H22C H 0.8573 0.0375 0.2310 0.180 Uiso 1 1 calc R B 3 Co2 Co 0.5000 0.0000 0.5000 0.0458(5) Uani 1 2 d S . . O3 O 0.5786(3) 0.0383(2) 0.4373(4) 0.0496(13) Uani 1 1 d . . . O4 O 0.4589(3) 0.0894(2) 0.5215(4) 0.0505(13) Uani 1 1 d . . . C4 C 0.4000(4) 0.0830(4) 0.5707(5) 0.0418(18) Uani 1 1 d . . . C3 C 0.6207(4) -0.0129(4) 0.4082(5) 0.0428(18) Uani 1 1 d . . . C18 C 0.7248(4) -0.0555(4) 0.3283(6) 0.051(2) Uani 1 1 d . . . N2 N 0.5807(3) 0.0075(3) 0.6471(5) 0.0493(16) Uani 1 1 d . . . C19 C 0.2984(4) 0.1243(4) 0.6525(6) 0.051(2) Uani 1 1 d . . . H19 H 0.2706 0.1614 0.6740 0.061 Uiso 1 1 calc R . . C24 C 0.3601(4) 0.1407(4) 0.6037(5) 0.0438(18) Uani 1 1 d . . . C20 C 0.7940(5) -0.0442(5) 0.2738(7) 0.070(2) Uani 1 1 d . . . C17 C 0.6837(4) -0.0004(4) 0.3588(5) 0.0488(19) Uani 1 1 d . . . H17 H 0.6977 0.0456 0.3467 0.059 Uiso 1 1 calc R B . C25 C 0.3838(5) 0.2160(4) 0.5847(7) 0.060(2) Uani 1 1 d . . . C34 C 0.5861(5) -0.0412(4) 0.7248(8) 0.066(2) Uani 1 1 d . . . H34 H 0.5517 -0.0805 0.7076 0.080 Uiso 1 1 calc R . . C38 C 0.6311(5) 0.0631(4) 0.6725(7) 0.058(2) Uani 1 1 d . . . H38 H 0.6266 0.0979 0.6190 0.070 Uiso 1 1 calc R . . C27 C 0.3704(6) 0.2289(4) 0.4614(7) 0.084(3) Uani 1 1 d . . . H27A H 0.3857 0.2764 0.4505 0.127 Uiso 1 1 calc R . . H27B H 0.3127 0.2216 0.4210 0.127 Uiso 1 1 calc R . . H27C H 0.4042 0.1969 0.4348 0.127 Uiso 1 1 calc R . . C35 C 0.6420(6) -0.0346(5) 0.8309(8) 0.085(3) Uani 1 1 d . . . H35 H 0.6432 -0.0682 0.8851 0.103 Uiso 1 1 calc R . . C37 C 0.6897(5) 0.0709(5) 0.7753(8) 0.073(3) Uani 1 1 d . . . H37 H 0.7253 0.1095 0.7899 0.088 Uiso 1 1 calc R . . C28 C 0.3315(6) 0.2700(4) 0.6243(8) 0.089(3) Uani 1 1 d . . . H28A H 0.3484 0.3166 0.6111 0.133 Uiso 1 1 calc R . . H28B H 0.3397 0.2638 0.7024 0.133 Uiso 1 1 calc R . . H28C H 0.2737 0.2635 0.5841 0.133 Uiso 1 1 calc R . . C36 C 0.6950(6) 0.0215(5) 0.8553(8) 0.082(3) Uani 1 1 d . . . H36 H 0.7340 0.0259 0.9253 0.098 Uiso 1 1 calc R . . C26 C 0.4757(5) 0.2282(5) 0.6513(8) 0.093(3) Uani 1 1 d . . . H26A H 0.4912 0.2755 0.6397 0.139 Uiso 1 1 calc R . . H26B H 0.5102 0.1958 0.6266 0.139 Uiso 1 1 calc R . . H26C H 0.4831 0.2209 0.7290 0.139 Uiso 1 1 calc R . . C21 C 0.8753(6) -0.0752(6) 0.3496(9) 0.117(4) Uani 1 1 d . B . H21A H 0.8899 -0.0521 0.4206 0.176 Uiso 1 1 calc R . . H21B H 0.9190 -0.0683 0.3162 0.176 Uiso 1 1 calc R . . H21C H 0.8682 -0.1246 0.3594 0.176 Uiso 1 1 calc R . . C23 C 0.7731(7) -0.0799(6) 0.1627(8) 0.127(4) Uani 1 1 d . B . H23A H 0.7630 -0.1290 0.1714 0.191 Uiso 1 1 calc R . . H23B H 0.8188 -0.0748 0.1326 0.191 Uiso 1 1 calc R . . H23C H 0.7241 -0.0589 0.1130 0.191 Uiso 1 1 calc R . . Co1 Co 0.0000 0.0000 0.0000 0.0424(5) Uani 1 2 d S . . O1 O -0.0963(3) 0.0438(3) 0.0363(4) 0.0532(13) Uani 1 1 d . . . O2 O 0.0086(3) 0.0973(2) -0.0598(4) 0.0502(13) Uani 1 1 d . . . N1 N 0.0808(4) 0.0301(3) 0.1541(5) 0.0499(16) Uani 1 1 d . . . C13 C 0.0008(5) 0.2462(4) -0.1379(7) 0.058(2) Uani 1 1 d . . . C2 C -0.0500(4) 0.1389(4) -0.0488(5) 0.0463(19) Uani 1 1 d . . . C5 C -0.0604(4) 0.2106(4) -0.0863(6) 0.0476(19) Uani 1 1 d . A . C8 C -0.1726(4) 0.1509(4) 0.0193(6) 0.054(2) Uani 1 1 d . . . H8 H -0.2082 0.1320 0.0555 0.065 Uiso 1 1 calc R . . C1 C -0.1067(4) 0.1091(4) 0.0049(6) 0.0439(18) Uani 1 1 d . . . C15 C 0.0011(5) 0.2081(5) -0.2443(7) 0.085(3) Uani 1 1 d . . . H15A H 0.0394 0.2309 -0.2761 0.128 Uiso 1 1 calc R . . H15B H -0.0539 0.2093 -0.2965 0.128 Uiso 1 1 calc R . . H15C H 0.0178 0.1601 -0.2272 0.128 Uiso 1 1 calc R . . C7 C -0.1844(4) 0.2175(4) -0.0185(6) 0.055(2) Uani 1 1 d . A . C9 C -0.2569(5) 0.2644(5) -0.0090(8) 0.070(2) Uani 1 1 d D . . C33 C 0.1361(6) 0.0810(5) 0.1640(8) 0.079(3) Uani 1 1 d . . . H33 H 0.1372 0.1047 0.1000 0.094 Uiso 1 1 calc R . . C6 C -0.1275(5) 0.2465(4) -0.0704(6) 0.058(2) Uani 1 1 d . . . H6 H -0.1360 0.2928 -0.0953 0.069 Uiso 1 1 calc R A . C16 C -0.0205(5) 0.3229(4) -0.1661(8) 0.092(3) Uani 1 1 d . . . H16A H 0.0191 0.3429 -0.1986 0.138 Uiso 1 1 calc R . . H16B H -0.0187 0.3482 -0.0995 0.138 Uiso 1 1 calc R . . H16C H -0.0755 0.3263 -0.2180 0.138 Uiso 1 1 calc R . . C31 C 0.1902(6) 0.0679(6) 0.3569(8) 0.086(3) Uani 1 1 d . . . H31 H 0.2265 0.0812 0.4255 0.104 Uiso 1 1 calc R . . C14 C 0.0889(5) 0.2430(5) -0.0542(8) 0.085(3) Uani 1 1 d . . . H14A H 0.1278 0.2650 -0.0860 0.128 Uiso 1 1 calc R . . H14B H 0.1046 0.1948 -0.0373 0.128 Uiso 1 1 calc R . . H14C H 0.0893 0.2671 0.0128 0.128 Uiso 1 1 calc R . . C11 C -0.2241(6) 0.3340(5) 0.0457(10) 0.121(4) Uani 1 1 d . A . H11A H -0.1927 0.3571 0.0037 0.182 Uiso 1 1 calc R . . H11B H -0.1889 0.3257 0.1202 0.182 Uiso 1 1 calc R . . H11C H -0.2701 0.3633 0.0478 0.182 Uiso 1 1 calc R . . C32 C 0.1919(5) 0.1008(6) 0.2637(9) 0.090(3) Uani 1 1 d . . . H32 H 0.2302 0.1365 0.2663 0.108 Uiso 1 1 calc R . . C30 C 0.1353(8) 0.0153(5) 0.3500(8) 0.101(4) Uani 1 1 d . . . H30 H 0.1338 -0.0094 0.4132 0.121 Uiso 1 1 calc R . . C29 C 0.0814(6) -0.0010(5) 0.2470(8) 0.082(3) Uani 1 1 d . . . H29 H 0.0427 -0.0366 0.2430 0.099 Uiso 1 1 calc R . . C12 C -0.3126(6) 0.2828(6) -0.1241(9) 0.123(4) Uani 1 1 d . A . H12A H -0.2802 0.3057 -0.1650 0.185 Uiso 1 1 calc R . . H12B H -0.3561 0.3138 -0.1182 0.185 Uiso 1 1 calc R . . H12C H -0.3368 0.2406 -0.1623 0.185 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 C22 0.146(10) 0.083(8) 0.189(12) 0.016(8) 0.136(9) 0.002(7) Co2 0.0507(10) 0.0388(10) 0.0539(11) -0.0007(9) 0.0246(8) -0.0016(9) O3 0.057(3) 0.037(3) 0.064(3) -0.001(3) 0.032(3) 0.000(2) O4 0.055(3) 0.040(3) 0.066(3) -0.001(3) 0.032(3) -0.003(2) C4 0.049(4) 0.039(5) 0.037(4) -0.005(4) 0.011(4) -0.002(4) C3 0.052(5) 0.036(5) 0.044(4) 0.002(4) 0.020(4) 0.002(4) C18 0.058(5) 0.048(5) 0.053(5) 0.008(4) 0.026(4) 0.008(4) N2 0.056(4) 0.032(4) 0.069(4) 0.003(4) 0.032(3) -0.001(3) C19 0.062(5) 0.045(5) 0.049(5) -0.008(4) 0.021(4) 0.009(4) C24 0.050(5) 0.037(5) 0.042(4) -0.003(4) 0.011(4) -0.002(4) C20 0.075(6) 0.069(6) 0.084(7) 0.008(5) 0.052(5) 0.012(5) C17 0.059(5) 0.044(5) 0.049(4) -0.001(4) 0.024(4) -0.005(4) C25 0.068(6) 0.039(5) 0.075(6) -0.003(5) 0.026(5) 0.002(4) C34 0.077(6) 0.038(5) 0.082(7) -0.004(5) 0.021(6) -0.008(5) C38 0.065(5) 0.049(6) 0.063(6) 0.001(5) 0.024(5) -0.006(5) C27 0.130(8) 0.039(5) 0.093(7) 0.023(5) 0.047(6) 0.002(5) C35 0.112(8) 0.055(6) 0.071(7) 0.009(6) 0.001(6) -0.003(6) C37 0.074(6) 0.064(6) 0.077(7) -0.009(6) 0.015(6) -0.012(5) C28 0.107(7) 0.045(6) 0.123(8) -0.018(6) 0.047(6) -0.002(5) C36 0.089(7) 0.076(7) 0.062(6) 0.001(6) -0.006(5) 0.003(6) C26 0.075(7) 0.066(6) 0.129(9) -0.018(6) 0.017(6) -0.017(5) C21 0.076(7) 0.154(11) 0.144(10) 0.020(8) 0.067(7) 0.012(7) C23 0.158(10) 0.167(12) 0.087(8) -0.047(8) 0.083(8) -0.052(9) Co1 0.0440(10) 0.0364(10) 0.0475(10) 0.0005(9) 0.0147(8) 0.0043(8) O1 0.054(3) 0.054(4) 0.058(3) -0.003(3) 0.026(3) -0.004(3) O2 0.050(3) 0.050(3) 0.054(3) -0.002(3) 0.021(3) 0.001(3) N1 0.059(4) 0.038(4) 0.056(5) 0.005(4) 0.023(3) 0.007(3) C13 0.057(5) 0.049(5) 0.073(6) 0.004(5) 0.026(5) -0.002(4) C2 0.039(4) 0.059(6) 0.042(5) -0.012(4) 0.013(4) -0.001(4) C5 0.050(5) 0.038(5) 0.052(5) -0.002(4) 0.012(4) 0.000(4) C8 0.053(5) 0.058(6) 0.056(5) -0.005(5) 0.022(4) -0.002(4) C1 0.049(5) 0.037(5) 0.047(5) -0.010(4) 0.015(4) 0.000(4) C15 0.096(7) 0.089(7) 0.089(7) 0.003(6) 0.056(6) -0.007(6) C7 0.051(5) 0.064(6) 0.054(5) -0.009(5) 0.023(4) 0.005(4) C9 0.064(6) 0.069(6) 0.085(7) -0.009(5) 0.036(5) 0.016(5) C33 0.070(6) 0.097(8) 0.065(6) 0.018(6) 0.014(5) -0.012(6) C6 0.060(5) 0.046(5) 0.068(6) 0.000(4) 0.023(5) 0.009(4) C16 0.089(7) 0.060(6) 0.144(9) 0.022(6) 0.059(7) 0.004(5) C31 0.095(8) 0.089(9) 0.061(7) -0.004(7) 0.001(6) 0.029(7) C14 0.058(6) 0.084(7) 0.109(8) 0.008(6) 0.017(6) -0.016(5) C11 0.107(8) 0.101(9) 0.168(11) -0.040(8) 0.061(8) 0.030(7) C32 0.064(6) 0.118(9) 0.077(7) -0.002(7) 0.003(6) -0.024(6) C30 0.188(12) 0.058(7) 0.051(7) 0.002(6) 0.028(7) -0.001(7) C29 0.138(9) 0.046(6) 0.066(7) -0.005(6) 0.037(6) -0.013(6) C12 0.079(7) 0.131(10) 0.147(11) -0.021(8) 0.014(7) 0.050(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 C40 C41 1.367(17) . ? C40 C39 1.443(17) . ? N3 C41 1.367(17) . ? N3 C39 1.443(17) . ? C41 C39 1.619(19) 3_675 ? C39 C41 1.619(19) 3_675 ? C10A C9 1.498(14) . ? C10B C9 1.543(19) . ? C22 C20 1.515(11) . ? Co2 O3 1.880(4) . ? Co2 O3 1.880(4) 3_656 ? Co2 O4 1.886(4) 3_656 ? Co2 O4 1.886(4) . ? Co2 N2 1.944(6) . ? Co2 N2 1.944(6) 3_656 ? O3 C3 1.321(7) . ? O4 C4 1.326(7) . ? C4 C24 1.412(9) . ? C4 C3 1.422(9) 3_656 ? C3 C17 1.402(9) . ? C3 C4 1.422(9) 3_656 ? C18 C17 1.374(9) . ? C18 C19 1.407(10) 3_656 ? C18 C20 1.535(10) . ? N2 C34 1.330(9) . ? N2 C38 1.333(9) . ? C19 C24 1.393(9) . ? C19 C18 1.407(10) 3_656 ? C24 C25 1.526(10) . ? C20 C23 1.499(12) . ? C20 C21 1.531(12) . ? C25 C27 1.521(10) . ? C25 C28 1.530(10) . ? C25 C26 1.538(10) . ? C34 C35 1.390(11) . ? C38 C37 1.380(10) . ? C35 C36 1.366(12) . ? C37 C36 1.361(11) . ? Co1 O1 1.995(4) 3 ? Co1 O1 1.995(4) . ? Co1 O2 2.020(5) 3 ? Co1 O2 2.020(5) . ? Co1 N1 2.087(6) . ? Co1 N1 2.087(6) 3 ? O1 C1 1.298(8) . ? O2 C2 1.304(8) . ? N1 C29 1.308(10) . ? N1 C33 1.321(10) . ? C13 C16 1.519(10) . ? C13 C15 1.525(10) . ? C13 C5 1.532(10) . ? C13 C14 1.540(10) . ? C2 C5 1.436(10) . ? C2 C1 1.443(9) . ? C5 C6 1.385(9) . ? C8 C7 1.345(10) . ? C8 C1 1.420(9) . ? C7 C6 1.424(10) . ? C7 C9 1.545(10) . ? C9 C12 1.512(12) . ? C9 C11 1.518(12) . ? C33 C32 1.374(11) . ? C31 C32 1.339(12) . ? C31 C30 1.347(12) . ? C30 C29 1.376(12) . ? 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 C41 C40 C39 114.0(14) . . ? C41 N3 C39 114.0(14) . . ? N3 C41 C39 124.9(14) . 3_675 ? C40 C41 C39 124.9(14) . 3_675 ? N3 C39 C41 121.0(14) . 3_675 ? C40 C39 C41 121.0(14) . 3_675 ? O3 Co2 O3 180.00(16) . 3_656 ? O3 Co2 O4 87.39(19) . 3_656 ? O3 Co2 O4 92.61(19) 3_656 3_656 ? O3 Co2 O4 92.61(19) . . ? O3 Co2 O4 87.39(19) 3_656 . ? O4 Co2 O4 180.000(1) 3_656 . ? O3 Co2 N2 89.7(2) . . ? O3 Co2 N2 90.3(2) 3_656 . ? O4 Co2 N2 91.3(2) 3_656 . ? O4 Co2 N2 88.7(2) . . ? O3 Co2 N2 90.3(2) . 3_656 ? O3 Co2 N2 89.7(2) 3_656 3_656 ? O4 Co2 N2 88.7(2) 3_656 3_656 ? O4 Co2 N2 91.3(2) . 3_656 ? N2 Co2 N2 180.0(3) . 3_656 ? C3 O3 Co2 109.6(4) . . ? C4 O4 Co2 110.0(4) . . ? O4 C4 C24 123.8(6) . . ? O4 C4 C3 115.7(6) . 3_656 ? C24 C4 C3 120.5(6) . 3_656 ? O3 C3 C17 122.6(6) . . ? O3 C3 C4 117.2(6) . 3_656 ? C17 C3 C4 120.2(7) . 