data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Sally Brooker' _publ_contact_author_address ; Department of Chemistry University of Otago PO Box 56 Dunedin NEW ZEALAND ; _publ_contact_author_email SBROOKER@ALKALI.OTAGO.AC.NZ _publ_section_title ; Control of molecular architecture by use of the appropriate ligand isomer: a mononuclear corner-type versus a tetranuclear [2 x 2] grid-type cobalt(III) complex ; loop_ _publ_author_name 'Sally Brooker' 'Julia Hausmann' data_co2lgmzz _database_code_depnum_ccdc_archive 'CCDC 233195' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H72 B0 Co4 F0 N24 O8' _chemical_formula_weight 1733.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.3906(19) _cell_length_b 19.6881(19) _cell_length_c 35.419(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.916(2) _cell_angle_gamma 90.00 _cell_volume 13514(2) _cell_formula_units_Z 4 _cell_measurement_temperature 164(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type 'Semi-empirical (SADABS)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 164(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _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 93070 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.41 _reflns_number_total 27173 _reflns_number_gt 16302 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. In view of the disordered anion (4 BF4- per Co4 grid) and solvent (many MeCN) sites, and the fact that the best attempt to model this gave an R1 on observed data of 0.129, cf R(int) = 0.072, the structure was subjected to the SQUEEZE procedure of the PLATON suite (P. van der Sluis, A. L. Spek, Acta Crystallogr., Section A, 1990, 46, 194-201). A total potential solvent/anion accessible volume of 7451 A^3^ per cell containing 1798 electrons was calculated. The electron count is very close to that calculated (1794 electrons) for 16BF4- and 51MeCN per cell. The final value for R1 on observed data on reincorporation of electron density in the void volume was 0.077. The chemical formulae, electron count, absorption coefficient and other derived parameters reported above and below are for the cation only. ; _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^)+(0.1217P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27173 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2116 _refine_ls_wR_factor_gt 0.1982 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 Co1 Co 0.35964(3) 0.67138(3) 0.841982(15) 0.02501(15) Uani 1 1 d . . . Co2 Co 0.14773(3) 0.40904(3) 0.845782(15) 0.02430(14) Uani 1 1 d . . . Co3 Co 0.12170(3) 0.41894(3) 0.658572(15) 0.02364(14) Uani 1 1 d . . . Co4 Co 0.36516(3) 0.65246(3) 0.655057(15) 0.02379(14) Uani 1 1 d . . . N1 N 0.29242(18) 0.59841(16) 0.83818(9) 0.0242(8) Uani 1 1 d . . . N2 N 0.42263(18) 0.59615(18) 0.84899(10) 0.0300(8) Uani 1 1 d . . . N3 N 0.43568(17) 0.74022(16) 0.84529(9) 0.0228(7) Uani 1 1 d . . . N4 N 0.21472(16) 0.48209(16) 0.84074(9) 0.0211(7) Uani 1 1 d . . . N5 N 0.08468(18) 0.48292(17) 0.85102(9) 0.0274(8) Uani 1 1 d . . . N6 N 0.07403(18) 0.34093(17) 0.85001(9) 0.0271(8) Uani 1 1 d . . . O1 O 0.43259(16) 0.48200(15) 0.83669(9) 0.0365(7) Uani 1 1 d . . . O2 O 0.07245(15) 0.59707(14) 0.83427(9) 0.0355(7) Uani 1 1 d . . . C1 C 0.3219(2) 0.5355(2) 0.83791(11) 0.0254(9) Uani 1 1 d . . . C2 C 0.2831(2) 0.4771(2) 0.83900(11) 0.0242(9) Uani 1 1 d . . . H2 H 0.3047 0.4339 0.8385 0.029 Uiso 1 1 calc R . . C3 C 0.1842(2) 0.5445(2) 0.83811(11) 0.0263(9) Uani 1 1 d . . . C4 C 0.2249(2) 0.6024(2) 0.83656(11) 0.0269(9) Uani 1 1 d . . . H4 H 0.2034 0.6457 0.8343 0.032 Uiso 1 1 calc R . . C5 C 0.4012(2) 0.5363(2) 0.84108(12) 0.0249(9) Uani 1 1 d . . . C6 C 0.4968(2) 0.6057(2) 0.85784(14) 0.0362(11) Uani 1 1 d . . . H6A H 0.5212 0.6137 0.8341 0.043 Uiso 1 1 calc R . . H6B H 0.5158 0.5638 0.8696 0.043 Uiso 1 1 calc R . . C7 C 0.5093(2) 0.6649(2) 0.88433(13) 0.0398(12) Uani 1 1 d . . . H7A H 0.4807 0.6590 0.9067 0.048 Uiso 1 1 calc R . . H7B H 0.5583 0.6646 0.8932 0.048 Uiso 1 1 calc R . . C8 C 0.4932(2) 0.7317(2) 0.86662(13) 0.0366(11) Uani 1 1 d . . . C9 C 0.5421(3) 0.7851(3) 0.87079(15) 0.0461(13) Uani 1 1 d . . . H9 H 0.5830 0.7795 0.8860 0.055 Uiso 1 1 calc R . . C10 C 0.5287(3) 0.8445(2) 0.85243(15) 0.0453(13) Uani 1 1 d . . . H10 H 0.5593 0.8819 0.8557 0.054 Uiso 1 1 calc R . . C11 C 0.4720(2) 0.8505(3) 0.82956(14) 0.0419(12) Uani 1 1 d . . . H11 H 0.4639 0.8916 0.8161 0.050 Uiso 1 1 calc R . . C12 C 0.4277(2) 0.8000(2) 0.82574(12) 0.0316(10) Uani 1 1 d . . . H12 H 0.3890 0.8051 0.8089 0.038 Uiso 1 1 calc R . . C13 C 0.1080(2) 0.5442(2) 0.84068(11) 0.0263(9) Uani 1 1 d . . . C14 C 0.0130(2) 0.4754(2) 0.85991(14) 0.0382(11) Uani 1 1 d . . . H14A H -0.0144 0.4650 0.8365 0.046 Uiso 1 1 calc R . . H14B H -0.0043 0.5187 0.8702 0.046 Uiso 1 1 calc R . . C15 C 0.0034(2) 0.4204(2) 0.88786(13) 0.0372(11) Uani 1 1 d . . . H15A H -0.0446 0.4217 0.8966 0.045 Uiso 1 1 calc R . . H15B H 0.0348 0.4282 0.9100 0.045 Uiso 1 1 calc R . . C16 C 0.0178(2) 0.3502(2) 0.87124(12) 0.0363(11) Uani 1 1 d . . . C17 C -0.0308(3) 0.2975(3) 0.87746(14) 0.0466(13) Uani 1 1 d . . . H17 H -0.0706 0.3051 0.8918 0.056 Uiso 1 1 calc R . . C18 C -0.0175(3) 0.2343(3) 0.86150(15) 0.0447(13) Uani 1 1 d . . . H18 H -0.0451 0.1961 0.8673 0.054 Uiso 1 1 calc R . . C19 C 0.0359(2) 0.2276(2) 0.83733(15) 0.0443(13) Uani 1 1 d . . . H19 H 0.0428 0.1861 0.8243 0.053 Uiso 1 1 calc R . . C20 C 0.0786(2) 0.2806(2) 0.83231(13) 0.0332(10) Uani 1 1 d . . . H20 H 0.1145 0.2751 0.8150 0.040 Uiso 1 1 calc R . . N7 N 0.13442(17) 0.41423(16) 0.79131(9) 0.0243(7) Uani 1 1 d . . . N8 N 0.21617(18) 0.34177(16) 0.83298(9) 0.0258(8) Uani 1 1 d . . . N9 N 0.17308(17) 0.40523(18) 0.90048(9) 0.0275(8) Uani 1 1 d . . . N10 N 0.13334(16) 0.40953(16) 0.71347(9) 0.0212(7) Uani 1 1 d . . . N11 N 0.04911(16) 0.48104(17) 0.67123(10) 0.0261(8) Uani 1 1 d . . . N12 N 0.10748(18) 0.43595(18) 0.60347(9) 0.0283(8) Uani 1 1 d . . . O3 O 0.27528(17) 0.30013(15) 0.78205(8) 0.0360(8) Uani 1 1 d . . . O4 O 0.00329(16) 0.53581(16) 0.72257(8) 0.0379(8) Uani 1 1 d . . . C21 C 0.1794(2) 0.37344(19) 0.77236(11) 0.0212(8) Uani 1 1 d . . . C22 C 0.1780(2) 0.37300(19) 0.73338(11) 0.0219(9) Uani 1 1 d . . . H22 H 0.2102 0.3456 0.7206 0.026 Uiso 1 1 calc R . . C23 C 0.0894(2) 0.4511(2) 0.73204(11) 0.0231(9) Uani 1 1 d . . . C24 C 0.0884(2) 0.4516(2) 0.77122(11) 0.0228(9) Uani 1 1 d . . . H24 H 0.0553 0.4782 0.7837 0.027 Uiso 1 1 calc R . . C25 C 0.2287(2) 0.3352(2) 0.79682(12) 0.0264(9) Uani 1 1 d . . . C26 C 0.2559(2) 0.2997(2) 0.86041(12) 0.0344(11) Uani 1 1 d . . . H26A H 0.2990 0.3234 0.8683 0.041 Uiso 1 1 calc R . . H26B H 0.2683 0.2560 0.8487 0.041 Uiso 1 1 calc R . . C27 C 0.2112(2) 0.2868(2) 0.89521(12) 0.0348(11) Uani 1 1 d . . . H27A H 0.1660 0.2682 0.8865 0.042 Uiso 1 1 calc R . . H27B H 0.2342 0.2522 0.9115 0.042 Uiso 1 1 calc R . . C28 C 0.1998(2) 0.3476(2) 0.91742(12) 0.0307(10) Uani 1 1 d . . . C29 C 0.2192(3) 0.3500(3) 0.95637(13) 0.0451(13) Uani 1 1 d . . . H29 H 0.2389 0.3109 0.9682 0.054 Uiso 1 1 calc R . . C30 C 0.2100(3) 0.4074(3) 0.97702(14) 0.0436(12) Uani 1 1 d . . . H30 H 0.2213 0.4078 1.0033 0.052 Uiso 1 1 calc R . . C31 C 0.1839(3) 0.4660(3) 0.95919(12) 0.0478(14) Uani 1 1 d . . . H31 H 0.1777 0.5068 0.9730 0.057 Uiso 1 1 calc R . . C32 C 0.1675(2) 0.4628(2) 0.92140(13) 0.0370(11) Uani 1 1 d . . . H32 H 0.1515 0.5030 0.9091 0.044 Uiso 1 1 calc R . . C33 C 0.0428(2) 0.4946(2) 0.70765(12) 0.0267(9) Uani 1 1 d . . . C34 C 0.0015(2) 0.5135(2) 0.64340(11) 0.0321(10) Uani 1 1 d . . . H34A H 0.0236 0.5542 0.6327 0.038 Uiso 1 1 calc R . . H34B H -0.0409 0.5280 0.6559 0.038 Uiso 1 1 calc R . . C35 C -0.0168(2) 0.4630(3) 0.61173(13) 0.0422(12) Uani 1 1 d . . . H35A H -0.0308 0.4192 0.6228 0.051 Uiso 1 1 calc R . . H35B H -0.0562 0.4807 0.5962 0.051 Uiso 1 1 calc R . . C36 C 0.0448(2) 0.4519(2) 0.58698(12) 0.0329(10) Uani 1 1 d . . . C37 C 0.0364(3) 0.4535(2) 0.54809(13) 0.0411(12) Uani 1 1 d . . . H37 H -0.0088 0.4566 0.5370 0.049 Uiso 1 1 calc R . . C38 C 0.0930(3) 0.4507(3) 0.52496(14) 0.0622(17) Uani 1 1 d . . . H38 H 0.0880 0.4568 0.4984 0.075 Uiso 1 1 calc R . . C39 C 0.1560(3) 0.4387(3) 0.54216(14) 0.0565(15) Uani 1 1 d . . . H39 H 0.1959 0.4352 0.5274 0.068 Uiso 1 1 calc R . . C40 C 0.1619(3) 0.4316(2) 0.58132(12) 0.0364(11) Uani 1 1 d . . . H40 H 0.2062 0.4234 0.5927 0.044 Uiso 1 1 calc R . . N13 N 0.18934(16) 0.49178(17) 0.66116(9) 0.0236(7) Uani 1 1 d . . . N14 N 0.20253(19) 0.36515(17) 0.65218(10) 0.0295(8) Uani 1 1 d . . . N15 N 0.05934(19) 0.33961(17) 0.65631(10) 0.0313(9) Uani 1 1 d . . . N16 N 0.29953(16) 0.57906(17) 0.65949(9) 0.0230(7) Uani 1 1 d . . . N17 N 0.28499(17) 0.70681(16) 0.64808(9) 0.0242(8) Uani 1 1 d . . . N18 N 0.42711(17) 0.73237(18) 0.65072(9) 0.0261(8) Uani 1 1 d . . . O5 O 0.31979(15) 0.36587(15) 0.66599(9) 0.0362(7) Uani 1 1 d . . . O6 O 0.16669(16) 0.70490(15) 0.66004(9) 0.0377(8) Uani 1 1 d . . . C41 C 0.2553(2) 0.46881(19) 0.66238(11) 0.0214(9) Uani 1 1 d . . . C42 C 0.3105(2) 0.5128(2) 0.66238(10) 0.0230(9) Uani 1 1 d . . . H42 H 0.3563 0.4957 0.6644 0.028 Uiso 1 1 calc R . . C43 C 0.2328(2) 0.6033(2) 0.66065(10) 0.0241(9) Uani 1 1 d . . . C44 C 0.1777(2) 0.5581(2) 0.66201(10) 0.0214(8) Uani 1 1 d . . . H44 H 0.1319 0.5747 0.6635 0.026 Uiso 1 1 calc R . . C45 C 0.2641(2) 0.3926(2) 0.66068(12) 0.0302(10) Uani 1 1 d . . . C46 C 0.2000(3) 0.2917(2) 0.64381(13) 0.0376(11) Uani 1 1 d . . . H46A H 0.1947 0.2660 0.6676 0.045 