# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 909985' #TrackingRef 'complex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H33 Br8 Cl2 Co2 N8 O12.50' _chemical_formula_weight 1413.58 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' 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 15.5601(6) _cell_length_b 28.2409(10) _cell_length_c 8.9927(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3951.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 80659 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour dark-blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 2.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2708 _exptl_absorpt_coefficient_mu 9.129 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1704 _exptl_absorpt_correction_T_max 0.2903 _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 14873 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.45 _reflns_number_total 8705 _reflns_number_gt 7335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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. Two Uiso/Uij, four distance and angle restraints and 15 least-squares restraints to remove unusual anisotropic displacements and to model disorder perchlorate ions ; _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^)+(0.0514P)^2^+57.9128P] 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 none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.22(2) _refine_ls_number_reflns 8705 _refine_ls_number_parameters 461 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.092 _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 Br8 Br 0.26804(8) 0.30163(5) 0.77099(15) 0.0313(3) Uani 1 1 d . . . Br2 Br 0.37346(9) 0.45767(5) 1.62976(16) 0.0340(3) Uani 1 1 d . . . Br4 Br 0.27948(8) 0.29916(5) 1.26403(14) 0.0308(3) Uani 1 1 d . . . Br5 Br 0.38153(9) 0.48037(5) 1.19339(15) 0.0339(3) Uani 1 1 d . . . Br1 Br 0.16405(9) 0.48046(5) 1.67461(16) 0.0357(3) Uani 1 1 d . . . Br7 Br 0.11644(8) 0.36687(5) 0.93057(15) 0.0329(3) Uani 1 1 d . . . Br3 Br 0.43161(8) 0.36548(5) 1.42478(15) 0.0325(3) Uani 1 1 d . . . Br6 Br 0.17376(9) 0.46061(5) 1.13126(17) 0.0376(3) Uani 1 1 d . . . Co1 Co -0.00516(10) 0.35858(6) 1.42136(19) 0.0242(3) Uani 1 1 d . . . Co2 Co 0.55270(10) 0.36263(6) 0.9227(2) 0.0271(4) Uani 1 1 d . . . O2 O 0.0561(6) 0.4078(3) 1.5179(11) 0.036(2) Uani 1 1 d . . . O1 O 0.1004(5) 0.3355(3) 1.3486(10) 0.030(2) Uani 1 1 d . . . O3 O 0.4458(5) 0.3405(3) 0.8453(9) 0.0283(19) Uani 1 1 d . . . C16 C 0.2979(8) 0.3553(4) 0.8899(13) 0.022(3) Uani 1 1 d . . . O4 O 0.4923(6) 0.4118(3) 1.0158(11) 0.032(2) Uani 1 1 d . . . N4 N -0.0636(6) 0.3056(4) 1.3272(11) 0.025(2) Uani 1 1 d . . . H4A H -0.1221 0.3104 1.3288 0.030 Uiso 1 1 calc R . . H4B H -0.0463 0.3028 1.2298 0.030 Uiso 1 1 calc R . . N6 N 0.6603(7) 0.3913(4) 1.0011(14) 0.040(3) Uani 1 1 d . . . H6A H 0.6504 0.4035 1.0946 0.048 Uiso 1 1 calc R . . H6B H 0.7021 0.3684 1.0088 0.048 Uiso 1 1 calc R . . N5 N 0.5742(7) 0.4018(4) 0.7458(13) 0.034(2) Uani 1 1 d . . . H5A H 0.5612 0.3847 0.6616 0.040 Uiso 1 1 calc R . . H5B H 0.5391 0.4280 0.7482 0.040 Uiso 1 1 calc R . . N2 N -0.1105(7) 0.3883(4) 1.4947(12) 0.028(2) Uani 1 1 d . . . H2A H -0.1496 0.3654 1.5212 0.034 Uiso 1 1 calc R . . H2B H -0.0985 0.4063 1.5773 0.034 Uiso 1 1 calc R . . N1 N -0.0165(7) 0.3996(3) 1.2477(13) 0.031(2) Uani 1 1 d . . . H1A H 0.0365 0.4108 1.2193 0.037 Uiso 1 1 calc R . . H1B H -0.0398 0.3830 1.1695 0.037 Uiso 1 1 calc R . . N3 N 0.0062(7) 0.3172(4) 1.5955(12) 0.033(3) Uani 1 1 d . . . H3A H 0.0627 0.3082 1.6068 0.040 Uiso 1 1 calc R . . H3B H -0.0104 0.3332 1.6798 0.040 Uiso 1 1 calc R . . C3 C 0.2020(9) 0.4285(4) 1.5579(15) 0.031(3) Uani 1 1 d . . . N8 N 0.6109(7) 0.3074(4) 0.8312(13) 0.035(3) Uani 1 1 d . . . H8A H 0.5892 0.3022 0.7374 0.042 Uiso 1 1 calc R . . H8B H 0.6688 0.3133 0.8229 0.042 Uiso 1 1 calc R . . C14 C 0.2566(8) 0.4216(4) 1.0475(13) 0.022(3) Uani 1 1 d . . . C13 C 0.3437(8) 0.4313(4) 1.0634(13) 0.023(2) Uani 1 1 d . . . N7 N 0.5360(8) 0.3215(4) 1.0950(11) 0.036(3) Uani 1 1 d . . . H7A H 0.5619 0.3348 1.1769 0.043 Uiso 1 1 calc R . . H7B H 0.4781 0.3187 1.1147 0.043 Uiso 1 1 calc R . . C4 C 0.2902(8) 0.4186(5) 1.5322(15) 0.030(3) Uani 1 1 d . . . C8 C -0.1478(9) 0.4194(6) 1.3729(19) 0.046(4) Uani 1 1 d . . . H8C H -0.1850 0.4004 1.3061 0.056 Uiso 1 1 calc R . . H8D H -0.1825 0.4452 1.4165 0.056 Uiso 1 1 calc R . . C10 C -0.0412(8) 0.2614(4) 1.4118(14) 0.029(3) Uani 1 1 d . . . H10A H 0.0177 0.2506 1.3871 0.035 Uiso 1 1 calc R . . H10B H -0.0822 0.2356 1.3889 0.035 Uiso 1 1 calc R . . C12 C 0.4071(8) 0.4034(5) 0.9986(15) 0.030(3) Uani 1 1 d . . . C11 C 0.3861(8) 0.3649(4) 0.9054(12) 0.023(2) Uani 1 1 d . . . C6 C 0.2529(7) 0.3512(4) 1.3848(13) 0.023(3) Uani 1 1 d . . . C2 C 0.1380(8) 0.4002(4) 1.4970(14) 0.026(3) Uani 1 1 d . . . C1 C 0.1653(8) 0.3600(5) 1.4096(17) 0.034(3) Uani 1 1 d . . . C9 C -0.0473(8) 0.2757(4) 1.5753(18) 0.036(3) Uani 1 1 d . . . H9A H -0.1076 0.2830 1.6017 0.043 Uiso 1 1 calc R . . H9B H -0.0270 0.2496 1.6397 0.043 Uiso 1 1 calc R . . C17 C 0.6665(10) 0.4173(5) 0.7398(18) 0.045(4) Uani 1 1 d . . . H17A H 0.6731 0.4456 0.6756 0.055 Uiso 1 1 calc R . . H17B H 0.7035 0.3916 0.7009 0.055 Uiso 1 1 calc R . . C7 C -0.0730(10) 0.4392(5) 1.289(2) 0.050(4) Uani 1 1 d . . . H7C H -0.0933 0.4557 1.1980 0.060 Uiso 1 1 calc R . . H7D H -0.0413 0.4622 1.3510 0.060 Uiso 1 1 calc R . . C18 C 0.6899(10) 0.4291(7) 0.903(2) 0.062(5) Uani 1 1 d . . . H18A H 0.7530 0.4326 0.9121 0.074 Uiso 1 1 calc R . . H18B H 0.6628 0.4594 0.9319 0.074 Uiso 1 1 calc R . . C19 C 0.5735(18) 0.2729(8) 1.068(2) 0.092(5) Uani 1 1 d . . . H19A H 0.6243 0.2684 1.1324 0.110 Uiso 1 1 calc R . . H19B H 0.5304 0.2485 1.0947 0.110 Uiso 1 1 calc R . . C20 C 0.5975(17) 0.2667(6) 0.921(2) 0.085(4) Uani 1 1 d . . . H20A H 0.5527 0.2472 0.8719 0.102 Uiso 1 1 calc R . . H20B H 0.6512 0.2480 0.9196 0.102 Uiso 1 1 calc R . . Cl2 Cl 0.6795(2) 0.31931(16) 1.4219(4) 0.0477(9) Uani 1 1 d . . . Cl1 Cl -0.1342(2) 0.33188(18) 1.9335(4) 0.0498(10) Uani 1 1 d D . . O5 O -0.1599(12) 0.3589(9) 2.0584(17) 0.139(5) Uani 1 1 d . A . O9 O 0.7390(12) 0.3224(7) 1.533(2) 0.116 Uani 1 1 d . . . O10 O 0.7350(11) 0.3165(7) 1.302(2) 0.105(3) Uani 1 1 d . . . O6 O -0.0582(8) 0.3137(8) 1.9603(16) 0.103(3) Uani 1 1 d . A 1 O7 O -0.1169(18) 0.3637(10) 1.8043(18) 0.162(8) Uani 1 1 d . A . O8 O -0.2062(12) 0.3084(8) 1.890(3) 0.164 Uani 1 1 d D A 2 O11 O 0.6396(15) 0.3594(7) 1.379(2) 0.147(8) Uani 1 1 d . . . O12 O 0.6317(11) 0.2789(6) 1.440(2) 0.113 Uani 1 1 d . . . O13 O 0.5000 0.5000 0.865(2) 0.053(4) Uani 1 2 d SD . . C5 C 0.3103(8) 0.3798(4) 1.4539(13) 0.024(3) Uani 1 1 d U . . C15 C 0.2317(8) 0.3818(4) 0.9569(14) 0.027(3) Uani 1 1 d U . . H13O H 0.484(12) 0.477(4) 0.921(16) 0.07(6) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br8 0.0252(6) 0.0332(7) 0.0355(7) -0.0120(6) 0.0051(5) -0.0059(5) Br2 0.0288(6) 0.0306(7) 0.0426(7) -0.0021(6) -0.0114(6) -0.0071(5) Br4 0.0224(6) 0.0365(7) 0.0335(6) -0.0080(6) -0.0049(5) 0.0056(5) Br5 0.0408(7) 0.0229(6) 0.0381(7) -0.0065(5) 0.0050(6) -0.0027(5) Br1 0.0382(7) 0.0257(6) 0.0432(7) -0.0075(6) -0.0003(6) -0.0029(6) Br7 0.0215(6) 0.0389(7) 0.0383(7) -0.0040(6) 0.0046(5) -0.0008(5) Br3 0.0194(6) 0.0425(7) 0.0355(7) -0.0028(6) -0.0037(5) -0.0010(5) Br6 0.0332(7) 0.0274(6) 0.0522(8) -0.0046(6) 0.0151(6) 0.0047(6) Co1 0.0184(7) 0.0230(8) 0.0313(8) -0.0043(7) -0.0004(7) -0.0022(6) Co2 0.0200(8) 0.0292(9) 0.0321(9) -0.0052(8) 0.0029(7) -0.0026(7) O2 0.029(5) 0.035(5) 0.043(5) -0.013(4) 0.009(4) -0.009(4) O1 0.015(4) 0.033(5) 0.040(5) -0.009(4) -0.007(4) 0.003(4) O3 0.024(4) 0.029(4) 0.031(5) -0.014(4) 0.005(4) -0.001(4) C16 0.032(7) 0.016(5) 0.019(5) -0.002(4) 0.006(5) -0.007(5) O4 0.025(4) 0.024(4) 0.049(6) -0.017(4) 0.012(4) 0.005(3) N4 0.021(5) 0.030(5) 0.025(5) -0.012(4) -0.012(4) 0.004(4) N6 0.020(5) 0.049(7) 0.050(7) -0.011(6) 0.000(5) -0.004(5) N5 0.034(6) 0.031(6) 0.035(6) -0.006(5) -0.005(5) 0.005(5) N2 0.029(6) 0.023(5) 0.032(6) -0.007(4) 0.003(5) 0.008(4) N1 0.025(5) 0.023(5) 0.045(6) 0.010(5) 0.013(5) -0.002(4) N3 0.029(6) 0.035(6) 0.035(6) 0.000(5) -0.010(5) -0.003(5) C3 0.031(7) 0.025(6) 0.038(8) -0.008(6) 0.018(6) -0.017(5) N8 0.028(6) 0.029(6) 0.049(7) 0.006(5) 0.014(5) 0.006(5) C14 0.024(6) 0.020(6) 0.023(6) 0.003(5) 0.014(5) 0.000(5) C13 0.029(6) 0.019(5) 0.022(6) 0.005(5) 0.001(5) 0.006(5) N7 0.041(6) 0.052(7) 0.014(5) -0.003(5) -0.001(4) -0.013(6) C4 0.024(6) 0.030(6) 0.037(7) -0.004(6) -0.001(5) -0.004(5) C8 0.021(7) 0.053(9) 0.065(10) -0.008(8) -0.002(7) 0.007(6) C10 0.034(7) 0.024(6) 0.030(6) -0.007(5) -0.010(5) 0.009(5) C12 0.022(6) 0.035(7) 0.033(7) 0.000(6) 0.006(5) -0.009(5) C11 0.027(6) 0.020 0.022(5) -0.012(5) 0.008(5) -0.003(5) C6 0.017(5) 0.032(6) 0.021(6) -0.009(5) 0.009(4) -0.006(5) C2 0.029(6) 0.024(6) 0.026(6) -0.003(5) -0.004(5) -0.010(5) C1 0.019(6) 0.029(7) 0.054(9) 0.004(6) 0.012(6) 0.001(5) C9 0.020(6) 0.026(7) 0.062(9) 0.010(6) -0.010(6) -0.003(5) C17 0.047(9) 0.033(7) 0.056(10) -0.002(7) 0.015(8) -0.001(6) C7 0.035(8) 0.035(8) 0.079(12) 0.018(8) -0.002(8) 0.005(6) C18 0.022(7) 0.075(13) 0.089(14) -0.003(10) -0.018(8) -0.015(8) C19 0.141 0.070(14) 0.064(13) -0.007(11) 0.055(13) -0.013(14) C20 0.150 0.041(9) 0.065(11) 0.021(8) 0.079(11) 0.039(11) Cl2 0.0260(16) 0.075(3) 0.0420(19) -0.0105(19) 0.0075(15) -0.0034(17) Cl1 0.0163(14) 0.105(3) 0.0275(17) -0.0052(19) -0.0063(13) 0.0132(17) O5 0.116(14) 0.247 0.054(9) -0.051(12) -0.020(9) 0.097(14) O9 0.114 0.118 0.115 0.053(9) -0.063(8) -0.059(9) O10 0.076(10) 0.118 0.123 -0.016(11) 0.058(9) -0.025(9) O6 0.037(7) 0.203 0.068(9) 0.019(11) -0.001(6) 0.008(10) O7 0.229 0.20(2) 0.053(10) 0.023(12) 0.049(13) 0.08(2) O8 0.151 0.157 0.184 -0.086(14) -0.052(16) 0.045(16) O11 0.17(2) 0.130(16) 0.140 -0.012(14) -0.102(13) 0.078(15) O12 0.110 0.111 0.119 0.046(9) -0.022(11) -0.080(7) O13 0.044(9) 0.063(12) 0.052(10) 0.000 0.000 0.008(8) C5 0.023(3) 0.024(3) 0.024(3) 0.0000(10) 0.0001(10) 0.0004(10) C15 0.027(3) 0.027(3) 0.027(3) 0.0004(10) 0.0008(10) 0.0008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br8 C16 1.911(12) . ? Br2 C4 1.914(13) . ? Br4 C6 1.874(12) . ? Br5 C13 1.907(12) . ? Br1 C3 1.898(13) . ? Br7 C15 1.858(13) . ? Br3 C5 1.948(12) . ? Br6 C14 1.855(12) . ? Co1 O1 1.885(9) . ? Co1 O2 1.896(9) . ? Co1 N4 1.945(10) . ? Co1 N1 1.952(11) . ? Co1 N2 1.956(10) . ? Co1 N3 1.962(11) . ? Co2 O4 1.875(8) . ? Co2 O3 1.908(9) . ? Co2 N7 1.955(11) . ? Co2 N5 1.966(12) . ? Co2 N8 1.983(11) . ? Co2 N6 1.989(11) . ? O2 C2 1.307(15) . ? O1 C1 1.340(16) . ? O3 C11 1.278(14) . ? C16 C11 1.406(16) . ? C16 C15 1.409(17) . ? O4 C12 1.356(15) . ? N4 C10 1.504(15) . ? N6 C18 1.46(2) . ? N5 C17 1.503(18) . ? N2 C8 1.518(19) . ? N1 C7 1.468(17) . ? N3 C9 1.449(16) . ? C3 C2 1.389(17) . ? C3 C4 1.420(18) . ? N8 C20 1.417(18) . ? C14 C13 1.390(17) . ? C14 C15 1.441(17) . ? C13 C12 1.391(17) . ? N7 C19 1.51(2) . ? C4 C5 1.340(18) . ? C8 C7 1.50(2) . ? C10 C9 1.53(2) . ? C12 C11 1.410(17) . ? C6 C5 1.355(17) . ? C6 C1 1.404(16) . ? C2 C1 1.444(18) . ? C17 C18 1.55(2) . ? C19 C20 1.39(2) . ? Cl2 O11 1.347(17) . ? Cl2 O9 1.366(15) . ? Cl2 O12 1.372(14) . ? Cl2 O10 1.381(15) . ? Cl1 O6 1.312(14) . ? Cl1 O8 1.358(16) . ? Cl1 O5 1.415(16) . ? Cl1 O7 1.49(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 88.5(4) . . ? O1 Co1 N4 89.5(4) . . ? O2 Co1 N4 176.8(4) . . ? O1 Co1 N1 90.4(4) . . ? O2 Co1 N1 88.7(5) . . ? N4 Co1 N1 93.8(4) . . ? O1 Co1 N2 174.8(4) . . ? O2 Co1 N2 87.3(4) . . ? N4 Co1 N2 94.9(4) . . ? N1 Co1 N2 86.5(4) . . ? O1 Co1 N3 89.6(4) . . ? O2 Co1 N3 91.5(4) . . ? N4 Co1 N3 86.1(4) . . ? N1 Co1 N3 179.8(5) . . ? N2 Co1 N3 93.6(5) . . ? O4 Co2 O3 88.2(4) . . ? O4 Co2 N7 91.1(5) . . ? O3 Co2 N7 88.7(4) . . ? O4 Co2 N5 91.7(4) . . ? O3 Co2 N5 92.2(4) . . ? N7 Co2 N5 177.1(5) . . ? O4 Co2 N8 175.9(4) . . ? O3 Co2 N8 89.4(4) . . ? N7 Co2 N8 85.5(5) . . ? N5 Co2 N8 91.7(5) . . ? O4 Co2 N6 87.8(5) . . ? O3 Co2 N6 175.1(5) . . ? N7 Co2 N6 94.2(5) . . ? N5 Co2 N6 85.1(5) . . ? N8 Co2 N6 94.8(5) . . ? C2 O2 Co1 107.7(7) . . ? C1 O1 Co1 109.6(8) . . ? C11 O3 Co2 107.6(7) . . ? C11 C16 C15 124.6(11) . . ? C11 C16 Br8 116.5(9) . . ? C15 C16 Br8 118.9(9) . . ? C12 O4 Co2 107.9(8) . . ? C10 N4 Co1 108.1(7) . . ? C18 N6 Co2 110.4(9) . . ? C17 N5 Co2 110.8(9) . . ? C8 N2 Co1 109.0(8) . . ? C7 N1 Co1 107.8(9) . . ? C9 N3 Co1 109.3(9) . . ? C2 C3 C4 121.0(12) . . ? C2 C3 Br1 116.1(10) . . ? C4 C3 Br1 122.9(10) . . ? C20 N8 Co2 109.6(9) . . ? C13 C14 C15 118.2(11) . . ? C13 C14 Br6 121.2(9) . . ? C15 C14 Br6 120.4(9) . . ? C14 C13 C12 122.5(11) . . ? C14 C13 Br5 120.5(9) . . ? C12 C13 Br5 116.7(9) . . ? C19 N7 Co2 111.1(10) . . ? C5 C4 C3 118.2(12) . . ? C5 C4 Br2 123.6(10) . . ? C3 C4 Br2 117.8(10) . . ? C7 C8 N2 106.5(11) . . ? N4 C10 C9 104.6(9) . . ? O4 C12 C13 123.1(11) . . ? O4 C12 C11 115.5(11) . . ? C13 C12 C11 121.4(12) . . ? O3 C11 C16 124.3(10) . . ? O3 C11 C12 119.9(11) . . ? C16 C11 C12 115.8(11) . . ? C5 C6 C1 117.6(12) . . ? C5 C6 Br4 126.0(9) . . ? C1 C6 Br4 116.4(9) . . ? O2 C2 C3 123.2(12) . . ? O2 C2 C1 119.6(11) . . ? C3 C2 C1 117.2(12) . . ? O1 C1 C6 125.1(12) . . ? O1 C1 C2 114.0(11) . . ? C6 C1 C2 120.7(12) . . ? N3 C9 C10 107.4(11) . . ? N5 C17 C18 104.7(12) . . ? N1 C7 C8 107.9(11) . . ? N6 C18 C17 110.1(13) . . ? C20 C19 N7 111.9(18) . . ? C19 C20 N8 118.7(17) . . ? O11 Cl2 O9 117.8(12) . . ? O11 Cl2 O12 118.9(14) . . ? O9 Cl2 O12 109.5(10) . . ? O11 Cl2 O10 96.6(15) . . ? O9 Cl2 O10 98.6(12) . . ? O12 Cl2 O10 112.6(12) . . ? O6 Cl1 O8 127.3(14) . . ? O6 Cl1 O5 108.7(10) . . ? O8 Cl1 O5 104.8(14) . . ? O6 Cl1 O7 102.5(12) . . ? O8 Cl1 O7 102.7(16) . . ? O5 Cl1 O7 110.1(13) . . ? C4 C5 C6 125.1(12) . . ? C4 C5 Br3 117.8(9) . . ? C6 C5 Br3 117.0(9) . . ? C16 C15 C14 117.4(11) . . ? C16 C15 Br7 122.1(9) . . ? C14 C15 Br7 120.5(9) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.614 _refine_diff_density_min -1.317 _refine_diff_density_rms 0.212 data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 909986' #TrackingRef 'complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 Br4 Cl Co N4 O6' _chemical_formula_weight 730.34 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.476(2) _cell_length_b 9.327(3) _cell_length_c 13.954(5) _cell_angle_alpha 85.457(2) _cell_angle_beta 80.366(3) _cell_angle_gamma 81.064(2) _cell_volume 1072.8(1) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10148 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour Greenish-red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 8.410 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3129 _exptl_absorpt_correction_T_max 0.6323 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 8000 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.44 _reflns_number_total 4808 _reflns_number_gt 4105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0443P)^2^+1.9353P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4808 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 C1 C 0.3773(4) 0.0535(4) 0.8156(3) 0.0202(7) Uani 1 1 d . . . C2 C 0.2584(4) 0.1074(4) 0.8920(3) 0.0196(7) Uani 1 1 d . . . C3 C 0.2430(4) 0.0291(4) 0.9813(3) 0.0211(7) Uani 1 1 d . . . C4 C 0.3387(4) -0.1057(4) 0.9946(3) 0.0230(8) Uani 1 1 d . . . C5 C 0.4556(4) -0.1585(4) 0.9187(3) 0.0220(7) Uani 1 1 d . . . C6 C 0.4748(4) -0.0778(4) 0.8298(3) 0.0195(7) Uani 1 1 d . . . C7 C 0.3488(5) 0.5661(5) 0.7376(3) 0.0305(9) Uani 1 1 d . . . H7A H 0.3704(10) 0.5758(6) 0.670(3) 0.037 Uiso 1 1 calc R . . H7B H 0.425(3) 0.6080(17) 0.7622(10) 0.037 Uiso 1 1 calc R . . C8 C 0.1815(6) 0.6443(5) 0.7729(4) 0.0360(10) Uani 1 1 d . . . H8A H 0.1812(6) 0.749(4) 0.7594(6) 0.043 Uiso 1 1 calc R . . H8B H 0.1567(11) 0.6269(8) 0.844(3) 0.043 Uiso 1 1 calc R . . C9 C 0.0490(5) 0.5972(5) 0.7262(3) 0.0333(10) Uani 1 1 d . . . H9A H -0.046(4) 0.656(2) 0.7447(8) 0.040 Uiso 1 1 calc R . . H9B H 0.0747(11) 0.6078(6) 0.660(3) 0.040 Uiso 1 1 calc R . . C10 C 0.1450(5) 0.0380(5) 0.6365(3) 0.0314(9) Uani 1 1 d . . . H10A H 0.072(3) -0.020(2) 0.6319(4) 0.038 Uiso 1 1 calc R . . H10B H 0.231(3) -0.018(2) 0.6557(8) 0.038 Uiso 1 1 calc R . . C11 C 0.1951(5) 0.1105(5) 0.5376(3) 0.0292(8) Uani 1 1 d . . . H11A H 0.099(3) 0.171(2) 0.5165(8) 0.035 Uiso 1 1 calc R . . H11B H 0.2348(15) 0.035(3) 0.4902(18) 0.035 Uiso 1 1 calc R . . C12 C 0.3256(5) 0.2052(4) 0.5361(3) 0.0265(8) Uani 1 1 d . . . H12A H 0.415(3) 0.150(2) 0.5588(8) 0.032 Uiso 1 1 calc R . . H12B H 0.3590(14) 0.2386(13) 0.472(2) 0.032 Uiso 1 1 calc R . . N1 N 0.3615(4) 0.4099(3) 0.7692(2) 0.0233(6) Uani 1 1 d . . . H1A H 0.3535 0.4044 0.8360 0.028 Uiso 1 1 calc R . . H1B H 0.4646 0.3679 0.7451 0.028 Uiso 1 1 calc R . . N2 N 0.0281(4) 0.4431(4) 0.7548(2) 0.0259(7) Uani 1 1 d . . . H2A H -0.0484 0.4203 0.7212 0.031 Uiso 1 1 calc R . . H2B H -0.0159 0.4396 0.8197 0.031 Uiso 1 1 calc R . . N3 N 0.0746(4) 0.1457(4) 0.7110(2) 0.0245(7) Uani 1 1 d . . . H3A H 0.0432 0.0953 0.7686 0.029 Uiso 1 1 calc R . . H3B H -0.0173 0.1981 0.6920 0.029 Uiso 1 1 calc R . . N4 N 0.2673(4) 0.3318(3) 0.5976(2) 0.0212(6) Uani 1 1 d . . . H4A H 0.1770 0.3833 0.5761 0.025 Uiso 1 1 calc R . . H4B H 0.3458 0.3918 0.5882 0.025 Uiso 1 1 calc R . . O1 O 0.3900(3) 0.1336(3) 0.73219(18) 0.0207(5) Uani 1 1 d . . . O2 O 0.1650(3) 0.2329(3) 0.87312(19) 0.0238(6) Uani 1 1 d . . . O3 O 0.7280(5) 0.3454(8) 0.6843(3) 0.098(2) Uani 1 1 d . . . O4 O 0.6083(4) 0.4206(5) 0.5511(3) 0.0545(11) Uani 1 1 d . . . O5 O 0.8860(4) 0.4249(4) 0.5477(3) 0.0390(8) Uani 1 1 d . . . O6 O 0.7893(6) 0.2053(6) 0.5578(7) 0.146(4) Uani 1 1 d . . . Cl1 Cl 0.75192(10) 0.34838(11) 0.58163(7) 0.0273(2) Uani 1 1 d . . . Co1 Co 0.21354(5) 0.28552(5) 0.73734(3) 0.01805(12) Uani 1 1 d . . . Br1 Br 0.08240(4) 0.10939(4) 1.08105(3) 0.02507(10) Uani 1 1 d . . . Br2 Br 0.30778(5) -0.21190(5) 1.11573(3) 0.03010(11) Uani 1 1 d . . . Br3 Br 0.58481(5) -0.34146(4) 0.93450(3) 0.03114(11) Uani 1 1 d . . . Br4 Br 0.63327(5) -0.13910(4) 0.72318(3) 0.02642(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0202(17) 0.0254(18) 0.0155(17) 0.0077(14) -0.0078(13) -0.0040(14) C2 0.0157(16) 0.0275(18) 0.0157(17) 0.0044(14) -0.0071(12) -0.0014(13) C3 0.0162(16) 0.0318(19) 0.0146(17) 0.0072(15) -0.0038(12) -0.0039(14) C4 0.0216(18) 0.031(2) 0.0184(18) 0.0088(15) -0.0087(13) -0.0084(15) C5 0.0256(18) 0.0197(17) 0.0216(19) 0.0081(14) -0.0108(14) -0.0034(14) C6 0.0206(17) 0.0212(17) 0.0170(17) 0.0027(14) -0.0049(13) -0.0033(13) C7 0.033(2) 0.029(2) 0.031(2) 0.0008(17) -0.0076(17) -0.0063(17) C8 0.039(2) 0.026(2) 0.040(3) -0.0020(19) -0.0046(19) 