data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-bis(dimesitylglyoximato)-methyl-(pyridine)-cobalt(III) ; _chemical_name_common 'Methyl cobalt(III) Mesitylglyoxime Pyridine' _chemical_melting_point ? _chemical_formula_moiety '(C47 H56 Cl2 Co1 N5 O4)2' _chemical_formula_sum 'C94 H112 Cl4 Co2 N10 O8' _chemical_formula_weight 1769.60 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 27.939(15) _cell_length_b 9.226(5) _cell_length_c 37.232(2) _cell_angle_alpha 90.000(0) _cell_angle_beta 108.006(17) _cell_angle_gamma 90.000(0) _cell_volume 9127(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min -28.0 _cell_measurement_theta_max +28.0 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8903 _exptl_absorpt_correction_T_max 0.9330 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method \f/\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.05 _diffrn_reflns_number 29710 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.38 _reflns_number_total 11254 _reflns_number_gt 7754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (BRUKER, 2003)' _computing_cell_refinement 'SMART 5.628 (BRUKER, 2003)' _computing_data_reduction 'SAINT+ 6.45 (BRUKER, 2003)' _computing_structure_solution 'SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0924P)^2^+5.1353P] 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 11254 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1806 _refine_ls_wR_factor_gt 0.1621 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.009 _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 0.746778(13) 0.16310(4) 0.632344(10) 0.02739(12) Uani 1 1 d . . . Cl1 Cl 0.66990(5) -0.24131(13) 0.51110(4) 0.0905(4) Uani 1 1 d . . . Cl2 Cl 0.69059(7) -0.1746(2) 0.44201(4) 0.1336(7) Uani 1 1 d . . . O1 O 0.73913(7) 0.0842(2) 0.55744(5) 0.0383(5) Uani 1 1 d . . . O2 O 0.67520(8) 0.3079(2) 0.65938(6) 0.0405(5) Uani 1 1 d . . . O3 O 0.75748(8) 0.2564(2) 0.70748(6) 0.0413(5) Uani 1 1 d . . . H1 H 0.7253 0.2826 0.6942 0.062 Uiso 1 1 d . . . O4 O 0.82006(7) 0.0187(2) 0.60592(6) 0.0412(5) Uani 1 1 d . . . H2 H 0.7833 0.0391 0.5773 0.062 Uiso 1 1 d . . . N1 N 0.71538(9) 0.1446(2) 0.58006(6) 0.0305(5) Uani 1 1 d . . . N2 N 0.68437(9) 0.2520(2) 0.62877(7) 0.0318(5) Uani 1 1 d . . . N3 N 0.77964(9) 0.1876(2) 0.68473(6) 0.0309(5) Uani 1 1 d . . . N4 N 0.80962(8) 0.0744(2) 0.63604(6) 0.0310(5) Uani 1 1 d . . . N5 N 0.71989(8) -0.0396(3) 0.64181(7) 0.0332(5) Uani 1 1 d . . . C1 C 0.66854(10) 0.1889(3) 0.56603(8) 0.0311(6) Uani 1 1 d . . . C2 C 0.64930(10) 0.2504(3) 0.59574(8) 0.0309(6) Uani 1 1 d . . . C3 C 0.64046(11) 0.1787(3) 0.52504(8) 0.0353(6) Uani 1 1 d . . . C4 C 0.65771(12) 0.2593(3) 0.49934(9) 0.0404(7) Uani 1 1 d . . . C5 C 0.63402(15) 0.2406(4) 0.46086(10) 0.0551(9) Uani 1 1 d . . . H5 H 0.6452 0.2941 0.4438 0.066 Uiso 1 1 calc R . . C6 C 0.59437(16) 0.1451(5) 0.44705(10) 0.0642(11) Uani 1 1 d . . . C7 C 0.57750(13) 0.0678(5) 0.47259(11) 0.0608(10) Uani 1 1 d . . . H7 H 0.5506 0.0043 0.4635 0.073 Uiso 1 1 calc R . . C8 C 0.59957(12) 0.0821(4) 0.51139(10) 0.0450(8) Uani 1 1 d . . . C9 C 0.70081(13) 0.3652(4) 0.51214(10) 0.0486(8) Uani 1 1 d . . . H9A H 0.7321 0.3135 0.5183 0.073 Uiso 1 1 calc R . . H9B H 0.6986 0.4165 0.5340 0.073 Uiso 1 1 calc R . . H9C H 0.6991 0.4329 0.4922 0.073 Uiso 1 1 calc R . . C10 C 0.5719(2) 0.1220(7) 0.40452(12) 0.109(2) Uani 1 1 d . . . H10A H 0.5657 0.2143 0.3920 0.163 Uiso 1 1 calc R . . H10B H 0.5407 0.0698 0.3994 0.163 Uiso 1 1 calc R . . H10C H 0.5950 0.0674 0.3954 0.163 Uiso 1 1 calc R . . C11 C 0.58084(14) -0.0114(4) 0.53736(12) 0.0610(10) Uani 1 1 d . . . H11A H 0.5566 0.0416 0.5456 0.092 Uiso 1 1 calc R . . H11B H 0.6086 -0.0382 0.5589 0.092 Uiso 1 1 calc R . . H11C H 0.5654 -0.0971 0.5242 0.092 Uiso 1 1 calc R . . C12 C 0.59594(11) 0.2950(3) 0.58986(8) 0.0340(6) Uani 1 1 d . . . C13 C 0.56774(12) 0.2169(4) 0.60895(9) 0.0411(7) Uani 1 1 d . . . C14 C 0.51786(12) 0.2560(4) 0.60350(10) 0.0480(8) Uani 1 1 d . . . H14 H 0.4995 0.2051 0.6164 0.058 Uiso 1 1 calc R . . C15 C 0.49463(12) 0.3676(4) 0.57968(10) 0.0506(9) Uani 1 1 d . . . C16 C 0.52281(12) 0.4430(4) 0.56119(10) 0.0472(8) Uani 1 1 d . . . H16 H 0.5077 0.5182 0.5450 0.057 Uiso 1 1 calc R . . C17 C 0.57306(11) 0.4100(3) 0.56603(9) 0.0376(7) Uani 1 1 d . . . C18 C 0.58949(13) 0.0903(4) 0.63469(11) 0.0543(9) Uani 1 1 d . . . H18A H 0.6097 0.1260 0.6588 0.081 Uiso 1 1 calc R . . H18B H 0.6100 0.0327 0.6237 0.081 Uiso 1 1 calc R . . H18C H 0.5626 0.0320 0.6378 0.081 Uiso 1 1 calc R . . C19 C 0.44044(13) 0.4091(6) 0.57521(14) 0.0832(14) Uani 1 1 d . . . H19A H 0.4276 0.4688 0.5532 0.125 Uiso 1 1 calc R . . H19B H 0.4391 0.4617 0.5971 0.125 Uiso 1 1 calc R . . H19C H 0.4204 0.3229 0.5725 0.125 Uiso 1 1 calc R . . C20 C 0.60144(13) 0.5022(4) 0.54614(10) 0.0503(8) Uani 1 1 d . . . H20A H 0.5926 0.4739 0.5201 0.075 Uiso 1 1 calc R . . H20B H 0.6370 0.4893 0.5579 0.075 Uiso 1 1 calc R . . H20C H 0.5929 0.6022 0.5478 0.075 Uiso 1 1 calc R . . C21 C 0.82448(10) 0.1324(3) 0.69891(8) 0.0298(6) Uani 1 1 d . . . C22 C 0.84208(10) 0.0591(3) 0.66987(8) 0.0303(6) Uani 1 1 d . . . C23 C 0.85446(10) 0.1441(3) 0.73961(8) 0.0333(6) Uani 1 1 d . . . C24 C 0.86188(10) 0.0219(3) 0.76346(8) 0.0333(6) Uani 1 1 d . . . C25 C 0.89054(11) 0.0366(4) 0.80096(8) 0.0393(7) Uani 1 1 d . . . H25 H 0.8949 -0.0437 0.8168 0.047 Uiso 1 1 calc R . . C26 C 0.91291(12) 0.1665(4) 0.81573(9) 0.0436(8) Uani 1 1 d . . . C27 C 0.90433(12) 0.2861(4) 0.79213(9) 0.0435(7) Uani 1 1 d . . . H27 H 0.9189 0.3742 0.8018 0.052 Uiso 1 1 calc R . . C28 C 0.87483(11) 0.2791(3) 0.75459(9) 0.0371(7) Uani 1 1 d . . . C29 C 0.83758(13) -0.1225(4) 0.74973(10) 0.0493(8) Uani 1 1 d . . . H29A H 0.8582 -0.1755 0.7379 0.074 Uiso 1 1 calc R . . H29B H 0.8050 -0.1068 0.7318 0.074 Uiso 1 1 calc R . . H29C H 0.8341 -0.1769 0.7708 0.074 Uiso 1 1 calc R . . C30 C 0.94395(16) 0.1767(5) 0.85667(11) 0.0678(11) Uani 1 1 d . . . H30A H 0.9547 0.2751 0.8626 0.102 Uiso 1 1 calc R . . H30B H 0.9729 0.1151 0.8613 0.102 Uiso 1 1 calc R . . H30C H 0.9241 0.1465 0.8722 0.102 Uiso 1 1 calc R . . C31 C 0.86426(14) 0.4172(4) 0.73150(10) 0.0538(9) Uani 1 1 d . . . H31A H 0.8329 0.4576 0.7321 0.081 Uiso 1 1 calc R . . H31B H 0.8624 0.3959 0.7059 0.081 Uiso 1 1 calc R . . H31C H 0.8908 0.4856 0.7419 0.081 Uiso 1 1 calc R . . C32 C 0.88935(10) -0.0285(3) 0.67788(8) 0.0346(6) Uani 1 1 d . . . C33 C 0.88588(11) -0.1795(4) 0.67274(8) 0.0394(7) Uani 1 1 d . . . C34 C 0.93017(13) -0.2603(4) 0.68197(10) 0.0501(9) Uani 1 1 d . . . H34 H 0.9280 -0.3601 0.6784 0.060 Uiso 1 1 calc R . . C35 C 0.97734(13) -0.1974(5) 0.69630(10) 0.0539(9) Uani 1 1 d . . . C36 C 0.97987(12) -0.0485(5) 0.70016(10) 0.0537(9) Uani 1 1 d . . . H36 H 1.0113 -0.0050 0.7093 0.064 Uiso 1 1 calc R . . C37 C 0.93705(11) 0.0396(4) 0.69094(9) 0.0429(8) Uani 1 1 d . . . C38 C 0.83610(12) -0.2571(4) 0.65746(10) 0.0496(8) Uani 1 1 d . . . H38A H 0.8213 -0.2337 0.6312 0.074 Uiso 1 1 calc R . . H38B H 0.8139 -0.2271 0.6713 0.074 Uiso 1 1 calc R . . H38C H 0.8414 -0.3598 0.6602 0.074 Uiso 1 1 calc R . . C39 C 1.02468(15) -0.2898(6) 0.70791(13) 0.0825(15) Uani 1 1 d . . . H39A H 1.0466 -0.2609 0.6938 0.124 Uiso 1 1 calc R . . H39B H 1.0157 -0.3899 0.7029 0.124 Uiso 1 1 calc R . . H39C H 1.0417 -0.2770 0.7344 0.124 Uiso 1 1 calc R . . C40 C 0.94309(13) 0.2013(4) 0.69462(11) 0.0570(10) Uani 1 1 d . . . H40A H 0.9462 0.2296 0.7201 0.086 Uiso 1 1 calc R . . H40B H 0.9142 0.2476 0.6775 0.086 Uiso 1 1 calc R . . H40C H 0.9728 0.2300 0.6886 0.086 Uiso 1 1 calc R . . C41 C 0.71244(12) -0.1447(3) 0.61573(10) 0.0435(7) Uani 1 1 d . . . H41 H 0.7151 -0.1217 0.5921 0.052 Uiso 1 1 calc R . . C42 C 0.70103(14) -0.2856(4) 0.62257(12) 0.0563(9) Uani 1 1 d . . . H42 H 0.6959 -0.3553 0.6037 0.068 Uiso 1 1 calc R . . C43 C 0.69731(14) -0.3217(4) 0.65707(14) 0.0624(11) Uani 1 1 d . . . H43 H 0.6902 -0.4166 0.6622 0.075 Uiso 1 1 calc R . . C44 C 0.70412(13) -0.2164(4) 0.68403(11) 0.0527(9) Uani 1 1 d . . . H44 H 0.7015 -0.2382 0.7077 0.063 Uiso 1 1 calc R . . C45 C 0.71498(11) -0.0762(3) 0.67539(9) 0.0407(7) Uani 1 1 d . . . H45 H 0.7190 -0.0045 0.6937 0.049 Uiso 1 1 calc R . . C46 C 0.77451(12) 0.3550(3) 0.62327(10) 0.0435(7) Uani 1 1 d . . . H46A H 0.8079 0.3419 0.6217 0.065 Uiso 1 1 calc R . . H46B H 0.7756 0.4194 0.6437 0.065 Uiso 1 1 calc R . . H46C