Uiso 1 1 calc R . . H46B H 0.2437 0.2775 0.6326 0.045 Uiso 1 1 calc R . . C47 C 0.1399(3) 0.2758(2) 0.61657(13) 0.0396(12) Uani 1 1 d . . . H47A H 0.1423 0.3062 0.5944 0.048 Uiso 1 1 calc R . . H47B H 0.1447 0.2285 0.6075 0.048 Uiso 1 1 calc R . . C48 C 0.0716(2) 0.2835(2) 0.63336(13) 0.0383(11) Uani 1 1 d . . . C49 C 0.0210(3) 0.2343(3) 0.62704(15) 0.0505(14) Uani 1 1 d . . . H49 H 0.0289 0.1973 0.6105 0.061 Uiso 1 1 calc R . . C50 C -0.0419(3) 0.2399(3) 0.64544(17) 0.0555(15) Uani 1 1 d . . . H50 H -0.0780 0.2082 0.6404 0.067 Uiso 1 1 calc R . . C51 C -0.0500(3) 0.2912(3) 0.67042(15) 0.0456(13) Uani 1 1 d . . . H51 H -0.0909 0.2935 0.6844 0.055 Uiso 1 1 calc R . . C52 C -0.0003(2) 0.3393(2) 0.67564(13) 0.0324(10) Uani 1 1 d . . . H52 H -0.0074 0.3742 0.6936 0.039 Uiso 1 1 calc R . . C53 C 0.2233(2) 0.6789(2) 0.65626(11) 0.0241(9) Uani 1 1 d . . . C54 C 0.2830(2) 0.7796(2) 0.63716(13) 0.0368(11) Uani 1 1 d . . . H54A H 0.2888 0.8085 0.6599 0.044 Uiso 1 1 calc R . . H54B H 0.2379 0.7905 0.6246 0.044 Uiso 1 1 calc R . . C55 C 0.3413(2) 0.7930(2) 0.61013(14) 0.0403(12) Uani 1 1 d . . . H55A H 0.3365 0.7613 0.5885 0.048 Uiso 1 1 calc R . . H55B H 0.3364 0.8398 0.6001 0.048 Uiso 1 1 calc R . . C56 C 0.4104(3) 0.7854(2) 0.62750(13) 0.0378(11) Uani 1 1 d . . . C57 C 0.4603(3) 0.8382(2) 0.62270(15) 0.0450(13) Uani 1 1 d . . . H57 H 0.4495 0.8760 0.6069 0.054 Uiso 1 1 calc R . . C58 C 0.5224(3) 0.8342(3) 0.64063(15) 0.0483(14) Uani 1 1 d . . . H58 H 0.5575 0.8662 0.6354 0.058 Uiso 1 1 calc R . . C59 C 0.5347(3) 0.7839(3) 0.66627(14) 0.0420(12) Uani 1 1 d . . . H59 H 0.5760 0.7839 0.6815 0.050 Uiso 1 1 calc R . . C60 C 0.4887(2) 0.7351(2) 0.66992(12) 0.0355(11) Uani 1 1 d . . . H60 H 0.4996 0.6994 0.6872 0.043 Uiso 1 1 calc R . . N19 N 0.36110(16) 0.66514(16) 0.70937(9) 0.0215(7) Uani 1 1 d . . . N20 N 0.43985(17) 0.59239(17) 0.66896(9) 0.0253(8) Uani 1 1 d . . . N21 N 0.37122(18) 0.63065(17) 0.60081(10) 0.0298(8) Uani 1 1 d . . . N22 N 0.36701(17) 0.66500(16) 0.78781(9) 0.0249(8) Uani 1 1 d . . . N23 N 0.29005(17) 0.73764(16) 0.82807(10) 0.0264(8) Uani 1 1 d . . . N24 N 0.33947(18) 0.67891(19) 0.89649(10) 0.0310(8) Uani 1 1 d . . . O7 O 0.48993(16) 0.53829(16) 0.72048(8) 0.0391(8) Uani 1 1 d . . . O8 O 0.22592(16) 0.77881(15) 0.77666(8) 0.0349(7) Uani 1 1 d . . . C61 C 0.4055(2) 0.6237(2) 0.72914(11) 0.0235(9) Uani 1 1 d . . . C62 C 0.40974(19) 0.6242(2) 0.76802(11) 0.0206(8) Uani 1 1 d . . . H62 H 0.4424 0.5961 0.7811 0.025 Uiso 1 1 calc R . . C63 C 0.3217(2) 0.7027(2) 0.76755(11) 0.0247(9) Uani 1 1 d . . . C64 C 0.3199(2) 0.70389(19) 0.72904(11) 0.0232(9) Uani 1 1 d . . . H64 H 0.2884 0.7333 0.7161 0.028 Uiso 1 1 calc R . . C65 C 0.4508(2) 0.5789(2) 0.70607(12) 0.0280(9) Uani 1 1 d . . . C66 C 0.4848(2) 0.5575(2) 0.64311(11) 0.0289(10) Uani 1 1 d . . . H66A H 0.4637 0.5138 0.6352 0.035 Uiso 1 1 calc R . . H66B H 0.5298 0.5478 0.6560 0.035 Uiso 1 1 calc R . . C67 C 0.4959(2) 0.6025(2) 0.60808(12) 0.0346(11) Uani 1 1 d . . . H67A H 0.5131 0.6475 0.6165 0.042 Uiso 1 1 calc R . . H67B H 0.5316 0.5815 0.5925 0.042 Uiso 1 1 calc R . . C68 C 0.4307(2) 0.6119(2) 0.58420(12) 0.0299(10) Uani 1 1 d . . . C69 C 0.4325(3) 0.5976(3) 0.54662(14) 0.0505(14) Uani 1 1 d . . . H69 H 0.4746 0.5834 0.5362 0.061 Uiso 1 1 calc R . . C70 C 0.3728(3) 0.6036(3) 0.52282(13) 0.0516(14) Uani 1 1 d . . . H70 H 0.3745 0.5975 0.4963 0.062 Uiso 1 1 calc R . . C71 C 0.3097(3) 0.6192(3) 0.54056(15) 0.0513(14) Uani 1 1 d . . . H71 H 0.2675 0.6203 0.5262 0.062 Uiso 1 1 calc R . . C72 C 0.3104(2) 0.6327(2) 0.57859(12) 0.0345(11) Uani 1 1 d . . . H72 H 0.2684 0.6437 0.5901 0.041 Uiso 1 1 calc R . . C73 C 0.2734(2) 0.7438(2) 0.79218(12) 0.0278(10) Uani 1 1 d . . . C74 C 0.2529(2) 0.7804(2) 0.85431(12) 0.0337(11) Uani 1 1 d . . . H74A H 0.2112 0.7565 0.8627 0.040 Uiso 1 1 calc R . . H74B H 0.2382 0.8230 0.8416 0.040 Uiso 1 1 calc R . . C75 C 0.3004(2) 0.7966(2) 0.88832(12) 0.0339(11) Uani 1 1 d . . . H75A H 0.3446 0.8145 0.8793 0.041 Uiso 1 1 calc R . . H75B H 0.2789 0.8325 0.9036 0.041 Uiso 1 1 calc R . . C76 C 0.3146(3) 0.7367(2) 0.91263(13) 0.0390(11) Uani 1 1 d . . . C77 C 0.3001(3) 0.7369(3) 0.95166(14) 0.0534(14) Uani 1 1 d . . . H77 H 0.2844 0.7776 0.9629 0.064 Uiso 1 1 calc R . . C78 C 0.3079(3) 0.6819(3) 0.97281(14) 0.0637(17) Uani 1 1 d . . . H78 H 0.2973 0.6830 0.9988 0.076 Uiso 1 1 calc R . . C79 C 0.3322(3) 0.6213(3) 0.95616(15) 0.0619(17) Uani 1 1 d . . . H79 H 0.3392 0.5813 0.9708 0.074 Uiso 1 1 calc R . . C80 C 0.3454(3) 0.6218(2) 0.91902(14) 0.0437(12) Uani 1 1 d . . . H80 H 0.3594 0.5805 0.9077 0.052 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 0.0247(3) 0.0206(3) 0.0299(3) -0.0028(2) 0.0032(2) -0.0037(2) Co2 0.0240(3) 0.0194(3) 0.0294(3) 0.0022(2) 0.0007(2) -0.0024(2) Co3 0.0229(3) 0.0194(3) 0.0284(3) -0.0001(2) -0.0021(2) -0.0043(2) Co4 0.0223(3) 0.0203(3) 0.0288(3) 0.0002(2) 0.0018(2) -0.0019(2) N1 0.034(2) 0.0106(17) 0.0280(18) -0.0023(13) 0.0052(15) 0.0023(15) N2 0.025(2) 0.030(2) 0.035(2) -0.0027(16) -0.0007(15) 0.0037(16) N3 0.0236(19) 0.0154(18) 0.0295(18) -0.0105(14) 0.0041(14) -0.0026(14) N4 0.0197(18) 0.0129(17) 0.0304(18) 0.0010(13) -0.0032(14) 0.0053(14) N5 0.030(2) 0.0203(19) 0.0320(19) 0.0070(15) 0.0040(15) 0.0053(16) N6 0.026(2) 0.024(2) 0.0302(19) 0.0049(15) -0.0030(15) -0.0046(15) O1 0.0355(19) 0.0194(17) 0.054(2) 0.0054(14) -0.0031(15) 0.0014(14) O2 0.0325(18) 0.0100(15) 0.064(2) 0.0050(13) 0.0011(15) 0.0039(13) C1 0.012(2) 0.026(2) 0.039(2) -0.0026(18) 0.0003(17) 0.0018(17) C2 0.018(2) 0.014(2) 0.042(2) 0.0028(17) 0.0042(17) 0.0076(17) C3 0.032(2) 0.013(2) 0.034(2) 0.0010(17) 0.0013(18) 0.0050(18) C4 0.022(2) 0.023(2) 0.036(2) -0.0046(18) 0.0019(18) 0.0022(18) C5 0.012(2) 0.022(2) 0.042(2) 0.0018(18) 0.0050(17) -0.0076(17) C6 0.022(2) 0.029(3) 0.057(3) 0.000(2) -0.004(2) 0.0006(19) C7 0.024(3) 0.044(3) 0.051(3) -0.003(2) -0.003(2) -0.004(2) C8 0.034(3) 0.038(3) 0.038(3) -0.009(2) 0.006(2) -0.006(2) C9 0.034(3) 0.046(3) 0.059(3) -0.018(3) 0.008(2) -0.015(2) C10 0.040(3) 0.024(3) 0.072(4) 0.004(2) 0.002(3) -0.008(2) C11 0.034(3) 0.033(3) 0.059(3) -0.010(2) 0.016(2) -0.008(2) C12 0.031(3) 0.030(3) 0.035(2) 0.0002(19) 0.0087(19) 0.002(2) C13 0.025(2) 0.030(3) 0.024(2) -0.0016(17) 0.0050(17) -0.0087(19) C14 0.016(2) 0.034(3) 0.065(3) 0.002(2) 0.013(2) -0.001(2) C15 0.028(3) 0.035(3) 0.049(3) 0.009(2) 0.011(2) 0.004(2) C16 0.040(3) 0.038(3) 0.031(2) 0.008(2) -0.006(2) -0.007(2) C17 0.029(3) 0.057(4) 0.054(3) 0.013(3) -0.001(2) -0.003(2) C18 0.041(3) 0.028(3) 0.065(3) 0.010(2) 0.000(3) -0.007(2) C19 0.030(3) 0.029(3) 0.072(4) 0.010(2) -0.018(3) -0.010(2) C20 0.028(3) 0.024(2) 0.047(3) 0.004(2) -0.002(2) 0.001(2) N7 0.0251(19) 0.0168(18) 0.0310(18) -0.0004(14) 0.0019(14) -0.0038(15) N8 0.029(2) 0.0123(18) 0.036(2) 0.0030(14) -0.0017(15) 0.0027(15) N9 0.0217(19) 0.031(2) 0.0297(19) -0.0006(15) 0.0033(14) 0.0017(16) N10 0.0213(18) 0.0153(17) 0.0273(17) 0.0000(13) 0.0049(14) 0.0003(14) N11 0.0167(18) 0.0230(19) 0.038(2) -0.0028(15) -0.0043(15) -0.0023(15) N12 0.030(2) 0.025(2) 0.0292(19) 0.0054(15) -0.0033(16) -0.0049(16) O3 0.053(2) 0.0217(16) 0.0326(16) 0.0008(13) -0.0041(14) 0.0154(15) O4 0.0339(18) 0.041(2) 0.0390(18) 0.0026(14) -0.0023(14) 0.0135(15) C21 0.022(2) 0.014(2) 0.028(2) 0.0021(16) 0.0021(16) -0.0028(16) C22 0.022(2) 0.015(2) 0.029(2) -0.0007(16) -0.0012(16) 0.0022(16) C23 0.024(2) 0.017(2) 0.029(2) -0.0036(16) -0.0007(17) -0.0078(17) C24 0.019(2) 0.021(2) 0.028(2) 0.0017(16) 0.0019(16) -0.0014(17) C25 0.029(2) 0.013(2) 0.037(2) 0.0015(17) -0.0020(18) -0.0062(18) C26 0.036(3) 0.028(3) 0.039(3) 0.009(2) 0.000(2) 0.002(2) C27 0.034(3) 0.030(3) 0.040(3) 0.015(2) -0.004(2) -0.001(2) C28 0.027(2) 0.034(3) 0.032(2) 0.0043(19) 0.0008(18) -0.004(2) C29 0.049(3) 0.052(3) 0.034(3) 0.019(2) 0.003(2) 0.006(3) C30 0.038(3) 0.051(3) 0.042(3) -0.002(2) -0.006(2) 0.000(2) C31 0.063(4) 0.059(4) 0.021(2) -0.010(2) 0.001(2) -0.001(3) C32 0.025(2) 0.041(3) 0.044(3) 0.009(2) -0.010(2) -0.004(2) C33 0.018(2) 0.020(2) 0.042(3) 0.0031(18) 0.0061(18) -0.0043(18) C34 0.032(3) 0.041(3) 0.023(2) 0.0014(19) -0.0012(18) 0.007(2) C35 0.033(3) 0.050(3) 0.042(3) 0.011(2) -0.018(2) 0.003(2) C36 0.039(3) 0.027(3) 0.033(2) -0.0025(18) 0.000(2) 0.004(2) C37 0.045(3) 0.039(3) 0.039(3) 0.005(2) -0.007(2) 0.002(2) C38 0.067(4) 0.092(5) 0.028(3) -0.004(3) -0.002(3) 0.003(4) C39 0.067(4) 0.063(4) 0.040(3) 0.007(3) 0.015(3) -0.009(3) C40 0.045(3) 0.034(3) 0.031(2) -0.0014(19) 0.000(2) -0.009(2) N13 0.0134(17) 0.026(2) 0.0312(18) -0.0005(14) -0.0010(13) -0.0087(14) N14 0.035(2) 0.0156(19) 0.037(2) -0.0046(15) -0.0007(16) -0.0055(16) N15 0.034(2) 0.019(2) 0.041(2) 0.0052(15) -0.0031(17) -0.0110(16) N16 0.0164(17) 0.0224(19) 0.0302(18) 0.0019(14) -0.0003(13) 0.0002(14) N17 0.0222(19) 0.0136(17) 0.0372(19) 0.0060(14) 0.0056(15) 0.0025(14) N18 0.0178(18) 0.029(2) 0.0322(19) -0.0016(15) 0.0079(14) -0.0052(15) O5 0.0208(17) 0.0280(18) 0.060(2) -0.0044(15) 0.0013(14) 0.0117(14) O6 0.0322(19) 0.0250(17) 0.056(2) 0.0047(14) 0.0075(15) 0.0019(14) C41 0.018(2) 0.016(2) 0.031(2) -0.0036(16) 0.0012(16) 0.0020(16) C42 0.020(2) 0.028(2) 0.021(2) -0.0035(16) 0.0038(16) 0.0010(18) C43 0.026(2) 0.028(2) 0.0180(19) -0.0039(16) 0.0020(16) -0.0001(18) C44 0.019(2) 0.022(2) 0.023(2) 0.0012(16) -0.0008(16) 0.0004(17) C45 0.042(3) 0.015(2) 0.034(2) -0.0020(17) 0.000(2) -0.001(2) C46 0.045(3) 0.022(2) 0.046(3) -0.005(2) 0.000(2) -0.002(2) C47 0.058(3) 0.018(2) 0.044(3) -0.013(2) -0.001(2) -0.008(2) C48 