0.0029(17) C9 0.030(2) 0.029(2) 0.034(2) 0.0070(18) -0.0020(17) 0.0095(17) C10 0.033(2) 0.029(2) 0.033(2) 0.0022(18) -0.0100(17) -0.0080(17) C11 0.037(2) 0.032(2) 0.020(2) -0.0018(16) -0.0072(16) -0.0045(17) C12 0.029(2) 0.034(2) 0.0144(18) 0.0028(16) -0.0019(14) -0.0024(16) N1 0.0248(16) 0.0265(16) 0.0174(15) 0.0034(13) -0.0058(12) 0.0000(13) N2 0.0185(15) 0.0328(18) 0.0238(17) 0.0079(14) -0.0042(12) 0.0006(13) N3 0.0214(15) 0.0317(17) 0.0200(16) 0.0113(14) -0.0064(12) -0.0057(13) N4 0.0209(15) 0.0254(16) 0.0163(15) 0.0073(12) -0.0050(11) -0.0021(12) O1 0.0192(12) 0.0258(13) 0.0148(12) 0.0078(10) -0.0043(9) 0.0014(10) O2 0.0205(12) 0.0331(15) 0.0138(12) 0.0088(11) -0.0041(9) 0.0045(11) O3 0.034(2) 0.220(7) 0.037(2) 0.062(3) -0.0135(16) -0.038(3) O4 0.0217(15) 0.083(3) 0.058(2) 0.042(2) -0.0195(14) -0.0141(16) O5 0.0240(15) 0.0496(19) 0.0440(19) 0.0211(16) -0.0107(13) -0.0135(13) O6 0.046(3) 0.073(4) 0.321(11) -0.094(5) 0.011(4) -0.017(2) Cl1 0.0168(4) 0.0348(5) 0.0288(5) 0.0122(4) -0.0050(3) -0.0049(4) Co1 0.0159(2) 0.0237(3) 0.0129(2) 0.00743(19) -0.00398(17) 0.00001(18) Br1 0.02181(19) 0.0366(2) 0.01464(18) 0.00664(15) -0.00206(13) -0.00260(15) Br2 0.0235(2) 0.0403(2) 0.0235(2) 0.01978(17) -0.00546(14) -0.00423(16) Br3 0.0407(2) 0.02164(19) 0.0285(2) 0.00887(16) -0.00888(16) 0.00186(16) Br4 0.0306(2) 0.0272(2) 0.01826(19) 0.00117(15) -0.00422(14) 0.00502(15) _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 C1 O1 1.330(4) . ? C1 C6 1.387(5) . ? C1 C2 1.405(5) . ? C2 O2 1.342(4) . ? C2 C3 1.390(5) . ? C3 C4 1.404(5) . ? C3 Br1 1.888(4) . ? C4 C5 1.388(6) . ? C4 Br2 1.891(4) . ? C5 C6 1.398(5) . ? C5 Br3 1.897(4) . ? C6 Br4 1.890(4) . ? C7 N1 1.481(5) . ? C7 C8 1.513(6) . ? C8 C9 1.523(7) . ? C9 N2 1.490(5) . ? C10 N3 1.489(6) . ? C10 C11 1.512(6) . ? C11 C12 1.515(6) . ? C12 N4 1.487(5) . ? N1 Co1 1.959(3) . ? N2 Co1 1.975(3) . ? N3 Co1 1.979(3) . ? N4 Co1 1.957(3) . ? O1 Co1 1.890(3) . ? O2 Co1 1.912(3) . ? O3 Cl1 1.412(4) . ? O4 Cl1 1.411(3) . ? O5 Cl1 1.430(3) . ? O6 Cl1 1.376(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 123.4(3) . . ? O1 C1 C2 117.1(3) . . ? C6 C1 C2 119.6(3) . . ? O2 C2 C3 124.0(3) . . ? O2 C2 C1 116.9(3) . . ? C3 C2 C1 119.1(3) . . ? C2 C3 C4 121.1(3) . . ? C2 C3 Br1 116.8(3) . . ? C4 C3 Br1 122.1(3) . . ? C5 C4 C3 119.4(3) . . ? C5 C4 Br2 121.0(3) . . ? C3 C4 Br2 119.6(3) . . ? C4 C5 C6 119.6(3) . . ? C4 C5 Br3 120.1(3) . . ? C6 C5 Br3 120.3(3) . . ? C1 C6 C5 121.1(3) . . ? C1 C6 Br4 116.3(3) . . ? C5 C6 Br4 122.6(3) . . ? N1 C7 C8 110.7(3) . . ? C7 C8 C9 113.7(4) . . ? N2 C9 C8 111.7(3) . . ? N3 C10 C11 112.1(3) . . ? C10 C11 C12 113.6(3) . . ? N4 C12 C11 111.7(3) . . ? C7 N1 Co1 121.9(2) . . ? C9 N2 Co1 121.1(2) . . ? C10 N3 Co1 117.4(2) . . ? C12 N4 Co1 115.7(2) . . ? C1 O1 Co1 109.3(2) . . ? C2 O2 Co1 108.4(2) . . ? O6 Cl1 O4 113.8(4) . . ? O6 Cl1 O3 105.7(5) . . ? O4 Cl1 O3 107.5(3) . . ? O6 Cl1 O5 110.6(3) . . ? O4 Cl1 O5 111.9(2) . . ? O3 Cl1 O5 106.9(3) . . ? O1 Co1 O2 87.00(11) . . ? O1 Co1 N4 91.04(12) . . ? O2 Co1 N4 177.84(13) . . ? O1 Co1 N1 86.38(13) . . ? O2 Co1 N1 88.28(13) . . ? N4 Co1 N1 92.52(14) . . ? O1 Co1 N2 175.15(13) . . ? O2 Co1 N2 88.33(13) . . ? N4 Co1 N2 93.64(14) . . ? N1 Co1 N2 92.16(15) . . ? O1 Co1 N3 89.40(14) . . ? O2 Co1 N3 88.91(13) . . ? N4 Co1 N3 90.15(13) . . ? N1 Co1 N3 175.05(13) . . ? N2 Co1 N3 91.83(15) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.182 _refine_diff_density_min -1.443 _refine_diff_density_rms 0.134 data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 909987' #TrackingRef 'complex3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H32 Br4 Co N5 O6' _chemical_formula_weight 781.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.136(6) _cell_length_b 8.720(3) _cell_length_c 19.343(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.925(2) _cell_angle_gamma 90.00 _cell_volume 2617.2(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8259 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour Green-red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 6.804 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2811 _exptl_absorpt_correction_T_max 0.5494 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 10876 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5962 _reflns_number_gt 4243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0108P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 5962 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 Br2 Br 0.64082(2) 0.24828(4) 0.50067(2) 0.02092(10) Uani 1 1 d . . . Br1 Br 0.45586(2) 0.10282(4) 0.39573(2) 0.02202(10) Uani 1 1 d . . . Br3 Br 0.63432(2) 0.45918(4) 0.64234(2) 0.02057(10) Uani 1 1 d . . . Br4 Br 0.44531(2) 0.51233(4) 0.67770(2) 0.02106(10) Uani 1 1 d . . . Co1 Co 0.21634(3) 0.25311(5) 0.49607(3) 0.01221(11) Uani 1 1 d . . . O5 O -0.06614(16) 0.3677(3) 0.46730(14) 0.0227(6) Uani 1 1 d . . . O3 O -0.04799(16) 0.1436(3) 0.51808(14) 0.0266(7) Uani 1 1 d . . . O2 O 0.30331(14) 0.2044(3) 0.45003(13) 0.0175(6) Uani 1 1 d . . . O1 O 0.30094(14) 0.3658(2) 0.56383(12) 0.0140(5) Uani 1 1 d . . . O4 O -0.17541(16) 0.2445(3) 0.48549(16) 0.0321(7) Uani 1 1 d . . . O6 O 0.22855(18) -0.0153(3) 0.32592(16) 0.0371(8) Uani 1 1 d . . . H6 H 0.2783 -0.0225 0.3540 0.056 Uiso 1 1 calc R . . N4 N 0.13132(17) 0.3023(3) 0.54769(15) 0.0144(7) Uani 1 1 d . . . H4A H 0.1084 0.3973 0.5329 0.017 Uiso 1 1 calc R . . H4B H 0.0872 0.2321 0.5349 0.017 Uiso 1 1 calc R . . N5 N -0.09672(19) 0.2525(3) 0.49033(17) 0.0189(7) Uani 1 1 d . . . N2 N 0.13622(17) 0.1345(3) 0.42012(15) 0.0152(7) Uani 1 1 d . . . H2A H 0.1687 0.0891 0.3934 0.018 Uiso 1 1 calc R . . H2B H 0.1155 0.0563 0.4427 0.018 Uiso 1 1 calc R . . C8 C 0.0783(2) 0.3546(4) 0.33428(19) 0.0187(9) Uani 1 1 d . . . C2 C 0.3797(2) 0.2554(4) 0.49075(19) 0.0123(8) Uani 1 1 d . . . C7 C 0.1069(2) 0.4775(4) 0.39187(18) 0.0168(8) Uani 1 1 d . . . H7A H 0.1090 0.5776 0.3683 0.020 Uiso 1 1 calc R . . H7B H 0.0637 0.4853 0.4195 0.020 Uiso 1 1 calc R . . N1 N 0.19282(18) 0.4454(3) 0.44239(15) 0.0149(7) Uani 1 1 d . . . H1A H 0.2043 0.5236 0.4756 0.018 Uiso 1 1 calc R . . H1B H 0.2327 0.4534 0.4165 0.018 Uiso 1 1 calc R . . N3 N 0.25074(18) 0.0676(3) 0.55478(16) 0.0176(7) Uani 1 1 d . . . H3A H 0.2070 -0.0031 0.5409 0.021 Uiso 1 1 calc R . . H3B H 0.2984 0.0268 0.5442 0.021 Uiso 1 1 calc R . . C13 C 0.1965(2) 0.1470(4) 0.66093(19) 0.0165(8) Uani 1 1 d . . . C14 C 0.1648(2) 0.3036(4) 0.62755(19) 0.0178(8) Uani 1 1 d . . . H14A H 0.1186 0.3404 0.6481 0.021 Uiso 1 1 calc R . . H14B H 0.2130 0.3777 0.6414 0.021 Uiso 1 1 calc R . . C4 C 0.5349(2) 0.2868(4) 0.5211(2) 0.0147(8) Uani 1 1 d . . . C12 C 0.2712(2) 0.0863(4) 0.6341(2) 0.0206(9) Uani 1 1 d . . . H12A H 0.3205 0.1576 0.6499 0.025 Uiso 1 1 calc R . . H12B H 0.2895 -0.0142 0.6571 0.025 Uiso 1 1 calc R . . C1 C 0.3775(2) 0.3429(4) 0.55174(19) 0.0133(8) Uani 1 1 d . . . C6 C 0.4546(2) 0.4005(4) 0.59626(19) 0.0147(8) Uani 1 1 d . . . C10 C 0.1448(2) 0.3351(4) 0.2917(2) 0.0261(10) Uani 1 1 d . . . H10A H 0.1251 0.2556 0.2550 0.039 Uiso 1 1 calc R . . H10B H 0.2002 0.3047 0.3243 0.039 Uiso 1 1 calc R . . H10C H 0.1515 0.4323 0.2684 0.039 Uiso 1 1 calc R . . C16 C 0.2311(2) 0.1708(5) 0.74154(19) 0.0279(10) Uani 1 1 d . . . H16A H 0.1849 0.2098 0.7607 0.042 Uiso 1 1 calc R . . H16B H 0.2785 0.2450 0.7512 0.042 Uiso 1 1 calc R . . H16C H 0.2521 0.0729 0.7647 0.042 Uiso 1 1 calc R . . C9 C 0.0603(2) 0.2045(4) 0.36795(19) 0.0179(8) Uani 1 1 d . . . H9A H 0.0151 0.2232 0.3928 0.021 Uiso 1 1 calc R . . H9B H 0.0369 0.1297 0.3290 0.021 Uiso 1 1 calc R . . C3 C 0.4579(2) 0.2266(4) 0.47688(19) 0.0138(8) Uani 1 1 d . . . C15 C 0.1216(2) 0.0313(4) 0.6454(2) 0.0228(9) Uani 1 1 d . . . H15A H 0.0995 0.0163 0.5933 0.034 Uiso 1 1 calc R . . H15B H 0.0755 0.0708 0.6644 0.034 Uiso 1 1 calc R . . H15C H 0.1423 -0.0668 0.6684 0.034 Uiso 1 1 calc R . . C11 C -0.0081(2) 0.4075(5) 0.2832(2) 0.0322(11) Uani 1 1 d . . . H11A H -0.0284 0.3307 0.2453 0.048 Uiso 1 1 calc R . . H11B H 0.0001 0.5058 0.2614 0.048 Uiso 1 1 calc R . . H11C H -0.0508 0.4196 0.3103 0.048 Uiso 1 1 calc R . . C17 C 0.1899(3) -0.1637(5) 0.3142(2) 0.0408(12) Uani 1 1 d . . . H17A H 0.1900 -0.2094 0.3605 0.061 Uiso 1 1 calc R . . H17B H 0.2227 -0.2291 0.2900 0.061 Uiso 1 1 calc R . . H17C H 0.1304 -0.1543 0.2841 0.061 Uiso 1 1 calc R . . C5 C 0.5326(2) 0.3733(4) 0.58054(19) 0.0143(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br2 0.01129(18) 0.0214(2) 0.0325(2) -0.00037(17) 0.01001(16) 0.00194(16) Br1 0.0203(2) 0.0217(2) 0.0271(2) -0.00695(17) 0.01169(17) -0.00088(16) Br3 0.01086(18) 0.0277(2) 0.0214(2) 0.00153(17) 0.00137(15) -0.00379(16) Br4 0.0172(2) 0.0279(2) 0.0182(2) -0.00561(17) 0.00483(16) -0.00222(16) Co1 0.0091(2) 0.0110(2) 0.0171(3) -0.0018(2) 0.0044(2) -0.0017(2) O5 0.0209(14) 0.0141(13) 0.0366(17) 0.0016(12) 0.0135(13) -0.0020(11) O3 0.0187(14) 0.0168(14) 0.0411(18) 0.0083(13) 0.0030(13) 0.0037(12) O2 0.0123(13) 0.0185(13) 0.0220(15) -0.0054(11) 0.0051(11) -0.0018(11) O1 0.0104(13) 0.0148(13) 0.0172(14) -0.0028(10) 0.0045(11) -0.0023(10) O4 0.0102(14) 0.0249(15) 0.064(2) -0.0134(14) 0.0152(13) -0.0045(12) O6 0.0267(17) 0.0420(18) 0.041(2) -0.0058(15) 0.0059(14) -0.0022(14) N4 0.0138(15) 0.0126(15) 0.0164(17) 0.0021(13) 0.0037(13) -0.0013(13) N5 0.0152(17) 0.0152(17) 0.0272(19) -0.0094(14) 0.0072(14) -0.0026(14) N2 0.0142(16) 0.0124(15) 0.0213(18) -0.0022(13) 0.0088(14) -0.0039(13) C8 0.016(2) 0.022(2) 0.016(2) -0.0033(17) 0.0016(16) -0.0016(17) C2 0.0121(18) 0.0104(17) 0.014(2) 0.0027(15) 0.0021(15) -0.0027(14) C7 0.0155(19) 0.0164(19) 0.018(2) 0.0010(16) 0.0047(16) 0.0027(16) N1 0.0154(16) 0.0132(15) 0.0174(17) -0.0011(13) 0.0070(13) -0.0033(13) N3 0.0131(16) 0.0143(15) 0.0249(19) -0.0003(14) 0.0041(14) 0.0008(13) C13 0.0142(19) 0.0188(19) 0.016(2) 0.0037(16) 0.0033(16) -0.0040(16) C14 0.0138(19) 0.0193(19) 0.022(2) -0.0029(17) 0.0078(17) -0.0024(16) C4 0.0093(17) 0.0132(17) 0.024(2) 0.0052(16) 0.0080(16) 0.0042(15) C12 0.018(2) 0.0162(19) 0.025(2) 0.0030(17) 0.0010(17) -0.0006(16) C1 0.0125(18) 0.0094(17) 0.019(2) 0.0018(15) 0.0059(16) 0.0026(15) C6 0.0160(19) 0.0131(18) 0.017(2) 0.0034(15) 0.0080(16) -0.0004(15) C10 0.032(2) 0.030(2) 0.019(2) -0.0023(18) 0.0113(19) -0.0052(19) C16 0.024(2) 0.036(2) 0.022(2) 0.0015(19) 0.0037(19) -0.0052(19) C9 0.0119(18) 0.0205(19) 0.021(2) -0.0057(17) 0.0031(16) -0.0035(16) C3 0.0179(19) 0.0105(17) 0.015(2) 0.0010(15) 0.0082(16) -0.0003(15) C15 0.019(2) 0.022(2) 0.025(2) 0.0063(17) 0.0035(17) -0.0033(17) C11 0.027(2) 0.034(2) 0.029(3) 0.000(2) -0.004(2) 0.002(2) C17 0.039(3) 0.034(3) 0.048(3) 0.002(2) 0.010(2) 0.003(2) C5 0.0135(19) 0.0113(18) 0.015(2) 0.0041(15) -0.0005(16) -0.0042(15) _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 Br2 C4 1.887(3) . ? Br1 C3 1.898(3) . ? Br3 C5 1.900(3) . ? Br4 C6 1.893(4) . ? Co1 O1 1.888(2) . ? Co1 O2 1.905(2) . ? Co1 N4 1.953(3) . ? Co1 N1 1.954(3) . ? Co1 N2 1.964(3) . ? Co1 N3 1.967(3) . ? O5 N5 1.254(4) . ? O3 N5 1.256(4) . ? O2 C2 1.343(4) . ? O1 C1 1.334(4) . ? O4 N5 1.249(4) . ? O6 C17 1.427(5) . ? N4 C14 1.490(4) . ? N2 C9 1.488(4) . ? C8 C7 1.523(5) . ? C8 C9 1.525(5) . ? C8 C10 1.531(5) . ? C8 C11 1.542(5) . ? C2 C3 1.384(5) . ? C2 C1 1.413(5) . ? C7 N1 1.487(4) . ? N3 C12 1.488(4) . ? C13 C16 1.519(5) . ? C13 C12 1.531(5) . ? C13 C14 1.537(5) . ? C13 C15 1.539(5) . ? C4 C5 1.384(5) . ? C4 C3 1.402(5) . ? C1 C6 1.398(5) . ? C6 C5 1.393(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 87.44(10) . . ? O1 Co1 N4 90.36(11) . . ? O2 Co1 N4 177.27(11) . . ? O1 Co1 N1 85.44(11) . . ? O2 Co1 N1 90.19(11) . . ? N4 Co1 N1 91.25(12) . . ? O1 Co1 N2 174.55(11) . . ? O2 Co1 N2 87.20(11) . . ? N4 Co1 N2 95.03(12) . . ? N1 Co1 N2 93.59(12) . . ? O1 Co1 N3 89.50(11) . . ? O2 Co1 N3 87.67(11) . . ? N4 Co1 N3 90.69(12) . . ? N1 Co1 N3 174.59(12) . . ? N2 Co1 N3 91.28(12) . . ? C2 O2 Co1 109.1(2) . . ? C1 O1 Co1 109.2(2) . . ? C14 N4 Co1 115.2(2) . . ? O4 N5 O5 120.6(3) . . ? O4 N5 O3 119.6(3) . . ? O5 N5 O3 119.8(3) . . ? C9 N2 Co1 122.8(2) . . ? C7 C8 C9 110.3(3) . . ? C7 C8 C10 110.8(3) . . ? C9 C8 C10 112.2(3) . . ? C7 C8 C11 107.3(3) . . ? C9 C8 C11 106.6(3) . . ? C10 C8 C11 109.4(3) . . ? O2 C2 C3 124.4(3) . . ? O2 C2 C1 116.0(3) . . ? C3 C2 C1 119.5(3) . . ? N1 C7 C8 112.9(3) . . ? C7 N1 Co1 121.4(2) . . ? C12 N3 Co1 117.0(2) . . ? C16 C13 C12 107.0(3) . . ? C16 C13 C14 107.2(3) . . ? C12 C13 C14 111.5(3) . . ? C16 C13 C15 109.7(3) . . ? C12 C13 C15 110.8(3) . . ? C14 C13 C15 110.3(3) . . ? N4 C14 C13 114.4(3) . . ? C5 C4 C3 119.3(3) . . ? C5 C4 Br2 120.2(3) . . ? C3 C4 Br2 120.5(3) . . ? N3 C12 C13 114.5(3) . . ? O1 C1 C6 123.3(3) . . ? O1 C1 C2 117.6(3) . . ? C6 C1 C2 119.1(3) . . ? C5 C6 C1 120.6(3) . . ? C5 C6 Br4 123.5(3) . . ? C1 C6 Br4 115.9(3) . . ? N2 C9 C8 115.1(3) . . ? C2 C3 C4 121.1(3) . . ? C2 C3 Br1 117.0(3) . . ? C4 C3 Br1 121.9(3) . . ? C4 C5 C6 120.4(3) . . ? C4 C5 Br3 121.5(3) . . ? C6 C5 Br3 118.2(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.595 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.136 data_Complex4 _database_code_depnum_ccdc_archive 'CCDC 909988' #TrackingRef 'complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 Br4 Cl Co N4 O6' _chemical_formula_weight 798.37 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 6.546(2) _cell_length_b 31.167(11) _cell_length_c 11.809(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.774(2) _cell_angle_gamma 90.00 _cell_volume 2330(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8545 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour greenish-red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 7.757 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3060 _exptl_absorpt_correction_T_max 0.6532 _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 5192 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2640 _reflns_number_gt 2231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.1130P)^2^+0.7815P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2640 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br2 Br 0.33850(9) -0.084366(17) 0.83782(5) 0.0331(2) Uani 1 1 d . . . Br1 Br 0.17985(9) 0.008474(19) 0.92174(5) 0.0319(2) Uani 1 1 d . . . Co1 Co 0.5000 0.12772(3) 0.7500 0.0236(3) Uani 1 2 d S . . Cl1 Cl 1.0000 0.26055(6) 0.7500 0.0334(4) Uani 1 2 d S . . O1 O 0.3722(6) 0.08414(10) 0.8182(3) 0.0231(7) Uani 1 1 d . . . C8 C 0.7245(8) 0.16472(18) 0.9602(5) 0.0294(11) Uani 1 1 d . . . N2 N 0.3706(7) 0.16908(15) 0.8351(4) 0.0309(10) Uani 1 1 d . . . H2A H 0.2952 0.1889 0.7831 0.037 Uiso 1 1 calc R . . H2B H 0.2775 0.1550 0.8687 0.037 Uiso 1 1 calc R . . C6 C 1.0694(9) 0.14759(19) 1.0822(5) 0.0362(13) Uani 1 1 d . . . H6 H 1.1836 0.1529 1.1486 0.043 Uiso 1 1 calc R . . N1 N 0.7386(7) 0.13260(14) 0.8875(4) 0.0260(9) Uani 1 1 d . . . C4 C 0.9108(8) 0.10798(18) 0.9085(5) 0.0326(11) Uani 1 1 d . . . H4 H 0.9189 0.0854 0.8557 0.039 Uiso 1 1 calc R . . O3 O 0.9549(16) 0.2300(3) 0.8265(8) 0.050(2) Uani 0.50 1 d P A 2 C5 C 1.0801(9) 0.1148(2) 1.0069(5) 0.0358(12) Uani 1 1 d . . . H5 H 1.2011 0.0967 1.0212 0.043 Uiso 1 1 calc R . . C7 C 0.8878(9) 0.17318(18) 1.0598(5) 0.0331(12) Uani 1 1 d . . . H7 H 0.8758 0.1959 1.1114 0.040 Uiso 1 1 calc R . . C1 C 0.4301(7) 0.04596(16) 0.7869(4) 0.0195(9) Uani 1 1 d . . . C9 C 0.5286(9) 0.1917(2) 0.9271(6) 0.0406(14) Uani 1 1 d . . . H9A H 0.4724 0.1964 0.9963 0.049 Uiso 1 1 calc R . . H9B H 0.5615 0.2199 0.8978 0.049 Uiso 1 1 calc R . . C2 C 0.3644(7) 0.00670(16) 0.8218(4) 0.0216(10) Uani 1 1 d . . . C3 C 0.4330(7) -0.03219(16) 0.7862(4) 0.0241(10) Uani 1 1 d . . . O4 O 1.154(2) 0.2547(4) 0.8692(9) 0.078(4) Uani 0.50 1 d P A 3 O2 O 0.795(2) 0.2545(4) 0.7673(15) 0.086(4) Uani 0.50 1 d P A 1 O5 O 1.022(2) 0.3033(3) 0.7147(8) 0.057(3) Uani 0.50 1 d P . . 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 Br2 0.0314(3) 0.0286(3) 0.0432(4) 0.00496(19) 0.0166(3) -0.0040(2) Br1 0.0291(3) 0.0381(4) 0.0371(4) 0.0039(2) 0.0239(2) 0.0003(2) Co1 0.0185(5) 0.0263(5) 0.0287(5) 0.000 0.0109(4) 0.000 Cl1 0.0308(9) 0.0297(10) 0.0410(10) 0.000 0.0117(8) 0.000 O1 0.0222(17) 0.0236(19) 0.0275(18) 0.0010(12) 0.0136(14) 0.0027(13) C8 0.028(3) 0.029(3) 0.034(3) 0.001(2) 0.014(2) 0.002(2) N2 0.023(2) 0.031(2) 0.041(3) -0.0010(18) 0.0115(19) 0.0023(17) C6 0.031(3) 0.039(3) 0.036(3) 0.001(2) 0.004(2) -0.007(2) N1 0.023(2) 0.029(2) 0.030(2) 0.0010(16) 0.0124(17) -0.0020(17) C4 0.024(2) 0.038(3) 0.037(3) -0.001(2) 0.011(2) -0.001(2) O3 0.051(6) 0.048(6) 0.053(5) 0.019(4) 0.018(4) -0.013(5) C5 0.022(2) 0.045(3) 0.041(3) 0.000(2) 0.009(2) -0.001(2) C7 0.042(3) 0.028(3) 0.030(3) -0.004(2) 0.011(2) -0.003(2) C1 0.016(2) 0.024(2) 0.020(2) -0.0012(16) 0.0082(17) 0.0030(17) C9 0.037(3) 0.033(3) 0.052(4) -0.011(3) 0.012(3) 0.000(2) C2 0.013(2) 0.034(3) 0.019(2) 0.0018(17) 0.0057(17) 0.0019(18) C3 0.016(2) 0.028(3) 0.028(3) 0.0089(18) 0.0044(18) -0.0022(18) O4 0.095(9) 0.085(8) 0.037(6) -0.017(5) -0.014(6) 0.046(7) O2 0.061(7) 0.058(7) 0.165(13) -0.049(8) 0.077(8) -0.025(6) O5 0.080(8) 0.041(5) 0.044(7) 0.009(3) 0.006(6) -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 Br2 C3 1.895(5) . ? Br1 C2 1.893(5) . ? Co1 O1 1.880(4) . ? Co1 O1 1.880(4) 2_656 ? Co1 N1 1.951(4) 2_656 ? Co1 N1 1.951(4) . ? Co1 N2 1.955(5) 2_656 ? Co1 N2 1.955(5) . ? Cl1 O3 1.395(8) . ? Cl1 O3 1.395(8) 2_756 ? Cl1 O5 1.413(9) 2_756 ? Cl1 O5 1.413(9) . ? Cl1 O2 1.420(11) . ? Cl1 O2 1.420(11) 2_756 ? Cl1 O4 1.518(10) . ? Cl1 O4 1.518(10) 2_756 ? O1 C1 1.329(6) . ? C8 N1 1.338(7) . ? C8 C7 1.398(8) . ? C8 C9 1.498(8) . ? N2 C9 1.473(7) . ? C6 C5 1.368(9) . ? C6 C7 1.399(9) . ? N1 C4 1.334(7) . ? C4 C5 1.403(8) . ? C1 C2 1.394(7) . ? C1 C1 1.416(9) 2_656 ? C2 C3 1.394(7) . ? C3 C3 1.372(10) 2_656 ? O5 O5 0.95(2) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 87.5(2) . 2_656 ? O1 Co1 N1 93.64(17) . 2_656 ? O1 Co1 N1 92.81(16) 2_656 2_656 ? O1 Co1 N1 92.81(16) . . ? O1 Co1 N1 93.64(17) 2_656 . ? N1 Co1 N1 171.1(3) 2_656 . ? O1 Co1 N2 173.99(18) . 2_656 ? O1 Co1 N2 87.59(18) 2_656 2_656 ? N1 Co1 N2 83.14(18) 2_656 2_656 ? N1 Co1 N2 90.96(18) . 2_656 ? O1 Co1 N2 87.59(18) . . ? O1 Co1 N2 173.99(18) 2_656 . ? N1 Co1 N2 90.96(18) 2_656 . ? N1 Co1 N2 83.14(18) . . ? N2 Co1 N2 97.5(3) 2_656 . ? O3 Cl1 O3 93.8(9) . 2_756 ? O3 Cl1 O5 113.5(6) . 2_756 ? O3 Cl1 O5 152.7(6) 2_756 2_756 ? O3 Cl1 O5 152.7(6) . . ? O3 Cl1 O5 113.5(6) 2_756 . ? O5 Cl1 O5 39.2(9) 2_756 . ? O3 Cl1 O2 56.8(8) . . ? O3 Cl1 O2 111.4(6) 2_756 . ? O5 Cl1 O2 85.0(7) 2_756 . ? O5 Cl1 O2 109.8(8) . . ? O3 Cl1 O2 111.4(6) . 