# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_1 _database_code_depnum_ccdc_archive 'CCDC 908081' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H41 Co2 N14 O2' _chemical_formula_weight 771.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.855(12) _cell_length_b 12.339(4) _cell_length_c 19.200(7) _cell_angle_alpha 90.00 _cell_angle_beta 113.975(5) _cell_angle_gamma 90.00 _cell_volume 7112(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2885 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 21.97 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8125 _exptl_absorpt_correction_T_max 0.8745 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\p and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34359 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.44 _reflns_number_total 6533 _reflns_number_gt 4421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6533 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 C1 C 0.04194(13) 0.2783(3) 0.3551(2) 0.0228(9) Uani 1 1 d . . . C2 C 0.03959(13) 0.3917(3) 0.3509(2) 0.0232(9) Uani 1 1 d . . . C3 C -0.00031(14) 0.4433(4) 0.3427(2) 0.0268(10) Uani 1 1 d . . . H3 H -0.0014 0.5202 0.3409 0.032 Uiso 1 1 calc R . . C4 C -0.03790(14) 0.3878(3) 0.3374(2) 0.0257(10) Uani 1 1 d . . . C5 C -0.03575(14) 0.2753(3) 0.3363(2) 0.0263(10) Uani 1 1 d . . . H5 H -0.0617 0.2345 0.3288 0.032 Uiso 1 1 calc R . . C6 C 0.00324(13) 0.2204(3) 0.3458(2) 0.0229(9) Uani 1 1 d . . . C7 C -0.07883(14) 0.4433(4) 0.3357(3) 0.0325(11) Uani 1 1 d . . . H7A H -0.1054 0.4130 0.2937 0.039 Uiso 1 1 calc R . . H7B H -0.0772 0.5216 0.3256 0.039 Uiso 1 1 calc R . . C8 C -0.08359(17) 0.4291(4) 0.4107(3) 0.0467(14) Uani 1 1 d . . . H8A H -0.0870 0.3519 0.4193 0.070 Uiso 1 1 calc R . . H8B H -0.1099 0.4687 0.4087 0.070 Uiso 1 1 calc R . . H8C H -0.0570 0.4574 0.4525 0.070 Uiso 1 1 calc R . . C9 C 0.00131(14) 0.1033(3) 0.3423(2) 0.0255(10) Uani 1 1 d . . . H9 H -0.0275 0.0719 0.3197 0.031 Uiso 1 1 calc R . . C10 C 0.07519(14) 0.4628(4) 0.3523(2) 0.0265(10) Uani 1 1 d . . . H10 H 0.0675 0.5369 0.3407 0.032 Uiso 1 1 calc R . . C11 C 0.02450(14) -0.0783(3) 0.3507(2) 0.0245(9) Uani 1 1 d . . . H11A H 0.0358 -0.1020 0.3126 0.029 Uiso 1 1 calc R . . H11B H -0.0082 -0.0887 0.3282 0.029 Uiso 1 1 calc R . . C12 C 0.04507(14) -0.1501(3) 0.4214(2) 0.0260(10) Uani 1 1 d . . . C13 C 0.02991(15) -0.2658(3) 0.3960(3) 0.0338(11) Uani 1 1 d . . . H13A H 0.0446 -0.3156 0.4387 0.051 Uiso 1 1 calc R . . H13B H 0.0378 -0.2854 0.3536 0.051 Uiso 1 1 calc R . . H13C H -0.0025 -0.2708 0.3794 0.051 Uiso 1 1 calc R . . C14 C 0.03124(15) -0.1150(4) 0.4846(2) 0.0322(11) Uani 1 1 d . . . H14A H -0.0013 -0.1169 0.4658 0.048 Uiso 1 1 calc R . . H14B H 0.0418 -0.0411 0.5007 0.048 Uiso 1 1 calc R . . H14C H 0.0443 -0.1644 0.5281 0.048 Uiso 1 1 calc R . . C15 C 0.09577(13) -0.1477(3) 0.4492(2) 0.0263(10) Uani 1 1 d . . . H15A H 0.1088 -0.2016 0.4906 0.032 Uiso 1 1 calc R . . H15B H 0.1038 -0.1695 0.4068 0.032 Uiso 1 1 calc R . . C16 C 0.14757(13) -0.0392(4) 0.5434(2) 0.0264(10) Uani 1 1 d . . . H16 H 0.1536 -0.1051 0.5713 0.032 Uiso 1 1 calc R . . C17 C 0.17572(13) 0.0517(4) 0.5801(2) 0.0252(10) Uani 1 1 d . . . C18 C 0.20387(14) 0.0403(4) 0.6576(2) 0.0325(11) Uani 1 1 d . . . H18 H 0.2023 -0.0245 0.6831 0.039 Uiso 1 1 calc R . . C19 C 0.23376(14) 0.1195(4) 0.6981(2) 0.0334(11) Uani 1 1 d . . . C20 C 0.23659(14) 0.2097(4) 0.6584(2) 0.0293(10) Uani 1 1 d . . . H20 H 0.2575 0.2642 0.6851 0.035 Uiso 1 1 calc R . . C21 C 0.21018(13) 0.2255(3) 0.5806(2) 0.0257(10) Uani 1 1 d . . . C22 C 0.17847(13) 0.1460(3) 0.5406(2) 0.0241(9) Uani 1 1 d . . . C23 C 0.26343(16) 0.1025(4) 0.7818(3) 0.0451(13) Uani 1 1 d . . . H23A H 0.2823 0.1675 0.8017 0.054 Uiso 1 1 calc R . . H23B H 0.2446 0.0936 0.8106 0.054 Uiso 1 1 calc R . . C24 C 0.2931(2) 0.0037(6) 0.7944(3) 0.072(2) Uani 1 1 d . . . H24A H 0.2746 -0.0611 0.7758 0.108 Uiso 1 1 calc R . . H24B H 0.3117 -0.0043 0.8490 0.108 Uiso 1 1 calc R . . H24C H 0.3122 0.0127 0.7667 0.108 Uiso 1 1 calc R . . C25 C 0.22073(14) 0.3210(4) 0.5466(2) 0.0291(10) Uani 1 1 d . . . H25 H 0.2451 0.3639 0.5789 0.035 Uiso 1 1 calc R . . C26 C 0.21794(14) 0.4507(3) 0.4554(3) 0.0292(10) Uani 1 1 d . . . H26A H 0.2254 0.4329 0.4117 0.035 Uiso 1 1 calc R . . H26B H 0.2458 0.4724 0.4985 0.035 Uiso 1 1 calc R . . C27 C 0.18569(14) 0.5468(3) 0.4336(2) 0.0271(10) Uani 1 1 d . . . C28 C 0.17258(16) 0.5766(4) 0.4982(3) 0.0403(12) Uani 1 1 d . . . H28A H 0.1569 0.5156 0.5088 0.060 Uiso 1 1 calc R . . H28B H 0.1530 0.6401 0.4836 0.060 Uiso 1 1 calc R . . H28C H 0.1994 0.5934 0.5439 0.060 Uiso 1 1 calc R . . C29 C 0.21030(16) 0.6423(4) 0.4157(3) 0.0402(12) Uani 1 1 d . . . H29A H 0.1906 0.7055 0.4002 0.060 Uiso 1 1 calc R . . H29B H 0.2189 0.6218 0.3743 0.060 Uiso 1 1 calc R . . H29C H 0.2370 0.6602 0.4613 0.060 Uiso 1 1 calc R . . C30 C 0.14472(14) 0.5234(3) 0.3600(2) 0.0291(10) Uani 1 1 d . . . H30A H 0.1271 0.5908 0.3430 0.035 Uiso 1 1 calc R . . H30B H 0.1549 0.5021 0.3199 0.035 Uiso 1 1 calc R . . C31 C 0.1199(3) 0.8640(6) 0.1951(4) 0.096(3) Uani 1 1 d . . . H31A H 0.0976 0.8963 0.1486 0.144 Uiso 1 1 calc R . . H31B H 0.1407 0.8200 0.1821 0.144 Uiso 1 1 calc R . . H31C H 0.1364 0.9216 0.2305 0.144 Uiso 1 1 calc R . . C32 C 0.09735(18) 0.7945(5) 0.2315(3) 0.0457(13) Uani 1 1 d . . . Co1 Co 0.093964(18) 0.08846(4) 0.41927(3) 0.02301(17) Uani 1 1 d . . . Co2 Co 0.143084(19) 0.28734(5) 0.39657(3) 0.02674(18) Uani 1 1 d . . . N1 N 0.03418(11) 0.0374(3) 0.36624(18) 0.0223(8) Uani 1 1 d . . . N2 N 0.11546(11) -0.0408(3) 0.47749(18) 0.0240(8) Uani 1 1 d . . . N3 N 0.20042(11) 0.3533(3) 0.47721(19) 0.0251(8) Uani 1 1 d . . . N4 N 0.11555(11) 0.4375(3) 0.36721(19) 0.0252(8) Uani 1 1 d . . . N5 N 0.07718(12) 0.1452(3) 0.49976(19) 0.0283(8) Uani 1 1 d . . . N6 N 0.09035(12) 0.2367(3) 0.5202(2) 0.0311(9) Uani 1 1 d . . . N7 N 0.10260(15) 0.3230(4) 0.5412(2) 0.0490(11) Uani 1 1 d . . . N8 N 0.10881(12) 0.0305(3) 0.33816(19) 0.0288(8) Uani 1 1 d . . . N9 N 0.14638(13) -0.0023(3) 0.3567(2) 0.0328(9) Uani 1 1 d . . . N10 N 0.18233(14) -0.0329(4) 0.3722(2) 0.0533(13) Uani 1 1 d . . . N11 N 0.16272(13) 0.2593(3) 0.3136(2) 0.0394(10) Uani 1 1 d . . . N12 N 0.15239(13) 0.2084(3) 0.2570(2) 