0.037(3) 0.036(3) 0.041(3) 0.000(2) -0.008(2) -0.006(2) C49 0.057(4) 0.031(3) 0.062(3) -0.005(2) -0.023(3) -0.014(3) C50 0.043(3) 0.039(3) 0.083(4) 0.002(3) -0.026(3) -0.015(3) C51 0.043(3) 0.034(3) 0.060(3) 0.017(2) -0.005(2) -0.011(2) C52 0.031(3) 0.023(2) 0.043(3) 0.0106(19) 0.001(2) -0.0060(19) C53 0.010(2) 0.027(2) 0.035(2) -0.0015(18) -0.0027(16) -0.0015(18) C54 0.035(3) 0.030(3) 0.046(3) 0.003(2) 0.005(2) -0.002(2) C55 0.040(3) 0.018(2) 0.063(3) 0.013(2) 0.006(2) -0.001(2) C56 0.044(3) 0.021(2) 0.050(3) -0.008(2) 0.010(2) -0.004(2) C57 0.044(3) 0.024(3) 0.068(3) 0.007(2) 0.019(3) -0.009(2) C58 0.036(3) 0.046(3) 0.063(3) -0.013(3) 0.013(3) -0.029(3) C59 0.038(3) 0.042(3) 0.045(3) -0.005(2) 0.000(2) -0.006(2) C60 0.035(3) 0.039(3) 0.033(2) -0.003(2) 0.001(2) -0.013(2) N19 0.0155(17) 0.0199(18) 0.0292(18) 0.0024(14) 0.0022(13) -0.0020(14) N20 0.0248(19) 0.0217(19) 0.0297(19) -0.0018(14) 0.0050(14) 0.0065(15) N21 0.026(2) 0.022(2) 0.041(2) 0.0048(15) -0.0071(16) -0.0014(15) N22 0.0209(18) 0.0183(18) 0.0353(19) 0.0026(14) -0.0009(15) -0.0029(15) N23 0.0167(18) 0.0147(18) 0.048(2) -0.0024(15) 0.0113(15) 0.0000(14) N24 0.024(2) 0.030(2) 0.040(2) -0.0033(17) 0.0073(16) -0.0046(16) O7 0.040(2) 0.0364(19) 0.0407(18) 0.0009(14) -0.0017(15) 0.0045(16) O8 0.0370(18) 0.0276(17) 0.0401(18) 0.0003(13) 0.0002(14) 0.0179(14) C61 0.015(2) 0.020(2) 0.036(2) -0.0005(17) 0.0062(17) -0.0047(17) C62 0.0096(19) 0.022(2) 0.030(2) -0.0023(16) 0.0034(15) 0.0008(16) C63 0.031(2) 0.014(2) 0.029(2) -0.0027(16) 0.0035(18) -0.0075(17) C64 0.020(2) 0.009(2) 0.041(2) 0.0007(17) 0.0039(17) -0.0034(16) C65 0.018(2) 0.034(3) 0.033(2) 0.0017(19) 0.0031(17) 0.0002(19) C66 0.022(2) 0.041(3) 0.024(2) -0.0035(18) 0.0035(17) 0.000(2) C67 0.035(3) 0.033(3) 0.037(3) -0.0023(19) 0.010(2) -0.001(2) C68 0.031(3) 0.027(2) 0.032(2) 0.0065(18) 0.0044(19) 0.0020(19) C69 0.059(4) 0.048(3) 0.045(3) -0.011(2) 0.019(3) -0.012(3) C70 0.062(4) 0.065(4) 0.027(3) -0.006(2) -0.003(2) 0.008(3) C71 0.028(3) 0.074(4) 0.051(3) 0.007(3) -0.003(2) -0.006(3) C72 0.029(3) 0.042(3) 0.033(2) -0.009(2) -0.0022(19) -0.010(2) C73 0.022(2) 0.018(2) 0.044(3) -0.0083(18) 0.0129(19) -0.0037(18) C74 0.043(3) 0.019(2) 0.040(3) -0.0038(18) 0.008(2) 0.004(2) C75 0.038(3) 0.026(2) 0.038(3) -0.0149(19) 0.006(2) -0.003(2) C76 0.043(3) 0.033(3) 0.042(3) -0.005(2) 0.012(2) -0.010(2) C77 0.067(4) 0.054(4) 0.040(3) -0.013(3) 0.004(3) -0.003(3) C78 0.094(5) 0.072(4) 0.025(3) 0.001(3) 0.006(3) 0.004(4) C79 0.104(5) 0.037(3) 0.045(3) 0.001(2) 0.012(3) -0.002(3) C80 0.049(3) 0.028(3) 0.055(3) -0.005(2) 0.017(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 Co1 N23 1.929(3) . y Co1 N2 1.931(4) . y Co1 N22 1.933(3) . y Co1 N1 1.941(3) . y Co1 N24 1.988(4) . y Co1 N3 2.003(3) . y Co2 N5 1.913(3) . y Co2 N8 1.939(3) . y Co2 N7 1.941(3) . y Co2 N4 1.950(3) . y Co2 N6 1.969(3) . y Co2 N9 1.984(3) . y Co3 N14 1.911(4) . y Co3 N11 1.929(3) . y Co3 N13 1.943(3) . y Co3 N10 1.959(3) . y Co3 N15 1.975(3) . y Co3 N12 1.990(3) . y Co4 N17 1.897(3) . y Co4 N20 1.921(3) . y Co4 N16 1.935(3) . y Co4 N19 1.944(3) . y Co4 N21 1.976(4) . y Co4 N18 1.989(3) . y N1 C4 1.312(5) . ? N1 C1 1.364(5) . ? N2 C5 1.278(5) . ? N2 C6 1.473(5) . ? N3 C8 1.336(6) . ? N3 C12 1.371(5) . ? N4 C2 1.332(5) . ? N4 C3 1.366(5) . ? N5 C13 1.343(5) . ? N5 C14 1.444(5) . ? N6 C20 1.346(5) . ? N6 C16 1.357(6) . ? O1 C5 1.242(5) . ? O2 C13 1.265(5) . ? C1 C2 1.376(6) . ? C1 C5 1.538(5) . ? C3 C4 1.388(6) . ? C3 C13 1.484(6) . ? C6 C7 1.511(6) . ? C7 C8 1.486(7) . ? C8 C9 1.422(6) . ? C9 C10 1.358(7) . ? C10 C11 1.348(7) . ? C11 C12 1.317(6) . ? C14 C15 1.483(6) . ? C15 C16 1.532(7) . ? C16 C17 1.424(7) . ? C17 C18 1.395(7) . ? C18 C19 1.372(7) . ? C19 C20 1.347(6) . ? N7 C24 1.342(5) . ? N7 C21 1.377(5) . ? N8 C25 1.318(5) . ? N8 C26 1.474(5) . ? N9 C32 1.361(6) . ? N9 C28 1.377(5) . ? N10 C22 1.313(5) . ? N10 C23 1.366(5) . ? N11 C33 1.327(5) . ? N11 C34 1.473(5) . ? N12 C40 1.338(6) . ? N12 C36 1.368(5) . ? O3 C25 1.264(5) . ? O4 C33 1.246(5) . ? C21 C22 1.380(5) . ? C21 C25 1.475(5) . ? C23 C24 1.388(5) . ? C23 C33 1.498(6) . ? C26 C27 1.551(6) . ? C27 C28 1.453(6) . ? C28 C29 1.419(6) . ? C29 C30 1.362(7) . ? C30 C31 1.401(7) . ? C31 C32 1.367(6) . ? C34 C35 1.531(6) . ? C35 C36 1.520(6) . ? C36 C37 1.382(6) . ? C37 C38 1.393(7) . ? C38 C39 1.368(8) . ? C39 C40 1.395(6) . ? N13 C44 1.325(5) . ? N13 C41 1.356(5) . ? N14 C45 1.336(5) . ? N14 C46 1.476(5) . ? N15 C52 1.363(6) . ? N15 C48 1.396(6) . ? N16 C42 1.325(5) . ? N16 C43 1.381(5) . ? N17 C53 1.357(5) . ? N17 C54 1.484(5) . ? N18 C60 1.356(5) . ? N18 C56 1.362(6) . ? O5 C45 1.210(5) . ? O6 C53 1.223(5) . ? C41 C42 1.377(5) . ? C41 C45 1.511(6) . ? C43 C44 1.393(6) . ? C43 C53 1.506(6) . ? C46 C47 1.520(6) . ? C47 C48 1.478(7) . ? C48 C49 1.391(6) . ? C49 C50 1.406(8) . ? C50 C51 1.355(7) . ? C51 C52 1.360(6) . ? C54 C55 1.530(6) . ? C55 C56 1.462(7) . ? C56 C57 1.434(6) . ? C57 C58 1.346(7) . ? C58 C59 1.359(7) . ? C59 C60 1.319(6) . ? N19 C64 1.320(5) . ? N19 C61 1.363(5) . ? N20 C65 1.351(5) . ? N20 C66 1.457(5) . ? N21 C68 1.363(5) . ? N21 C72 1.396(5) . ? N22 C63 1.341(5) . ? N22 C62 1.365(5) . ? N23 C73 1.307(5) . ? N23 C74 1.461(5) . ? N24 C76 1.368(6) . ? N24 C80 1.381(6) . ? O7 C65 1.204(5) . ? O8 C73 1.262(5) . ? C61 C62 1.377(5) . ? C61 C65 1.505(6) . ? C63 C64 1.363(5) . ? C63 C73 1.531(6) . ? C66 C67 1.545(6) . ? C67 C68 1.508(6) . ? C68 C69 1.362(6) . ? C69 C70 1.414(7) . ? C70 C71 1.427(7) . ? C71 C72 1.372(6) . ? C74 C75 1.525(6) . ? C75 C76 1.481(6) . ? C76 C77 1.420(6) . ? C77 C78 1.322(8) . ? C78 C79 1.419(8) . ? C79 C80 1.348(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 N23 Co1 N2 170.36(15) . . y N23 Co1 N22 82.23(14) . . y N2 Co1 N22 90.59(14) . . y N23 Co1 N1 91.17(14) . . y N2 Co1 N1 82.04(15) . . y N22 Co1 N1 87.41(14) . . y N23 Co1 N24 92.24(15) . . y N2 Co1 N24 94.38(15) . . y N22 Co1 N24 172.88(14) . . y N1 Co1 N24 88.23(14) . . y N23 Co1 N3 93.71(14) . . y N2 Co1 N3 92.88(15) . . y N22 Co1 N3 91.33(13) . . y N1 Co1 N3 174.75(14) . . y N24 Co1 N3 93.50(14) . . y N5 Co2 N8 170.55(14) . . y N5 Co2 N7 89.56(14) . . y N8 Co2 N7 82.69(14) . . y N5 Co2 N4 82.99(14) . . y N8 Co2 N4 91.10(14) . . y N7 Co2 N4 86.39(13) . . y N5 Co2 N6 92.44(15) . . y N8 Co2 N6 93.25(15) . . y N7 Co2 N6 92.22(14) . . y N4 Co2 N6 175.23(14) . . y N5 Co2 N9 94.15(14) . . y N8 Co2 N9 93.05(14) . . y N7 Co2 N9 173.26(14) . . y N4 Co2 N9 88.47(14) . . y N6 Co2 N9 93.25(14) . . y N14 Co3 N11 170.61(14) . . y N14 Co3 N13 81.94(14) . . y N11 Co3 N13 91.02(14) . . y N14 Co3 N10 89.86(14) . . y N11 Co3 N10 83.68(14) . . y N13 Co3 N10 88.15(13) . . y N14 Co3 N15 93.46(15) . . y N11 Co3 N15 93.45(15) . . y N13 Co3 N15 175.30(15) . . y N10 Co3 N15 90.89(14) . . y N14 Co3 N12 93.69(15) . . y N11 Co3 N12 92.46(15) . . y N13 Co3 N12 89.62(14) . . y N10 Co3 N12 175.51(14) . . y N15 Co3 N12 91.65(14) . . y N17 Co4 N20 171.23(14) . . y N17 Co4 N16 83.89(14) . . y N20 Co4 N16 90.67(14) . . y N17 Co4 N19 89.80(14) . . y N20 Co4 N19 83.13(13) . . y N16 Co4 N19 88.12(13) . . y N17 Co4 N21 94.07(14) . . y N20 Co4 N21 92.68(14) . . y N16 Co4 N21 88.69(14) . . y N19 Co4 N21 174.71(14) . . y N17 Co4 N18 92.19(14) . . y N20 Co4 N18 93.13(15) . . y N16 Co4 N18 176.01(14) . . y N19 Co4 N18 91.11(13) . . y N21 Co4 N18 92.35(14) . . y C4 N1 C1 118.2(3) . . ? C4 N1 Co1 128.7(3) . . ? C1 N1 Co1 113.0(3) . . ? C5 N2 C6 118.1(4) . . ? C5 N2 Co1 118.7(3) . . ? C6 N2 Co1 122.6(3) . . ? C8 N3 C12 118.1(4) . . ? C8 N3 Co1 123.1(3) . . ? C12 N3 Co1 118.7(3) . . ? C2 N4 C3 119.5(3) . . ? C2 N4 Co2 128.1(3) . . ? C3 N4 Co2 112.4(3) . . ? C13 N5 C14 119.1(4) . . ? C13 N5 Co2 115.8(3) . . ? C14 N5 Co2 124.5(3) . . ? C20 N6 C16 116.2(4) . . ? C20 N6 Co2 120.4(3) . . ? C16 N6 Co2 123.3(3) . . ? N1 C1 C2 121.8(4) . . ? N1 C1 C5 114.2(3) . . ? C2 C1 C5 123.6(4) . . ? N4 C2 C1 119.1(4) . . ? N4 C3 C4 119.8(4) . . ? N4 C3 C13 114.9(4) . . ? C4 C3 C13 125.1(4) . . ? N1 C4 C3 121.1(4) . . ? O1 C5 N2 131.6(4) . . ? O1 C5 C1 118.4(4) . . ? N2 C5 C1 110.0(4) . . ? N2 C6 C7 111.5(4) . . ? C8 C7 C6 113.2(4) . . ? N3 C8 C9 120.5(5) . . ? N3 C8 C7 120.7(4) . . ? C9 C8 C7 118.7(4) . . ? C10 C9 C8 118.0(5) . . ? C11 C10 C9 120.2(5) . . ? C12 C11 C10 120.7(5) . . ? C11 C12 N3 122.3(4) . . ? O2 C13 N5 127.0(4) . . ? O2 C13 C3 121.5(4) . . ? N5 C13 C3 111.4(4) . . ? N5 C14 C15 111.3(4) . . ? C14 C15 C16 112.0(4) . . ? N6 C16 C17 122.4(4) . . ? N6 C16 C15 119.6(4) . . ? C17 C16 C15 117.9(4) . . ? C18 C17 C16 117.0(5) . . ? C19 C18 C17 119.5(5) . . ? C20 C19 C18 119.2(5) . . ? N6 C20 C19 124.9(5) . . ? C24 N7 C21 118.8(3) . . ? C24 N7 Co2 128.3(3) . . ? C21 N7 Co2 112.9(3) . . ? C25 N8 C26 118.5(3) . . ? C25 N8 Co2 116.4(3) . . ? C26 N8 Co2 125.2(3) . . ? C32 N9 C28 119.0(4) . . ? C32 N9 Co2 118.6(3) . . ? C28 N9 Co2 122.3(3) . . ? C22 N10 C23 118.7(3) . . ? C22 N10 Co3 129.6(3) . . ? C23 N10 Co3 111.6(3) . . ? C33 N11 C34 119.2(3) . . ? C33 N11 Co3 116.4(3) . . ? C34 N11 Co3 124.4(3) . . ? C40 N12 C36 118.1(4) . . ? C40 N12 Co3 118.6(3) . . ? C36 N12 Co3 123.3(3) . . ? N7 C21 C22 120.0(4) . . ? N7 C21 C25 114.8(3) . . ? C22 C21 C25 125.1(4) . . ? N10 C22 C21 121.6(4) . . ? N10 C23 C24 121.0(4) . . ? N10 C23 C33 116.0(3) . . ? C24 C23 C33 123.0(4) . . ? N7 C24 C23 119.6(4) . . ? O3 C25 N8 127.8(4) . . ? O3 C25 C21 119.6(4) . . ? N8 C25 C21 112.6(4) . . ? N8 C26 C27 108.8(4) . . ? C28 C27 C26 113.2(4) . . ? N9 C28 C29 118.7(4) . . ? N9 