2_756 ? O3 Cl1 O2 56.8(8) 2_756 2_756 ? O5 Cl1 O2 109.8(8) 2_756 2_756 ? O5 Cl1 O2 85.0(7) . 2_756 ? O2 Cl1 O2 164.6(10) . 2_756 ? O3 Cl1 O4 61.1(7) . . ? O3 Cl1 O4 108.5(6) 2_756 . ? O5 Cl1 O4 86.2(6) 2_756 . ? O5 Cl1 O4 107.1(7) . . ? O2 Cl1 O4 106.1(9) . . ? O2 Cl1 O4 71.9(8) 2_756 . ? O3 Cl1 O4 108.5(6) . 2_756 ? O3 Cl1 O4 61.1(7) 2_756 2_756 ? O5 Cl1 O4 107.1(7) 2_756 2_756 ? O5 Cl1 O4 86.2(6) . 2_756 ? O2 Cl1 O4 71.9(9) . 2_756 ? O2 Cl1 O4 106.1(9) 2_756 2_756 ? O4 Cl1 O4 166.1(10) . 2_756 ? C1 O1 Co1 109.8(3) . . ? N1 C8 C7 121.2(5) . . ? N1 C8 C9 116.5(5) . . ? C7 C8 C9 122.3(5) . . ? C9 N2 Co1 112.3(3) . . ? C5 C6 C7 119.0(5) . . ? C4 N1 C8 120.3(5) . . ? C4 N1 Co1 124.7(4) . . ? C8 N1 Co1 114.9(4) . . ? N1 C4 C5 121.3(5) . . ? C6 C5 C4 119.4(6) . . ? C8 C7 C6 118.8(5) . . ? O1 C1 C2 124.9(4) . . ? O1 C1 C1 116.5(3) . 2_656 ? C2 C1 C1 118.6(3) . 2_656 ? N2 C9 C8 108.6(5) . . ? C1 C2 C3 121.8(4) . . ? C1 C2 Br1 116.9(3) . . ? C3 C2 Br1 121.3(4) . . ? C3 C3 C2 119.6(3) 2_656 . ? C3 C3 Br2 120.89(16) 2_656 . ? C2 C3 Br2 119.5(4) . . ? O5 O5 Cl1 70.4(4) 2_756 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.743 _refine_diff_density_min -2.207 _refine_diff_density_rms 0.259 data_Complex5 _database_code_depnum_ccdc_archive 'CCDC 909989' #TrackingRef 'complex5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H40 Br8 Co2 N10 O12' _chemical_formula_weight 1730.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.152(8) _cell_length_b 12.333(3) _cell_length_c 30.405(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.404(5) _cell_angle_gamma 90.00 _cell_volume 11212(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30145 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6720 _exptl_absorpt_coefficient_mu 6.365 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2141 _exptl_absorpt_correction_T_max 0.3937 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 18530 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.55 _reflns_number_total 12557 _reflns_number_gt 8942 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0860P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 12557 _refine_ls_number_parameters 743 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co2 Co 0.18138(2) 0.03070(5) 0.160571(18) 0.02149(14) Uani 1 1 d . . . Br1 Br 0.128223(17) 0.27380(4) 0.003953(15) 0.02962(13) Uani 1 1 d . . . Br8 Br 0.043061(19) 0.06918(5) 0.055095(16) 0.03696(14) Uani 1 1 d . . . Br3 Br -0.03442(2) 0.24506(6) -0.114692(19) 0.05024(18) Uani 1 1 d . . . Br5 Br 0.12971(2) 0.36033(4) 0.225301(17) 0.03910(15) Uani 1 1 d . . . Br4 Br 0.007459(18) 0.03209(5) -0.161833(15) 0.03727(14) Uani 1 1 d . . . Br2 Br 0.02460(2) 0.36089(5) -0.02825(2) 0.04475(16) Uani 1 1 d . . . Co1 Co 0.15897(2) -0.04515(5) -0.084647(17) 0.01937(14) Uani 1 1 d . . . Br6 Br 0.02964(2) 0.43037(5) 0.17108(3) 0.0685(2) Uani 1 1 d . . . N1 N 0.19145(13) 0.0293(3) -0.12584(11) 0.0211(8) Uani 1 1 d . . . C12 C 0.32591(17) 0.0481(4) -0.07709(15) 0.0270(10) Uani 1 1 d . . . H12 H 0.3567 0.0510 -0.0654 0.032 Uiso 1 1 calc R . . O2 O 0.15191(11) 0.0847(2) -0.05321(9) 0.0225(7) Uani 1 1 d . . . C40 C 0.12109(18) -0.0044(4) 0.22765(14) 0.0285(11) Uani 1 1 d . . . H40 H 0.1248 0.0701 0.2353 0.034 Uiso 1 1 calc R . . N8 N 0.19363(14) -0.1117(3) 0.13741(11) 0.0244(9) Uani 1 1 d . . . H8A H 0.1887 -0.1106 0.1069 0.029 Uiso 1 1 calc R . . H8B H 0.2231 -0.1297 0.1459 0.029 Uiso 1 1 calc R . . O4 O 0.16642(12) 0.1653(2) 0.18292(9) 0.0260(7) Uani 1 1 d . . . C21 C 0.1234(2) -0.4523(4) -0.07723(18) 0.0403(14) Uani 1 1 d . . . H21 H 0.1210 -0.5260 -0.0862 0.048 Uiso 1 1 calc R . . C8 C 0.20473(18) 0.1241(4) -0.19135(14) 0.0296(11) Uani 1 1 d . . . H8 H 0.1928 0.1521 -0.2195 0.035 Uiso 1 1 calc R . . N2 N 0.21671(13) -0.0675(3) -0.05031(11) 0.0211(8) Uani 1 1 d . . . H2A H 0.2159 -0.0433 -0.0218 0.025 Uiso 1 1 calc R . . H2B H 0.2232 -0.1404 -0.0491 0.025 Uiso 1 1 calc R . . C43 C 0.11159(16) -0.2217(4) 0.20757(14) 0.0249(10) Uani 1 1 d . . . C27 C 0.10226(19) 0.2813(4) 0.17551(15) 0.0298(11) Uani 1 1 d . . . C11 C 0.31174(18) 0.0963(4) -0.11741(15) 0.0289(11) Uani 1 1 d . . . H11 H 0.3326 0.1330 -0.1330 0.035 Uiso 1 1 calc R . . C3 C 0.09205(16) 0.2092(4) -0.04430(13) 0.0218(9) Uani 1 1 d . . . O5 O 0.24230(14) 0.7613(3) 0.07682(11) 0.0384(9) Uani 1 1 d . . . C41 C 0.09148(17) -0.0663(4) 0.24877(15) 0.0296(11) Uani 1 1 d . . . H41 H 0.0747 -0.0341 0.2698 0.036 Uiso 1 1 calc R . . C32 C 0.24146(19) 0.1817(4) 0.05836(15) 0.0345(12) Uani 1 1 d . . . H32 H 0.2328 0.2068 0.0290 0.041 Uiso 1 1 calc R . . C7 C 0.17616(17) 0.0708(4) -0.16494(14) 0.0261(10) Uani 1 1 d . . . H7 H 0.1452 0.0647 -0.1755 0.031 Uiso 1 1 calc R . . N4 N 0.16095(14) -0.1822(3) -0.11748(11) 0.0245(8) Uani 1 1 d . . . H4A H 0.1444 -0.1760 -0.1450 0.029 Uiso 1 1 calc R . . H4B H 0.1900 -0.1982 -0.1214 0.029 Uiso 1 1 calc R . . C31 C 0.20952(18) 0.1316(4) 0.08193(14) 0.0277(11) Uani 1 1 d . . . H31 H 0.1798 0.1218 0.0679 0.033 Uiso 1 1 calc R . . C33 C 0.28448(19) 0.1943(4) 0.07735(16) 0.0348(12) Uani 1 1 d . . . H33 H 0.3058 0.2282 0.0614 0.042 Uiso 1 1 calc R . . C35 C 0.34056(19) 0.1633(4) 0.14499(17) 0.0374(13) Uani 1 1 d . . . H35 H 0.3642 0.1947 0.1314 0.045 Uiso 1 1 calc R . . C26 C 0.12611(16) 0.1932(4) 0.16284(14) 0.0235(10) Uani 1 1 d . . . C39 C 0.26325(17) 0.1093(3) 0.14320(14) 0.0239(10) Uani 1 1 d . . . O1 O 0.10280(11) -0.0156(2) -0.11804(9) 0.0232(7) Uani 1 1 d . . . C45 C 0.13380(18) -0.3681(4) 0.16236(16) 0.0311(11) Uani 1 1 d . . . H45 H 0.1315 -0.4419 0.1534 0.037 Uiso 1 1 calc R . . C36 C 0.34865(19) 0.1247(4) 0.18773(17) 0.0360(12) Uani 1 1 d . . . H36 H 0.3782 0.1274 0.2029 0.043 Uiso 1 1 calc R . . C19 C 0.11276(16) -0.3137(4) -0.02343(15) 0.0280(11) Uani 1 1 d . . . N5 N 0.22057(14) 0.0979(3) 0.12355(11) 0.0239(8) Uani 1 1 d . . . C24 C 0.12876(15) -0.2367(4) -0.05251(14) 0.0215(9) Uani 1 1 d . . . N6 N 0.23395(15) 0.0267(3) 0.20567(11) 0.0272(9) Uani 1 1 d . . . H6A H 0.2285 0.0663 0.2300 0.033 Uiso 1 1 calc R . . H6B H 0.2399 -0.0437 0.2146 0.033 Uiso 1 1 calc R . . C17 C 0.10476(18) -0.1679(4) 0.02674(15) 0.0327(12) Uani 1 1 d . . . H17 H 0.0965 -0.1417 0.0539 0.039 Uiso 1 1 calc R . . C44 C 0.10947(18) -0.3328(4) 0.19472(15) 0.0306(11) Uani 1 1 d . . . H44 H 0.0913 -0.3821 0.2085 0.037 Uiso 1 1 calc R . . C2 C 0.11102(15) 0.1220(3) -0.06529(13) 0.0197(9) Uani 1 1 d . . . N3 N 0.13207(13) -0.1290(3) -0.04164(11) 0.0223(8) Uani 1 1 d . . . C37 C 0.3139(2) 0.0811(4) 0.20965(16) 0.0362(13) Uani 1 1 d . . . H37 H 0.3198 0.0586 0.2397 0.043 Uiso 1 1 calc R . . C18 C 0.10068(18) -0.2753(4) 0.01660(16) 0.0329(12) Uani 1 1 d . . . H18 H 0.0896 -0.3242 0.0368 0.039 Uiso 1 1 calc R . . C1 C 0.08417(16) 0.0688(4) -0.10044(13) 0.0225(10) Uani 1 1 d . . . C34 C 0.29712(18) 0.1563(4) 0.12126(15) 0.0295(11) Uani 1 1 d . . . O6 O 0.21726(13) 0.9122(3) 0.04588(10) 0.0353(9) Uani 1 1 d . . . C13 C 0.29541(17) -0.0054(4) -0.05287(14) 0.0278(11) Uani 1 1 d . . . H13 H 0.3056 -0.0379 -0.0251 0.033 Uiso 1 1 calc R . . N7 N 0.14422(14) -0.0446(3) 0.19746(11) 0.0226(8) Uani 1 1 d . . . C16 C 0.12123(18) -0.0957(4) -0.00328(15) 0.0298(11) Uani 1 1 d . . . H16 H 0.1246 -0.0212 0.0044 0.036 Uiso 1 1 calc R . . O3 O 0.13138(11) 0.0430(2) 0.11645(9) 0.0245(7) Uani 1 1 d . . . C48 C 0.13963(16) -0.1527(4) 0.18686(13) 0.0221(10) Uani 1 1 d . . . O7 O 0.27598(14) 0.8331(4) 0.02573(12) 0.0492(11) Uani 1 1 d . . . C38 C 0.27221(17) 0.0717(4) 0.18736(14) 0.0261(10) Uani 1 1 d . . . C30 C 0.06585(18) 0.1564(4) 0.10378(15) 0.0287(11) Uani 1 1 d . . . N9 N 0.24527(15) 0.8361(3) 0.04942(12) 0.0305(10) Uani 1 1 d . . . C22 C 0.14039(19) -0.3753(4) -0.10513(16) 0.0332(12) Uani 1 1 d . . . H22 H 0.1500 -0.3972 -0.1323 0.040 Uiso 1 1 calc R . . C10 C 0.26689(17) 0.0913(4) -0.13540(14) 0.0231(10) Uani 1 1 d . . . C42 C 0.08685(18) -0.1746(4) 0.23879(15) 0.0309(11) Uani 1 1 d . . . H42 H 0.0669 -0.2179 0.2530 0.037 Uiso 1 1 calc R . . C47 C 0.16469(17) -0.1921(4) 0.15430(14) 0.0249(10) Uani 1 1 d . . . C25 C 0.10699(17) 0.1279(4) 0.12621(14) 0.0232(10) Uani 1 1 d . . . C28 C 0.06073(18) 0.3091(4) 0.15260(19) 0.0358(12) Uani 1 1 d . . . C15 C 0.23646(16) 0.0378(3) -0.11096(13) 0.0190(9) Uani 1 1 d . . . C46 C 0.16189(17) -0.2992(4) 0.14209(14) 0.0276(11) Uani 1 1 d . . . H46 H 0.1788 -0.3262 0.1202 0.033 Uiso 1 1 calc R . . C20 C 0.11052(19) -0.4226(4) -0.03763(18) 0.0356(12) Uani 1 1 d . . . H20 H 0.0998 -0.4764 -0.0192 0.043 Uiso 1 1 calc R . . C23 C 0.14277(17) -0.2680(4) -0.09229(14) 0.0262(10) Uani 1 1 d . . . C14 C 0.25151(16) -0.0101(3) -0.06970(13) 0.0211(9) Uani 1 1 d . . . C5 C 0.02299(16) 0.1940(4) -0.09374(14) 0.0282(11) Uani 1 1 d . . . C6 C 0.04162(17) 0.1058(4) -0.11430(13) 0.0283(11) Uani 1 1 d . . . C9 C 0.24891(18) 0.1359(4) -0.17716(14) 0.0288(11) Uani 1 1 d . . . H9 H 0.2677 0.1734 -0.1948 0.035 Uiso 1 1 calc R . . C4 C 0.04899(16) 0.2454(4) -0.05828(15) 0.0264(10) Uani 1 1 d . . . Br7 Br -0.01408(2) 0.28064(6) 0.08599(2) 0.05609(19) Uani 1 1 d . . . C29 C 0.04246(18) 0.2458(4) 0.11689(17) 0.0327(12) Uani 1 1 d . . . N10 N 0.26965(15) 0.7383(3) 0.20424(12) 0.0295(10) Uani 1 1 d . . . O8 O 0.28033(13) 0.7951(3) 0.17263(11) 0.0388(9) Uani 1 1 d . . . O10 O 0.28237(15) 0.6430(3) 0.20938(11) 0.0448(10) Uani 1 1 d . . . O9 O 0.24543(14) 0.7815(3) 0.23012(11) 0.0400(9) Uani 1 1 d . . . O11 O 0.08798(14) 0.8486(3) 0.81028(11) 0.0407(10) Uani 1 1 d . . . H11A H 0.0806 0.8913 0.8296 0.061 Uiso 1 1 calc R . . C49 C 0.0522(3) 0.7782(6) 0.7965(3) 0.075(2) Uani 1 1 d . . . H49A H 0.0584 0.7067 0.8101 0.112 Uiso 1 1 calc R . . H49B H 0.0487 0.7712 0.7642 0.112 Uiso 1 1 calc R . . H49C H 0.0247 0.8075 0.8058 0.112 Uiso 1 1 calc R . . O12 O 0.4617(5) 0.0902(9) 0.2254(3) 0.190(5) Uani 1 1 d . . . H12A H 0.4540 0.1347 0.2439 0.285 Uiso 1 1 calc R . . C50 C 0.4685(6) 0.1471(12) 0.1848(5) 0.231(11) Uani 1 1 d . . . H50A H 0.4479 0.2087 0.1804 0.347 Uiso 1 1 calc R . . H50B H 0.4627 0.0974 0.1595 0.347 Uiso 1 1 calc R . . H50C H 0.4994 0.1733 0.1871 0.347 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 Co2 0.0290(4) 0.0154(3) 0.0203(3) 0.0008(2) 0.0044(2) 0.0010(3) Br1 0.0319(3) 0.0247(3) 0.0318(2) -0.00738(18) 0.00219(19) -0.0005(2) Br8 0.0313(3) 0.0422(3) 0.0364(3) -0.0033(2) 0.0006(2) 0.0025(2) Br3 0.0288(3) 0.0666(4) 0.0529(3) -0.0109(3) -0.0040(3) 0.0198(3) Br5 0.0524(4) 0.0226(3) 0.0454(3) -0.0105(2) 0.0181(3) -0.0054(2) Br4 0.0257(3) 0.0532(4) 0.0314(2) -0.0092(2) -0.0022(2) -0.0002(2) Br2 0.0318(3) 0.0357(3) 0.0678(4) -0.0179(3) 0.0104(3) 0.0065(2) Co1 0.0209(3) 0.0161(3) 0.0213(3) 0.0005(2) 0.0036(2) 0.0002(2) Br6 0.0389(4) 0.0337(4) 0.1343(7) -0.0322(4) 0.0172(4) 0.0051(3) N1 0.027(2) 0.0159(19) 0.0216(17) 0.0022(14) 0.0063(15) 0.0001(16) C12 0.024(3) 0.025(3) 0.033(2) -0.0074(19) 0.007(2) -0.002(2) O2 0.0262(19) 0.0150(16) 0.0251(15) -0.0028(12) -0.0011(13) 0.0003(13) C40 0.043(3) 0.020(2) 0.023(2) 0.0019(18) 0.002(2) -0.001(2) N8 0.032(2) 0.023(2) 0.0197(17) 0.0013(15) 0.0058(15) 0.0024(17) O4 0.033(2) 0.0177(17) 0.0274(15) -0.0032(12) 0.0036(14) 0.0025(14) C21 0.049(4) 0.018(3) 0.054(3) -0.004(2) 0.005(3) -0.004(2) C8 0.045(3) 0.023(3) 0.022(2) 0.0022(18) 0.007(2) -0.006(2) N2 0.024(2) 0.0171(19) 0.0233(17) -0.0011(14) 0.0056(15) 0.0032(16) C43 0.022(3) 0.027(3) 0.024(2) 0.0001(18) 0.0006(18) 0.000(2) C27 0.041(3) 0.015(2) 0.035(2) -0.0047(19) 0.012(2) -0.002(2) C11 0.031(3) 0.022(2) 0.036(2) -0.007(2) 0.014(2) -0.008(2) C3 0.026(3) 0.018(2) 0.022(2) -0.0001(17) 0.0048(17) -0.0023(19) O5 0.058(3) 0.031(2) 0.0287(17) 0.0054(15) 0.0124(17) 0.0171(18) C41 0.029(3) 0.035(3) 0.025(2) 0.0015(19) 0.0034(19) 0.006(2) C32 0.047(4) 0.031(3) 0.027(2) 0.008(2) 0.011(2) 0.003(3) C7 0.030(3) 0.023(2) 0.024(2) -0.0034(17) -0.0004(19) 0.002(2) N4 0.027(2) 0.021(2) 0.0256(18) -0.0023(15) 0.0057(16) 0.0003(17) C31 0.037(3) 0.023(2) 0.023(2) 0.0005(18) 0.006(2) 0.000(2) C33 0.041(3) 0.029(3) 0.037(3) 0.002(2) 0.020(2) -0.003(2) C35 0.032(3) 0.033(3) 0.048(3) -0.011(2) 0.007(2) -0.003(2) C26 0.028(3) 0.016(2) 0.028(2) 0.0046(17) 0.0107(19) -0.0059(19) C39 0.032(3) 0.012(2) 0.028(2) -0.0018(17) 0.0064(19) -0.0034(19) O1 0.0241(19) 0.0205(17) 0.0244(14) -0.0032(12) 0.0014(13) 0.0014(13) C45 0.035(3) 0.020(2) 0.039(3) -0.006(2) 0.005(2) 0.001(2) C36 0.025(3) 0.035(3) 0.047(3) -0.008(2) -0.001(2) -0.004(2) C19 0.023(3) 0.023(3) 0.038(2) 0.007(2) 0.002(2) -0.001(2) N5 0.031(2) 0.0163(19) 0.0257(18) 0.0031(15) 0.0078(16) -0.0007(17) C24 0.015(2) 0.019(2) 0.030(2) 0.0019(17) 0.0004(17) -0.0004(18) N6 0.039(3) 0.021(2) 0.0224(18) 0.0024(15) 0.0053(17) 0.0000(18) C17 0.038(3) 0.033(3) 0.029(2) 0.002(2) 0.013(2) 0.005(2) C44 0.037(3) 0.019(2) 0.035(2) 0.0039(19) 0.002(2) -0.006(2) C2 0.022(2) 0.016(2) 0.0209(19) 0.0062(16) 0.0033(17) -0.0008(18) N3 0.019(2) 0.019(2) 0.0288(18) 0.0025(15) 0.0034(15) -0.0012(16) C37 0.049(4) 0.029(3) 0.030(2) -0.003(2) -0.001(2) -0.004(3) C18 0.032(3) 0.026(3) 0.042(3) 0.012(2) 0.009(2) -0.002(2) C1 0.028(3) 0.017(2) 0.022(2) 0.0022(17) 0.0027(18) -0.0027(19) C34 0.034(3) 0.023(3) 0.032(2) -0.0060(19) 0.007(2) 0.001(2) O6 0.050(3) 0.029(2) 0.0270(16) 0.0016(14) 0.0056(15) 0.0198(18) C13 0.034(3) 0.025(3) 0.024(2) -0.0025(18) 0.0023(19) -0.002(2) N7 0.034(2) 0.0170(19) 0.0166(16) -0.0004(14) 0.0034(15) 0.0003(17) C16 0.036(3) 0.023(3) 0.032(2) -0.0030(19) 0.009(2) 0.004(2) O3 0.0279(19) 0.0216(17) 0.0245(15) 0.0002(12) 0.0049(13) 0.0034(14) C48 0.023(3) 0.019(2) 0.024(2) 0.0031(17) -0.0005(18) 0.0005(19) O7 0.033(2) 0.077(3) 0.039(2) 0.0132(19) 0.0104(18) 0.011(2) C38 0.034(3) 0.017(2) 0.027(2) -0.0012(17) 0.003(2) 0.002(2) C30 0.029(3) 0.028(3) 0.030(2) 0.0044(19) 0.007(2) 0.000(2) N9 0.036(3) 0.034(2) 0.0206(18) -0.0026(16) -0.0004(17) 0.003(2) C22 0.039(3) 0.025(3) 0.037(3) -0.005(2) 0.010(2) -0.002(2) C10 0.030(3) 0.014(2) 0.026(2) -0.0031(17) 0.0086(19) -0.0021(19) C42 0.031(3) 0.033(3) 0.029(2) 0.006(2) 0.004(2) -0.005(2) C47 0.033(3) 0.022(2) 0.020(2) 0.0027(17) 0.0045(18) 0.003(2) C25 0.029(3) 0.018(2) 0.024(2) 0.0041(17) 0.0085(18) -0.002(2) C28 0.025(3) 0.022(3) 0.064(3) -0.003(2) 0.018(3) 0.000(2) C15 0.024(2) 0.011(2) 0.0231(19) -0.0030(16) 0.0066(17) -0.0014(18) C46 0.034(3) 0.021(2) 0.027(2) -0.0021(18) 0.001(2) 0.004(2) C20 0.035(3) 0.023(3) 0.051(3) 0.008(2) 0.012(2) -0.003(2) C23 0.025(3) 0.022(2) 0.030(2) 0.0024(18) 0.0004(19) 0.000(2) C14 0.026(3) 0.014(2) 0.025(2) -0.0029(16) 0.0067(18) -0.0011(18) C5 0.020(3) 0.035(3) 0.030(2) 0.007(2) 0.0049(19) 0.008(2) C6 0.031(3) 0.034(3) 0.020(2) 0.0053(19) 0.0043(18) -0.004(2) C9 0.043(3) 0.021(2) 0.025(2) 0.0006(18) 0.013(2) -0.005(2) C4 0.020(3) 0.022(2) 0.039(2) -0.0013(19) 0.012(2) 0.0016(19) Br7 0.0316(4) 0.0570(4) 0.0784(4) -0.0021(3) 0.0021(3) 0.0155(3) C29 0.025(3) 0.025(3) 0.051(3) 0.004(2) 0.015(2) 0.002(2) N10 0.035(3) 0.028(2) 0.0237(19) -0.0034(16) 0.0000(17) 0.0072(19) O8 0.043(2) 0.041(2) 0.0344(18) 0.0099(16) 0.0130(16) 0.0087(18) O10 0.074(3) 0.022(2) 0.0394(19) 0.0019(15) 0.0093(19) 0.0123(19) O9 0.048(3) 0.045(2) 0.0290(17) -0.0068(16) 0.0131(16) 0.0103(19) O11 0.053(3) 0.037(2) 0.0322(19) -0.0080(15) 0.0048(17) -0.0018(19) C49 0.055(5) 0.073(5) 0.098(6) -0.054(4) 0.017(4) -0.014(4) O12 0.223(13) 0.177(10) 0.189(10) 0.009(8) 0.101(9) 0.046(9) C50 0.29(2) 0.180(15) 0.275(19) 0.135(14) 0.224(18) 0.085(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co2 O4 1.871(3) . ? Co2 O3 1.891(3) . ? Co2 N5 1.922(4) . ? Co2 N7 1.924(4) . ? Co2 N8 1.945(4) . ? Co2 N6 1.958(4) . ? Br1 C3 1.888(4) . ? Br8 C30 1.887(5) . ? Br3 C5 1.875(5) . ? Br5 C27 1.899(5) . ? Br4 C6 1.896(5) . ? Br2 C4 1.891(5) . ? Co1 O2 1.891(3) . ? Co1 O1 1.894(3) . ? Co1 N1 1.920(4) . ? Co1 N3 1.926(4) . ? Co1 N2 1.931(4) . ? Co1 N4 1.968(4) . ? Br6 C28 1.889(5) . ? N1 C7 1.321(5) . ? N1 C15 1.378(6) . ? C12 C11 1.380(7) . ? C12 C13 1.413(7) . ? O2 C2 1.323(5) . ? C40 N7 1.319(6) . ? C40 C41 1.393(7) . ? N8 C47 1.458(6) . ? O4 C26 1.333(6) . ? C21 C20 1.362(7) . ? C21 C22 1.412(7) . ? C8 C9 1.354(7) . ? C8 C7 1.413(7) . ? N2 C14 1.452(6) . ? C43 C48 1.404(6) . ? C43 C42 1.406(7) . ? C43 C44 1.424(6) . ? C27 C26 1.385(7) . ? C27 C28 1.395(7) . ? C11 C10 1.393(7) . ? C3 C4 1.387(7) . ? C3 C2 1.409(6) . ? O5 N9 1.254(5) . ? C41 C42 1.373(7) . ? C32 C33 1.359(7) . ? C32 C31 1.415(7) . ? N4 C23 1.454(6) . ? C31 N5 1.333(5) . ? C33 C34 1.420(7) . ? C35 C36 1.376(7) . ? C35 C34 1.414(7) . ? C26 C25 1.434(6) . ? C39 N5 1.354(6) . ? C39 C38 1.413(6) . ? C39 C34 1.414(7) . ? O1 C1 1.328(5) . ? C45 C44 1.372(7) . ? C45 C46 1.398(7) . ? C36 C37 1.419(8) . ? C19 C18 1.397(7) . ? C19 C20 1.410(7) . ? C19 C24 1.424(6) . ? C24 N3 1.369(6) . ? C24 C23 1.387(6) . ? N6 C38 1.454(6) . ? C17 C18 1.362(7) . ? C17 C16 1.410(7) . ? C2 C1 1.416(6) . ? N3 C16 1.317(6) . ? C37 C38 1.354(7) . ? C1 C6 1.376(7) . ? O6 N9 1.258(5) . ? C13 C14 1.357(7) . ? N7 C48 1.374(5) . ? O3 C25 1.335(5) . ? C48 C47 1.407(6) . ? O7 N9 1.245(5) . ? C30 C25 1.382(7) . ? C30 C29 1.394(7) . ? C22 C23 1.379(7) . ? C10 C15 1.416(6) . ? C10 C9 1.425(6) . ? C47 C46 1.371(6) . ? C28 C29 1.392(7) . ? C15 C14 1.407(6) . ? C5 C4 1.400(7) . ? C5 C6 1.407(7) . ? Br7 C29 1.887(5) . ? N10 O10 1.239(5) . ? N10 O9 1.259(5) . ? N10 O8 1.264(5) . ? O11 C49 1.405(8) . ? O12 C50 1.456(13) . ? 