3_656 ? C17 C18 C19 118.2(6) . 3_656 ? C17 C18 C20 122.2(7) . . ? C19 C18 C20 119.6(7) 3_656 . ? C34 N2 C38 118.6(7) . . ? C34 N2 Co2 121.6(5) . . ? C38 N2 Co2 119.8(6) . . ? C24 C19 C18 124.5(7) . 3_656 ? C19 C24 C4 116.1(6) . . ? C19 C24 C25 123.0(7) . . ? C4 C24 C25 120.9(6) . . ? C23 C20 C22 109.5(8) . . ? C23 C20 C21 108.7(8) . . ? C22 C20 C21 106.0(8) . . ? C23 C20 C18 111.1(7) . . ? C22 C20 C18 112.4(7) . . ? C21 C20 C18 108.9(7) . . ? C18 C17 C3 120.4(7) . . ? C27 C25 C24 110.2(6) . . ? C27 C25 C28 107.6(7) . . ? C24 C25 C28 112.0(6) . . ? C27 C25 C26 110.4(7) . . ? C24 C25 C26 108.9(6) . . ? C28 C25 C26 107.7(7) . . ? N2 C34 C35 121.5(8) . . ? N2 C38 C37 122.2(8) . . ? C36 C35 C34 119.5(9) . . ? C36 C37 C38 119.4(8) . . ? C37 C36 C35 118.8(9) . . ? O1 Co1 O1 180.0(3) 3 . ? O1 Co1 O2 81.79(19) 3 3 ? O1 Co1 O2 98.21(19) . 3 ? O1 Co1 O2 98.21(19) 3 . ? O1 Co1 O2 81.79(19) . . ? O2 Co1 O2 180.0(3) 3 . ? O1 Co1 N1 89.0(2) 3 . ? O1 Co1 N1 91.0(2) . . ? O2 Co1 N1 90.2(2) 3 . ? O2 Co1 N1 89.8(2) . . ? O1 Co1 N1 91.0(2) 3 3 ? O1 Co1 N1 89.0(2) . 3 ? O2 Co1 N1 89.8(2) 3 3 ? O2 Co1 N1 90.2(2) . 3 ? N1 Co1 N1 180.0(5) . 3 ? C1 O1 Co1 112.0(4) . . ? C2 O2 Co1 112.0(4) . . ? C29 N1 C33 115.6(8) . . ? C29 N1 Co1 122.4(6) . . ? C33 N1 Co1 122.1(6) . . ? C16 C13 C15 108.3(7) . . ? C16 C13 C5 112.4(6) . . ? C15 C13 C5 110.2(6) . . ? C16 C13 C14 108.0(7) . . ? C15 C13 C14 109.0(7) . . ? C5 C13 C14 108.9(6) . . ? O2 C2 C5 124.2(6) . . ? O2 C2 C1 116.1(7) . . ? C5 C2 C1 119.7(7) . . ? C6 C5 C2 116.4(7) . . ? C6 C5 C13 121.8(7) . . ? C2 C5 C13 121.9(6) . . ? C7 C8 C1 121.4(7) . . ? O1 C1 C8 122.4(7) . . ? O1 C1 C2 118.1(6) . . ? C8 C1 C2 119.4(7) . . ? C8 C7 C6 118.6(7) . . ? C8 C7 C9 123.5(7) . . ? C6 C7 C9 117.9(7) . . ? C10A C9 C12 124.2(14) . . ? C10A C9 C11 95.1(13) . . ? C12 C9 C11 105.6(8) . . ? C12 C9 C10B 95.8(13) . . ? C11 C9 C10B 121.0(12) . . ? C10A C9 C7 110.3(10) . . ? C12 C9 C7 109.5(7) . . ? C11 C9 C7 110.6(7) . . ? C10B C9 C7 112.6(9) . . ? N1 C33 C32 123.6(8) . . ? C5 C6 C7 124.5(7) . . ? C32 C31 C30 119.1(10) . . ? C31 C32 C33 119.0(10) . . ? C31 C30 C29 118.1(10) . . ? N1 C29 C30 124.6(9) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 51.44 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.616 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.055 #===END data_compound_1_py_rt _database_code_depnum_ccdc_archive 'CCDC 744069' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H105 Co2 N5 O8' _chemical_formula_weight 1394.63 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.836(4) _cell_length_b 19.038(6) _cell_length_c 12.611(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.490(3) _cell_angle_gamma 90.00 _cell_volume 3855(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 3.816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2978 _exptl_absorpt_correction_T_max 0.5166 _exptl_absorpt_process_details SADABS _exptl_special_details ; Crystals were weakly diffracting and as a result data was only collected to a theta angle of 51.5. ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9136 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 51.50 _reflns_number_total 4111 _reflns_number_gt 2661 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The non-coordinated pyridine molecule is disordered across a centre of symmetry. Two opposing atoms in the pyridine molecule were tentatively assigned as N/C atoms (50% N, 50% C). No hydrogen atoms were assigned on the non-coordinated pyridine molecule. 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^)+(0.0900P)^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_number_reflns 4111 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1750 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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 C40 C 0.9842(6) 0.9186(6) 0.5069(10) 0.173(4) Uiso 0.50 1 d P . . N3 N 0.9842(6) 0.9186(6) 0.5069(10) 0.173(4) Uiso 0.50 1 d P . . C41 C 0.9535(7) 0.9585(8) 0.4120(11) 0.182(5) Uiso 1 1 d . . . C39 C 1.0308(8) 0.9609(8) 0.6021(11) 0.201(5) Uiso 1 1 d . . . C10A C 0.2070(11) 0.2374(8) 0.5807(18) 0.081(6) Uiso 0.51(3) 1 d P A 1 H10A H 0.1832 0.1917 0.5608 0.121 Uiso 0.51(3) 1 calc PR A 1 H10B H 0.1647 0.2691 0.5883 0.121 Uiso 0.51(3) 1 calc PR A 1 H10C H 0.2507 0.2346 0.6500 0.121 Uiso 0.51(3) 1 calc PR A 1 C10B C 0.1733(12) 0.2213(9) 0.517(2) 0.088(7) Uiso 0.49(3) 1 d P A 2 H10D H 0.1621 0.1796 0.4720 0.132 Uiso 0.49(3) 1 calc PR A 2 H10E H 0.1236 0.2492 0.5015 0.132 Uiso 0.49(3) 1 calc PR A 2 H10F H 0.1911 0.2085 0.5941 0.132 Uiso 0.49(3) 1 calc PR A 2 Co1 Co 0.5000 0.0000 0.5000 0.0462(4) Uani 1 2 d S . . Co2 Co 0.0000 0.0000 0.0000 0.0488(4) Uani 1 2 d S . . O3 O -0.0408(2) 0.08910(17) 0.0218(3) 0.0517(10) Uani 1 1 d . . . O4 O 0.0783(2) 0.03801(19) -0.0635(3) 0.0533(10) Uani 1 1 d . . . O2 O 0.5077(2) 0.09840(19) 0.4394(3) 0.0543(10) Uani 1 1 d . . . C3 C -0.0998(3) 0.0832(3) 0.0706(4) 0.0444(14) Uani 1 1 d . . . O1 O 0.4031(2) 0.0446(2) 0.5364(3) 0.0581(10) Uani 1 1 d . . . N1 N 0.5813(3) 0.0306(3) 0.6565(4) 0.0542(12) Uani 1 1 d . . . C4 C 0.1207(3) -0.0125(3) -0.0922(4) 0.0428(14) Uani 1 1 d . . . C5 C 0.4388(3) 0.2114(3) 0.4136(4) 0.0492(14) Uani 1 1 d . . . C1 C 0.3927(3) 0.1101(3) 0.5048(4) 0.0494(14) Uani 1 1 d . . . C18 C -0.1392(3) 0.1405(3) 0.1035(4) 0.0480(14) Uani 1 1 d . . . C20 C -0.2244(3) 0.0554(3) 0.1721(4) 0.0512(15) Uani 1 1 d . . . C13 C 0.5005(3) 0.2466(3) 0.3630(5) 0.0625(17) Uani 1 1 d . . . C2 C 0.4492(3) 0.1394(3) 0.4502(4) 0.0484(15) Uani 1 1 d . . . C8 C 0.3261(3) 0.1512(3) 0.5173(5) 0.0572(16) Uani 1 1 d . . . H8 H 0.2895 0.1317 0.5516 0.069 Uiso 1 1 calc R . . C19 C -0.2008(3) 0.1249(3) 0.1526(4) 0.0546(15) Uani 1 1 d . . . H19 H -0.2283 0.1621 0.1740 0.066 Uiso 1 1 calc R . . N2 N 0.0808(3) 0.0069(2) 0.1472(4) 0.0521(12) Uani 1 1 d . . . C21 C -0.2933(4) 0.0447(3) 0.2263(6) 0.0729(18) Uani 1 1 d . . . C33 C 0.6365(4) 0.0825(4) 0.6651(6) 0.082(2) Uani 1 1 d . . . H33 H 0.6377 0.1057 0.6007 0.098 Uiso 1 1 calc R . . C6 C 0.3718(3) 0.2457(3) 0.4287(5) 0.0598(16) Uani 1 1 d . . . H6 H 0.3629 0.2915 0.4025 0.072 Uiso 1 1 calc R . . C17 C 0.1829(3) -0.0007(3) -0.1419(4) 0.0523(15) Uani 1 1 d . . . H17 H 0.1966 0.0452 -0.1548 0.063 Uiso 1 1 calc R . . C7 C 0.3145(3) 0.2180(3) 0.4806(5) 0.0591(16) Uani 1 1 d . A . C9 C 0.2427(4) 0.2644(4) 0.4894(6) 0.077(2) Uani 1 1 d . . . C15 C 0.4791(4) 0.3236(3) 0.3344(6) 0.098(2) Uani 1 1 d . . . H15A H 0.5191 0.3435 0.3025 0.147 Uiso 1 1 calc R . . H15B H 0.4803 0.3489 0.4008 0.147 Uiso 1 1 calc R . . H15C H 0.4245 0.3268 0.2819 0.147 Uiso 1 1 calc R . . C38 C 0.1305(4) 0.0625(3) 0.1715(5) 0.0630(17) Uani 1 1 d . . . H38 H 0.1255 0.0969 0.1177 0.076 Uiso 1 1 calc R . . C22 C -0.3091(5) -0.0324(4) 0.2421(8) 0.132(3) Uani 1 1 d . . . H22A H -0.3230 -0.0559 0.1716 0.197 Uiso 1 1 calc R . . H22B H -0.3545 -0.0369 0.2730 0.197 Uiso 1 1 calc R . . H22C H -0.2600 -0.0531 0.2917 0.197 Uiso 1 1 calc R . . C25 C -0.1155(4) 0.2157(3) 0.0850(5) 0.0627(17) Uani 1 1 d . . . C37 C 0.1887(4) 0.0709(4) 0.2731(7) 0.078(2) Uani 1 1 d . . . H37 H 0.2232 0.1101 0.2877 0.093 Uiso 1 1 calc R . . C34 C 0.0864(4) -0.0423(3) 0.2238(6) 0.0695(18) Uani 1 1 d . . . H34 H 0.0526 -0.0818 0.2061 0.083 Uiso 1 1 calc R . . C35 C 0.1420(5) -0.0357(4) 0.3300(6) 0.092(2) Uani 1 1 d . . . H35 H 0.1429 -0.0689 0.3845 0.110 Uiso 1 1 calc R . . C32 C 0.6916(4) 0.1031(5) 0.7647(7) 0.096(2) Uani 1 1 d . . . H32 H 0.7283 0.1401 0.7677 0.115 Uiso 1 1 calc R . . C29 C 0.5842(5) -0.0019(3) 0.7505(6) 0.086(2) Uani 1 1 d . . . H29 H 0.5473 -0.0388 0.7474 0.103 Uiso 1 1 calc R . . C14 C 0.5011(4) 0.2090(4) 0.2562(5) 0.091(2) Uani 1 1 d . . . H14A H 0.5401 0.2317 0.2253 0.136 Uiso 1 1 calc R . . H14B H 0.4465 0.2108 0.2035 0.136 Uiso 1 1 calc R . . H14C H 0.5173 0.1609 0.2726 0.136 Uiso 1 1 calc R . . C26 C -0.1282(4) 0.2289(3) -0.0383(6) 0.092(2) Uani 1 1 d . . . H26A H -0.1128 0.2764 -0.0487 0.138 Uiso 1 1 calc R . . H26B H -0.1856 0.2215 -0.0792 0.138 Uiso 1 1 calc R . . H26C H -0.0940 0.1971 -0.0646 0.138 Uiso 1 1 calc R . . C31 C 0.6912(5) 0.0689(5) 0.8575(7) 0.094(2) Uani 1 1 d . . . H31 H 0.7276 0.0821 0.9259 0.113 Uiso 1 1 calc R . . C36 C 0.1952(4) 0.0201(4) 0.3534(6) 0.084(2) Uani 1 1 d . . . H36 H 0.2353 0.0238 0.4224 0.101 Uiso 1 1 calc R . . C12 C 0.2741(4) 0.3337(4) 0.5451(7) 0.127(3) Uani 1 1 d . A . H12A H 0.3069 0.3569 0.5050 0.190 Uiso 1 1 calc R . . H12B H 0.3078 0.3253 0.6202 0.190 Uiso 1 1 calc R . . H12C H 0.2276 0.3628 0.5454 0.190 Uiso 1 1 calc R . . C16 C 0.5885(3) 0.2436(3) 0.4451(6) 0.088(2) Uani 1 1 d . . . H16A H 0.6269 0.2657 0.4125 0.131 Uiso 1 1 calc R . . H16B H 0.6044 0.1955 0.4620 0.131 Uiso 1 1 calc R . . H16C H 0.5894 0.2679 0.5122 0.131 Uiso 1 1 calc R . . C27 C -0.1679(4) 0.2695(3) 0.1235(7) 0.100(2) Uani 1 1 d . . . H27A H -0.1508 0.3160 0.1106 0.149 Uiso 1 1 calc R . . H27B H -0.1604 0.2633 0.2015 0.149 Uiso 1 1 calc R . . H27C H -0.2256 0.2631 0.0828 0.149 Uiso 1 1 calc R . . C30 C 0.6381(7) 0.0156(4) 0.8514(6) 0.108(3) Uani 1 1 d . . . H30 H 0.6379 -0.0091 0.9150 0.130 Uiso 1 1 calc R . . C28 C -0.0237(4) 0.2281(3) 0.1510(6) 0.098(2) Uani 1 1 d . . . H28A H -0.0085 0.2755 0.1395 0.148 Uiso 1 1 calc R . . H28B H 0.0108 0.1960 0.1259 0.148 Uiso 1 1 calc R . . H28C H -0.0161 0.2206 0.2287 0.148 Uiso 1 1 calc R . . C11 C 0.1866(4) 0.2826(5) 0.3746(7) 0.131(3) Uani 1 1 d . A . H11A H 0.2185 0.3058 0.3335 0.196 Uiso 1 1 calc R . . H11B H 0.1429 0.3131 0.3809 0.196 Uiso 1 1 calc R . . H11C H 0.1629 0.2403 0.3366 0.196 Uiso 1 1 calc R . . C24 C -0.2731(5) 0.0802(5) 0.3375(6) 0.134(3) Uani 1 1 d . . . H24A H -0.2223 0.0611 0.3860 0.200 Uiso 1 1 calc R . . H24B H -0.3176 0.0725 0.3691 0.200 Uiso 1 1 calc R . . H24C H -0.2663 0.1297 0.3285 0.200 Uiso 1 1 calc R . . C23 C -0.3746(4) 0.0753(5) 0.1511(7) 0.132(3) Uani 1 1 d . . . H23A H -0.3887 0.0527 0.0798 0.197 Uiso 1 1 calc R . . H23B H -0.3679 0.1248 0.1420 0.197 Uiso 1 1 calc R . . H23C H -0.4183 0.0676 0.1842 0.197 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 Co1 0.0455(7) 0.0413(8) 0.0532(8) 0.0006(7) 0.0169(6) 0.0038(6) Co2 0.0515(8) 0.0405(8) 0.0617(9) -0.0013(7) 0.0282(7) -0.0006(6) O3 0.060(2) 0.038(2) 0.069(3) 0.0012(19) 0.037(2) -0.0032(18) O4 0.056(2) 0.042(2) 0.071(3) -0.005(2) 0.033(2) 0.0052(19) O2 0.049(2) 0.056(2) 0.062(3) 