H 0.7533 0.3955 0.6001 0.065 Uiso 1 1 calc R . . C47 C 0.69595(17) -0.1198(5) 0.48684(12) 0.0683(11) Uani 1 1 d . . . H47A H 0.6795 -0.0266 0.4857 0.082 Uiso 1 1 calc R . . H47B H 0.7313 -0.1068 0.5007 0.082 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 0.0278(2) 0.0267(2) 0.0289(2) -0.00102(15) 0.01060(15) 0.00110(14) Cl1 0.1048(10) 0.0665(8) 0.1052(10) 0.0092(7) 0.0399(8) -0.0056(6) Cl2 0.1384(14) 0.196(2) 0.0704(9) -0.0358(10) 0.0388(9) -0.0055(13) O1 0.0354(11) 0.0492(13) 0.0329(11) -0.0036(9) 0.0145(9) 0.0082(9) O2 0.0423(12) 0.0453(12) 0.0379(12) -0.0045(9) 0.0180(10) 0.0099(9) O3 0.0400(11) 0.0478(13) 0.0371(12) -0.0091(10) 0.0134(9) 0.0092(10) O4 0.0370(11) 0.0600(14) 0.0289(11) -0.0048(10) 0.0134(9) 0.0096(10) N1 0.0350(13) 0.0287(12) 0.0299(12) 0.0021(9) 0.0130(10) 0.0026(9) N2 0.0350(13) 0.0290(13) 0.0346(13) 0.0006(10) 0.0156(11) 0.0034(10) N3 0.0362(13) 0.0291(12) 0.0299(12) -0.0034(9) 0.0138(10) -0.0003(9) N4 0.0294(12) 0.0325(13) 0.0340(13) -0.0025(10) 0.0141(10) -0.0003(9) N5 0.0278(12) 0.0305(13) 0.0415(14) -0.0002(10) 0.0111(10) 0.0004(9) C1 0.0317(14) 0.0275(14) 0.0360(15) 0.0032(11) 0.0130(12) 0.0011(11) C2 0.0333(14) 0.0268(14) 0.0349(15) 0.0034(11) 0.0136(12) 0.0017(11) C3 0.0315(15) 0.0342(16) 0.0383(16) -0.0007(12) 0.0079(12) 0.0050(12) C4 0.0464(18) 0.0388(18) 0.0391(17) 0.0088(13) 0.0178(14) 0.0134(14) C5 0.071(2) 0.055(2) 0.0388(19) 0.0155(16) 0.0158(18) 0.0189(19) C6 0.063(2) 0.084(3) 0.0350(19) 0.0019(19) -0.0012(17) 0.018(2) C7 0.0408(19) 0.073(3) 0.055(2) -0.010(2) -0.0052(17) -0.0028(18) C8 0.0355(16) 0.0477(19) 0.0493(19) -0.0035(15) 0.0093(15) 0.0033(14) C9 0.058(2) 0.0412(19) 0.056(2) 0.0074(15) 0.0311(18) 0.0034(15) C10 0.110(4) 0.149(5) 0.039(2) 0.001(3) -0.017(3) 0.012(4) C11 0.051(2) 0.064(2) 0.071(3) -0.006(2) 0.0218(19) -0.0179(18) C12 0.0315(15) 0.0354(15) 0.0353(16) 0.0019(12) 0.0105(12) 0.0032(12) C13 0.0386(17) 0.0434(18) 0.0431(18) 0.0010(14) 0.0151(14) 0.0028(14) C14 0.0343(16) 0.058(2) 0.055(2) -0.0001(17) 0.0177(15) -0.0007(15) C15 0.0314(16) 0.064(2) 0.052(2) -0.0021(17) 0.0055(15) 0.0064(15) C16 0.0399(17) 0.0479(19) 0.0463(19) 0.0025(15) 0.0024(15) 0.0107(14) C17 0.0370(16) 0.0350(16) 0.0389(16) -0.0018(13) 0.0089(13) 0.0024(12) C18 0.0461(19) 0.058(2) 0.063(2) 0.0221(18) 0.0232(18) 0.0088(16) C19 0.033(2) 0.109(4) 0.103(4) 0.011(3) 0.014(2) 0.018(2) C20 0.053(2) 0.0422(19) 0.055(2) 0.0100(16) 0.0144(17) 0.0038(15) C21 0.0333(15) 0.0237(14) 0.0343(15) 0.0010(11) 0.0131(12) 0.0001(10) C22 0.0285(14) 0.0321(15) 0.0316(15) -0.0011(11) 0.0111(12) -0.0019(11) C23 0.0297(14) 0.0397(17) 0.0316(15) -0.0027(12) 0.0112(12) 0.0002(12) C24 0.0308(14) 0.0360(16) 0.0347(15) 0.0029(12) 0.0122(12) 0.0021(12) C25 0.0378(16) 0.0467(18) 0.0341(16) 0.0068(14) 0.0121(13) 0.0072(13) C26 0.0369(16) 0.059(2) 0.0340(16) -0.0045(15) 0.0095(13) 0.0061(15) C27 0.0430(17) 0.0455(18) 0.0413(18) -0.0128(15) 0.0120(14) -0.0079(14) C28 0.0377(16) 0.0389(16) 0.0361(16) -0.0038(13) 0.0135(13) -0.0015(13) C29 0.055(2) 0.0430(19) 0.048(2) 0.0042(15) 0.0122(17) -0.0063(15) C30 0.068(3) 0.078(3) 0.043(2) -0.0053(19) -0.0033(19) 0.006(2) C31 0.066(2) 0.0370(19) 0.054(2) -0.0036(16) 0.0122(18) -0.0091(16) C32 0.0271(14) 0.0478(18) 0.0298(15) 0.0013(13) 0.0104(12) 0.0032(12) C33 0.0365(16) 0.0478(19) 0.0353(16) -0.0007(14) 0.0131(13) 0.0092(13) C34 0.051(2) 0.056(2) 0.0459(19) 0.0040(16) 0.0179(16) 0.0182(17) C35 0.0396(19) 0.079(3) 0.047(2) 0.0109(19) 0.0202(16) 0.0201(17) C36 0.0270(16) 0.090(3) 0.046(2) 0.0057(19) 0.0141(14) 0.0019(17) C37 0.0309(15) 0.062(2) 0.0370(17) 0.0037(15) 0.0115(13) -0.0024(14) C38 0.0479(19) 0.0411(19) 0.057(2) -0.0063(16) 0.0112(17) 0.0036(15) C39 0.052(2) 0.121(4) 0.077(3) 0.017(3) 0.023(2) 0.043(3) C40 0.044(2) 0.065(2) 0.063(2) -0.0023(19) 0.0180(18) -0.0124(17) C41 0.0379(17) 0.0400(18) 0.0491(19) -0.0036(15) 0.0082(14) -0.0010(13) C42 0.053(2) 0.0365(18) 0.074(3) -0.0095(18) 0.0111(19) -0.0063(16) C43 0.053(2) 0.036(2) 0.104(3) 0.012(2) 0.033(2) -0.0038(16) C44 0.048(2) 0.053(2) 0.064(2) 0.0135(18) 0.0271(18) -0.0008(16) C45 0.0378(16) 0.0399(17) 0.0486(18) 0.0027(14) 0.0196(14) -0.0019(13) C46 0.0496(19) 0.0300(16) 0.0505(19) 0.0035(14) 0.0150(16) -0.0047(13) C47 0.072(3) 0.064(3) 0.071(3) -0.008(2) 0.026(2) 0.004(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 N1 1.880(2) . yes Co1 N2 1.894(2) . yes Co1 N3 1.895(2) . yes Co1 N4 1.903(2) . yes Co1 C46 2.002(3) . yes Co1 N5 2.086(3) . yes Cl1 C47 1.734(5) . ? Cl2 C47 1.706(4) . ? O1 N1 1.344(3) . ? O2 N2 1.345(3) . ? O3 N3 1.352(3) . ? O4 N4 1.345(3) . ? N1 C1 1.315(4) . ? N2 C2 1.314(4) . ? N3 C21 1.303(4) . ? N4 C22 1.313(3) . ? N5 C41 1.342(4) . ? N5 C45 1.342(4) . ? C1 C2 1.484(4) . ? C1 C3 1.488(4) . ? C2 C12 1.496(4) . ? C3 C4 1.409(4) . ? C3 C8 1.414(4) . ? C4 C5 1.391(5) . ? C4 C9 1.509(5) . ? C5 C6 1.384(6) . ? C6 C7 1.382(6) . ? C6 C10 1.528(5) . ? C7 C8 1.391(5) . ? C8 C11 1.505(5) . ? C12 C17 1.404(4) . ? C12 C13 1.411(4) . ? C13 C14 1.392(4) . ? C13 C18 1.514(5) . ? C14 C15 1.383(5) . ? C15 C16 1.383(5) . ? C15 C19 1.520(5) . ? C16 C17 1.393(4) . ? C17 C20 1.505(4) . ? C21 C22 1.482(4) . ? C21 C23 1.492(4) . ? C22 C32 1.498(4) . ? C23 C24 1.410(4) . ? C23 C28 1.411(4) . ? C24 C25 1.385(4) . ? C24 C29 1.511(4) . ? C25 C26 1.385(5) . ? C26 C27 1.384(5) . ? C26 C30 1.506(5) . ? C27 C28 1.387(4) . ? C28 C31 1.514(5) . ? C32 C33 1.405(4) . ? C32 C37 1.416(4) . ? C33 C34 1.394(4) . ? C33 C38 1.510(5) . ? C34 C35 1.387(5) . ? C35 C36 1.381(6) . ? C35 C39 1.520(5) . ? C36 C37 1.398(5) . ? C37 C40 1.503(5) . ? C41 C42 1.380(5) . ? C42 C43 1.362(6) . ? C43 C44 1.368(6) . ? C44 C45 1.389(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N2 80.90(10) . . yes N1 Co1 N3 177.99(10) . . yes N2 Co1 N3 99.39(10) . . yes N1 Co1 N4 99.24(10) . . yes N2 Co1 N4 179.78(13) . . yes N3 Co1 N4 80.46(10) . . yes N1 Co1 C46 89.23(12) . . ? N2 Co1 C46 90.06(12) . . ? N3 Co1 C46 88.77(12) . . ? N4 Co1 C46 89.77(12) . . ? N1 Co1 N5 90.93(10) . . ? N2 Co1 N5 91.63(10) . . ? N3 Co1 N5 91.05(10) . . ? N4 Co1 N5 88.54(10) . . ? C46 Co1 N5 178.30(11) . . yes C1 N1 O1 120.2(2) . . ? C1 N1 Co1 118.14(19) . . ? O1 N1 Co1 121.61(17) . . ? C2 N2 O2 121.0(2) . . ? C2 N2 Co1 117.68(19) . . ? O2 N2 Co1 121.24(18) . . ? C21 N3 O3 119.9(2) . . ? C21 N3 Co1 117.99(19) . . ? O3 N3 Co1 122.06(17) . . ? C22 N4 O4 119.7(2) . . ? C22 N4 Co1 117.62(18) . . ? O4 N4 Co1 122.48(17) . . ? C41 N5 C45 117.1(3) . . ? C41 N5 Co1 120.6(2) . . ? C45 N5 Co1 121.9(2) . . ? N1 C1 C2 111.6(2) . . ? N1 C1 C3 122.1(2) . . ? C2 C1 C3 126.3(2) . . ? N2 C2 C1 111.4(2) . . ? N2 C2 C12 123.7(2) . . ? C1 C2 C12 124.8(3) . . ? C4 C3 C8 119.8(3) . . ? C4 C3 C1 118.7(3) . . ? C8 C3 C1 121.3(3) . . ? C5 C4 C3 118.7(3) . . ? C5 C4 C9 119.0(3) . . ? C3 C4 C9 122.3(3) . . ? C6 C5 C4 122.2(3) . . ? C7 C6 C5 118.5(3) . . ? C7 C6 C10 121.5(4) . . ? C5 C6 C10 120.0(4) . . ? C6 C7 C8 122.0(4) . . ? C7 C8 C3 118.9(3) . . ? C7 C8 C11 118.9(3) . . ? C3 C8 C11 122.2(3) . . ? C17 C12 C13 119.2(3) . . ? C17 C12 C2 122.6(3) . . ? C13 C12 C2 118.2(3) . . ? C14 C13 C12 118.9(3) . . ? C14 C13 C18 118.7(3) . . ? C12 C13 C18 122.4(3) . . ? C15 C14 C13 122.4(3) . . ? C16 C15 C14 117.8(3) . . ? C16 C15 C19 121.3(3) . . ? C14 C15 C19 120.8(4) . . ? C15 C16 C17 122.1(3) . . ? C16 C17 C12 119.4(3) . . ? C16 C17 C20 118.4(3) . . ? C12 C17 C20 122.2(3) . . ? N3 C21 C22 112.1(2) . . ? N3 C21 C23 123.4(2) . . ? C22 C21 C23 124.4(2) . . ? N4 C22 C21 111.4(2) . . ? N4 C22 C32 123.6(2) . . ? C21 C22 C32 124.9(2) . . ? C24 C23 C28 119.6(3) . . ? C24 C23 C21 120.6(3) . . ? C28 C23 C21 119.8(3) . . ? C25 C24 C23 118.9(3) . . ? C25 C24 C29 119.1(3) . . ? C23 C24 C29 121.9(3) . . ? C26 C25 C24 122.3(3) . . ? C27 C26 C25 118.0(3) . . ? C27 C26 C30 121.7(3) . . ? C25 C26 C30 120.3(3) . . ? C26 C27 C28 122.4(3) . . ? C27 C28 C23 118.7(3) . . ? C27 C28 C31 119.0(3) . . ? C23 C28 C31 122.3(3) . . ? C33 C32 C37 120.3(3) . . ? C33 C32 C22 119.2(3) . . ? C37 C32 C22 120.5(3) . . ? C34 C33 C32 118.6(3) . . ? C34 C33 C38 118.9(3) . . ? C32 C33 C38 122.5(3) . . ? C35 C34 C33 122.5(4) . . ? C36 C35 C34 117.9(3) . . ? C36 C35 C39 121.1(4) . . ? C34 C35 C39 121.0(4) . . ? C35 C36 C37 122.7(3) . . ? C36 C37 C32 118.0(3) . . ? C36 C37 C40 119.4(3) . . ? C32 C37 C40 122.6(3) . . ? N5 C41 C42 122.7(3) . . ? C43 C42 C41 119.6(4) . . ? C42 C43 C44 119.0(3) . . ? C43 C44 C45 118.9(3) . . ? N5 C45 C44 122.8(3) . . ? Cl2 C47 Cl1 113.2(3) . . ? 