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 O4 Co2 O3 88.79(14) . . ? O4 Co2 N5 91.43(15) . . ? O3 Co2 N5 92.52(15) . . ? O4 Co2 N7 91.78(15) . . ? O3 Co2 N7 88.93(15) . . ? N5 Co2 N7 176.50(17) . . ? O4 Co2 N8 176.92(16) . . ? O3 Co2 N8 89.25(15) . . ? N5 Co2 N8 91.03(16) . . ? N7 Co2 N8 85.81(16) . . ? O4 Co2 N6 88.81(15) . . ? O3 Co2 N6 176.70(15) . . ? N5 Co2 N6 85.28(16) . . ? N7 Co2 N6 93.40(16) . . ? N8 Co2 N6 93.24(16) . . ? O2 Co1 O1 87.53(13) . . ? O2 Co1 N1 91.43(15) . . ? O1 Co1 N1 93.11(15) . . ? O2 Co1 N3 91.53(15) . . ? O1 Co1 N3 92.37(15) . . ? N1 Co1 N3 173.88(16) . . ? O2 Co1 N2 89.99(14) . . ? O1 Co1 N2 177.10(15) . . ? N1 Co1 N2 85.46(16) . . ? N3 Co1 N2 89.18(15) . . ? O2 Co1 N4 175.24(16) . . ? O1 Co1 N4 88.67(15) . . ? N1 Co1 N4 91.64(15) . . ? N3 Co1 N4 85.77(16) . . ? N2 Co1 N4 93.88(16) . . ? C7 N1 C15 118.7(4) . . ? C7 N1 Co1 128.6(4) . . ? C15 N1 Co1 112.7(3) . . ? C11 C12 C13 121.1(5) . . ? C2 O2 Co1 108.4(3) . . ? N7 C40 C41 122.8(4) . . ? C47 N8 Co2 109.7(3) . . ? C26 O4 Co2 108.1(3) . . ? C20 C21 C22 121.2(5) . . ? C9 C8 C7 121.0(4) . . ? C14 N2 Co1 111.1(3) . . ? C48 C43 C42 117.1(4) . . ? C48 C43 C44 117.9(4) . . ? C42 C43 C44 125.0(5) . . ? C26 C27 C28 121.3(4) . . ? C26 C27 Br5 115.8(4) . . ? C28 C27 Br5 122.9(4) . . ? C12 C11 C10 120.2(4) . . ? C4 C3 C2 121.7(4) . . ? C4 C3 Br1 121.8(3) . . ? C2 C3 Br1 116.5(3) . . ? C42 C41 C40 119.0(5) . . ? C33 C32 C31 120.6(4) . . ? N1 C7 C8 121.6(5) . . ? C23 N4 Co1 108.7(3) . . ? N5 C31 C32 120.9(5) . . ? C32 C33 C34 119.2(5) . . ? C36 C35 C34 120.0(5) . . ? O4 C26 C27 123.4(4) . . ? O4 C26 C25 117.6(4) . . ? C27 C26 C25 119.0(4) . . ? N5 C39 C38 116.1(4) . . ? N5 C39 C34 122.5(4) . . ? C38 C39 C34 121.4(5) . . ? C1 O1 Co1 109.3(3) . . ? C44 C45 C46 122.2(5) . . ? C35 C36 C37 121.6(5) . . ? C18 C19 C20 125.6(5) . . ? C18 C19 C24 117.5(4) . . ? C20 C19 C24 116.9(4) . . ? C31 N5 C39 119.6(4) . . ? C31 N5 Co2 126.4(4) . . ? C39 N5 Co2 114.0(3) . . ? N3 C24 C23 117.4(4) . . ? N3 C24 C19 121.2(4) . . ? C23 C24 C19 121.4(4) . . ? C38 N6 Co2 109.4(3) . . ? C18 C17 C16 119.8(4) . . ? C45 C44 C43 119.6(5) . . ? O2 C2 C3 123.9(4) . . ? O2 C2 C1 118.1(4) . . ? C3 C2 C1 118.0(4) . . ? C16 N3 C24 119.8(4) . . ? C16 N3 Co1 127.5(3) . . ? C24 N3 Co1 112.4(3) . . ? C38 C37 C36 119.4(5) . . ? C17 C18 C19 120.0(5) . . ? O1 C1 C6 124.3(4) . . ? O1 C1 C2 115.9(4) . . ? C6 C1 C2 119.8(4) . . ? C39 C34 C35 117.5(4) . . ? C39 C34 C33 117.1(5) . . ? C35 C34 C33 125.3(5) . . ? C14 C13 C12 119.4(4) . . ? C40 N7 C48 118.8(4) . . ? C40 N7 Co2 128.6(3) . . ? C48 N7 Co2 112.4(3) . . ? N3 C16 C17 121.6(5) . . ? C25 O3 Co2 108.5(3) . . ? N7 C48 C43 122.0(4) . . ? N7 C48 C47 116.9(4) . . ? C43 C48 C47 121.0(4) . . ? C37 C38 C39 119.9(5) . . ? C37 C38 N6 124.9(4) . . ? C39 C38 N6 115.2(4) . . ? C25 C30 C29 121.0(5) . . ? C25 C30 Br8 117.1(4) . . ? C29 C30 Br8 121.9(4) . . ? O7 N9 O5 119.0(4) . . ? O7 N9 O6 121.0(4) . . ? O5 N9 O6 120.0(4) . . ? C23 C22 C21 119.0(5) . . ? C11 C10 C15 118.4(4) . . ? C11 C10 C9 124.8(4) . . ? C15 C10 C9 116.7(4) . . ? C41 C42 C43 120.2(5) . . ? C46 C47 C48 120.2(4) . . ? C46 C47 N8 125.4(4) . . ? C48 C47 N8 114.4(4) . . ? O3 C25 C30 125.1(4) . . ? O3 C25 C26 115.8(4) . . ? C30 C25 C26 119.1(4) . . ? C29 C28 C27 119.4(5) . . ? C29 C28 Br6 121.0(4) . . ? C27 C28 Br6 119.6(4) . . ? N1 C15 C14 116.9(4) . . ? N1 C15 C10 122.7(4) . . ? C14 C15 C10 120.4(4) . . ? C47 C46 C45 119.1(5) . . ? C21 C20 C19 121.2(5) . . ? C22 C23 C24 120.3(4) . . ? C22 C23 N4 124.0(4) . . ? C24 C23 N4 115.7(4) . . ? C13 C14 C15 120.3(4) . . ? C13 C14 N2 126.0(4) . . ? C15 C14 N2 113.5(4) . . ? C4 C5 C6 118.4(4) . . ? C4 C5 Br3 120.7(4) . . ? C6 C5 Br3 120.9(4) . . ? C1 C6 C5 122.1(4) . . ? C1 C6 Br4 117.9(4) . . ? C5 C6 Br4 120.0(4) . . ? C8 C9 C10 119.2(4) . . ? C3 C4 C5 120.0(4) . . ? C3 C4 Br2 120.1(3) . . ? C5 C4 Br2 119.9(4) . . ? C28 C29 C30 120.2(5) . . ? C28 C29 Br7 120.1(4) . . ? C30 C29 Br7 119.7(4) . . ? O10 N10 O9 121.2(4) . . ? O10 N10 O8 121.1(4) . . ? O9 N10 O8 117.8(4) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.959 _refine_diff_density_min -1.326 _refine_diff_density_rms 0.155 data_Complex6 _database_code_depnum_ccdc_archive 'CCDC 909990' #TrackingRef 'complex6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H36 Br8 Cl2 Co2 N8 O13' _chemical_formula_weight 1917.02 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.845(3) _cell_length_b 15.798(3) _cell_length_c 16.567(3) _cell_angle_alpha 115.922(1) _cell_angle_beta 103.402(1) _cell_angle_gamma 102.119(1) _cell_volume 3176.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23789 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 5.709 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.1625 _exptl_absorpt_correction_T_max 0.5474 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 25468 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14402 _reflns_number_gt 10183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0814P)^2^+2.2695P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 14402 _refine_ls_number_parameters 849 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1300 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Br6 Br 0.09409(5) 0.90387(4) 0.96206(4) 0.05678(15) Uani 1 1 d . . . Br4 Br 0.13035(4) 0.70615(5) 0.77466(4) 0.05993(15) Uani 1 1 d . . . Co2 Co 0.04660(4) 1.23056(4) 0.80671(4) 0.03498(13) Uani 1 1 d . . . Br7 Br 0.21161(4) 1.12649(5) 1.15805(4) 0.06002(15) Uani 1 1 d . . . Br3 Br -0.06730(4) 0.62271(5) 0.57737(5) 0.06923(18) Uani 1 1 d . . . Br5 Br 0.00740(5) 0.88967(4) 0.74936(3) 0.05775(15) Uani 1 1 d . . . Co1 Co 0.43007(4) 0.74503(4) 0.69899(4) 0.03784(14) Uani 1 1 d . . . Br8 Br 0.22296(6) 1.33177(4) 1.14466(4) 0.0765(2) Uani 1 1 d . . . Br1 Br 0.19734(5) 0.62890(6) 0.37538(4) 0.07220(19) Uani 1 1 d . . . Br2 Br -0.03122(5) 0.59419(5) 0.37819(4) 0.0760(2) Uani 1 1 d . . . Cl2 Cl 0.64424(10) 0.01283(11) 0.58037(10) 0.0611(3) Uani 1 1 d . . . Cl1 Cl 0.40477(11) 0.59237(10) 0.95131(10) 0.0613(3) Uani 1 1 d . . . O3 O 0.1143(2) 1.2760(2) 0.9373(2) 0.0432(7) Uani 1 1 d . . . O4 O 0.0321(2) 1.0985(2) 0.7784(2) 0.0404(7) Uani 1 1 d . . . O1 O 0.3197(2) 0.7418(2) 0.7359(2) 0.0410(7) Uani 1 1 d . . . O2 O 0.3450(2) 0.6946(3) 0.5719(2) 0.0459(7) Uani 1 1 d . . . C41 C 0.2000(5) 1.1442(5) 0.5473(5) 0.0680(16) Uani 1 1 d . . . H41 H 0.2485 1.1346 0.5210 0.082 Uiso 1 1 calc R . . N8 N 0.0533(3) 1.3666(3) 0.8386(2) 0.0407(8) Uani 1 1 d . . . N3 N 0.4505(3) 0.8823(3) 0.7297(3) 0.0412(8) Uani 1 1 d . . . N6 N -0.0142(3) 1.1805(3) 0.6690(2) 0.0389(8) Uani 1 1 d . . . N4 N 0.5185(3) 0.8083(3) 0.8334(3) 0.0419(8) Uani 1 1 d . . . C32 C 0.0712(3) 1.1006(3) 0.8610(3) 0.0368(9) Uani 1 1 d . . . O7 O 0.3488(5) 0.6213(6) 0.8930(4) 0.116(2) Uani 1 1 d . . . N7 N -0.0759(3) 1.2200(3) 0.8302(2) 0.0391(8) Uani 1 1 d . . . C35 C 0.1527(3) 1.1152(4) 1.0378(3) 0.0425(10) Uani 1 1 d . . . N2 N 0.5400(3) 0.7350(3) 0.6548(2) 0.0417(8) Uani 1 1 d . . . C1 C 0.2379(3) 0.7043(3) 0.6571(3) 0.0387(9) Uani 1 1 d . . . N1 N 0.4158(3) 0.6109(3) 0.6765(3) 0.0461(9) Uani 1 1 d . . . C22 C 0.5287(4) 1.0552(4) 0.8652(4) 0.0495(11) Uani 1 1 d . . . C30 C 0.5079(3) 0.9511(3) 0.8238(3) 0.0424(10) Uani 1 1 d . . . C17 C 0.5561(4) 0.6477(4) 0.6381(3) 0.0455(11) Uani 1 1 d . . . C59 C -0.0270(3) 1.3853(3) 0.8582(3) 0.0410(10) Uani 1 1 d . . . N5 N 0.1685(3) 1.2408(3) 0.7824(3) 0.0404(8) Uani 1 1 d . . . C14 C 0.6935(4) 0.6916(5) 0.5942(4) 0.0629(15) Uani 1 1 d . . . H14 H 0.7459 0.6792 0.5754 0.075 Uiso 1 1 calc R . . C31 C 0.1148(3) 1.1956(3) 0.9462(3) 0.0381(9) Uani 1 1 d . . . C34 C 0.1072(3) 1.0217(4) 0.9547(3) 0.0407(9) Uani 1 1 d . . . C55 C -0.0408(4) 1.4771(3) 0.8832(3) 0.0480(12) Uani 1 1 d . . . O8 O 0.4159(5) 0.6565(5) 1.0469(4) 0.117(2) Uani 1 1 d . . . C56 C 0.0316(5) 1.5511(4) 0.8853(4) 0.0576(14) Uani 1 1 d . . . H56 H 0.0247 1.6125 0.8988 0.069 Uiso 1 1 calc R . . C58 C 0.1210(4) 1.4392(4) 0.8437(3) 0.0474(11) Uani 1 1 d . . . H58 H 0.1765 1.4278 0.8311 0.057 Uiso 1 1 calc R . . C6 C 0.1434(3) 0.6844(3) 0.6577(3) 0.0431(10) Uani 1 1 d . . . C52 C -0.1789(4) 1.3190(4) 0.8805(3) 0.0505(12) Uani 1 1 d . . . C16 C 0.5983(4) 0.7972(4) 0.6393(3) 0.0479(11) Uani 1 1 d . . . H16 H 0.5876 0.8563 0.6493 0.057 Uiso 1 1 calc R . . C60 C -0.0962(3) 1.3062(3) 0.8557(3) 0.0403(10) Uani 1 1 d . . . O11 O 0.6384(6) -0.0227(9) 0.4872(5) 0.178(4) Uani 1 1 d . . . C15 C 0.6761(4) 0.7770(5) 0.6083(4) 0.0579(14) Uani 1 1 d . . . H15 H 0.7154 0.8222 0.5976 0.069 Uiso 1 1 calc R . . C5 C 0.0608(3) 0.6506(3) 0.5743(4) 0.0475(11) Uani 1 1 d . . . C28 C 0.5532(4) 0.7681(4) 0.8839(4) 0.0490(11) Uani 1 1 d . . . H28 H 0.5349 0.6985 0.8537 0.059 Uiso 1 1 calc R . . C19 C 0.4141(4) 0.9152(4) 0.6725(4) 0.0514(12) Uani 1 1 d . . . H19 H 0.3773 0.8692 0.6074 0.062 Uiso 1 1 calc R . . C49 C -0.1362(3) 1.1449(4) 0.8299(3) 0.0441(10) Uani 1 1 d . . . H49 H -0.1237 1.0852 0.8113 0.053 Uiso 1 1 calc R . . C48 C 0.1521(4) 1.1990(3) 0.6867(3) 0.0434(10) Uani 1 1 d . . . C36 C 0.1594(4) 1.2020(4) 1.0336(3) 0.0443(10) Uani 1 1 d . . . C9 C 0.4241(5) 0.4250(4) 0.6451(4) 0.0682(16) Uani 1 1 d . . . H9 H 0.4258 0.3628 0.6350 0.082 Uiso 1 1 calc R . . C47 C 0.0528(4) 1.1670(4) 0.6248(3) 0.0430(10) Uani 1 1 d . . . C25 C 0.6091(3) 0.9755(4) 0.9773(3) 0.0477(11) Uani 1 1 d . . . C51 C -0.2400(4) 1.2386(5) 0.8813(4) 0.0565(13) Uani 1 1 d . . . H51 H -0.2948 1.2438 0.8985 0.068 Uiso 1 1 calc R . . C18 C 0.4887(4) 0.5806(4) 0.6499(3) 0.0458(11) Uani 1 1 d . . . C50 C -0.2184(4) 1.1528(5) 0.8566(4) 0.0550(12) Uani 1 1 d . . . H50 H -0.2582 1.0996 0.8576 0.066 Uiso 1 1 calc R . . C2 C 0.2527(3) 0.6826(3) 0.5701(3) 0.0420(10) Uani 1 1 d . . . C7 C 0.3473(4) 0.5506(4) 0.6861(4) 0.0559(12) Uani 1 1 d . . . H7 H 0.2965 0.5706 0.7029 0.067 Uiso 1 1 calc R . . C33 C 0.0677(3) 1.0148(3) 0.8662(3) 0.0397(9) Uani 1 1 d . . . C57 C 0.1127(5) 1.5326(4) 0.8672(4) 0.0582(13) Uani 1 1 d . . . H57 H 0.1625 1.5824 0.8707 0.070 Uiso 1 1 calc R . . C45 C -0.1363(4) 1.1185(5) 0.5146(4) 0.0628(15) Uani 1 1 d . . . H45 H -0.2014 1.1038 0.4783 0.075 Uiso 1 1 calc R . . C40 C 0.2272(4) 1.1895(4) 0.6500(4) 0.0532(12) Uani 1 1 d . . . C23 C 0.5911(4) 1.1191(4) 0.9649(4) 0.0581(14) Uani 1 1 d . . . H23 H 0.6053 1.1882 0.9940 0.070 Uiso 1 1 calc R . . C44 C -0.0697(5) 1.1026(5) 0.4706(4) 0.0634(15) Uani 1 1 d . . . H44 H -0.0896 1.0756 0.4042 0.076 Uiso 1 1 calc R . . C26 C 0.6454(4) 0.9308(5) 1.0274(3) 0.0584(14) Uani 1 1 d . . . H26 H 0.6887 0.9705 1.0914 0.070 Uiso 1 1 calc R . . C12 C 0.6399(5) 0.5278(5) 0.5919(4) 0.0640(16) Uani 1 1 d . . . H12 H 0.6903 0.5099 0.5722 0.077 Uiso 1 1 calc R . . O12 O 0.7277(4) -0.0028(4) 0.6283(3) 0.0882(15) Uani 1 1 d . . . C27 C 0.6166(4) 0.8275(5) 0.9815(4) 0.0578(13) Uani 1 1 d . . . H27 H 0.6390 0.7971 1.0150 0.069 Uiso 1 1 calc R . . C3 C 0.1707(4) 0.6506(3) 0.4874(3) 0.0454(11) Uani 1 1 d . . . C38 C 0.3402(4) 1.2697(5) 0.8119(5) 0.0631(15) Uani 1 1 d . . . H38 H 0.4043 1.2963 0.8566 0.076 Uiso 1 1 calc R . . C46 C -0.1072(4) 1.1571(4) 0.6147(3) 0.0481(11) Uani 1 1 d . . . H46 H -0.1540 1.1663 0.6435 0.058 Uiso 1 1 calc R . . C53 C -0.1915(5) 1.4137(5) 0.9054(4) 0.0638(16) Uani 1 1 d . . . H53 H -0.2458 1.4240 0.9215 0.077 Uiso 1 1 calc R . . C24 C 0.6295(4) 1.0815(4) 1.0173(4) 0.0595(14) Uani 1 1 d . . . H24 H 0.6706 1.1254 1.0817 0.071 Uiso 1 1 calc R . . C11 C 0.5772(5) 0.4641(5) 0.6042(4) 0.0660(17) Uani 1 1 d . . . H11 H 0.5851 0.4037 0.5936 0.079 Uiso 1 1 calc R . . C42 C 0.1069(5) 1.1152(5) 0.4883(4) 0.0677(16) Uani 1 1 d . . . H42 H 0.0923 1.0871 0.4223 0.081 Uiso 1 1 calc R . . C37 C 0.2597(4) 1.2749(4) 0.8429(4) 0.0516(12) Uani 1 1 d . . . H37 H 0.2716 1.3035 0.9086 0.062 Uiso 1 1 calc R . . C13 C 0.6325(4) 0.6220(4) 0.6078(3) 0.0541(13) Uani 1 1 d . . . C29 C 0.5467(3) 0.9114(4) 0.8796(3) 0.0432(10) Uani 1 1 d . . . C8 C 0.3511(5) 0.4574(5) 0.6710(5) 0.0711(16) Uani 1 1 d . . . H8 H 0.3030 0.4165 0.6787 0.085 Uiso 1 1 calc R . . C10 C 0.4967(4) 0.4886(4) 0.6340(3) 0.0568(14) Uani 1 1 d . . . O9 O 0.5564(5) -0.0382(8) 0.5785(8) 0.171(4) Uani 1 1 d . . . C4 C 0.0766(4) 0.6356(3) 0.4905(3) 0.0501(12) Uani 1 1 d . . . C39 C 0.3233(4) 1.2258(5) 0.7165(5) 0.0657(15) Uani 1 1 d . . . H39 H 0.3755 1.2197 0.6951 0.079 Uiso 1 1 calc R . . C43 C 0.0288(4) 1.1269(4) 0.5254(3) 0.0525(12) Uani 1 1 d . . . C54 C -0.1263(5) 1.4886(4) 0.9061(4) 0.0594(14) Uani 1 1 d . . . H54 H -0.1374 1.5486 0.9218 0.071 Uiso 1 1 calc R . . C20 C 0.4299(5) 1.0169(4) 0.7082(4) 0.0621(14) Uani 1 1 d . . . H20 H 0.4023 1.0378 0.6672 0.074 Uiso 1 1 calc R . . C21 C 0.4861(5) 1.0868(4) 0.8036(5) 0.0614(14) Uani 1 1 d . . . H21 H 0.4957 1.1546 0.8272 0.074 Uiso 1 1 calc R . . O5 O 0.5005(5) 0.6068(6) 0.9472(5) 0.120(2) Uani 1 1 d . . . O6 O 0.3568(5) 0.4952(5) 0.9223(8) 0.177(4) Uani 1 1 d . . . O10 O 0.6603(6) 0.1138(5) 0.6201(8) 0.197(5) Uani 1 1 d . . . O13 O 0.4906(4) 0.7507(5) 0.3706(5) 0.109(2) Uani 1 1 d . . . H13A H 0.4736 0.7810 0.4155 0.163 Uiso 1 1 calc R . . C61 C 0.4118(6) 0.7042(9) 0.2857(7) 0.114(3) Uani 1 1 d . . . H61A H 0.3515 0.6887 0.2969 0.171 Uiso 1 1 calc R . . H61B H 0.4169 0.6431 0.2406 0.171 Uiso 1 1 calc R . . H61C H 0.4117 0.7480 0.2599 0.171 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 Br6 0.0810(4) 0.0560(3) 0.0523(3) 0.0356(2) 0.0273(3) 0.0379(3) Br4 0.0584(3) 0.0741(4) 0.0518(3) 0.0295(3) 0.0275(2) 0.0296(3) Co2 0.0423(3) 0.0368(3) 0.0272(3) 0.0158(2) 0.0116(2) 0.0189(2) Br7 0.0724(4) 0.0724(3) 0.0375(2) 0.0330(2) 0.0100(2) 0.0300(3) Br3 0.0431(3) 0.0621(3) 0.0817(4) 0.0239(3) 0.0143(3) 0.0196(2) Br5 0.0883(4) 0.0416(2) 0.0371(2) 0.0159(2) 0.0164(2) 0.0287(3) Co1 0.0416(3) 0.0425(3) 0.0290(3) 0.0152(2) 0.0124(2) 0.0218(3) Br8 0.1095(5) 0.0521(3) 0.0346(3) 0.0114(2) -0.0060(3) 0.0284(3) Br1 0.0882(4) 0.0953(5) 0.0374(3) 0.0330(3) 0.0187(3) 0.0474(4) Br2 0.0643(4) 0.0755(4) 0.0549(3) 0.0242(3) -0.0113(3) 0.0215(3) Cl2 0.0587(8) 0.0683(8) 0.0568(7) 0.0311(6) 0.0219(6) 0.0246(7) Cl1 0.0606(8) 0.0526(7) 0.0602(8) 0.0227(6) 0.0177(6) 0.0199(6) O3 0.0563(19) 0.0372(15) 0.0288(14) 0.0135(12) 0.0082(13) 0.0194(14) O4 0.0529(18) 0.0390(15) 0.0299(14) 0.0169(12) 0.0114(12) 0.0233(14) O1 0.0428(17) 0.0458(16) 0.0299(14) 0.0150(13) 0.0118(12) 0.0189(14) O2 0.0518(19) 0.0533(19) 0.0297(14) 0.0164(14) 0.0138(13) 0.0254(15) C41 0.091(5) 0.083(4) 0.069(4) 0.047(3) 0.055(4) 0.054(4) N8 0.052(2) 0.0405(19) 0.0305(17) 0.0178(15) 0.0123(15) 0.0210(17) N3 0.040(2) 0.045(2) 0.0378(18) 0.0180(16) 0.0146(15) 0.0198(16) N6 0.048(2) 0.0386(18) 0.0307(17) 0.0185(15) 0.0125(15) 0.0177(16) N4 0.042(2) 0.056(2) 0.0334(17) 0.0220(17) 0.0160(15) 0.0268(18) C32 0.043(2) 0.044(2) 0.0299(19) 0.0199(17) 0.0156(16) 0.0245(19) O7 0.115(5) 0.148(6) 0.096(4) 0.071(4) 0.024(3) 0.063(4) N7 0.047(2) 0.046(2) 0.0292(16) 0.0196(15) 0.0147(15) 0.0239(17) C35 0.044(2) 0.055(3) 0.034(2) 0.024(2) 0.0137(17) 0.023(2) N2 0.046(2) 0.051(2) 0.0303(17) 0.0186(16) 0.0138(15) 0.0261(18) C1 0.043(2) 0.038(2) 0.0305(19) 0.0159(17) 0.0073(16) 0.0177(18) N1 0.055(2) 0.045(2) 0.0337(18) 0.0159(16) 0.0125(16) 0.0243(19) C22 0.047(3) 0.046(3) 0.055(3) 0.020(2) 0.029(2) 0.018(2) C30 0.040(2) 0.045(2) 0.041(2) 0.0166(19) 0.0221(18) 0.0181(19) C17 0.052(3) 0.055(3) 0.029(2) 0.0159(19) 0.0135(18) 0.032(2) C59 0.051(3) 0.043(2) 0.0258(19) 0.0141(17) 0.0092(17) 0.023(2) N5 0.043(2) 0.0380(18) 0.0418(19) 0.0205(16) 0.0143(16) 0.0187(16) C14 0.058(3) 0.093(4) 0.043(3) 0.029(3) 0.022(2) 0.045(3) C31 0.040(2) 0.042(2) 0.034(2) 0.0194(18) 0.0132(17) 0.0184(18) C34 0.045(2) 0.049(2) 0.044(2) 0.028(2) 0.0216(19) 0.029(2) C55 0.068(3) 0.041(2) 0.029(2) 0.0134(18) 0.009(2) 0.027(2) O8 0.129(5) 0.134(5) 0.075(3) 0.034(3) 0.039(3) 0.066(4) C56 0.087(4) 0.047(3) 0.043(3) 0.024(2) 0.018(3) 0.035(3) C58 0.058(3) 0.048(3) 0.038(2) 0.023(2) 0.016(2) 0.020(2) C6 0.048(3) 0.038(2) 0.042(2) 0.0173(19) 0.0155(19) 0.020(2) C52 0.050(3) 0.066(3) 0.037(2) 0.021(2) 0.016(2) 0.035(2) C16 0.048(3) 0.061(3) 0.038(2) 0.026(2) 0.0165(19) 0.024(2) C60 0.045(2) 0.048(2) 0.0298(19) 0.0192(18) 0.0112(17) 0.023(2) O11 0.155(7) 0.331(13) 0.086(4) 0.109(6) 0.050(4) 0.146(8) C15 0.059(3) 0.085(4) 0.042(3) 0.034(3) 0.026(2) 0.034(3) C5 0.038(2) 0.038(2) 0.052(3) 0.014(2) 0.0069(19) 0.0159(19) C28 0.049(3) 0.061(3) 0.045(2) 0.030(2) 0.016(2) 0.028(2) C19 0.058(3) 0.059(3) 0.048(3) 0.031(2) 0.021(2) 0.029(2) C49 0.049(3) 0.045(2) 0.037(2) 0.0207(19) 0.0127(19) 0.019(2) C48 0.054(3) 0.043(2) 0.044(2) 0.024(2) 0.024(2) 0.025(2) C36 0.049(3) 0.046(2) 0.0286(19) 0.0136(18) 0.0073(17) 0.021(2) C9 0.093(5) 0.050(3) 0.055(3) 0.022(3) 0.017(3) 0.036(3) C47 0.055(3) 0.046(2) 0.036(2) 0.0231(19) 0.0186(19) 0.024(2) C25 0.035(2) 0.057(3) 0.038(2) 0.015(2) 0.0144(18) 0.012(2) C51 0.049(3) 0.075(4) 0.052(3) 0.031(3) 0.025(2) 0.030(3) C18 0.054(3) 0.047(2) 0.032(2) 0.0139(19) 0.0117(19) 0.027(2) C50 0.048(3) 0.071(3) 0.053(3) 0.036(3) 0.022(2) 0.020(3) C2 0.048(3) 0.038(2) 0.035(2) 0.0140(18) 0.0109(18) 0.0207(19) C7 0.067(3) 0.050(3) 0.056(3) 0.028(2) 0.026(3) 0.024(3) C33 0.048(2) 0.042(2) 0.031(2) 0.0163(18) 0.0154(17) 0.026(2) C57 0.076(4) 0.047(3) 0.049(3) 0.029(2) 0.016(3) 0.017(3) C45 0.056(3) 0.074(4) 0.039(3) 0.025(3) 0.002(2) 0.014(3) C40 0.061(3) 0.055(3) 0.066(3) 0.037(3) 0.036(3) 0.034(3) C23 0.061(3) 0.041(2) 0.055(3) 0.009(2) 0.030(3) 0.011(2) C44 0.075(4) 0.067(3) 0.033(2) 0.020(2) 0.013(2) 0.019(3) C26 0.045(3) 0.083(4) 0.033(2) 0.022(2) 0.0102(19) 0.020(3) C12 0.068(4) 0.080(4) 0.045(3) 0.021(3) 0.022(3) 0.052(3) O12 0.086(3) 0.096(4) 0.064(3) 0.031(3) 0.009(2) 0.042(3) C27 0.051(3) 0.083(4) 0.045(3) 0.036(3) 0.015(2) 0.030(3) C3 0.057(3) 0.038(2) 0.033(2) 0.0144(18) 0.0068(19) 0.023(2) C38 0.043(3) 0.063(3) 0.080(4) 0.035(3) 0.018(3) 0.024(3) C46 0.050(3) 0.056(3) 0.039(2) 0.026(2) 0.013(2) 0.020(2) C53 0.068(4) 0.074(4) 0.051(3) 0.023(3) 0.019(3) 0.052(3) C24 0.049(3) 0.056(3) 0.046(3) 0.009(2) 0.019(2) 0.005(2) C11 0.080(4) 0.060(3) 0.049(3) 0.015(3) 0.015(3) 0.046(3) C42 0.095(5) 0.083(4) 0.046(3) 0.035(3) 0.042(3) 0.046(4) C37 0.048(3) 0.054(3) 0.053(3) 0.027(2) 0.013(2) 0.023(2) C13 0.058(3) 0.070(3) 0.036(2) 0.019(2) 0.019(2) 0.041(3) C29 0.037(2) 0.053(3) 0.036(2) 0.018(2) 0.0169(17) 0.017(2) C8 0.093(5) 0.054(3) 0.072(4) 0.036(3) 0.030(3) 0.030(3) C10 0.078(4) 0.048(3) 0.035(2) 0.013(2) 0.009(2) 0.036(3) O9 0.102(5) 0.265(10) 0.326(12) 0.250(10) 0.134(6) 0.109(6) C4 0.056(3) 0.037(2) 0.037(2) 0.0122(19) -0.002(2) 0.018(2) C39 0.058(3) 0.073(4) 0.095(5) 0.051(4) 0.045(3) 0.039(3) C43 0.070(3) 0.058(3) 0.036(2) 0.025(2) 0.024(2) 0.028(3) C54 0.078(4) 0.053(3) 0.046(3) 0.021(2) 0.013(2) 0.042(3) C20 0.070(4) 0.057(3) 0.069(4) 0.035(3) 0.024(3) 0.034(3) C21 0.073(4) 0.046(3) 0.079(4) 0.034(3) 0.038(3) 0.031(3) O5 0.096(4) 0.167(6) 0.145(6) 0.101(5) 0.067(4) 0.059(4) O6 0.108(5) 0.069(4) 0.301(12) 0.091(6) 0.014(6) 0.011(4) O10 0.142(7) 0.077(4) 0.264(11) 0.049(6) -0.026(7) 0.041(4) O13 0.098(4) 0.095(4) 0.112(4) 0.035(3) 0.022(3) 0.055(3) C61 0.083(6) 0.161(9) 0.115(7) 0.080(7) 0.029(5) 0.060(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br6 C34 1.891(5) . ? Br4 C6 1.879(5) . ? Co2 O4 1.878(3) . ? Co2 O3 1.881(3) . ? Co2 N5 1.932(4) . ? Co2 N7 1.935(4) . ? Co2 N8 1.950(4) . ? Co2 N6 1.953(3) . ? Br7 C35 1.891(4) . ? Br3 C5 1.878(5) . ? Br5 C33 1.888(4) . ? Co1 O1 1.876(3) . ? Co1 O2 1.882(3) . ? Co1 N3 1.935(4) . ? Co1 N1 1.939(4) . ? Co1 N2 1.945(4) . ? Co1 N4 1.957(4) . ? Br8 C36 1.888(5) . ? Br1 C3 1.887(5) . ? Br2 C4 1.889(4) . ? Cl2 O11 1.366(7) . ? Cl2 O9 1.368(6) . ? Cl2 O10 1.373(7) . ? Cl2 O12 1.439(5) . ? Cl1 O6 1.354(6) . ? Cl1 O8 1.403(6) . ? Cl1 O5 1.413(6) . ? Cl1 O7 1.417(6) . ? O3 C31 1.342(5) . ? O4 C32 1.340(5) . ? O1 C1 1.348(5) . ? O2 C2 1.334(6) . ? C41 C42 1.339(9) . ? C41 C40 1.437(8) . ? N8 C58 1.313(6) . ? N8 C59 1.362(6) . ? N3 C19 1.330(6) . ? N3 C30 1.361(6) . ? N6 C46 1.331(6) . ? N6 C47 1.364(6) . ? N4 C28 