C28 C27 120.3(4) . . ? C29 C28 C27 120.9(4) . . ? C30 C29 C28 121.0(5) . . ? C29 C30 C31 119.5(5) . . ? C32 C31 C30 118.2(5) . . ? N9 C32 C31 123.4(4) . . ? O4 C33 N11 128.4(4) . . ? O4 C33 C23 119.7(4) . . ? N11 C33 C23 111.8(4) . . ? N11 C34 C35 109.5(4) . . ? C36 C35 C34 110.4(4) . . ? N12 C36 C37 120.3(4) . . ? N12 C36 C35 119.4(4) . . ? C37 C36 C35 120.2(4) . . ? C36 C37 C38 121.1(5) . . ? C39 C38 C37 117.1(5) . . ? C38 C39 C40 120.1(5) . . ? N12 C40 C39 122.5(5) . . ? C44 N13 C41 119.3(3) . . ? C44 N13 Co3 127.8(3) . . ? C41 N13 Co3 112.9(3) . . ? C45 N14 C46 117.7(4) . . ? C45 N14 Co3 118.6(3) . . ? C46 N14 Co3 123.0(3) . . ? C52 N15 C48 116.9(4) . . ? C52 N15 Co3 120.8(3) . . ? C48 N15 Co3 122.2(3) . . ? C42 N16 C43 119.1(3) . . ? C42 N16 Co4 129.6(3) . . ? C43 N16 Co4 111.3(3) . . ? C53 N17 C54 115.5(3) . . ? C53 N17 Co4 117.9(3) . . ? C54 N17 Co4 126.4(3) . . ? C60 N18 C56 117.4(4) . . ? C60 N18 Co4 121.1(3) . . ? C56 N18 Co4 121.4(3) . . ? N13 C41 C42 121.5(4) . . ? N13 C41 C45 116.0(4) . . ? C42 C41 C45 122.4(4) . . ? N16 C42 C41 119.8(4) . . ? N16 C43 C44 120.0(4) . . ? N16 C43 C53 116.7(3) . . ? C44 C43 C53 122.9(4) . . ? N13 C44 C43 119.9(4) . . ? O5 C45 N14 130.1(4) . . ? O5 C45 C41 121.8(4) . . ? N14 C45 C41 108.0(4) . . ? N14 C46 C47 110.5(4) . . ? C48 C47 C46 113.7(4) . . ? C49 C48 N15 120.8(5) . . ? C49 C48 C47 120.0(5) . . ? N15 C48 C47 119.2(4) . . ? C48 C49 C50 119.2(5) . . ? C51 C50 C49 118.9(5) . . ? C50 C51 C52 120.6(5) . . ? C51 C52 N15 123.0(5) . . ? O6 C53 N17 130.9(4) . . ? O6 C53 C43 120.6(4) . . ? N17 C53 C43 108.5(3) . . ? N17 C54 C55 108.4(4) . . ? C56 C55 C54 113.9(4) . . ? N18 C56 C57 118.7(4) . . ? N18 C56 C55 121.9(4) . . ? C57 C56 C55 119.2(4) . . ? C58 C57 C56 119.9(5) . . ? C57 C58 C59 119.5(5) . . ? C60 C59 C58 119.5(5) . . ? C59 C60 N18 124.5(5) . . ? C64 N19 C61 117.2(3) . . ? C64 N19 Co4 129.9(3) . . ? C61 N19 Co4 112.7(3) . . ? C65 N20 C66 116.2(3) . . ? C65 N20 Co4 117.6(3) . . ? C66 N20 Co4 126.2(3) . . ? C68 N21 C72 118.4(4) . . ? C68 N21 Co4 123.8(3) . . ? C72 N21 Co4 117.7(3) . . ? C63 N22 C62 116.7(3) . . ? C63 N22 Co1 115.2(3) . . ? C62 N22 Co1 127.9(3) . . ? C73 N23 C74 117.0(3) . . ? C73 N23 Co1 117.3(3) . . ? C74 N23 Co1 125.6(3) . . ? C76 N24 C80 117.3(4) . . ? C76 N24 Co1 123.5(3) . . ? C80 N24 Co1 119.0(3) . . ? N19 C61 C62 121.7(4) . . ? N19 C61 C65 116.2(3) . . ? C62 C61 C65 122.1(4) . . ? N22 C62 C61 120.1(4) . . ? N22 C63 C64 122.6(4) . . ? N22 C63 C73 112.9(4) . . ? C64 C63 C73 124.5(4) . . ? N19 C64 C63 121.6(4) . . ? O7 C65 N20 128.3(4) . . ? O7 C65 C61 122.0(4) . . ? N20 C65 C61 109.7(4) . . ? N20 C66 C67 109.7(4) . . ? C68 C67 C66 112.6(4) . . ? C69 C68 N21 121.8(4) . . ? C69 C68 C67 118.3(4) . . ? N21 C68 C67 119.8(4) . . ? C68 C69 C70 121.2(5) . . ? C69 C70 C71 116.9(4) . . ? C72 C71 C70 119.5(4) . . ? C71 C72 N21 121.9(4) . . ? O8 C73 N23 128.8(4) . . ? O8 C73 C63 119.4(4) . . ? N23 C73 C63 111.7(4) . . ? N23 C74 C75 109.0(4) . . ? C76 C75 C74 112.9(4) . . ? N24 C76 C77 119.6(5) . . ? N24 C76 C75 118.7(4) . . ? C77 C76 C75 121.7(4) . . ? C78 C77 C76 121.8(5) . . ? C77 C78 C79 119.1(5) . . ? C80 C79 C78 118.4(5) . . ? C79 C80 N24 123.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N23 Co1 N1 C4 -14.9(4) . . . . ? N2 Co1 N1 C4 172.0(4) . . . . ? N22 Co1 N1 C4 -97.0(4) . . . . ? N24 Co1 N1 C4 77.3(4) . . . . ? N3 Co1 N1 C4 -173.3(13) . . . . ? N23 Co1 N1 C1 166.3(3) . . . . ? N2 Co1 N1 C1 -6.8(3) . . . . ? N22 Co1 N1 C1 84.2(3) . . . . ? N24 Co1 N1 C1 -101.5(3) . . . . ? N3 Co1 N1 C1 7.9(16) . . . . ? N23 Co1 N2 C5 -31.9(11) . . . . ? N22 Co1 N2 C5 -73.5(3) . . . . ? N1 Co1 N2 C5 13.8(3) . . . . ? N24 Co1 N2 C5 101.4(3) . . . . ? N3 Co1 N2 C5 -164.9(3) . . . . ? N23 Co1 N2 C6 139.2(8) . . . . ? N22 Co1 N2 C6 97.5(3) . . . . ? N1 Co1 N2 C6 -175.2(3) . . . . ? N24 Co1 N2 C6 -87.6(3) . . . . ? N3 Co1 N2 C6 6.1(3) . . . . ? N23 Co1 N3 C8 155.0(3) . . . . ? N2 Co1 N3 C8 -32.1(3) . . . . ? N22 Co1 N3 C8 -122.7(3) . . . . ? N1 Co1 N3 C8 -46.6(16) . . . . ? N24 Co1 N3 C8 62.5(3) . . . . ? N23 Co1 N3 C12 -22.9(3) . . . . ? N2 Co1 N3 C12 150.1(3) . . . . ? N22 Co1 N3 C12 59.4(3) . . . . ? N1 Co1 N3 C12 135.5(14) . . . . ? N24 Co1 N3 C12 -115.3(3) . . . . ? N5 Co2 N4 C2 173.0(4) . . . . ? N8 Co2 N4 C2 -14.4(3) . . . . ? N7 Co2 N4 C2 -97.0(3) . . . . ? N6 Co2 N4 C2 -170.2(15) . . . . ? N9 Co2 N4 C2 78.6(3) . . . . ? N5 Co2 N4 C3 -8.4(3) . . . . ? N8 Co2 N4 C3 164.3(3) . . . . ? N7 Co2 N4 C3 81.6(3) . . . . ? N6 Co2 N4 C3 8.5(18) . . . . ? N9 Co2 N4 C3 -102.7(3) . . . . ? N8 Co2 N5 C13 -37.1(10) . . . . ? N7 Co2 N5 C13 -71.9(3) . . . . ? N4 Co2 N5 C13 14.5(3) . . . . ? N6 Co2 N5 C13 -164.1(3) . . . . ? N9 Co2 N5 C13 102.5(3) . . . . ? N8 Co2 N5 C14 133.9(8) . . . . ? N7 Co2 N5 C14 99.0(3) . . . . ? N4 Co2 N5 C14 -174.5(4) . . . . ? N6 Co2 N5 C14 6.8(4) . . . . ? N9 Co2 N5 C14 -86.6(4) . . . . ? N5 Co2 N6 C20 149.9(3) . . . . ? N8 Co2 N6 C20 -22.5(3) . . . . ? N7 Co2 N6 C20 60.3(3) . . . . ? N4 Co2 N6 C20 133.2(16) . . . . ? N9 Co2 N6 C20 -115.8(3) . . . . ? N5 Co2 N6 C16 -32.1(3) . . . . ? N8 Co2 N6 C16 155.4(3) . . . . ? N7 Co2 N6 C16 -121.8(3) . . . . ? N4 Co2 N6 C16 -48.9(18) . . . . ? N9 Co2 N6 C16 62.2(3) . . . . ? C4 N1 C1 C2 -5.2(6) . . . . ? Co1 N1 C1 C2 173.7(3) . . . . ? C4 N1 C1 C5 -178.3(3) . . . . ? Co1 N1 C1 C5 0.6(4) . . . . ? C3 N4 C2 C1 5.6(6) . . . . ? Co2 N4 C2 C1 -175.8(3) . . . . ? N1 C1 C2 N4 -0.7(6) . . . . ? C5 C1 C2 N4 171.8(4) . . . . ? C2 N4 C3 C4 -4.9(6) . . . . ? Co2 N4 C3 C4 176.3(3) . . . . ? C2 N4 C3 C13 -179.6(3) . . . . ? Co2 N4 C3 C13 1.6(4) . . . . ? C1 N1 C4 C3 6.0(6) . . . . ? Co1 N1 C4 C3 -172.7(3) . . . . ? N4 C3 C4 N1 -1.1(6) . . . . ? C13 C3 C4 N1 173.0(4) . . . . ? C6 N2 C5 O1 -5.7(7) . . . . ? Co1 N2 C5 O1 165.8(4) . . . . ? C6 N2 C5 C1 172.6(4) . . . . ? Co1 N2 C5 C1 -16.0(5) . . . . ? N1 C1 C5 O1 -171.8(4) . . . . ? C2 C1 C5 O1 15.2(6) . . . . ? N1 C1 C5 N2 9.7(5) . . . . ? C2 C1 C5 N2 -163.3(4) . . . . ? C5 N2 C6 C7 -151.3(4) . . . . ? Co1 N2 C6 C7 37.6(5) . . . . ? N2 C6 C7 C8 -68.6(5) . . . . ? C12 N3 C8 C9 4.2(6) . . . . ? Co1 N3 C8 C9 -173.6(3) . . . . ? C12 N3 C8 C7 -171.7(4) . . . . ? Co1 N3 C8 C7 10.4(6) . . . . ? C6 C7 C8 N3 44.0(6) . . . . ? C6 C7 C8 C9 -132.0(4) . . . . ? N3 C8 C9 C10 -0.2(7) . . . . ? C7 C8 C9 C10 175.8(5) . . . . ? C8 C9 C10 C11 -3.2(8) . . . . ? C9 C10 C11 C12 2.4(8) . . . . ? C10 C11 C12 N3 1.9(7) . . . . ? C8 N3 C12 C11 -5.2(6) . . . . ? Co1 N3 C12 C11 172.8(3) . . . . ? C14 N5 C13 O2 -7.0(6) . . . . ? Co2 N5 C13 O2 164.5(3) . . . . ? C14 N5 C13 C3 171.7(4) . . . . ? Co2 N5 C13 C3 -16.8(4) . . . . ? N4 C3 C13 O2 -171.6(4) . . . . ? C4 C3 C13 O2 14.1(6) . . . . ? N4 C3 C13 N5 9.7(5) . . . . ? C4 C3 C13 N5 -164.7(4) . . . . ? C13 N5 C14 C15 -151.0(4) . . . . ? Co2 N5 C14 C15 38.4(5) . . . . ? N5 C14 C15 C16 -68.5(5) . . . . ? C20 N6 C16 C17 5.5(6) . . . . ? Co2 N6 C16 C17 -172.6(3) . . . . ? C20 N6 C16 C15 -171.6(4) . . . . ? Co2 N6 C16 C15 10.4(5) . . . . ? C14 C15 C16 N6 44.3(6) . . . . ? C14 C15 C16 C17 -133.0(4) . . . . ? N6 C16 C17 C18 1.7(7) . . . . ? C15 C16 C17 C18 178.8(4) . . . . ? C16 C17 C18 C19 -7.7(7) . . . . ? C17 C18 C19 C20 6.4(7) . . . . ? C16 N6 C20 C19 -7.3(6) . . . . ? Co2 N6 C20 C19 170.8(3) . . . . ? C18 C19 C20 N6 1.4(7) . . . . ? N5 Co2 N7 C24 -8.4(3) . . . . ? N8 Co2 N7 C24 177.0(3) . . . . ? N4 Co2 N7 C24 -91.4(3) . . . . ? N6 Co2 N7 C24 84.0(3) . . . . ? N9 Co2 N7 C24 -131.8(12) . . . . ? N5 Co2 N7 C21 171.5(3) . . . . ? N8 Co2 N7 C21 -3.1(3) . . . . ? N4 Co2 N7 C21 88.5(3) . . . . ? N6 Co2 N7 C21 -96.1(3) . . . . ? N9 Co2 N7 C21 48.1(13) . . . . ? N5 Co2 N8 C25 -28.0(10) . . . . ? N7 Co2 N8 C25 7.1(3) . . . . ? N4 Co2 N8 C25 -79.1(3) . . . . ? N6 Co2 N8 C25 98.9(3) . . . . ? N9 Co2 N8 C25 -167.6(3) . . . . ? N5 Co2 N8 C26 150.1(8) . . . . ? N7 Co2 N8 C26 -174.7(3) . . . . ? N4 Co2 N8 C26 99.0(3) . . . . ? N6 Co2 N8 C26 -82.9(3) . . . . ? N9 Co2 N8 C26 10.5(3) . . . . ? N5 Co2 N9 C32 -26.6(3) . . . . ? N8 Co2 N9 C32 147.3(3) . . . . ? N7 Co2 N9 C32 96.6(12) . . . . ? N4 Co2 N9 C32 56.3(3) . . . . ? N6 Co2 N9 C32 -119.3(3) . . . . ? N5 Co2 N9 C28 157.3(3) . . . . ? N8 Co2 N9 C28 -28.8(3) . . . . ? N7 Co2 N9 C28 -79.5(13) . . . . ? N4 Co2 N9 C28 -119.8(3) . . . . ? N6 Co2 N9 C28 64.6(3) . . . . ? N14 Co3 N10 C22 -5.6(4) . . . . ? N11 Co3 N10 C22 -178.8(4) . . . . ? N13 Co3 N10 C22 -87.6(3) . . . . ? N15 Co3 N10 C22 87.8(4) . . . . ? N12 Co3 N10 C22 -147.9(17) . . . . ? N14 Co3 N10 C23 170.6(3) . . . . ? N11 Co3 N10 C23 -2.6(3) . . . . ? N13 Co3 N10 C23 88.6(3) . . . . ? N15 Co3 N10 C23 -96.0(3) . . . . ? N12 Co3 N10 C23 28.3(19) . . . . ? N14 Co3 N11 C33 -41.2(11) . . . . ? N13 Co3 N11 C33 -82.4(3) . . . . ? N10 Co3 N11 C33 5.6(3) . . . . ? N15 Co3 N11 C33 96.1(3) . . . . ? N12 Co3 N11 C33 -172.1(3) . . . . ? N14 Co3 N11 C34 138.8(9) . . . . ? N13 Co3 N11 C34 97.5(3) . . . . ? N10 Co3 N11 C34 -174.5(3) . . . . ? N15 Co3 N11 C34 -83.9(3) . . . . ? N12 Co3 N11 C34 7.9(3) . . . . ? N14 Co3 N12 C40 -24.0(3) . . . . ? N11 Co3 N12 C40 148.9(3) . . . . ? N13 Co3 N12 C40 57.9(3) . . . . ? N10 Co3 N12 C40 118.2(17) . . . . ? N15 Co3 N12 C40 -117.5(3) . . . . ? N14 Co3 N12 C36 156.1(3) . . . . ? N11 Co3 N12 C36 -31.0(3) . . . . ? N13 Co3 N12 C36 -122.0(3) . . . . ? N10 Co3 N12 C36 -61.7(19) . . . . ? N15 Co3 N12 C36 62.5(3) . . . . ? C24 N7 C21 C22 1.9(5) . . . . ? Co2 N7 C21 C22 -178.0(3) . . . . ? C24 N7 C21 C25 179.1(3) . . . . ? Co2 N7 C21 C25 -0.8(4) . . . . ? C23 N10 C22 