0.0373(10) Uani 1 1 d . . . N13 N 0.14328(16) 0.1606(4) 0.2015(3) 0.0552(12) Uani 1 1 d . . . N14 N 0.07929(15) 0.7442(4) 0.2577(2) 0.0474(11) Uani 1 1 d . . . O1 O 0.07941(9) 0.2254(2) 0.36629(15) 0.0230(6) Uani 1 1 d . . . O2 O 0.15164(9) 0.1571(2) 0.46677(15) 0.0235(6) 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 0.023(2) 0.029(2) 0.014(2) 0.0008(18) 0.0052(17) 0.0035(19) C2 0.022(2) 0.026(2) 0.019(2) -0.0016(18) 0.0064(18) 0.0032(18) C3 0.029(2) 0.027(2) 0.024(2) 0.0010(18) 0.011(2) 0.0063(19) C4 0.027(2) 0.028(2) 0.021(2) 0.0064(18) 0.0085(19) 0.0062(19) C5 0.024(2) 0.032(3) 0.019(2) 0.0047(19) 0.0051(18) -0.0017(19) C6 0.020(2) 0.029(2) 0.019(2) 0.0013(18) 0.0079(18) 0.0008(18) C7 0.024(2) 0.034(3) 0.038(3) 0.007(2) 0.011(2) 0.008(2) C8 0.056(3) 0.053(3) 0.038(3) 0.004(3) 0.026(3) 0.017(3) C9 0.023(2) 0.036(3) 0.016(2) 0.0008(18) 0.0062(18) -0.003(2) C10 0.028(2) 0.026(2) 0.022(2) 0.0017(18) 0.0066(19) -0.0002(19) C11 0.024(2) 0.020(2) 0.025(2) 0.0000(18) 0.0063(19) -0.0009(18) C12 0.028(2) 0.027(2) 0.022(2) 0.0013(19) 0.0087(19) 0.0009(19) C13 0.033(3) 0.029(3) 0.037(3) 0.001(2) 0.011(2) -0.002(2) C14 0.036(3) 0.033(3) 0.033(3) 0.004(2) 0.020(2) 0.004(2) C15 0.030(2) 0.024(2) 0.027(2) 0.0017(19) 0.013(2) 0.0041(19) C16 0.025(2) 0.030(2) 0.027(2) 0.0050(19) 0.013(2) 0.0080(19) C17 0.021(2) 0.034(3) 0.019(2) 0.0008(19) 0.0071(18) 0.0077(19) C18 0.025(2) 0.045(3) 0.027(2) 0.006(2) 0.009(2) 0.007(2) C19 0.023(2) 0.054(3) 0.024(2) -0.003(2) 0.010(2) -0.001(2) C20 0.020(2) 0.043(3) 0.023(2) -0.007(2) 0.0064(19) 0.002(2) C21 0.017(2) 0.032(3) 0.026(2) -0.0085(19) 0.0071(19) 0.0036(18) C22 0.017(2) 0.033(3) 0.021(2) -0.0055(19) 0.0064(18) 0.0070(18) C23 0.034(3) 0.072(4) 0.021(3) -0.001(2) 0.002(2) -0.002(3) C24 0.057(4) 0.120(6) 0.035(3) 0.008(4) 0.013(3) 0.023(4) C25 0.019(2) 0.033(3) 0.031(3) -0.010(2) 0.006(2) -0.0004(19) C26 0.023(2) 0.032(3) 0.033(3) -0.003(2) 0.012(2) -0.0026(19) C27 0.026(2) 0.026(2) 0.025(2) -0.0049(19) 0.0065(19) -0.0028(19) C28 0.043(3) 0.046(3) 0.028(3) -0.009(2) 0.011(2) 0.009(2) C29 0.042(3) 0.032(3) 0.040(3) -0.004(2) 0.009(2) -0.006(2) C30 0.028(2) 0.027(2) 0.029(2) -0.0014(19) 0.009(2) -0.0059(19) C31 0.123(6) 0.130(7) 0.055(4) -0.040(4) 0.056(4) -0.071(5) C32 0.047(3) 0.062(4) 0.029(3) -0.010(3) 0.016(3) -0.010(3) Co1 0.0213(3) 0.0257(3) 0.0194(3) -0.0002(2) 0.0054(2) 0.0015(2) Co2 0.0221(3) 0.0286(3) 0.0281(3) -0.0004(3) 0.0088(3) -0.0001(3) N1 0.0214(18) 0.0257(19) 0.0170(18) 0.0010(15) 0.0049(15) 0.0006(15) N2 0.0224(19) 0.028(2) 0.0188(18) -0.0010(15) 0.0060(16) 0.0027(16) N3 0.0180(18) 0.026(2) 0.029(2) -0.0050(16) 0.0071(16) 0.0039(15) N4 0.025(2) 0.027(2) 0.0221(19) 0.0000(15) 0.0076(16) -0.0017(16) N5 0.031(2) 0.031(2) 0.0215(19) -0.0026(17) 0.0100(16) 0.0040(17) N6 0.031(2) 0.036(3) 0.021(2) -0.0027(18) 0.0050(17) 0.0094(19) N7 0.057(3) 0.040(3) 0.046(3) -0.009(2) 0.017(2) 0.004(2) N8 0.024(2) 0.033(2) 0.027(2) -0.0005(17) 0.0079(17) 0.0025(17) N9 0.033(2) 0.037(2) 0.028(2) -0.0098(17) 0.0110(18) -0.0015(19) N10 0.032(2) 0.078(3) 0.046(3) -0.021(2) 0.012(2) 0.012(2) N11 0.033(2) 0.051(3) 0.041(3) -0.016(2) 0.023(2) -0.009(2) N12 0.036(2) 0.040(2) 0.041(3) -0.005(2) 0.020(2) 0.0019(19) N13 0.065(3) 0.058(3) 0.048(3) -0.009(3) 0.029(3) 0.008(3) N14 0.051(3) 0.051(3) 0.045(3) 0.008(2) 0.025(2) 0.007(2) O1 0.0229(15) 0.0227(15) 0.0216(15) 0.0018(12) 0.0073(12) 0.0030(12) O2 0.0215(15) 0.0264(16) 0.0200(15) -0.0022(12) 0.0055(13) 0.0030(12) _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 1.332(5) . ? C1 C2 1.402(6) . ? C1 C6 1.405(6) . ? C2 C3 1.408(6) . ? C2 C10 1.454(6) . ? C3 C4 1.379(6) . ? C4 C5 1.391(6) . ? C4 C7 1.498(6) . ? C5 C6 1.394(6) . ? C6 C9 1.448(6) . ? C7 C8 1.521(6) . ? C9 N1 1.278(5) . ? C10 N4 1.276(5) . ? C11 N1 1.467(5) . ? C11 C12 1.529(5) . ? C12 C14 1.522(6) . ? C12 C13 1.526(6) . ? C12 C15 1.529(6) . ? C15 N2 1.472(5) . ? C16 N2 1.277(5) . ? C16 C17 1.442(6) . ? C17 C18 1.403(6) . ? C17 C22 1.412(6) . ? C18 C19 1.380(6) . ? C19 C20 1.373(6) . ? C19 C23 1.517(6) . ? C20 C21 1.404(6) . ? C21 C22 1.410(6) . ? C21 C25 1.456(6) . ? C22 O2 1.337(5) . ? C23 C24 1.517(8) . ? C25 N3 1.286(5) . ? C26 N3 1.465(5) . ? C26 C27 1.532(6) . ? C27 C28 1.514(6) . ? C27 C30 1.532(6) . ? C27 C29 1.544(6) . ? C30 N4 1.472(5) . ? C31 C32 1.482(8) . ? C32 N14 1.110(6) . ? Co1 N2 1.911(3) . ? Co1 N1 1.915(3) . ? Co1 O1 1.929(3) . ? Co1 O2 1.933(3) . ? Co1 N8 1.947(4) . ? Co1 N5 1.969(3) . ? Co2 N11 1.978(4) . ? Co2 N4 2.039(4) . ? Co2 O2 2.042(3) . ? Co2 N3 2.059(3) . ? Co2 O1 2.076(3) . ? N5 N6 1.216(5) . ? N6 N7 1.152(5) . ? N8 N9 1.207(5) . ? N9 N10 1.158(5) . ? N11 N12 1.179(5) . ? N12 N13 1.146(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 C2 121.7(4) . . ? O1 C1 C6 120.0(4) . . ? C2 C1 C6 118.3(4) . . ? C1 C2 C3 119.0(4) . . ? C1 C2 C10 125.2(4) . . ? C3 C2 C10 115.8(4) . . ? C4 C3 C2 123.3(4) . . ? C3 C4 C5 116.6(4) . . ? C3 C4 C7 122.9(4) . . ? C5 C4 C7 120.5(4) . . ? C4 C5 C6 122.2(4) . . ? C5 C6 C1 120.4(4) . . ? C5 C6 C9 117.3(4) . . ? C1 C6 C9 122.3(4) . . ? C4 C7 C8 111.3(4) . . ? N1 C9 C6 127.1(4) . . ? N4 C10 C2 127.7(4) . . ? N1 C11 C12 113.8(3) . . ? C14 C12 C13 110.9(4) . . ? C14 C12 C15 110.6(3) . . ? C13 C12 C15 107.3(3) . . ? C14 C12 C11 112.1(3) . . ? C13 C12 C11 106.8(3) . . ? C15 C12 C11 108.9(3) . . ? N2 C15 C12 113.5(3) . . ? N2 C16 C17 127.2(4) . . ? C18 C17 C22 119.6(4) . . ? C18 C17 C16 117.1(4) . . ? C22 C17 C16 123.1(4) . . ? C19 C18 C17 122.6(4) . . ? C20 C19 C18 117.0(4) . . ? C20 C19 C23 122.7(4) . . ? C18 C19 C23 120.2(4) . . ? C19 C20 C21 123.5(4) . . ? C20 C21 C22 118.9(4) . . ? C20 C21 C25 115.7(4) . . ? C22 C21 C25 125.2(4) . . ? O2 C22 C21 121.9(4) . . ? O2 C22 C17 119.7(4) . . ? C21 C22 C17 118.4(4) . . ? C24 C23 C19 112.0(4) . . ? N3 C25 C21 126.7(4) . . ? N3 C26 C27 113.9(3) . . ? C28 C27 C26 111.1(4) . . ? C28 C27 C30 111.5(4) . . ? C26 C27 C30 110.9(4) . . ? C28 C27 C29 110.2(4) . . ? C26 C27 C29 106.6(4) . . ? C30 C27 C29 106.4(3) . . ? N4 C30 C27 114.2(3) . . ? N14 C32 C31 177.8(7) . . ? N2 Co1 N1 95.27(14) . . ? N2 Co1 O1 173.20(13) . . ? N1 Co1 O1 91.53(13) . . ? N2 Co1 O2 91.80(13) . . ? N1 Co1 O2 172.89(13) . . ? O1 Co1 O2 81.41(11) . . ? N2 Co1 N8 90.46(15) . . ? N1 