1.331(6) . ? N4 C29 1.374(6) . ? C32 C33 1.386(6) . ? C32 C31 1.407(6) . ? N7 C49 1.325(6) . ? N7 C60 1.360(6) . ? C35 C34 1.380(6) . ? C35 C36 1.389(7) . ? N2 C16 1.321(7) . ? N2 C17 1.369(6) . ? C1 C6 1.376(7) . ? C1 C2 1.410(6) . ? N1 C7 1.329(7) . ? N1 C18 1.359(6) . ? C22 C21 1.403(8) . ? C22 C30 1.405(7) . ? C22 C23 1.430(7) . ? C30 C29 1.410(7) . ? C17 C13 1.408(7) . ? C17 C18 1.412(8) . ? C59 C55 1.398(6) . ? C59 C60 1.418(7) . ? N5 C37 1.312(6) . ? N5 C48 1.358(6) . ? C14 C15 1.357(9) . ? C14 C13 1.405(9) . ? C31 C36 1.395(6) . ? C34 C33 1.393(6) . ? C55 C56 1.394(8) . ? C55 C54 1.431(8) . ? C56 C57 1.365(8) . ? C58 C57 1.392(7) . ? C6 C5 1.411(6) . ? C52 C51 1.404(8) . ? C52 C60 1.408(7) . ? C52 C53 1.433(8) . ? C16 C15 1.409(7) . ? C5 C4 1.386(8) . ? C28 C27 1.407(7) . ? C19 C20 1.391(8) . ? C49 C50 1.403(7) . ? C48 C40 1.394(7) . ? C48 C47 1.419(7) . ? C9 C8 1.370(9) . ? C9 C10 1.414(9) . ? C47 C43 1.400(6) . ? C25 C26 1.393(8) . ? C25 C29 1.407(6) . ? C25 C24 1.435(8) . ? C51 C50 1.366(8) . ? C18 C10 1.396(7) . ? C2 C3 1.406(6) . ? C7 C8 1.398(8) . ? C45 C44 1.360(8) . ? C45 C46 1.409(7) . ? C40 C39 1.397(8) . ? C23 C24 1.340(9) . ? C44 C43 1.398(8) . ? C26 C27 1.377(9) . ? C12 C11 1.340(10) . ? C12 C13 1.426(8) . ? C3 C4 1.385(8) . ? C38 C39 1.352(9) . ? C38 C37 1.411(8) . ? C53 C54 1.356(9) . ? C11 C10 1.457(8) . ? C42 C43 1.441(8) . ? C20 C21 1.374(8) . ? O13 C61 1.363(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 O4 Co2 O3 88.67(13) . . ? O4 Co2 N5 88.37(15) . . ? O3 Co2 N5 91.34(15) . . ? O4 Co2 N7 91.67(15) . . ? O3 Co2 N7 89.06(15) . . ? N5 Co2 N7 179.60(15) . . ? O4 Co2 N8 175.89(16) . . ? O3 Co2 N8 90.86(14) . . ? N5 Co2 N8 95.72(16) . . ? N7 Co2 N8 84.24(16) . . ? O4 Co2 N6 89.56(14) . . ? O3 Co2 N6 175.18(16) . . ? N5 Co2 N6 84.13(16) . . ? N7 Co2 N6 95.47(15) . . ? N8 Co2 N6 91.23(15) . . ? O1 Co1 O2 88.66(14) . . ? O1 Co1 N3 89.43(15) . . ? O2 Co1 N3 91.36(15) . . ? O1 Co1 N1 90.92(16) . . ? O2 Co1 N1 92.36(15) . . ? N3 Co1 N1 176.27(16) . . ? O1 Co1 N2 174.79(16) . . ? O2 Co1 N2 89.70(14) . . ? N3 Co1 N2 95.56(17) . . ? N1 Co1 N2 84.20(17) . . ? O1 Co1 N4 90.63(14) . . ? O2 Co1 N4 175.34(16) . . ? N3 Co1 N4 84.02(16) . . ? N1 Co1 N4 92.26(17) . . ? N2 Co1 N4 91.40(15) . . ? O11 Cl2 O9 107.9(6) . . ? O11 Cl2 O10 106.7(7) . . ? O9 Cl2 O10 111.4(6) . . ? O11 Cl2 O12 106.7(4) . . ? O9 Cl2 O12 113.1(4) . . ? O10 Cl2 O12 110.6(4) . . ? O6 Cl1 O8 110.8(6) . . ? O6 Cl1 O5 111.1(5) . . ? O8 Cl1 O5 107.6(4) . . ? O6 Cl1 O7 109.8(5) . . ? O8 Cl1 O7 107.2(4) . . ? O5 Cl1 O7 110.2(4) . . ? C31 O3 Co2 108.4(2) . . ? C32 O4 Co2 108.7(3) . . ? C1 O1 Co1 108.7(3) . . ? C2 O2 Co1 108.7(3) . . ? C42 C41 C40 121.9(5) . . ? C58 N8 C59 117.7(4) . . ? C58 N8 Co2 130.5(3) . . ? C59 N8 Co2 111.7(3) . . ? C19 N3 C30 118.6(4) . . ? C19 N3 Co1 128.6(3) . . ? C30 N3 Co1 112.8(3) . . ? C46 N6 C47 117.9(4) . . ? C46 N6 Co2 130.6(3) . . ? C47 N6 Co2 111.4(3) . . ? C28 N4 C29 117.9(4) . . ? C28 N4 Co1 130.8(4) . . ? C29 N4 Co1 111.3(3) . . ? O4 C32 C33 123.5(4) . . ? O4 C32 C31 117.0(4) . . ? C33 C32 C31 119.5(4) . . ? C49 N7 C60 118.4(4) . . ? C49 N7 Co2 129.1(3) . . ? C60 N7 Co2 112.3(3) . . ? C34 C35 C36 120.4(4) . . ? C34 C35 Br7 120.3(4) . . ? C36 C35 Br7 119.3(3) . . ? C16 N2 C17 117.7(4) . . ? C16 N2 Co1 130.8(3) . . ? C17 N2 Co1 111.5(3) . . ? O1 C1 C6 123.5(4) . . ? O1 C1 C2 116.6(4) . . ? C6 C1 C2 119.9(4) . . ? C7 N1 C18 119.7(5) . . ? C7 N1 Co1 128.1(4) . . ? C18 N1 Co1 112.2(4) . . ? C21 C22 C30 116.2(5) . . ? C21 C22 C23 126.0(5) . . ? C30 C22 C23 117.8(5) . . ? N3 C30 C22 123.7(5) . . ? N3 C30 C29 115.7(4) . . ? C22 C30 C29 120.7(4) . . ? N2 C17 C13 123.7(5) . . ? N2 C17 C18 116.0(4) . . ? C13 C17 C18 120.3(5) . . ? N8 C59 C55 123.5(5) . . ? N8 C59 C60 115.8(4) . . ? C55 C59 C60 120.6(4) . . ? C37 N5 C48 118.2(4) . . ? C37 N5 Co2 129.4(4) . . ? C48 N5 Co2 112.1(3) . . ? C15 C14 C13 120.2(5) . . ? O3 C31 C36 123.6(4) . . ? O3 C31 C32 117.2(4) . . ? C36 C31 C32 119.2(4) . . ? C35 C34 C33 119.7(4) . . ? C35 C34 Br6 119.9(3) . . ? C33 C34 Br6 120.3(3) . . ? C56 C55 C59 116.8(5) . . ? C56 C55 C54 125.2(5) . . ? C59 C55 C54 118.0(5) . . ? C57 C56 C55 119.5(5) . . ? N8 C58 C57 122.5(5) . . ? C1 C6 C5 121.0(4) . . ? C1 C6 Br4 116.8(3) . . ? C5 C6 Br4 122.1(4) . . ? C51 C52 C60 116.8(5) . . ? C51 C52 C53 126.0(5) . . ? C60 C52 C53 117.2(5) . . ? N2 C16 C15 122.3(5) . . ? N7 C60 C52 123.2(5) . . ? N7 C60 C59 115.9(4) . . ? C52 C60 C59 121.0(4) . . ? C14 C15 C16 119.8(6) . . ? C4 C5 C6 118.6(4) . . ? C4 C5 Br3 121.5(4) . . ? C6 C5 Br3 119.9(4) . . ? N4 C28 C27 122.1(5) . . ? N3 C19 C20 121.3(5) . . ? N7 C49 C50 121.9(5) . . ? N5 C48 C40 123.2(5) . . ? N5 C48 C47 115.9(4) . . ? C40 C48 C47 120.9(4) . . ? C35 C36 C31 120.3(4) . . ? C35 C36 Br8 122.1(3) . . ? C31 C36 Br8 117.5(4) . . ? C8 C9 C10 118.4(6) . . ? N6 C47 C43 123.9(4) . . ? N6 C47 C48 115.7(4) . . ? C43 C47 C48 120.4(5) . . ? C26 C25 C29 117.4(5) . . ? C26 C25 C24 125.3(5) . . ? C29 C25 C24 117.3(5) . . ? C50 C51 C52 119.6(5) . . ? N1 C18 C10 122.7(5) . . ? N1 C18 C17 115.8(4) . . ? C10 C18 C17 121.4(5) . . ? C51 C50 C49 120.1(5) . . ? O2 C2 C3 123.9(4) . . ? O2 C2 C1 117.3(4) . . ? C3 C2 C1 118.8(4) . . ? N1 C7 C8 120.3(6) . . ? C32 C33 C34 120.7(4) . . ? C32 C33 Br5 117.4(3) . . ? C34 C33 Br5 121.9(3) . . ? C56 C57 C58 120.0(5) . . ? C44 C45 C46 120.5(5) . . ? C48 C40 C39 117.0(5) . . ? C48 C40 C41 117.6(5) . . ? C39 C40 C41 125.4(5) . . ? C24 C23 C22 121.4(5) . . ? C45 C44 C43 119.8(5) . . ? C27 C26 C25 119.6(5) . . ? C11 C12 C13 122.5(5) . . ? C26 C27 C28 119.9(5) . . ? C4 C3 C2 120.3(5) . . ? C4 C3 Br1 123.4(3) . . ? C2 C3 Br1 116.3(4) . . ? C39 C38 C37 119.3(5) . . ? N6 C46 C45 121.3(5) . . ? C54 C53 C52 121.8(5) . . ? C23 C24 C25 122.1(5) . . ? C12 C11 C10 120.6(5) . . ? C41 C42 C43 121.1(5) . . ? N5 C37 C38 122.2(5) . . ? C14 C13 C17 116.2(5) . . ? C14 C13 C12 126.1(5) . . ? C17 C13 C12 117.7(6) . . ? N4 C29 C25 123.1(5) . . ? N4 C29 C30 116.1(4) . . ? C25 C29 C30 120.8(5) . . ? C9 C8 C7 121.5(7) . . ? C18 C10 C9 117.4(5) . . ? C18 C10 C11 117.4(6) . . ? C9 C10 C11 125.1(5) . . ? C3 C4 C5 121.1(4) . . ? C3 C4 Br2 118.8(4) . . ? C5 C4 Br2 120.1(4) . . ? C38 C39 C40 120.0(5) . . ? C44 C43 C47 116.6(5) . . ? C44 C43 C42 125.5(5) . . ? C47 C43 C42 117.9(5) . . ? C53 C54 C55 121.3(5) . . ? C21 C20 C19 120.6(5) . . ? C20 C21 C22 119.6(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.270 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.118 data_Complex7 _database_code_depnum_ccdc_archive 'CCDC 909991' #TrackingRef 'complex7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Br8 Co N5 O9' _chemical_formula_weight 1346.81 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 12.733(3) _cell_length_b 20.347(5) _cell_length_c 15.916(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.654(4) _cell_angle_gamma 90.00 _cell_volume 4052(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 32995 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour green-red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 8.371 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.1346 _exptl_absorpt_correction_T_max 0.3665 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 15593 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9253 _reflns_number_gt 6720 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0512P)^2^+0.9086P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9253 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Br3 Br 0.76821(4) 0.89471(2) 0.60148(3) 0.02365(12) Uani 1 1 d . . . Br1 Br 0.69626(4) 0.99600(3) 0.92080(3) 0.02492(12) Uani 1 1 d . . . Br2 Br 0.76721(4) 0.87210(2) 0.80833(3) 0.02701(12) Uani 1 1 d . . . Br7 Br 0.17334(4) 0.09323(3) 0.89239(3) 0.03382(14) Uani 1 1 d . . . Br4 Br 0.66191(5) 1.03280(3) 0.50795(3) 0.03095(13) Uani 1 1 d . . . Br5 Br 0.43597(4) -0.07315(3) 0.72902(3) 0.02915(13) Uani 1 1 d . . . Co1 Co 0.59697(5) 1.18621(3) 0.73319(4) 0.01773(14) Uani 1 1 d . . . Br6 Br 0.41379(4) 0.04023(3) 0.87282(3) 0.03070(13) Uani 1 1 d . . . Br8 Br -0.04037(4) 0.02776(4) 0.76508(5) 0.05124(18) Uani 1 1 d . . . O2 O 0.6279(3) 1.11455(16) 0.80766(19) 0.0204(7) Uani 1 1 d . . . O1 O 0.6221(3) 1.13156(16) 0.6434(2) 0.0218(7) Uani 1 1 d . . . O4 O 0.2253(3) -0.1210(2) 0.6411(2) 0.0369(9) Uani 1 1 d . . . H4A H 0.1654 -0.1323 0.6133 0.055 Uiso 1 1 calc R . . N1 N 0.4472(3) 1.1644(2) 0.7113(2) 0.0207(9) Uani 1 1 d . . . N2 N 0.5601(3) 1.2365(2) 0.8254(2) 0.0219(9) Uani 1 1 d . . . N3 N 0.7448(3) 1.2120(2) 0.7523(2) 0.0223(9) Uani 1 1 d . . . N4 N 0.5797(3) 1.26169(19) 0.6570(2) 0.0183(8) Uani 1 1 d . . . C6 C 0.6775(4) 1.0199(2) 0.6273(3) 0.0185(10) Uani 1 1 d . . . C4 C 0.7182(4) 0.9517(2) 0.7532(3) 0.0185(10) Uani 1 1 d . . . C29 C 0.3002(4) -0.0445(3) 0.7465(3) 0.0239(11) Uani 1 1 d . . . C3 C 0.6902(4) 1.0040(2) 0.8017(3) 0.0169(9) Uani 1 1 d . . . C12 C 0.4532(4) 1.2374(2) 0.8276(3) 0.0230(10) Uani 1 1 d . . . O3 O 0.0284(3) -0.0809(3) 0.6526(4) 0.0637(15) Uani 1 1 d . . . H3A H -0.0297 -0.0685 0.6653 0.096 Uiso 1 1 calc R . . C17 C 0.8235(4) 1.1863(3) 0.8109(3) 0.0298(12) Uani 1 1 d . . . H17 H 0.8074 1.1523 0.8474 0.036 Uiso 1 1 calc R . . C1 C 0.6532(4) 1.0721(2) 0.6755(3) 0.0193(10) Uani 1 1 d . . . C11 C 0.3888(4) 1.1972(2) 0.7603(3) 0.0217(10) Uani 1 1 d . . . C7 C 0.3985(4) 1.1222(3) 0.6513(3) 0.0269(11) Uani 1 1 d . . . H7 H 0.4397 1.0978 0.6182 0.032 Uiso 1 1 calc R . . C15 C 0.5897(5) 1.3027(3) 0.9512(3) 0.0325(13) Uani 1 1 d . . . H15 H 0.6385 1.3248 0.9943 0.039 Uiso 1 1 calc R . . C2 C 0.6563(3) 1.0637(2) 0.7644(3) 0.0205(10) Uani 1 1 d . . . C30 C 0.2900(4) 0.0041(3) 0.8058(3) 0.0243(11) Uani 1 1 d . . . C31 C 0.1893(4) 0.0263(3) 0.8141(3) 0.0263(11) Uani 1 1 d . . . C24 C 0.5819(4) 1.3623(3) 0.5391(3) 0.0310(12) Uani 1 1 d . . . H24 H 0.5828 1.3956 0.4974 0.037 Uiso 1 1 calc R . . C21 C 0.7670(4) 1.2604(3) 0.6997(3) 0.0230(11) Uani 1 1 d . . . C32 C 0.1001(4) -0.0010(3) 0.7609(4) 0.0314(12) Uani 1 1 d . . . C23 C 0.6768(4) 1.3365(3) 0.5842(3) 0.0308(12) Uani 1 1 d . . . H23 H 0.7436 1.3522 0.5739 0.037 Uiso 1 1 calc R . . C9 C 0.2287(4) 1.1486(3) 0.6841(3) 0.0316(12) Uani 1 1 d . . . H9 H 0.1532 1.1435 0.6740 0.038 Uiso 1 1 calc R . . C22 C 0.6733(4) 1.2875(2) 0.6444(3) 0.0233(10) Uani 1 1 d . . . C10 C 0.2780(4) 1.1918(3) 0.7469(3) 0.0313(12) Uani 1 1 d . . . H10 H 0.2372 1.2169 0.7796 0.038 Uiso 1 1 calc R . . C16 C 0.6267(4) 1.2677(2) 0.8873(3) 0.0279(11) Uani 1 1 d . . . H16 H 0.7014 1.2659 0.8878 0.033 Uiso 1 1 calc R . . C20 C 0.8704(4) 1.2834(3) 0.7059(4) 0.0353(13) Uani 1 1 d . . . H20 H 0.8857 1.3170 0.6685 0.042 Uiso 1 1 calc R . . C25 C 0.4862(4) 1.3387(3) 0.5558(3) 0.0268(11) Uani 1 1 d . . . H25 H 0.4202 1.3568 0.5277 0.032 Uiso 1 1 calc R . . C18 C 0.9273(4) 1.2085(3) 0.8192(4) 0.0366(13) Uani 1 1 d . . . H18 H 0.9821 1.1900 0.8612 0.044 Uiso 1 1 calc R . . C26 C 0.4878(4) 1.2879(2) 0.6145(3) 0.0227(10) Uani 1 1 d . . . H26 H 0.4219 1.2710 0.6250 0.027 Uiso 1 1 calc R . . C5 C 0.7133(4) 0.9602(2) 0.6656(3) 0.0216(10) Uani 1 1 d . . . C28 C 0.2123(4) -0.0730(3) 0.6958(3) 0.0282(11) Uani 1 1 d . . . C13 C 0.4127(5) 1.2709(3) 0.8897(3) 0.0328(13) Uani 1 1 d . . . H13 H 0.3382 1.2707 0.8901 0.039 Uiso 1 1 calc R . . C27 C 0.1102(4) -0.0506(3) 0.7039(4) 0.0374(14) Uani 1 1 d . . . C8 C 0.2879(4) 1.1141(3) 0.6376(3) 0.0301(12) Uani 1 1 d . . . H8 H 0.2542 1.0841 0.5953 0.036 Uiso 1 1 calc R . . C19 C 0.9508(4) 1.2575(3) 0.7661(4) 0.0417(15) Uani 1 1 d . . . H19 H 1.0219 1.2733 0.7711 0.050 Uiso 1 1 calc R . . C14 C 0.4825(5) 1.3047(3) 0.9511(3) 0.0374(14) Uani 1 1 d . . . H14 H 0.4561 1.3295 0.9933 0.045 Uiso 1 1 calc R . . N5 N 0.1552(3) 0.2503(2) 0.5179(3) 0.0322(11) Uani 1 1 d . . . O5 O 0.1055(3) 0.2694(2) 0.5751(3) 0.0439(10) Uani 1 1 d . . . O8 O 0.0790(4) 0.6485(3) 0.4766(4) 0.0629(14) Uani 1 1 d . . . H8A H 0.0419 0.6734 0.4408 0.094 Uiso 1 1 calc R . . O7 O 0.2513(3) 0.2624(3) 0.5227(3) 0.0610(14) Uani 1 1 d . . . O9 O 0.0900(4) 0.8273(3) 0.5193(4) 0.0769(17) Uani 1 1 d . . . H9A H 0.0290 0.8133 0.5231 0.115 Uiso 1 1 calc R . . O6 O 0.1082(4) 0.2158(3) 0.4590(3) 0.0771(19) Uani 1 1 d . . . C33 C 0.0410(5) 0.5851(4) 0.4649(5) 0.0575(19) Uani 1 1 d . . . H33A H 0.0831 0.5562 0.5076 0.086 Uiso 1 1 calc R . . H33B H 0.0470 0.5700 0.4075 0.086 Uiso 1 1 calc R . . H33C H -0.0341 0.5839 0.4712 0.086 Uiso 1 1 calc R . . C34 C 0.0884(10) 0.8500(9) 0.4418(7) 0.187(9) Uani 1 1 d . . . H34A H 0.0550 0.8935 0.4363 0.280 Uiso 1 1 calc R . . H34B H 0.0474 0.8200 0.4000 0.280 Uiso 1 1 calc R . . H34C H 0.1617 0.8534 0.4314 0.280 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 Br3 0.0240(2) 0.0153(2) 0.0314(3) -0.0041(2) 0.00462(19) 0.00151(19) Br1 0.0314(3) 0.0210(3) 0.0204(2) 0.00462(19) -0.00042(19) 0.0042(2) Br2 0.0323(3) 0.0142(2) 0.0327(3) 0.0050(2) 0.0013(2) 0.0052(2) Br7 0.0372(3) 0.0338(3) 0.0312(3) 0.0028(2) 0.0082(2) 0.0111(2) Br4 0.0487(3) 0.0220(3) 0.0225(2) 0.0010(2) 0.0074(2) 0.0096(2) Br5 0.0187(2) 0.0298(3) 0.0374(3) -0.0054(2) 0.0011(2) 0.0012(2) Co1 0.0210(3) 0.0122(3) 0.0193(3) 0.0015(2) 0.0020(2) 0.0028(3) Br6 0.0247(3) 0.0293(3) 0.0346(3) -0.0057(2) -0.0038(2) -0.0018(2) Br8 0.0203(3) 0.0557(4) 0.0773(5) -0.0065(4) 0.0080(3) 0.0062(3) O2 0.0277(18) 0.0129(17) 0.0198(16) 0.0039(13) 0.0025(13) 0.0062(14) O1 0.0300(18) 0.0116(17) 0.0241(16) 0.0034(13) 0.0055(14) 0.0078(14) O4 0.028(2) 0.033(2) 0.045(2) -0.0151(19) -0.0047(17) -0.0004(18) N1 0.024(2) 0.013(2) 0.022(2) 0.0042(16) -0.0028(17) 0.0012(17) N2 0.031(2) 0.013(2) 0.021(2) 0.0010(16) 0.0032(17) 0.0016(18) N3 0.021(2) 0.016(2) 0.028(2) -0.0003(17) 0.0022(17) 0.0033(17) N4 0.0196(19) 0.012(2) 0.023(2) -0.0002(16) 0.0031(16) 0.0006(16) C6 0.024(2) 0.014(2) 0.016(2) 0.0018(18) 0.0014(18) -0.0002(19) C4 0.018(2) 0.016(2) 0.021(2) 0.0027(19) 0.0019(18) 0.0017(19) C29 0.014(2) 0.025(3) 0.030(3) 0.001(2) -0.0005(19) -0.002(2) C3 0.020(2) 0.018(2) 0.012(2) 0.0028(18) -0.0007(17) -0.0020(19) C12 0.025(2) 0.015(3) 0.029(3) 0.004(2) 0.006(2) 0.007(2) O3 0.021(2) 0.059(3) 0.103(4) -0.033(3) -0.010(2) -0.004(2) C17 0.029(3) 0.021(3) 0.037(3) 0.006(2) 0.000(2) 0.005(2) C1 0.021(2) 0.013(2) 0.022(2) 0.0006(19) -0.0015(19) 0.0019(19) C11 0.029(3) 0.013(2) 0.023(2) 0.0041(19) 0.006(2) 0.007(2) C7 0.034(3) 0.019(3) 0.026(3) 0.002(2) 0.001(2) -0.003(2) C15 0.057(4) 0.014(3) 0.024(3) -0.006(2) -0.001(2) -0.002(3) C2 0.014(2) 0.020(3) 0.025(2) 0.001(2) -0.0038(18) 0.0004(19) C30 0.022(2) 0.026(3) 0.024(2) 0.006(2) 0.001(2) -0.002(2) C31 0.029(3) 0.021(3) 0.031(3) 0.005(2) 0.010(2) 0.001(2) C24 0.038(3) 0.019(3) 0.034(3) 0.014(2) 0.002(2) 0.001(2) C21 0.021(2) 0.018(3) 0.030(3) 0.002(2) 0.006(2) 0.001(2) C32 0.013(2) 0.032(3) 0.048(3) 0.002(3) 0.002(2) 0.002(2) C23 0.030(3) 0.023(3) 0.040(3) 0.009(2) 0.006(2) -0.004(2) C9 0.025(3) 0.028(3) 0.040(3) 0.011(3) -0.001(2) -0.006(2) C22 0.025(2) 0.017(3) 0.030(3) 0.003(2) 0.008(2) 0.003(2) C10 0.030(3) 0.022(3) 0.043(3) 0.014(2) 0.010(2) 0.010(2) C16 0.037(3) 0.014(3) 0.028(3) 0.000(2) -0.005(2) -0.006(2) C20 0.026(3) 0.033(3) 0.048(3) 0.007(3) 0.009(2) 0.003(2) C25 0.025(3) 0.021(3) 0.032(3) 0.008(2) 0.000(2) 0.006(2) C18 0.025(3) 0.033(3) 0.048(3) 0.006(3) -0.001(2) 0.008(2) C26 0.023(2) 0.019(3) 0.024(2) 0.004(2) -0.0007(19) 0.002(2) C5 0.017(2) 0.015(3) 0.031(3) -0.004(2) 0.0003(19) -0.0003(19) C28 0.025(3) 0.022(3) 0.034(3) 0.000(2) -0.004(2) -0.001(2) C13 0.041(3) 0.028(3) 0.032(3) 0.004(2) 0.013(2) 0.008(3) C27 0.015(2) 0.033(3) 0.061(4) -0.006(3) -0.002(2) -0.003(2) C8 0.032(3) 0.028(3) 0.028(3) 0.007(2) 0.001(2) -0.006(2) C19 0.022(3) 0.046(4) 0.054(4) 0.005(3) 0.001(3) 0.000(3) C14 0.060(4) 0.025(3) 0.027(3) -0.006(2) 0.008(3) 0.013(3) N5 0.025(2) 0.029(3) 0.040(3) -0.008(2) -0.002(2) 0.007(2) O5 0.036(2) 0.040(3) 0.056(3) -0.017(2) 0.0092(19) 0.000(2) O8 0.046(3) 0.052(3) 0.092(4) 0.019(3) 0.015(3) 0.008(2) O7 0.040(3) 0.070(4) 0.077(3) -0.017(3) 0.021(2) -0.021(2) O9 0.062(4) 0.090(5) 0.070(3) -0.026(3) -0.010(3) -0.032(3) O6 0.038(3) 0.106(5) 0.081(3) -0.066(4) -0.008(2) 0.011(3) C33 0.043(4) 0.055(5) 0.076(5) -0.004(4) 0.015(4) 0.002(4) C34 0.142(11) 0.35(2) 0.065(7) -0.038(10) 0.013(7) -0.167(14) _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 Br3 C5 1.889(5) . ? Br1 C3 1.890(4) . ? Br2 C4 1.891(5) . ? Br7 C31 1.882(5) . ? Br4 C6 1.892(4) . ? Br5 C29 1.894(5) . ? Co1 O2 1.874(3) . ? Co1 O1 1.884(3) . ? Co1 N2 1.918(4) . ? Co1 N3 1.923(4) . ? Co1 N1 1.927(4) . ? Co1 N4 1.944(4) . ? Br6 C30 1.882(5) . ? Br8 C32 1.895(5) . ? O2 C2 1.330(6) . ? O1 C1 1.343(6) . ? O4 C28 1.339(6) . ? N1 C7 1.346(6) . ? N1 C11 1.350(6) . ? N2 C16 1.335(6) . ? N2 C12 1.368(6) . ? N3 C17 1.343(6) . ? N3 C21 1.356(6) . ? N4 C26 1.348(6) . ? N4 C22 1.351(6) . ? C6 C1 1.379(7) . ? C6 C5 1.398(7) . ? C4 C5 1.395(7) . ? C4 C3 1.399(7) . ? C29 C28 1.381(7) . ? C29 C30 1.389(7) . ? C3 C2 1.385(7) . ? C12 C13 1.376(7) . ? C12 C11 1.470(7) . ? O3 C27 1.349(7) . ? C17 C18 1.379(8) . ? C1 C2 1.418(6) . ? C11 C10 1.392(7) . ? C7 C8 1.394(7) . ? C15 C14 1.365(9) . ? C15 C16 1.393(7) . ? C30 C31 1.389(7) . ? C31 C32 1.400(7) . ? C24 C25 1.381(7) . ? C24 C23 1.389(7) . ? C21 C20 1.383(7) . ? C21 C22 1.455(7) . ? C32 C27 1.378(8) . ? C23 C22 1.389(7) . ? C9 C8 1.349(8) . ? C9 C10 1.389(8) . ? C20 C19 1.371(8) . ? C25 C26 1.392(7) . ? C18 C19 1.375(8) . ? C28 C27 1.406(7) . ? C13 C14 1.378(8) . ? N5 O6 1.235(6) . ? N5 O7 1.237(6) . ? N5 O5 1.262(6) . ? O8 C33 1.380(9) . ? O9 C34 1.313(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O1 88.58(14) . . ? O2 Co1 N2 89.06(15) . . ? O1 Co1 N2 174.53(17) . . ? O2 Co1 N3 91.57(16) . . ? O1 Co1 N3 89.00(16) . . ? N2 Co1 N3 96.00(17) . . ? O2 Co1 N1 91.16(15) . . ? O1 Co1 N1 91.59(16) . . ? N2 Co1 N1 83.52(18) . . ? N3 Co1 N1 177.21(17) . . ? O2 Co1 N4 174.47(15) . . ? O1 Co1 N4 90.50(15) . . ? N2 Co1 N4 92.31(17) . . ? N3 Co1 N4 82.96(16) . . ? N1 Co1 N4 94.31(16) . . ? C2 O2 Co1 108.9(3) . . ? C1 O1 Co1 108.8(3) . . ? C7 N1 C11 119.7(4) . . ? C7 N1 Co1 125.9(4) . . ? C11 N1 Co1 114.4(3) . . ? C16 N2 C12 118.3(4) . . ? C16 N2 Co1 127.3(4) . . ? C12 N2 Co1 114.3(3) . . ? C17 N3 C21 119.8(4) . . ? C17 N3 Co1 125.9(4) . . ? C21 N3 Co1 114.2(3) . . ? C26 N4 C22 118.6(4) . . ? C26 N4 Co1 127.8(3) . . ? C22 N4 Co1 113.5(3) . . ? C1 C6 C5 121.1(4) . . ? C1 C6 Br4 117.3(3) . . ? C5 C6 Br4 121.6(4) . . ? C5 C4 C3 119.2(4) . . ? C5 C4 Br2 121.3(4) . . ? C3 C4 Br2 119.5(3) . . ? C28 C29 C30 121.9(5) . . ? C28 C29 Br5 116.6(4) . . ? C30 C29 Br5 121.4(3) . . ? C2 C3 C4 121.5(4) . . ? C2 C3 Br1 117.2(4) . . ? C4 C3 Br1 121.3(3) . . ? N2 C12 C13 122.1(5) . . ? N2 C12 C11 113.4(4) . . ? C13 C12 C11 124.5(5) . . ? N3 C17 C18 121.2(5) . . ? O1 C1 C6 124.2(4) . . ? O1 C1 C2 116.2(4) . . ? C6 C1 C2 119.5(4) . . ? N1 C11 C10 121.5(5) . . ? N1 C11 C12 113.8(4) . . ? C10 C11 C12 124.7(5) . . ? N1 C7 C8 120.4(5) . . ? C14 C15 C16 119.2(5) . . ? O2 C2 C3 123.6(4) . . ? O2 C2 C1 117.5(4) . . ? C3 C2 C1 118.9(4) . . ? C31 C30 C29 120.0(5) . . ? C31 C30 Br6 120.7(4) . . ? C29 C30 Br6 119.3(4) . . ? C30 C31 C32 118.2(5) . . ? C30 C31 Br7 120.8(4) . . ? C32 C31 Br7 120.9(4) . . ? C25 C24 C23 118.9(5) . . ? N3 C21 C20 120.4(5) . . ? N3 C21 C22 114.0(4) . . ? C20 C21 C22 125.4(5) . . ? C27 C32 C31 121.6(5) . . ? C27 C32 Br8 116.9(4) . . ? C31 C32 Br8 121.4(4) . . ? C22 C23 C24 119.4(5) . . ? C8 C9 C10 120.0(5) . . ? N4 C22 C23 121.6(4) . . ? N4 C22 C21 114.2(4) . . ? C23 C22 C21 124.2(4) . . ? C9 C10 C11 118.2(5) . . ? N2 C16 C15 121.8(5) . . ? C19 C20 C21 119.9(5) . . ? C24 C25 C26 118.9(5) . . ? C19 C18 C17 119.5(5) . . ? N4 C26 C25 122.3(4) . . ? C4 C5 C6 119.6(4) . . ? C4 C5 Br3 120.0(4) . . ? C6 C5 Br3 120.1(4) . . ? O4 C28 C29 120.2(5) . . ? O4 C28 C27 121.6(5) . . ? C29 C28 C27 118.2(5) . . ? C12 C13 C14 118.6(5) . . ? O3 C27 C32 125.2(5) . . ? O3 C27 C28 114.9(5) . . ? C32 C27 C28 119.9(5) . . ? C9 C8 C7 120.2(5) . . ? C20 C19 C18 119.2(5) . . ? C15 C14 C13 119.9(5) . . ? O6 N5 O7 119.7(5) . . ? O6 N5 O5 119.0(5) . . ? O7 N5 O5 121.1(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.156 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.148 data_complex8 _database_code_depnum_ccdc_archive 'CCDC 909992' #TrackingRef 'complex8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 Br8 Co N5 O5' _chemical_formula_weight 1186.