C21 2.9(6) . . . . ? Co3 N10 C22 C21 178.9(3) . . . . ? N7 C21 C22 N10 -1.7(6) . . . . ? C25 C21 C22 N10 -178.6(4) . . . . ? C22 N10 C23 C24 -4.3(5) . . . . ? Co3 N10 C23 C24 179.0(3) . . . . ? C22 N10 C23 C33 176.3(3) . . . . ? Co3 N10 C23 C33 -0.4(4) . . . . ? C21 N7 C24 C23 -3.3(5) . . . . ? Co2 N7 C24 C23 176.6(3) . . . . ? N10 C23 C24 N7 4.6(6) . . . . ? C33 C23 C24 N7 -176.1(3) . . . . ? C26 N8 C25 O3 -5.9(6) . . . . ? Co2 N8 C25 O3 172.3(3) . . . . ? C26 N8 C25 C21 172.6(3) . . . . ? Co2 N8 C25 C21 -9.1(4) . . . . ? N7 C21 C25 O3 -174.9(3) . . . . ? C22 C21 C25 O3 2.1(6) . . . . ? N7 C21 C25 N8 6.4(5) . . . . ? C22 C21 C25 N8 -176.5(4) . . . . ? C25 N8 C26 C27 -151.0(4) . . . . ? Co2 N8 C26 C27 30.9(5) . . . . ? N8 C26 C27 C28 -68.5(5) . . . . ? C32 N9 C28 C29 1.3(6) . . . . ? Co2 N9 C28 C29 177.4(3) . . . . ? C32 N9 C28 C27 -175.3(4) . . . . ? Co2 N9 C28 C27 0.8(5) . . . . ? C26 C27 C28 N9 53.7(5) . . . . ? C26 C27 C28 C29 -122.8(5) . . . . ? N9 C28 C29 C30 1.8(7) . . . . ? C27 C28 C29 C30 178.4(5) . . . . ? C28 C29 C30 C31 -2.9(8) . . . . ? C29 C30 C31 C32 0.9(8) . . . . ? C28 N9 C32 C31 -3.4(7) . . . . ? Co2 N9 C32 C31 -179.7(4) . . . . ? C30 C31 C32 N9 2.3(8) . . . . ? C34 N11 C33 O4 -4.9(6) . . . . ? Co3 N11 C33 O4 175.0(3) . . . . ? C34 N11 C33 C23 173.1(3) . . . . ? Co3 N11 C33 C23 -7.0(4) . . . . ? N10 C23 C33 O4 -177.1(4) . . . . ? C24 C23 C33 O4 3.6(6) . . . . ? N10 C23 C33 N11 4.7(5) . . . . ? C24 C23 C33 N11 -174.6(4) . . . . ? C33 N11 C34 C35 -142.5(4) . . . . ? Co3 N11 C34 C35 37.6(5) . . . . ? N11 C34 C35 C36 -71.6(5) . . . . ? C40 N12 C36 C37 9.4(6) . . . . ? Co3 N12 C36 C37 -170.7(3) . . . . ? C40 N12 C36 C35 -174.9(4) . . . . ? Co3 N12 C36 C35 5.0(6) . . . . ? C34 C35 C36 N12 50.9(5) . . . . ? C34 C35 C36 C37 -133.5(4) . . . . ? N12 C36 C37 C38 -11.2(7) . . . . ? C35 C36 C37 C38 173.1(5) . . . . ? C36 C37 C38 C39 7.1(9) . . . . ? C37 C38 C39 C40 -1.6(9) . . . . ? C36 N12 C40 C39 -4.0(7) . . . . ? Co3 N12 C40 C39 176.1(4) . . . . ? C38 C39 C40 N12 0.1(8) . . . . ? N14 Co3 N13 C44 172.3(3) . . . . ? N11 Co3 N13 C44 -14.0(3) . . . . ? N10 Co3 N13 C44 -97.6(3) . . . . ? N15 Co3 N13 C44 -176(22) . . . . ? N12 Co3 N13 C44 78.5(3) . . . . ? N14 Co3 N13 C41 -8.1(3) . . . . ? N11 Co3 N13 C41 165.7(3) . . . . ? N10 Co3 N13 C41 82.0(3) . . . . ? N15 Co3 N13 C41 3.7(19) . . . . ? N12 Co3 N13 C41 -101.9(3) . . . . ? N11 Co3 N14 C45 -26.6(11) . . . . ? N13 Co3 N14 C45 15.2(3) . . . . ? N10 Co3 N14 C45 -73.0(3) . . . . ? N15 Co3 N14 C45 -163.9(3) . . . . ? N12 Co3 N14 C45 104.2(3) . . . . ? N11 Co3 N14 C46 143.9(8) . . . . ? N13 Co3 N14 C46 -174.3(3) . . . . ? N10 Co3 N14 C46 97.5(3) . . . . ? N15 Co3 N14 C46 6.7(3) . . . . ? N12 Co3 N14 C46 -85.2(3) . . . . ? N14 Co3 N15 C52 149.5(3) . . . . ? N11 Co3 N15 C52 -24.2(3) . . . . ? N13 Co3 N15 C52 137.7(16) . . . . ? N10 Co3 N15 C52 59.5(3) . . . . ? N12 Co3 N15 C52 -116.7(3) . . . . ? N14 Co3 N15 C48 -34.6(3) . . . . ? N11 Co3 N15 C48 151.8(3) . . . . ? N13 Co3 N15 C48 -46.3(19) . . . . ? N10 Co3 N15 C48 -124.5(3) . . . . ? N12 Co3 N15 C48 59.2(3) . . . . ? N17 Co4 N16 C42 173.9(4) . . . . ? N20 Co4 N16 C42 -13.0(3) . . . . ? N19 Co4 N16 C42 -96.1(3) . . . . ? N21 Co4 N16 C42 79.6(3) . . . . ? N18 Co4 N16 C42 -175(22) . . . . ? N17 Co4 N16 C43 -8.1(3) . . . . ? N20 Co4 N16 C43 165.0(3) . . . . ? N19 Co4 N16 C43 81.9(3) . . . . ? N21 Co4 N16 C43 -102.3(3) . . . . ? N18 Co4 N16 C43 3(2) . . . . ? N20 Co4 N17 C53 -39.2(11) . . . . ? N16 Co4 N17 C53 12.7(3) . . . . ? N19 Co4 N17 C53 -75.4(3) . . . . ? N21 Co4 N17 C53 101.0(3) . . . . ? N18 Co4 N17 C53 -166.5(3) . . . . ? N20 Co4 N17 C54 135.8(9) . . . . ? N16 Co4 N17 C54 -172.3(3) . . . . ? N19 Co4 N17 C54 99.6(3) . . . . ? N21 Co4 N17 C54 -84.0(3) . . . . ? N18 Co4 N17 C54 8.5(3) . . . . ? N17 Co4 N18 C60 148.3(3) . . . . ? N20 Co4 N18 C60 -24.7(3) . . . . ? N16 Co4 N18 C60 137.4(19) . . . . ? N19 Co4 N18 C60 58.5(3) . . . . ? N21 Co4 N18 C60 -117.5(3) . . . . ? N17 Co4 N18 C56 -33.8(3) . . . . ? N20 Co4 N18 C56 153.2(3) . . . . ? N16 Co4 N18 C56 -45(2) . . . . ? N19 Co4 N18 C56 -123.6(3) . . . . ? N21 Co4 N18 C56 60.4(3) . . . . ? C44 N13 C41 C42 -3.6(6) . . . . ? Co3 N13 C41 C42 176.7(3) . . . . ? C44 N13 C41 C45 -179.1(3) . . . . ? Co3 N13 C41 C45 1.3(4) . . . . ? C43 N16 C42 C41 7.0(5) . . . . ? Co4 N16 C42 C41 -175.1(3) . . . . ? N13 C41 C42 N16 -3.0(6) . . . . ? C45 C41 C42 N16 172.2(3) . . . . ? C42 N16 C43 C44 -4.8(5) . . . . ? Co4 N16 C43 C44 177.0(3) . . . . ? C42 N16 C43 C53 -178.5(3) . . . . ? Co4 N16 C43 C53 3.2(4) . . . . ? C41 N13 C44 C43 5.8(5) . . . . ? Co3 N13 C44 C43 -174.6(3) . . . . ? N16 C43 C44 N13 -1.8(5) . . . . ? C53 C43 C44 N13 171.6(3) . . . . ? C46 N14 C45 O5 -7.1(7) . . . . ? Co3 N14 C45 O5 163.9(4) . . . . ? C46 N14 C45 C41 171.8(3) . . . . ? Co3 N14 C45 C41 -17.2(4) . . . . ? N13 C41 C45 O5 -171.2(4) . . . . ? C42 C41 C45 O5 13.4(6) . . . . ? N13 C41 C45 N14 9.8(5) . . . . ? C42 C41 C45 N14 -165.6(4) . . . . ? C45 N14 C46 C47 -150.8(4) . . . . ? Co3 N14 C46 C47 38.6(5) . . . . ? N14 C46 C47 C48 -69.7(5) . . . . ? C52 N15 C48 C49 7.9(6) . . . . ? Co3 N15 C48 C49 -168.2(3) . . . . ? C52 N15 C48 C47 -170.3(4) . . . . ? Co3 N15 C48 C47 13.5(6) . . . . ? C46 C47 C48 C49 -135.5(4) . . . . ? C46 C47 C48 N15 42.7(6) . . . . ? N15 C48 C49 C50 -2.9(7) . . . . ? C47 C48 C49 C50 175.4(5) . . . . ? C48 C49 C50 C51 -3.5(8) . . . . ? C49 C50 C51 C52 4.6(8) . . . . ? C50 C51 C52 N15 0.7(7) . . . . ? C48 N15 C52 C51 -7.0(6) . . . . ? Co3 N15 C52 C51 169.2(3) . . . . ? C54 N17 C53 O6 -8.6(6) . . . . ? Co4 N17 C53 O6 166.9(4) . . . . ? C54 N17 C53 C43 171.2(3) . . . . ? Co4 N17 C53 C43 -13.3(4) . . . . ? N16 C43 C53 O6 -174.0(4) . . . . ? C44 C43 C53 O6 12.4(6) . . . . ? N16 C43 C53 N17 6.1(5) . . . . ? C44 C43 C53 N17 -167.5(3) . . . . ? C53 N17 C54 C55 -150.3(4) . . . . ? Co4 N17 C54 C55 34.6(5) . . . . ? N17 C54 C55 C56 -66.0(5) . . . . ? C60 N18 C56 C57 4.2(6) . . . . ? Co4 N18 C56 C57 -173.7(3) . . . . ? C60 N18 C56 C55 -170.2(4) . . . . ? Co4 N18 C56 C55 11.8(6) . . . . ? C54 C55 C56 N18 43.9(6) . . . . ? C54 C55 C56 C57 -130.5(4) . . . . ? N18 C56 C57 C58 0.8(7) . . . . ? C55 C56 C57 C58 175.4(5) . . . . ? C56 C57 C58 C59 -7.1(8) . . . . ? C57 C58 C59 C60 8.2(8) . . . . ? C58 C59 C60 N18 -3.0(8) . . . . ? C56 N18 C60 C59 -3.3(7) . . . . ? Co4 N18 C60 C59 174.7(4) . . . . ? N17 Co4 N19 C64 -6.0(3) . . . . ? N20 Co4 N19 C64 179.2(4) . . . . ? N16 Co4 N19 C64 -89.9(3) . . . . ? N21 Co4 N19 C64 -143.0(14) . . . . ? N18 Co4 N19 C64 86.1(3) . . . . ? N17 Co4 N19 C61 169.6(3) . . . . ? N20 Co4 N19 C61 -5.2(3) . . . . ? N16 Co4 N19 C61 85.7(3) . . . . ? N21 Co4 N19 C61 32.6(16) . . . . ? N18 Co4 N19 C61 -98.2(3) . . . . ? N17 Co4 N20 C65 -28.8(11) . . . . ? N16 Co4 N20 C65 -80.3(3) . . . . ? N19 Co4 N20 C65 7.7(3) . . . . ? N21 Co4 N20 C65 -169.0(3) . . . . ? N18 Co4 N20 C65 98.5(3) . . . . ? N17 Co4 N20 C66 148.7(9) . . . . ? N16 Co4 N20 C66 97.2(3) . . . . ? N19 Co4 N20 C66 -174.8(3) . . . . ? N21 Co4 N20 C66 8.5(3) . . . . ? N18 Co4 N20 C66 -84.0(3) . . . . ? N17 Co4 N21 C68 156.4(3) . . . . ? N20 Co4 N21 C68 -29.2(3) . . . . ? N16 Co4 N21 C68 -119.8(3) . . . . ? N19 Co4 N21 C68 -66.8(16) . . . . ? N18 Co4 N21 C68 64.0(3) . . . . ? N17 Co4 N21 C72 -25.7(3) . . . . ? N20 Co4 N21 C72 148.7(3) . . . . ? N16 Co4 N21 C72 58.1(3) . . . . ? N19 Co4 N21 C72 111.1(15) . . . . ? N18 Co4 N21 C72 -118.0(3) . . . . ? N23 Co1 N22 C63 -3.8(3) . . . . ? N2 Co1 N22 C63 169.8(3) . . . . ? N1 Co1 N22 C63 87.8(3) . . . . ? N24 Co1 N22 C63 35.4(13) . . . . ? N3 Co1 N22 C63 -97.3(3) . . . . ? N23 Co1 N22 C62 -179.7(3) . . . . ? N2 Co1 N22 C62 -6.1(3) . . . . ? N1 Co1 N22 C62 -88.1(3) . . . . ? N24 Co1 N22 C62 -140.5(11) . . . . ? N3 Co1 N22 C62 86.8(3) . . . . ? N2 Co1 N23 C73 -35.1(10) . . . . ? N22 Co1 N23 C73 7.1(3) . . . . ? N1 Co1 N23 C73 -80.1(3) . . . . ? N24 Co1 N23 C73 -168.4(3) . . . . ? N3 Co1 N23 C73 97.9(3) . . . . ? N2 Co1 N23 C74 143.2(8) . . . . ? N22 Co1 N23 C74 -174.6(3) . . . . ? N1 Co1 N23 C74 98.1(3) . . . . ? N24 Co1 N23 C74 9.9(3) . . . . ? N3 Co1 N23 C74 -83.8(3) . . . . ? N23 Co1 N24 C76 -28.8(4) . . . . ? N2 Co1 N24 C76 158.2(4) . . . . ? N22 Co1 N24 C76 -67.6(13) . . . . ? N1 Co1 N24 C76 -119.9(4) . . . . ? N3 Co1 N24 C76 65.0(4) . . . . ? N23 Co1 N24 C80 145.8(3) . . . . ? N2 Co1 N24 C80 -27.2(4) . . . . ? N22 Co1 N24 C80 107.0(12) . . . . ? N1 Co1 N24 C80 54.7(3) . . . . ? N3 Co1 N24 C80 -120.3(3) . . . . ? C64 N19 C61 C62 -2.8(5) . . . . ? Co4 N19 C61 C62 -179.0(3) . . . . ? C64 N19 C61 C65 178.6(3) . . . . ? Co4 N19 C61 C65 2.4(4) . . . . ? C63 N22 C62 C61 0.8(5) . . . . ? Co1 N22 C62 C61 176.6(3) . . . . ? N19 C61 C62 N22 2.4(6) . . . . ? C65 C61 C62 N22 -179.1(3) . . . . ? C62 N22 C63 C64 -3.6(6) . . . . ? Co1 N22 C63 C64 -179.9(3) . . . . ? C62 N22 C63 C73 176.8(3) . . . . ? Co1 N22 C63 C73 0.4(4) . . . . ? C61 N19 C64 C63 0.0(5) . . . . ? Co4 N19 C64 C63 175.4(3) . . . . ? N22 C63 C64 N19 3.3(6) . . . . ? C73 C63 C64 N19 -177.1(3) . . . . ? C66 N20 C65 O7 -5.4(6) . . . . ? Co4 N20 C65 O7 172.4(4) . . . . ? C66 N20 C65 C61 174.3(3) . . . . ? Co4 N20 C65 C61 -8.0(4) . . . . ? N19 C61 C65 O7 -176.9(4) . . . . ? C62 C61 C65 O7 4.5(6) . . . . ? N19 C61 C65 N20 3.4(5) . . . . ? C62 C61 C65 N20 -175.2(4) . . . . ? C65 N20 C66 C67 -149.0(4) . . . . ? Co4 N20 C66 C67 33.5(5) . . . . ? N20 C66 C67 C68 -66.8(5) . . . . ? C72 N21 C68 C69 2.4(6) . . . . ? Co4 N21 C68 C69 -179.7(3) . . . . ? C72 N21 C68 C67 -174.0(4) . . . . ? Co4 N21 C68 C67 3.9(6) . . . . ? C66 C67 C68 C69 -127.4(4) . . . . ? C66 C67 C68 N21 49.2(5) . . . . ? N21 C68 C69 C70 1.9(8) . . . . ? C67 C68 C69 C70 178.3(5) . . . . ? C68 C69 C70 C71 -5.5(8) . . . . ? C69 C70 C71 C72 4.9(8) . . . . ? C70 C71 C72 N21 -0.9(8) . . . . ? C68 N21 C72 C71 -2.8(7) . . . . ? Co4 N21 C72 C71 179.1(4) . . . . ? C74 N23 C73 O8 -5.1(6) . . . . ? Co1 N23 C73 O8 173.3(3) . . . . ? C74 N23 C73 C63 173.2(3) . . . . ? Co1 N23 C73 C63 -8.4(4) . . . . ? N22 C63 C73 O8 -176.5(4) . . . . ? C64 C63 C73 O8 3.9(6) . . . . ? N22 C63 C73 N23 5.1(5) . . . . ? C64 C63 C73 N23 -174.5(4) . . . . ? C73 N23 C74 C75 -149.3(4) . . . . ? Co1 N23 C74 C75 32.4(5) . . . . ? N23 C74 C75 C76 -69.7(5) . . . . ? C80 N24 C76 C77 3.8(7) . . . . ? Co1 N24 C76 C77 178.5(4) . . . . ? C80 N24 C76 C75 -173.4(4) . . . . ? Co1 N24 C76 C75 1.3(6) . . . . ? C74 C75 C76 N24 53.7(6) . . . . ? C74 C75 C76 C77 -123.4(5) . . . . ? N24 C76 C77 C78 -2.2(8) . . . . ? C75 C76 C77 C78 174.9(6) . . . . ? C76 C77 C78 C79 0.8(10) . . . . ? C77 C78 C79 C80 -1.2(10) . . . . ? C78 C79 C80 N24 3.1(9) . . . . ? C76 N24 C80 C79 -4.4(7) . . . . ? Co1 N24 C80 C79 -179.