Co1 N8 89.44(14) . . ? O1 Co1 N8 89.36(13) . . ? O2 Co1 N8 91.26(13) . . ? N2 Co1 N5 89.57(14) . . ? N1 Co1 N5 88.87(14) . . ? O1 Co1 N5 90.81(13) . . ? O2 Co1 N5 90.43(13) . . ? N8 Co1 N5 178.30(15) . . ? N11 Co2 N4 100.95(16) . . ? N11 Co2 O2 113.05(15) . . ? N4 Co2 O2 145.53(12) . . ? N11 Co2 N3 100.19(15) . . ? N4 Co2 N3 90.94(14) . . ? O2 Co2 N3 88.62(12) . . ? N11 Co2 O1 109.35(14) . . ? N4 Co2 O1 88.51(12) . . ? O2 Co2 O1 75.39(10) . . ? N3 Co2 O1 150.01(12) . . ? C9 N1 C11 117.6(4) . . ? C9 N1 Co1 121.1(3) . . ? C11 N1 Co1 121.3(3) . . ? C16 N2 C15 116.3(4) . . ? C16 N2 Co1 121.8(3) . . ? C15 N2 Co1 122.0(3) . . ? C25 N3 C26 116.8(4) . . ? C25 N3 Co2 126.0(3) . . ? C26 N3 Co2 117.1(3) . . ? C10 N4 C30 117.4(4) . . ? C10 N4 Co2 126.0(3) . . ? C30 N4 Co2 116.6(3) . . ? N6 N5 Co1 114.0(3) . . ? N7 N6 N5 178.3(5) . . ? N9 N8 Co1 116.5(3) . . ? N10 N9 N8 177.8(5) . . ? N12 N11 Co2 140.3(3) . . ? N13 N12 N11 177.9(5) . . ? C1 O1 Co1 122.0(2) . . ? C1 O1 Co2 128.6(2) . . ? Co1 O1 Co2 99.74(12) . . ? C22 O2 Co1 123.6(3) . . ? C22 O2 Co2 129.4(3) . . ? Co1 O2 Co2 100.82(12) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.982 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.083 data_2 _database_code_depnum_ccdc_archive 'CCDC 908082' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H41 Co2 N8 O5' _chemical_formula_weight 771.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.631(4) _cell_length_b 12.255(5) _cell_length_c 16.296(7) _cell_angle_alpha 96.958(5) _cell_angle_beta 101.226(5) _cell_angle_gamma 104.979(5) _cell_volume 1792.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3953 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.84 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 802 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7920 _exptl_absorpt_correction_T_max 0.8436 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12975 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6530 _reflns_number_gt 4891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Largest residual electron density peak has been 2.305 which is related to the heavy element Co1 in the structure. ; _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^)+(0.1000P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6530 _refine_ls_number_parameters 489 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.2300 _refine_ls_wR_factor_gt 0.2088 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.026 _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 Co2 Co 0.33938(12) 0.15039(11) 0.31157(7) 0.0381(3) Uani 0.85 1 d P . . Co1 Co 0.00922(9) 0.07042(8) 0.22370(5) 0.0481(3) Uani 1 1 d . . . N2 N -0.1557(5) -0.0140(4) 0.2612(3) 0.0408(11) Uani 1 1 d . . . O1 O 0.1937(4) 0.1576(3) 0.2018(3) 0.0420(9) Uani 1 1 d . . . C18 C -0.1040(6) 0.1081(5) 0.4830(4) 0.0387(13) Uani 1 1 d . . . H18 H -0.2025 0.0759 0.4835 0.046 Uiso 1 1 calc R . . O4 O 0.055(2) 0.4051(9) 0.3053(15) 0.213(9) Uani 0.80 1 d PD . . O2 O 0.1354(4) 0.1017(3) 0.3366(2) 0.0365(8) Uani 1 1 d . . . C17 C -0.0575(6) 0.0836(5) 0.4090(4) 0.0369(12) Uani 1 1 d . . . C19 C -0.0094(7) 0.1783(5) 0.5557(4) 0.0404(13) Uani 1 1 d . . . C16 C -0.1663(6) 0.0058(5) 0.3382(4) 0.0379(12) Uani 1 1 d . . . H16 H -0.2540 -0.0345 0.3500 0.045 Uiso 1 1 calc R . . C7 C 0.2412(13) 0.4439(10) -0.0477(8) 0.115(4) Uani 1 1 d D . . H7A H 0.3423 0.4626 -0.0541 0.138 Uiso 1 1 calc R . . H7B H 0.1776 0.3985 -0.1011 0.138 Uiso 1 1 calc R . . N5 N 0.0531(6) -0.0526(10) 0.1961(4) 0.112(4) Uani 1 1 d . . . C33 C 0.4529(8) -0.0568(7) 0.3466(5) 0.0632(19) Uani 1 1 d . . . C15 C -0.2754(6) -0.1066(5) 0.2024(4) 0.0469(15) Uani 1 1 d . . . H15A H -0.3526 -0.1345 0.2316 0.056 Uiso 1 1 calc R . . H15B H -0.2370 -0.1698 0.1866 0.056 Uiso 1 1 calc R . . C12 C -0.3423(7) -0.0687(6) 0.1222(4) 0.0485(15) Uani 1 1 d . . . C13 C -0.4706(8) -0.1728(7) 0.0717(5) 0.065(2) Uani 1 1 d . . . H13A H -0.5456 -0.1893 0.1032 0.098 Uiso 1 1 calc R . . H13B H -0.4345 -0.2383 0.0625 0.098 Uiso 1 1 calc R . . H13C H -0.5117 -0.1559 0.0178 0.098 Uiso 1 1 calc R . . C11 C -0.2298(7) -0.0432(6) 0.0682(4) 0.0483(15) Uani 1 1 d . . . H11A H -0.1987 -0.1113 0.0554 0.058 Uiso 1 1 calc R . . H11B H -0.2775 -0.0272 0.0147 0.058 Uiso 1 1 calc R . . N1 N -0.0975(5) 0.0543(4) 0.1083(3) 0.0428(11) Uani 1 1 d . . . C9 C -0.0559(7) 0.1276(6) 0.0620(4) 0.0459(14) Uani 1 1 d . . . H9 H -0.1220 0.1216 0.0107 0.055 Uiso 1 1 calc R . . C6 C 0.0808(7) 0.2182(5) 0.0797(4) 0.0448(14) Uani 1 1 d . . . C5 C 0.0945(8) 0.2923(6) 0.0208(5) 0.0592(18) Uani 1 1 d . . . H5 H 0.0115 0.2879 -0.0211 0.071 Uiso 1 1 calc R . . C4 C 0.2273(9) 0.3719(7) 0.0227(5) 0.067(2) Uani 1 1 d . . . C3 C 0.3477(9) 0.3746(7) 0.0859(5) 0.066(2) Uani 1 1 d . . . H3 H 0.4385 0.4261 0.0877 0.079 Uiso 1 1 calc R . . C2 C 0.3403(7) 0.3042(5) 0.1470(4) 0.0486(15) Uani 1 1 d . . . C1 C 0.2034(6) 0.2250(5) 0.1455(4) 0.0410(13) Uani 1 1 d . . . C10 C 0.4783(7) 0.3175(6) 0.2078(4) 0.0505(16) Uani 1 1 d . . . H10 H 0.5625 0.3677 0.1991 0.061 Uiso 1 1 calc R . . N4 N 0.4965(5) 0.2679(5) 0.2715(3) 0.0467(12) Uani 1 1 d . . . C28 C 0.6475(6) 0.2974(6) 0.3243(4) 0.0519(16) Uani 1 1 d . . . H28A H 0.7144 0.3465 0.2975 0.062 Uiso 1 1 calc R . . H28B H 0.6768 0.2277 0.3274 0.062 Uiso 1 1 calc R . . C27 C 0.6620(6) 0.3586(5) 0.4143(4) 0.0456(14) Uani 1 1 d . . . C29 C 0.6047(9) 0.4629(6) 0.4137(5) 0.0646(19) Uani 1 1 d . . . H29A H 0.5005 0.4388 0.3883 0.097 Uiso 1 1 calc R . . H29B H 0.6551 0.5136 0.3814 0.097 Uiso 1 1 calc R . . H29C H 0.6224 0.5024 0.4710 0.097 Uiso 1 1 calc R . . C26 C 0.5853(6) 0.2771(6) 0.4653(4) 0.0489(15) Uani 1 1 d . . . H26A H 0.6243 0.2116 0.4641 0.059 Uiso 1 1 calc R . . H26B H 0.6096 0.3158 0.5240 0.059 Uiso 1 1 calc R . . N3 N 0.4233(5) 0.2348(4) 0.4354(3) 0.0395(11) Uani 1 1 d . . . C25 C 0.3490(6) 0.2386(5) 0.4916(4) 0.0389(13) Uani 1 1 d . . . H25 H 0.4034 0.2745 0.5463 0.047 Uiso 1 1 calc R . . C21 C 0.1911(6) 0.1946(5) 0.4819(3) 0.0357(12) Uani 1 1 d . . . C22 C 0.0911(6) 0.1274(4) 0.4065(3) 0.0343(12) Uani 1 1 d . . . C23 C -0.0654(8) 0.2060(6) 0.6342(4) 0.0547(16) Uani 1 1 d . . . H23A H -0.1664 0.2084 0.6159 0.066 Uiso 1 1 calc R . . H23B H -0.0675 0.1436 0.6658 0.066 Uiso 1 1 calc R . . C24 C 