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 -3.3(2) . . . . ? N3 Co1 N1 C1 -102(3) . . . . ? N4 Co1 N1 C1 176.9(2) . . . . ? C46 Co1 N1 C1 -93.5(2) . . . . ? N5 Co1 N1 C1 88.2(2) . . . . ? N2 Co1 N1 O1 178.6(2) . . . . ? N3 Co1 N1 O1 80(3) . . . . ? N4 Co1 N1 O1 -1.3(2) . . . . ? C46 Co1 N1 O1 88.4(2) . . . . ? N5 Co1 N1 O1 -89.9(2) . . . . ? N1 Co1 N2 C2 5.1(2) . . . . ? N3 Co1 N2 C2 -176.9(2) . . . . ? N4 Co1 N2 C2 135(32) . . . . ? C46 Co1 N2 C2 94.3(2) . . . . ? N5 Co1 N2 C2 -85.6(2) . . . . ? N1 Co1 N2 O2 -178.5(2) . . . . ? N3 Co1 N2 O2 -0.5(2) . . . . ? N4 Co1 N2 O2 -49(28) . . . . ? C46 Co1 N2 O2 -89.2(2) . . . . ? N5 Co1 N2 O2 90.9(2) . . . . ? N1 Co1 N3 C21 -85(3) . . . . ? N2 Co1 N3 C21 176.9(2) . . . . ? N4 Co1 N3 C21 -3.3(2) . . . . ? C46 Co1 N3 C21 -93.3(2) . . . . ? N5 Co1 N3 C21 85.1(2) . . . . ? N1 Co1 N3 O3 97(3) . . . . ? N2 Co1 N3 O3 -1.4(2) . . . . ? N4 Co1 N3 O3 178.5(2) . . . . ? C46 Co1 N3 O3 88.5(2) . . . . ? N5 Co1 N3 O3 -93.2(2) . . . . ? N1 Co1 N4 C22 -176.3(2) . . . . ? N2 Co1 N4 C22 54(28) . . . . ? N3 Co1 N4 C22 5.7(2) . . . . ? C46 Co1 N4 C22 94.5(2) . . . . ? N5 Co1 N4 C22 -85.6(2) . . . . ? N1 Co1 N4 O4 -1.1(2) . . . . ? N2 Co1 N4 O4 -131(33) . . . . ? N3 Co1 N4 O4 -179.1(2) . . . . ? C46 Co1 N4 O4 -90.3(2) . . . . ? N5 Co1 N4 O4 89.6(2) . . . . ? N1 Co1 N5 C41 30.5(2) . . . . ? N2 Co1 N5 C41 111.4(2) . . . . ? N3 Co1 N5 C41 -149.2(2) . . . . ? N4 Co1 N5 C41 -68.7(2) . . . . ? C46 Co1 N5 C41 -65(4) . . . . ? N1 Co1 N5 C45 -157.4(2) . . . . ? N2 Co1 N5 C45 -76.5(2) . . . . ? N3 Co1 N5 C45 22.9(2) . . . . ? N4 Co1 N5 C45 103.3(2) . . . . ? C46 Co1 N5 C45 107(4) . . . . ? O1 N1 C1 C2 179.3(2) . . . . ? Co1 N1 C1 C2 1.2(3) . . . . ? O1 N1 C1 C3 -1.8(4) . . . . ? Co1 N1 C1 C3 -179.9(2) . . . . ? O2 N2 C2 C1 177.9(2) . . . . ? Co1 N2 C2 C1 -5.7(3) . . . . ? O2 N2 C2 C12 -6.4(4) . . . . ? Co1 N2 C2 C12 170.1(2) . . . . ? N1 C1 C2 N2 2.9(3) . . . . ? C3 C1 C2 N2 -176.0(3) . . . . ? N1 C1 C2 C12 -172.8(3) . . . . ? C3 C1 C2 C12 8.3(4) . . . . ? N1 C1 C3 C4 -63.7(4) . . . . ? C2 C1 C3 C4 115.0(3) . . . . ? N1 C1 C3 C8 111.4(3) . . . . ? C2 C1 C3 C8 -69.8(4) . . . . ? C8 C3 C4 C5 -0.5(4) . . . . ? C1 C3 C4 C5 174.8(3) . . . . ? C8 C3 C4 C9 179.4(3) . . . . ? C1 C3 C4 C9 -5.4(4) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? C9 C4 C5 C6 179.8(3) . . . . ? C4 C5 C6 C7 1.0(6) . . . . ? C4 C5 C6 C10 -176.2(4) . . . . ? C5 C6 C7 C8 -0.8(6) . . . . ? C10 C6 C7 C8 176.4(4) . . . . ? C6 C7 C8 C3 0.0(5) . . . . ? C6 C7 C8 C11 -176.9(4) . . . . ? C4 C3 C8 C7 0.7(5) . . . . ? C1 C3 C8 C7 -174.5(3) . . . . ? C4 C3 C8 C11 177.4(3) . . . . ? C1 C3 C8 C11 2.3(5) . . . . ? N2 C2 C12 C17 119.6(3) . . . . ? C1 C2 C12 C17 -65.2(4) . . . . ? N2 C2 C12 C13 -60.9(4) . . . . ? C1 C2 C12 C13 114.3(3) . . . . ? C17 C12 C13 C14 0.2(5) . . . . ? C2 C12 C13 C14 -179.4(3) . . . . ? C17 C12 C13 C18 179.1(3) . . . . ? C2 C12 C13 C18 -0.4(5) . . . . ? C12 C13 C14 C15 0.8(5) . . . . ? C18 C13 C14 C15 -178.2(3) . . . . ? C13 C14 C15 C16 -0.8(5) . . . . ? C13 C14 C15 C19 -178.6(4) . . . . ? C14 C15 C16 C17 -0.2(5) . . . . ? C19 C15 C16 C17 177.6(4) . . . . ? C15 C16 C17 C12 1.2(5) . . . . ? C15 C16 C17 C20 -177.2(3) . . . . ? C13 C12 C17 C16 -1.1(5) . . . . ? C2 C12 C17 C16 178.4(3) . . . . ? C13 C12 C17 C20 177.2(3) . . . . ? C2 C12 C17 C20 -3.3(5) . . . . ? O3 N3 C21 C22 178.9(2) . . . . ? Co1 N3 C21 C22 0.6(3) . . . . ? O3 N3 C21 C23 -1.8(4) . . . . ? Co1 N3 C21 C23 179.9(2) . . . . ? O4 N4 C22 C21 177.9(2) . . . . ? Co1 N4 C22 C21 -6.8(3) . . . . ? O4 N4 C22 C32 -5.2(4) . . . . ? Co1 N4 C22 C32 170.1(2) . . . . ? N3 C21 C22 N4 3.9(3) . . . . ? C23 C21 C22 N4 -175.4(2) . . . . ? N3 C21 C22 C32 -172.9(3) . . . . ? C23 C21 C22 C32 7.8(4) . . . . ? N3 C21 C23 C24 108.1(3) . . . . ? C22 C21 C23 C24 -72.7(4) . . . . ? N3 C21 C23 C28 -70.8(4) . . . . ? C22 C21 C23 C28 108.4(3) . . . . ? C28 C23 C24 C25 -2.1(4) . . . . ? C21 C23 C24 C25 179.1(3) . . . . ? C28 C23 C24 C29 175.1(3) . . . . ? C21 C23 C24 C29 -3.7(4) . . . . ? C23 C24 C25 C26 -1.1(4) . . . . ? C29 C24 C25 C26 -178.4(3) . . . . ? C24 C25 C26 C27 2.5(5) . . . . ? C24 C25 C26 C30 -179.7(3) . . . . ? C25 C26 C27 C28 -0.6(5) . . . . ? C30 C26 C27 C28 -178.4(3) . . . . ? C26 C27 C28 C23 -2.5(5) . . . . ? C26 C27 C28 C31 175.6(3) . . . . ? C24 C23 C28 C27 3.8(4) . . . . ? C21 C23 C28 C27 -177.3(3) . . . . ? C24 C23 C28 C31 -174.2(3) . . . . ? C21 C23 C28 C31 4.7(4) . . . . ? N4 C22 C32 C33 -66.2(4) . . . . ? C21 C22 C32 C33 110.3(3) . . . . ? N4 C22 C32 C37 114.6(3) . . . . ? C21 C22 C32 C37 -69.0(4) . . . . ? C37 C32 C33 C34 2.2(4) . . . . ? C22 C32 C33 C34 -177.1(3) . . . . ? C37 C32 C33 C38 -177.6(3) . . . . ? C22 C32 C33 C38 3.2(4) . . . . ? C32 C33 C34 C35 0.6(5) . . . . ? C38 C33 C34 C35 -179.7(3) . . . . ? C33 C34 C35 C36 -2.3(5) . . . . ? C33 C34 C35 C39 176.9(3) . . . . ? C34 C35 C36 C37 1.3(5) . . . . ? C39 C35 C36 C37 -177.9(3) . . . . ? C35 C36 C37 C32 1.3(5) . . . . ? C35 C36 C37 C40 -177.8(3) . . . . ? C33 C32 C37 C36 -3.1(4) . . . . ? C22 C32 C37 C36 176.1(3) . . . . ? C33 C32 C37 C40 176.0(3) . . . . ? C22 C32 C37 C40 -4.7(5) . . . . ? C45 N5 C41 C42 -1.1(5) . . . . ? Co1 N5 C41 C42 171.4(3) . . . . ? N5 C41 C42 C43 -0.4(5) . . . . ? C41 C42 C43 C44 1.2(6) . . . . ? C42 C43 C44 C45 -0.5(5) . . . . ? C41 N5 C45 C44 1.8(4) . . . . ? Co1 N5 C45 C44 -170.5(2) . . . . ? C43 C44 C45 N5 -1.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.797 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.078 #===END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-bis(dimesitylglyoximato)-chloro-(pyridine)-cobalt(III) ; _chemical_name_common 'Chloro cobalt(III) Mesitylglyoxime Pyridine' _chemical_melting_point ? _chemical_formula_moiety '(C47 H54 Cl1 Co1 N6 O4)2' _chemical_formula_sum 'C94 H108 Cl2 Co2 N12 O8' _chemical_formula_weight 1722.68 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 27.776(8) _cell_length_b 9.071(2) _cell_length_c 36.827(10) _cell_angle_alpha 90.000(0) _cell_angle_beta 108.043(6) _cell_angle_gamma 90.000(0) _cell_volume 8822(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min -28.0 _cell_measurement_theta_max +28.0 _exptl_crystal_description block _exptl_crystal_colour 'yellow orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8853 _exptl_absorpt_correction_T_max 0.9333 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; trans-bis(dimesitylglyoximato)-chloro-(pyridine)-cobalt(III) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method \f/\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.05 _diffrn_reflns_number 28547 _diffrn_reflns_av_R_equivalents 0.0981 _diffrn_reflns_av_sigmaI/netI 0.1346 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.30 _reflns_number_total 10846 _reflns_number_gt 5747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (BRUKER, 2003)' _computing_cell_refinement 'SMART 5.628 (BRUKER, 2003)' _computing_data_reduction 'SAINT+ 6.45 (BRUKER, 2003)' _computing_structure_solution 'SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0808P)^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 10846 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1634 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1683 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Co1 Co 0.74584(2) 0.36499(6) 0.130611(15) 0.02578(16) Uani 1 1 d . . . Cl1 Cl 0.77700(5) 0.14667(12) 0.12187(3) 0.0425(3) Uani 1 1 d . . . O1 O 0.81889(11) 0.5087(3) 0.10364(8) 0.0375(8) Uani 1 1 d . . . O2 O 0.75566(12) 0.2755(3) 0.20697(8) 0.0388(8) Uani 1 1 d . . . H1 H 0.7257 0.2171 0.1859 0.058 Uiso 1 1 d . . . O3 O 0.67275(12) 0.2287(3) 0.15829(8) 0.0385(8) Uani 1 1 d . . . O4 O 0.73985(11) 0.4312(3) 0.05426(8) 0.0368(7) Uani 1 1 d . . . H2 H 0.7815 0.4746 0.0748 0.055 Uiso 1 1 d . . . N1 N 0.80935(13) 0.4549(4) 0.13429(10) 0.0285(8) Uani 1 1 d . . . N2 N 0.77835(14) 0.3443(4) 0.18393(9) 0.0294(8) Uani 1 1 d . . . N3 N 0.68226(13) 0.2785(3) 0.12711(9) 0.0284(8) Uani 1 1 d . . . N4 N 0.71460(14) 0.3789(4) 0.07730(9) 0.0295(8) Uani 1 1 d . . . N5 N 0.72040(13) 0.5624(4) 0.13834(10) 0.0296(8) Uani 1 1 d . . . N6 N 0.6799(3) 0.7504(6) 0.01606(18) 0.089(2) Uani 1 1 d . . . C1 