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.637(3) _cell_length_b 10.995(3) _cell_length_c 16.387(4) _cell_angle_alpha 96.351(2) _cell_angle_beta 93.693(2) _cell_angle_gamma 104.486(2) _cell_volume 1835.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 19209 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour Green-red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 2.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 9.215 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2601 _exptl_absorpt_correction_T_max 0.4043 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 13511 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8322 _reflns_number_gt 5730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.1101P)^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 none _refine_ls_number_reflns 8322 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1721 _refine_ls_wR_factor_gt 0.1585 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br4 Br 0.59317(6) 0.33011(7) 0.24142(4) 0.05055(18) Uani 1 1 d . . . Br3 Br 0.46086(7) 0.56548(7) 0.19940(5) 0.0574(2) Uani 1 1 d . . . Co2 Co 0.0000 0.0000 0.5000 0.0336(2) Uani 1 2 d S . . Br5 Br 0.39413(7) 0.06861(7) 0.34925(4) 0.0550(2) Uani 1 1 d . . . Br1 Br 0.22559(6) 0.25895(7) -0.10472(4) 0.05191(19) Uani 1 1 d . . . Co1 Co 0.5000 0.0000 0.0000 0.0379(3) Uani 1 2 d S . . Br2 Br 0.27831(8) 0.53018(7) 0.02133(5) 0.0608(2) Uani 1 1 d . . . Br8 Br 0.15407(8) -0.35769(8) 0.58614(5) 0.0665(2) Uani 1 1 d . . . O1 O 0.5410(4) 0.1235(4) 0.0943(2) 0.0429(9) Uani 1 1 d . . . C5 C 0.4372(5) 0.4190(6) 0.1214(4) 0.0395(12) Uani 1 1 d . . . C11 C 0.1712(5) -0.1370(6) 0.5108(3) 0.0380(12) Uani 1 1 d . . . O4 O 0.1533(4) 0.0370(4) 0.4452(2) 0.0394(9) Uani 1 1 d . . . C4 C 0.3598(6) 0.4023(6) 0.0481(4) 0.0429(13) Uani 1 1 d . . . O3 O 0.0700(4) -0.1196(4) 0.5507(2) 0.0386(9) Uani 1 1 d . . . C6 C 0.4963(5) 0.3218(6) 0.1397(3) 0.0383(12) Uani 1 1 d . . . C13 C 0.3293(5) -0.0561(6) 0.4163(4) 0.0414(13) Uani 1 1 d . . . C10 C 0.6314(7) 0.1141(7) -0.1317(4) 0.0519(16) Uani 1 1 d . . . H10 H 0.5518 0.0810 -0.1633 0.062 Uiso 1 1 calc R . . N1 N 0.6416(5) 0.0981(5) -0.0521(3) 0.0425(11) Uani 1 1 d . . . O2 O 0.3881(4) 0.0931(4) -0.0423(2) 0.0426(9) Uani 1 1 d . . . C16 C 0.2322(6) -0.2336(6) 0.5208(4) 0.0429(13) Uani 1 1 d . . . C3 C 0.3405(5) 0.2930(6) -0.0072(4) 0.0393(12) Uani 1 1 d . . . C2 C 0.4018(5) 0.1980(6) 0.0080(3) 0.0363(12) Uani 1 1 d . . . N3 N 0.0811(5) 0.1399(5) 0.5874(3) 0.0386(10) Uani 1 1 d . . . C12 C 0.2186(5) -0.0502(6) 0.4563(3) 0.0351(11) Uani 1 1 d . . . C15 C 0.3409(6) -0.2436(7) 0.4793(4) 0.0468(14) Uani 1 1 d . . . C1 C 0.4846(5) 0.2156(6) 0.0828(3) 0.0383(12) Uani 1 1 d . . . Br6 Br 0.53702(7) -0.16426(9) 0.37158(6) 0.0701(2) Uani 1 1 d . . . Br7 Br 0.42094(9) -0.37522(9) 0.49549(6) 0.0753(3) Uani 1 1 d . . . C14 C 0.3897(6) -0.1544(7) 0.4289(4) 0.0478(15) Uani 1 1 d . . . N5 N 0.9318(11) 0.7390(11) 0.7868(5) 0.101(3) Uani 1 1 d . . . C24 C 0.9098(15) 0.9164(13) 0.8836(13) 0.137(6) Uani 1 1 d . . . H24A H 0.8612 0.9281 0.9299 0.205 Uiso 1 1 calc R . . H24B H 0.8831 0.9583 0.8398 0.205 Uiso 1 1 calc R . . H24C H 1.0012 0.9516 0.8999 0.205 Uiso 1 1 calc R . . C22 C 1.0505(13) 0.5890(16) 0.8328(14) 0.180(10) Uani 1 1 d . . . H22A H 1.0399 0.4991 0.8268 0.270 Uiso 1 1 calc R . . H22B H 1.0647 0.6222 0.8903 0.270 Uiso 1 1 calc R . . H22C H 1.1242 0.6282 0.8053 0.270 Uiso 1 1 calc R . . C26 C 0.7820(15) 0.6744(19) 0.6737(19) 0.224(14) Uani 1 1 d . . . H26A H 0.7488 0.6898 0.6210 0.336 Uiso 1 1 calc R . . H26B H 0.7239 0.6879 0.7142 0.336 Uiso 1 1 calc R . . H26C H 0.7888 0.5886 0.6701 0.336 Uiso 1 1 calc R . . C23 C 0.8881(18) 0.795(2) 0.8580(12) 0.202(12) Uani 1 1 d . . . H23A H 0.7940 0.7620 0.8523 0.242 Uiso 1 1 calc R . . H23B H 0.9203 0.7588 0.9039 0.242 Uiso 1 1 calc R . . C21 C 0.9464(17) 0.613(2) 0.8003(18) 0.250(17) Uani 1 1 d . . . H21A H 0.8772 0.5783 0.8337 0.300 Uiso 1 1 calc R . . H21B H 0.9255 0.5614 0.7468 0.300 Uiso 1 1 calc R . . C25 C 0.8950(19) 0.750(3) 0.6947(19) 0.255(17) Uani 1 1 d . . . H25A H 0.8928 0.8367 0.6887 0.306 Uiso 1 1 calc R . . H25B H 0.9585 0.7276 0.6603 0.306 Uiso 1 1 calc R . . O5A O 0.2528(9) -0.0433(11) -0.2479(7) 0.062(3) Uani 0.50 1 d P A 1 O5B O 0.1021(11) -0.1065(12) -0.2812(6) 0.071(3) Uani 0.50 1 d P B 2 N4 N 0.0839(7) 0.2424(7) 0.7218(3) 0.0617(16) Uani 1 1 d . . . C17 C 0.0413(6) 0.1457(7) 0.6629(3) 0.0459(14) Uani 1 1 d . . . H17 H -0.0215 0.0762 0.6750 0.055 Uiso 1 1 calc R . . C20 C 0.1721(6) 0.2393(6) 0.5708(4) 0.0454(14) Uani 1 1 d . . . H20 H 0.2022 0.2386 0.5187 0.054 Uiso 1 1 calc R . . C18 C 0.1755(7) 0.3394(8) 0.7041(4) 0.0582(18) Uani 1 1 d . . . H18 H 0.2090 0.4080 0.7449 0.070 Uiso 1 1 calc R . . C19 C 0.2225(7) 0.3430(7) 0.6294(4) 0.0524(16) Uani 1 1 d . . . H19 H 0.2860 0.4125 0.6180 0.063 Uiso 1 1 calc R . . N2 N 0.8627(6) 0.2151(7) -0.0389(4) 0.0652(17) Uani 1 1 d . . . C9 C 0.7376(7) 0.1794(8) -0.1677(5) 0.0587(18) Uani 1 1 d . . . H9 H 0.7315 0.1889 -0.2234 0.070 Uiso 1 1 calc R . . C7 C 0.7589(7) 0.1522(8) -0.0087(4) 0.0584(18) Uani 1 1 d . . . H7 H 0.7661 0.1438 0.0471 0.070 Uiso 1 1 calc R . . C8 C 0.8512(8) 0.2291(9) -0.1188(5) 0.068(2) Uani 1 1 d . . . H8 H 0.9233 0.2743 -0.1418 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 Br4 0.0566(4) 0.0509(4) 0.0424(3) -0.0006(3) -0.0065(3) 0.0162(3) Br3 0.0625(4) 0.0449(4) 0.0641(4) -0.0070(3) 0.0026(3) 0.0198(3) Co2 0.0336(5) 0.0393(6) 0.0322(5) 0.0075(4) 0.0046(4) 0.0159(4) Br5 0.0505(4) 0.0622(5) 0.0564(4) 0.0132(3) 0.0181(3) 0.0164(3) Br1 0.0529(4) 0.0601(4) 0.0471(3) 0.0082(3) -0.0054(3) 0.0247(3) Co1 0.0400(5) 0.0397(6) 0.0366(5) 0.0018(4) -0.0014(4) 0.0180(4) Br2 0.0733(5) 0.0522(4) 0.0684(4) 0.0126(3) 0.0044(3) 0.0361(4) Br8 0.0773(5) 0.0628(5) 0.0757(5) 0.0318(4) 0.0181(4) 0.0358(4) O1 0.045(2) 0.048(3) 0.038(2) 0.0013(18) -0.0044(16) 0.0213(19) C5 0.041(3) 0.033(3) 0.043(3) 0.002(2) 0.006(2) 0.008(2) C11 0.033(3) 0.046(3) 0.038(3) 0.005(2) 0.003(2) 0.015(2) O4 0.038(2) 0.043(2) 0.045(2) 0.0123(17) 0.0101(16) 0.0193(17) C4 0.047(3) 0.041(3) 0.047(3) 0.011(3) 0.009(2) 0.018(3) O3 0.038(2) 0.046(2) 0.0385(19) 0.0139(17) 0.0070(15) 0.0183(17) C6 0.040(3) 0.039(3) 0.034(3) 0.001(2) 0.003(2) 0.010(2) C13 0.033(3) 0.049(4) 0.042(3) 0.001(3) 0.006(2) 0.012(2) C10 0.052(4) 0.052(4) 0.050(4) 0.001(3) 0.003(3) 0.013(3) N1 0.044(3) 0.046(3) 0.038(2) 0.000(2) -0.003(2) 0.015(2) O2 0.046(2) 0.045(2) 0.040(2) -0.0004(18) -0.0043(17) 0.0222(18) C16 0.047(3) 0.041(3) 0.044(3) 0.006(3) 0.002(2) 0.019(3) C3 0.035(3) 0.044(3) 0.042(3) 0.006(2) 0.005(2) 0.015(2) C2 0.034(3) 0.041(3) 0.034(3) 0.005(2) 0.002(2) 0.011(2) N3 0.042(2) 0.040(3) 0.039(2) 0.009(2) 0.0037(19) 0.020(2) C12 0.035(3) 0.036(3) 0.036(3) 0.000(2) 0.000(2) 0.014(2) C15 0.044(3) 0.047(4) 0.055(4) 0.006(3) -0.002(3) 0.026(3) C1 0.041(3) 0.044(3) 0.036(3) 0.011(2) 0.009(2) 0.017(2) Br6 0.0508(4) 0.0860(6) 0.0842(5) 0.0042(4) 0.0228(4) 0.0361(4) Br7 0.0725(5) 0.0679(6) 0.1026(6) 0.0143(5) 0.0106(4) 0.0479(4) C14 0.037(3) 0.056(4) 0.052(3) -0.004(3) 0.001(3) 0.020(3) N5 0.134(8) 0.125(8) 0.065(5) 0.035(5) 0.032(5) 0.056(6) C24 0.134(11) 0.070(8) 0.225(18) 0.021(10) 0.045(12) 0.054(8) C22 0.085(8) 0.146(14) 0.29(2) -0.098(15) 0.036(11) 0.036(9) C26 0.073(9) 0.138(16) 0.47(4) 0.11(2) -0.013(16) 0.014(9) C23 0.157(15) 0.22(2) 0.167(15) -0.059(15) 0.104(13) -0.056(14) C21 0.118(12) 0.25(3) 0.40(4) 0.26(3) -0.046(17) -0.008(14) C25 0.148(18) 0.33(4) 0.38(4) 0.22(3) 0.15(2) 0.14(2) O5A 0.049(5) 0.067(7) 0.072(6) 0.016(5) -0.004(5) 0.017(5) O5B 0.077(7) 0.083(8) 0.049(5) 0.016(5) 0.015(5) 0.008(6) N4 0.073(4) 0.069(4) 0.038(3) 0.002(3) 0.004(3) 0.011(3) C17 0.052(3) 0.048(4) 0.033(3) 0.009(2) -0.001(2) 0.004(3) C20 0.047(3) 0.043(4) 0.045(3) 0.009(3) 0.009(3) 0.009(3) C18 0.064(4) 0.055(5) 0.049(4) -0.004(3) 0.000(3) 0.008(3) C19 0.059(4) 0.037(4) 0.060(4) 0.003(3) 0.002(3) 0.012(3) N2 0.048(3) 0.069(5) 0.074(4) 0.015(3) 0.007(3) 0.005(3) C9 0.061(4) 0.064(5) 0.054(4) 0.014(3) 0.015(3) 0.017(3) C7 0.050(4) 0.072(5) 0.048(4) -0.001(3) -0.008(3) 0.013(3) C8 0.067(5) 0.065(5) 0.080(5) 0.024(4) 0.025(4) 0.020(4) _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 Br4 C6 1.883(6) . ? Br3 C5 1.895(6) . ? Co2 O4 1.890(4) 2_556 ? Co2 O4 1.890(4) . ? Co2 O3 1.905(4) . ? Co2 O3 1.905(4) 2_556 ? Co2 N3 1.962(5) . ? Co2 N3 1.962(5) 2_556 ? Br5 C13 1.877(7) . ? Br1 C3 1.891(6) . ? Co1 O1 1.890(4) 2_655 ? Co1 O1 1.890(4) . ? Co1 O2 1.899(4) 2_655 ? Co1 O2 1.899(4) . ? Co1 N1 1.928(5) 2_655 ? Co1 N1 1.928(5) . ? Br2 C4 1.903(6) . ? Br8 C16 1.890(7) . ? O1 C1 1.323(7) . ? C5 C4 1.379(9) . ? C5 C6 1.418(9) . ? C11 O3 1.338(7) . ? C11 C16 1.395(8) . ? C11 C12 1.403(9) . ? O4 C12 1.338(7) . ? C4 C3 1.386(9) . ? C6 C1 1.385(8) . ? C13 C12 1.396(8) . ? C13 C14 1.415(9) . ? C10 N1 1.336(8) . ? C10 C9 1.383(10) . ? N1 C7 1.356(8) . ? O2 C2 1.312(7) . ? C16 C15 1.400(9) . ? C3 C2 1.398(8) . ? C2 C1 1.428(8) . ? N3 C20 1.333(8) . ? N3 C17 1.334(8) . ? C15 C14 1.376(10) . ? C15 Br7 1.887(6) . ? Br6 C14 1.897(6) . ? N5 C23 1.420(17) . ? N5 C21 1.47(2) . ? N5 C25 1.56(3) . ? C24 C23 1.31(2) . ? C22 C21 1.30(2) . ? C26 C25 1.28(3) . ? N4 C17 1.320(9) . ? N4 C18 1.325(10) . ? C20 C19 1.376(9) . ? C18 C19 1.354(10) . ? N2 C7 1.306(10) . ? N2 C8 1.337(11) . ? C9 C8 1.359(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Co2 O4 180.00(13) 2_556 . ? O4 Co2 O3 92.87(17) 2_556 . ? O4 Co2 O3 87.13(17) . . ? O4 Co2 O3 87.13(17) 2_556 2_556 ? O4 Co2 O3 92.87(17) . 2_556 ? O3 Co2 O3 180.0(2) . 2_556 ? O4 Co2 N3 90.31(19) 2_556 . ? O4 Co2 N3 89.69(19) . . ? O3 Co2 N3 93.69(19) . . ? O3 Co2 N3 86.31(19) 2_556 . ? O4 Co2 N3 89.69(19) 2_556 2_556 ? O4 Co2 N3 90.31(19) . 2_556 ? O3 Co2 N3 86.31(19) . 2_556 ? O3 Co2 N3 93.69(19) 2_556 2_556 ? N3 Co2 N3 180.000(1) . 2_556 ? O1 Co1 O1 180.0(3) 2_655 . ? O1 Co1 O2 87.46(17) 2_655 2_655 ? O1 Co1 O2 92.54(17) . 2_655 ? O1 Co1 O2 92.54(17) 2_655 . ? O1 Co1 O2 87.46(17) . . ? O2 Co1 O2 180.0(3) 2_655 . ? O1 Co1 N1 90.16(19) 2_655 2_655 ? O1 Co1 N1 89.84(19) . 2_655 ? O2 Co1 N1 89.7(2) 2_655 2_655 ? O2 Co1 N1 90.3(2) . 2_655 ? O1 Co1 N1 89.84(19) 2_655 . ? O1 Co1 N1 90.16(19) . . ? O2 Co1 N1 90.3(2) 2_655 . ? O2 Co1 N1 89.7(2) . . ? N1 Co1 N1 180.0(5) 2_655 . ? C1 O1 Co1 109.5(3) . . ? C4 C5 C6 118.8(5) . . ? C4 C5 Br3 121.6(5) . . ? C6 C5 Br3 119.6(4) . . ? O3 C11 C16 124.4(6) . . ? O3 C11 C12 116.8(5) . . ? C16 C11 C12 118.8(5) . . ? C12 O4 Co2 108.9(4) . . ? C5 C4 C3 120.8(6) . . ? C5 C4 Br2 120.2(5) . . ? C3 C4 Br2 119.0(5) . . ? C11 O3 Co2 108.1(3) . . ? C1 C6 C5 120.9(5) . . ? C1 C6 Br4 117.0(5) . . ? C5 C6 Br4 122.0(4) . . ? C12 C13 C14 119.0(6) . . ? C12 C13 Br5 118.6(5) . . ? C14 C13 Br5 122.5(4) . . ? N1 C10 C9 120.9(6) . . ? C10 N1 C7 116.7(6) . . ? C10 N1 Co1 122.8(4) . . ? C7 N1 Co1 120.4(5) . . ? C2 O2 Co1 108.9(3) . . ? C11 C16 C15 121.5(6) . . ? C11 C16 Br8 117.1(5) . . ? C15 C16 Br8 121.3(5) . . ? C4 C3 C2 121.4(5) . . ? C4 C3 Br1 122.8(5) . . ? C2 C3 Br1 115.8(4) . . ? O2 C2 C3 124.1(5) . . ? O2 C2 C1 117.6(5) . . ? C3 C2 C1 118.3(5) . . ? C20 N3 C17 117.1(5) . . ? C20 N3 Co2 120.3(4) . . ? C17 N3 Co2 122.4(4) . . ? O4 C12 C13 122.5(6) . . ? O4 C12 C11 117.0(5) . . ? C13 C12 C11 120.6(5) . . ? C14 C15 C16 118.9(6) . . ? C14 C15 Br7 121.1(5) . . ? C16 C15 Br7 119.9(5) . . ? O1 C1 C6 124.3(5) . . ? O1 C1 C2 116.1(5) . . ? C6 C1 C2 119.5(5) . . ? C15 C14 C13 121.2(6) . . ? C15 C14 Br6 120.3(5) . . ? C13 C14 Br6 118.5(5) . . ? C23 N5 C21 109.4(16) . . ? C23 N5 C25 127.7(16) . . ? C21 N5 C25 113.8(17) . . ? C24 C23 N5 126.9(17) . . ? C22 C21 N5 125.7(18) . . ? C26 C25 N5 107(2) . . ? C17 N4 C18 116.7(6) . . ? N4 C17 N3 125.1(6) . . ? N3 C20 C19 121.2(6) . . ? N4 C18 C19 122.8(6) . . ? C18 C19 C20 117.1(7) . . ? C7 N2 C8 117.1(7) . . ? C8 C9 C10 117.7(7) . . ? N2 C7 N1 125.4(7) . . ? N2 C8 C9 122.2(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.329 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.162 data_Complex9 _database_code_depnum_ccdc_archive 'CCDC 909993' #TrackingRef 'complex9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H70 Br12 Co3 N15 O20' _chemical_formula_weight 2204.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 18.519(3) _cell_length_b 14.082(3) _cell_length_c 26.628(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.790(3) _cell_angle_gamma 90.00 _cell_volume 6941(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17580 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4211 _exptl_absorpt_coefficient_mu 7.691 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4753 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 31908 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 27.50 _reflns_number_total 27800 _reflns_number_gt 21296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0726P)^2^+50.6232P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.065(10) _refine_ls_number_reflns 27800 _refine_ls_number_parameters 1604 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Br14 Br 0.48228(6) 0.14345(9) 1.17714(4) 0.0268(2) Uani 1 1 d . . . Br13 Br 0.43055(6) 0.27932(8) 1.07936(4) 0.0228(2) Uani 1 1 d . . . Br22 Br 0.81825(6) 0.65002(9) 0.67598(4) 0.0295(3) Uani 1 1 d . . . Br24 Br 1.11269(6) 0.71139(9) 0.62436(4) 0.0275(3) Uani 1 1 d . . . Br19 Br 0.74525(7) 0.68842(9) -0.13522(4) 0.0294(3) Uani 1 1 d . . . Br17 Br 1.04730(7) 0.77309(10) -0.13668(5) 0.0331(3) Uani 1 1 d . . . Br8 Br 0.54744(6) 0.35700(8) 0.75825(4) 0.0263(2) Uani 1 1 d . . . Br9 Br 0.70985(7) 0.14726(9) 0.38574(5) 0.0331(3) Uani 1 1 d . . . Br20 Br 0.73968(6) 0.79673(11) -0.02311(5) 0.0359(3) Uani 1 1 d . . . Br21 Br 0.76870(6) 0.74127(10) 0.56500(5) 0.0353(3) Uani 1 1 d . . . Br15 Br 0.65545(7) 0.08483(10) 1.19058(5) 0.0382(3) Uani 1 1 d . . . Br7 Br 0.67083(8) 0.53025(8) 0.75655(5) 0.0336(3) Uani 1 1 d . . . Br18 Br 0.89869(7) 0.69826(9) -0.19643(4) 0.0330(3) Uani 1 1 d . . . Br16 Br 0.77324(6) 0.17969(10) 1.11291(5) 0.0370(3) Uani 1 1 d . . . Br3 Br 0.05650(7) 0.37602(9) 0.74274(5) 0.0332(3) Uani 1 1 d . . . Br12 Br 0.40002(7) 0.32111(10) 0.45310(7) 0.0456(4) Uani 1 1 d . . . Br10 Br 0.56340(8) 0.11227(10) 0.31186(5) 0.0423(3) Uani 1 1 d . . . Br23 Br 0.99390(7) 0.63061(10) 0.70519(4) 0.0323(3) Uani 1 1 d . . . Br4 Br 0.06076(7) 0.14029(10) 0.75396(6) 0.0409(3) Uani 1 1 d . . . Br2 Br 0.20879(8) 0.49046(9) 0.72107(6) 0.0412(3) Uani 1 1 d . . . Br11 Br 0.40758(8) 0.20447(10) 0.34418(6) 0.0420(3) Uani 1 1 d . . . Co6 Co 0.98309(8) 0.84048(11) 0.47585(6) 0.0219(3) Uani 1 1 d . . . Co5 Co 0.98411(8) 0.88927(11) 0.03143(6) 0.0202(3) Uani 1 1 d . . . Br6 Br 0.84292(8) 0.47253(10) 0.76758(7) 0.0542(5) Uani 1 1 d . . . Co4 Co 0.64314(8) 0.36104(10) 0.98116(5) 0.0182(3) Uani 1 1 d . . . Co3 Co 0.63902(9) 0.34179(12) 0.53231(6) 0.0269(4) Uani 1 1 d . . . Br5 Br 0.88965(7) 0.24549(11) 0.76827(9) 0.0651(6) Uani 1 1 d . . . Co2 Co 0.67435(8) 0.04599(10) 0.75730(7) 0.0239(4) Uani 1 1 d . . . Co1 Co 0.30755(9) 0.02441(12) 0.73260(8) 0.0347(4) Uani 1 1 d . . . O12 O 0.8993(4) 0.7941(6) 0.5053(3) 0.0254(17) Uani 1 1 d . . . O8 O 0.5592(4) 0.3326(5) 1.0178(3) 0.0198(16) Uani 1 1 d . . . O5 O 0.5450(4) 0.3266(6) 0.5055(3) 0.0267(18) Uani 1 1 d . . . O1 O 0.2108(4) 0.0655(6) 0.7387(4) 0.033(2) Uani 1 1 d . . . O10 O 1.0146(4) 0.8397(6) -0.0311(3) 0.0274(19) Uani 1 1 d . . . O9 O 0.8889(4) 0.8582(6) 0.0110(3) 0.0281(19) Uani 1 1 d . . . O2 O 0.3337(4) 0.1545(6) 0.7259(4) 0.037(2) Uani 1 1 d . . . O33 O 0.7481(7) 0.1025(10) 0.5544(6) 0.086(4) Uani 1 1 d . . . O32 O 0.5949(10) 0.6779(11) 0.3660(6) 0.108(6) Uani 1 1 d . . . O31 O 0.7614(11) 0.6877(13) 0.1395(6) 0.113(6) Uani 1 1 d . . . O34 O 0.9940(11) 0.0513(13) 0.8899(7) 0.122(6) Uani 1 1 d . . . C75 C 0.7080(12) 0.0326(13) 0.5241(7) 0.077(6) Uani 1 1 d . . . C76 C 0.9452(11) 0.0190(14) 0.8546(9) 0.083(7) Uani 1 1 d . . . C73 C 0.7112(16) 0.766(2) 0.1340(10) 0.116(9) Uani 1 1 d . . . O35 O 0.9723(18) 0.956(2) 0.6503(13) 0.225(15) Uani 1 1 d . . . C77 C 0.925(2) 0.984(3) 0.6139(8) 0.141(16) Uani 1 1 d . . . C74 C 0.641(2) 0.728(2) 0.4058(10) 0.135(12) Uani 1 1 d . . . O37 O 0.4722(5) 0.1362(7) 0.7791(4) 0.048(2) Uani 1 1 d . . . O38 O 0.8215(5) 0.2372(7) 0.4971(4) 0.047(2) Uani 1 1 d . . . O39 O 0.1632(6) 0.8791(9) 0.9601(4) 0.060(3) Uani 1 1 d . . . O40 O 0.1327(11) 0.9969(14) 0.8675(9) 0.145(8) Uani 1 1 d . . . N20 N 0.9661(6) 1.0160(7) 0.0015(4) 0.038(3) Uani 1 1 d . . . H20A H 1.0071 1.0386 -0.0113 0.045 Uiso 1 1 calc R . . H20B H 0.9326 1.0114 -0.0236 0.045 Uiso 1 1 calc R . . O7 O 0.6966(4) 0.2945(6) 1.0316(3) 0.0249(17) Uani 1 1 d . . . N24 N 1.0695(5) 0.8919(7) 0.4453(4) 0.025(2) Uani 1 1 d . . . H24A H 1.0993 0.9161 0.4694 0.030 Uiso 1 1 calc R . . H24B H 1.0931 0.8450 0.4297 0.030 Uiso 1 1 calc R . . O36 O 0.5743(6) 0.0719(8) 0.9808(4) 0.054(3) Uani 1 1 d . . . O4 O 0.7582(4) 