0.0210(10) 0.3153(8) 0.6930(5) 0.081(3) Uani 1 1 d . . . H24A H 0.1204 0.3131 0.7140 0.121 Uiso 1 1 calc R . . H24B H -0.0241 0.3252 0.7399 0.121 Uiso 1 1 calc R . . H24C H 0.0227 0.3784 0.6632 0.121 Uiso 1 1 calc R . . C20 C 0.1370(7) 0.2193(5) 0.5534(4) 0.0412(13) Uani 1 1 d . . . H20 H 0.2032 0.2657 0.6020 0.049 Uiso 1 1 calc R . . C30 C 0.8282(7) 0.3975(7) 0.4579(5) 0.067(2) Uani 1 1 d . . . H30A H 0.8811 0.4483 0.4266 0.100 Uiso 1 1 calc R . . H30B H 0.8643 0.3316 0.4593 0.100 Uiso 1 1 calc R . . H30C H 0.8427 0.4368 0.5150 0.100 Uiso 1 1 calc R . . C14 C -0.3987(8) 0.0347(6) 0.1437(5) 0.0590(18) Uani 1 1 d . . . H14A H -0.3169 0.0992 0.1741 0.089 Uiso 1 1 calc R . . H14B H -0.4682 0.0161 0.1785 0.089 Uiso 1 1 calc R . . H14C H -0.4462 0.0535 0.0921 0.089 Uiso 1 1 calc R . . C31 C 0.1273(8) -0.1157(7) 0.1708(4) 0.0594(19) Uani 1 1 d . . . O3 O 0.1972(8) -0.1787(7) 0.1456(4) 0.103(2) Uani 1 1 d . . . N6 N -0.0390(7) 0.2125(5) 0.2533(4) 0.0435(13) Uani 0.85 1 d P . . C32 C 0.0078(16) 0.3080(8) 0.2744(10) 0.099(5) Uani 0.80 1 d PD . . N7 N 0.4229(6) 0.0223(6) 0.3216(4) 0.0645(16) Uani 1 1 d . . . O5 O 0.4866(9) -0.1321(8) 0.3693(6) 0.132(3) Uani 1 1 d . . . C8 C 0.203(3) 0.5468(15) -0.0307(13) 0.262(13) Uani 1 1 d D . . H8A H 0.2123 0.5880 -0.0768 0.393 Uiso 1 1 calc R . . H8B H 0.2678 0.5934 0.0210 0.393 Uiso 1 1 calc R . . H8C H 0.1026 0.5289 -0.0249 0.393 Uiso 1 1 calc R . . Co2A Co 0.3260(6) 0.2059(6) 0.3142(4) 0.0297(12) Uani 0.15 1 d P . . N6A N 0.251(3) 0.337(3) 0.325(2) 0.045(9) Uani 0.15 1 d P . . C32A C 0.148(4) 0.371(5) 0.316(3) 0.066(12) Uani 0.20 1 d P . . N8 N 0.5649(11) 0.6199(7) 0.2384(7) 0.109(3) Uani 1 1 d . . . C34 C 0.3027(12) 0.6109(10) 0.2442(8) 0.112(4) Uani 1 1 d . . . H34A H 0.2826 0.6803 0.2308 0.168 Uiso 1 1 calc R . . H34B H 0.2892 0.6024 0.3002 0.168 Uiso 1 1 calc R . . H34C H 0.2361 0.5463 0.2035 0.168 Uiso 1 1 calc R . . C35 C 0.4487(11) 0.6162(7) 0.2415(6) 0.079(2) Uani 1 1 d . . . O4A O -0.035(9) 0.369(6) 0.235(5) 0.21(3) Uiso 0.20 1 d PD . . 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 0.0302(5) 0.0397(7) 0.0450(6) 0.0060(5) 0.0105(4) 0.0106(5) Co1 0.0378(5) 0.0570(6) 0.0434(5) 0.0129(4) 0.0082(4) 0.0025(4) N2 0.032(2) 0.044(3) 0.042(3) 0.008(2) 0.007(2) 0.003(2) O1 0.033(2) 0.048(2) 0.045(2) 0.0152(19) 0.0120(17) 0.0074(18) C18 0.035(3) 0.041(3) 0.044(3) 0.014(3) 0.015(2) 0.012(2) O4 0.236(19) 0.064(7) 0.35(2) -0.029(10) 0.194(19) 0.005(9) O2 0.0306(19) 0.042(2) 0.036(2) 0.0020(16) 0.0104(16) 0.0092(16) C17 0.034(3) 0.035(3) 0.041(3) 0.010(2) 0.007(2) 0.008(2) C19 0.045(3) 0.043(3) 0.040(3) 0.012(3) 0.016(3) 0.017(3) C16 0.034(3) 0.037(3) 0.046(3) 0.008(2) 0.014(2) 0.013(2) C7 0.106(8) 0.115(9) 0.132(10) 0.082(8) 0.036(7) 0.014(7) N5 0.018(3) 0.256(12) 0.051(4) 0.079(6) 0.004(3) -0.001(5) C33 0.052(4) 0.050(4) 0.090(6) 0.020(4) 0.016(4) 0.014(4) C15 0.034(3) 0.049(4) 0.046(3) 0.004(3) 0.004(3) -0.001(3) C12 0.035(3) 0.060(4) 0.044(3) 0.008(3) 0.004(3) 0.006(3) C13 0.045(4) 0.079(5) 0.053(4) 0.007(4) -0.004(3) -0.001(4) C11 0.039(3) 0.057(4) 0.041(3) 0.004(3) 0.003(3) 0.007(3) N1 0.035(3) 0.053(3) 0.041(3) 0.011(2) 0.011(2) 0.012(2) C9 0.043(3) 0.057(4) 0.039(3) 0.009(3) 0.009(3) 0.019(3) C6 0.045(3) 0.051(4) 0.045(3) 0.013(3) 0.020(3) 0.015(3) C5 0.063(4) 0.068(5) 0.055(4) 0.025(4) 0.019(3) 0.025(4) C4 0.069(5) 0.068(5) 0.067(5) 0.035(4) 0.022(4) 0.009(4) C3 0.061(5) 0.069(5) 0.067(5) 0.025(4) 0.025(4) 0.004(4) C2 0.050(4) 0.050(4) 0.045(3) 0.011(3) 0.019(3) 0.005(3) C1 0.043(3) 0.046(3) 0.038(3) 0.008(3) 0.020(3) 0.012(3) C10 0.044(4) 0.050(4) 0.053(4) 0.005(3) 0.020(3) 0.001(3) N4 0.035(3) 0.055(3) 0.049(3) 0.004(3) 0.016(2) 0.009(2) C28 0.031(3) 0.058(4) 0.064(4) 0.008(3) 0.015(3) 0.006(3) C27 0.032(3) 0.041(3) 0.059(4) 0.006(3) 0.007(3) 0.006(3) C29 0.063(5) 0.047(4) 0.083(5) 0.007(4) 0.020(4) 0.014(3) C26 0.035(3) 0.051(4) 0.056(4) 0.013(3) 0.005(3) 0.007(3) N3 0.033(2) 0.036(3) 0.045(3) 0.004(2) 0.007(2) 0.006(2) C25 0.039(3) 0.036(3) 0.040(3) 0.006(2) 0.006(2) 0.009(2) C21 0.037(3) 0.032(3) 0.038(3) 0.008(2) 0.007(2) 0.010(2) C22 0.034(3) 0.034(3) 0.038(3) 0.008(2) 0.010(2) 0.013(2) C23 0.062(4) 0.065(4) 0.045(4) 0.009(3) 0.026(3) 0.021(3) C24 0.089(6) 0.084(6) 0.065(5) -0.018(4) 0.038(5) 0.018(5) C20 0.047(3) 0.037(3) 0.038(3) 0.005(2) 0.009(3) 0.010(3) C30 0.034(4) 0.073(5) 0.075(5) 0.016(4) 0.003(3) -0.008(3) C14 0.049(4) 0.073(5) 0.062(4) 0.015(4) 0.013(3) 0.027(4) C31 0.042(4) 0.075(5) 0.044(4) 0.010(3) 0.003(3) -0.006(4) O3 0.086(5) 0.136(6) 0.087(4) -0.014(4) 0.007(4) 0.061(5) N6 0.047(3) 0.037(3) 0.050(3) 0.005(3) 0.017(3) 0.016(3) C32 0.141(12) 0.044(6) 0.159(12) 0.031(7) 0.115(11) 0.044(7) N7 0.047(3) 0.066(4) 0.074(4) -0.008(3) 0.020(3) 0.011(3) O5 0.107(6) 0.130(6) 0.196(9) 0.087(6) 0.051(6) 0.062(5) C8 0.41(4) 0.201(19) 0.30(3) 0.20(2) 0.20(3) 0.16(2) Co2A 0.026(3) 0.027(3) 0.038(3) 0.003(3) 0.011(2) 0.010(2) N6A 0.023(15) 0.09(3) 0.040(18) 0.035(18) 0.023(13) 0.027(17) C32A 0.032(19) 0.11(3) 0.07(3) 0.04(2) 0.029(17) 0.02(2) N8 0.084(6) 0.075(5) 0.163(9) 0.034(6) 0.016(6) 0.018(5) C34 0.091(8) 0.101(8) 0.148(11) 0.017(7) 0.034(7) 0.031(6) C35 0.074(6) 0.060(5) 0.101(7) 0.023(5) 0.017(5) 0.017(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 Co2 Co2A 0.722(6) . ? Co2 N7 1.950(7) . ? Co2 O2 2.036(4) . ? Co2 N3 2.055(5) . ? Co2 N4 2.068(5) . ? Co2 O1 2.074(4) . ? Co1 N5 1.700(12) . ? Co1 N2 1.910(5) . ? Co1 N1 1.919(5) . ? Co1 O2 1.930(4) . ? Co1 N6 1.945(6) . ? Co1 O1 1.945(4) . ? N2 C16 1.278(7) . ? N2 C15 1.471(7) . ? O1 C1 1.308(7) . ? O1 Co2A 1.941(7) . ? C18 C19 1.378(8) . ? C18 C17 1.393(8) . ? C18 H18 0.9300 . ? O4 C32A 1.08(4) . ? O4 C32 1.167(13) . ? O4 O4A 1.25(7) . ? O2 C22 1.324(6) . ? O2 Co2A 2.072(7) . ? C17 C22 1.403(8) . ? C17 C16 1.444(8) . ? C19 C20 1.378(8) . ? C19 C23 1.518(8) . ? C16 H16 0.9300 . ? C7 C8 1.413(15) . ? C7 C4 1.536(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N5 C31 1.266(13) . ? C33 O5 1.133(10) . ? C33 N7 1.176(10) . ? C15 C12 1.522(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C12 C11 1.519(9) . ? C12 C14 1.531(10) . ? C12 C13 1.539(9) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C11 N1 1.476(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N1 