C 0.84160(16) 0.4714(4) 0.16849(11) 0.0269(9) Uani 1 1 d . . . C2 C 0.82305(16) 0.3995(4) 0.19789(12) 0.0277(9) Uani 1 1 d . . . C3 C 0.88920(17) 0.5572(5) 0.17687(11) 0.0311(10) Uani 1 1 d . . . C4 C 0.93678(17) 0.4886(5) 0.19054(12) 0.0363(11) Uani 1 1 d . . . C5 C 0.97953(18) 0.5771(6) 0.19976(13) 0.0479(13) Uani 1 1 d . . . H5 H 1.0110 0.5323 0.2094 0.057 Uiso 1 1 calc R . . C6 C 0.9778(2) 0.7292(6) 0.19532(14) 0.0475(13) Uani 1 1 d . . . C7 C 0.9305(2) 0.7920(6) 0.18045(13) 0.0472(13) Uani 1 1 d . . . H7 H 0.9285 0.8935 0.1767 0.057 Uiso 1 1 calc R . . C8 C 0.88592(18) 0.7115(5) 0.17076(12) 0.0365(11) Uani 1 1 d . . . C9 C 0.94291(19) 0.3251(5) 0.19533(14) 0.0484(13) Uani 1 1 d . . . H9A H 0.9102 0.2791 0.1879 0.073 Uiso 1 1 calc R . . H9B H 0.9605 0.3025 0.2216 0.073 Uiso 1 1 calc R . . H9C H 0.9621 0.2887 0.1795 0.073 Uiso 1 1 calc R . . C10 C 1.0253(2) 0.8208(7) 0.20720(16) 0.0722(18) Uani 1 1 d . . . H10A H 1.0542 0.7575 0.2169 0.108 Uiso 1 1 calc R . . H10B H 1.0238 0.8888 0.2268 0.108 Uiso 1 1 calc R . . H10C H 1.0284 0.8745 0.1856 0.108 Uiso 1 1 calc R . . C11 C 0.8364(2) 0.7898(5) 0.15506(15) 0.0504(13) Uani 1 1 d . . . H11A H 0.8092 0.7197 0.1501 0.076 Uiso 1 1 calc R . . H11B H 0.8355 0.8389 0.1317 0.076 Uiso 1 1 calc R . . H11C H 0.8328 0.8612 0.1733 0.076 Uiso 1 1 calc R . . C12 C 0.85305(16) 0.3863(4) 0.23891(12) 0.0294(10) Uani 1 1 d . . . C13 C 0.87352(18) 0.2490(5) 0.25389(12) 0.0366(11) Uani 1 1 d . . . C14 C 0.90309(18) 0.2428(5) 0.29180(12) 0.0391(11) Uani 1 1 d . . . H14 H 0.9176 0.1529 0.3015 0.047 Uiso 1 1 calc R . . C15 C 0.91212(18) 0.3626(6) 0.31583(13) 0.0419(12) Uani 1 1 d . . . C16 C 0.88956(17) 0.4960(5) 0.30090(13) 0.0378(11) Uani 1 1 d . . . H16 H 0.8941 0.5779 0.3168 0.045 Uiso 1 1 calc R . . C17 C 0.86068(16) 0.5094(5) 0.26313(12) 0.0317(10) Uani 1 1 d . . . C18 C 0.8621(2) 0.1094(5) 0.23046(13) 0.0500(14) Uani 1 1 d . . . H18A H 0.8410 0.1323 0.2051 0.075 Uiso 1 1 calc R . . H18B H 0.8447 0.0412 0.2420 0.075 Uiso 1 1 calc R . . H18C H 0.8931 0.0661 0.2294 0.075 Uiso 1 1 calc R . . C19 C 0.9441(2) 0.3554(6) 0.35694(14) 0.0639(16) Uani 1 1 d . . . H19A H 0.9453 0.4508 0.3684 0.096 Uiso 1 1 calc R . . H19B H 0.9778 0.3252 0.3585 0.096 Uiso 1 1 calc R . . H19C H 0.9298 0.2855 0.3702 0.096 Uiso 1 1 calc R . . C20 C 0.8360(2) 0.6558(5) 0.24881(14) 0.0478(13) Uani 1 1 d . . . H20A H 0.8174 0.6479 0.2222 0.072 Uiso 1 1 calc R . . H20B H 0.8616 0.7303 0.2524 0.072 Uiso 1 1 calc R . . H20C H 0.8133 0.6822 0.2628 0.072 Uiso 1 1 calc R . . C21 C 0.64821(16) 0.2768(4) 0.09352(12) 0.0286(10) Uani 1 1 d . . . C22 C 0.66823(17) 0.3328(4) 0.06346(12) 0.0293(10) Uani 1 1 d . . . C23 C 0.59425(17) 0.2320(4) 0.08745(12) 0.0312(10) Uani 1 1 d . . . C24 C 0.57201(18) 0.1113(5) 0.06409(12) 0.0356(11) Uani 1 1 d . . . C25 C 0.52154(19) 0.0783(6) 0.05935(14) 0.0460(13) Uani 1 1 d . . . H25 H 0.5067 -0.0005 0.0437 0.055 Uiso 1 1 calc R . . C26 C 0.49279(19) 0.1569(6) 0.07673(14) 0.0469(13) Uani 1 1 d . . . C27 C 0.51533(19) 0.2736(6) 0.09972(14) 0.0455(12) Uani 1 1 d . . . H27 H 0.4963 0.3272 0.1120 0.055 Uiso 1 1 calc R . . C28 C 0.56534(18) 0.3140(5) 0.10531(12) 0.0358(11) Uani 1 1 d . . . C29 C 0.6014(2) 0.0132(5) 0.04584(14) 0.0505(13) Uani 1 1 d . . . H29A H 0.6355 0.0490 0.0518 0.076 Uiso 1 1 calc R . . H29B H 0.5858 0.0132 0.0187 0.076 Uiso 1 1 calc R . . H29C H 0.6018 -0.0854 0.0554 0.076 Uiso 1 1 calc R . . C30 C 0.4384(2) 0.1159(7) 0.07191(19) 0.081(2) Uani 1 1 d . . . H30A H 0.4247 0.1826 0.0864 0.121 Uiso 1 1 calc R . . H30B H 0.4370 0.0170 0.0808 0.121 Uiso 1 1 calc R . . H30C H 0.4189 0.1221 0.0454 0.121 Uiso 1 1 calc R . . C31 C 0.58653(19) 0.4457(5) 0.12992(15) 0.0519(14) Uani 1 1 d . . . H31A H 0.5609 0.4870 0.1394 0.078 Uiso 1 1 calc R . . H31B H 0.5972 0.5183 0.1151 0.078 Uiso 1 1 calc R . . H31C H 0.6150 0.4157 0.1510 0.078 Uiso 1 1 calc R . . C32 C 0.64157(17) 0.3330(4) 0.02178(12) 0.0318(10) Uani 1 1 d . . . C33 C 0.65972(18) 0.2416(5) -0.00204(12) 0.0368(11) Uani 1 1 d . . . C34 C 0.6368(2) 0.2476(6) -0.04099(14) 0.0526(14) Uani 1 1 d . . . H34 H 0.6485 0.1868 -0.0568 0.063 Uiso 1 1 calc R . . C35 C 0.5967(2) 0.3424(7) -0.05720(14) 0.0604(16) Uani 1 1 d . . . C36 C 0.5792(2) 0.4300(6) -0.03380(15) 0.0568(15) Uani 1 1 d . . . H36 H 0.5518 0.4919 -0.0447 0.068 Uiso 1 1 calc R . . C37 C 0.60099(18) 0.4297(5) 0.00575(13) 0.0397(11) Uani 1 1 d . . . C38 C 0.7027(2) 0.1344(5) 0.01394(14) 0.0502(13) Uani 1 1 d . . . H38A H 0.7145 0.1423 0.0413 0.075 Uiso 1 1 calc R . . H38B H 0.7298 0.1569 0.0039 0.075 Uiso 1 1 calc R . . H38C H 0.6909 0.0358 0.0068 0.075 Uiso 1 1 calc R . . C39 C 0.5747(3) 0.3524(8) -0.10045(15) 0.100(3) Uani 1 1 d . . . H39A H 0.5916 0.2831 -0.1121 0.149 Uiso 1 1 calc R . . H39B H 0.5794 0.4503 -0.1086 0.149 Uiso 1 1 calc R . . H39C H 0.5392 0.3300 -0.1080 0.149 Uiso 1 1 calc R . . C40 C 0.5823(2) 0.5365(6) 0.02990(15) 0.0574(15) Uani 1 1 d . . . H40A H 0.6013 0.5230 0.0563 0.086 Uiso 1 1 calc R . . H40B H 0.5471 0.5187 0.0264 0.086 Uiso 1 1 calc R . . H40C H 0.5867 0.6356 0.0224 0.086 Uiso 1 1 calc R . . C41 C 0.71450(17) 0.6680(5) 0.11155(13) 0.0376(11) Uani 1 1 d . . . H41 H 0.7178 0.6429 0.0880 0.045 Uiso 1 1 calc R . . C42 C 0.70373(19) 0.8117(5) 0.11810(16) 0.0461(13) Uani 1 1 d . . . H42 H 0.7005 0.8827 0.0993 0.055 Uiso 1 1 calc R . . C43 C 0.6978(2) 0.8496(5) 0.15243(17) 0.0556(15) Uani 1 1 d . . . H43 H 0.6911 0.9467 0.1573 0.067 Uiso 1 1 calc R . . C44 C 0.70192(19) 0.7430(5) 0.17937(16) 0.0492(13) Uani 1 1 d . . . H44 H 0.6972 0.7659 0.2026 0.059 Uiso 1 1 calc R . . C45 C 0.71315(17) 0.6014(5) 0.17159(13) 0.0362(11) Uani 1 1 d . . . H45 H 0.7159 0.5292 0.1901 0.043 Uiso 1 1 calc R . . C46 C 0.6851(3) 0.7003(8) -0.0102(2) 0.076(2) Uani 1 1 d . . . C47 C 0.6904(3) 0.6366(9) -0.0454(2) 0.110(3) Uani 1 1 d . . . H47A H 0.6857 0.5318 -0.0452 0.164 Uiso 1 1 calc R . . H47B H 0.7236 0.6578 -0.0469 0.164 Uiso 1 1 calc R . . H47C H 0.6654 0.6786 -0.0670 0.164 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 0.0269(3) 0.0243(3) 0.0272(3) 0.0010(2) 0.0099(2) -0.0004(3) Cl1 0.0473(8) 0.0295(6) 0.0481(7) -0.0041(5) 0.0111(6) 0.0071(5) O1 0.0379(19) 0.0500(19) 0.0276(16) 0.0057(14) 0.0143(14) -0.0085(15) O2 0.042(2) 0.0429(18) 0.0322(16) 0.0067(14) 0.0128(15) -0.0094(15) O3 0.039(2) 0.0458(18) 0.0333(16) 0.0072(14) 0.0157(15) -0.0107(15) O4 0.0363(19) 0.0450(18) 0.0331(16) 0.0047(14) 0.0164(15) -0.0045(15) N1 0.026(2) 0.0284(18) 0.0320(19) 0.0008(16) 0.0103(17) -0.0011(15) N2 0.038(2) 0.0266(18) 0.0245(18) 0.0008(15) 0.0117(17) -0.0010(16) N3 0.030(2) 0.0258(18) 0.0290(19) 0.0023(15) 0.0089(16) -0.0038(16) N4 0.035(2) 0.0278(19) 0.0299(18) -0.0013(16) 0.0166(17) -0.0033(17) N5 0.025(2) 0.0277(18) 0.037(2) 0.0004(16) 0.0116(17) 0.0021(16) N6 0.125(6) 0.065(4) 0.081(4) 0.009(3) 0.038(4) -0.002(4) C1 0.028(2) 0.024(2) 0.030(2) -0.0005(18) 0.010(2) 0.0045(18) C2 0.029(2) 0.022(2) 0.032(2) -0.0008(18) 0.011(2) 0.0034(18) C3 0.029(3) 0.038(2) 0.027(2) -0.0004(19) 0.010(2) -0.003(2) C4 0.030(3) 0.050(3) 0.031(2) -0.001(2) 0.013(2) 0.002(2) C5 0.020(3) 0.081(4) 0.042(3) -0.004(3) 0.008(2) 0.002(3) C6 0.036(3) 0.066(4) 0.044(3) -0.011(3) 0.017(2) -0.018(3) C7 0.047(3) 0.051(3) 0.046(3) -0.002(2) 0.019(3) -0.019(3) C8 0.033(3) 0.043(3) 0.032(2) 0.000(2) 0.008(2) -0.006(2) C9 0.039(3) 0.056(3) 0.052(3) -0.001(3) 0.016(3) 0.008(2) C10 0.042(4) 0.107(5) 0.065(4) -0.009(4) 0.014(3) -0.034(3) C11 0.052(4) 0.033(3) 0.062(3) 0.004(2) 0.012(3) -0.006(2) C12 0.029(2) 0.032(2) 0.031(2) 0.0007(19) 0.0137(19) 0.0006(19) C13 0.039(3) 0.036(2) 0.035(2) 0.002(2) 0.010(2) 0.000(2) C14 0.042(3) 0.036(3) 0.038(3) 0.010(2) 0.010(2) 0.004(2) C15 0.035(3) 0.055(3) 0.037(3) 0.004(2) 0.013(2) -0.008(2) C16 0.036(3) 0.041(3) 0.038(3) -0.010(2) 0.016(2) -0.006(2) C17 0.025(2) 0.038(2) 0.033(2) 0.000(2) 0.011(2) 0.002(2) C18 0.071(4) 0.025(2) 0.048(3) 0.002(2) 0.008(3) 0.008(2) C19 0.063(4) 0.073(4) 0.042(3) 0.000(3) -0.004(3) 0.000(3) C20 0.057(4) 0.037(3) 0.049(3) -0.009(2) 0.017(3) 0.002(2) C21 0.032(3) 0.022(2) 0.034(2) -0.0043(18) 0.013(2) -0.0018(19) C22 0.033(3) 0.023(2) 0.032(2) -0.0034(18) 0.011(2) -0.0003(18) C23 0.037(3) 0.028(2) 0.029(2) 0.0036(19) 0.010(2) -0.002(2) C24 0.039(3) 0.034(3) 0.031(2) 0.001(2) 0.008(2) -0.002(2) C25 0.037(3) 0.047(3) 0.045(3) -0.003(2) 0.000(2) -0.013(2) C26 