0.000(2) 0.023(2) 0.001(2) C3 0.043(3) 0.043(4) 0.047(4) -0.006(3) 0.013(3) -0.002(3) O1 0.053(2) 0.060(3) 0.066(3) 0.005(2) 0.024(2) 0.000(2) N1 0.056(3) 0.049(3) 0.057(4) -0.001(3) 0.018(3) 0.010(3) C4 0.050(3) 0.045(4) 0.039(3) 0.003(3) 0.021(3) 0.000(3) C5 0.046(3) 0.049(4) 0.052(4) 0.001(3) 0.014(3) 0.004(3) C1 0.046(3) 0.054(4) 0.048(4) -0.004(3) 0.014(3) -0.003(3) C18 0.049(3) 0.045(4) 0.051(4) -0.002(3) 0.017(3) 0.000(3) C20 0.055(3) 0.053(4) 0.051(4) 0.001(3) 0.025(3) 0.004(3) C13 0.055(4) 0.059(4) 0.076(4) 0.001(4) 0.023(4) 0.000(3) C2 0.040(3) 0.055(4) 0.053(4) -0.009(3) 0.018(3) -0.002(3) C8 0.047(3) 0.067(4) 0.063(4) -0.004(4) 0.025(3) 0.002(3) C19 0.065(4) 0.047(4) 0.054(4) 0.001(3) 0.021(3) 0.010(3) N2 0.050(3) 0.038(3) 0.070(4) -0.004(3) 0.022(3) -0.003(3) C21 0.084(5) 0.066(5) 0.088(5) 0.011(4) 0.056(4) 0.016(4) C33 0.071(4) 0.101(6) 0.071(5) 0.019(4) 0.018(4) -0.011(4) C6 0.062(4) 0.052(4) 0.069(4) -0.003(3) 0.024(3) 0.006(3) C17 0.060(4) 0.045(4) 0.057(4) 0.005(3) 0.025(3) 0.003(3) C7 0.056(4) 0.064(5) 0.064(4) -0.011(4) 0.027(3) 0.005(3) C9 0.068(4) 0.082(5) 0.095(6) -0.010(4) 0.043(4) 0.013(4) C15 0.092(5) 0.064(5) 0.156(7) 0.024(5) 0.064(5) 0.008(4) C38 0.064(4) 0.066(5) 0.057(4) 0.001(4) 0.016(4) 0.000(4) C22 0.169(8) 0.087(6) 0.202(10) 0.009(6) 0.151(8) -0.004(6) C25 0.076(4) 0.038(4) 0.079(5) -0.005(3) 0.029(4) 0.001(3) C37 0.076(5) 0.061(5) 0.092(6) 0.002(5) 0.019(5) -0.007(4) C34 0.086(5) 0.039(4) 0.079(5) -0.001(4) 0.018(4) -0.005(3) C35 0.121(6) 0.066(5) 0.072(5) 0.011(4) 0.003(5) -0.009(5) C32 0.069(5) 0.129(7) 0.075(6) 0.001(6) -0.001(5) -0.026(5) C29 0.142(7) 0.063(5) 0.054(5) -0.005(4) 0.032(5) -0.013(4) C14 0.094(5) 0.105(6) 0.089(5) 0.001(5) 0.051(4) -0.009(4) C26 0.133(6) 0.057(4) 0.094(6) 0.017(4) 0.048(5) -0.008(4) C31 0.099(6) 0.093(7) 0.074(6) -0.012(5) 0.002(5) 0.023(5) C36 0.088(5) 0.073(5) 0.072(5) -0.004(4) -0.005(4) 0.003(4) C12 0.108(6) 0.113(7) 0.166(9) -0.061(6) 0.051(6) 0.025(5) C16 0.059(4) 0.086(5) 0.114(6) 0.009(4) 0.019(4) -0.013(4) C27 0.119(5) 0.048(4) 0.149(7) -0.018(4) 0.067(5) 0.004(4) C30 0.195(9) 0.076(6) 0.047(5) 0.002(4) 0.026(6) 0.004(6) C28 0.078(5) 0.073(5) 0.135(7) -0.022(5) 0.018(5) -0.023(4) C11 0.083(5) 0.157(9) 0.140(8) -0.021(7) 0.015(6) 0.058(6) C24 0.160(7) 0.173(9) 0.100(7) -0.048(6) 0.089(6) -0.046(7) C23 0.085(5) 0.184(10) 0.148(8) 0.033(7) 0.069(6) 0.023(6) _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 C40 C41 1.380(13) . ? C40 C39 1.463(14) . ? N3 C41 1.380(13) . ? N3 C39 1.463(14) . ? C41 C39 1.576(16) 3_776 ? C39 C41 1.576(16) 3_776 ? C10A C9 1.539(14) . ? C10B C9 1.549(15) . ? Co1 O1 2.010(3) . ? Co1 O1 2.010(3) 3_656 ? Co1 O2 2.042(4) . ? Co1 O2 2.042(4) 3_656 ? Co1 N1 2.118(5) . ? Co1 N1 2.118(5) 3_656 ? Co2 O4 1.880(3) . ? Co2 O4 1.880(3) 3 ? Co2 O3 1.881(3) . ? Co2 O3 1.881(3) 3 ? Co2 N2 1.949(5) . ? Co2 N2 1.949(5) 3 ? O3 C3 1.321(6) . ? O4 C4 1.311(6) . ? O2 C2 1.295(6) . ? C3 C18 1.403(7) . ? C3 C4 1.438(7) 3 ? O1 C1 1.306(6) . ? N1 C29 1.325(7) . ? N1 C33 1.338(7) . ? C4 C17 1.391(7) . ? C4 C3 1.438(7) 3 ? C5 C6 1.365(7) . ? C5 C2 1.441(7) . ? C5 C13 1.527(7) . ? C1 C8 1.414(7) . ? C1 C2 1.444(7) . ? C18 C19 1.391(7) . ? C18 C25 1.522(7) . ? C20 C17 1.370(7) 3 ? C20 C19 1.424(7) . ? C20 C21 1.526(8) . ? C13 C14 1.529(8) . ? C13 C15 1.527(8) . ? C13 C16 1.533(7) . ? C8 C7 1.348(7) . ? N2 C34 1.328(7) . ? N2 C38 1.326(7) . ? C21 C24 1.501(9) . ? C21 C22 1.514(9) . ? C21 C23 1.527(9) . ? C33 C32 1.375(9) . ? C6 C7 1.419(7) . ? C17 C20 1.370(7) 3 ? C7 C9 1.528(8) . ? C9 C11 1.512(9) . ? C9 C12 1.514(9) . ? C38 C37 1.368(8) . ? C25 C27 1.523(8) . ? C25 C26 1.525(8) . ? C25 C28 1.538(8) . ? C37 C36 1.382(9) . ? C34 C35 1.390(8) . ? C35 C36 1.363(9) . ? C32 C31 1.341(9) . ? C29 C30 1.364(10) . ? C31 C30 1.340(10) . ? 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 C41 C40 C39 112.1(11) . . ? C41 N3 C39 112.1(11) . . ? N3 C41 C39 127.0(11) . 3_776 ? C40 C41 C39 127.0(11) . 3_776 ? N3 C39 C41 120.7(11) . 3_776 ? C40 C39 C41 120.7(11) . 3_776 ? O1 Co1 O1 180.00(19) . 3_656 ? O1 Co1 O2 81.09(15) . . ? O1 Co1 O2 98.91(15) 3_656 . ? O1 Co1 O2 98.91(15) . 3_656 ? O1 Co1 O2 81.09(15) 3_656 3_656 ? O2 Co1 O2 180.00(8) . 3_656 ? O1 Co1 N1 90.74(15) . . ? O1 Co1 N1 89.26(15) 3_656 . ? O2 Co1 N1 90.05(17) . . ? O2 Co1 N1 89.95(17) 3_656 . ? O1 Co1 N1 89.26(15) . 3_656 ? O1 Co1 N1 90.74(15) 3_656 3_656 ? O2 Co1 N1 89.95(17) . 3_656 ? O2 Co1 N1 90.05(17) 3_656 3_656 ? N1 Co1 N1 180.000(1) . 3_656 ? O4 Co2 O4 180.0(3) . 3 ? O4 Co2 O3 92.79(14) . . ? O4 Co2 O3 87.21(14) 3 . ? O4 Co2 O3 87.21(14) . 3 ? O4 Co2 O3 92.79(14) 3 3 ? O3 Co2 O3 180.0(3) . 3 ? O4 Co2 N2 90.10(18) . . ? O4 Co2 N2 89.90(18) 3 . ? O3 Co2 N2 88.92(16) . . ? O3 Co2 N2 91.08(16) 3 . ? O4 Co2 N2 89.90(18) . 3 ? O4 Co2 N2 90.10(18) 3 3 ? O3 Co2 N2 91.08(16) . 3 ? O3 Co2 N2 88.92(16) 3 3 ? N2 Co2 N2 180.0(3) . 3 ? C3 O3 Co2 110.5(3) . . ? C4 O4 Co2 110.2(3) . . ? C2 O2 Co1 112.2(3) . . ? O3 C3 C18 124.0(5) . . ? O3 C3 C4 115.4(5) . 3 ? C18 C3 C4 120.5(5) . 3 ? C1 O1 Co1 112.2(3) . . ? C29 N1 C33 115.8(6) . . ? C29 N1 Co1 123.0(5) . . ? C33 N1 Co1 121.1(5) . . ? O4 C4 C17 123.6(5) . . ? O4 C4 C3 116.7(4) . 3 ? C17 C4 C3 119.8(5) . 3 ? C6 C5 C2 115.9(5) . . ? C6 C5 C13 122.9(5) . . ? C2 C5 C13 121.3(5) . . ? O1 C1 C8 122.2(5) . . ? O1 C1 C2 117.8(5) . . ? C8 C1 C2 119.9(6) . . ? C19 C18 C3 116.6(5) . . ? C19 C18 C25 122.2(5) . . ? C3 C18 C25 121.2(5) . . ? C17 C20 C19 117.8(5) 3 . ? C17 C20 C21 122.8(5) 3 . ? C19 C20 C21 119.4(5) . . ? C14 C13 C5 110.4(5) . . ? C14 C13 C15 107.8(6) . . ? C5 C13 C15 112.2(5) . . ? C14 C13 C16 108.4(5) . . ? C5 C13 C16 110.0(5) . . ? C15 C13 C16 107.8(5) . . ? O2 C2 C5 124.2(5) . . ? O2 C2 C1 116.7(5) . . ? C5 C2 C1 119.1(5) . . ? C7 C8 C1 121.5(6) . . ? C18 C19 C20 124.0(5) . . ? C34 N2 C38 119.5(5) . . ? C34 N2 Co2 121.5(4) . . ? C38 N2 Co2 119.0(4) . . ? C24 C21 C22 108.2(6) . . ? C24 C21 C20 111.6(6) . . ? C22 C21 C20 112.1(5) . . ? C24 C21 C23 108.5(6) . . ? C22 C21 C23 106.9(6) . . ? C20 C21 C23 109.3(5) . . ? N1 C33 C32 123.1(6) . . ? C5 C6 C7 126.3(6) . . ? C20 C17 C4 121.2(5) 3 . ? C8 C7 C6 117.4(5) . . ? C8 C7 C9 123.8(6) . . ? C6 C7 C9 118.8(6) . . ? C11 C9 C12 106.0(7) . . ? C11 C9 C7 110.0(5) . . ? C12 C9 C7 111.3(5) . . ? C11 C9 C10A 121.4(9) . . ? C12 C9 C10A 96.0(9) . . ? C7 C9 C10A 111.0(7) . . ? C11 C9 C10B 92.2(10) . . ? C12 C9 C10B 122.6(10) . . ? C7 C9 C10B 112.2(8) . . ? N2 C38 C37 122.3(6) . . ? C27 C25 C26 107.3(5) . . ? C27 C25 C18 112.4(5) . . ? C26 C25 C18 110.4(5) . . ? C27 C25 C28 108.0(5) . . ? C26 C25 C28 109.6(5) . . ? C18 C25 C28 109.2(5) . . ? C38 C37 C36 118.7(6) . . ? N2 C34 C35 121.2(6) . . ? C36 C35 C34 119.2(7) . . ? C31 C32 C33 118.7(8) . . ? N1 C29 C30 123.8(7) . . ? C30 C31 C32 119.7(8) . . ? C35 C36 C37 119.0(7) . . ? C31 C30 C29 119.0(8) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 51.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.562 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.067 #===END data_compound_1_mecn _database_code_depnum_ccdc_archive 'CCDC 744070' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H62 Co N6 O4' _chemical_formula_weight 821.95 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' O O 0.0106 0.0060 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.181(5) _cell_length_b 8.875(2) _cell_length_c 18.171(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.949(5) _cell_angle_gamma 90.00 _cell_volume 4496.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756 _exptl_absorpt_coefficient_mu 0.429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9003 _exptl_absorpt_correction_T_max 0.9583 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13753 _diffrn_reflns_av_R_equivalents 0.1206 _diffrn_reflns_av_sigmaI/netI 0.1813 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.53 _reflns_number_total 5121 _reflns_number_gt 2634 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0200P)^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_number_reflns 5121 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 0.786 _refine_ls_restrained_S_all 0.786 _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 Co01 Co 0.5000 0.0000 0.5000 0.01771(16) Uani 1 2 d S . . O1 O 0.44403(7) -0.1024(2) 0.47914(13) 0.0199(5) Uani 1 1 d . . . O2 O 0.47283(6) 0.1756(2) 0.51682(13) 0.0186(5) Uani 1 1 d . . . N1 N 0.52848(8) -0.0487(3) 0.61985(17) 0.0207(6) Uani 1 1 d . . . C19 C 0.54560(11) 0.0608(4) 0.6795(2) 0.0263(8) Uani 1 1 d . . . H4 H 0.5438 0.1625 0.6618 0.032 Uiso 1 1 calc R . . C3 C 0.40086(10) 0.2513(3) 0.51902(19) 0.0174(7) Uani 1 1 d . . . C1 C 0.41452(10) -0.0085(3) 0.48764(18) 0.0175(7) Uani 1 1 d . . . N3 N 0.38552(13) 0.5705(4) 0.2417(2) 0.0671(12) Uani 1 1 d . . . C2 C 0.43026(10) 0.1439(3) 0.50923(19) 0.0159(7) Uani 1 1 d . . . N2 N 0.27613(12) 0.4508(4) 0.3047(2) 0.0553(10) Uani 1 1 d . . . C22 C 0.36644(13) 0.6560(4) 0.2604(2) 0.0405(10) Uani 1 1 d . . . C11 C 0.41653(11) 0.4171(3) 0.5407(2) 0.0202(7) Uani 1 1 d . . . C6 C 0.37069(10) -0.0544(3) 0.47806(19) 0.0171(7) Uani 1 1 d . . . H013 H 0.3609 -0.1564 0.4645 0.021 Uiso 1 1 calc R . . C4 C 0.35779(10) 0.1977(3) 0.50958(19) 0.0206(7) Uani 1 1 d . . . H014 H 0.3381 0.2668 0.5182 0.025 Uiso 1 1 calc R . . C10 C 0.25333(11) 0.1089(4) 0.4162(2) 0.0320(9) Uani 1 1 d . . . H01A H 0.2225 0.0795 0.4106 0.048 Uiso 1 1 calc R . . H01B H 0.2513 0.1034 0.3606 0.048 Uiso 1 1 calc R . . H01C H 0.2611 0.2123 0.4379 0.048 Uiso 1 1 calc R . . C5 C 0.34135(10) 0.0473(3) 0.4881(2) 0.0193(7) Uani 1 1 d . . . C12 C 0.42646(12) 0.4841(3) 0.4725(2) 0.0315(8) Uani 1 1 d . . . H01D H 0.4366 0.5893 0.4864 0.047 Uiso 1 1 calc R . . H01E H 0.3972 0.4791 0.4168 0.047 Uiso 1 1 calc R . . H01F H 0.4519 0.4261 0.4709 0.047 Uiso 1 1 calc R . . C16 C 0.55157(11) -0.2298(4) 0.7310(2) 0.0296(9) Uani 1 1 d . . . H018 H 0.5537 -0.3324 0.7474 0.035 Uiso 1 1 calc R . . C8 C 0.27855(10) -0.1577(3) 0.4436(2) 0.0308(9) Uani 1 1 d . . . H01G H 0.2477 -0.1832 0.4391 0.046 Uiso 1 1 calc R . . H01H H 0.3031 -0.2291 0.4819 0.046 Uiso 1 1 calc R . . H01I H 0.2756 -0.1632 0.3873 0.046 Uiso 1 1 calc R . . C15 C 0.53147(10) -0.1914(4) 0.6463(2) 0.0253(8) Uani 1 1 d . . . H020 H 0.5192 -0.2694 0.6050 0.030 Uiso 1 1 calc R . . C18 C 0.56573(11) 0.0305(3) 0.7655(2) 0.0306(9) Uani 