C9 1.278(8) . ? C9 C6 1.438(9) . ? C9 H9 0.9300 . ? C6 C5 1.401(9) . ? C6 C1 1.409(9) . ? C5 C4 1.386(10) . ? C5 H5 0.9300 . ? C4 C3 1.383(11) . ? C3 C2 1.395(9) . ? C3 H3 0.9300 . ? C2 C1 1.415(8) . ? C2 C10 1.453(9) . ? C10 N4 1.271(8) . ? C10 H10 0.9300 . ? N4 C28 1.467(8) . ? N4 Co2A 1.920(7) . ? C28 C27 1.528(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C27 C26 1.515(9) . ? C27 C29 1.517(9) . ? C27 C30 1.541(8) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C26 N3 1.472(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? N3 C25 1.271(7) . ? N3 Co2A 1.961(7) . ? C25 C21 1.446(8) . ? C25 H25 0.9300 . ? C21 C20 1.398(8) . ? C21 C22 1.413(8) . ? C23 C24 1.485(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C20 H20 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C31 O3 1.232(10) . ? N6 C32 1.123(12) . ? C32 O4A 1.15(2) . ? C32 C32A 1.36(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? Co2A N6A 1.92(4) . ? N6A C32A 1.17(5) . ? N8 C35 1.119(12) . ? C34 C35 1.401(14) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? 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 Co2A Co2 N7 166.0(5) . . ? Co2A Co2 O2 82.7(5) . . ? N7 Co2 O2 107.0(2) . . ? Co2A Co2 N3 72.3(5) . . ? N7 Co2 N3 97.3(2) . . ? O2 Co2 N3 89.04(17) . . ? Co2A Co2 N4 68.1(5) . . ? N7 Co2 N4 103.4(2) . . ? O2 Co2 N4 149.34(19) . . ? N3 Co2 N4 91.0(2) . . ? Co2A Co2 O1 69.4(5) . . ? N7 Co2 O1 122.4(2) . . ? O2 Co2 O1 74.97(15) . . ? N3 Co2 O1 139.91(19) . . ? N4 Co2 O1 85.62(19) . . ? N5 Co1 N2 90.5(2) . . ? N5 Co1 N1 89.3(2) . . ? N2 Co1 N1 95.4(2) . . ? N5 Co1 O2 92.6(2) . . ? N2 Co1 O2 91.48(18) . . ? N1 Co1 O2 172.84(19) . . ? N5 Co1 N6 178.7(3) . . ? N2 Co1 N6 90.6(2) . . ? N1 Co1 N6 90.0(2) . . ? O2 Co1 N6 88.0(2) . . ? N5 Co1 O1 89.0(2) . . ? N2 Co1 O1 171.82(19) . . ? N1 Co1 O1 92.74(19) . . ? O2 Co1 O1 80.38(16) . . ? N6 Co1 O1 89.9(2) . . ? C16 N2 C15 117.0(5) . . ? C16 N2 Co1 121.9(4) . . ? C15 N2 Co1 121.1(4) . . ? C1 O1 Co2A 120.4(4) . . ? C1 O1 Co1 124.7(4) . . ? Co2A O1 Co1 103.2(2) . . ? C1 O1 Co2 133.1(4) . . ? Co2A O1 Co2 20.37(18) . . ? Co1 O1 Co2 99.36(17) . . ? C19 C18 C17 122.3(5) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C32A O4 C32 75(3) . . ? C32A O4 O4A 117(5) . . ? C32 O4 O4A 57(2) . . ? C22 O2 Co1 123.3(3) . . ? C22 O2 Co2 130.4(3) . . ? Co1 O2 Co2 101.20(17) . . ? C22 O2 Co2A 120.8(4) . . ? Co1 O2 Co2A 99.0(2) . . ? Co2 O2 Co2A 20.22(16) . . ? C18 C17 C22 120.6(5) . . ? C18 C17 C16 116.9(5) . . ? C22 C17 C16 122.3(5) . . ? C20 C19 C18 116.8(5) . . ? C20 C19 C23 122.4(6) . . ? C18 C19 C23 120.8(5) . . ? N2 C16 C17 127.4(5) . . ? N2 C16 H16 116.3 . . ? C17 C16 H16 116.3 . . ? C8 C7 C4 112.8(11) . . ? C8 C7 H7A 109.0 . . ? C4 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? C4 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C31 N5 Co1 157.9(6) . . ? O5 C33 N7 177.3(10) . . ? N2 C15 C12 113.1(5) . . ? N2 C15 H15A 109.0 . . ? C12 C15 H15A 109.0 . . ? N2 C15 H15B 109.0 . . ? C12 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C11 C12 C15 109.8(5) . . ? C11 C12 C14 111.6(6) . . ? C15 C12 C14 111.2(5) . . ? C11 C12 C13 107.4(5) . . ? C15 C12 C13 105.9(5) . . ? C14 C12 C13 110.7(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C11 C12 114.3(5) . . ? N1 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N1 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C9 N1 C11 116.6(5) . . ? C9 N1 Co1 121.2(4) . . ? C11 N1 Co1 122.2(4) . . ? N1 C9 C6 127.9(6) . . ? N1 C9 H9 116.1 . . ? C6 C9 H9 116.1 . . ? C5 C6 C1 120.2(6) . . ? C5 C6 C9 116.4(6) . . ? C1 C6 C9 122.9(5) . . ? C4 C5 C6 122.4(7) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C3 C4 C5 116.7(6) . . ? C3 C4 C7 122.3(8) . . ? C5 C4 C7 120.8(8) . . ? C4 C3 C2 123.5(7) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 C10 116.1(6) . . ? C1 C2 C10 124.7(6) . . ? O1 C1 C6 121.6(5) . . ? O1 C1 C2 120.4(5) . . ? C6 C1 C2 117.9(5) . . ? N4 C10 C2 127.1(6) . . ? N4 C10 H10 116.4 . . ? C2 C10 H10 116.4 . . ? C10 N4 C28 116.6(5) . . ? C10 N4 Co2A 117.5(5) . . ? C28 N4 Co2A 122.2(5) . . ? C10 N4 Co2 128.3(4) . . ? C28 N4 Co2 115.1(4) . . ? Co2A N4 Co2 20.43(18) . . ? N4 C28 C27 112.5(5) . . ? N4 C28 H28A 109.1 . . ? C27 C28 H28A 109.1 . . ? N4 C28 H28B 109.1 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? C26 C27 C29 110.8(6) . . ? C26 C27 C28 111.2(5) . . ? C29 C27 C28 111.8(6) . . ? C26 C27 C30 107.0(5) . . ? C29 C27 C30 109.3(6) . . ? C28 C27 C30 106.5(5) . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C26 C27 114.9(5) . . ? N3 C26 H26A 108.5 . . ? C27 C26 H26A 108.5 . . ? N3 C26 H26B 108.5 . . ? C27 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? C25 N3 C26 116.7(5) . . ? C25 N3 Co2A 120.6(4) . . ? C26 N3 Co2A 121.4(4) . . ? C25 N3 Co2 125.4(4) . . ? C26 N3 Co2 117.1(4) . . ? Co2A N3 Co2 20.54(18) . . ? N3 C25 C21 128.6(5) . . ? N3 C25 H25 115.7 . . ? C21 C25 H25 115.7 . . ? C20 C21 C22 119.1(5) . . ? C20 C21 C25 116.5(5) . . ? C22 C21 C25 124.5(5) . . ? O2 C22 C17 120.4(5) . . ? O2 C22 C21 121.9(5) . . ? C17 C22 C21 117.7(5) . . ? C24 C23 C19 116.1(6) . . ? C24 C23 H23A 108.3 . . ? C19 C23 H23A 108.3 . . ? C24 C23 H23B 108.3 . . ? C19 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C20 C21 123.4(6) . . ? C19 C20 H20 118.3 . . ? C21 C20 H20 118.3 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C31 N5 178.8(9) . . ? C32 N6 Co1 144.6(8) . . ? N6 C32 O4A 120(5) . . ? N6 C32 O4 172.5(19) . . ? O4A C32 O4 65(4) . . ? N6 C32 C32A 129(3) . . ? O4A C32 C32A 104(5) . . ? O4 C32 C32A 50(2) . . ? C33 N7 Co2 160.7(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Co2 Co2A N6A 168.0(11) . . ? Co2 Co2A N4 91.4(5) . . ? N6A Co2A N4 100.4(9) . . ? Co2 Co2A O1 90.3(5) . . ? N6A Co2A O1 86.9(10) . . ? N4 Co2A O1 93.6(3) . . ? Co2 Co2A N3 87.1(5) . . ? N6A Co2A N3 93.2(10) . . ? N4 Co2A N3 98.5(3) . . ? O1 Co2A N3 167.7(4) . . ? Co2 Co2A O2 77.1(5) . . ? N6A Co2A O2 90.9(9) . . ? N4 Co2A O2 165.0(4) . . ? O1 Co2A O2 77.0(2) . . ? N3 Co2A O2 90.6(3) . . ? C32A N6A Co2A 147(4) . . ? O4 C32A N6A 177(4) . . ? O4 C32A C32 55.7(19) . . ? N6A C32A C32 126(5) . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N8 C35 C34 179.3(13) . . ? C32 O4A O4 58(2) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.305 _refine_diff_density_min -1.604 _refine_diff_density_rms 0.094 data_3 _database_code_depnum_ccdc_archive 'CCDC 908083' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H44 Cl Co2 N4 O10' _chemical_formula_weight 822.07 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2 / c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.792(4) _cell_length_b 11.677(6) _cell_length_c 21.775(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.040(10) _cell_angle_gamma 90.00 _cell_volume 3895(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.02 _cell_measurement_theta_max 11.76 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type none # No absorption correction: small crystal _exptl_absorpt_correction_T_min 0.8100 _exptl_absorpt_correction_T_max 0.8672 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-nonius CAD4' _diffrn_measurement_method '\w - 2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 22630 _diffrn_reflns_av_R_equivalents 0.1166 _diffrn_reflns_av_sigmaI/netI 0.1394 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 30.02 _reflns_number_total 11352 _reflns_number_gt 4726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR92(Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0585P)^2^+0.1750P] 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 11352 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1652 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 0.15293(18) 0.0791(3) 0.49045(14) 0.0500(7) Uani 1 1 d . . . C2 C 0.12519(19) 0.0700(3) 0.54785(15) 0.0553(7) Uani 1 1 d . . . C3 C 0.0956(2) -0.0355(3) 0.56379(16) 0.0630(9) Uani 1 1 d . . . H3 H 0.0767 -0.0407 0.6010 0.076 Uiso 1 1 calc R . . C4 C 0.0927(2) -0.1326(3) 0.52746(19) 0.0696(10) Uani 1 1 d . . . C5 C 0.1170(2) -0.1224(3) 0.47160(18) 0.0687(9) Uani 1 1 d . . . H5 H 0.1137 -0.1862 0.4456 0.082 Uiso 1 1 calc R . . C6 C 0.1470(2) -0.0174(3) 0.45229(16) 0.0596(8) Uani 1 1 d . . . C7 C 0.0599(3) -0.2471(4) 0.5498(3) 0.0992(14) Uani 1 1 d . . . H7A H 0.0911 -0.2600 0.5934 0.119 Uiso 1 1 calc R . . H7B H -0.0014 -0.2384 0.5491 0.119 Uiso 1 1 calc R . . C9 C 0.1622(2) -0.0088(3) 0.38975(16) 0.0642(9) Uani 1 1 d . . . H9 H 0.1431 -0.0699 0.3626 0.077 Uiso 1 1 calc R . . C10 C 0.1226(2) 0.1659(3) 0.58984(15) 0.0579(8) Uani 1 1 d . . . H10 H 0.0952 0.1525 0.6224 0.070 Uiso 1 1 calc R . . C11 C 0.1935(3) 0.0702(4) 0.29855(17) 0.0795(11) Uani 1 1 d . . . H11B H 0.1549 0.1310 0.2782 0.095 Uiso 1 1 calc R . . H11A H 0.1677 -0.0020 0.2816 0.095 Uiso 1 1 calc R . . C12 C 0.2811(3) 0.0838(4) 0.28153(16) 0.0746(10) Uani 1 1 d . . . C13 C 0.2643(4) 0.0741(6) 0.20899(18) 0.124(2) Uani 1 1 d . . . H13A H 0.3186 0.0811 0.1968 0.186 Uiso 1 1 calc R . . H13B H 0.2254 0.1340 0.1894 0.186 Uiso 1 1 calc R . . H13C H 0.2385 0.0010 0.1955 0.186 Uiso 1 1 calc R . . C14 C 0.3449(3) -0.0077(4) 0.3132(2) 0.0945(13) Uani 1 1 d . . . H14A H 0.3994 0.0025 0.3018 0.142 Uiso 1 1 calc R . . H14B H 0.3216 -0.0819 0.2997 0.142 Uiso 1 1 calc R . . H14C H 0.3541 -0.0016 0.3584 0.142 Uiso 1 1 calc R . . C15 C 0.3166(3) 0.2027(4) 0.29999(16) 0.0746(10) Uani 1 1 d . . . H15B H 0.3672 0.2151 0.2830 0.090 Uiso 1 1 calc R . . H15A H 0.2727 0.2585 0.2807 0.090 Uiso 1 1 calc R . . C16 C 0.4201(2) 0.2551(3) 0.39223(15) 0.0571(8) Uani 1 1 d . . . H16 H 0.4580 0.2529 0.3656 0.069 Uiso 1 1 calc R . . C17 C 0.45559(18) 0.2951(3) 0.45575(14) 0.0504(7) Uani 1 1 d . . . C18 C 0.54620(19) 0.3108(3) 0.47562(16) 0.0579(8) Uani 1 1 d . . . H18 H 0.5816 0.2880 0.4494 0.070 Uiso 1 1 calc R . . C19 C 0.5837(2) 0.3603(3) 0.53410(18) 0.0646(9) Uani 1 1 d . . . C20 C 0.5286(2) 0.3957(3) 0.57054(16) 0.0622(8) Uani 1 1 d . . . H20 H 0.5530 0.4305 0.6092 0.075 Uiso 1 1 calc R . . C21 C 0.4380(2) 0.3822(3) 0.55249(15) 0.0553(7) Uani 1 1 d . . . C22 C 0.40081(18) 0.3292(2) 0.49369(14) 0.0486(7) Uani 1 1 d . . . C23 C 0.6822(2) 0.3741(4) 0.5561(2) 0.0852(12) Uani 1 1 d . . . H23B H 0.7072 0.3669 0.5198 0.102 Uiso 1 1 calc R . . H23A H 0.6951 0.4506 0.5732 0.102 Uiso 1 1 calc R . . C24 C 0.7232(3) 0.2928(6) 0.6030(3) 0.132(2) Uani 1 1 d . . . H24C H 0.7852 0.3044 0.6133 0.198 Uiso 1 1 calc R . . H24A H 0.7102 0.2166 0.5868 0.198 Uiso 1 1 calc R . . H24B H 0.7018 0.3026 0.6403 0.198 Uiso 1 1 calc R . . C25 C 0.3878(2) 0.4311(3) 0.59429(16) 0.0632(8) Uani 1 1 d . . . H25 H 0.4188 0.4750 0.6279 0.076 Uiso 1 1 calc R . . C26 C 0.2704(3) 0.4808(3) 0.63691(17) 0.0699(9) Uani 1 1 d . . . H26A H 0.2293 0.5381 0.6154 0.084 Uiso 1 1 calc R . . H26B H 0.3174 0.5205 0.6661 0.084 Uiso 1 1 calc R . . C27 C 0.2243(3) 0.4023(3) 0.67481(17) 0.0696(9) Uani 1 1 d . . . C28 C 0.1987(3) 0.4777(4) 0.7252(2) 0.0987(14) Uani 1 1 d . . . H28B H 0.1611 0.5383 0.7049 0.148 Uiso 1 1 calc R . . H28A H 0.2503 0.5099 0.7523 0.148 Uiso 1 1 calc R . . H28C H 0.1687 0.4321 0.7499 0.148 Uiso 1 1 calc R . . C29 C 0.2857(3) 0.3079(4) 0.70718(17) 0.0855(12) Uani 1 1 d . . . H29B H 0.2560 0.2600 0.7311 0.128 Uiso 1 1 calc R . . H29C H 0.3360 0.3415 0.7351 0.128 Uiso 1 1 calc R . . H29A H 0.3036 0.2627 0.6758 0.128 Uiso 1 1 calc R . . C30 C 0.1409(2) 0.3515(3) 0.63461(18) 0.0701(9) Uani 1 1 d . . . H30A H 0.1092 0.3153 0.6624 0.084 Uiso 1 1 calc R . . H30B H 0.1048 0.4132 0.6126 0.084 Uiso 1 1 calc R . . C31 C 0.35340(19) 0.0917(3) 0.53269(16) 0.0539(7) Uani 1 1 d . . . C32 C 0.4154(3) 0.0001(4) 0.5642(2) 0.1000(15) Uani 1 1 d . . . H32B H 0.4328 -0.0452 0.5326 0.150 Uiso 1 1 calc R . . H32A H 0.3870 -0.0480 0.5889 0.150 Uiso 1 1 calc R . . H32C H 0.4659 0.0348 0.5913 0.150 Uiso 1 1 calc R . . C33 C 0.1424(2) 0.3825(4) 0.3983(2) 0.0682(10) Uani 1 1 d . . . C34 C 0.0750(3) 0.4544(5) 0.3523(2) 0.1128(18) Uani 1 1 d . . . H34B H 0.0498 0.5091 0.3756 0.169 Uiso 1 1 calc R . . H34C H 0.0300 0.4055 0.3286 0.169 Uiso 1 1 calc R . . H34A H 0.1028 0.4940 0.3239 0.169 Uiso 1 1 calc R . . Cl2 Cl 0.5000 0.38247(13) 0.2500 0.0746(4) Uani 1 2 d S . . Co1 Co 0.25815(3) 0.19754(4) 0.419208(19) 0.05093(12) Uani 1 1 d . . . Co2 Co 0.23145(3) 0.30850(4) 0.529860(19) 0.05533(13) Uani 1 1 d . . . N1 N 0.19895(17) 0.0731(3) 0.36758(13) 0.0625(7) Uani 1 1 d . . . N2 N 0.34156(17) 0.2224(2) 0.36875(12) 0.0584(6) Uani 1 1 d . . . N3 N 0.30648(17) 0.4203(2) 0.58984(13) 