0.030(3) 0.058(3) 0.048(3) 0.009(3) 0.005(2) -0.006(3) C27 0.035(3) 0.053(3) 0.050(3) 0.001(3) 0.016(2) 0.003(2) C28 0.032(3) 0.036(2) 0.038(2) 0.002(2) 0.010(2) 0.001(2) C29 0.051(4) 0.040(3) 0.060(3) -0.013(3) 0.016(3) -0.007(3) C30 0.044(4) 0.095(5) 0.096(5) -0.004(4) 0.012(3) -0.020(4) C31 0.044(3) 0.052(3) 0.066(3) -0.019(3) 0.025(3) -0.003(3) C32 0.034(3) 0.029(2) 0.032(2) 0.0015(19) 0.009(2) -0.0053(19) C33 0.044(3) 0.037(3) 0.033(2) -0.006(2) 0.016(2) -0.009(2) C34 0.069(4) 0.056(3) 0.037(3) -0.013(3) 0.022(3) -0.017(3) C35 0.057(4) 0.077(4) 0.036(3) -0.006(3) -0.001(3) -0.017(3) C36 0.042(3) 0.073(4) 0.045(3) 0.004(3) -0.002(3) 0.002(3) C37 0.039(3) 0.037(3) 0.042(3) 0.006(2) 0.010(2) -0.005(2) C38 0.057(4) 0.046(3) 0.057(3) -0.006(3) 0.032(3) 0.003(3) C39 0.106(6) 0.138(7) 0.034(3) -0.002(4) -0.008(3) 0.000(5) C40 0.051(4) 0.059(3) 0.066(4) 0.004(3) 0.024(3) 0.017(3) C41 0.036(3) 0.034(3) 0.042(3) 0.009(2) 0.010(2) 0.004(2) C42 0.042(3) 0.030(2) 0.067(4) 0.010(2) 0.018(3) 0.009(2) C43 0.051(4) 0.034(3) 0.088(4) -0.009(3) 0.030(3) 0.010(3) C44 0.046(3) 0.045(3) 0.063(3) -0.015(3) 0.027(3) 0.007(2) C45 0.035(3) 0.036(3) 0.041(3) -0.001(2) 0.018(2) -0.001(2) C46 0.056(4) 0.075(5) 0.086(5) 0.026(4) 0.004(4) -0.015(4) C47 0.074(6) 0.139(7) 0.114(6) -0.043(6) 0.026(5) -0.008(5) _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 N4 1.889(3) . yes Co1 N2 1.899(3) . yes Co1 N3 1.900(3) . yes Co1 N1 1.910(3) . yes Co1 N5 1.978(3) . yes Co1 Cl1 2.2243(15) . yes O1 N1 1.329(4) . ? O2 N2 1.356(4) . ? O3 N3 1.335(4) . ? O4 N4 1.344(4) . ? N1 C1 1.308(5) . yes N2 C2 1.289(5) . yes N3 C21 1.304(5) . yes N4 C22 1.299(5) . yes N5 C41 1.348(5) . ? N5 C45 1.348(5) . ? N6 C46 1.119(8) . ? C1 C3 1.482(6) . ? C1 C2 1.486(6) . yes C2 C12 1.487(6) . ? C3 C4 1.406(6) . ? C3 C8 1.416(6) . ? C4 C5 1.386(6) . ? C4 C9 1.497(7) . ? C5 C6 1.388(7) . ? C6 C7 1.381(7) . ? C6 C10 1.505(7) . ? C7 C8 1.387(6) . ? C8 C11 1.496(6) . ? C12 C17 1.404(6) . ? C12 C13 1.409(6) . ? C13 C14 1.385(6) . ? C13 C18 1.509(6) . ? C14 C15 1.375(6) . ? C15 C16 1.395(6) . ? C15 C19 1.501(6) . ? C16 C17 1.379(6) . ? C17 C20 1.513(6) . ? C21 C22 1.474(6) . yes C21 C23 1.502(6) . ? C22 C32 1.483(6) . ? C23 C28 1.399(6) . ? C23 C24 1.411(6) . ? C24 C25 1.391(6) . ? C24 C29 1.500(6) . ? C25 C26 1.368(7) . ? C26 C27 1.379(7) . ? C26 C30 1.512(7) . ? C27 C28 1.389(6) . ? C28 C31 1.504(6) . ? C32 C37 1.406(6) . ? C32 C33 1.409(6) . ? C33 C34 1.378(6) . ? C33 C38 1.510(6) . ? C34 C35 1.387(8) . ? C35 C36 1.367(8) . ? C35 C39 1.522(7) . ? C36 C37 1.394(6) . ? C37 C40 1.511(7) . ? C41 C42 1.375(6) . ? C42 C43 1.368(7) . ? C43 C44 1.365(7) . ? C44 C45 1.373(6) . ? C46 C47 1.466(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 N4 Co1 N2 177.88(15) . . ? N4 Co1 N3 80.73(15) . . yes N2 Co1 N3 99.43(15) . . yes N4 Co1 N1 99.32(15) . . yes N2 Co1 N1 80.55(15) . . yes N3 Co1 N1 179.07(15) . . ? N4 Co1 N5 91.13(14) . . ? N2 Co1 N5 90.99(14) . . ? N3 Co1 N5 91.01(14) . . ? N1 Co1 N5 88.07(14) . . ? N4 Co1 Cl1 89.03(11) . . ? N2 Co1 Cl1 88.85(11) . . ? N3 Co1 Cl1 91.02(11) . . ? N1 Co1 Cl1 89.90(11) . . ? N5 Co1 Cl1 177.96(11) . . yes C1 N1 O1 121.2(3) . . ? C1 N1 Co1 117.3(3) . . ? O1 N1 Co1 121.3(3) . . ? C2 N2 O2 120.4(3) . . ? C2 N2 Co1 117.7(3) . . ? O2 N2 Co1 121.9(3) . . ? C21 N3 O3 122.2(3) . . ? C21 N3 Co1 117.1(3) . . ? O3 N3 Co1 120.6(3) . . ? C22 N4 O4 120.9(3) . . ? C22 N4 Co1 117.8(3) . . ? O4 N4 Co1 121.2(3) . . ? C41 N5 C45 117.4(4) . . ? C41 N5 Co1 120.4(3) . . ? C45 N5 Co1 121.9(3) . . ? N1 C1 C3 124.1(4) . . ? N1 C1 C2 111.3(4) . . ? C3 C1 C2 124.5(4) . . ? N2 C2 C1 112.8(4) . . ? N2 C2 C12 122.8(4) . . ? C1 C2 C12 124.3(4) . . ? C4 C3 C8 120.1(4) . . ? C4 C3 C1 121.4(4) . . ? C8 C3 C1 118.5(4) . . ? C5 C4 C3 118.1(4) . . ? C5 C4 C9 119.2(4) . . ? C3 C4 C9 122.8(4) . . ? C4 C5 C6 123.5(5) . . ? C7 C6 C5 116.8(5) . . ? C7 C6 C10 121.9(5) . . ? C5 C6 C10 121.3(5) . . ? C6 C7 C8 123.3(5) . . ? C7 C8 C3 118.1(5) . . ? C7 C8 C11 119.4(4) . . ? C3 C8 C11 122.5(4) . . ? C17 C12 C13 119.4(4) . . ? C17 C12 C2 120.5(4) . . ? C13 C12 C2 120.0(4) . . ? C14 C13 C12 118.2(4) . . ? C14 C13 C18 119.8(4) . . ? C12 C13 C18 122.0(4) . . ? C15 C14 C13 123.4(4) . . ? C14 C15 C16 117.5(4) . . ? C14 C15 C19 123.2(5) . . ? C16 C15 C19 119.3(4) . . ? C17 C16 C15 121.6(4) . . ? C16 C17 C12 119.8(4) . . ? C16 C17 C20 119.2(4) . . ? C12 C17 C20 120.9(4) . . ? N3 C21 C22 112.1(4) . . ? N3 C21 C23 122.8(4) . . ? C22 C21 C23 125.0(4) . . ? N4 C22 C21 112.0(4) . . ? N4 C22 C32 121.5(4) . . ? C21 C22 C32 126.4(4) . . ? C28 C23 C24 119.5(4) . . ? C28 C23 C21 118.5(4) . . ? C24 C23 C21 121.9(4) . . ? C25 C24 C23 118.5(4) . . ? C25 C24 C29 118.9(4) . . ? C23 C24 C29 122.5(4) . . ? C26 C25 C24 122.7(5) . . ? C25 C26 C27 117.9(5) . . ? C25 C26 C30 121.6(5) . . ? C27 C26 C30 120.5(5) . . ? C26 C27 C28 122.5(5) . . ? C27 C28 C23 118.9(4) . . ? C27 C28 C31 119.0(4) . . ? C23 C28 C31 122.1(4) . . ? C37 C32 C33 120.0(4) . . ? C37 C32 C22 120.9(4) . . ? C33 C32 C22 118.9(4) . . ? C34 C33 C32 119.1(5) . . ? C34 C33 C38 119.0(4) . . ? C32 C33 C38 121.9(4) . . ? C33 C34 C35 121.5(5) . . ? C36 C35 C34 118.9(5) . . ? C36 C35 C39 121.2(6) . . ? C34 C35 C39 119.8(6) . . ? C35 C36 C37 122.3(5) . . ? C36 C37 C32 118.2(5) . . ? C36 C37 C40 119.8(5) . . ? C32 C37 C40 122.0(4) . . ? N5 C41 C42 121.9(4) . . ? C43 C42 C41 119.7(5) . . ? C44 C43 C42 119.1(5) . . ? C43 C44 C45 119.0(5) . . ? N5 C45 C44 122.8(4) . . ? N6 C46 C47 178.1(8) . . ? 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 N4 Co1 N1 C1 177.1(3) . . . . ? N2 Co1 N1 C1 -5.1(3) . . . . ? N3 Co1 N1 C1 84(10) . . . . ? N5 Co1 N1 C1 86.3(3) . . . . ? Cl1 Co1 N1 C1 -93.9(3) . . . . ? N4 Co1 N1 O1 2.1(3) . . . . ? N2 Co1 N1 O1 179.9(3) . . . . ? N3 Co1 N1 O1 -91(9) . . . . ? N5 Co1 N1 O1 -88.8(3) . . . . ? Cl1 Co1 N1 O1 91.1(3) . . . . ? N4 Co1 N2 C2 89(4) . . . . ? N3 Co1 N2 C2 -176.4(3) . . . . ? N1 Co1 N2 C2 2.7(3) . . . . ? N5 Co1 N2 C2 -85.2(3) . . . . ? Cl1 Co1 N2 C2 92.8(3) . . . . ? N4 Co1 N2 O2 -91(4) . . . . ? N3 Co1 N2 O2 3.0(3) . . . . ? N1 Co1 N2 O2 -177.9(3) . . . . ? N5 Co1 N2 O2 94.2(3) . . . . ? Cl1 Co1 N2 O2 -87.9(3) . . . . ? N4 Co1 N3 C21 -4.0(3) . . . . ? N2 Co1 N3 C21 178.1(3) . . . . ? N1 Co1 N3 C21 89(9) . . . . ? N5 Co1 N3 C21 87.0(3) . . . . ? Cl1 Co1 N3 C21 -92.9(3) . . . . ? N4 Co1 N3 O3 179.1(3) . . . . ? N2 Co1 N3 O3 1.2(3) . . . . ? N1 Co1 N3 O3 -88(9) . . . . ? N5 Co1 N3 O3 -90.0(3) . . . . ? Cl1 Co1 N3 O3 90.2(3) . . . . ? N2 Co1 N4 C22 96(4) . . . . ? N3 Co1 N4 C22 1.9(3) . . . . ? N1 Co1 N4 C22 -177.2(3) . . . . ? N5 Co1 N4 C22 -88.9(3) . . . . ? Cl1 Co1 N4 C22 93.1(3) . . . . ? N2 Co1 N4 O4 -82(4) . . . . ? N3 Co1 N4 O4 -176.4(3) . . . . ? N1 Co1 N4 O4 4.5(3) . . . . ? N5 Co1 N4 O4 92.7(3) . . . . ? Cl1 Co1 N4 O4 -85.2(3) . . . . ? N4 Co1 N5 C41 -32.1(3) . . . . ? N2 Co1 N5 C41 147.7(3) . . . . ? N3 Co1 N5 C41 -112.8(3) . . . . ? N1 Co1 N5 C41 67.2(3) . . . . ? Cl1 Co1 N5 C41 62(3) . . . . ? N4 Co1 N5 C45 154.6(3) . . . . ? N2 Co1 N5 C45 -25.6(3) . . . . ? N3 Co1 N5 C45 73.8(3) . . . . ? N1 Co1 N5 C45 -106.2(3) . . . . ? Cl1 Co1 N5 C45 -111(3) . . . . ? O1 N1 C1 C3 4.0(6) . . . . ? Co1 N1 C1 C3 -171.0(3) . . . . ? O1 N1 C1 C2 -178.9(3) . . . . ? Co1 N1 C1 C2 6.1(4) . . . . ? O2 N2 C2 C1 -179.6(3) . . . . ? Co1 N2 C2 C1 -0.2(4) . . . . ? O2 N2 C2 C12 2.7(6) . . . . ? Co1 N2 C2 C12 -178.0(3) . . . . ? N1 C1 C2 N2 -3.8(5) . . . . ? C3 C1 C2 N2 173.3(4) . . . . ? N1 C1 C2 C12 173.9(4) . . . . ? C3 C1 C2 C12 -8.9(6) . . . . ? N1 C1 C3 C4 -114.1(5) . . . . ? C2 C1 C3 C4 69.1(5) . . . . ? N1 C1 C3 C8 65.8(6) . . . . ? C2 C1 C3 C8 -111.0(5) . . . . ? C8 C3 C4 C5 3.6(6) . . . . ? C1 C3 C4 C5 -176.4(4) . . . . ? C8 C3 C4 C9 -176.2(4) . . . . ? C1 C3 C4 C9 3.8(6) . . . . ? C3 C4 C5 C6 -1.7(7) . . . . ? C9 C4 C5 C6 178.1(4) . . . . ? C4 C5 C6 C7 -0.8(7) . . . . ? C4 C5 C6 C10 177.6(4) . . . . ? C5 C6 C7 C8 1.2(7) . . . . ? C10 C6 C7 C8 -177.1(4) . . . . ? C6 C7 C8 C3 0.7(7) . . . . ? C6 C7 C8 C11 179.6(5) . . . . ? C4 C3 C8 C7 -3.2(6) . . . . ? C1 C3 C8 C7 176.9(4) . . . . ? C4 C3 C8 C11 177.9(4) . . . . ? C1 C3 C8 C11 -2.0(6) . . . . ? N2 C2 C12 C17 -108.1(5) . . . . ? C1 C2 C12 C17 74.4(5) . . . . ? N2 C2 C12 C13 71.1(6) . . . . ? C1 C2 C12 C13 -106.4(5) . . . . ? C17 C12 C13 C14 -3.7(6) . . . . ? C2 