1 1 d . . . H021 H 0.5774 0.1097 0.8060 0.037 Uiso 1 1 calc R . . C17 C 0.56839(11) -0.1181(4) 0.7908(2) 0.0340(9) Uani 1 1 d . . . H022 H 0.5818 -0.1422 0.8492 0.041 Uiso 1 1 calc R . . C13 C 0.46174(11) 0.4271(3) 0.6280(2) 0.0311(9) Uani 1 1 d . . . H02A H 0.4716 0.5327 0.6411 0.047 Uiso 1 1 calc R . . H02B H 0.4875 0.3689 0.6277 0.047 Uiso 1 1 calc R . . H02C H 0.4551 0.3863 0.6712 0.047 Uiso 1 1 calc R . . C7 C 0.29294(10) 0.0013(4) 0.4787(2) 0.0232(7) Uani 1 1 d . . . C14 C 0.37764(11) 0.5142(3) 0.5425(2) 0.0310(8) Uani 1 1 d . . . H02D H 0.3889 0.6185 0.5562 0.046 Uiso 1 1 calc R . . H02E H 0.3707 0.4752 0.5856 0.046 Uiso 1 1 calc R . . H02F H 0.3484 0.5110 0.4867 0.046 Uiso 1 1 calc R . . C20 C 0.29656(13) 0.3532(5) 0.2961(3) 0.0426(11) Uani 1 1 d . . . C9 C 0.29679(11) 0.0104(4) 0.5663(2) 0.0327(8) Uani 1 1 d . . . H02G H 0.2662 -0.0192 0.5613 0.049 Uiso 1 1 calc R . . H02H H 0.3045 0.1139 0.5876 0.049 Uiso 1 1 calc R . . H02I H 0.3221 -0.0576 0.6057 0.049 Uiso 1 1 calc R . . C21 C 0.32208(13) 0.2283(4) 0.2836(3) 0.0518(11) Uani 1 1 d . . . H21A H 0.2989 0.1541 0.2450 0.078 Uiso 1 1 calc R . . H21B H 0.3434 0.1805 0.3384 0.078 Uiso 1 1 calc R . . H21C H 0.3411 0.2666 0.2590 0.078 Uiso 1 1 calc R . . C23 C 0.34262(13) 0.7657(4) 0.2866(2) 0.0500(11) Uani 1 1 d . . . H23A H 0.3224 0.7129 0.3046 0.075 Uiso 1 1 calc R . . H23B H 0.3226 0.8324 0.2388 0.075 Uiso 1 1 calc R . . H23C H 0.3668 0.8256 0.3340 0.075 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 Co01 0.0179(3) 0.0138(3) 0.0225(4) -0.0019(3) 0.0109(3) -0.0011(3) O1 0.0171(11) 0.0161(12) 0.0278(14) 0.0002(10) 0.0120(11) 0.0003(9) O2 0.0183(11) 0.0107(11) 0.0288(14) -0.0024(9) 0.0131(11) -0.0013(9) N1 0.0194(14) 0.0159(14) 0.0297(18) 0.0001(12) 0.0145(14) 0.0003(11) C19 0.0283(19) 0.0175(17) 0.031(2) -0.0026(16) 0.0131(18) -0.0014(14) C3 0.0195(17) 0.0160(17) 0.0172(19) 0.0005(14) 0.0096(15) 0.0008(13) C1 0.0188(15) 0.0140(16) 0.0184(17) 0.0020(15) 0.0084(14) 0.0040(15) N3 0.082(3) 0.069(3) 0.059(3) -0.003(2) 0.041(3) 0.017(2) C2 0.0195(16) 0.0148(17) 0.0125(18) 0.0004(13) 0.0074(15) -0.0004(13) N2 0.056(2) 0.050(2) 0.053(3) 0.0068(19) 0.023(2) 0.0034(18) C22 0.044(2) 0.043(3) 0.032(3) -0.003(2) 0.017(2) -0.005(2) C11 0.0244(18) 0.0123(17) 0.023(2) -0.0022(14) 0.0110(17) 0.0003(13) C6 0.0209(17) 0.0140(16) 0.0168(18) -0.0014(13) 0.0096(16) -0.0021(13) C4 0.0226(17) 0.0190(17) 0.0184(19) 0.0001(14) 0.0088(16) 0.0063(14) C10 0.0231(19) 0.032(2) 0.039(2) 0.0010(18) 0.0135(19) 0.0016(16) C5 0.0215(17) 0.0180(17) 0.0197(19) 0.0029(14) 0.0113(16) 0.0002(13) C12 0.047(2) 0.0169(18) 0.036(2) 0.0016(17) 0.0245(19) -0.0012(17) C16 0.035(2) 0.024(2) 0.031(2) 0.0087(17) 0.0180(19) 0.0001(16) C8 0.0235(19) 0.027(2) 0.046(3) 0.0010(18) 0.020(2) -0.0029(15) C15 0.0258(19) 0.0230(19) 0.031(2) -0.0002(16) 0.0166(18) -0.0002(15) C18 0.034(2) 0.027(2) 0.023(2) -0.0064(16) 0.0079(18) -0.0018(15) C17 0.037(2) 0.041(2) 0.020(2) -0.0009(18) 0.0110(19) -0.0003(18) C13 0.031(2) 0.0188(19) 0.035(2) -0.0081(16) 0.0110(19) -0.0006(15) C7 0.0218(16) 0.0206(16) 0.0278(19) 0.0041(18) 0.0128(15) 0.0020(16) C14 0.0351(19) 0.0159(18) 0.042(2) -0.0064(17) 0.0194(19) -0.0001(16) C20 0.041(2) 0.041(3) 0.034(3) 0.004(2) 0.009(2) -0.007(2) C9 0.0320(19) 0.0310(19) 0.042(2) -0.0020(19) 0.0234(19) -0.0029(17) C21 0.050(3) 0.053(3) 0.043(3) -0.004(2) 0.015(2) -0.002(2) C23 0.053(3) 0.057(3) 0.041(3) -0.016(2) 0.024(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co01 O1 1.8792(18) . ? Co01 O1 1.8792(18) 5_656 ? Co01 O2 1.8855(18) 5_656 ? Co01 O2 1.8855(18) . ? Co01 N1 1.943(3) 5_656 ? Co01 N1 1.943(3) . ? O1 C1 1.329(3) . ? O2 C2 1.337(3) . ? N1 C15 1.341(3) . ? N1 C19 1.351(4) . ? C19 C18 1.387(4) . ? C3 C4 1.393(4) . ? C3 C2 1.415(4) . ? C3 C11 1.542(4) . ? C1 C6 1.393(4) . ? C1 C2 1.429(4) . ? N3 C22 1.131(4) . ? N2 C20 1.145(4) . ? C22 C23 1.458(5) . ? C11 C13 1.528(4) . ? C11 C14 1.533(4) . ? C11 C12 1.546(4) . ? C6 C5 1.382(4) . ? C4 C5 1.417(4) . ? C10 C7 1.543(4) . ? C5 C7 1.536(4) . ? C16 C17 1.367(4) . ? C16 C15 1.381(4) . ? C8 C7 1.522(4) . ? C18 C17 1.385(4) . ? C7 C9 1.535(4) . ? C20 C21 1.463(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 O1 Co01 O1 180.00(7) . 5_656 ? O1 Co01 O2 92.46(8) . 5_656 ? O1 Co01 O2 87.54(8) 5_656 5_656 ? O1 Co01 O2 87.54(8) . . ? O1 Co01 O2 92.46(8) 5_656 . ? O2 Co01 O2 180.00(12) 5_656 . ? O1 Co01 N1 90.76(9) . 5_656 ? O1 Co01 N1 89.24(9) 5_656 5_656 ? O2 Co01 N1 89.99(9) 5_656 5_656 ? O2 Co01 N1 90.01(9) . 5_656 ? O1 Co01 N1 89.24(9) . . ? O1 Co01 N1 90.76(9) 5_656 . ? O2 Co01 N1 90.01(9) 5_656 . ? O2 Co01 N1 89.99(9) . . ? N1 Co01 N1 180.00(8) 5_656 . ? C1 O1 Co01 110.00(17) . . ? C2 O2 Co01 110.10(16) . . ? C15 N1 C19 117.7(3) . . ? C15 N1 Co01 121.4(2) . . ? C19 N1 Co01 120.9(2) . . ? N1 C19 C18 122.5(3) . . ? C4 C3 C2 116.2(3) . . ? C4 C3 C11 122.4(3) . . ? C2 C3 C11 121.4(2) . . ? O1 C1 C6 122.7(3) . . ? O1 C1 C2 116.7(2) . . ? C6 C1 C2 120.6(3) . . ? O2 C2 C3 124.1(2) . . ? O2 C2 C1 115.6(2) . . ? C3 C2 C1 120.3(3) . . ? N3 C22 C23 178.7(5) . . ? C13 C11 C14 108.1(2) . . ? C13 C11 C3 109.9(2) . . ? C14 C11 C3 112.1(2) . . ? C13 C11 C12 109.8(2) . . ? C14 C11 C12 107.4(3) . . ? C3 C11 C12 109.5(3) . . ? C5 C6 C1 120.6(3) . . ? C3 C4 C5 124.6(3) . . ? C6 C5 C4 117.8(3) . . ? C6 C5 C7 122.2(3) . . ? C4 C5 C7 120.0(3) . . ? C17 C16 C15 119.1(3) . . ? N1 C15 C16 122.8(3) . . ? C17 C18 C19 118.4(3) . . ? C16 C17 C18 119.5(3) . . ? C8 C7 C9 109.5(3) . . ? C8 C7 C5 111.9(2) . . ? C9 C7 C5 108.6(3) . . ? C8 C7 C10 107.4(3) . . ? C9 C7 C10 109.8(3) . . ? C5 C7 C10 109.7(2) . . ? N2 C20 C21 179.1(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.830 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.073 #===END data_compound_1_hex_130K _database_code_depnum_ccdc_archive 'CCDC 744071' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H220 Co3 N6 O12' _chemical_formula_weight 2404.05 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' O O 0.0492 0.0322 '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' Co Co -2.3653 3.6143 '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 20.456(7) _cell_length_b 15.477(5) _cell_length_c 23.064(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.183(4) _cell_angle_gamma 90.00 _cell_volume 7013(4) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2606 _exptl_absorpt_coefficient_mu 3.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5024 _exptl_absorpt_correction_T_max 0.7842 _exptl_absorpt_process_details SADABS _exptl_special_details ; Crystals were weakly diffracting and as a result data was only collected to a theta angle of 51.3. ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15525 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.1269 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 51.28 _reflns_number_total 7167 _reflns_number_gt 3790 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0929P)^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_number_reflns 7167 _refine_ls_number_parameters 713 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.907 _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 Co2 Co 0.0000 0.0000 0.0000 0.0362(4) Uani 1 2 d S . . Co1 Co 0.37854(5) 0.82648(7) 0.18975(5) 0.0402(4) Uani 1 1 d . . . O5 O -0.0517(2) -0.0593(2) 0.04232(18) 0.0361(11) Uani 1 1 d . . . O1 O 0.3600(2) 0.8576(3) 0.26127(18) 0.0454(12) Uani 1 1 d . . . O6 O 0.0522(2) -0.0980(2) -0.00399(19) 0.0346(11) Uani 1 1 d . . . O2 O 0.3000(2) 0.7599(3) 0.17144(19) 0.0399(12) Uani 1 1 d . . . O3 O 0.4603(2) 0.8940(3) 0.2059(2) 0.0409(12) Uani 1 1 d . . . O4 O 0.3972(2) 0.7968(3) 0.11602(19) 0.0390(12) Uani 1 1 d . . . N1 N 0.3272(3) 0.9260(3) 0.1510(3) 0.0361(14) Uani 1 1 d . . . N3 N -0.0637(3) -0.0320(4) -0.0758(2) 0.0379(15) Uani 1 1 d . . . N2 N 0.4334(3) 0.7307(4) 0.2302(3) 0.0416(15) Uani 1 1 d . . . C5 C -0.0959(3) -0.0060(4) 0.0571(3) 0.0333(17) Uani 1 1 d . . . C6 C 0.0969(3) -0.0816(4) -0.0348(3) 0.0327(17) Uani 1 1 d . . . C4 C 0.4524(4) 0.8342(4) 0.1111(3) 0.0363(17) Uani 1 1 d . . . C2 C 0.2636(3) 0.7781(4) 0.2106(3) 0.0362(18) Uani 1 1 d . . . C37 C 0.1413(3) -0.1420(4) -0.0465(3) 0.0368(18) Uani 1 1 d . . . H016 H 0.1413 -0.1992 -0.0314 0.044 Uiso 1 1 calc R . . C7 C 0.2645(3) 0.8544(4) 0.3023(3) 0.0385(18) Uani 1 1 d . . . H017 H 0.2877 0.8910 0.3347 0.046 Uiso 1 1 calc R . . C33 C -0.1415(4) -0.1223(5) 0.1131(3) 0.048(2) Uani 1 1 d . . . C1 C 0.2957(3) 0.8302(4) 0.2593(3) 0.0358(17) Uani 1 1 d . . . C21 C 0.5364(4) 0.8673(5) 0.0580(3) 0.0425(19) Uani 1 1 d . . . C47 C 0.2857(3) 0.9218(4) 0.0954(3) 0.0363(18) Uani 1 1 d . . . H021 H 0.2787 0.8675 0.0753 0.044 Uiso 1 1 calc R . . C15 C 0.1597(3) 0.6882(4) 0.1522(3) 0.0455(19) Uani 1 1 d . . . C39 C 0.2349(3) -0.1868(4) -0.0941(3) 0.0455(19) Uani 1 1 d . . . C10 C 0.1971(3) 0.7484(4) 0.2044(3) 0.0384(18) Uani 1 1 d . . . C31 C -0.1412(3) -0.0292(4) 0.0905(3) 0.0369(18) Uani 1 1 d . . . C19 C 0.5498(3) 0.9311(4) 0.1604(3) 0.0422(19) Uani 1 1 d . . . C17 C 0.0870(3) 0.6684(5) 0.1532(3) 0.060(2) Uani 1 1 d . . . H02A H 0.0877 0.6412 0.1918 0.090 Uiso 1 1 calc R . . H02B H 0.0659 0.6289 0.1201 0.090 Uiso 1 1 calc R . . H02C H 0.0608 0.7221 0.1485 0.090 Uiso 1 1 calc R . . C46 C 0.2525(3) 0.9933(5) 0.0660(3) 0.0441(19) Uani 1 1 d . . . H028 H 0.2240 0.9887 0.0258 0.053 Uiso 1 1 calc R . . C42 C 0.2224(4) -0.1908(4) -0.1628(3) 0.055(2) Uani 1 1 d . . . H02D H 0.1755 -0.2093 -0.1818 0.083 Uiso 1 1 calc R . . H02E H 0.2540 -0.2321 -0.1726 0.083 Uiso 1 1 calc R . . H02F H 0.2296 -0.1334 -0.1780 0.083 Uiso 1 1 calc R . . C56 C -0.1361(4) 0.0053(5) -0.1733(3) 0.048(2) Uani 1 1 d . . . H030 H -0.1541 0.0492 -0.2021 0.057 Uiso 1 1 calc R . . C32 C -0.1846(3) 0.0353(4) 0.1004(3) 0.0399(18) Uani 1 1 d . . . H031 H -0.2157 0.0206 0.1227 0.048 Uiso 1 1 calc R . . C55 C -0.1536(3) -0.0803(6) -0.1858(3) 0.050(2) Uani 1 1 d . . . H032 H -0.1841 -0.0966 -0.2233 0.061 Uiso 1 1 calc R . . C11 C 0.1635(4) 0.8530(4) 0.3450(3) 0.049(2) Uani 1 1 d . . . C20 C 0.5707(3) 0.9194(4) 0.1090(3) 0.0451(19) Uani 1 1 d . . . H034 H 0.6111 0.9482 0.1071 0.054 Uiso 1 1 calc R . . C8 C 0.1984(4) 0.8251(4) 0.2986(3) 0.0394(18) Uani 1 1 d . . . C38 C 0.1851(3) -0.1209(5) -0.0794(3) 0.0402(19) Uani 1 1 d . . . C25 C 0.5433(4) 1.0576(4) 0.2271(3) 0.062(2) Uani 1 1 d . . . H03A H 0.5693 1.0916 0.2617 0.093 Uiso 1 1 calc R . . H03B H 0.5033 1.0326 0.2363 0.093 Uiso 1 1 calc R . . H03C H 0.5285 1.0950 0.1916 0.093 Uiso 1 1 calc R . . C45 C 0.2610(4) 1.0717(5) 0.0954(4) 0.0428(19) Uani 1 1 d . . . H038 H 0.2380 1.1218 0.0761 0.051 Uiso 1 1 calc R . . C27 C 0.5658(4) 0.8582(5) 0.0044(3) 0.049(2) Uani 1 1 d . . . C9 C 0.1672(4) 0.7740(4) 0.2495(3) 0.0424(19) Uani 1 1 d . . . H040 H 0.1222 0.7547 0.2461 0.051 Uiso 1 1 calc R . . C3 C 0.4879(3) 0.8893(4) 0.1618(3) 0.0395(19) Uani 1 1 d . . . C18 C 0.1568(3) 0.7306(4) 0.0910(3) 0.047(2) Uani 1 1 d . . . H04A H 0.2031 0.7440 0.0895 0.070 Uiso 1 1 calc R . . H04B H 0.1302 0.7841 0.0866 0.070 Uiso 1 1 calc R . . H04C H 0.1354 0.6908 0.0582 0.070 Uiso 1 1 calc R . . C16 C 0.2003(4) 0.6026(4) 0.1568(3) 0.054(2) Uani 1 1 d . . . H04D H 0.2469 0.6152 0.1559 0.082 Uiso 1 1 calc R . . H04E H 0.1783 0.5651 0.1227 0.082 Uiso 1 1 calc R . . H04F H 0.2013 0.5733 0.1947 0.082 Uiso 1 1 calc R . . C24 C 0.6136(4) 0.9280(5) 0.2693(3) 0.062(2) Uani 1 1 d . . . H04G H 0.6393 0.9635 0.3031 0.093 Uiso 1 1 calc R . . H04H H 0.6430 0.8821 0.2613 0.093 Uiso 1 1 calc R . . H04I H 0.5744 0.9020 0.2793 0.093 Uiso 1 1 calc R . . C57 C -0.0914(4) 0.0254(5) -0.1177(3) 0.0437(19) Uani 1 1 d . . . H045 H -0.0800 0.0844 -0.1092 0.052 Uiso 1 1 calc R . . C69 C 0.2944(6) 0.9462(8) 0.5650(5) 0.151(5) Uiso 1 1 d . . . H69J H 0.2805 0.8865 0.5696 0.227 Uiso 1 1 calc R . . H69K H 0.2652 0.9706 0.5275 0.227 Uiso 1 1 calc R . . H69L H 0.2902 0.9807 0.5994 0.227 Uiso 1 1 calc R . . C34 C -0.0704(4) -0.1475(4) 0.1537(3) 0.060(2) Uani 1 1 d . . . H04J H -0.0368 -0.1416 0.1308 0.090 Uiso 1 1 calc R . . H04K H -0.0712 -0.2075 0.1670 0.090 Uiso 1 1 calc R . . H04L H -0.0580 -0.1094 0.1890 0.090 Uiso 1 1 calc R . . C41 C 0.3081(3) -0.1588(5) -0.0641(3) 0.058(2) Uani 1 1 d . . . H04M H 0.3159 -0.1569 -0.0202 0.088 Uiso 1 1 calc R . . H04N H 0.3158 -0.1013 -0.0788 0.088 Uiso 1 1 calc R . . H04O H 0.3395 -0.2003 -0.0740 0.088 Uiso 1 1 calc R . . C22 C 0.4776(4) 0.8264(4) 0.0602(3) 0.0419(18) Uani 1 1 d . . . H049 H 0.4534 0.7923 0.0269 0.050 Uiso 1 1 calc R . . C48 C 0.4322(4) 0.6525(5) 0.2049(4) 0.053(2) Uani 1 1 d . . . H050 H 0.4009 0.6420 0.1666 0.064 Uiso 1 1 calc R . . C54 C -0.1258(3) -0.1410(5) -0.1428(4) 0.0455(19) Uani 1 1 d . . . H051 H -0.1364 -0.2004 -0.1506 0.055 Uiso 1 1 calc R . . C23 C 0.5890(3) 0.9836(5) 0.2139(3) 0.049(2) Uani 1 1 d . . . C63 C 0.1776(7) 0.7961(7) 0.6741(5) 0.144(5) Uani 1 1 d . . . H63A H 0.1527 0.7418 0.6730 0.216 Uiso 1 1 calc R . . H63B H 0.2157 0.7982 0.7110 0.216 Uiso 1 1 calc R . . H63C H 0.1951 0.7995 0.6387 0.216 Uiso 1 1 calc R . . C44 C 0.3035(4) 1.0761(5) 0.1532(4) 0.047(2) Uani 1 1 d . . . H054 H 0.3101 1.1293 0.1746 0.057 Uiso 1 1 calc R . . C43 C 0.3363(3) 1.0020(5) 0.1798(3) 0.0465(19) Uani 1 1 d . . . H055 H 0.3661 1.0052 0.2195 0.056 Uiso 1 1 calc R . . C35 C -0.1921(4) -0.1330(5) 0.1513(3) 0.059(2) Uani 1 1 d . . . H05A H -0.1912 -0.1929 0.1652 0.089 Uiso 1 1 calc R . . H05B H -0.2381 -0.1185 0.1266 0.089 Uiso 1 1 calc R . . H05C H -0.1791 -0.0943 0.1862 0.089 Uiso 1 1 calc R . . C14 C 0.1651(5) 0.9526(4) 0.3515(4) 0.086(3) Uani 1 1 d . . . H05D H 0.1423 0.9695 0.3819 0.129 Uiso 1 1 calc R . . H05E H 0.1416 0.9789 0.3127 0.129 Uiso 1 1 calc R . . H05F H 0.2125 0.9724 0.3641 0.129 Uiso 1 1 calc R . . C26 C 0.6508(4) 1.0299(5) 0.2016(3) 0.068(2) Uani 1 1 d . . . H05G H 0.6749 1.0630 0.2373 0.102 Uiso 1 1 calc R . . H05H H 0.6349 1.0691 0.1671 0.102 Uiso 1 1 calc R . . H05I H 0.6816 0.9868 0.1924 0.102 Uiso 1 1 calc R . . C40 C 0.2239(4) -0.2772(4) -0.0722(4) 0.068(2) Uani 1 1 d . . . H06A H 0.1771 -0.2958 -0.0916 0.102 Uiso 1 1 calc R . . H06B H 0.2316 -0.2764 -0.0283 0.102 Uiso 1 1 calc R . . H06C H 0.2558 -0.3176 -0.0825 0.102 Uiso 1 1 calc R . . C12 C 0.2018(4) 0.8183(5) 0.4074(3) 0.080(3) Uani 1 1 d . . . H06D H 0.1789 0.8373 0.4372 0.120 Uiso 1 1 calc R . . H06E H 0.2486 0.8403 0.4186 0.120 Uiso 1 1 calc R . . H06F H 0.2026 0.7550 0.4062 0.120 Uiso 1 1 calc R . . C53 C -0.0823(3) -0.1158(5) -0.0879(3) 0.0439(19) Uani 1 1 d . . . H062 H -0.0649 -0.1584 -0.0579 0.053 Uiso 1 1 calc R . . C66 C 0.4962(8) 0.8678(10) 0.4410(7) 0.180(6) Uiso 1 1 d . . . H66G H 0.5028 0.8223 0.4130 0.217 Uiso 1 1 calc R . . H66H H 0.5236 0.8514 0.4821 0.217 Uiso 1 1 calc R . . C36 C -0.1631(4) -0.1836(4) 0.0588(3) 0.063(2) Uani 1 1 d . . . H06G H -0.1314 -0.1780 0.0341 0.094 Uiso 1 1 calc R . . H06H H -0.2092 -0.1687 0.0345 0.094 Uiso 1 1 calc R . . H06I H -0.1626 -0.2433 0.0731 0.094 Uiso 1 1 calc R . . C50 C 0.5191(5) 0.6022(7) 0.2887(5) 0.080(3) Uani 1 1 d . . . H065 H 0.5487 0.5576 0.3087 0.096 Uiso 1 1 calc R . . C49 C 0.4743(4) 0.5878(5) 0.2324(5) 0.068(2) Uani 1 1 d . . . H066 H 0.4730 0.5333 0.2132 0.081 Uiso 1 1 calc R . . C52 C 0.4761(4) 0.7456(5) 0.2850(4) 0.052(2) Uani 1 1 d . . . H067 H 0.4760 0.8006 0.3033 0.063 Uiso 1 1 calc R . . C29 C 0.5897(5) 0.9453(5) -0.0129(4) 0.092(3) Uani 1 1 d . . . H06J H 0.6233 0.9701 0.0221 0.137 Uiso 1 1 calc R . . H06K H 0.5507 0.9845 -0.0258 0.137 Uiso 1 1 calc R . . H06L H 0.6104 0.9374 -0.0460 0.137 Uiso 1 1 calc R . . C51 C 0.5202(4) 0.6823(7) 0.3154(4) 0.068(3) Uani 1 1 d . . . H069 H 0.5507 0.6936 0.3540 0.081 Uiso 1 1 calc R . . C28 C 0.6256(5) 0.7991(6) 0.0213(4) 0.099(3) Uani 1 1 d . . . H07A H 0.6595 0.8223 0.0567 0.148 Uiso 1 1 calc R . . H07B H 0.6457 0.7943 -0.0125 0.148 Uiso 1 1 calc R . . H07C H 0.6109 0.7419 0.0309 0.148 Uiso 1 1 calc R . . C13 C 0.0890(4) 0.8258(6) 0.3315(4) 0.097(3) Uani 1 1 d . . . H07D H 0.0702 0.8470 0.3635 0.145 Uiso 1 1 calc R . . H07E H 0.0859 0.7626 0.3295 0.145 Uiso 1 1 calc R . . H07F H 0.0632 0.8503 0.2927 0.145 Uiso 1 1 calc R . . C68 C 0.3662(9) 0.9471(11) 0.5629(7) 0.214(7) Uiso 1 1 d . . . H68G H 0.3939 0.9169 0.5993 0.257 Uiso 1 1 calc R . . H68H H 0.3689 0.9126 0.5275 0.257 Uiso 1 1 calc R . . C58 C 0.0995(5) 1.1963(6) 0.6789(4) 0.091(3) Uani 1 1 d . . . H58I H 0.1253 1.2485 0.6754 0.137 Uiso 1 1 calc R . . H58J H 0.0896 1.1961 0.7181 0.137 Uiso 1 1 calc R . . H58K H 0.0567 1.1954 0.6465 0.137 Uiso 1 1 calc R . . C61 C 0.1583(6) 0.9588(8) 0.6750(5) 0.115(4) Uani 1 1 d . . . H07L H 0.1749 0.9649 0.6388 0.138 Uiso 1 1 calc R . . H07M H 0.1987 0.9618 0.7105 0.138 Uiso 1 1 calc R . . C67 C 0.4302(8) 0.8684(10) 0.4402(7) 0.211(7) Uiso 1 1 d . . . H07N H 0.4176 0.8116 0.4524 0.316 Uiso 1 1 calc R . . H07O H 0.4021 0.8816 0.3993 0.316 Uiso 1 1 calc R . . H07P H 0.4229 0.9125 0.4682 0.316 Uiso 1 1 calc R . . C30 C 0.5141(4) 0.8220(7) -0.0507(3) 0.099(3) Uani 1 1 d . . . H07G H 0.5347 0.8177 -0.0842 0.148 Uiso 1 1 calc R . . H07H H 0.4745 0.8603 -0.0621 0.148 Uiso 1 1 calc R . . H07I H 0.4998 0.7644 -0.0413 0.148 Uiso 1 1 calc R . . C60 C 0.1158(7) 1.0363(8) 0.6773(5) 0.124(5) Uani 1 1 d . . . H07Q H 0.0735 1.0311 0.6438 0.149 Uiso 1 1 calc R . . H07R H 0.1026 1.0333 0.7154 0.149 Uiso 1 1 calc R . . C64 C 0.6020(9) 0.9700(11) 0.4405(8) 0.231(8) Uiso 1 1 d . . . H07S H 0.6219 0.9501 0.4826 0.277 Uiso 1 1 calc R . . H07T H 0.6203 0.9308 0.4149 0.277 Uiso 1 1 calc R . . C62 C 0.1303(6) 0.8714(9) 0.6736(5) 0.124(4) Uani 1 1 d . . . H08A H 0.0914 0.8665 0.6368 0.149 Uiso 1 1 calc R . . H08B H 0.1119 0.8652 0.7088 0.149 Uiso 1 1 calc R . . C59 C 0.1416(7) 1.1163(9) 0.6739(5) 0.144(5) Uani 1 1 d . . . H08C H 0.1529 1.1201 0.6349 0.173 Uiso 1 1 calc R . . H08D H 0.1851 1.1204 0.7062 0.173 Uiso 1 1 calc R . . C65 C 0.5222(9) 0.9464(11) 0.4252(7) 0.217(7) Uiso 1 1 d . . . H10A H 0.5010 0.9931 0.4431 0.260 Uiso 1 1 calc R . . H10B H 0.5037 0.9520 0.3809 0.260 Uiso 1 1 calc R . . C70B C 0.1254(9) 0.1019(18) 0.4744(14) 0.087(9) Uiso 0.58(2) 1 d PD A 1 H70A H 0.1309 0.1379 0.4411 0.131 Uiso 0.58(2) 1 calc PR A 1 H70B H 0.1541 0.0503 0.4781 0.131 Uiso 0.58(2) 1 calc PR A 1 H70C H 0.1389 0.1348 0.5121 0.131 Uiso 0.58(2) 1 calc PR A 1 C71B C 0.0548(10) 0.0761(15) 0.4623(8) 0.114(9) Uiso 0.58(2) 1 d PD A 1 H71A H 0.0432 0.0458 0.4230 0.137 Uiso 0.58(2) 1 calc PR A 1 H71B H 0.0279 0.1302 0.4559 0.137 Uiso 0.58(2) 1 calc PR A 1 C72B C 0.0272(11) 0.0215(16) 0.5037(9) 0.093(8) Uiso 0.58(2) 1 d PD . 1 H72A H 0.0637 -0.0213 0.5200 0.112 Uiso 0.58(2) 1 calc PR A 1 H72B H 0.0277 0.0605 0.5378 0.112 Uiso 0.58(2) 1 calc PR A 1 C70A C 0.119(2) 0.093(4) 0.486(3) 0.16(3) Uiso 0.42(2) 1 d P A 2 H70D H 0.1625 0.0784 0.4796 0.235 Uiso 0.42(2) 1 calc PR A 2 H70E H 0.1264 0.1171 0.5272 0.235 Uiso 0.42(2) 1 calc PR A 2 H70F H 0.0953 0.1361 0.4566 0.235 Uiso 0.42(2) 1 calc PR A 2 C71A C 0.0768(12) 0.016(2) 0.4806(14) 0.119(12) Uiso 0.42(2) 1 d PD A 2 H71C H 0.0981 -0.0278 0.5117 0.142 Uiso 0.42(2) 1 calc PR A 2 H71D H 0.0689 -0.0107 0.4401 0.142 Uiso 0.42(2) 1 calc PR A 2 C72A C 0.0090(16) 0.050(2) 0.4904(18) 0.141(18) Uiso 0.42(2) 1 d PD . 