0.1202(6) 0.7603(4) 0.042(2) Uani 1 1 d . . . N16 N 0.6480(5) 0.4797(7) 1.0178(4) 0.029(2) Uani 1 1 d . . . H16A H 0.6271 0.4727 1.0477 0.035 Uiso 1 1 calc R . . H16B H 0.6944 0.4962 1.0235 0.035 Uiso 1 1 calc R . . N15 N 0.7299(5) 0.3889(7) 0.9440(3) 0.021(2) Uani 1 1 d . . . H15A H 0.7534 0.4386 0.9581 0.025 Uiso 1 1 calc R . . H15B H 0.7597 0.3384 0.9450 0.025 Uiso 1 1 calc R . . O16 O 0.4847(6) 0.5518(9) 0.4291(4) 0.062(3) Uani 1 1 d . . . O22 O 0.4332(6) 1.0256(9) 0.8913(4) 0.058(3) Uani 1 1 d . . . O11 O 1.0370(4) 0.7827(6) 0.5293(3) 0.0214(16) Uani 1 1 d . . . C64 C 0.8897(6) 0.6922(8) 0.6310(4) 0.023(2) Uani 1 1 d . . . N6 N 0.5885(5) -0.0347(7) 0.7542(4) 0.030(2) Uani 1 1 d . . . H6A H 0.5543 -0.0102 0.7736 0.036 Uiso 1 1 calc R . . H6B H 0.5707 -0.0375 0.7224 0.036 Uiso 1 1 calc R . . N12 N 0.6432(5) 0.4617(7) 0.4930(4) 0.032(2) Uani 1 1 d . . . H12A H 0.6893 0.4748 0.4860 0.039 Uiso 1 1 calc R . . H12B H 0.6181 0.4547 0.4637 0.039 Uiso 1 1 calc R . . N28 N 0.4849(8) 0.9972(9) 0.8689(5) 0.047(3) Uani 1 1 d . . . O26 O 0.7608(6) 0.1808(8) 0.8980(4) 0.060(3) Uani 1 1 d . . . O3 O 0.6214(4) 0.1611(5) 0.7600(3) 0.029(2) Uani 1 1 d . . . C38 C 0.5771(5) 0.2832(8) 1.0576(4) 0.019(2) Uani 1 1 d . . . N3 N 0.2887(6) 0.0104(8) 0.6611(5) 0.045(3) Uani 1 1 d . . . H3A H 0.2561 0.0540 0.6504 0.054 Uiso 1 1 calc R . . H3B H 0.3297 0.0196 0.6445 0.054 Uiso 1 1 calc R . . O21 O 0.8980(5) 0.5631(7) 0.4774(5) 0.055(3) Uani 1 1 d . . . N8 N 0.6813(5) 0.0515(7) 0.6848(4) 0.030(2) Uani 1 1 d . . . H8A H 0.6367 0.0529 0.6704 0.036 Uiso 1 1 calc R . . H8B H 0.7046 0.1048 0.6761 0.036 Uiso 1 1 calc R . . C44 C 0.5740(6) 0.2648(8) 0.8983(5) 0.033(3) Uani 1 1 d . . . H44A H 0.5391 0.2138 0.8945 0.039 Uiso 1 1 calc R . . H44B H 0.6004 0.2698 0.8675 0.039 Uiso 1 1 calc R . . C5 C 0.1453(7) 0.3099(8) 0.7375(4) 0.025(3) Uani 1 1 d . . . C57 C 1.0178(7) 0.9720(10) 0.1262(5) 0.038(3) Uani 1 1 d . . . H57A H 1.0138 1.0395 0.1327 0.046 Uiso 1 1 calc R . . H57B H 1.0184 0.9391 0.1582 0.046 Uiso 1 1 calc R . . O18 O 0.5658(6) 0.4691(7) 0.3909(4) 0.044(2) Uani 1 1 d . . . C52 C 0.8947(6) 0.7412(8) -0.1299(4) 0.023(2) Uani 1 1 d . . . C48 C 0.6099(7) 0.5555(9) 0.9881(5) 0.031(3) Uani 1 1 d . . . H48A H 0.6442 0.5894 0.9679 0.037 Uiso 1 1 calc R . . H48B H 0.5882 0.6006 1.0107 0.037 Uiso 1 1 calc R . . O19 O 0.8050(7) 0.4763(10) 0.4808(6) 0.093(5) Uani 1 1 d . . . C25 C 0.5472(6) 0.2813(7) 0.4625(4) 0.021(2) Uani 1 1 d . . . C32 C 0.5896(9) 0.2586(11) 0.6231(5) 0.045(4) Uani 1 1 d . . . H32A H 0.6274 0.2636 0.6490 0.054 Uiso 1 1 calc R . . H32B H 0.5547 0.2118 0.6334 0.054 Uiso 1 1 calc R . . O6 O 0.6716(4) 0.2679(6) 0.4776(3) 0.0292(19) Uani 1 1 d . . . C59 C 0.9058(7) 1.0218(10) 0.0810(5) 0.036(3) Uani 1 1 d . . . H59A H 0.8975 1.0604 0.1104 0.043 Uiso 1 1 calc R . . H59B H 0.8595 0.9980 0.0684 0.043 Uiso 1 1 calc R . . C55 C 0.9132(6) 0.8607(10) 0.1189(5) 0.032(3) Uani 1 1 d . . . H55A H 0.9045 0.8757 0.1537 0.039 Uiso 1 1 calc R . . H55B H 0.8670 0.8518 0.1014 0.039 Uiso 1 1 calc R . . N10 N 0.6210(6) 0.2303(8) 0.5745(4) 0.038(3) Uani 1 1 d . . . H10A H 0.5904 0.1907 0.5580 0.046 Uiso 1 1 calc R . . H10B H 0.6628 0.1991 0.5805 0.046 Uiso 1 1 calc R . . N30 N 0.8309(8) 0.1955(12) 0.6371(6) 0.069(4) Uani 1 1 d . . . N18 N 0.9868(5) 0.7643(7) 0.0642(3) 0.024(2) Uani 1 1 d . . . H18A H 0.9603 0.7226 0.0458 0.029 Uiso 1 1 calc R . . H18B H 1.0326 0.7430 0.0663 0.029 Uiso 1 1 calc R . . N19 N 1.0802(5) 0.9224(7) 0.0532(4) 0.029(2) Uani 1 1 d . . . H19A H 1.1090 0.8713 0.0504 0.034 Uiso 1 1 calc R . . H19B H 1.0969 0.9681 0.0330 0.034 Uiso 1 1 calc R . . N5 N 0.7305(5) -0.0704(6) 0.7534(4) 0.027(2) Uani 1 1 d . . . N9 N 0.6024(6) 0.4169(8) 0.5871(4) 0.035(3) Uani 1 1 d . . . O24 O 0.5491(6) 1.0178(8) 0.8830(4) 0.057(3) Uani 1 1 d . . . C40 C 0.5512(6) 0.1908(8) 1.1329(4) 0.018(2) Uani 1 1 d . . . N7 N 0.6841(5) 0.0360(7) 0.8292(4) 0.032(2) Uani 1 1 d . . . H7A H 0.7031 0.0901 0.8419 0.038 Uiso 1 1 calc R . . H7B H 0.6403 0.0277 0.8422 0.038 Uiso 1 1 calc R . . N17 N 0.9541(5) 0.9400(7) 0.0951(4) 0.026(2) Uani 1 1 d . . . O17 O 0.4705(6) 0.5126(9) 0.3507(4) 0.064(3) Uani 1 1 d . . . C49 C 0.8878(6) 0.8187(8) -0.0340(4) 0.018(2) Uani 1 1 d . . . C66 C 1.0109(6) 0.7157(7) 0.6095(4) 0.020(2) Uani 1 1 d . . . N23 N 0.9702(6) 0.9563(7) 0.5130(4) 0.029(2) Uani 1 1 d . . . H23A H 0.9545 0.9420 0.5437 0.035 Uiso 1 1 calc R . . H23B H 1.0131 0.9857 0.5169 0.035 Uiso 1 1 calc R . . N4 N 0.4050(6) -0.0215(8) 0.7264(5) 0.044(3) Uani 1 1 d . . . H4A H 0.4245 0.0058 0.6994 0.052 Uiso 1 1 calc R . . H4B H 0.4315 -0.0039 0.7537 0.052 Uiso 1 1 calc R . . C43 C 0.5355(6) 0.3593(8) 0.9094(4) 0.024(2) Uani 1 1 d . . . H43A H 0.5119 0.3833 0.8790 0.028 Uiso 1 1 calc R . . H43B H 0.4990 0.3491 0.9342 0.028 Uiso 1 1 calc R . . C35 C 0.5664(7) 0.4992(10) 0.5608(5) 0.038(3) Uani 1 1 d . . . H35A H 0.5212 0.4781 0.5452 0.046 Uiso 1 1 calc R . . H35B H 0.5554 0.5476 0.5854 0.046 Uiso 1 1 calc R . . N22 N 0.9807(6) 0.7247(7) 0.4344(4) 0.037(3) Uani 1 1 d . . . H22A H 1.0260 0.7066 0.4278 0.045 Uiso 1 1 calc R . . H22B H 0.9594 0.6773 0.4511 0.045 Uiso 1 1 calc R . . C42 C 0.6720(6) 0.2043(8) 1.1056(4) 0.025(2) Uani 1 1 d . . . C71 C 0.9752(7) 0.9535(11) 0.3880(6) 0.044(4) Uani 1 1 d . . . H71A H 0.9772 0.9187 0.3566 0.053 Uiso 1 1 calc R . . H71B H 0.9553 1.0158 0.3806 0.053 Uiso 1 1 calc R . . N13 N 0.5886(5) 0.4282(7) 0.9285(3) 0.023(2) Uani 1 1 d . . . N21 N 0.9251(6) 0.9013(8) 0.4233(4) 0.036(3) Uani 1 1 d . . . N14 N 0.6239(5) 0.2460(6) 0.9411(3) 0.023(2) Uani 1 1 d . . . H14A H 0.6658 0.2235 0.9297 0.028 Uiso 1 1 calc R . . H14B H 0.6048 0.2012 0.9608 0.028 Uiso 1 1 calc R . . C13 C 0.6670(6) 0.2338(8) 0.7607(4) 0.025(3) Uani 1 1 d . . . C21 C 0.7779(7) -0.0681(9) 0.8013(6) 0.035(3) Uani 1 1 d . . . H21A H 0.8007 -0.1293 0.8068 0.043 Uiso 1 1 calc R . . H21B H 0.8153 -0.0205 0.7985 0.043 Uiso 1 1 calc R . . O15 O 0.8900(6) 0.6076(7) 0.0252(6) 0.070(4) Uani 1 1 d . . . C14 C 0.7399(6) 0.2100(8) 0.7624(6) 0.034(3) Uani 1 1 d . . . O13 O 0.7783(7) 0.5909(10) 0.0505(6) 0.082(4) Uani 1 1 d . . . O23 O 0.4769(6) 0.9454(8) 0.8304(4) 0.057(3) Uani 1 1 d . . . N2 N 0.3148(6) 0.0290(9) 0.8044(6) 0.061(4) Uani 1 1 d . . . H2A H 0.3610 0.0398 0.8140 0.073 Uiso 1 1 calc R . . H2B H 0.2881 0.0778 0.8153 0.073 Uiso 1 1 calc R . . C17 C 0.6990(7) 0.4014(8) 0.7605(4) 0.025(3) Uani 1 1 d . . . C56 C 0.9573(7) 0.7724(10) 0.1158(4) 0.032(3) Uani 1 1 d . . . H56A H 0.9275 0.7175 0.1228 0.039 Uiso 1 1 calc R . . H56B H 0.9967 0.7744 0.1407 0.039 Uiso 1 1 calc R . . O30 O 0.8734(7) 0.2369(12) 0.6135(4) 0.092(5) Uani 1 1 d . . . C37 C 0.6508(6) 0.2605(7) 1.0637(4) 0.017(2) Uani 1 1 d . . . C39 C 0.5282(5) 0.2476(7) 1.0920(3) 0.0123(19) Uani 1 1 d . . . C47 C 0.5523(7) 0.5109(8) 0.9546(5) 0.029(3) Uani 1 1 d . . . H47A H 0.5338 0.5566 0.9301 0.035 Uiso 1 1 calc R . . H47B H 0.5125 0.4885 0.9743 0.035 Uiso 1 1 calc R . . O29 O 0.7690(7) 0.2264(10) 0.6450(5) 0.080(4) Uani 1 1 d . . . C23 C 0.7738(7) -0.0637(10) 0.7077(6) 0.039(3) Uani 1 1 d . . . H23C H 0.7944 -0.1248 0.6994 0.047 Uiso 1 1 calc R . . H23D H 0.8126 -0.0179 0.7123 0.047 Uiso 1 1 calc R . . N27 N 0.8363(7) 0.5440(8) 0.4628(5) 0.044(3) Uani 1 1 d . . . O27 O 0.8534(7) 0.2253(10) 0.9438(6) 0.086(4) Uani 1 1 d . . . C27 C 0.6190(6) 0.1956(8) 0.4023(4) 0.025(3) Uani 1 1 d . . . C22 C 0.7315(7) -0.0452(9) 0.8435(5) 0.033(3) Uani 1 1 d . . . H22C H 0.7611 -0.0289 0.8729 0.040 Uiso 1 1 calc R . . H22D H 0.7022 -0.0999 0.8516 0.040 Uiso 1 1 calc R . . C69 C 0.8764(7) 0.9695(11) 0.4495(5) 0.039(3) Uani 1 1 d . . . H69A H 0.8554 1.0140 0.4253 0.047 Uiso 1 1 calc R . . H69B H 0.8375 0.9350 0.4648 0.047 Uiso 1 1 calc R . . C7 C 0.2441(10) -0.1126(11) 0.7887(6) 0.059(5) Uani 1 1 d . . . H7C H 0.2375 -0.1784 0.7982 0.070 Uiso 1 1 calc R . . H7D H 0.1968 -0.0831 0.7859 0.070 Uiso 1 1 calc R . . C41 C 0.6235(6) 0.1674(8) 1.1383(4) 0.026(3) Uani 1 1 d . . . C36 C 0.6125(8) 0.5413(9) 0.5217(6) 0.042(3) Uani 1 1 d . . . H36A H 0.5838 0.5822 0.4996 0.050 Uiso 1 1 calc R . . H36B H 0.6509 0.5789 0.5374 0.050 Uiso 1 1 calc R . . C65 C 0.9615(6) 0.6838(7) 0.6433(3) 0.017(2) Uani 1 1 d . . . C1 C 0.2080(6) 0.1589(8) 0.7370(5) 0.028(3) Uani 1 1 d . . . C54 C 0.8263(6) 0.7849(8) -0.0579(4) 0.022(2) Uani 1 1 d . . . O14 O 0.8046(7) 0.5608(8) -0.0248(5) 0.065(3) Uani 1 1 d . . . C45 C 0.6382(7) 0.4636(9) 0.8899(5) 0.030(3) Uani 1 1 d . . . H45A H 0.6471 0.5308 0.8953 0.036 Uiso 1 1 calc R . . H45B H 0.6153 0.4561 0.8568 0.036 Uiso 1 1 calc R . . C53 C 0.8297(6) 0.7440(8) -0.1064(4) 0.021(2) Uani 1 1 d . . . C24 C 0.7205(7) -0.0316(9) 0.6673(5) 0.034(3) Uani 1 1 d . . . H24C H 0.7459 -0.0158 0.6371 0.041 Uiso 1 1 calc R . . H24D H 0.6868 -0.0825 0.6593 0.041 Uiso 1 1 calc R . . N25 N 0.8262(7) 0.5872(9) 0.0180(5) 0.048(3) Uani 1 1 d . . . N26 N 0.5072(7) 0.5101(11) 0.3915(5) 0.052(3) Uani 1 1 d . . . C50 C 0.9558(6) 0.8106(8) -0.0576(4) 0.018(2) Uani 1 1 d . . . C18 C 0.6480(6) 0.3297(8) 0.7600(4) 0.023(2) Uani 1 1 d . . . C61 C 0.9922(6) 0.7514(8) 0.5623(4) 0.023(2) Uani 1 1 d . . . C62 C 0.9169(6) 0.7569(8) 0.5500(4) 0.022(2) Uani 1 1 d . . . C70 C 0.9187(8) 1.0213(10) 0.4883(6) 0.041(3) Uani 1 1 d . . . H70A H 0.9445 1.0733 0.4731 0.049 Uiso 1 1 calc R . . H70B H 0.8867 1.0475 0.5129 0.049 Uiso 1 1 calc R . . N11 N 0.7342(5) 0.3582(8) 0.5614(4) 0.031(2) Uani 1 1 d . . . H11A H 0.7467 0.3068 0.5797 0.037 Uiso 1 1 calc R . . H11B H 0.7663 0.3651 0.5369 0.037 Uiso 1 1 calc R . . C19 C 0.6809(7) -0.1558(8) 0.7529(5) 0.031(3) Uani 1 1 d . . . H19C H 0.6757 -0.1803 0.7190 0.037 Uiso 1 1 calc R . . H19D H 0.7021 -0.2053 0.7740 0.037 Uiso 1 1 calc R . . O25 O 0.8246(10) 0.0749(10) 0.9388(8) 0.129(8) Uani 1 1 d . . . C63 C 0.8672(6) 0.7273(7) 0.5847(4) 0.020(2) Uani 1 1 d . . . C9 C 0.2283(9) -0.1244(10) 0.6954(7) 0.056(5) Uani 1 1 d . . . H9A H 0.2184 -0.1917 0.6918 0.067 Uiso 1 1 calc R . . H9B H 0.1828 -0.0921 0.7006 0.067 Uiso 1 1 calc R . . O20 O 0.8079(10) 0.5890(11) 0.4279(7) 0.121(7) Uani 1 1 d . . . C51 C 0.9564(6) 0.7756(8) -0.1046(4) 0.024(2) Uani 1 1 d . . . C15 C 0.7911(6) 0.2825(9) 0.7643(6) 0.037(3) Uani 1 1 d . . . C2 C 0.2723(6) 0.2073(8) 0.7300(5) 0.028(3) Uani 1 1 d . . . C16 C 0.7715(7) 0.3760(9) 0.7635(5) 0.033(3) Uani 1 1 d . . . N1 N 0.2786(6) -0.1083(8) 0.7400(5) 0.038(3) Uani 1 1 d . . . N29 N 0.8142(8) 0.1594(10) 0.9255(5) 0.058(4) Uani 1 1 d . . . C28 C 0.5582(7) 0.1800(7) 0.3724(4) 0.023(2) Uani 1 1 d . . . C26 C 0.6147(6) 0.2469(8) 0.4464(4) 0.021(2) Uani 1 1 d . . . C29 C 0.4916(6) 0.2207(8) 0.3859(4) 0.025(3) Uani 1 1 d . . . C34 C 0.7350(8) 0.4443(10) 0.5940(5) 0.041(3) Uani 1 1 d . . . H34A H 0.7742 0.4399 0.6189 0.049 Uiso 1 1 calc R . . H34B H 0.7425 0.5006 0.5739 0.049 Uiso 1 1 calc R . . C33 C 0.6661(8) 0.4511(12) 0.6190(6) 0.049(4) Uani 1 1 d . . . H33A H 0.6580 0.5167 0.6282 0.058 Uiso 1 1 calc R . . H33B H 0.6689 0.4140 0.6497 0.058 Uiso 1 1 calc R . . C67 C 0.8861(8) 0.8246(11) 0.3962(5) 0.047(4) Uani 1 1 d . . . H67A H 0.8651 0.8488 0.3649 0.057 Uiso 1 1 calc R . . H67B H 0.8474 0.8010 0.4165 0.057 Uiso 1 1 calc R . . C68 C 0.9386(9) 0.7448(11) 0.3855(6) 0.048(4) Uani 1 1 d . . . H68A H 0.9712 0.7636 0.3595 0.057 Uiso 1 1 calc R . . H68B H 0.9126 0.6885 0.3743 0.057 Uiso 1 1 calc R . . C4 C 0.2091(6) 0.3559(8) 0.7300(4) 0.026(3) Uani 1 1 d . . . C60 C 0.9403(8) 1.0823(10) 0.0408(6) 0.042(3) Uani 1 1 d . . . H60A H 0.9052 1.1264 0.0262 0.050 Uiso 1 1 calc R . . H60B H 0.9805 1.1184 0.0552 0.050 Uiso 1 1 calc R . . C72 C 1.0503(8) 0.9647(15) 0.4096(7) 0.072(6) Uani 1 1 d . . . H72A H 1.0842 0.9635 0.3826 0.087 Uiso 1 1 calc R . . H72B H 1.0544 1.0261 0.4260 0.087 Uiso 1 1 calc R . . O28 O 0.8457(8) 0.1174(11) 0.6584(5) 0.088(5) Uani 1 1 d . . . C12 C 0.4087(9) -0.1235(11) 0.7212(8) 0.061(5) Uani 1 1 d . . . H12C H 0.4513 -0.1464 0.7395 0.073 Uiso 1 1 calc R . . H12D H 0.4143 -0.1389 0.6860 0.073 Uiso 1 1 calc R . . C78 C 0.6347(11) 0.0187(15) 1.0031(9) 0.079(6) Uani 1 1 d . . . C30 C 0.4872(6) 0.2680(8) 0.4303(4) 0.022(2) Uani 1 1 d . . . C11 C 0.3461(8) -0.1729(11) 0.7391(7) 0.058(5) Uani 1 1 d . . . H11C H 0.3567 -0.1965 0.7728 0.070 Uiso 1 1 calc R . . H11D H 0.3357 -0.2271 0.7176 0.070 Uiso 1 1 calc R . . C10 C 0.2595(8) -0.0893(11) 0.6502(7) 0.055(5) Uani 1 1 d . . . H10C H 0.2233 -0.0872 0.6232 0.066 Uiso 1 1 calc R . . H10D H 0.2984 -0.1308 0.6402 0.066 Uiso 1 1 calc R . . C8 C 0.2891(11) -0.0627(14) 0.8288(6) 0.070(5) Uani 1 1 d . . . H8C H 0.3299 -0.1017 0.8395 0.084 Uiso 1 1 calc R . . H8D H 0.2604 -0.0488 0.8577 0.084 Uiso 1 1 calc R . . C6 C 0.1445(6) 0.2110(9) 0.7417(4) 0.026(3) Uani 1 1 d . . . Br1 Br 0.36252(7) 0.36787(10) 0.71756(6) 0.0461(4) Uani 1 1 d . . . C20 C 0.6081(7) -0.1301(9) 0.7717(5) 0.035(3) Uani 1 1 d . . . H20C H 0.5724 -0.1756 0.7594 0.042 Uiso 1 1 calc R . . H20D H 0.6090 -0.1318 0.8081 0.042 Uiso 1 1 calc R . . C46 C 0.7086(7) 0.4112(11) 0.8917(5) 0.037(3) Uani 1 1 d . . . H46A H 0.7039 0.3529 0.8725 0.045 Uiso 1 1 calc R . . H46B H 0.7456 0.4499 0.8768 0.045 Uiso 1 1 calc R . . C3 C 0.2722(6) 0.3055(8) 0.7271(5) 0.032(3) Uani 1 1 d . . . C31 C 0.5529(8) 0.3549(11) 0.6147(5) 0.045(4) Uani 1 1 d . . . H31A H 0.5080 0.3467 0.5955 0.055 Uiso 1 1 calc R . . H31B H 0.5420 0.3834 0.6468 0.055 Uiso 1 1 calc R . . C58 C 1.0839(8) 0.954(2) 0.1016(7) 0.118(12) Uani 1 1 d . . . H58A H 1.1120 1.0118 0.1024 0.142 Uiso 1 1 calc R . . H58B H 1.1108 0.9070 0.1214 0.142 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 Br1 0.0298(7) 0.0339(8) 0.0746(11) -0.0107(7) 0.0052(7) -0.0150(6) Br2 0.0496(8) 0.0186(6) 0.0546(9) -0.0011(6) -0.0120(7) -0.0028(6) Br3 0.0315(7) 0.0384(7) 0.0295(6) -0.0056(5) -0.0018(5) 0.0128(6) Br4 0.0258(7) 0.0383(7) 0.0594(9) 0.0014(7) 0.0136(6) -0.0057(6) Br5 0.0195(7) 0.0395(8) 0.1357(18) 0.0238(10) -0.0085(8) -0.0088(6) Br6 0.0525(9) 0.0324(8) 0.0758(12) 0.0278(8) -0.0292(8) -0.0283(7) Br7 0.0613(9) 0.0131(5) 0.0267(6) 0.0005(5) 0.0063(6) -0.0027(5) Br8 0.0292(6) 0.0220(6) 0.0279(6) 0.0013(5) 0.0015(5) 0.0072(5) Br9 0.0347(7) 0.0349(7) 0.0302(6) -0.0082(6) 0.0095(5) 0.0085(6) Br10 0.0607(9) 0.0429(8) 0.0230(7) -0.0115(6) -0.0031(6) -0.0063(7) Br11 0.0448(8) 0.0296(7) 0.0502(9) 0.0069(6) -0.0220(6) -0.0091(6) Br12 0.0185(6) 0.0425(8) 0.0758(11) -0.0162(7) 0.0018(6) 0.0003(6) Br13 0.0148(5) 0.0257(6) 0.0280(6) 0.0023(5) 0.0014(4) -0.0002(4) Br14 0.0313(6) 0.0288(6) 0.0208(5) 0.0060(5) 0.0080(5) -0.0043(5) Br15 0.0431(8) 0.0425(8) 0.0294(7) 0.0174(6) 0.0063(6) 0.0184(6) Br16 0.0218(6) 0.0546(9) 0.0347(7) 0.0130(6) 0.0032(5) 0.0176(6) Br17 0.0298(6) 0.0419(7) 0.0284(6) -0.0020(5) 0.0138(5) 0.0052(6) Br18 0.0529(8) 0.0266(6) 0.0193(6) -0.0076(5) 0.0002(5) 0.0053(6) Br19 0.0363(7) 0.0260(6) 0.0252(6) 0.0009(5) -0.0087(5) -0.0090(5) Br20 0.0187(6) 0.0592(9) 0.0300(7) -0.0093(6) 0.0029(5) -0.0051(6) Br21 0.0167(6) 0.0472(8) 0.0420(8) 0.0147(6) -0.0009(5) -0.0025(5) Br22 0.0282(6) 0.0368(7) 0.0241(6) 0.0029(5) 0.0104(5) -0.0006(5) Br23 0.0354(7) 0.0438(8) 0.0180(6) 0.0041(5) 0.0030(5) 0.0105(6) Br24 0.0197(6) 0.0356(7) 0.0267(6) 0.0002(5) -0.0033(5) 0.0001(5) Co1 0.0265(9) 0.0228(9) 0.0541(12) -0.0062(8) -0.0081(8) 0.0007(7) Co2 0.0179(8) 0.0115(7) 0.0424(10) 0.0035(7) 0.0018(7) -0.0009(6) Co3 0.0292(9) 0.0318(9) 0.0194(8) -0.0093(7) -0.0024(6) 0.0081(7) Co4 0.0168(7) 0.0188(7) 0.0191(7) 0.0054(6) 0.0028(6) 0.0020(6) Co5 0.0152(7) 0.0220(8) 0.0235(8) -0.0066(6) 0.0016(6) -0.0009(6) Co6 0.0251(8) 0.0199(8) 0.0207(8) 0.0055(6) 0.0013(6) -0.0029(6) O1 0.018(4) 0.024(4) 0.058(6) -0.003(4) 0.001(4) -0.003(3) O2 0.026(5) 0.028(5) 0.057(6) -0.014(4) 0.004(4) -0.003(4) O3 0.013(4) 0.014(4) 0.061(6) 0.001(4) -0.006(4) 0.000(3) O4 0.023(5) 0.026(5) 0.076(7) -0.002(5) 0.004(4) 0.002(4) O5 0.025(4) 0.031(5) 0.024(4) -0.010(4) 0.006(3) 0.003(3) O6 0.034(5) 0.037(5) 0.016(4) -0.008(4) 0.002(3) 0.011(4) O7 0.020(4) 0.035(5) 0.019(4) 0.011(4) 0.001(3) -0.001(3) O8 0.014(4) 0.025(4) 0.020(4) 0.007(3) 0.006(3) 0.003(3) O9 0.017(4) 0.042(5) 0.026(4) -0.013(4) -0.001(3) 0.002(4) O10 0.009(4) 0.037(5) 0.036(5) -0.010(4) 0.005(3) -0.003(3) O11 0.022(4) 0.030(4) 0.012(4) 0.000(3) 0.003(3) -0.004(3) O12 0.027(4) 0.028(4) 0.020(4) 0.010(3) -0.002(3) -0.006(3) O13 0.067(9) 0.078(9) 0.104(12) -0.021(8) 0.019(8) -0.008(7) O14 0.076(8) 0.038(6) 0.083(10) -0.019(6) 0.008(7) -0.007(6) O15 0.047(7) 0.026(5) 0.136(13) -0.005(6) -0.025(7) -0.001(5) O16 0.068(8) 0.080(9) 0.037(6) 0.000(6) 0.004(6) -0.001(7) O17 0.056(7) 0.094(10) 0.041(6) -0.022(6) -0.021(5) 0.015(6) O18 0.052(6) 0.045(6) 0.037(6) 0.012(5) 0.009(5) 0.010(5) O19 0.077(9) 0.056(8) 0.148(15) 0.015(9) 0.025(9) -0.032(7) O20 0.151(15) 0.066(10) 0.140(16) 0.030(10) -0.098(13) -0.012(10) O21 0.026(5) 0.033(6) 0.105(10) -0.004(6) -0.002(5) -0.001(4) O22 0.051(7) 0.079(8) 0.044(6) 0.019(6) 0.031(5) 0.005(6) O23 0.077(8) 0.047(7) 0.049(7) 0.005(5) 0.025(6) 0.014(6) O24 0.045(7) 0.058(7) 0.068(8) 0.014(6) 0.013(6) -0.001(5) O25 0.161(16) 0.042(8) 0.178(19) 0.009(10) -0.096(14) 0.016(9) O26 0.056(7) 0.065(8) 0.058(7) -0.028(6) -0.020(6) 0.023(6) O27 0.080(9) 0.076(9) 0.101(11) -0.033(8) -0.016(8) -0.029(7) O28 0.096(10) 0.084(10) 0.086(10) 0.043(8) 0.028(8) -0.002(8) O29 0.055(8) 0.102(11) 0.084(10) 0.063(8) -0.010(6) 0.001(7) O30 0.070(8) 0.160(15) 0.046(7) 0.051(8) 0.013(6) -0.048(9) O31 0.155(16) 0.106(13) 0.082(11) -0.010(10) 0.039(11) -0.009(12) O32 0.149(15) 0.080(11) 0.098(12) 0.001(9) 0.044(11) -0.036(10) O33 0.072(9) 0.071(9) 0.115(13) 0.014(8) 0.014(8) 0.004(7) O34 0.136(15) 0.098(13) 0.130(16) 0.017(11) -0.022(12) -0.039(12) O35 0.25(3) 0.19(3) 0.25(3) -0.15(3) 0.07(3) 0.00(2) O36 0.047(6) 0.043(6) 0.073(8) 0.003(6) 0.016(6) -0.007(5) O37 0.055(6) 0.038(6) 0.049(6) 0.010(5) -0.012(5) -0.011(5) O38 0.050(6) 0.040(6) 0.050(6) -0.006(5) 0.004(5) 0.002(5) O39 0.046(6) 0.065(8) 0.070(8) -0.023(6) 0.009(5) 0.014(6) O40 0.143(17) 0.106(15) 0.19(2) -0.017(14) 0.030(15) -0.003(13) N1 0.043(7) 0.028(6) 0.042(7) -0.008(5) -0.010(5) -0.005(5) N2 0.025(7) 0.038(7) 0.121(14) 0.005(8) 0.008(7) 0.004(6) N3 0.035(7) 0.039(7) 0.061(9) 0.001(6) -0.010(6) 0.000(5) N4 0.024(6) 0.037(7) 0.069(9) -0.006(6) -0.006(5) 0.001(5) N5 0.034(6) 0.011(4) 0.036(6) 0.005(4) 0.015(5) 0.001(4) N6 0.024(5) 0.030(6) 0.038(6) -0.004(5) 0.012(5) -0.007(4) N7 0.024(5) 0.032(6) 0.039(6) -0.004(5) -0.006(4) -0.006(4) N8 0.023(5) 0.035(6) 0.032(6) 0.009(5) -0.009(4) 0.002(4) N9 0.037(6) 0.038(6) 0.029(6) -0.014(5) -0.002(5) 0.010(5) N10 0.050(7) 0.033(6) 0.031(6) 0.001(5) 0.009(5) 0.007(5) N11 0.035(6) 0.038(6) 0.020(5) -0.004(5) -0.009(4) 0.002(5) N12 0.024(6) 