C12 C13 C14 177.2(4) . . . . ? C17 C12 C13 C18 173.3(4) . . . . ? C2 C12 C13 C18 -5.8(7) . . . . ? C12 C13 C14 C15 2.2(7) . . . . ? C18 C13 C14 C15 -174.9(5) . . . . ? C13 C14 C15 C16 0.8(7) . . . . ? C13 C14 C15 C19 179.9(5) . . . . ? C14 C15 C16 C17 -2.3(7) . . . . ? C19 C15 C16 C17 178.6(5) . . . . ? C15 C16 C17 C12 0.7(7) . . . . ? C15 C16 C17 C20 178.4(4) . . . . ? C13 C12 C17 C16 2.3(6) . . . . ? C2 C12 C17 C16 -178.5(4) . . . . ? C13 C12 C17 C20 -175.3(4) . . . . ? C2 C12 C17 C20 3.8(6) . . . . ? O3 N3 C21 C22 -178.0(3) . . . . ? Co1 N3 C21 C22 5.1(4) . . . . ? O3 N3 C21 C23 5.8(6) . . . . ? Co1 N3 C21 C23 -171.1(3) . . . . ? O4 N4 C22 C21 178.6(3) . . . . ? Co1 N4 C22 C21 0.2(4) . . . . ? O4 N4 C22 C32 1.3(6) . . . . ? Co1 N4 C22 C32 -177.1(3) . . . . ? N3 C21 C22 N4 -3.4(5) . . . . ? C23 C21 C22 N4 172.7(4) . . . . ? N3 C21 C22 C32 173.7(4) . . . . ? C23 C21 C22 C32 -10.2(6) . . . . ? N3 C21 C23 C28 61.0(6) . . . . ? C22 C21 C23 C28 -114.7(5) . . . . ? N3 C21 C23 C24 -119.7(5) . . . . ? C22 C21 C23 C24 64.6(6) . . . . ? C28 C23 C24 C25 0.4(6) . . . . ? C21 C23 C24 C25 -178.9(4) . . . . ? C28 C23 C24 C29 -176.5(4) . . . . ? C21 C23 C24 C29 4.3(6) . . . . ? C23 C24 C25 C26 -0.7(7) . . . . ? C29 C24 C25 C26 176.3(5) . . . . ? C24 C25 C26 C27 0.1(8) . . . . ? C24 C25 C26 C30 -178.3(5) . . . . ? C25 C26 C27 C28 0.8(7) . . . . ? C30 C26 C27 C28 179.3(5) . . . . ? C26 C27 C28 C23 -1.1(7) . . . . ? C26 C27 C28 C31 178.2(5) . . . . ? C24 C23 C28 C27 0.5(6) . . . . ? C21 C23 C28 C27 179.8(4) . . . . ? C24 C23 C28 C31 -178.8(4) . . . . ? C21 C23 C28 C31 0.5(6) . . . . ? N4 C22 C32 C37 -111.2(5) . . . . ? C21 C22 C32 C37 71.9(6) . . . . ? N4 C22 C32 C33 64.5(5) . . . . ? C21 C22 C32 C33 -112.4(5) . . . . ? C37 C32 C33 C34 -0.7(7) . . . . ? C22 C32 C33 C34 -176.4(4) . . . . ? C37 C32 C33 C38 -179.0(4) . . . . ? C22 C32 C33 C38 5.2(6) . . . . ? C32 C33 C34 C35 0.6(7) . . . . ? C38 C33 C34 C35 179.0(5) . . . . ? C33 C34 C35 C36 -1.0(8) . . . . ? C33 C34 C35 C39 176.2(5) . . . . ? C34 C35 C36 C37 1.4(9) . . . . ? C39 C35 C36 C37 -175.7(5) . . . . ? C35 C36 C37 C32 -1.5(8) . . . . ? C35 C36 C37 C40 175.8(5) . . . . ? C33 C32 C37 C36 1.1(7) . . . . ? C22 C32 C37 C36 176.7(4) . . . . ? C33 C32 C37 C40 -176.1(4) . . . . ? C22 C32 C37 C40 -0.5(7) . . . . ? C45 N5 C41 C42 2.8(6) . . . . ? Co1 N5 C41 C42 -170.8(4) . . . . ? N5 C41 C42 C43 -1.2(7) . . . . ? C41 C42 C43 C44 -1.1(8) . . . . ? C42 C43 C44 C45 1.6(8) . . . . ? C41 N5 C45 C44 -2.3(6) . . . . ? Co1 N5 C45 C44 171.3(4) . . . . ? C43 C44 C45 N5 0.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.512 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.081 #===END data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-bis(dimesitylglyoximato)-bromo-(pyridine)-cobalt(III) ; _chemical_name_common 'Bromo cobalt(III) Mesitylglyoxime Pyridine' _chemical_melting_point ? _chemical_formula_moiety '(C46 H53 Br1 Cl2 Co1 N5 O4)2' _chemical_formula_sum 'C92 H106 Br2 Cl4 Co2 N10 O8' _chemical_formula_weight 1899.35 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 27.579(17) _cell_length_b 9.116(5) _cell_length_c 36.610(2) _cell_angle_alpha 90.000(0) _cell_angle_beta 108.493(2) _cell_angle_gamma 90.000(0) _cell_volume 8729(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min -28.0 _cell_measurement_theta_max +28.0 _exptl_crystal_description block _exptl_crystal_colour 'yellow orange' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 1.481 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6995 _exptl_absorpt_correction_T_max 0.8084 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; trans-bis(dimesitylglyoximato)-chloro-(pyridine)-cobalt(III) ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method \f/\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.05 _diffrn_reflns_number 28518 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.32 _reflns_number_total 10790 _reflns_number_gt 8180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (BRUKER, 2003)' _computing_cell_refinement 'SMART 5.628 (BRUKER, 2003)' _computing_data_reduction 'SAINT+ 6.45 (BRUKER, 2003)' _computing_structure_solution 'SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1304P)^2^+54.4573P] 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 10790 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2268 _refine_ls_wR_factor_gt 0.2119 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Co1 Co 0.24553(2) 0.15486(6) 0.632041(15) 0.00781(15) Uani 1 1 d . . . Br1 Br 0.27846(2) 0.38127(6) 0.621148(16) 0.02766(16) Uani 1 1 d . . . Cl1 Cl 0.17106(6) -0.23647(15) 0.51454(4) 0.0337(3) Uani 1 1 d . . . Cl2 Cl 0.18799(7) -0.1970(2) 0.44106(5) 0.0481(4) Uani 1 1 d . . . O1 O 0.25659(11) 0.2489(3) 0.70881(9) 0.0139(6) Uani 1 1 d . . . H1 H 0.2338 0.2754 0.6964 0.021 Uiso 1 1 d . . . O2 O 0.32011(11) 0.0115(3) 0.60576(8) 0.0124(6) Uani 1 1 d . . . H2 H 0.2991 0.0375 0.5870 0.019 Uiso 1 1 d . . . O3 O 0.23881(11) 0.0803(3) 0.55607(8) 0.0125(6) Uani 1 1 d . . . O4 O 0.17278(11) 0.2952(3) 0.65937(8) 0.0129(6) Uani 1 1 d . . . N1 N 0.27874(13) 0.1799(4) 0.68595(10) 0.0100(7) Uani 1 1 d . . . N2 N 0.30980(13) 0.0666(4) 0.63626(10) 0.0097(7) Uani 1 1 d . . . N3 N 0.21366(13) 0.1367(4) 0.57839(10) 0.0100(7) Uani 1 1 d . . . N4 N 0.18175(13) 0.2411(4) 0.62827(10) 0.0107(7) Uani 1 1 d . . . N5 N 0.21993(12) -0.0414(4) 0.64081(10) 0.0087(6) Uani 1 1 d . . . C1 C 0.32434(15) 0.1257(4) 0.70027(12) 0.0101(8) Uani 1 1 d . . . C2 C 0.34229(15) 0.0532(4) 0.67060(12) 0.0101(8) Uani 1 1 d . . . C3 C 0.39044(15) -0.0319(5) 0.67895(12) 0.0112(8) Uani 1 1 d . . . C4 C 0.43839(15) 0.0375(5) 0.69197(12) 0.0132(8) Uani 1 1 d . . . C5 C 0.48248(16) -0.0475(6) 0.70083(13) 0.0181(9) Uani 1 1 d . . . H5 H 0.5149 -0.0009 0.7100 0.022 Uiso 1 1 calc R . . C6 C 0.48012(17) -0.2004(5) 0.69659(13) 0.0184(9) Uani 1 1 d . . . C7 C 0.43285(18) -0.2650(5) 0.68279(13) 0.0182(9) Uani 1 1 d . . . H7 H 0.4310 -0.3684 0.6794 0.022 Uiso 1 1 calc R . . C8 C 0.38772(16) -0.1855(5) 0.67355(12) 0.0137(8) Uani 1 1 d . . . C9 C 0.44418(17) 0.2018(5) 0.69637(14) 0.0176(9) Uani 1 1 d . . . H9A H 0.4137 0.2497 0.6790 0.026 Uiso 1 1 calc R . . H9B H 0.4744 0.2332 0.6899 0.026 Uiso 1 1 calc R . . H9C H 0.4481 0.2292 0.7230 0.026 Uiso 1 1 calc R . . C10 C 0.52849(19) -0.2910(7) 0.70794(16) 0.0289(12) Uani 1 1 d . . . H10A H 0.5500 -0.2611 0.6925 0.043 Uiso 1 1 calc R . . H10B H 0.5197 -0.3951 0.7034 0.043 Uiso 1 1 calc R . . H10C H 0.5471 -0.2756 0.7353 0.043 Uiso 1 1 calc R . . C11 C 0.33725(17) -0.2641(5) 0.65873(14) 0.0180(9) Uani 1 1 d . . . H11A H 0.3153 -0.2347 0.6739 0.027 Uiso 1 1 calc R . . H11B H 0.3430 -0.3702 0.6610 0.027 Uiso 1 1 calc R . . H11C H 0.3206 -0.2383 0.6316 0.027 Uiso 1 1 calc R . . C12 C 0.35508(15) 0.1406(5) 0.74132(12) 0.0125(8) Uani 1 1 d . . . C13 C 0.36296(15) 0.0191(5) 0.76628(13) 0.0128(8) Uani 1 1 d . . . C14 C 0.39242(16) 0.0354(5) 0.80427(13) 0.0140(8) Uani 1 1 d . . . H14 H 0.3972 -0.0463 0.8211 0.017 Uiso 1 1 calc R . . C15 C 0.41535(16) 0.1685(5) 0.81853(13) 0.0159(9) Uani 1 1 d . . . C16 C 0.40654(16) 0.2882(5) 0.79401(13) 0.0146(8) Uani 1 1 d . . . H16 H 0.4219 0.3796 0.8035 0.017 Uiso 1 1 calc R . . C17 C 0.37553(16) 0.2778(5) 0.75550(12) 0.0133(8) Uani 1 1 d . . . C18 C 0.33884(18) -0.1274(5) 0.75262(14) 0.0175(9) Uani 1 1 d . . . H18A H 0.3035 -0.1128 0.7360 0.026 Uiso 1 1 calc R . . H18B H 0.3389 -0.1873 0.7749 0.026 Uiso 1 1 calc R . . H18C H 0.3583 -0.1776 0.7381 0.026 Uiso 1 1 calc R . . C19 C 0.4478(2) 0.1808(6) 0.86008(14) 0.0244(10) Uani 1 1 d . . . H19A H 0.4730 0.1011 0.8664 0.037 Uiso 1 1 calc R . . H19B H 0.4260 0.1740 0.8766 0.037 Uiso 1 1 calc R . . H19C H 0.4656 0.2754 0.8643 0.037 Uiso 1 1 calc R . . C20 C 0.36409(18) 0.4157(5) 0.73125(13) 0.0185(9) Uani 1 1 d . . . H20A H 0.3567 0.3898 0.7040 0.028 Uiso 1 1 calc R . . H20B H 0.3938 0.4812 0.7392 0.028 Uiso 1 1 calc R . . H20C H 0.3344 0.4655 0.7348 0.028 Uiso 1 1 calc R . . C21 C 0.16647(15) 0.1827(4) 0.56428(12) 0.0106(8) Uani 1 1 d . . . C22 C 0.14684(16) 0.2411(4) 0.59438(12) 0.0113(8) Uani 1 1 d . . . C23 C 0.13918(16) 0.1742(5) 0.52228(12) 0.0126(8) Uani 1 1 d . . . C24 C 0.09859(16) 0.0754(5) 0.50742(13) 0.0162(9) Uani 1 1 d . . . C25 C 0.07809(18) 0.0594(6) 0.46756(13) 0.0220(10) Uani 1 1 d . . . H25 H 0.0504 -0.0064 