2 H72C H -0.0236 0.0726 0.4531 0.169 Uiso 0.42(2) 1 calc PR A 2 H72D H 0.0157 0.0929 0.5237 0.169 Uiso 0.42(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co2 0.0371(9) 0.0361(9) 0.0374(10) 0.0024(8) 0.0138(8) 0.0060(8) Co1 0.0364(7) 0.0471(7) 0.0384(7) 0.0008(6) 0.0126(5) -0.0014(6) O5 0.039(3) 0.032(2) 0.042(3) 0.001(2) 0.019(2) 0.003(2) O1 0.043(3) 0.060(3) 0.034(3) 0.000(2) 0.011(2) -0.005(3) O6 0.033(3) 0.026(2) 0.045(3) -0.002(2) 0.012(2) 0.009(2) O2 0.032(3) 0.045(3) 0.043(3) -0.002(2) 0.012(2) -0.005(2) O3 0.031(3) 0.052(3) 0.041(3) 0.000(3) 0.014(3) -0.003(2) O4 0.032(3) 0.047(3) 0.041(3) -0.002(2) 0.015(2) -0.004(2) N1 0.036(3) 0.041(4) 0.031(4) -0.004(3) 0.009(3) -0.005(3) N3 0.051(4) 0.027(3) 0.040(4) 0.004(3) 0.019(3) 0.016(3) N2 0.028(3) 0.056(5) 0.043(4) 0.013(4) 0.013(3) 0.002(3) C5 0.026(4) 0.046(5) 0.025(4) 0.000(4) 0.004(4) 0.000(4) C6 0.029(4) 0.041(5) 0.031(5) -0.001(4) 0.014(4) -0.002(4) C4 0.038(5) 0.037(4) 0.035(5) 0.001(4) 0.012(4) 0.005(4) C2 0.029(4) 0.047(4) 0.034(5) 0.001(4) 0.011(4) 0.013(4) C37 0.035(4) 0.031(4) 0.044(5) -0.005(4) 0.011(4) 0.004(4) C7 0.043(5) 0.049(4) 0.027(4) -0.002(4) 0.016(4) -0.001(4) C33 0.049(5) 0.061(5) 0.041(5) -0.003(4) 0.023(4) -0.003(4) C1 0.030(4) 0.043(4) 0.036(5) 0.000(4) 0.011(4) -0.005(4) C21 0.033(4) 0.055(5) 0.040(5) 0.006(4) 0.011(4) 0.001(4) C47 0.035(4) 0.042(5) 0.032(5) -0.005(4) 0.009(4) -0.001(4) C15 0.038(4) 0.048(5) 0.047(5) 0.002(4) 0.006(4) -0.002(4) C39 0.047(5) 0.048(5) 0.045(5) -0.002(4) 0.020(4) 0.006(4) C10 0.029(4) 0.044(4) 0.044(5) 0.007(4) 0.012(4) 0.000(4) C31 0.039(4) 0.036(4) 0.034(5) -0.001(4) 0.008(4) 0.000(4) C19 0.037(5) 0.049(5) 0.042(5) 0.002(4) 0.014(4) 0.013(4) C17 0.048(5) 0.062(5) 0.066(6) -0.013(5) 0.010(4) -0.019(4) C46 0.033(4) 0.063(5) 0.036(5) 0.002(5) 0.011(4) -0.007(4) C42 0.054(5) 0.043(4) 0.069(6) -0.007(4) 0.017(4) 0.013(4) C56 0.046(5) 0.062(6) 0.031(5) 0.015(5) 0.003(4) 0.007(4) C32 0.035(4) 0.047(5) 0.038(5) 0.001(4) 0.012(4) -0.004(4) C55 0.038(5) 0.071(6) 0.046(6) -0.008(5) 0.017(4) 0.006(5) C11 0.053(5) 0.052(5) 0.047(5) 0.006(4) 0.023(4) -0.004(4) C20 0.034(4) 0.057(5) 0.045(5) -0.002(4) 0.011(4) -0.013(4) C8 0.046(5) 0.035(4) 0.042(5) 0.009(4) 0.020(4) 0.007(4) C38 0.027(4) 0.062(5) 0.033(5) -0.006(4) 0.011(4) 0.004(4) C25 0.064(5) 0.056(5) 0.067(6) -0.019(5) 0.020(5) -0.016(5) C45 0.041(5) 0.048(5) 0.043(6) 0.007(5) 0.017(4) 0.003(4) C27 0.043(5) 0.070(5) 0.039(5) 0.000(4) 0.019(4) 0.002(4) C9 0.044(5) 0.040(4) 0.048(5) 0.012(4) 0.021(4) -0.002(4) C3 0.029(4) 0.050(5) 0.046(5) 0.004(4) 0.022(4) 0.004(4) C18 0.047(5) 0.053(4) 0.033(5) -0.003(4) -0.001(4) -0.005(4) C16 0.062(5) 0.041(4) 0.056(5) -0.007(4) 0.010(4) 0.000(4) C24 0.055(5) 0.086(6) 0.040(5) 0.000(5) 0.004(4) -0.009(5) C57 0.046(5) 0.047(5) 0.043(6) 0.004(5) 0.020(5) -0.006(4) C34 0.069(6) 0.047(5) 0.074(6) 0.018(4) 0.036(5) 0.010(4) C41 0.036(5) 0.092(6) 0.050(5) -0.005(5) 0.017(4) 0.015(4) C22 0.043(5) 0.046(4) 0.035(5) -0.007(4) 0.010(4) 0.010(4) C48 0.049(5) 0.044(5) 0.072(6) 0.012(5) 0.026(5) 0.005(4) C54 0.038(4) 0.050(5) 0.050(6) -0.002(5) 0.015(4) 0.006(4) C23 0.038(4) 0.075(5) 0.035(5) -0.009(5) 0.009(4) -0.018(4) C63 0.203(14) 0.148(11) 0.078(8) -0.016(8) 0.037(9) 0.052(11) C44 0.046(5) 0.041(5) 0.057(6) -0.009(5) 0.019(5) -0.001(4) C43 0.044(5) 0.059(5) 0.040(5) -0.009(5) 0.019(4) -0.003(5) C35 0.059(5) 0.062(5) 0.062(6) -0.002(4) 0.025(5) -0.015(4) C14 0.120(8) 0.045(5) 0.125(8) 0.005(5) 0.087(7) 0.013(5) C26 0.063(5) 0.091(6) 0.052(6) -0.021(5) 0.020(5) -0.023(5) C40 0.063(6) 0.055(5) 0.097(7) 0.000(5) 0.040(5) 0.019(4) C12 0.108(7) 0.083(6) 0.059(6) -0.001(5) 0.042(6) 0.005(6) C53 0.042(5) 0.053(6) 0.036(5) 0.004(4) 0.010(4) 0.012(4) C36 0.092(6) 0.038(4) 0.070(6) -0.008(5) 0.041(5) -0.018(5) C50 0.052(6) 0.086(8) 0.108(9) 0.055(7) 0.033(7) 0.024(6) C49 0.050(5) 0.063(6) 0.097(8) 0.019(6) 0.030(6) 0.018(5) C52 0.035(4) 0.078(6) 0.045(6) 0.015(5) 0.014(4) 0.011(5) C29 0.133(8) 0.077(6) 0.091(7) -0.002(6) 0.075(7) -0.015(6) C51 0.037(5) 0.103(7) 0.062(6) 0.034(7) 0.012(5) 0.004(6) C28 0.095(7) 0.140(9) 0.070(7) 0.010(6) 0.037(6) 0.047(7) C13 0.068(6) 0.143(8) 0.100(7) -0.057(7) 0.058(6) -0.047(6) C58 0.082(7) 0.094(7) 0.105(8) 0.027(6) 0.039(6) -0.005(6) C61 0.123(10) 0.105(9) 0.123(10) 0.012(8) 0.047(8) 0.022(9) C30 0.093(7) 0.173(10) 0.035(5) -0.028(6) 0.026(5) -0.040(7) C60 0.176(13) 0.121(10) 0.057(7) 0.016(7) 0.003(8) -0.067(10) C62 0.119(10) 0.176(13) 0.077(8) -0.004(9) 0.028(7) -0.009(10) C59 0.204(15) 0.162(13) 0.053(8) 0.000(9) 0.013(8) -0.018(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 Co2 O5 1.869(4) . ? Co2 O5 1.869(4) 3 ? Co2 O6 1.873(4) . ? Co2 O6 1.873(4) 3 ? Co2 N3 1.931(6) 3 ? Co2 N3 1.931(6) . ? Co1 O2 1.855(4) . ? Co1 O1 1.856(4) . ? Co1 O4 1.900(4) . ? Co1 O3 1.918(4) . ? Co1 N2 1.935(6) . ? Co1 N1 1.936(5) . ? O5 C5 1.336(7) . ? O1 C1 1.371(7) . ? O6 C6 1.330(7) . ? O2 C2 1.353(7) . ? O3 C3 1.295(7) . ? O4 C4 1.302(7) . ? N1 C47 1.327(7) . ? N1 C43 1.339(8) . ? N3 C57 1.318(8) . ? N3 C53 1.359(8) . ? N2 C48 1.340(8) . ? N2 C52 1.341(8) . ? C5 C31 1.407(9) . ? C5 C6 1.448(8) 3 ? C6 C37 1.382(8) . ? C6 C5 1.448(8) 3 ? C4 C22 1.411(9) . ? C4 C3 1.466(9) . ? C2 C1 1.390(8) . ? C2 C10 1.405(9) . ? C37 C38 1.364(9) . ? C7 C1 1.373(8) . ? C7 C8 1.406(9) . ? C33 C31 1.534(9) . ? C33 C36 1.535(9) . ? C33 C35 1.543(9) . ? C33 C34 1.544(9) . ? C21 C22 1.373(9) . ? C21 C20 1.437(9) . ? C21 C27 1.526(9) . ? C47 C46 1.375(8) . ? C15 C17 1.524(9) . ? C15 C18 1.542(8) . ? C15 C10 1.545(9) . ? C15 C16 1.552(9) . ? C39 C40 1.526(9) . ? C39 C41 1.526(9) . ? C39 C42 1.536(9) . ? C39 C38 1.545(9) . ? C10 C9 1.402(9) . ? C31 C32 1.395(9) . ? C19 C20 1.380(8) . ? C19 C3 1.432(9) . ? C19 C23 1.508(9) . ? C46 C45 1.377(9) . ? C56 C55 1.381(9) . ? C56 C57 1.388(9) . ? C32 C38 1.410(9) 3 ? C55 C54 1.370(9) . ? C11 C8 1.506(9) . ? C11 C13 1.527(10) . ? C11 C12 1.531(9) . ? C11 C14 1.548(9) . ? C8 C9 1.384(9) . ? C38 C32 1.410(9) 3 ? C25 C23 1.561(9) . ? C45 C44 1.376(9) . ? C27 C28 1.490(10) . ? C27 C30 1.515(9) . ? C27 C29 1.524(10) . ? C24 C23 1.504(9) . ? C69 C68 1.484(16) . ? C48 C49 1.358(9) . ? C54 C53 1.385(9) . ? C23 C26 1.547(9) . ? C63 C62 1.514(14) . ? C44 C43 1.383(9) . ? C66 C67 1.344(17) . ? C66 C65 1.416(18) . ? C50 C49 1.381(11) . ? C50 C51 1.382(11) . ? C52 C51 1.384(10) . ? C68 C64 1.450(19) 3_676 ? C58 C59 1.531(14) . ? C61 C62 1.465(14) . ? C61 C60 1.491(14) . ? C60 C59 1.357(13) . ? C64 C68 1.450(19) 3_676 ? C64 C65 1.612(19) . ? C70B C71B 1.447(18) . ? C71B C72B 1.498(17) . ? C72B C72B 1.27(3) 3_556 ? C70A C71A 1.46(5) . ? C71A C72A 1.562(19) . ? C72A C72A 1.69(7) 3_556 ? 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 O5 Co2 O5 180.0(3) . 3 ? O5 Co2 O6 92.37(18) . . ? O5 Co2 O6 87.63(18) 3 . ? O5 Co2 O6 87.63(18) . 3 ? O5 Co2 O6 92.37(18) 3 3 ? O6 Co2 O6 180.0(3) . 3 ? O5 Co2 N3 89.5(2) . 3 ? O5 Co2 N3 90.5(2) 3 3 ? O6 Co2 N3 90.14(19) . 3 ? O6 Co2 N3 89.86(19) 3 3 ? O5 Co2 N3 90.5(2) . . ? O5 Co2 N3 89.5(2) 3 . ? O6 Co2 N3 89.86(19) . . ? O6 Co2 N3 90.14(19) 3 . ? N3 Co2 N3 180.0(4) 3 . ? O2 Co1 O1 88.2(2) . . ? O2 Co1 O4 92.23(19) . . ? O1 Co1 O4 178.93(19) . . ? O2 Co1 O3 177.9(2) . . ? O1 Co1 O3 93.9(2) . . ? O4 Co1 O3 85.64(19) . . ? O2 Co1 N2 91.9(2) . . ? O1 Co1 N2 90.3(2) . . ? O4 Co1 N2 90.6(2) . . ? O3 Co1 N2 88.1(2) . . ? O2 Co1 N1 90.7(2) . . ? O1 Co1 N1 89.1(2) . . ? O4 Co1 N1 89.9(2) . . ? O3 Co1 N1 89.3(2) . . ? N2 Co1 N1 177.3(3) . . ? C5 O5 Co2 110.6(4) . . ? C1 O1 Co1 108.8(4) . . ? C6 O6 Co2 110.9(4) . . ? C2 O2 Co1 109.6(4) . . ? C3 O3 Co1 111.3(4) . . ? C4 O4 Co1 111.5(4) . . ? C47 N1 C43 119.0(6) . . ? C47 N1 Co1 121.7(5) . . ? C43 N1 Co1 119.2(5) . . ? C57 N3 C53 117.0(6) . . ? C57 N3 Co2 122.3(5) . . ? C53 N3 Co2 120.7(5) . . ? C48 N2 C52 119.6(7) . . ? C48 N2 Co1 123.0(5) . . ? C52 N2 Co1 117.4(6) . . ? O5 C5 C31 125.3(6) . . ? O5 C5 C6 115.6(6) . 3 ? C31 C5 C6 119.1(6) . 3 ? O6 C6 C37 124.2(6) . . ? O6 C6 C5 115.2(6) . 3 ? C37 C6 C5 120.7(6) . 3 ? O4 C4 C22 124.1(6) . . ? O4 C4 C3 116.0(6) . . ? C22 C4 C3 120.0(7) . . ? O2 C2 C1 115.9(6) . . ? O2 C2 C10 124.2(7) . . ? C1 C2 C10 120.0(7) . . ? C38 C37 C6 121.0(6) . . ? C1 C7 C8 120.0(6) . . ? C31 C33 C36 109.3(6) . . ? C31 C33 C35 111.2(6) . . ? C36 C33 C35 108.2(6) . . ? C31 C33 C34 110.6(6) . . ? C36 C33 C34 110.3(6) . . ? C35 C33 C34 107.2(6) . . ? O1 C1 C7 121.7(6) . . ? O1 C1 C2 116.1(6) . . ? C7 C1 C2 122.2(6) . . ? C22 C21 C20 117.5(7) . . ? C22 C21 C27 122.4(7) . . ? C20 C21 C27 120.1(6) . . ? N1 C47 C46 122.1(6) . . ? C17 C15 C18 108.1(6) . . ? C17 C15 C10 112.5(6) . . ? C18 C15 C10 109.9(5) . . ? C17 C15 C16 109.4(6) . . ? C18 C15 C16 108.0(6) . . ? C10 C15 C16 108.8(5) . . ? C40 C39 C41 109.1(6) . . ? C40 C39 C42 107.9(6) . . ? C41 C39 C42 109.9(6) . . ? C40 C39 C38 111.4(6) . . ? C41 C39 C38 109.7(6) . . ? C42 C39 C38 108.8(5) . . ? C9 C10 C2 116.2(7) . . ? C9 C10 C15 121.6(6) . . ? C2 C10 C15 122.1(7) . . ? C32 C31 C5 116.9(6) . . ? C32 C31 C33 123.6(6) . . ? C5 C31 C33 119.4(6) . . ? C20 C19 C3 116.7(7) . . ? C20 C19 C23 123.6(7) . . ? C3 C19 C23 119.7(7) . . ? C47 C46 C45 119.3(6) . . ? C55 C56 C57 118.2(7) . . ? C31 C32 C38 124.0(6) . 3 ? C54 C55 C56 118.4(7) . . ? C8 C11 C13 114.8(6) . . ? C8 C11 C12 110.3(6) . . ? C13 C11 C12 108.4(6) . . ? C8 C11 C14 110.7(6) . . ? C13 C11 C14 106.7(7) . . ? C12 C11 C14 105.5(6) . . ? C19 C20 C21 125.3(6) . . ? C9 C8 C7 116.8(6) . . ? C9 C8 C11 122.9(7) . . ? C7 C8 C11 120.1(7) . . ? C37 C38 C32 118.3(6) . 3 ? C37 C38 C39 122.6(6) . . ? C32 C38 C39 119.1(6) 3 . ? C44 C45 C46 118.6(7) . . ? C28 C27 C30 108.8(7) . . ? C28 C27 C29 108.2(7) . . ? C30 C27 C29 108.0(7) . . ? C28 C27 C21 108.9(6) . . ? C30 C27 C21 111.9(6) . . ? C29 C27 C21 111.0(6) . . ? C8 C9 C10 124.8(7) . . ? O3 C3 C19 125.1(7) . . ? O3 C3 C4 115.6(6) . . ? C19 C3 C4 119.3(7) . . ? N3 C57 C56 124.4(6) . . ? C21 C22 C4 121.2(7) . . ? N2 C48 C49 122.0(8) . . ? C55 C54 C53 120.0(7) . . ? C24 C23 C19 111.3(6) . . ? C24 C23 C26 108.9(6) . . ? C19 C23 C26 111.9(6) . . ? C24 C23 C25 109.4(6) . . ? C19 C23 C25 110.1(6) . . ? C26 C23 C25 105.1(6) . . ? C45 C44 C43 119.2(7) . . ? N1 C43 C44 121.7(6) . . ? N3 C53 C54 121.9(7) . . ? C67 C66 C65 115.9(16) . . ? C49 C50 C51 119.2(8) . . ? C48 C49 C50 119.2(9) . . ? N2 C52 C51 121.1(8) . . ? C50 C51 C52 118.8(8) . . ? C64 C68 C69 118.3(15) 3_676 . ? C62 C61 C60 121.0(11) . . ? C59 C60 C61 119.5(13) . . ? C68 C64 C65 129.1(17) 3_676 . ? C61 C62 C63 117.7(10) . . ? C60 C59 C58 119.8(13) . . ? C66 C65 C64 124.6(16) . . ? C70B C71B C72B 124(2) . . ? C72B C72B C71B 133(3) 3_556 . ? C70A C71A C72A 103(3) . . ? C71A C72A C72A 89(3) . 3_556 ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 51.28 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.536 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.058 #===END data_compound_1_hex_rt _database_code_depnum_ccdc_archive 'CCDC 744072' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H220 Co3 N6 O12' _chemical_formula_weight 2404.05 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' O O 0.0106 0.0060 '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 20.720(4) _cell_length_b 15.660(3) _cell_length_c 22.570(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.97(3) _cell_angle_gamma 90.00 _cell_volume 7041(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2606 _exptl_absorpt_coefficient_mu 0.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9230 _exptl_absorpt_correction_T_max 0.9799 _exptl_absorpt_process_details SADABS _exptl_special_details ; Crystals were weakly diffracting and as a result data was only collected to a theta angle of 21.5. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.73444 _diffrn_radiation_type 'synchrotron radiation' _diffrn_radiation_source 'Australian synchrotron' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52922 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 21.53 _reflns_number_total 6989 _reflns_number_gt 5636 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Inspection of Fourier difference maps reveals that the hexane within the crystal exhibits considerable disorder that prevents the solvent molecules from being satisfactorily modelled. As a result the SQUEEZE routine within PLATON was used to generate a data set in which the contribution of the hexane to the diffraction data was removed. 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^)+(0.1174P)^2^+1.7773P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6989 _refine_ls_number_parameters 611 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1717 _refine_ls_wR_factor_gt 0.1626 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _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 C56A C 0.9611(9) 0.2188(14) 1.0283(9) 0.103(6) Uiso 0.46(3) 1 d P A 1 H56A H 1.0070 0.2067 1.0499 0.154 Uiso 0.46(3) 1 calc PR A 1 H56B H 0.9364 0.2318 1.0574 0.154 Uiso 0.46(3) 1 calc PR A 1 H56C H 0.9595 0.2668 1.0014 0.154 Uiso 0.46(3) 1 calc PR A 1 C56B C 0.9808(7) 0.1773(11) 1.0491(6) 0.091(5) Uiso 0.54(3) 1 d P A 2 H56D H 1.0209 0.1433 1.0589 0.137 Uiso 0.54(3) 1 calc PR A 2 H56E H 0.9611 0.1756 1.0829 0.137 Uiso 0.54(3) 1 calc PR A 2 H56F H 0.9917 0.2352 1.0419 0.137 Uiso 0.54(3) 1 calc PR A 2 C24A C 0.8394(8) -0.0060(15) 0.7840(7) 0.097(6) Uiso 0.47(3) 1 d P A 3 H24A H 0.8153 -0.0414 0.7504 0.146 Uiso 0.47(3) 1 calc PR A 3 H24B H 0.8183 0.0490 0.7809 0.146 Uiso 0.47(3) 1 calc PR A 3 H24C H 0.8390 -0.0323 0.8223 0.146 Uiso 0.47(3) 1 calc PR A 3 C24B C 0.8598(8) -0.0539(13) 0.7953(6) 0.098(6) Uiso 0.53(3) 1 d P A 4 H24D H 0.8388 -0.0871 0.7594 0.147 Uiso 0.53(3) 1 calc PR A 4 H24E H 0.8266 -0.0195 0.8064 0.147 Uiso 0.53(3) 1 calc PR A 4 H24F H 0.8804 -0.0914 0.8288 0.147 Uiso 0.53(3) 1 calc PR A 4 C11A C 1.3409(12) 0.0310(7) 0.6454(10) 0.081(4) Uiso 0.57(4) 1 d P B 5 H11A H 1.3653 0.0142 0.6863 0.121 Uiso 0.57(4) 1 calc PR B 5 H11B H 1.3650 0.0134 0.6168 0.121 Uiso 0.57(4) 1 calc PR B 5 H11C H 1.2974 0.0045 0.6347 0.121 Uiso 0.57(4) 1 calc PR B 5 C11B C 1.3135(14) 0.0274(8) 0.6220(12) 0.078(6) Uiso 0.43(4) 1 d P B 6 H11D H 1.3331 -0.0101 0.6558 0.117 Uiso 0.43(4) 1 calc PR B 6 H11E H 1.3303 0.0134 0.5876 0.117 Uiso 0.43(4) 1 calc PR B 6 H11F H 1.2655 0.0208 0.6103 0.117 Uiso 0.43(4) 1 calc PR B 6 C39A C -0.2178(8) 0.2269(7) 0.5818(10) 0.099(5) Uiso 0.58(3) 1 d P C 7 H39A H -0.2231 0.2199 0.5384 0.149 Uiso 0.58(3) 1 calc PR C 7 H39B H -0.2478 0.1889 0.5945 0.149 Uiso 0.58(3) 1 calc PR C 7 H39C H -0.1723 0.2138 0.6042 0.149 Uiso 0.58(3) 1 calc PR C 7 C39B C -0.2418(9) 0.2376(9) 0.5490(10) 0.080(6) Uiso 0.42(3) 1 d P C 8 H39D H -0.2493 0.2581 0.5076 0.120 Uiso 0.42(3) 1 calc PR C 8 H39E H -0.2795 0.2038 0.5518 0.120 Uiso 0.42(3) 1 calc PR C 8 H39F H -0.2019 0.2032 0.5599 0.120 Uiso 0.42(3) 1 calc PR C 8 C55 C 0.9302(3) 0.1412(5) 0.9904(3) 0.106(2) Uani 1 1 d . . . C54 C 0.9292(2) 0.0774(4) 0.8856(3) 0.0927(18) Uani 1 1 d . . . H54 H 0.8889 0.0523 0.8869 0.111 Uiso 1 1 calc R A . C57 C 0.9195(5) 0.0548(6) 1.0162(4) 0.171(4) Uani 1 1 d . A . H57A H 0.9619 0.0264 1.0311 0.256 Uiso 1 1 calc R . . H57B H 0.8904 0.0210 0.9843 0.256 Uiso 1 1 calc R . . H57C H 0.8995 0.0622 1.0494 0.256 Uiso 1 1 calc R . . C58 C 0.8635(4) 0.1845(7) 0.9661(4) 0.213(5) Uani 1 1 d . A . H58A H 0.8352 0.1504 0.9339 0.319 Uiso 1 1 calc R . . H58B H 0.8699 0.2396 0.9500 0.319 Uiso 1 1 calc R . . H58C H 0.8426 0.1911 0.9989 0.319 Uiso 1 1 calc R . . C28 C 1.0292(3) 0.3901(4) 0.7625(4) 0.111(2) Uani 1 1 d . . . H28 H 1.0295 0.4432 0.7811 0.133 Uiso 1 1 calc R . . C27 C 0.9840(3) 0.2967(5) 0.6786(3) 0.106(2) Uani 1 1 d . . . H27 H 0.9543 0.2847 0.6404 0.127 Uiso 1 1 calc R . . Co2 Co 0.0000 0.5000 0.5000 0.0503(3) Uani 1 2 d S . . Co1 Co 1.12442(3) 0.15523(4) 0.80748(3) 0.0546(3) Uani 1 1 d . . . O1 O 1.20221(12) 0.22066(18) 0.82512(12) 0.0570(7) Uani 1 1 d . . . O2 O 1.14218(14) 0.1210(2) 0.73474(12) 0.0639(8) Uani 1 1 d . . . O6 O 0.04643(13) 0.44407(17) 0.45032(12) 0.0562(7) Uani 1 1 d . . . O4 O 1.10428(13) 0.18749(18) 0.88231(12) 0.0573(7) Uani 1 1 d . . . C3 C 1.0484(2) 0.1541(3) 0.8857(2) 0.0574(11) Uani 1 1 d . A . O5 O -0.05421(12) 0.40471(16) 0.50192(12) 0.0536(7) Uani 1 1 d . . . C2 C 1.2043(2) 0.1483(3) 0.7350(2) 0.0570(11) Uani 1 1 d . B . O3 O 1.04347(13) 0.08973(18) 0.79188(12) 0.0607(8) Uani 1 1 d . A . N3 N 0.06601(15) 0.4583(2) 0.57416(16) 0.0549(9) Uani 1 1 d . . . C5 C 0.09165(19) 0.4967(3) 0.43725(19) 0.0542(11) Uani 1 1 d . . . C6 C -0.09542(19) 0.4214(3) 0.53590(19) 0.0514(10) Uani 1 1 d . . . C4 C 1.0145(2) 0.0999(3) 0.8358(2) 0.0625(12) Uani 1 1 d . . . C7 C 1.3013(2) 0.2332(3) 0.7880(2) 0.0584(11) Uani 1 1 d . . . C1 C 1.2372(2) 0.2026(3) 0.78364(19) 0.0541(11) Uani 1 1 d . . . C44 C 0.1784(2) 0.5365(3) 0.3928(2) 0.0686(13) Uani 1 1 d . . . H44 H 0.2074 0.5232 0.3692 0.082 Uiso 1 1 calc R . . N1 N 1.17380(16) 0.0577(2) 0.84888(16) 0.0547(9) Uani 1 1 d . . . C36 C -0.14093(19) 0.3610(3) 0.5463(2) 0.0586(11) Uani 1 1 d . . . H36 H -0.1430 0.3068 0.5290 0.070 Uiso 1 1 calc R . . C15 C 1.3443(3) 0.2547(3) 0.9030(2) 0.0841(15) Uani 1 1 d . . . H15A H 1.3673 0.2939 0.9344 0.126 Uiso 1 1 calc R . . H15B H 1.3693 0.2024 0.9069 0.126 Uiso 1 1 calc R . . H15C H 1.3004 0.2431 0.9076 0.126 Uiso 1 1 calc R . . N2 N 1.07128(18) 0.2497(3) 0.76553(19) 0.0658(10) Uani 1 1 d . . . C18 C 1.0215(2) 0.1670(3) 0.9360(2) 0.0691(13) Uani 1 1 d . . . H18 H 1.0440 0.2011 0.9690 0.083 Uiso 1 1 calc R A . C20 C 0.9515(2) 0.0607(4) 0.8345(2) 0.0828(15) Uani 1 1 d . A . C17 C 1.2992(2) 0.1539(3) 0.6931(2) 0.0647(13) Uani 1 1 d . B . C43 C 0.1342(2) 0.4736(3) 0.4004(2) 0.0604(12) Uani 1 1 d . . . C12 C 1.3376(2) 0.2942(3) 0.8389(2) 0.0630(12) Uani 1 1 d . . . C7A C 1.3302(2) 0.2068(3) 0.7409(2) 0.0640(12) Uani 1 1 d . . . H6 H 1.3730 0.2267 0.7425 0.077 Uiso 1 1 calc R . . C34 C 1.2166(2) 0.0642(3) 0.9054(2) 0.0611(12) Uani 1 1 d . . . H34 H 1.2247 0.1179 0.9236 0.073 Uiso 1 1 calc R . . C8 C 1.3328(3) 0.1260(3) 0.6428(3) 0.0860(16) Uani 1 1 d . . . C32 C 1.2367(2) -0.0846(3) 0.9109(3) 0.0712(13) Uani 1 1 d . . . H32 H 1.2568 -0.1328 0.9323 0.085 Uiso 1 1 calc R . . C16 C 1.2349(2) 0.1252(3) 0.6903(2) 0.0666(12) Uani 1 1 d . . . H3 H 1.2124 0.0901 0.6580 0.080 Uiso 1 1 calc R B . C37 C -0.1825(2) 0.3820(3) 0.5820(2) 0.0655(12) Uani 1 1 d . . . C52 C 0.1254(3) 0.3426(4) 0.6319(3) 0.0878(17) Uani 1 1 d . . . H52 H 0.1352 0.2846 0.6352 0.105 Uiso 1 1 calc R . . C25 C 1.0283(3) 0.2348(4) 0.7093(3) 0.0856(16) Uani 1 1 d . . . H25 H 1.0287 0.1817 0.6909 0.103 Uiso 1 1 calc R . . C31 C 1.1949(3) -0.0915(3) 0.8533(3) 0.0751(14) Uani 1 1 d . . . H31 H 1.1873 -0.1445 0.8340 0.090 Uiso 1 1 calc R . . C19 C 0.9618(2) 0.1288(4) 0.9358(3) 0.0798(15) Uani 1 1 d . A . C33 C 1.2490(2) -0.0050(3) 0.9372(2) 0.0634(12) Uani 1 1 d . . . H33 H 1.2788 0.0017 0.9761 0.076 Uiso 1 1 calc R . . C49 C 0.0963(2) 0.5112(3) 0.6207(2) 0.0679(13) Uani 1 1 d . . . H49 H 0.0862 0.5692 0.6167 0.081 Uiso 1 1 calc R . . C26 C 0.9840(3) 0.3728(6) 0.7038(4) 0.122(3) Uani 1 1 d . . . H26 H 0.9546 0.4148 0.6833 0.146 Uiso 1 1 calc R . . C46 C 0.0589(3) 0.3697(4) 0.3289(3) 0.107(2) Uani 1 1 d . . . H46A H 0.0485 0.4130 0.2976 0.160 Uiso 1 1 calc R . . H46B H 0.0272 0.3722 0.3528 0.160 Uiso 1 1 calc R . . H46C H 0.0568 0.3146 0.3098 0.160 Uiso 1 1 calc R . . C41 C -0.2208(3) 0.3071(5) 0.6646(3) 0.136(3) Uani 1 1 d . C . H41A H -0.2247 0.3622 0.6819 0.204 Uiso 1 1 calc R . . H41B H -0.1766 0.2848 0.6825 0.204 Uiso 1 1 calc R . . H41C H -0.2534 0.2691 0.6732 0.204 Uiso 1 1 calc R . . C29 C 1.0727(2) 0.3261(4) 0.7913(3) 0.0817(15) Uani 1 1 d . . . H29 H 1.1034 0.3368 0.8292 0.098 Uiso 1 1 calc R . . C13 C 1.4099(2) 0.3167(4) 0.8361(3) 0.1040(19) Uani 1 1 d . . . H13A H 1.4301 0.3554 0.8690 0.156 Uiso 1 1 calc R . . H13B H 1.4079 0.3431 0.7973 0.156 Uiso 1 1 calc R . . H13C H 1.4363 0.2655 0.8405 0.156 Uiso 1 1 calc R . . C30 C 1.1639(2) -0.0197(3) 0.8237(2) 0.0652(12) Uani 1 1 d . . . H30 H 1.1347 -0.0255 0.7844 0.078 Uiso 1 1 calc R . . C53 C 0.0813(2) 0.3752(3) 0.5801(2) 0.0674(13) Uani 1 1 d . . . H53 H 0.0614 0.3384 0.5480 0.081 Uiso 1 1 calc R . . C51 C 0.1411(3) 0.4834(5) 0.6734(2) 0.0851(16) Uani 1 1 d . . . H51 H 0.1616 0.5214 0.7045 0.102 Uiso 1 1 calc R . . C47 C 0.1472(3) 0.3171(4) 0.4215(3) 0.114(2) Uani 1 1 d . . . H47A H 0.1444 0.2614 0.4032 0.172 Uiso 1 1 calc R . . H47B H 0.1162 0.3208 0.4462 0.172 Uiso 1 1 calc R . . H47C H 0.1920 0.3267 0.4470 0.172 Uiso 1 1 calc R . . C9 C 1.2960(4) 0.1653(5) 0.5826(3) 0.147(3) Uani 1 1 d . B . H9A H 1.2981 0.2264 0.5862 0.220 Uiso 1 1 calc R . . H9B H 1.2499 0.1472 0.5717 0.220 Uiso 1 1 calc R . . H9C H 1.3163 0.1474 0.5512 0.220 Uiso 1 1 calc R . . C50 C 0.1549(3) 0.3979(6) 0.6789(3) 0.098(2) Uani 1 1 d . . . H50 H 0.1844 0.3769 0.7148 0.118 Uiso 1 1 calc R . . C45 C 0.1296(2) 0.3845(3) 0.3710(2) 0.0796(15) Uani 1 1 d . . . C14 C 1.2986(2) 0.3777(3) 0.8348(3) 0.0841(15) Uani 1 1 d . . . H14A H 1.3222 0.4156 0.8669 0.126 Uiso 1 1 calc R . . H14B H 1.2548 0.3661 0.8395 0.126 Uiso 1 1 calc R . . H14C H 1.2943 0.4038 0.7954 0.126 Uiso 1 1 calc R . . C38 C -0.2332(2) 0.3155(4) 0.5943(3) 0.0898(17) Uani 1 1 d . . . C22 C 0.8958(4) 0.0581(6) 0.7223(3) 0.156(3) Uani 1 1 d . A . H22A H 0.8728 0.0229 0.6882 0.233 Uiso 1 1 calc R . . H22B H 0.9360 0.0807 0.7149 0.233 Uiso 1 1 calc R . . H22C H 0.8671 0.1043 0.7269 0.233 Uiso 1 1 calc R . . C48 C 0.1797(3) 0.3746(4) 0.3318(3) 0.113(2) Uani 1 1 d . . . H48A H 0.1703 0.4168 0.2997 0.169 Uiso 1 1 calc R . . H48B H 0.1753 0.3186 0.3138 0.169 Uiso 1 1 calc R . . H48C H 0.2246 0.3823 0.3575 0.169 Uiso 1 1 calc R . . C21 C 0.9142(3) 0.0048(5) 0.7812(3) 0.111(2) Uani 1 1 d . . . C40 C -0.3054(3) 0.3518(5) 0.5667(3) 0.121(2) Uani 1 1 d . C . H40A H -0.3137 0.3587 0.5230 0.182 Uiso 1 1 calc R . . H40B H -0.3091 0.4062 0.5851 0.182 Uiso 1 1 calc R . . H40C H -0.3377 0.3130 0.5750 0.182 Uiso 1 1 calc R . . C10 C 1.4062(3) 0.1560(5) 0.6572(4) 0.157(3) Uani 1 1 d . B . H10A H 1.4314 0.1320 0.6958 0.235 Uiso 1 1 calc R . . H10B H 1.4078 0.2172 0.6598 0.235 Uiso 1 1 calc R . . H10C H 1.4251 0.1375 0.6250 0.235 Uiso 1 1 calc R . . C23 C 0.9583(4) -0.0706(5) 0.7730(4) 0.153(3) Uani 