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.980 _refine_diff_density_min -1.220 _refine_diff_density_rms 0.093 data_coh2l6 _database_code_depnum_ccdc_archive 'CCDC 233196' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H52 B3 Co F12 N12 O6' _chemical_formula_weight 1164.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6949(8) _cell_length_b 19.2367(14) _cell_length_c 22.1692(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.4370(10) _cell_angle_gamma 90.00 _cell_volume 4904.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type 'Semi-empirical (SADABS)' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _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 60533 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.45 _reflns_number_total 10050 _reflns_number_gt 8182 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0543P)^2^+6.7384P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10050 _refine_ls_number_parameters 762 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1243 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.045 _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 Co1 Co 0.67165(3) 0.739755(16) 0.804502(14) 0.01729(9) Uani 1 1 d . . . N1 N 0.76814(16) 0.81179(10) 0.77667(9) 0.0196(4) Uani 1 1 d . . . N2 N 0.78144(17) 0.75103(10) 0.87976(9) 0.0214(4) Uani 1 1 d . . . N3 N 0.58318(17) 0.67245(11) 0.84590(9) 0.0225(4) Uani 1 1 d . . . N4 N 0.90771(19) 0.92266(11) 0.75561(10) 0.0277(5) Uani 1 1 d . . . N5 N 1.0943(2) 0.92583(12) 0.87629(10) 0.0294(5) Uani 1 1 d . . . H5N H 1.123(3) 0.8930(17) 0.8583(15) 0.035 Uiso 1 1 d . . . N6 N 1.1485(2) 0.80287(13) 0.97345(10) 0.0308(5) Uani 1 1 d . . . H6N H 1.073(3) 0.8122(16) 0.9596(14) 0.037 Uiso 1 1 d . . . O1 O 0.92277(15) 0.82513(10) 0.92940(8) 0.0289(4) Uani 1 1 d . . . O2 O 0.93401(18) 0.98545(11) 0.88961(10) 0.0427(5) Uani 1 1 d . . . C1 C 0.7660(2) 0.83529(13) 0.72023(11) 0.0232(5) Uani 1 1 d . . . H1 H 0.7155 0.8146 0.6867 0.028 Uiso 1 1 calc R . . C2 C 0.8380(2) 0.89047(14) 0.71006(12) 0.0267(5) Uani 1 1 d . . . H2 H 0.8370 0.9055 0.6692 0.032 Uiso 1 1 calc R . . C3 C 0.9085(2) 0.89867(13) 0.81237(11) 0.0249(5) Uani 1 1 d . . . C4 C 0.8414(2) 0.84226(12) 0.82349(11) 0.0206(5) Uani 1 1 d . . . C5 C 0.8506(2) 0.80584(13) 0.88373(11) 0.0218(5) Uani 1 1 d . . . C6 C 0.7993(2) 0.70313(14) 0.93169(12) 0.0288(6) Uani 1 1 d . . . H6A H 0.7531 0.7188 0.9624 0.035 Uiso 1 1 calc R . . H6B H 0.8824 0.7034 0.9514 0.035 Uiso 1 1 calc R . . C7 C 0.7633(2) 0.62958(14) 0.91111(12) 0.0290(6) Uani 1 1 d . . . H7A H 0.8052 0.6151 0.8782 0.035 Uiso 1 1 calc R . . H7B H 0.7847 0.5971 0.9460 0.035 Uiso 1 1 calc R . . C8 C 0.6349(2) 0.62601(13) 0.88799(12) 0.0256(5) Uani 1 1 d . . . C9 C 0.5682(2) 0.57815(15) 0.91379(14) 0.0355(6) Uani 1 1 d . . . H9 H 0.6056 0.5441 0.9416 0.043 Uiso 1 1 calc R . . C10 C 0.4490(3) 0.57974(16) 0.89942(15) 0.0406(7) Uani 1 1 d . . . H10 H 0.4036 0.5470 0.9169 0.049 Uiso 1 1 calc R . . C11 C 0.3963(2) 0.62971(15) 0.85918(13) 0.0333(6) Uani 1 1 d . . . H11 H 0.3140 0.6335 0.8499 0.040 Uiso 1 1 calc R . . C12 C 0.4653(2) 0.67398(13) 0.83266(12) 0.0254(5) Uani 1 1 d . . . H12 H 0.4287 0.7072 0.8037 0.031 Uiso 1 1 calc R . . C13 C 0.9807(2) 0.93976(14) 0.86420(12) 0.0294(6) Uani 1 1 d . . . C14 C 1.1714(3) 0.96100(16) 0.92608(13) 0.0358(7) Uani 1 1 d . . . H14A H 1.1487 1.0105 0.9268 0.043 Uiso 1 1 calc R . . H14B H 1.2520 0.9590 0.9183 0.043 Uiso 1 1 calc R . . C15 C 1.1674(3) 0.92820(16) 0.98919(13) 0.0396(7) Uani 1 1 d . . . H15A H 1.2112 0.9580 1.0219 0.047 Uiso 1 1 calc R . . H15B H 1.0858 0.9260 0.9953 0.047 Uiso 1 1 calc R . . C16 C 1.2180(2) 0.85700(16) 0.99439(12) 0.0343(6) Uani 1 1 d . . . C17 C 1.3337(3) 0.8420(2) 1.01777(15) 0.0479(8) Uani 1 1 d . . . H17 H 1.3858 0.8783 1.0333 0.057 Uiso 1 1 calc R . . C18 C 1.3729(3) 0.7746(2) 1.01848(17) 0.0557(9) Uani 1 1 d . . . H18 H 1.4521 0.7647 1.0347 0.067 Uiso 1 1 calc R . . C19 C 1.2986(3) 0.7210(2) 0.99597(15) 0.0472(8) Uani 1 1 d . . . H19 H 1.3258 0.6744 0.9962 0.057 Uiso 1 1 calc R . . C20 C 1.1849(3) 0.73674(16) 0.97338(12) 0.0359(6) Uani 1 1 d . . . H20 H 1.1318 0.7009 0.9577 0.043 Uiso 1 1 calc R . . N7 N 0.57210(17) 0.81668(10) 0.82297(9) 0.0202(4) Uani 1 1 d . . . N8 N 0.56015(16) 0.73941(10) 0.72873(9) 0.0195(4) Uani 1 1 d . . . N9 N 0.76596(17) 0.66765(10) 0.77270(9) 0.0207(4) Uani 1 1 d . . . N10 N 0.42940(19) 0.93119(12) 0.82995(10) 0.0297(5) Uani 1 1 d . . . N11 N 0.23446(19) 0.91414(12) 0.71433(10) 0.0257(5) Uani 1 1 d . . . H11N H 0.210(3) 0.8876(16) 0.7381(14) 0.031 Uiso 1 1 d . . . N12 N 0.1783(2) 0.77963(14) 0.62847(11) 0.0357(6) Uani 1 1 d . . . H12N H 0.252(3) 0.7888(18) 0.6435(15) 0.043 Uiso 1 1 d . . . O3 O 0.40896(15) 0.80168(9) 0.67222(8) 0.0264(4) Uani 1 1 d . . . O4 O 0.39202(16) 0.96627(10) 0.68844(9) 0.0335(4) Uani 1 1 d . . . C21 C 0.5779(2) 0.85166(14) 0.87549(11) 0.0256(5) Uani 1 1 d . . . H21 H 0.6318 0.8378 0.9108 0.031 Uiso 1 1 calc R . . C22 C 0.5053(2) 0.90832(14) 0.87847(12) 0.0303(6) Uani 1 1 d . . . H22 H 0.5097 0.9318 0.9165 0.036 Uiso 1 1 calc R . . C23 C 0.4252(2) 0.89581(13) 0.77765(11) 0.0237(5) Uani 1 1 d . . . C24 C 0.4938(2) 0.83762(12) 0.77360(11) 0.0208(5) Uani 1 1 d . . . C25 C 0.4850(2) 0.79132(12) 0.71901(11) 0.0201(5) Uani 1 1 d . . . C26 C 0.5495(2) 0.68520(13) 0.68176(11) 0.0250(5) Uani 1 1 d . . . H26A H 0.5967 0.6979 0.6506 0.030 Uiso 1 1 calc R . . H26B H 0.4674 0.6813 0.6610 0.030 Uiso 1 1 calc R . . C27 C 0.5906(2) 0.61573(13) 0.71030(12) 0.0246(5) Uani 1 1 d . . . H27A H 0.5486 0.6054 0.7442 0.029 Uiso 1 1 calc R . . H27B H 0.5720 0.5786 0.6791 0.029 Uiso 1 1 calc R . . C28 C 0.7188(2) 0.61594(12) 0.73451(11) 0.0211(5) Uani 1 1 d . . . C29 C 0.7890(2) 0.56551(13) 0.71537(12) 0.0267(5) Uani 1 1 d . . . H29 H 0.7547 0.5296 0.6887 0.032 Uiso 1 1 calc R . . C30 C 0.9077(2) 0.56687(15) 0.73450(13) 0.0332(6) Uani 1 1 d . . . H30 H 0.9554 0.5316 0.7221 0.040 Uiso 1 1 calc R . . C31 C 0.9558(2) 0.62039(14) 0.77190(13) 0.0298(6) Uani 1 1 d . . . H31 H 1.0376 0.6233 0.7851 0.036 Uiso 1 1 calc R . . C32 C 0.8836(2) 0.66950(13) 0.78975(12) 0.0249(5) Uani 1 1 d . . . H32 H 0.9175 0.7066 0.8152 0.030 Uiso 1 1 calc R . . C33 C 0.3480(2) 0.92760(13) 0.72168(11) 0.0245(5) Uani 1 1 d . . . C34 C 0.1525(2) 0.94320(15) 0.66283(12) 0.0322(6) Uani 1 1 d . . . H34A H 0.1732 0.9923 0.6569 0.039 Uiso 1 1 calc R . . H34B H 0.0733 0.9423 0.6727 0.039 Uiso 1 1 calc R . . C35 C 0.1523(3) 0.90289(17) 0.60287(13) 0.0379(7) Uani 1 1 d . . . H35A H 0.1048 0.9285 0.5685 0.046 Uiso 1 1 calc R . . H35B H 0.2328 0.9003 0.5949 0.046 Uiso 1 1 calc R . . C36 C 0.1052(2) 0.83094(17) 0.60499(12) 0.0349(7) Uani 1 1 d . . . C37 C -0.0104(3) 0.8136(2) 0.58462(14) 0.0438(8) Uani 1 1 d . . . H37 H -0.0645 0.8486 0.5681 0.053 Uiso 1 1 calc R . . C38 C -0.0470(3) 0.7459(2) 0.58830(15) 0.0510(9) Uani 1 1 d . . . H38 H -0.1264 0.7343 0.5745 0.061 Uiso 1 1 calc R . . C39 C 0.0318(3) 0.6948(2) 0.61213(15) 0.0487(8) Uani 1 1 d . . . H39 H 0.0074 0.6479 0.6143 0.058 Uiso 1 1 calc R . . C40 C 0.1453(3) 0.71307(18) 0.63244(14) 0.0428(7) Uani 1 1 d . . . H40 H 0.2005 0.6789 0.6493 0.051 Uiso 1 1 calc R . . B1 B 0.6735(3) 0.61845(18) 0.53987(15) 0.0365(7) Uani 1 1 d . . . F11 F 0.6323(2) 0.68332(11) 0.51643(9) 0.0643(6) Uani 1 1 d . . . F12 F 0.70767(19) 0.58097(11) 0.49335(8) 0.0570(6) Uani 1 1 d . . . F13 F 0.76409(19) 0.62820(11) 0.58782(9) 0.0601(6) Uani 1 1 d . . . F14 F 0.58570(18) 0.58381(13) 0.56093(11) 0.0677(6) Uani 1 1 d . . . B2 B 1.1666(3) 0.77041(19) 0.80050(17) 0.0414(8) Uani 1 1 d . . . F21 F 1.2449(2) 0.81857(13) 0.83151(14) 0.0830(8) Uani 1 1 d . . . F22 F 1.2245(2) 0.72732(14) 0.76856(10) 0.0772(8) Uani 1 1 d . . . F23 F 1.1163(2) 0.73571(14) 0.84202(9) 0.0802(9) Uani 1 1 d . . . F24 F 1.0828(2) 0.80604(13) 0.75984(13) 0.0787(8) Uani 1 1 d . . . B3 B 0.1465(4) 0.5328(2) 0.93151(19) 0.0481(9) Uani 1 1 d . . . F31 F 0.2366(11) 0.5588(8) 0.9698(6) 0.107(4) Uani 0.55 1 d P A 1 F32 F 0.1719(11) 0.5296(6) 0.8741(5) 0.091(4) Uani 0.55 1 d P A 1 F33 F 0.1193(11) 0.4704(6) 0.9508(6) 0.120(5) Uani 0.55 1 d P A 1 F34 F 0.0497(14) 0.5746(7) 0.9338(8) 0.110(5) Uani 0.55 1 d P A 1 F35 F 0.1794(8) 0.5439(7) 0.8746(5) 0.076(4) Uani 0.45 1 d P A 2 F36 F 0.2476(14) 0.5348(8) 0.9783(6) 0.061(3) Uani 0.45 1 d P