0.4574 0.026 Uiso 1 1 calc R . . C26 C 0.09684(19) 0.1364(6) 0.44233(14) 0.0241(10) Uani 1 1 d . . . C27 C 0.13676(18) 0.2356(5) 0.45779(14) 0.0202(10) Uani 1 1 d . . . H27 H 0.1497 0.2903 0.4408 0.024 Uiso 1 1 calc R . . C28 C 0.15791(16) 0.2564(5) 0.49692(13) 0.0143(8) Uani 1 1 d . . . C29 C 0.07782(18) -0.0178(6) 0.53316(14) 0.0217(10) Uani 1 1 d . . . H29A H 0.1063 -0.0580 0.5542 0.033 Uiso 1 1 calc R . . H29B H 0.0575 -0.0983 0.5181 0.033 Uiso 1 1 calc R . . H29C H 0.0562 0.0426 0.5439 0.033 Uiso 1 1 calc R . . C30 C 0.0775(2) 0.1107(8) 0.39953(15) 0.0377(14) Uani 1 1 d . . . H30A H 0.0701 0.2051 0.3861 0.057 Uiso 1 1 calc R . . H30B H 0.0462 0.0516 0.3930 0.057 Uiso 1 1 calc R . . H30C H 0.1036 0.0586 0.3916 0.057 Uiso 1 1 calc R . . C31 C 0.20036(18) 0.3670(5) 0.51102(15) 0.0195(9) Uani 1 1 d . . . H31A H 0.2155 0.3586 0.5390 0.029 Uiso 1 1 calc R . . H31B H 0.1866 0.4661 0.5044 0.029 Uiso 1 1 calc R . . H31C H 0.2266 0.3483 0.4988 0.029 Uiso 1 1 calc R . . C32 C 0.09337(16) 0.2894(4) 0.58766(12) 0.0106(8) Uani 1 1 d . . . C33 C 0.06349(16) 0.2121(5) 0.60663(12) 0.0130(8) Uani 1 1 d . . . C34 C 0.01348(16) 0.2565(5) 0.60097(13) 0.0149(8) Uani 1 1 d . . . H34 H -0.0064 0.2049 0.6138 0.018 Uiso 1 1 calc R . . C35 C -0.00868(17) 0.3742(5) 0.57717(14) 0.0180(9) Uani 1 1 d . . . C36 C 0.02121(17) 0.4472(5) 0.55863(13) 0.0161(9) Uani 1 1 d . . . H36 H 0.0065 0.5260 0.5418 0.019 Uiso 1 1 calc R . . C37 C 0.07169(16) 0.4092(5) 0.56384(12) 0.0126(8) Uani 1 1 d . . . C38 C 0.08423(17) 0.0827(5) 0.63214(14) 0.0174(9) Uani 1 1 d . . . H38A H 0.1014 0.0162 0.6192 0.026 Uiso 1 1 calc R . . H38B H 0.0561 0.0309 0.6375 0.026 Uiso 1 1 calc R . . H38C H 0.1087 0.1166 0.6564 0.026 Uiso 1 1 calc R . . C39 C -0.06263(18) 0.4211(7) 0.57218(17) 0.0293(12) Uani 1 1 d . . . H39A H -0.0661 0.5266 0.5668 0.044 Uiso 1 1 calc R . . H39B H -0.0708 0.4000 0.5958 0.044 Uiso 1 1 calc R . . H39C H -0.0862 0.3672 0.5506 0.044 Uiso 1 1 calc R . . C40 C 0.10209(17) 0.4991(5) 0.54447(14) 0.0186(9) Uani 1 1 d . . . H40A H 0.1386 0.4814 0.5571 0.028 Uiso 1 1 calc R . . H40B H 0.0946 0.6034 0.5464 0.028 Uiso 1 1 calc R . . H40C H 0.0928 0.4712 0.5173 0.028 Uiso 1 1 calc R . . C41 C 0.21276(15) -0.0766(5) 0.67424(13) 0.0145(8) Uani 1 1 d . . . H41 H 0.2150 -0.0015 0.6927 0.017 Uiso 1 1 calc R . . C42 C 0.20212(17) -0.2188(5) 0.68288(14) 0.0183(9) Uani 1 1 d . . . H42 H 0.1977 -0.2406 0.7070 0.022 Uiso 1 1 calc R . . C43 C 0.19808(17) -0.3288(5) 0.65584(15) 0.0199(9) Uani 1 1 d . . . H43 H 0.1912 -0.4272 0.6612 0.024 Uiso 1 1 calc R . . C44 C 0.20437(17) -0.2917(5) 0.62092(14) 0.0181(9) Uani 1 1 d . . . H44 H 0.2012 -0.3642 0.6017 0.022 Uiso 1 1 calc R . . C45 C 0.21531(16) -0.1478(5) 0.61439(13) 0.0139(8) Uani 1 1 d . . . H45 H 0.2197 -0.1232 0.5904 0.017 Uiso 1 1 calc R . . C46 C 0.1983(2) -0.1252(6) 0.48756(16) 0.0282(11) Uani 1 1 d . . . H46A H 0.2355 -0.1167 0.5009 0.034 Uiso 1 1 calc R . . H46B H 0.1833 -0.0256 0.4855 0.034 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 0.0075(3) 0.0082(3) 0.0082(3) -0.00005(19) 0.0032(2) 0.00012(18) Br1 0.0292(3) 0.0217(3) 0.0308(3) 0.0007(2) 0.0078(2) -0.00143(19) Cl1 0.0405(8) 0.0294(7) 0.0333(7) 0.0017(6) 0.0150(6) -0.0030(5) Cl2 0.0529(10) 0.0638(11) 0.0307(8) -0.0119(7) 0.0178(7) -0.0041(8) O1 0.0123(14) 0.0187(15) 0.0112(15) -0.0023(12) 0.0046(12) 0.0056(11) O2 0.0104(13) 0.0196(15) 0.0075(14) -0.0014(11) 0.0032(11) 0.0039(11) O3 0.0105(14) 0.0182(15) 0.0106(14) -0.0009(12) 0.0059(11) 0.0031(11) O4 0.0148(14) 0.0168(15) 0.0088(14) -0.0033(11) 0.0061(11) 0.0037(11) N1 0.0124(16) 0.0077(15) 0.0114(16) -0.0027(13) 0.0059(13) -0.0015(12) N2 0.0094(15) 0.0105(16) 0.0114(17) -0.0014(13) 0.0065(13) -0.0020(12) N3 0.0116(16) 0.0100(16) 0.0101(17) 0.0013(13) 0.0058(13) -0.0006(12) N4 0.0147(17) 0.0104(16) 0.0087(16) 0.0002(13) 0.0059(13) 0.0014(13) N5 0.0076(15) 0.0079(15) 0.0089(16) 0.0026(12) 0.0002(12) 0.0024(11) C1 0.0115(18) 0.0079(18) 0.012(2) -0.0003(14) 0.0049(15) -0.0003(14) C2 0.0121(18) 0.0092(18) 0.0109(19) -0.0020(15) 0.0061(15) -0.0021(14) C3 0.0074(18) 0.016(2) 0.0091(19) 0.0002(15) 0.0015(14) 0.0014(15) C4 0.0106(19) 0.020(2) 0.0086(19) 0.0000(16) 0.0028(15) -0.0018(16) C5 0.0091(19) 0.031(3) 0.015(2) 0.0033(19) 0.0047(16) 0.0015(17) C6 0.015(2) 0.027(2) 0.013(2) 0.0032(18) 0.0061(17) 0.0076(18) C7 0.022(2) 0.021(2) 0.013(2) 0.0018(17) 0.0077(18) 0.0075(18) C8 0.014(2) 0.017(2) 0.011(2) 0.0005(16) 0.0039(16) 0.0020(16) C9 0.014(2) 0.021(2) 0.019(2) 0.0004(18) 0.0071(17) -0.0033(16) C10 0.018(2) 0.040(3) 0.029(3) 0.008(2) 0.009(2) 0.014(2) C11 0.021(2) 0.011(2) 0.020(2) -0.0038(17) 0.0033(18) 0.0016(16) C12 0.0088(18) 0.016(2) 0.013(2) -0.0009(16) 0.0045(15) -0.0007(15) C13 0.0087(18) 0.015(2) 0.017(2) 0.0010(16) 0.0070(16) 0.0023(15) C14 0.0123(19) 0.017(2) 0.015(2) 0.0046(16) 0.0071(16) 0.0060(15) C15 0.0124(19) 0.020(2) 0.014(2) 0.0010(17) 0.0036(16) 0.0025(16) C16 0.0131(19) 0.015(2) 0.015(2) -0.0039(16) 0.0039(16) -0.0024(15) C17 0.015(2) 0.013(2) 0.012(2) -0.0011(16) 0.0059(16) -0.0006(15) C18 0.021(2) 0.014(2) 0.018(2) 0.0036(17) 0.0065(18) -0.0026(16) C19 0.027(3) 0.028(3) 0.012(2) -0.0012(19) -0.0017(19) -0.001(2) C20 0.023(2) 0.016(2) 0.014(2) -0.0002(17) 0.0023(18) -0.0015(17) C21 0.0136(19) 0.0090(18) 0.0112(19) 0.0030(15) 0.0067(15) -0.0006(14) C22 0.0152(19) 0.0095(18) 0.011(2) 0.0035(15) 0.0074(16) -0.0005(15) C23 0.0150(19) 0.016(2) 0.0079(19) 0.0035(15) 0.0048(15) 0.0045(15) C24 0.0109(19) 0.021(2) 0.017(2) 0.0042(18) 0.0054(16) 0.0038(16) C25 0.015(2) 0.035(3) 0.013(2) -0.003(2) 0.0011(17) 0.0012(19) C26 0.023(2) 0.034(3) 0.013(2) 0.002(2) 0.0032(19) 0.008(2) C27 0.024(2) 0.024(2) 0.015(2) 0.0098(18) 0.0095(19) 0.0099(18) C28 0.015(2) 0.014(2) 0.016(2) 0.0065(16) 0.0082(17) 0.0061(16) C29 0.017(2) 0.028(3) 0.021(2) 0.001(2) 0.0068(18) -0.0096(18) C30 0.033(3) 0.066(4) 0.009(2) 0.003(3) 0.000(2) 0.006(3) C31 0.019(2) 0.019(2) 0.025(3) 0.0065(18) 0.0136(19) -0.0003(17) C32 0.0131(19) 0.0109(18) 0.0075(18) 0.0019(15) 0.0029(15) 0.0011(15) C33 0.0115(19) 0.016(2) 0.012(2) 0.0000(16) 0.0040(16) -0.0008(15) C34 0.014(2) 0.019(2) 0.014(2) 0.0005(17) 0.0065(17) -0.0007(16) C35 0.012(2) 0.023(2) 0.018(2) -0.0009(18) 0.0019(17) 0.0047(16) C36 0.016(2) 0.016(2) 0.015(2) 0.0005(17) 0.0020(17) 0.0034(16) C37 0.0124(19) 0.0116(19) 0.012(2) 0.0017(16) 0.0019(16) -0.0005(15) C38 0.015(2) 0.020(2) 0.021(2) 0.0099(18) 0.0105(18) 0.0052(17) C39 0.011(2) 0.041(3) 0.034(3) 0.003(2) 0.003(2) 0.008(2) C40 0.019(2) 0.015(2) 0.021(2) 0.0077(18) 0.0064(18) 0.0021(17) C41 0.0103(19) 0.019(2) 0.014(2) 0.0022(17) 0.0032(16) 0.0001(16) C42 0.015(2) 0.021(2) 0.021(2) 0.0075(18) 0.0080(18) 0.0008(17) C43 0.015(2) 0.014(2) 0.031(3) 0.0034(19) 0.0075(19) -0.0032(16) C44 0.014(2) 0.015(2) 0.022(2) -0.0014(18) -0.0001(17) -0.0030(16) C45 0.0108(19) 0.016(2) 0.013(2) 0.0005(16) 0.0009(16) -0.0017(15) C46 0.027(3) 0.032(3) 0.028(3) -0.007(2) 0.011(2) -0.001(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 N3 1.888(4) . yes Co1 N4 1.891(3) . yes Co1 N2 1.908(3) . yes Co1 N1 1.908(4) . yes Co1 N5 1.986(4) . yes Co1 Br1 2.3396(12) . yes Cl1 C46 1.744(6) . ? Cl2 C46 1.761(6) . ? O1 N1 1.339(4) . ? O2 N2 1.335(4) . ? O3 N3 1.331(4) . ? O4 N4 1.334(4) . ? N1 C1 1.297(5) . yes N2 C2 1.298(5) . yes N3 C21 1.307(5) . yes N4 C22 1.307(5) . yes N5 C41 1.339(5) . ? N5 C45 1.347(6) . ? C1 C12 1.479(6) . ? C1 C2 1.484(6) . yes C2 C3 1.484(5) . ? C3 C4 1.406(6) . ? C3 C8 1.413(6) . ? C4 C5 1.390(6) . ? C4 C9 1.509(6) . ? C5 C6 1.402(7) . ? C6 C7 1.373(7) . ? C6 C10 1.511(6) . ? C7 C8 1.386(6) . ? C8 C11 1.505(6) . ? C12 C17 1.402(6) . ? C12 C13 1.408(6) . ? C13 C14 1.378(6) . ? C13 C18 1.505(6) . ? C14 C15 1.391(6) . ? C15 C16 1.385(6) . ? C15 C19 1.505(6) . ? C16 C17 1.401(6) . ? C17 C20 1.513(6) . ? C21 C22 1.473(6) . yes C21 C23 1.484(6) . ? C22 C32 1.483(6) . ? C23 C24 1.405(6) . ? C23 C28 1.412(6) . ? C24 C25 1.395(6) . ? C24 C29 1.510(6) . ? C25 C26 1.384(7) . ? C26 C27 1.398(7) . ? C26 C30 1.505(7) . ? C27 C28 1.378(7) . ? C28 C31 1.507(6) . ? C32 C37 1.407(6) . ? C32 C33 1.422(6) . ? C33 C34 1.388(6) . ? C33 C38 1.501(6) . ? C34 C35 1.395(6) . ? C35 C36 1.392(7) . ? C35 C39 1.502(6) . ? C36 C37 1.388(6) . ? C37 C40 1.501(6) . ? C41 C42 1.388(6) . ? C42 C43 1.388(7) . ? C43 C44 1.385(7) . ? C44 C45 