1 1 d . A . H23A H 0.9339 -0.1056 0.7394 0.230 Uiso 1 1 calc R . . H23B H 0.9703 -0.1039 0.8101 0.230 Uiso 1 1 calc R . . H23C H 0.9982 -0.0494 0.7644 0.230 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 C55 0.084(4) 0.138(6) 0.120(5) -0.005(4) 0.071(4) 0.002(4) C54 0.059(3) 0.136(5) 0.096(4) -0.010(4) 0.042(3) -0.024(3) C57 0.221(9) 0.187(9) 0.164(7) -0.008(6) 0.151(7) -0.021(7) C58 0.126(6) 0.365(15) 0.177(8) 0.032(9) 0.093(6) 0.115(8) C28 0.096(4) 0.080(4) 0.165(7) 0.024(4) 0.046(5) 0.010(4) C27 0.073(4) 0.124(6) 0.113(5) 0.044(5) 0.015(4) 0.005(4) Co2 0.0416(5) 0.0564(5) 0.0574(5) -0.0031(4) 0.0211(4) -0.0048(4) Co1 0.0465(4) 0.0665(4) 0.0563(4) 0.0008(3) 0.0234(3) -0.0040(3) O1 0.0454(15) 0.0698(19) 0.0604(18) -0.0034(14) 0.0223(15) -0.0064(13) O2 0.0553(18) 0.088(2) 0.0558(18) -0.0084(15) 0.0270(15) -0.0114(16) O6 0.0489(16) 0.0603(18) 0.0652(18) -0.0109(14) 0.0253(15) -0.0023(14) O4 0.0496(17) 0.0663(19) 0.0633(19) -0.0031(14) 0.0279(15) -0.0030(14) C3 0.052(3) 0.063(3) 0.063(3) 0.000(2) 0.026(3) 0.004(2) O5 0.0455(15) 0.0544(17) 0.0678(18) -0.0064(14) 0.0273(15) -0.0071(13) C2 0.057(3) 0.061(3) 0.059(3) 0.006(2) 0.027(3) 0.003(2) O3 0.0502(16) 0.077(2) 0.0588(18) -0.0027(15) 0.0221(15) -0.0137(14) N3 0.0426(19) 0.063(3) 0.063(2) 0.007(2) 0.0216(19) -0.0003(18) C5 0.043(2) 0.064(3) 0.058(3) 0.006(2) 0.018(2) -0.001(2) C6 0.041(2) 0.055(3) 0.061(3) 0.002(2) 0.019(2) -0.002(2) C4 0.049(3) 0.077(3) 0.068(3) 0.006(2) 0.027(3) -0.004(2) C7 0.052(3) 0.052(3) 0.078(3) 0.015(2) 0.030(2) 0.001(2) C1 0.053(3) 0.056(3) 0.061(3) 0.009(2) 0.028(2) 0.004(2) C44 0.050(3) 0.093(4) 0.071(3) -0.002(3) 0.031(2) 0.005(3) N1 0.051(2) 0.064(3) 0.050(2) -0.0103(18) 0.016(2) -0.0079(17) C36 0.046(2) 0.059(3) 0.071(3) 0.003(2) 0.017(2) -0.001(2) C15 0.082(3) 0.084(4) 0.078(3) 0.016(3) 0.007(3) -0.003(3) N2 0.052(2) 0.079(3) 0.072(3) 0.014(2) 0.026(2) -0.005(2) C18 0.064(3) 0.073(3) 0.080(3) -0.007(2) 0.036(3) 0.003(2) C20 0.061(3) 0.110(4) 0.086(4) -0.006(3) 0.034(3) -0.027(3) C17 0.070(3) 0.060(3) 0.080(3) 0.011(3) 0.046(3) 0.005(2) C43 0.050(3) 0.074(3) 0.062(3) -0.003(2) 0.023(2) 0.006(2) C12 0.049(2) 0.061(3) 0.080(3) 0.011(2) 0.019(2) -0.003(2) C7A 0.059(3) 0.056(3) 0.090(4) 0.020(3) 0.042(3) 0.004(2) C34 0.057(3) 0.066(3) 0.067(3) -0.004(2) 0.027(3) -0.012(2) C8 0.107(4) 0.078(4) 0.101(4) 0.009(3) 0.075(4) 0.007(3) C32 0.060(3) 0.070(4) 0.088(4) 0.005(3) 0.029(3) 0.007(2) C16 0.073(3) 0.069(3) 0.065(3) 0.006(2) 0.033(3) 0.001(2) C37 0.044(3) 0.084(4) 0.071(3) 0.009(3) 0.020(2) -0.003(2) C52 0.068(4) 0.094(4) 0.106(5) 0.032(4) 0.030(4) 0.007(3) C25 0.067(3) 0.105(4) 0.088(4) 0.024(3) 0.027(3) 0.000(3) C31 0.079(3) 0.061(3) 0.089(4) -0.009(3) 0.030(3) 0.003(3) C19 0.063(3) 0.103(4) 0.089(4) -0.006(3) 0.046(3) 0.001(3) C33 0.046(3) 0.079(4) 0.064(3) 0.004(3) 0.013(2) -0.009(2) C49 0.059(3) 0.085(4) 0.063(3) -0.008(3) 0.023(3) -0.012(3) C26 0.080(5) 0.122(6) 0.165(8) 0.069(6) 0.038(5) 0.023(4) C46 0.087(4) 0.119(5) 0.114(5) -0.053(4) 0.028(4) -0.017(3) C41 0.109(5) 0.172(7) 0.140(6) 0.064(5) 0.055(5) -0.016(5) C29 0.065(3) 0.073(4) 0.110(4) 0.013(3) 0.029(3) 0.004(3) C13 0.064(3) 0.115(5) 0.139(5) -0.001(4) 0.038(3) -0.023(3) C30 0.060(3) 0.076(4) 0.061(3) -0.016(3) 0.018(2) -0.005(3) C53 0.049(3) 0.082(4) 0.078(4) 0.017(3) 0.028(3) 0.005(2) C51 0.063(3) 0.137(6) 0.053(4) 0.005(3) 0.011(3) -0.015(3) C47 0.153(6) 0.078(4) 0.129(5) 0.003(4) 0.066(5) 0.034(4) C9 0.226(9) 0.146(6) 0.107(5) 0.019(5) 0.111(6) 0.035(6) C50 0.061(3) 0.153(7) 0.083(4) 0.046(5) 0.023(3) 0.004(4) C45 0.075(3) 0.088(4) 0.089(4) -0.016(3) 0.045(3) 0.009(3) C14 0.076(3) 0.065(3) 0.107(4) 0.004(3) 0.019(3) 0.000(3) C38 0.067(3) 0.111(4) 0.110(4) 0.018(3) 0.056(3) -0.009(3) C22 0.107(5) 0.256(10) 0.087(5) -0.008(6) 0.000(4) -0.060(6) C48 0.103(4) 0.124(5) 0.136(5) -0.031(4) 0.075(4) 0.008(4) C21 0.078(4) 0.179(7) 0.084(4) -0.025(4) 0.035(4) -0.075(4) C40 0.067(4) 0.177(7) 0.129(5) 0.014(4) 0.041(4) -0.034(4) C10 0.130(6) 0.202(9) 0.185(8) -0.051(6) 0.122(6) -0.040(5) C23 0.181(8) 0.139(7) 0.152(7) -0.070(6) 0.067(6) -0.070(6) _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 C56A C55 1.522(15) . ? C56B C55 1.554(13) . ? C24A C21 1.578(14) . ? C24B C21 1.554(12) . ? C11A C8 1.497(11) . ? C11B C8 1.632(17) . ? C39A C38 1.469(11) . ? C39B C38 1.570(15) . ? C55 C58 1.501(9) . ? C55 C57 1.513(10) . ? C55 C19 1.557(7) . ? C54 C20 1.383(7) . ? C54 C19 1.403(7) . ? C28 C29 1.386(8) . ? C28 C26 1.421(10) . ? C27 C26 1.321(9) . ? C27 C25 1.382(8) . ? Co2 O5 1.875(2) 3_566 ? Co2 O5 1.875(2) . ? Co2 O6 1.882(2) 3_566 ? Co2 O6 1.882(2) . ? Co2 N3 1.960(3) . ? Co2 N3 1.960(3) 3_566 ? Co1 O2 1.858(3) . ? Co1 O1 1.858(3) . ? Co1 O3 1.914(3) . ? Co1 O4 1.916(3) . ? Co1 N2 1.930(4) . ? Co1 N1 1.930(4) . ? O1 C1 1.362(4) . ? O2 C2 1.356(5) . ? O6 C5 1.340(5) . ? O4 C3 1.291(5) . ? C3 C18 1.411(6) . ? C3 C4 1.430(6) . ? O5 C6 1.321(4) . ? C2 C16 1.378(6) . ? C2 C1 1.407(6) . ? O3 C4 1.302(5) . ? N3 C53 1.336(6) . ? N3 C49 1.351(5) . ? C5 C6 1.412(6) 3_566 ? C5 C43 1.415(6) . ? C6 C36 1.401(5) . ? C6 C5 1.412(6) 3_566 ? C4 C20 1.435(6) . ? C7 C1 1.391(6) . ? C7 C7A 1.417(6) . ? C7 C12 1.524(6) . ? C44 C43 1.387(6) . ? C44 C37 1.390(6) 3_566 ? N1 C30 1.331(5) . ? N1 C34 1.342(5) . ? C36 C37 1.372(6) . ? C15 C12 1.545(6) . ? N2 C29 1.327(6) . ? N2 C25 1.355(6) . ? C18 C19 1.373(6) . ? C20 C21 1.516(8) . ? C17 C7A 1.371(6) . ? C17 C16 1.390(6) . ? C17 C8 1.550(6) . ? C43 C45 1.537(7) . ? C12 C14 1.526(6) . ? C12 C13 1.556(6) . ? C34 C33 1.370(6) . ? C8 C9 1.495(8) . ? C8 C10 1.538(8) . ? C32 C31 1.353(7) . ? C32 C33 1.373(6) . ? C37 C44 1.390(6) 3_566 ? C37 C38 1.558(6) . ? C52 C53 1.368(7) . ? C52 C50 1.376(8) . ? C31 C30 1.374(6) . ? C49 C51 1.362(7) . ? C46 C45 1.528(7) . ? C41 C38 1.541(8) . ? C51 C50 1.368(8) . ? C47 C45 1.523(8) . ? C45 C48 1.545(6) . ? C38 C40 1.560(8) . ? C22 C21 1.526(9) . ? C21 C23 1.534(10) . ? 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 C58 C55 C57 109.0(6) . . ? C58 C55 C56A 92.7(10) . . ? C57 C55 C56A 125.5(11) . . ? C58 C55 C56B 119.0(8) . . ? C57 C55 C56B 97.6(9) . . ? C56A C55 C56B 31.7(6) . . ? C58 C55 C19 108.3(6) . . ? C57 C55 C19 109.3(5) . . ? C56A C55 C19 109.9(7) . . ? C56B C55 C19 112.9(6) . . ? C20 C54 C19 125.8(4) . . ? C29 C28 C26 118.4(7) . . ? C26 C27 C25 119.7(7) . . ? O5 Co2 O5 180.00(17) 3_566 . ? O5 Co2 O6 92.93(11) 3_566 3_566 ? O5 Co2 O6 87.07(11) . 3_566 ? O5 Co2 O6 87.07(11) 3_566 . ? O5 Co2 O6 92.93(11) . . ? O6 Co2 O6 180.00(11) 3_566 . ? O5 Co2 N3 90.20(13) 3_566 . ? O5 Co2 N3 89.80(13) . . ? O6 Co2 N3 89.86(13) 3_566 . ? O6 Co2 N3 90.14(13) . . ? O5 Co2 N3 89.80(13) 3_566 3_566 ? O5 Co2 N3 90.20(13) . 3_566 ? O6 Co2 N3 90.14(13) 3_566 3_566 ? O6 Co2 N3 89.86(13) . 3_566 ? N3 Co2 N3 180.000(1) . 3_566 ? O2 Co1 O1 88.71(12) . . ? O2 Co1 O3 93.40(12) . . ? O1 Co1 O3 177.86(12) . . ? O2 Co1 O4 178.19(12) . . ? O1 Co1 O4 92.99(12) . . ? O3 Co1 O4 84.89(12) . . ? O2 Co1 N2 90.73(16) . . ? O1 Co1 N2 91.52(14) . . ? O3 Co1 N2 88.15(14) . . ? O4 Co1 N2 89.83(15) . . ? O2 Co1 N1 89.54(14) . . ? O1 Co1 N1 91.12(13) . . ? O3 Co1 N1 89.20(13) . . ? O4 Co1 N1 89.82(13) . . ? N2 Co1 N1 177.35(14) . . ? C1 O1 Co1 109.4(2) . . ? C2 O2 Co1 108.9(3) . . ? C5 O6 Co2 110.4(2) . . ? C3 O4 Co1 111.2(3) . . ? O4 C3 C18 123.2(4) . . ? O4 C3 C4 116.7(4) . . ? C18 C3 C4 120.1(4) . . ? C6 O5 Co2 110.0(2) . . ? O2 C2 C16 122.8(4) . . ? O2 C2 C1 116.7(3) . . ? C16 C2 C1 120.5(4) . . ? C4 O3 Co1 111.0(3) . . ? C53 N3 C49 118.2(4) . . ? C53 N3 Co2 120.1(3) . . ? C49 N3 Co2 121.7(3) . . ? O6 C5 C6 115.0(3) . 3_566 ? O6 C5 C43 124.0(4) . . ? C6 C5 C43 120.9(4) 3_566 . ? O5 C6 C36 122.4(4) . . ? O5 C6 C5 117.5(3) . 3_566 ? C36 C6 C5 120.2(4) . 3_566 ? O3 C4 C3 116.2(4) . . ? O3 C4 C20 122.6(4) . . ? C3 C4 C20 121.2(4) . . ? C1 C7 C7A 116.1(4) . . ? C1 C7 C12 122.2(4) . . ? C7A C7 C12 121.7(4) . . ? O1 C1 C7 124.0(4) . . ? O1 C1 C2 115.3(3) . . ? C7 C1 C2 120.7(4) . . ? C43 C44 C37 124.7(4) . 3_566 ? C30 N1 C34 117.3(4) . . ? C30 N1 Co1 121.0(3) . . ? C34 N1 Co1 121.6(3) . . ? C37 C36 C6 119.8(4) . . ? C29 N2 C25 119.7(5) . . ? C29 N2 Co1 122.4(4) . . ? C25 N2 Co1 117.8(4) . . ? C19 C18 C3 119.4(5) . . ? C54 C20 C4 114.4(5) . . ? C54 C20 C21 123.8(4) . . ? C4 C20 C21 121.7(4) . . ? C7A C17 C16 117.9(4) . . ? C7A C17 C8 122.6(4) . . ? C16 C17 C8 119.5(5) . . ? C44 C43 C5 115.5(4) . . ? C44 C43 C45 123.7(4) . . ? C5 C43 C45 120.7(4) . . ? C7 C12 C14 110.4(4) . . ? C7 C12 C15 110.7(4) . . ? C14 C12 C15 108.0(4) . . ? C7 C12 C13 113.1(4) . . ? C14 C12 C13 107.6(4) . . ? C15 C12 C13 106.8(4) . . ? C17 C7A C7 124.1(4) . . ? N1 C34 C33 122.6(4) . . ? C9 C8 C11A 117.9(11) . . ? C9 C8 C10 107.1(5) . . ? C11A C8 C10 101.6(10) . . ? C9 C8 C17 109.3(4) . . ? C11A C8 C17 108.7(5) . . ? C10 C8 C17 112.1(5) . . ? C9 C8 C11B 96.0(12) . . ? C11A C8 C11B 24.0(6) . . ? C10 C8 C11B 120.0(9) . . ? C17 C8 C11B 110.7(6) . . ? C31 C32 C33 118.8(5) . . ? C2 C16 C17 120.6(5) . . ? C36 C37 C44 118.9(4) . 3_566 ? C36 C37 C38 120.5(5) . . ? C44 C37 C38 120.6(4) 3_566 . ? C53 C52 C50 118.4(6) . . ? N2 C25 C27 121.6(6) . . ? C32 C31 C30 119.4(5) . . ? C18 C19 C54 119.1(4) . . ? C18 C19 C55 121.2(5) . . ? C54 C19 C55 119.7(5) . . ? C34 C33 C32 119.1(5) . . ? N3 C49 C51 122.8(5) . . ? C27 C26 C28 119.7(7) . . ? N2 C29 C28 120.9(6) . . ? N1 C30 C31 122.8(5) . . ? N3 C53 C52 122.2(5) . . ? C49 C51 C50 117.9(5) . . ? C51 C50 C52 120.5(5) . . ? C47 C45 C46 110.5(5) . . ? C47 C45 C43 109.3(4) . . ? C46 C45 C43 110.0(4) . . ? C47 C45 C48 107.4(4) . . ? C46 C45 C48 108.0(4) . . ? C43 C45 C48 111.6(4) . . ? C39A C38 C41 97.8(9) . . ? C39A C38 C37 113.8(5) . . ? C41 C38 C37 108.1(5) . . ? C39A C38 C40 120.2(9) . . ? C41 C38 C40 108.2(5) . . ? C37 C38 C40 107.7(4) . . ? C39A C38 C39B 29.8(6) . . ? C41 C38 C39B 124.2(9) . . ? C37 C38 C39B 111.4(6) . . ? C40 C38 C39B 95.7(9) . . ? C20 C21 C22 109.0(6) . . ? C20 C21 C23 110.4(5) . . ? C22 C21 C23 109.3(6) . . ? C20 C21 C24B 114.8(6) . . ? C22 C21 C24B 118.8(8) . . ? C23 C21 C24B 93.4(10) . . ? C20 C21 C24A 108.8(7) . . ? C22 C21 C24A 94.6(9) . . ? C23 C21 C24A 123.1(10) . . ? C24B C21 C24A 32.0(5) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 21.53 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.263 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.059