0.029(6) 0.043(7) -0.005(5) 0.001(5) 0.004(4) N13 0.029(5) 0.021(5) 0.017(5) 0.014(4) 0.003(4) 0.010(4) N14 0.033(5) 0.010(4) 0.026(5) 0.001(4) -0.003(4) 0.000(4) N15 0.017(5) 0.027(5) 0.019(5) 0.001(4) 0.007(4) 0.005(4) N16 0.023(5) 0.031(6) 0.034(6) 0.002(5) 0.005(4) 0.001(4) N17 0.021(5) 0.034(6) 0.023(5) -0.011(4) -0.010(4) 0.004(4) N18 0.027(5) 0.023(5) 0.022(5) 0.004(4) 0.008(4) -0.002(4) N19 0.017(5) 0.029(6) 0.039(6) -0.005(5) -0.007(4) -0.006(4) N20 0.053(7) 0.027(6) 0.033(6) -0.002(5) 0.005(5) 0.006(5) N21 0.044(7) 0.030(6) 0.034(6) 0.014(5) -0.008(5) -0.021(5) N22 0.051(7) 0.018(5) 0.042(7) 0.001(5) -0.005(5) -0.013(5) N23 0.039(6) 0.023(5) 0.026(6) -0.004(4) 0.001(4) 0.003(4) N24 0.028(5) 0.017(5) 0.031(6) 0.011(4) 0.001(4) 0.003(4) N25 0.044(8) 0.053(8) 0.049(8) -0.021(7) 0.014(6) 0.011(6) N26 0.038(8) 0.076(10) 0.043(8) 0.004(7) -0.001(6) -0.013(7) N27 0.045(7) 0.022(6) 0.066(9) 0.007(6) -0.008(6) 0.001(5) N28 0.056(9) 0.047(8) 0.040(7) 0.020(6) 0.024(7) 0.015(6) N29 0.062(9) 0.051(9) 0.059(9) -0.014(7) -0.005(7) -0.007(7) N30 0.043(9) 0.071(10) 0.092(12) 0.041(9) -0.002(8) 0.014(8) C1 0.028(7) 0.020(6) 0.037(7) -0.006(5) -0.001(5) -0.001(5) C2 0.029(7) 0.015(6) 0.039(7) -0.003(5) -0.008(5) -0.005(5) C3 0.024(6) 0.020(6) 0.052(8) -0.006(6) -0.002(6) -0.005(5) C4 0.027(6) 0.022(6) 0.029(6) -0.005(5) -0.006(5) 0.000(5) C5 0.038(7) 0.023(6) 0.014(5) -0.001(4) 0.008(5) 0.005(5) C6 0.026(6) 0.032(7) 0.020(6) -0.006(5) 0.001(5) -0.014(5) C7 0.088(12) 0.035(8) 0.051(10) 0.016(7) -0.030(9) -0.020(8) C8 0.097(14) 0.078(13) 0.032(9) 0.009(9) -0.021(9) -0.026(11) C9 0.059(10) 0.019(7) 0.088(13) -0.018(8) -0.033(9) 0.000(7) C10 0.038(9) 0.036(9) 0.091(14) 0.003(9) -0.008(9) -0.004(7) C11 0.051(10) 0.039(9) 0.084(13) 0.013(9) -0.006(9) 0.014(7) C12 0.057(10) 0.027(8) 0.098(15) 0.001(9) 0.002(10) -0.001(7) C13 0.024(6) 0.021(6) 0.029(6) 0.002(5) -0.003(5) -0.008(5) C14 0.016(6) 0.009(5) 0.077(10) 0.003(6) 0.002(6) -0.009(4) C15 0.024(6) 0.021(6) 0.067(10) 0.016(6) -0.016(6) -0.006(5) C16 0.039(8) 0.030(7) 0.031(7) 0.009(5) 0.002(5) -0.017(6) C17 0.039(7) 0.023(6) 0.013(5) 0.009(4) 0.000(5) -0.005(5) C18 0.023(6) 0.022(6) 0.024(6) 0.001(5) -0.009(5) 0.000(5) C19 0.045(8) 0.007(5) 0.040(7) 0.007(5) 0.003(6) 0.003(5) C20 0.035(7) 0.024(7) 0.045(8) -0.008(6) 0.001(6) -0.007(6) C21 0.028(7) 0.019(6) 0.059(9) -0.003(6) -0.006(6) 0.005(5) C22 0.029(7) 0.028(7) 0.041(8) -0.012(6) -0.015(6) 0.006(5) C23 0.033(7) 0.030(7) 0.056(9) 0.013(6) 0.012(6) 0.016(6) C24 0.041(8) 0.030(7) 0.032(7) 0.003(6) 0.007(6) 0.014(6) C25 0.032(6) 0.011(5) 0.020(5) 0.006(4) -0.004(5) -0.004(5) C26 0.016(5) 0.027(6) 0.019(6) -0.005(5) -0.002(4) -0.010(5) C27 0.023(6) 0.026(6) 0.027(6) 0.004(5) 0.009(5) 0.007(5) C28 0.048(7) 0.009(5) 0.014(5) 0.001(4) 0.001(5) -0.013(5) C29 0.037(7) 0.017(6) 0.020(6) 0.002(4) -0.008(5) -0.006(5) C30 0.021(6) 0.022(6) 0.021(6) -0.002(5) -0.003(4) 0.008(5) C31 0.057(9) 0.051(9) 0.029(7) -0.009(7) 0.019(7) 0.004(7) C32 0.067(10) 0.050(9) 0.019(7) -0.004(6) 0.015(6) 0.008(8) C33 0.046(9) 0.063(10) 0.035(8) -0.021(7) -0.012(7) 0.030(8) C34 0.052(9) 0.041(8) 0.029(7) -0.010(6) -0.012(6) 0.005(7) C35 0.035(7) 0.038(8) 0.042(8) -0.019(6) -0.004(6) 0.017(6) C36 0.055(9) 0.022(7) 0.049(9) -0.002(6) -0.003(7) -0.003(6) C37 0.026(6) 0.008(5) 0.018(5) -0.001(4) 0.003(4) -0.005(4) C38 0.016(5) 0.018(5) 0.022(6) 0.000(5) 0.003(4) -0.002(4) C39 0.013(5) 0.015(5) 0.008(4) -0.006(4) 0.005(4) -0.001(4) C40 0.022(6) 0.022(6) 0.011(5) -0.004(4) 0.006(4) -0.009(5) C41 0.030(6) 0.028(7) 0.019(6) 0.010(5) 0.000(5) 0.005(5) C42 0.021(6) 0.026(6) 0.026(6) -0.001(5) -0.009(5) 0.015(5) C43 0.018(6) 0.027(6) 0.026(6) 0.000(5) 0.000(4) -0.004(5) C44 0.020(6) 0.019(6) 0.059(9) 0.012(6) -0.008(6) -0.011(5) C45 0.034(7) 0.033(7) 0.025(6) 0.002(5) 0.003(5) 0.001(5) C46 0.037(8) 0.060(9) 0.015(6) 0.013(6) 0.008(5) 0.001(7) C47 0.038(7) 0.023(6) 0.028(6) 0.007(5) 0.009(5) 0.014(5) C48 0.036(7) 0.022(6) 0.034(7) 0.005(5) 0.007(6) -0.002(5) C49 0.025(6) 0.018(5) 0.012(5) 0.006(4) 0.002(4) -0.005(4) C50 0.019(6) 0.027(6) 0.009(5) -0.001(4) 0.009(4) -0.002(4) C51 0.020(6) 0.017(6) 0.035(7) -0.005(5) 0.005(5) 0.001(5) C52 0.038(7) 0.015(5) 0.015(5) 0.002(4) -0.003(5) -0.002(5) C53 0.026(6) 0.017(5) 0.021(6) -0.002(4) -0.007(5) 0.000(5) C54 0.021(6) 0.025(6) 0.020(5) 0.006(5) -0.003(4) -0.004(5) C55 0.021(6) 0.052(8) 0.024(6) 0.000(6) 0.002(5) -0.013(6) C56 0.036(7) 0.050(8) 0.010(5) 0.011(5) 0.000(5) -0.004(6) C57 0.045(8) 0.035(7) 0.033(7) -0.021(6) -0.013(6) 0.004(6) C58 0.013(8) 0.29(3) 0.057(12) -0.081(17) 0.020(7) -0.056(13) C59 0.024(7) 0.038(7) 0.045(8) -0.018(6) 0.011(6) 0.010(6) C60 0.044(8) 0.029(7) 0.052(9) -0.002(6) -0.004(7) 0.015(6) C61 0.021(6) 0.027(6) 0.021(6) 0.003(5) 0.005(4) -0.004(5) C62 0.030(6) 0.024(6) 0.012(5) 0.003(4) 0.005(4) -0.006(5) C63 0.025(6) 0.010(5) 0.024(6) -0.003(4) -0.001(5) 0.004(4) C64 0.027(6) 0.023(6) 0.018(5) 0.005(5) 0.004(4) 0.005(5) C65 0.032(6) 0.015(5) 0.003(4) -0.002(4) 0.001(4) 0.007(4) C66 0.021(6) 0.012(5) 0.028(6) -0.005(4) -0.011(5) 0.004(4) C67 0.057(9) 0.056(10) 0.027(7) 0.015(7) -0.015(6) -0.028(8) C68 0.064(10) 0.038(8) 0.042(9) 0.001(7) 0.013(7) -0.024(8) C69 0.022(7) 0.051(9) 0.045(8) 0.009(7) 0.004(6) 0.017(6) C70 0.048(9) 0.028(7) 0.046(9) 0.007(6) 0.004(7) 0.011(6) C71 0.040(8) 0.045(9) 0.048(9) 0.014(7) 0.001(7) -0.015(7) C72 0.036(9) 0.091(14) 0.090(14) 0.067(12) 0.014(9) 0.013(9) C73 0.13(2) 0.13(3) 0.091(19) 0.013(17) 0.034(16) 0.03(2) C74 0.23(4) 0.11(2) 0.071(18) -0.012(16) -0.01(2) 0.04(2) C75 0.127(18) 0.046(10) 0.061(12) -0.026(9) 0.042(12) -0.025(11) C76 0.076(13) 0.054(11) 0.118(19) 0.043(12) -0.023(12) -0.025(10) C77 0.21(3) 0.19(3) 0.027(11) -0.036(14) -0.023(15) 0.13(3) C78 0.063(12) 0.067(13) 0.107(18) -0.007(12) -0.004(11) 0.022(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C3 1.914(12) . ? Br2 C4 1.910(12) . ? Br3 C5 1.898(12) . ? Br4 C6 1.881(11) . ? Br5 C15 1.898(12) . ? Br6 C16 1.898(12) . ? Br7 C17 1.890(12) . ? Br8 C18 1.901(11) . ? Br9 C27 1.880(11) . ? Br10 C28 1.878(11) . ? Br11 C29 1.897(11) . ? Br12 C30 1.897(10) . ? Br13 C39 1.883(10) . ? Br14 C40 1.886(10) . ? Br15 C41 1.894(11) . ? Br16 C42 1.910(11) . ? Br17 C51 1.911(11) . ? Br18 C52 1.876(11) . ? Br19 C53 1.890(11) . ? Br20 C54 1.885(11) . ? Br21 C63 1.893(11) . ? Br22 C64 1.907(11) . ? Br23 C65 1.890(10) . ? Br24 C66 1.914(10) . ? Co6 O12 1.877(8) . ? Co6 O11 1.896(7) . ? Co6 N23 1.926(10) . ? Co6 N21 1.938(11) . ? Co6 N24 1.958(9) . ? Co6 N22 1.968(11) . ? Co5 O9 1.881(8) . ? Co5 O10 1.907(8) . ? Co5 N19 1.912(9) . ? Co5 N17 1.937(10) . ? Co5 N18 1.963(9) . ? Co5 N20 1.979(11) . ? Co4 O7 1.891(8) . ? Co4 O8 1.903(7) . ? Co4 N16 1.935(10) . ? Co4 N13 1.948(9) . ? Co4 N15 1.952(8) . ? Co4 N14 1.967(9) . ? Co3 O5 1.873(8) . ? Co3 O6 1.903(7) . ? Co3 N11 1.917(10) . ? Co3 N9 1.942(10) . ? Co3 N10 1.964(11) . ? Co3 N12 1.990(11) . ? Co2 O4 1.872(9) . ? Co2 O3 1.898(7) . ? Co2 N7 1.923(11) . ? Co2 N8 1.940(10) . ? Co2 N5 1.946(9) . ? Co2 N6 1.954(9) . ? Co1 O1 1.895(8) . ? Co1 O2 1.905(9) . ? Co1 N2 1.913(16) . ? Co1 N4 1.929(11) . ? Co1 N3 1.936(13) . ? Co1 N1 1.956(11) . ? O1 C1 1.316(14) . ? O2 C2 1.366(15) . ? O3 C13 1.327(13) . ? O4 C14 1.311(14) . ? O5 C25 1.312(13) . ? O6 C26 1.355(13) . ? O7 C37 1.314(12) . ? O8 C38 1.303(12) . ? O9 C49 1.320(12) . ? O10 C50 1.342(13) . ? O11 C61 1.303(12) . ? O12 C62 1.332(13) . ? O13 N25 1.259(17) . ? O14 N25 1.253(17) . ? O15 N25 1.225(16) . ? O16 N26 1.244(17) . ? O17 N26 1.265(16) . ? O18 N26 1.230(16) . ? O19 N27 1.221(16) . ? O21 N27 1.226(15) . ? O22 N28 1.212(15) . ? O25 N29 1.255(19) . ? O26 N29 1.250(16) . ? O27 N29 1.265(17) . ? O31 C73 1.44(3) . ? O32 C74 1.52(3) . ? O33 C75 1.46(2) . ? O34 C76 1.36(3) . ? O35 C77 1.35(4) . ? O36 C78 1.46(2) . ? N1 C11 1.546(18) . ? N2 C8 1.53(2) . ? N3 C10 1.528(18) . ? N4 C12 1.445(19) . ? N5 C19 1.513(15) . ? N5 C21 1.526(17) . ? N5 C23 1.480(16) . ? N6 C20 1.464(17) . ? N7 C22 1.482(16) . ? N8 C24 1.463(16) . ? N9 C31 1.479(18) . ? N9 C35 1.500(17) . ? N9 C33 1.509(17) . ? N11 C34 1.492(16) . ? N12 C36 1.481(16) . ? N13 C45 1.485(14) . ? N13 C47 1.524(14) . ? N15 C46 1.471(15) . ? N16 C48 1.492(15) . ? N18 C56 1.501(14) . ? N19 C58 1.361(18) . ? N20 C60 1.490(17) . ? N21 C67 1.474(17) . ? N21 C69 1.503(17) . ? N22 C68 1.524(19) . ? N23 C70 1.462(16) . ? N24 C72 1.434(17) . ? N27 O20 1.229(17) . ? N28 O23 1.263(17) . ? N28 O24 1.268(17) . ? N30 O30 1.179(17) . ? N30 O29 1.249(18) . ? N30 O28 1.263(18) . ? C64 C65 1.364(15) . ? C64 C63 1.381(15) . ? C38 C39 1.400(14) . ? C38 C37 1.407(15) . ? C44 N14 1.468(15) . ? C44 C43 1.543(17) . ? C5 C4 1.367(17) . ? C5 C6 1.398(17) . ? C57 C58 1.43(2) . ? C57 N17 1.489(15) . ? C52 C53 1.375(16) . ? C52 C51 1.396(16) . ? C48 C47 1.507(18) . ? C25 C30 1.396(15) . ? C25 C26 1.419(16) . ? C32 N10 1.489(15) . ? C32 C31 1.53(2) . ? C59 N17 1.500(16) . ? C59 C60 1.52(2) . ? C55 C56 1.490(19) . ? C55 N17 1.502(16) . ? C40 C41 1.383(16) . ? C40 C39 1.407(14) . ? C49 C54 1.371(15) . ? C49 C50 1.430(15) . ? C66 C65 1.380(15) . ? C66 C61 1.388(15) . ? C43 N13 1.461(15) . ? C35 C36 1.489(19) . ? C42 C41 1.373(16) . ? C42 C37 1.412(15) . ? C71 C72 1.50(2) . ? C71 N21 1.529(16) . ? C13 C14 1.391(16) . ? C13 C18 1.395(16) . ? C21 C22 1.470(19) . ? C14 C15 1.393(16) . ? C17 C18 1.382(16) . ? C17 C16 1.389(18) . ? C23 C24 1.506(18) . ? C27 C28 1.376(16) . ? C27 C26 1.384(15) . ? C69 C70 1.47(2) . ? C7 N1 1.46(2) . ? C7 C8 1.51(2) . ? C1 C2 1.389(17) . ? C1 C6 1.394(17) . ? C54 C53 1.418(15) . ? C45 C46 1.497(18) . ? C50 C51 1.345(15) . ? C61 C62 1.425(16) . ? C62 C63 1.387(15) . ? C19 C20 1.498(17) . ? C9 C10 1.44(2) . ? C9 N1 1.506(18) . ? C15 C16 1.365(18) . ? C2 C3 1.385(16) . ? C28 C29 1.416(17) . ? C29 C30 1.360(15) . ? C34 C33 1.46(2) . ? C67 C68 1.52(2) . ? C4 C3 1.371(17) . ? C12 C11 1.45(2) . ? 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 O12 Co6 O11 87.7(3) . . ? O12 Co6 N23 87.8(4) . . ? O11 Co6 N23 92.8(4) . . ? O12 Co6 N21 90.5(4) . . ? O11 Co6 N21 177.6(4) . . ? N23 Co6 N21 85.5(5) . . ? O12 Co6 N24 178.6(4) . . ? O11 Co6 N24 93.0(4) . . ? N23 Co6 N24 91.0(4) . . ? N21 Co6 N24 88.7(4) . . ? O12 Co6 N22 86.7(4) . . ? O11 Co6 N22 93.8(4) . . ? N23 Co6 N22 171.2(5) . . ? N21 Co6 N22 87.7(5) . . ? N24 Co6 N22 94.5(5) . . ? O9 Co5 O10 87.8(3) . . ? O9 Co5 N19 178.9(4) . . ? O10 Co5 N19 93.2(4) . . ? O9 Co5 N17 92.7(4) . . ? O10 Co5 N17 179.4(4) . . ? N19 Co5 N17 86.2(4) . . ? O9 Co5 N18 86.0(4) . . ? O10 Co5 N18 93.2(4) . . ? N19 Co5 N18 94.2(4) . . ? N17 Co5 N18 86.9(4) . . ? O9 Co5 N20 87.1(5) . . ? O10 Co5 N20 91.7(4) . . ? N19 Co5 N20 92.6(5) . . ? N17 Co5 N20 88.3(4) . . ? N18 Co5 N20 171.4(4) . . ? O7 Co4 O8 87.1(3) . . ? O7 Co4 N16 93.2(4) . . ? O8 Co4 N16 87.1(4) . . ? O7 Co4 N13 179.1(4) . . ? O8 Co4 N13 93.3(3) . . ? N16 Co4 N13 87.6(4) . . ? O7 Co4 N15 92.2(4) . . ? O8 Co4 N15 179.3(4) . . ? N16 Co4 N15 93.2(4) . . ? N13 Co4 N15 87.4(4) . . ? O7 Co4 N14 93.4(4) . . ? O8 Co4 N14 88.1(4) . . ? N16 Co4 N14 171.7(4) . . ? N13 Co4 N14 85.9(4) . . ? N15 Co4 N14 91.7(4) . . ? O5 Co3 O6 87.7(3) . . ? O5 Co3 N11 178.5(4) . . ? O6 Co3 N11 93.7(4) . . ? O5 Co3 N9 90.4(4) . . ? O6 Co3 N9 178.0(4) . . ? N11 Co3 N9 88.2(4) . . ? O5 Co3 N10 87.4(5) . . ? O6 Co3 N10 93.7(4) . . ? N11 Co3 N10 92.1(5) . . ? N9 Co3 N10 86.3(5) . . ? O5 Co3 N12 87.0(4) . . ? O6 Co3 N12 92.5(4) . . ? N11 Co3 N12 93.4(5) . . ? N9 Co3 N12 87.3(5) . . ? N10 Co3 N12 171.5(4) . . ? O4 Co2 O3 87.2(3) . . ? O4 Co2 N7 86.9(4) . . ? O3 Co2 N7 93.3(4) . . ? O4 Co2 N8 86.5(4) . . ? O3 Co2 N8 93.1(4) . . ? N7 Co2 N8 170.6(4) . . ? O4 Co2 N5 91.6(4) . . ? O3 Co2 N5 178.4(4) . . ? N7 Co2 N5 87.6(4) . . ? N8 Co2 N5 85.9(4) . . ? O4 Co2 N6 178.4(4) . . ? O3 Co2 N6 94.4(4) . . ? N7 Co2 N6 92.9(4) . . ? N8 Co2 N6 93.5(4) . . ? N5 Co2 N6 86.8(4) . . ? O1 Co1 O2 87.6(4) . . ? O1 Co1 N2 86.6(5) . . ? O2 Co1 N2 92.9(5) . . ? O1 Co1 N4 178.2(4) . . ? O2 Co1 N4 94.2(4) . . ? N2 Co1 N4 93.5(5) . . ? O1 Co1 N3 88.5(5) . . ? O2 Co1 N3 92.6(5) . . ? N2 Co1 N3 172.5(5) . . ? N4 Co1 N3 91.2(5) . . ? O1 Co1 N1 91.2(4) . . ? O2 Co1 N1 178.7(5) . . ? N2 Co1 N1 86.7(5) . . ? N4 Co1 N1 87.0(5) . . ? N3 Co1 N1 87.7(5) . . ? C62 O12 Co6 109.2(7) . . ? C38 O8 Co4 109.8(6) . . ? C25 O5 Co3 109.5(7) . . ? C1 O1 Co1 109.8(7) . . ? C50 O10 Co5 108.2(6) . . ? C49 O9 Co5 110.4(6) . . ? C2 O2 Co1 107.5(7) . . ? C60 N20 Co5 109.7(8) . . ? C37 O7 Co4 108.0(6) . . ? C72 N24 Co6 110.5(8) . . ? C14 O4 Co2 108.9(7) . . ? C48 N16 Co4 109.8(8) . . ? C46 N15 Co4 108.8(7) . . ? C61 O11 Co6 108.6(7) . . ? C65 C64 C63 120.7(10) . . ? C65 C64 Br22 120.8(8) . . ? C63 C64 Br22 118.4(8) . . ? C20 N6 Co2 109.1(8) . . ? C36 N12 Co3 110.4(8) . . ? O22 N28 O23 121.1(15) . . ? O22 N28 O24 121.7(15) . . ? O23 N28 O24 117.3(12) . . ? C13 O3 Co2 109.3(7) . . ? O8 C38 C39 124.7(9) . . ? O8 C38 C37 115.9(9) . . ? C39 C38 C37 119.2(10) . . ? C10 N3 Co1 109.4(10) . . ? C24 N8 Co2 109.5(7) . . ? N14 C44 C43 106.8(10) . . ? C4 C5 C6 119.6(11) . . ? C4 C5 Br3 122.2(9) . . ? C6 C5 Br3 118.2(9) . . ? C58 C57 N17 111.4(11) . . ? C53 C52 C51 119.1(10) . . ? C53 C52 Br18 120.0(8) . . ? C51 C52 Br18 120.8(8) . . ? N16 C48 C47 109.2(10) . . ? O5 C25 C30 123.8(10) . . ? O5 C25 C26 118.8(9) . . ? C30 C25 C26 117.3(10) . . ? N10 C32 C31 107.1(11) . . ? C26 O6 Co3 109.2(6) . . ? N17 C59 C60 110.1(10) . . ? C56 C55 N17 108.2(9) . . ? C32 N10 Co3 111.1(8) . . ? O30 N30 O29 123.3(16) . . ? O30 N30 O28 122.0(16) . . ? O29 N30 O28 114.6(15) . . ? C56 N18 Co5 109.5(7) . . ? C58 N19 Co5 112.7(8) . . ? C23 N5 C19 112.9(10) . . ? C23 N5 C21 112.0(10) . . ? C19 N5 C21 110.8(9) . . ? C23 N5 Co2 107.1(7) . . ? C19 N5 Co2 110.1(7) . . ? C21 N5 Co2 103.4(7) . . ? C31 N9 C35 114.5(11) . . ? C31 N9 C33 113.2(12) . . ? C35 N9 C33 110.1(11) . . ? C31 N9 Co3 106.8(8) . . ? C35 N9 Co3 103.3(8) . . ? C33 N9 Co3 108.1(8) . . ? C41 C40 C39 119.0(9) . . ? C41 C40 Br14 121.6(8) . . ? C39 C40 Br14 119.4(8) . . ? C22 N7 Co2 110.3(8) . . ? C57 N17 C59 111.3(10) . . ? C57 N17 C55 113.0(10) . . ? C59 N17 C55 111.8(9) . . ? C57 N17 Co5 110.8(7) . . ? C59 N17 Co5 104.5(7) . . ? C55 N17 Co5 104.9(7) . . ? O9 C49 C54 123.7(10) . . ? O9 C49 C50 116.3(9) . . ? C54 C49 C50 120.0(10) . . ? C65 C66 C61 123.9(10) . . ? C65 C66 Br24 121.6(8) . . ? C61 C66 Br24 114.5(8) . . ? C70 N23 Co6 112.9(8) . . ? C12 N4 Co1 112.9(9) . . ? N13 C43 C44 109.2(9) . . ? C36 C35 N9 112.2(11) . . ? C68 N22 Co6 109.1(8) . . ? C41 C42 C37 122.8(10) . . ? C41 C42 Br16 121.7(8) . . ? C37 C42 Br16 115.5(8) . . ? C72 C71 N21 112.9(12) . . ? C43 N13 C45 114.0(9) . . ? C43 N13 C47 111.4(9) . . ? C45 N13 C47 110.5(9) . . ? C43 N13 Co4 104.8(7) . . ? C45 N13 Co4 110.1(7) . . ? C47 N13 Co4 105.6(7) . . ? C67 N21 C69 113.8(11) . . ? C67 N21 C71 110.4(11) . . ? C69 N21 C71 111.2(11) . . ? C67 N21 Co6 106.3(8) . . ? C69 N21 Co6 105.9(8) . . ? C71 N21 Co6 108.8(8) . . ? C44 N14 Co4 111.8(7) . . ? O3 C13 C14 115.5(10) . . ? O3 C13 C18 125.9(10) . . ? C14 C13 C18 118.6(10) . . ? C22 C21 N5 108.0(10) . . ? O4 C14 C13 119.0(10) . . ? O4 C14 C15 122.1(11) . . ? C13 C14 C15 118.8(11) . . ? C8 N2 Co1 112.5(10) . . ? C18 C17 C16 118.1(11) . . ? C18 C17 Br7 120.9(9) . . ? C16 C17 Br7 121.0(9) . . ? C55 C56 N18 109.2(9) . . ? O7 C37 C38 119.0(9) . . ? O7 C37 C42 123.4(10) . . ? C38 C37 C42 117.6(9) . . ? C38 C39 C40 121.6(9) . . ? C38 C39 Br13 115.8(8) . . ? C40 C39 Br13 122.6(7) . . ? C48 C47 N13 105.9(10) . . ? N5 C23 C24 104.3(10) . . ? O19 N27 O21 119.7(14) . . ? O19 N27 O20 120.2(15) . . ? O21 N27 O20 120.0(14) . . ? C28 C27 C26 120.4(10) . . ? C28 C27 Br9 121.9(9) . . ? C26 C27 Br9 117.7(9) . . ? C21 C22 N7 109.2(11) . . ? C70 C69 N21 109.2(10) . . ? N1 C7 C8 111.1(14) . . ? C42 C41 C40 119.7(10) . . ? C42 C41 Br15 120.2(8) . . ? C40 C41 Br15 120.1(8) . . ? N12 C36 C35 107.3(11) . . ? C64 C65 C66 118.4(9) . . ? C64 C65 Br23 121.6(8) . . ? C66 C65 Br23 119.9(8) . . ? O1 C1 C2 117.5(10) . . ? O1 C1 C6 123.6(11) . . ? C2 C1 C6 118.8(11) . . ? C49 C54 C53 120.2(10) . . ? C49 C54 Br20 116.7(8) . . ? C53 C54 Br20 123.1(8) . . ? N13 C45 C46 111.6(10) . . ? C52 C53 C54 119.4(10) . . ? C52 C53 Br19 121.9(8) . . ? C54 C53 Br19 118.6(8) . . ? N8 C24 C23 109.5(11) . . ? O15 N25 O14 119.2(13) . . ? O15 N25 O13 125.5(15) . . ? O14 N25 O13 115.2(14) . . ? O18 N26 O16 123.3(13) . . ? O18 N26 O17 117.0(13) . . ? O16 N26 O17 119.6(14) . . ? O10 C50 C51 124.8(9) . . ? O10 C50 C49 117.2(9) . . ? C51 C50 C49 118.1(10) . . ? C17 C18 C13 122.3(11) . . ? C17 C18 Br8 121.4(9) . . ? C13 C18 Br8 116.3(8) . . ? O11 C61 C66 125.9(10) . . ? O11 C61 C62 117.8(10) . . ? C66 C61 C62 116.2(9) . . ? O12 C62 C63 124.3(10) . . ? O12 C62 C61 115.8(9) . . ? C63 C62 C61 119.8(10) . . ? N23 C70 C69 109.4(11) . . ? C34 N11 Co3 109.0(8) . . ? C20 C19 N5 111.0(9) . . ? C64 C63 C62 120.9(10) . . ? C64 C63 Br21 123.1(8) . . ? C62 C63 Br21 116.0(8) . . ? C10 C9 N1 110.7(13) . . ? C50 C51 C52 123.1(10) . . ? C50 C51 Br17 117.1(8) . . ? C52 C51 Br17 119.8(8) . . ? C16 C15 C14 121.8(11) . . ? C16 C15 Br5 121.3(9) . . ? C14 C15 Br5 116.9(9) . . ? O2 C2 C3 122.6(11) . . ? O2 C2 C1 117.6(10) . . ? C3 C2 C1 119.8(11) . . ? C15 C16 C17 120.3(11) . . ? C15 C16 Br6 120.4(10) . . ? C17 C16 Br6 119.3(10) . . ? C7 N1 C9 114.6(12) . . ? C7 N1 C11 111.4(12) . . ? C9 N1 C11 112.3(12) . . ? C7 N1 Co1 104.9(8) . . ? C9 N1 Co1 103.2(9) . . ? C11 N1 Co1 109.7(9) . . ? O26 N29 O25 120.3(14) . . ? O26 N29 O27 118.9(15) . . ? O25 N29 O27 120.4(16) . . ? C27 C28 C29 119.5(10) . . ? C27 C28 Br10 120.9(9) . . ? C29 C28 Br10 119.5(8) . . ? O6 C26 C27 124.8(10) . . ? O6 C26 C25 114.5(9) . . ? C27 C26 C25 120.7(10) . . ? C30 C29 C28 119.6(10) . . ? C30 C29 Br11 119.8(9) . . ? C28 C29 Br11 120.5(8) . . ? C33 C34 N11 109.0(12) . . ? C34 C33 N9 113.7(11) . . ? N21 C67 C68 109.2(12) . . ? C67 C68 N22 106.9(11) . . ? C5 C4 C3 120.3(11) . . ? C5 C4 Br2 119.3(9) . . ? C3 C4 Br2 120.3(9) . . ? N20 C60 C59 107.1(10) . . ? N24 C72 C71 112.8(13) . . ? N4 C12 C11 113.9(14) . . ? C29 C30 C25 122.2(10) . . ? C29 C30 Br12 123.1(8) . . ? C25 C30 Br12 114.8(8) . . ? C12 C11 N1 112.2(13) . . ? C9 C10 N3 107.9(14) . . ? C7 C8 N2 105.4(13) . . ? C1 C6 C5 120.4(11) . . ? C1 C6 Br4 116.1(9) . . ? C5 C6 Br4 123.5(10) . . ? N6 C20 C19 109.4(10) . . ? N15 C46 C45 110.1(10) . . ? C4 C3 C2 120.9(12) . . ? C4 C3 Br1 121.4(9) . . ? C2 C3 Br1 117.8(9) . . ? N9 C31 C32 108.4(11) . . ? N19 C58 C57 118.2(12) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 3.097 _refine_diff_density_min -2.122 _refine_diff_density_rms 0.189