A 2 F37 F 0.0734(16) 0.5825(6) 0.9403(8) 0.075(4) Uani 0.45 1 d P A 2 F38 F 0.1014(10) 0.4656(7) 0.9294(6) 0.068(3) Uani 0.45 1 d P A 2 O50 O 0.7284(4) 1.06485(19) 0.85434(16) 0.1000(13) Uani 1 1 d . . . H50 H 0.7917 1.0413 0.8649 0.120 Uiso 1 1 d . . . C50 C 0.7318(6) 1.0623(3) 0.7933(4) 0.122(3) Uani 1 1 d . . . H50A H 0.8137 1.0562 0.7884 0.147 Uiso 1 1 calc R . . H50B H 0.7050 1.1076 0.7748 0.147 Uiso 1 1 calc R . . C51 C 0.6490(4) 0.9970(2) 0.7524(4) 0.142(3) Uani 1 1 d . . . H51A H 0.6568 0.9994 0.7092 0.170 Uiso 1 1 calc R . . H51B H 0.5672 1.0031 0.7558 0.170 Uiso 1 1 calc R . . H51C H 0.6764 0.9516 0.7693 0.170 Uiso 1 1 calc R . . O60 O 0.6835(6) 0.8035(4) 0.5827(3) 0.078(2) Uani 0.45 1 d PD B 1 H60 H 0.6941 0.7720 0.5581 0.094 Uiso 0.45 1 calc PR B 1 O61 O 0.5829(4) 0.9172(2) 0.6388(2) 0.0526(11) Uani 0.55 1 d PD C 2 H61 H 0.5309 0.9357 0.6550 0.063 Uiso 0.55 1 calc PR C 2 C60 C 0.5341(4) 0.8941(2) 0.57900(17) 0.0675(11) Uani 1 1 d D . . H66A H 0.5004 0.9281 0.5479 0.081 Uiso 0.45 1 calc PR C 1 H66B H 0.5700 0.9185 0.6165 0.081 Uiso 0.45 1 calc PR C 1 H66C H 0.4728 0.8632 0.5881 0.081 Uiso 0.45 1 calc PR C 1 H60A H 0.5108 0.9344 0.5518 0.081 Uiso 0.55 1 calc PR C 2 H60B H 0.4643 0.8653 0.5802 0.081 Uiso 0.55 1 calc PR C 2 C61 C 0.6274(5) 0.8507(2) 0.5546(2) 0.0778(13) Uani 1 1 d D B . H65A H 0.5882 0.8304 0.5152 0.093 Uiso 0.45 1 calc PR D 1 H65B H 0.6849 0.8844 0.5444 0.093 Uiso 0.45 1 calc PR D 1 H61A H 0.5956 0.8339 0.5132 0.093 Uiso 0.55 1 calc PR D 2 H61B H 0.6498 0.8109 0.5818 0.093 Uiso 0.55 1 calc PR D 2 H61C H 0.6958 0.8797 0.5534 0.093 Uiso 0.55 1 calc PR D 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 Co1 0.01332(15) 0.01835(16) 0.01946(16) -0.00132(12) 0.00099(11) -0.00127(12) N1 0.0171(10) 0.0200(10) 0.0210(10) -0.0016(8) 0.0017(8) -0.0009(8) N2 0.0179(10) 0.0245(11) 0.0209(10) 0.0006(8) 0.0009(8) -0.0011(8) N3 0.0197(10) 0.0234(10) 0.0247(10) -0.0005(8) 0.0046(8) -0.0027(8) N4 0.0250(11) 0.0282(11) 0.0296(11) 0.0015(9) 0.0040(9) -0.0059(9) N5 0.0281(12) 0.0309(12) 0.0280(12) -0.0042(9) 0.0020(9) -0.0105(10) N6 0.0229(11) 0.0445(14) 0.0226(11) 0.0000(10) -0.0021(9) -0.0059(10) O1 0.0216(9) 0.0400(11) 0.0232(9) -0.0039(8) -0.0011(7) -0.0083(8) O2 0.0380(12) 0.0427(12) 0.0472(13) -0.0201(10) 0.0069(9) -0.0062(10) C1 0.0204(12) 0.0274(13) 0.0212(12) -0.0003(10) 0.0020(9) -0.0004(10) C2 0.0243(13) 0.0306(14) 0.0250(13) 0.0042(10) 0.0035(10) -0.0019(10) C3 0.0224(12) 0.0262(13) 0.0261(13) -0.0025(10) 0.0044(10) -0.0035(10) C4 0.0159(11) 0.0230(12) 0.0226(12) -0.0026(9) 0.0027(9) -0.0011(9) C5 0.0157(11) 0.0268(13) 0.0223(12) -0.0024(10) 0.0015(9) -0.0010(9) C6 0.0250(13) 0.0342(15) 0.0252(13) 0.0066(11) -0.0008(10) -0.0035(11) C7 0.0241(13) 0.0298(14) 0.0322(14) 0.0088(11) 0.0023(11) 0.0011(10) C8 0.0238(13) 0.0240(12) 0.0292(13) 0.0021(10) 0.0057(10) -0.0007(10) C9 0.0312(15) 0.0326(15) 0.0429(16) 0.0112(12) 0.0073(12) -0.0016(12) C10 0.0341(16) 0.0394(17) 0.0508(18) 0.0096(14) 0.0142(14) -0.0070(13) C11 0.0205(13) 0.0359(15) 0.0442(16) 0.0009(12) 0.0080(11) -0.0038(11) C12 0.0205(12) 0.0252(13) 0.0309(13) -0.0004(10) 0.0053(10) -0.0020(10) C13 0.0292(14) 0.0298(14) 0.0295(14) -0.0035(11) 0.0065(11) -0.0110(11) C14 0.0313(15) 0.0372(16) 0.0356(15) -0.0033(12) -0.0031(12) -0.0155(12) C15 0.0419(17) 0.0460(18) 0.0287(14) -0.0076(13) 0.0008(12) -0.0127(14) C16 0.0302(14) 0.0503(18) 0.0214(13) -0.0015(12) 0.0016(11) -0.0101(13) C17 0.0298(16) 0.067(2) 0.0424(18) -0.0002(16) -0.0051(13) -0.0152(15) C18 0.0285(16) 0.078(3) 0.057(2) 0.0062(19) -0.0009(15) 0.0040(17) C19 0.0427(18) 0.059(2) 0.0390(17) 0.0039(15) 0.0048(14) 0.0097(16) C20 0.0363(16) 0.0452(17) 0.0252(13) 0.0022(12) 0.0028(11) -0.0031(13) N7 0.0169(10) 0.0224(10) 0.0208(10) -0.0018(8) 0.0021(8) -0.0007(8) N8 0.0172(9) 0.0191(9) 0.0210(10) -0.0032(8) 0.0000(7) -0.0012(8) N9 0.0178(10) 0.0201(10) 0.0241(10) -0.0003(8) 0.0034(8) 0.0002(8) N10 0.0270(12) 0.0304(12) 0.0303(12) -0.0052(9) 0.0013(9) 0.0051(9) N11 0.0236(11) 0.0270(11) 0.0251(11) 0.0000(9) 0.0008(9) 0.0032(9) N12 0.0228(12) 0.0568(17) 0.0253(12) -0.0082(11) -0.0015(9) -0.0038(11) O3 0.0220(9) 0.0292(10) 0.0250(9) -0.0037(7) -0.0034(7) 0.0034(7) O4 0.0279(10) 0.0354(11) 0.0369(11) 0.0077(9) 0.0047(8) 0.0041(8) C21 0.0230(12) 0.0319(14) 0.0207(12) -0.0034(10) 0.0009(10) 0.0011(10) C22 0.0286(14) 0.0344(15) 0.0266(13) -0.0085(11) 0.0014(11) 0.0050(11) C23 0.0208(12) 0.0233(12) 0.0269(13) -0.0030(10) 0.0043(10) -0.0008(10) C24 0.0165(11) 0.0224(12) 0.0226(12) 0.0000(9) 0.0013(9) -0.0020(9) C25 0.0160(11) 0.0213(12) 0.0225(12) -0.0005(9) 0.0023(9) -0.0025(9) C26 0.0243(13) 0.0234(12) 0.0240(12) -0.0064(10) -0.0039(10) 0.0029(10) C27 0.0246(13) 0.0203(12) 0.0274(13) -0.0056(10) 0.0009(10) -0.0014(10) C28 0.0236(12) 0.0174(11) 0.0222(11) 0.0027(9) 0.0035(9) -0.0010(9) C29 0.0310(14) 0.0195(12) 0.0292(13) -0.0025(10) 0.0040(11) 0.0010(10) C30 0.0301(14) 0.0299(14) 0.0409(16) -0.0048(12) 0.0097(12) 0.0081(11) C31 0.0197(12) 0.0309(14) 0.0393(15) -0.0002(12) 0.0065(11) 0.0022(10) C32 0.0192(12) 0.0252(13) 0.0301(13) -0.0010(10) 0.0035(10) -0.0004(10) C33 0.0266(13) 0.0209(12) 0.0254(12) -0.0039(10) 0.0029(10) 0.0056(10) C34 0.0254(14) 0.0384(15) 0.0307(14) 0.0032(12) -0.0006(11) 0.0057(12) C35 0.0285(14) 0.059(2) 0.0250(14) 0.0035(13) 0.0017(11) 0.0013(13) C36 0.0251(14) 0.0604(19) 0.0184(12) -0.0088(12) 0.0019(10) -0.0025(13) C37 0.0244(14) 0.071(2) 0.0338(15) -0.0139(15) -0.0010(12) -0.0004(14) C38 0.0280(16) 0.079(3) 0.0440(18) -0.0193(17) 0.0021(13) -0.0132(16) C39 0.0452(19) 0.060(2) 0.0393(17) -0.0136(15) 0.0045(14) -0.0155(16) C40 0.0402(17) 0.055(2) 0.0314(15) -0.0116(14) 0.0020(13) -0.0033(15) B1 0.0398(19) 0.0399(18) 0.0279(16) 0.0051(14) 0.0013(13) 0.0113(15) F11 0.0974(17) 0.0493(12) 0.0439(11) 0.0079(9) 0.0070(11) 0.0379(12) F12 0.0758(14) 0.0604(13) 0.0338(10) 0.0055(9) 0.0074(9) 0.0391(11) F13 0.0672(14) 0.0543(12) 0.0479(11) 0.0070(9) -0.0185(10) -0.0110(10) F14 0.0452(12) 0.0886(17) 0.0687(14) 0.0152(12) 0.0089(10) -0.0001(11) B2 0.049(2) 0.0349(18) 0.047(2) 0.0002(15) 0.0245(17) 0.0003(16) F21 0.0692(15) 0.0652(15) 0.126(2) -0.0333(15) 0.0482(15) -0.0402(12) F22 0.0741(15) 0.1047(19) 0.0455(12) -0.0206(12) -0.0089(10) 0.0575(14) F23 0.0834(16) 0.121(2) 0.0324(10) 0.0072(11) 0.0009(10) -0.0725(16) F24 0.0558(14) 0.0706(15) 0.117(2) 0.0394(14) 0.0368(14) 0.0344(12) B3 0.044(2) 0.049(2) 0.051(2) -0.0011(18) 0.0072(17) -0.0184(18) F31 0.073(7) 0.178(13) 0.081(8) -0.070(7) 0.039(6) -0.071(7) F32 0.153(9) 0.066(4) 0.051(5) -0.026(3) 0.009(5) -0.003(4) F33 0.109(7) 0.062(6) 0.179(12) 0.055(7) -0.001(7) -0.018(4) F34 0.067(5) 0.132(10) 0.140(11) 0.017(7) 0.040(6) 0.028(6) F35 0.045(4) 0.130(9) 0.051(6) 0.030(5) 0.003(3) -0.044(5) F36 0.047(4) 0.099(7) 0.034(3) 0.009(4) 0.000(3) 0.004(5) F37 0.108(11) 0.032(3) 0.079(6) -0.007(3) 0.001(6) 0.007(4) F38 0.054(4) 0.058(5) 0.096(6) -0.020(5) 0.025(5) -0.030(4) O50 0.159(4) 0.087(2) 0.0593(19) 0.0060(17) 0.034(2) 0.060(2) C50 0.106(5) 0.069(4) 0.171(7) 0.019(4) -0.029(5) 0.008(3) C51 0.050(3) 0.061(3) 0.333(10) 0.093(5) 0.082(4) 0.033(2) O60 0.071(4) 0.110(6) 0.044(3) -0.027(3) -0.014(3) 0.043(4) O61 0.048(3) 0.055(3) 0.054(3) -0.005(2) 0.008(2) 0.003(2) C60 0.103(3) 0.054(2) 0.041(2) -0.0101(17) 0.000(2) -0.009(2) C61 0.104(4) 0.067(3) 0.063(3) 0.006(2) 0.018(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.924(2) . y Co1 N8 1.9309(19) . y Co1 N1 1.956(2) . y Co1 N7 1.971(2) . y Co1 N9 1.980(2) . y Co1 N3 1.983(2) . y N1 C1 1.326(3) . ? N1 C4 1.354(3) . ? N2 C5 1.322(3) . ? N2 C6 1.460(3) . ? N3 C8 1.353(3) . ? N3 C12 1.356(3) . ? N4 C2 1.331(3) . ? N4 C3 1.339(3) . ? N5 C13 1.334(4) . ? N5 C14 1.459(3) . ? N6 C20 1.341(4) . ? N6 C16 1.351(4) . ? O1 C5 1.251(3) . ? O2 C13 1.224(3) . ? C1 C2 1.398(4) . ? C3 C4 1.388(3) . ? C3 C13 1.519(3) . ? C4 C5 1.494(3) . ? C6 C7 1.522(4) . ? C7 C8 1.498(4) . ? C8 C9 1.395(4) . ? C9 C10 1.373(4) . ? C10 C11 1.378(4) . ? C11 C12 1.376(4) . ? C14 C15 1.543(4) . ? C15 C16 1.488(4) . ? C16 C17 1.389(4) . ? C17 C18 1.374(5) . ? C18 C19 1.382(5) . ? C19 C20 1.368(4) . ? N7 C21 1.336(3) . ? N7 C24 1.355(3) . ? N8 C25 1.322(3) . ? N8 C26 1.463(3) . ? N9 C28 1.357(3) . ? N9 C32 1.360(3) . ? N10 C23 1.338(3) . ? N10 C22 1.339(3) . ? N11 C33 1.334(3) . ? N11 C34 1.462(3) . ? N12 C40 1.345(4) . ? N12 C36 1.347(4) . ? O3 C25 1.254(3) . ? O4 C33 1.224(3) . ? C21 C22 1.391(4) . ? C23 C24 1.389(3) . ? C23 C33 1.524(3) . ? C24 C25 1.491(3) . ? C26 C27 1.519(3) . ? C27 C28 1.498(3) . ? C28 C29 1.386(3) . ? C29 C30 1.376(4) . ? C30 C31 1.377(4) . ? C31 C32 1.372(4) . ? C34 C35 1.539(4) . ? C35 C36 1.494(4) . ? C36 C37 1.385(4) . ? C37 C38 1.379(5) . ? C38 C39 1.384(5) . ? C39 C40 1.368(4) . ? B1 F13 1.371(4) . ? B1 F14 1.374(4) . ? B1 F12 1.376(4) . ? B1 F11 1.403(4) . ? B2 F22 1.349(4) . ? B2 F23 1.355(4) . ? B2 F24 1.387(4) . ? B2 F21 1.393(4) . ? B3 F37 1.320(15) . ? B3 F31 1.325(14) . ? B3 F33 1.332(12) . ? B3 F32 1.360(11) . ? B3 F38 1.394(13) . ? B3 F34 1.397(16) . ? B3 F35 1.401(12) . ? B3 F36 1.425(14) . ? O50 C50 1.362(8) . ? C50 C51 1.738(9) . ? O60 C61 1.222(7) . ? O61 C60 1.417(5) . ? C60 C61 1.547(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 N2 Co1 N8 173.72(9) . . y N2 Co1 N1 82.02(8) . . y N8 Co1 N1 93.74(8) . . y N2 Co1 N7 93.54(8) . . y N8 Co1 N7 81.50(8) . . y N1 Co1 N7 85.98(8) . . y N2 Co1 N9 93.46(8) . . y N8 Co1 N9 91.14(8) . . y N1 Co1 N9 89.63(8) . . y N7 Co1 N9 171.15(8) . . y N2 Co1 