1.384(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 N3 Co1 N4 81.10(15) . . yes N3 Co1 N2 99.28(15) . . yes N4 Co1 N2 179.40(16) . . yes N3 Co1 N1 177.92(15) . . ? N4 Co1 N1 98.97(15) . . yes N2 Co1 N1 80.67(15) . . yes N3 Co1 N5 90.98(14) . . ? N4 Co1 N5 90.93(15) . . ? N2 Co1 N5 88.60(14) . . ? N1 Co1 N5 91.10(14) . . ? N3 Co1 Br1 88.73(11) . . ? N4 Co1 Br1 91.33(11) . . ? N2 Co1 Br1 89.14(11) . . ? N1 Co1 Br1 89.19(11) . . ? N5 Co1 Br1 177.65(10) . . yes C1 N1 O1 120.2(3) . . ? C1 N1 Co1 117.3(3) . . ? O1 N1 Co1 122.6(3) . . ? C2 N2 O2 120.7(3) . . ? C2 N2 Co1 117.2(3) . . ? O2 N2 Co1 122.0(3) . . ? C21 N3 O3 121.9(3) . . ? C21 N3 Co1 117.4(3) . . ? O3 N3 Co1 120.7(3) . . ? C22 N4 O4 122.0(3) . . ? C22 N4 Co1 117.2(3) . . ? O4 N4 Co1 120.8(3) . . ? C41 N5 C45 118.4(4) . . ? C41 N5 Co1 121.8(3) . . ? C45 N5 Co1 119.3(3) . . ? N1 C1 C12 123.0(4) . . ? N1 C1 C2 112.3(4) . . ? C12 C1 C2 124.6(4) . . ? N2 C2 C3 123.1(4) . . ? N2 C2 C1 112.3(4) . . ? C3 C2 C1 124.5(4) . . ? C4 C3 C8 119.7(4) . . ? C4 C3 C2 121.3(4) . . ? C8 C3 C2 119.0(4) . . ? C5 C4 C3 119.2(4) . . ? C5 C4 C9 118.2(4) . . ? C3 C4 C9 122.6(4) . . ? C4 C5 C6 121.4(4) . . ? C7 C6 C5 118.2(4) . . ? C7 C6 C10 121.3(5) . . ? C5 C6 C10 120.5(4) . . ? C6 C7 C8 122.7(5) . . ? C7 C8 C3 118.7(4) . . ? C7 C8 C11 119.7(4) . . ? C3 C8 C11 121.6(4) . . ? C17 C12 C13 120.0(4) . . ? C17 C12 C1 119.5(4) . . ? C13 C12 C1 120.5(4) . . ? C14 C13 C12 119.3(4) . . ? C14 C13 C18 119.2(4) . . ? C12 C13 C18 121.4(4) . . ? C13 C14 C15 121.7(4) . . ? C16 C15 C14 118.6(4) . . ? C16 C15 C19 121.5(4) . . ? C14 C15 C19 119.9(4) . . ? C15 C16 C17 121.7(4) . . ? C16 C17 C12 118.5(4) . . ? C16 C17 C20 118.8(4) . . ? C12 C17 C20 122.6(4) . . ? N3 C21 C22 112.1(4) . . ? N3 C21 C23 120.5(4) . . ? C22 C21 C23 127.4(4) . . ? N4 C22 C21 112.0(4) . . ? N4 C22 C32 123.5(4) . . ? C21 C22 C32 124.4(4) . . ? C24 C23 C28 119.9(4) . . ? C24 C23 C21 121.0(4) . . ? C28 C23 C21 118.8(4) . . ? C25 C24 C23 118.7(4) . . ? C25 C24 C29 119.1(4) . . ? C23 C24 C29 122.1(4) . . ? C26 C25 C24 122.1(5) . . ? C25 C26 C27 118.1(4) . . ? C25 C26 C30 122.1(5) . . ? C27 C26 C30 119.7(5) . . ? C28 C27 C26 121.9(4) . . ? C27 C28 C23 119.2(4) . . ? C27 C28 C31 118.3(4) . . ? C23 C28 C31 122.5(4) . . ? C37 C32 C33 119.3(4) . . ? C37 C32 C22 122.5(4) . . ? C33 C32 C22 118.2(4) . . ? C34 C33 C32 119.0(4) . . ? C34 C33 C38 119.1(4) . . ? C32 C33 C38 121.9(4) . . ? C33 C34 C35 122.4(4) . . ? C36 C35 C34 117.5(4) . . ? C36 C35 C39 121.4(4) . . ? C34 C35 C39 121.0(4) . . ? C37 C36 C35 122.5(4) . . ? C36 C37 C32 119.3(4) . . ? C36 C37 C40 119.0(4) . . ? C32 C37 C40 121.7(4) . . ? N5 C41 C42 122.4(4) . . ? C41 C42 C43 119.1(4) . . ? C44 C43 C42 118.5(4) . . ? C45 C44 C43 119.3(4) . . ? N5 C45 C44 122.3(4) . . ? Cl1 C46 Cl2 111.4(3) . . ? 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 N3 Co1 N1 C1 -92(4) . . . . ? N4 Co1 N1 C1 176.7(3) . . . . ? N2 Co1 N1 C1 -2.8(3) . . . . ? N5 Co1 N1 C1 85.6(3) . . . . ? Br1 Co1 N1 C1 -92.1(3) . . . . ? N3 Co1 N1 O1 89(4) . . . . ? N4 Co1 N1 O1 -2.7(3) . . . . ? N2 Co1 N1 O1 177.8(3) . . . . ? N5 Co1 N1 O1 -93.8(3) . . . . ? Br1 Co1 N1 O1 88.5(3) . . . . ? N3 Co1 N2 C2 -177.0(3) . . . . ? N4 Co1 N2 C2 -48(19) . . . . ? N1 Co1 N2 C2 5.1(3) . . . . ? N5 Co1 N2 C2 -86.2(3) . . . . ? Br1 Co1 N2 C2 94.4(3) . . . . ? N3 Co1 N2 O2 -1.4(3) . . . . ? N4 Co1 N2 O2 128(18) . . . . ? N1 Co1 N2 O2 -179.3(3) . . . . ? N5 Co1 N2 O2 89.4(3) . . . . ? Br1 Co1 N2 O2 -90.0(3) . . . . ? N4 Co1 N3 C21 -1.8(3) . . . . ? N2 Co1 N3 C21 177.7(3) . . . . ? N1 Co1 N3 C21 -94(4) . . . . ? N5 Co1 N3 C21 89.0(3) . . . . ? Br1 Co1 N3 C21 -93.3(3) . . . . ? N4 Co1 N3 O3 177.6(3) . . . . ? N2 Co1 N3 O3 -2.9(3) . . . . ? N1 Co1 N3 O3 85(4) . . . . ? N5 Co1 N3 O3 -91.6(3) . . . . ? Br1 Co1 N3 O3 86.1(3) . . . . ? N3 Co1 N4 C22 3.8(3) . . . . ? N2 Co1 N4 C22 -125(18) . . . . ? N1 Co1 N4 C22 -178.3(3) . . . . ? N5 Co1 N4 C22 -87.0(3) . . . . ? Br1 Co1 N4 C22 92.3(3) . . . . ? N3 Co1 N4 O4 -178.1(3) . . . . ? N2 Co1 N4 O4 53(19) . . . . ? N1 Co1 N4 O4 -0.2(3) . . . . ? N5 Co1 N4 O4 91.0(3) . . . . ? Br1 Co1 N4 O4 -89.6(3) . . . . ? N3 Co1 N5 C41 -154.3(3) . . . . ? N4 Co1 N5 C41 -73.2(3) . . . . ? N2 Co1 N5 C41 106.4(3) . . . . ? N1 Co1 N5 C41 25.8(3) . . . . ? Br1 Co1 N5 C41 123(3) . . . . ? N3 Co1 N5 C45 33.7(3) . . . . ? N4 Co1 N5 C45 114.8(3) . . . . ? N2 Co1 N5 C45 -65.6(3) . . . . ? N1 Co1 N5 C45 -146.2(3) . . . . ? Br1 Co1 N5 C45 -49(3) . . . . ? O1 N1 C1 C12 -2.4(6) . . . . ? Co1 N1 C1 C12 178.2(3) . . . . ? O1 N1 C1 C2 179.8(3) . . . . ? Co1 N1 C1 C2 0.4(4) . . . . ? O2 N2 C2 C3 -4.8(6) . . . . ? Co1 N2 C2 C3 170.9(3) . . . . ? O2 N2 C2 C1 178.2(3) . . . . ? Co1 N2 C2 C1 -6.1(4) . . . . ? N1 C1 C2 N2 3.6(5) . . . . ? C12 C1 C2 N2 -174.1(4) . . . . ? N1 C1 C2 C3 -173.3(4) . . . . ? C12 C1 C2 C3 8.9(6) . . . . ? N2 C2 C3 C4 113.8(5) . . . . ? C1 C2 C3 C4 -69.6(6) . . . . ? N2 C2 C3 C8 -66.0(6) . . . . ? C1 C2 C3 C8 110.6(5) . . . . ? C8 C3 C4 C5 -2.6(6) . . . . ? C2 C3 C4 C5 177.5(4) . . . . ? C8 C3 C4 C9 176.7(4) . . . . ? C2 C3 C4 C9 -3.1(6) . . . . ? C3 C4 C5 C6 0.9(7) . . . . ? C9 C4 C5 C6 -178.5(4) . . . . ? C4 C5 C6 C7 1.0(7) . . . . ? C4 C5 C6 C10 -177.5(4) . . . . ? C5 C6 C7 C8 -1.0(7) . . . . ? C10 C6 C7 C8 177.4(4) . . . . ? C6 C7 C8 C3 -0.7(7) . . . . ? C6 C7 C8 C11 -179.7(4) . . . . ? C4 C3 C8 C7 2.6(6) . . . . ? C2 C3 C8 C7 -177.6(4) . . . . ? C4 C3 C8 C11 -178.5(4) . . . . ? C2 C3 C8 C11 1.4(6) . . . . ? N1 C1 C12 C17 -71.3(6) . . . . ? C2 C1 C12 C17 106.2(5) . . . . ? N1 C1 C12 C13 107.4(5) . . . . ? C2 C1 C12 C13 -75.1(5) . . . . ? C17 C12 C13 C14 -2.3(6) . . . . ? C1 C12 C13 C14 179.0(4) . . . . ? C17 C12 C13 C18 176.1(4) . . . . ? C1 C12 C13 C18 -2.6(6) . . . . ? C12 C13 C14 C15 -1.1(6) . . . . ? C18 C13 C14 C15 -179.6(4) . . . . ? C13 C14 C15 C16 2.4(6) . . . . ? C13 C14 C15 C19 -179.1(4) . . . . ? C14 C15 C16 C17 -0.3(7) . . . . ? C19 C15 C16 C17 -178.8(4) . . . . ? C15 C16 C17 C12 -3.0(6) . . . . ? C15 C16 C17 C20 175.1(4) . . . . ? C13 C12 C17 C16 4.3(6) . . . . ? C1 C12 C17 C16 -177.0(4) . . . . ? C13 C12 C17 C20 -173.7(4) . . . . ? C1 C12 C17 C20 5.0(6) . . . . ? O3 N3 C21 C22 -179.7(3) . . . . ? Co1 N3 C21 C22 -0.3(4) . . . . ? O3 N3 C21 C23 -0.4(6) . . . . ? Co1 N3 C21 C23 179.0(3) . . . . ? O4 N4 C22 C21 177.1(3) . . . . ? Co1 N4 C22 C21 -4.9(5) . . . . ? O4 N4 C22 C32 -5.0(6) . . . . ? Co1 N4 C22 C32 173.0(3) . . . . ? N3 C21 C22 N4 3.3(5) . . . . ? C23 C21 C22 N4 -175.9(4) . . . . ? N3 C21 C22 C32 -174.6(4) . . . . ? C23 C21 C22 C32 6.2(7) . . . . ? N3 C21 C23 C24 110.4(5) . . . . ? C22 C21 C23 C24 -70.4(6) . . . . ? N3 C21 C23 C28 -63.2(5) . . . . ? C22 C21 C23 C28 116.0(5) . . . . ? C28 C23 C24 C25 0.9(6) . . . . ? C21 C23 C24 C25 -172.7(4) . . . . ? C28 C23 C24 C29 178.6(4) . . . . ? C21 C23 C24 C29 5.1(6) . . . . ? C23 C24 C25 C26 0.8(7) . . . . ? C29 C24 C25 C26 -177.0(5) . . . . ? C24 C25 C26 C27 -1.7(7) . . . . ? C24 C25 C26 C30 175.2(5) . . . . ? C25 C26 C27 C28 0.9(7) . . . . ? C30 C26 C27 C28 -176.0(5) . . . . ? C26 C27 C28 C23 0.7(7) . . . . ? C26 C27 C28 C31 -179.2(4) . . . . ? C24 C23 C28 C27 -1.6(6) . . . . ? C21 C23 C28 C27 172.1(4) . . . . ? C24 C23 C28 C31 178.3(4) . . . . ? C21 C23 C28 C31 -8.0(6) . . . . ? N4 C22 C32 C37 118.1(5) . . . . ? C21 C22 C32 C37 -64.2(6) . . . . ? N4 C22 C32 C33 -60.9(6) . . . . ? C21 C22 C32 C33 116.7(5) . . . . ? C37 C32 C33 C34 0.4(6) . . . . ? C22 C32 C33 C34 179.4(4) . . . . ? C37 C32 C33 C38 179.5(4) . . . . ? C22 C32 C33 C38 -1.4(6) . . . . ? C32 C33 C34 C35 0.2(7) . . . . ? C38 C33 C34 C35 -178.9(4) . . . . ? C33 C34 C35 C36 0.4(7) . . . . ? C33 C34 C35 C39 -178.9(5) . . . . ? C34 C35 C36 C37 -1.6(7) . . . . ? C39 C35 C36 C37 177.7(5) . . . . ? C35 C36 C37 C32 2.3(7) . . . . ? C35 C36 C37 C40 -176.6(4) . . . . ? C33 C32 C37 C36 -1.6(6) . . . . ? C22 C32 C37 C36 179.4(4) . . . . ? C33 C32 C37 C40 177.2(4) . . . . ? C22 C32 C37 C40 -1.8(7) . . . . ? C45 N5 C41 C42 1.7(6) . . . . ? Co1 N5 C41 C42 -170.4(3) . . . . ? N5 C41 C42 C43 -0.8(7) . . . . ? C41 C42 C43 C44 -0.6(7) . . . . ? C42 C43 C44 C45 1.2(7) . . . . ? C41 N5 C45 C44 -1.1(6) . . . . ? Co1 N5 C45 C44 171.2(3) . . . . ? C43 C44 C45 N5 -0.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.009 _refine_diff_density_min -1.862 _refine_diff_density_rms 0.180 #===END