0.0601(7) Uani 1 1 d . . . N4 N 0.15360(17) 0.2666(2) 0.58741(13) 0.0589(6) Uani 1 1 d . . . O1 O 0.17731(13) 0.17926(16) 0.47184(9) 0.0502(5) Uani 1 1 d . . . O2 O 0.31459(12) 0.31984(16) 0.47285(9) 0.0478(4) Uani 1 1 d . . . O3 O 0.32417(14) 0.16047(19) 0.56615(10) 0.0546(5) Uani 1 1 d . . . O4 O 0.33601(13) 0.08919(18) 0.47173(10) 0.0531(5) Uani 1 1 d . . . O5 O 0.15201(15) 0.4040(2) 0.45626(14) 0.0685(6) Uani 1 1 d . . . O6 O 0.17922(15) 0.3081(2) 0.37232(11) 0.0659(6) Uani 1 1 d . . . O9 O 0.4452(2) 0.4483(3) 0.27871(13) 0.1087(11) Uani 1 1 d . . . O10 O 0.5536(2) 0.3134(3) 0.29731(13) 0.1000(10) Uani 1 1 d . . . C8 C 0.0698(5) -0.3496(5) 0.5129(4) 0.159(3) Uani 1 1 d . . . H8A H 0.0480 -0.4153 0.5306 0.238 Uiso 1 1 calc R . . H8B H 0.1304 -0.3608 0.5140 0.238 Uiso 1 1 calc R . . H8C H 0.0375 -0.3396 0.4698 0.238 Uiso 1 1 calc R . . Cl1 Cl 0.0000 0.81501(16) 0.2500 0.0856(4) Uani 1 2 d S . . O8 O 0.0298(3) 0.8902(5) 0.2110(2) 0.181(2) Uani 1 1 d . A . O7A O 0.0825(6) 0.7748(11) 0.2779(6) 0.167(7) Uani 0.50 1 d P A 1 O7B O 0.0425(6) 0.7413(12) 0.2936(7) 0.174(6) Uani 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0400(13) 0.0503(17) 0.0570(17) 0.0090(14) 0.0065(12) -0.0058(13) C2 0.0463(15) 0.0592(19) 0.0589(18) 0.0135(15) 0.0100(13) -0.0043(15) C3 0.0552(17) 0.065(2) 0.068(2) 0.0211(18) 0.0125(15) -0.0064(16) C4 0.0578(19) 0.058(2) 0.092(3) 0.014(2) 0.0158(18) -0.0105(17) C5 0.0632(19) 0.057(2) 0.089(3) -0.0015(18) 0.0234(19) -0.0166(17) C6 0.0528(17) 0.0559(19) 0.069(2) -0.0042(16) 0.0124(15) -0.0092(15) C7 0.095(3) 0.056(2) 0.152(4) 0.017(3) 0.039(3) -0.020(2) C9 0.0596(18) 0.063(2) 0.068(2) -0.0105(17) 0.0096(16) -0.0168(17) C10 0.0532(16) 0.064(2) 0.0587(18) 0.0136(15) 0.0175(14) 0.0024(16) C11 0.079(2) 0.092(3) 0.060(2) -0.005(2) 0.0018(18) -0.027(2) C12 0.089(3) 0.085(3) 0.0476(19) -0.0106(18) 0.0126(18) -0.025(2) C13 0.143(4) 0.174(6) 0.056(2) -0.031(3) 0.025(3) -0.056(4) C14 0.111(3) 0.089(3) 0.088(3) -0.026(2) 0.033(3) -0.003(3) C15 0.083(2) 0.087(3) 0.0514(18) 0.0040(19) 0.0105(17) -0.014(2) C16 0.0588(17) 0.0519(18) 0.0642(19) 0.0014(15) 0.0216(15) -0.0063(16) C17 0.0483(14) 0.0446(16) 0.0589(17) 0.0022(14) 0.0140(13) -0.0039(13) C18 0.0490(15) 0.0529(18) 0.074(2) 0.0011(16) 0.0185(15) -0.0027(15) C19 0.0480(16) 0.065(2) 0.078(2) 0.0085(18) 0.0099(16) -0.0088(16) C20 0.0597(18) 0.062(2) 0.0610(19) -0.0015(16) 0.0064(16) -0.0114(17) C21 0.0597(17) 0.0477(17) 0.0568(18) -0.0008(14) 0.0106(15) -0.0032(15) C22 0.0484(15) 0.0355(15) 0.0600(17) 0.0054(12) 0.0099(13) -0.0031(12) C23 0.0546(19) 0.095(3) 0.097(3) 0.017(2) 0.001(2) -0.013(2) C24 0.077(3) 0.170(6) 0.145(5) 0.051(4) 0.017(3) 0.022(4) C25 0.071(2) 0.057(2) 0.0593(19) -0.0060(16) 0.0105(16) -0.0072(17) C26 0.077(2) 0.055(2) 0.081(2) -0.0100(18) 0.0265(19) -0.0033(19) C27 0.081(2) 0.067(2) 0.067(2) -0.0095(17) 0.0300(18) 0.0034(19) C28 0.116(3) 0.091(3) 0.102(3) -0.026(3) 0.051(3) 0.002(3) C29 0.107(3) 0.094(3) 0.054(2) -0.004(2) 0.018(2) 0.012(3) C30 0.078(2) 0.059(2) 0.084(2) -0.0024(18) 0.040(2) 0.0052(19) C31 0.0499(15) 0.0482(17) 0.061(2) 0.0068(15) 0.0088(14) 0.0016(14) C32 0.128(4) 0.093(3) 0.074(3) 0.016(2) 0.014(2) 0.048(3) C33 0.0582(19) 0.070(2) 0.077(2) 0.026(2) 0.0165(18) -0.0048(18) C34 0.093(3) 0.131(4) 0.114(4) 0.060(3) 0.024(3) 0.038(3) Cl2 0.0816(8) 0.0903(10) 0.0550(7) 0.000 0.0224(6) 0.000 Co1 0.0488(2) 0.0494(2) 0.0542(2) -0.00120(19) 0.01172(17) -0.00747(19) Co2 0.0574(2) 0.0566(3) 0.0531(2) 0.0015(2) 0.01569(18) -0.0095(2) N1 0.0589(15) 0.0647(18) 0.0605(16) -0.0033(14) 0.0079(13) -0.0145(14) N2 0.0630(15) 0.0590(16) 0.0555(15) -0.0018(12) 0.0187(12) -0.0118(14) N3 0.0608(16) 0.0565(16) 0.0639(16) -0.0013(13) 0.0172(13) -0.0037(14) N4 0.0609(15) 0.0535(15) 0.0633(16) 0.0062(13) 0.0172(13) 0.0003(13) O1 0.0494(10) 0.0461(11) 0.0554(11) 0.0075(9) 0.0133(9) -0.0051(9) O2 0.0459(10) 0.0455(11) 0.0509(10) 0.0000(9) 0.0096(8) -0.0047(9) O3 0.0584(11) 0.0517(12) 0.0532(12) 0.0019(10) 0.0128(10) 0.0008(10) O4 0.0591(11) 0.0462(11) 0.0545(12) -0.0013(9) 0.0145(10) -0.0019(10) O5 0.0609(13) 0.0541(14) 0.0964(19) 0.0088(13) 0.0304(13) 0.0063(11) O6 0.0599(12) 0.0752(16) 0.0604(13) 0.0192(12) 0.0101(11) 0.0006(13) O9 0.120(2) 0.121(3) 0.0818(19) -0.0226(18) 0.0191(17) 0.037(2) O10 0.099(2) 0.126(3) 0.0823(18) 0.0327(18) 0.0370(16) 0.027(2) C8 0.159(6) 0.084(4) 0.237(8) 0.030(5) 0.054(6) -0.011(4) Cl1 0.0697(7) 0.1168(13) 0.0697(8) 0.000 0.0160(7) 0.000 O8 0.188(5) 0.240(6) 0.147(4) -0.036(4) 0.101(4) -0.085(5) O7A 0.093(7) 0.161(10) 0.201(12) -0.095(10) -0.053(7) 0.059(6) O7B 0.094(7) 0.199(11) 0.203(10) 0.108(9) -0.014(7) 0.044(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.325(3) . ? C1 C6 1.390(5) . ? C1 C2 1.425(4) . ? C2 C3 1.391(4) . ? C2 C10 1.453(5) . ? C3 C4 1.378(5) . ? C3 H3 0.9300 . ? C4 C5 1.366(5) . ? C4 C7 1.553(5) . ? C5 C6 1.414(5) . ? C5 H5 0.9300 . ? C6 C9 1.443(5) . ? C7 C8 1.472(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 N1 1.272(4) . ? C9 H9 0.9300 . ? C10 N4 1.279(4) . ? C10 H10 0.9300 . ? C11 N1 1.485(4) . ? C11 C12 1.524(5) . ? C11 H11B 0.9700 . ? C11 H11A 0.9700 . ? C12 C14 1.515(6) . ? C12 C15 1.515(5) . ? C12 C13 1.541(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N2 1.471(4) . ? C15 H15B 0.9700 . ? C15 H15A 0.9700 . ? C16 N2 1.280(4) . ? C16 C17 1.438(4) . ? C16 H16 0.9300 . ? C17 C22 1.392(4) . ? C17 C18 1.403(4) . ? C18 C19 1.393(5) . ? C18 H18 0.9300 . ? C19 C20 1.376(5) . ? C19 C23 1.520(5) . ? C20 C21 1.398(5) . ? C20 H20 0.9300 . ? C21 C22 1.415(4) . ? C21 C25 1.461(5) . ? C22 O2 1.331(3) . ? C23 C24 1.430(6) . ? C23 H23B 0.9700 . ? C23 H23A 0.9700 . ? C24 H24C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C25 N3 1.270(4) . ? C25 H25 0.9300 . ? C26 N3 1.469(4) . ? C26 C27 1.531(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C30 1.514(5) . ? C27 C29 1.523(5) . ? C27 C28 1.535(5) . ? C28 H28B 0.9600 . ? C28 H28A 0.9600 . ? C28 H28C 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C29 H29A 0.9600 . ? C30 N4 1.476(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 O3 1.246(4) . ? C31 O4 1.289(4) . ? C31 C32 1.499(5) . ? C32 H32B 0.9600 . ? C32 H32A 0.9600 . ? C32 H32C 0.9600 . ? C33 O6 1.253(5) . ? C33 O5 1.260(5) . ? C33 C34 1.524(5) . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C34 H34A 0.9600 . ? Cl2 O9 1.412(3) . ? Cl2 O9 1.412(3) 2_655 ? Cl2 O10 1.416(3) . ? Cl2 O10 1.416(3) 2_655 ? Co1 O6 1.909(2) . ? Co1 O2 1.922(2) . ? Co1 O1 1.923(2) . ? Co1 N2 1.931(3) . ? Co1 N1 1.934(3) . ? Co1 O4 1.933(2) . ? Co1 Co2 2.8557(8) . ? Co2 N3 2.016(3) . ? Co2 O1 2.020(2) . ? Co2 O2 2.018(2) . ? Co2 N4 2.017(3) . ? Co2 O5 2.100(3) . ? Co2 O3 2.279(2) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? Cl1 O7B 1.335(11) . ? Cl1 O7B 1.335(11) 2 ? Cl1 O8 1.382(5) 2 ? Cl1 O8 1.382(5) . ? Cl1 O7A 1.380(9) . ? Cl1 O7A 1.380(9) 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 C1 C6 121.0(3) . . ? O1 C1 C2 120.5(3) . . ? C6 C1 C2 118.3(3) . . ? C3 C2 C1 118.6(3) . . ? C3 C2 C10 117.6(3) . . ? C1 C2 C10 123.8(3) . . ? C4 C3 C2 123.5(3) . . ? C4 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? C5 C4 C3 117.5(3) . . ? C5 C4 C7 122.8(4) . . ? C3 C4 C7 119.7(4) . . ? C4 C5 C6 121.8(3) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C1 C6 C5 120.2(3) . . ? C1 C6 C9 120.3(3) . . ? C5 C6 C9 119.1(3) . . ? C8 C7 C4 116.2(4) . . ? C8 C7 H7A 108.2 . . ? C4 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? C4 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? N1 C9 C6 127.3(3) . . ? N1 C9 H9 116.3 . . ? C6 C9 H9 116.3 . . ? N4 C10 C2 127.8(3) . . ? N4 C10 H10 116.1 . . ? C2 C10 H10 116.1 . . ? N1 C11 C12 114.2(3) . . ? N1 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? N1 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? H11B C11 H11A 107.6 . . ? C14 C12 C15 111.3(3) . . ? C14 C12 C11 111.0(3) . . ? C15 C12 C11 109.3(4) . . ? C14 C12 C13 110.2(4) . . ? C15 C12 C13 107.4(4) . . ? C11 C12 C13 107.5(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C12 113.8(3) . . ? N2 C15 H15B 108.8 . . ? C12 C15 H15B 108.8 . . ? N2 C15 H15A 108.8 . . ? C12 C15 H15A 108.8 . . ? H15B C15 H15A 107.7 . . ? N2 C16 C17 126.5(3) . . ? N2 C16 H16 116.8 . . ? C17 C16 H16 116.8 . . ? C22 C17 C18 120.9(3) . . ? C22 C17 C16 120.7(3) . . ? C18 C17 C16 118.0(3) . . ? C19 C18 C17 120.8(3) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 117.6(3) . . ? C20 C19 C23 121.9(4) . . ? C18 C19 C23 120.5(3) . . ? C19 C20 C21 123.5(3) . . ? C19 C20 H20 118.3 . . ? C21 C20 H20 118.3 . . ? C20 C21 C22 118.4(3) . . ? C20 C21 C25 117.0(3) . . ? C22 C21 C25 124.4(3) . . ? O2 C22 C17 120.4(3) . . ? O2 C22 C21 120.7(3) . . ? C17 C22 C21 118.7(3) . . ? C24 C23 C19 114.0(4) . . ? C24 C23 H23B 108.8 . . ? C19 C23 H23B 108.8 . . ? C24 C23 H23A 108.8 . . ? C19 C23 H23A 108.8 . . ? H23B C23 H23A 107.7 . . ? C23 C24 H24C 109.5 . . ? C23 C24 H24A 109.5 . . ? H24C C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24C C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C25 C21 127.3(3) . . ? N3 C25 H25 116.4 . . ? C21 C25 H25 116.4 . . ? N3 C26 C27 113.8(3) . . ? N3 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? N3 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C30 C27 C29 110.5(3) . . ? C30 C27 C26 112.6(3) . . ? C29 C27 C26 110.5(3) . . ? C30 C27 C28 107.2(3) . . ? C29 C27 C28 109.4(3) . . ? C26 C27 C28 106.5(3) . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? C27 C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? N4 C30 C27 114.8(3) . . ? N4 C30 H30A 108.6 . . ? C27 C30 H30A 108.6 . . ? N4 C30 H30B 108.6 . . ? C27 C30 H30B 108.6 . . ? H30A C30 H30B 107.5 . . ? O3 C31 O4 126.9(3) . . ? O3 C31 C32 119.0(3) . . ? O4 C31 C32 114.1(3) . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C31 C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? O6 C33 O5 129.3(3) . . ? O6 C33 C34 114.4(4) . . ? O5 C33 C34 116.3(4) . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C34 H34A 109.5 . . ? H34B C34 H34A 109.5 . . ? H34C C34 H34A 109.5 . . ? O9 Cl2 O9 114.1(3) . 2_655 ? O9 Cl2 O10 108.11(17) . . ? O9 Cl2 O10 108.01(18) 2_655 . ? O9 Cl2 O10 108.01(18) . 2_655 ? O9 Cl2 O10 108.10(17) 2_655 2_655 ? O10 Cl2 O10 110.6(3) . 2_655 ? O6 Co1 O2 88.22(10) . . ? O6 Co1 O1 87.25(9) . . ? O2 Co1 O1 89.85(8) . . ? O6 Co1 N2 92.36(11) . . ? O2 Co1 N2 87.39(10) . . ? O1 Co1 N2 177.22(10) . . ? O6 Co1 N1 92.08(12) . . ? O2 Co1 N1 177.85(10) . . ? O1 Co1 N1 88.04(10) . . ? N2 Co1 N1 94.72(12) . . ? O6 Co1 O4 176.18(10) . . ? O2 Co1 O4 89.55(9) . . ? O1 Co1 O4 89.64(8) . . ? N2 Co1 O4 90.64(10) . . ? N1 Co1 O4 90.03(11) . . ? O6 Co1 Co2 86.19(8) . . ? O2 Co1 Co2 44.90(6) . . ? O1 Co1 Co2 44.95(6) . . ? N2 Co1 Co2 132.28(8) . . ? N1 Co1 Co2 132.99(8) . . ? O4 Co1 Co2 90.04(7) . . ? N3 Co2 O1 169.17(10) . . ? N3 Co2 O2 89.32(9) . . ? O1 Co2 O2 84.50(8) . . ? N3 Co2 N4 96.06(11) . . ? O1 Co2 N4 88.74(10) . . ? O2 Co2 N4 169.60(10) . . ? N3 Co2 O5 107.39(11) . . ? O1 Co2 O5 80.53(9) . . ? O2 Co2 O5 81.55(9) . . ? N4 Co2 O5 105.16(10) . . ? N3 Co2 O3 92.26(10) . . ? O1 Co2 O3 77.82(9) . . ? O2 Co2 O3 78.69(8) . . ? N4 Co2 O3 92.17(10) . . ? O5 Co2 O3 151.86(9) . . ? N3 Co2 Co1 131.04(8) . . ? O1 Co2 Co1 42.28(6) . . ? O2 Co2 Co1 42.23(6) . . ? N4 Co2 Co1 130.63(9) . . ? O5 Co2 Co1 77.30(8) . . ? O3 Co2 Co1 74.60(6) . . ? C9 N1 C11 116.6(3) . . ? C9 N1 Co1 123.0(2) . . ? C11 N1 Co1 120.4(2) . . ? C16 N2 C15 116.6(3) . . ? C16 N2 Co1 123.1(2) . . ? C15 N2 Co1 120.3(2) . . ? C25 N3 C26 117.1(3) . . ? C25 N3 Co2 122.5(3) . . ? C26 N3 Co2 119.8(2) . . ? C10 N4 C30 118.1(3) . . ? C10 N4 Co2 123.0(2) . . ? C30 N4 Co2 118.4(2) . . ? C1 O1 Co1 124.35(18) . . ? C1 O1 Co2 125.35(18) . . ? Co1 O1 Co2 92.77(8) . . ? C22 O2 Co1 123.61(18) . . ? C22 O2 Co2 124.05(18) . . ? Co1 O2 Co2 92.87(8) . . ? C31 O3 Co2 125.7(2) . . ? C31 O4 Co1 122.70(19) . . ? C33 O5 Co2 124.3(2) . . ? C33 O6 Co1 122.8(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O7B Cl1 O7B 99.7(14) . 2 ? O7B Cl1 O8 99.2(7) . 2 ? O7B Cl1 O8 131.3(5) 2 2 ? O7B Cl1 O8 131.3(5) . . ? O7B Cl1 O8 99.2(7) 2 . ? O8 Cl1 O8 101.1(5) 2 . ? O7B Cl1 O7A 37.8(8) . . ? O7B Cl1 O7A 110.6(6) 2 . ? O8 Cl1 O7A 111.8(5) 2 . ? O8 Cl1 O7A 93.5(7) . . ? O7B Cl1 O7A 110.6(6) . 2 ? O7B Cl1 O7A 37.8(8) 2 2 ? O8 Cl1 O7A 93.5(7) 2 2 ? O8 Cl1 O7A 111.8(5) . 2 ? O7A Cl1 O7A 140.2(11) . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.486 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.067