N3 89.68(8) . . y N8 Co1 N3 94.22(8) . . y N1 Co1 N3 170.95(8) . . y N7 Co1 N3 90.95(8) . . y N9 Co1 N3 94.50(8) . . y C1 N1 C4 118.5(2) . . ? C1 N1 Co1 128.73(17) . . ? C4 N1 Co1 112.69(16) . . ? C5 N2 C6 116.9(2) . . ? C5 N2 Co1 116.85(16) . . ? C6 N2 Co1 126.18(16) . . ? C8 N3 C12 118.3(2) . . ? C8 N3 Co1 123.00(16) . . ? C12 N3 Co1 118.73(17) . . ? C2 N4 C3 116.9(2) . . ? C13 N5 C14 121.0(2) . . ? C20 N6 C16 124.1(3) . . ? N1 C1 C2 120.1(2) . . ? N4 C2 C1 122.4(2) . . ? N4 C3 C4 121.9(2) . . ? N4 C3 C13 116.1(2) . . ? C4 C3 C13 121.8(2) . . ? N1 C4 C3 120.1(2) . . ? N1 C4 C5 114.6(2) . . ? C3 C4 C5 125.0(2) . . ? O1 C5 N2 127.2(2) . . ? O1 C5 C4 120.9(2) . . ? N2 C5 C4 111.7(2) . . ? N2 C6 C7 111.0(2) . . ? C8 C7 C6 110.5(2) . . ? N3 C8 C9 120.4(2) . . ? N3 C8 C7 120.1(2) . . ? C9 C8 C7 119.4(2) . . ? C10 C9 C8 120.7(3) . . ? C9 C10 C11 118.8(3) . . ? C12 C11 C10 118.7(3) . . ? N3 C12 C11 123.1(2) . . ? O2 C13 N5 124.2(2) . . ? O2 C13 C3 119.2(2) . . ? N5 C13 C3 116.4(2) . . ? N5 C14 C15 112.4(2) . . ? C16 C15 C14 111.7(3) . . ? N6 C16 C17 116.9(3) . . ? N6 C16 C15 118.5(3) . . ? C17 C16 C15 124.6(3) . . ? C18 C17 C16 120.1(3) . . ? C17 C18 C19 120.9(3) . . ? C20 C19 C18 118.2(3) . . ? N6 C20 C19 119.8(3) . . ? C21 N7 C24 118.3(2) . . ? C21 N7 Co1 128.35(17) . . ? C24 N7 Co1 113.19(16) . . ? C25 N8 C26 117.02(19) . . ? C25 N8 Co1 117.61(16) . . ? C26 N8 Co1 125.34(15) . . ? C28 N9 C32 118.0(2) . . ? C28 N9 Co1 123.11(16) . . ? C32 N9 Co1 118.93(16) . . ? C23 N10 C22 116.4(2) . . ? C33 N11 C34 121.2(2) . . ? C40 N12 C36 123.6(3) . . ? N7 C21 C22 120.1(2) . . ? N10 C22 C21 122.8(2) . . ? N10 C23 C24 122.4(2) . . ? N10 C23 C33 115.1(2) . . ? C24 C23 C33 122.3(2) . . ? N7 C24 C23 120.1(2) . . ? N7 C24 C25 114.5(2) . . ? C23 C24 C25 125.3(2) . . ? O3 C25 N8 127.3(2) . . ? O3 C25 C24 120.7(2) . . ? N8 C25 C24 111.9(2) . . ? N8 C26 C27 110.5(2) . . ? C28 C27 C26 111.6(2) . . ? N9 C28 C29 120.5(2) . . ? N9 C28 C27 119.5(2) . . ? C29 C28 C27 119.9(2) . . ? C30 C29 C28 120.8(2) . . ? C29 C30 C31 118.7(2) . . ? C32 C31 C30 118.8(2) . . ? N9 C32 C31 123.1(2) . . ? O4 C33 N11 124.2(2) . . ? O4 C33 C23 118.8(2) . . ? N11 C33 C23 116.8(2) . . ? N11 C34 C35 112.4(2) . . ? C36 C35 C34 112.5(2) . . ? N12 C36 C37 117.6(3) . . ? N12 C36 C35 118.6(2) . . ? C37 C36 C35 123.8(3) . . ? C38 C37 C36 120.2(3) . . ? C37 C38 C39 120.0(3) . . ? C40 C39 C38 118.9(3) . . ? N12 C40 C39 119.7(3) . . ? F13 B1 F14 108.8(3) . . ? F13 B1 F12 111.3(3) . . ? F14 B1 F12 109.7(3) . . ? F13 B1 F11 109.3(3) . . ? F14 B1 F11 109.3(3) . . ? F12 B1 F11 108.4(2) . . ? F22 B2 F23 112.0(3) . . ? F22 B2 F24 109.0(3) . . ? F23 B2 F24 110.0(3) . . ? F22 B2 F21 108.7(3) . . ? F23 B2 F21 108.7(3) . . ? F24 B2 F21 108.4(3) . . ? F37 B3 F31 95.3(10) . . ? F37 B3 F33 113.9(10) . . ? F31 B3 F33 110.0(8) . . ? F37 B3 F32 115.4(10) . . ? F31 B3 F32 109.5(8) . . ? F33 B3 F32 111.4(8) . . ? F37 B3 F38 115.1(9) . . ? F31 B3 F38 128.5(9) . . ? F33 B3 F38 20.6(10) . . ? F32 B3 F38 94.1(7) . . ? F37 B3 F34 13.4(12) . . ? F31 B3 F34 108.3(10) . . ? F33 B3 F34 105.4(10) . . ? F32 B3 F34 112.1(10) . . ? F38 B3 F34 103.4(9) . . ? F37 B3 F35 108.3(10) . . ? F31 B3 F35 101.8(8) . . ? F33 B3 F35 123.2(9) . . ? F32 B3 F35 11.9(9) . . ? F38 B3 F35 106.0(8) . . ? F34 B3 F35 107.6(10) . . ? F37 B3 F36 110.3(10) . . ? F31 B3 F36 20.8(10) . . ? F33 B3 F36 90.3(8) . . ? F32 B3 F36 112.9(9) . . ? F38 B3 F36 108.0(9) . . ? F34 B3 F36 121.9(10) . . ? F35 B3 F36 108.9(8) . . ? O50 C50 C51 115.5(6) . . ? O61 C60 C61 107.8(4) . . ? O60 C61 C60 124.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Co1 N1 C1 170.5(2) . . . . ? N8 Co1 N1 C1 -14.2(2) . . . . ? N7 Co1 N1 C1 -95.4(2) . . . . ? N9 Co1 N1 C1 76.9(2) . . . . ? N3 Co1 N1 C1 -165.8(5) . . . . ? N2 Co1 N1 C4 -13.02(16) . . . . ? N8 Co1 N1 C4 162.32(16) . . . . ? N7 Co1 N1 C4 81.13(17) . . . . ? N9 Co1 N1 C4 -106.57(17) . . . . ? N3 Co1 N1 C4 10.7(6) . . . . ? N8 Co1 N2 C5 -35.2(8) . . . . ? N1 Co1 N2 C5 12.61(18) . . . . ? N7 Co1 N2 C5 -72.83(18) . . . . ? N9 Co1 N2 C5 101.75(18) . . . . ? N3 Co1 N2 C5 -163.77(18) . . . . ? N8 Co1 N2 C6 147.9(7) . . . . ? N1 Co1 N2 C6 -164.3(2) . . . . ? N7 Co1 N2 C6 110.3(2) . . . . ? N9 Co1 N2 C6 -75.1(2) . . . . ? N3 Co1 N2 C6 19.3(2) . . . . ? N2 Co1 N3 C8 -37.5(2) . . . . ? N8 Co1 N3 C8 147.4(2) . . . . ? N1 Co1 N3 C8 -61.0(6) . . . . ? N7 Co1 N3 C8 -131.0(2) . . . . ? N9 Co1 N3 C8 55.9(2) . . . . ? N2 Co1 N3 C12 140.85(19) . . . . ? N8 Co1 N3 C12 -34.23(19) . . . . ? N1 Co1 N3 C12 117.4(5) . . . . ? N7 Co1 N3 C12 47.31(19) . . . . ? N9 Co1 N3 C12 -125.70(19) . . . . ? C4 N1 C1 C2 -0.2(3) . . . . ? Co1 N1 C1 C2 176.13(18) . . . . ? C3 N4 C2 C1 1.7(4) . . . . ? N1 C1 C2 N4 -2.1(4) . . . . ? C2 N4 C3 C4 0.9(4) . . . . ? C2 N4 C3 C13 -175.0(2) . . . . ? C1 N1 C4 C3 2.7(3) . . . . ? Co1 N1 C4 C3 -174.20(18) . . . . ? C1 N1 C4 C5 -171.4(2) . . . . ? Co1 N1 C4 C5 11.7(2) . . . . ? N4 C3 C4 N1 -3.2(4) . . . . ? C13 C3 C4 N1 172.5(2) . . . . ? N4 C3 C4 C5 170.3(2) . . . . ? C13 C3 C4 C5 -14.0(4) . . . . ? C6 N2 C5 O1 -7.4(4) . . . . ? Co1 N2 C5 O1 175.4(2) . . . . ? C6 N2 C5 C4 167.9(2) . . . . ? Co1 N2 C5 C4 -9.3(3) . . . . ? N1 C4 C5 O1 173.7(2) . . . . ? C3 C4 C5 O1 0.0(4) . . . . ? N1 C4 C5 N2 -1.9(3) . . . . ? C3 C4 C5 N2 -175.7(2) . . . . ? C5 N2 C6 C7 -151.5(2) . . . . ? Co1 N2 C6 C7 25.4(3) . . . . ? N2 C6 C7 C8 -65.8(3) . . . . ? C12 N3 C8 C9 4.1(4) . . . . ? Co1 N3 C8 C9 -177.5(2) . . . . ? C12 N3 C8 C7 -170.7(2) . . . . ? Co1 N3 C8 C7 7.7(3) . . . . ? C6 C7 C8 N3 50.3(3) . . . . ? C6 C7 C8 C9 -124.6(3) . . . . ? N3 C8 C9 C10 -3.5(4) . . . . ? C7 C8 C9 C10 171.4(3) . . . . ? C8 C9 C10 C11 -0.3(5) . . . . ? C9 C10 C11 C12 3.1(5) . . . . ? C8 N3 C12 C11 -1.2(4) . . . . ? Co1 N3 C12 C11 -179.7(2) . . . . ? C10 C11 C12 N3 -2.4(4) . . . . ? C14 N5 C13 O2 5.8(4) . . . . ? C14 N5 C13 C3 -178.5(2) . . . . ? N4 C3 C13 O2 93.1(3) . . . . ? C4 C3 C13 O2 -82.9(3) . . . . ? N4 C3 C13 N5 -82.8(3) . . . . ? C4 C3 C13 N5 101.2(3) . . . . ? C13 N5 C14 C15 81.0(3) . . . . ? N5 C14 C15 C16 67.7(3) . . . . ? C20 N6 C16 C17 -0.8(4) . . . . ? C20 N6 C16 C15 177.3(3) . . . . ? C14 C15 C16 N6 -85.9(3) . . . . ? C14 C15 C16 C17 92.0(3) . . . . ? N6 C16 C17 C18 0.4(5) . . . . ? C15 C16 C17 C18 -177.5(3) . . . . ? C16 C17 C18 C19 0.2(5) . . . . ? C17 C18 C19 C20 -0.5(5) . . . . ? C16 N6 C20 C19 0.5(4) . . . . ? C18 C19 C20 N6 0.1(5) . . . . ? N2 Co1 N7 C21 -9.7(2) . . . . ? N8 Co1 N7 C21 174.1(2) . . . . ? N1 Co1 N7 C21 -91.5(2) . . . . ? N9 Co1 N7 C21 -151.9(5) . . . . ? N3 Co1 N7 C21 80.0(2) . . . . ? N2 Co1 N7 C24 165.88(17) . . . . ? N8 Co1 N7 C24 -10.25(16) . . . . ? N1 Co1 N7 C24 84.15(17) . . . . ? N9 Co1 N7 C24 23.7(6) . . . . ? N3 Co1 N7 C24 -104.38(17) . . . . ? N2 Co1 N8 C25 -28.7(9) . . . . ? N1 Co1 N8 C25 -76.12(18) . . . . ? N7 Co1 N8 C25 9.25(17) . . . . ? N9 Co1 N8 C25 -165.82(18) . . . . ? N3 Co1 N8 C25 99.58(18) . . . . ? N2 Co1 N8 C26 153.2(7) . . . . ? N1 Co1 N8 C26 105.8(2) . . . . ? N7 Co1 N8 C26 -168.8(2) . . . . ? N9 Co1 N8 C26 16.1(2) . . . . ? N3 Co1 N8 C26 -78.5(2) . . . . ? N2 Co1 N9 C28 149.79(19) . . . . ? N8 Co1 N9 C28 -34.49(19) . . . . ? N1 Co1 N9 C28 -128.23(19) . . . . ? N7 Co1 N9 C28 -68.0(6) . . . . ? N3 Co1 N9 C28 59.83(19) . . . . ? N2 Co1 N9 C32 -30.11(19) . . . . ? N8 Co1 N9 C32 145.61(19) . . . . ? N1 Co1 N9 C32 51.87(19) . . . . ? N7 Co1 N9 C32 112.1(5) . . . . ? N3 Co1 N9 C32 -120.06(19) . . . . ? C24 N7 C21 C22 -0.4(4) . . . . ? Co1 N7 C21 C22 175.01(19) . . . . ? C23 N10 C22 C21 1.0(4) . . . . ? N7 C21 C22 N10 -1.4(4) . . . . ? C22 N10 C23 C24 1.2(4) . . . . ? C22 N10 C23 C33 -173.6(2) . . . . ? C21 N7 C24 C23 2.5(3) . . . . ? Co1 N7 C24 C23 -173.56(18) . . . . ? C21 N7 C24 C25 -174.1(2) . . . . ? Co1 N7 C24 C25 9.8(3) . . . . ? N10 C23 C24 N7 -3.1(4) . . . . ? C33 C23 C24 N7 171.4(2) . . . . ? N10 C23 C24 C25 173.1(2) . . . . ? C33 C23 C24 C25 -12.4(4) . . . . ? C26 N8 C25 O3 -4.3(4) . . . . ? Co1 N8 C25 O3 177.44(19) . . . . ? C26 N8 C25 C24 172.0(2) . . . . ? Co1 N8 C25 C24 -6.2(3) . . . . ? N7 C24 C25 O3 174.0(2) . . . . ? C23 C24 C25 O3 -2.4(4) . . . . ? N7 C24 C25 N8 -2.6(3) . . . . ? C23 C24 C25 N8 -179.0(2) . . . . ? C25 N8 C26 C27 -150.2(2) . . . . ? Co1 N8 C26 C27 27.9(3) . . . . ? N8 C26 C27 C28 -67.3(3) . . . . ? C32 N9 C28 C29 2.1(3) . . . . ? Co1 N9 C28 C29 -177.80(18) . . . . ? C32 N9 C28 C27 -174.6(2) . . . . ? Co1 N9 C28 C27 5.5(3) . . . . ? C26 C27 C28 N9 51.5(3) . . . . ? C26 C27 C28 C29 -125.3(2) . . . . ? N9 C28 C29 C30 -0.2(4) . . . . ? C27 C28 C29 C30 176.5(2) . . . . ? C28 C29 C30 C31 -1.6(4) . . . . ? C29 C30 C31 C32 1.4(4) . . . . ? C28 N9 C32 C31 -2.4(4) . . . . ? Co1 N9 C32 C31 177.5(2) . . . . ? C30 C31 C32 N9 0.6(4) . . . . ? C34 N11 C33 O4 2.8(4) . . . . ? C34 N11 C33 C23 178.8(2) . . . . ? N10 C23 C33 O4 93.9(3) . . . . ? C24 C23 C33 O4 -80.9(3) . . . . ? N10 C23 C33 N11 -82.3(3) . . . . ? C24 C23 C33 N11 102.9(3) . . . . ? C33 N11 C34 C35 79.2(3) . . . . ? N11 C34 C35 C36 67.2(3) . . . . ? C40 N12 C36 C37 0.7(4) . . . . ? C40 N12 C36 C35 -179.8(3) . . . . ? C34 C35 C36 N12 -86.5(3) . . . . ? C34 C35 C36 C37 92.9(3) . . . . ? N12 C36 C37 C38 -0.4(4) . . . . ? C35 C36 C37 C38 -179.9(3) . . . . ? C36 C37 C38 C39 -0.3(5) . . . . ? C37 C38 C39 C40 0.8(5) . . . . ? C36 N12 C40 C39 -0.2(4) . . . . ? C38 C39 C40 N12 -0.5(5) . . . . ? O61 C60 C61 O60 49.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.887 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.062