# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email c.k.williams@imperial.ac.uk _publ_contact_author_name 'Charlotte Williams' loop_ _publ_author_name 'Charlotte Williams' 'Michael Kember' 'Antoine Burchard' 'Fabian Jutz' 'Andrew White' data_1a _database_code_depnum_ccdc_archive 'CCDC 825190' #TrackingRef '- kember et al_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H54 Co3 I4 N4 O2, 3(C4 H8 O)' _chemical_formula_sum 'C46 H78 Co3 I4 N4 O5' _chemical_formula_weight 1451.51 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.79263(10) _cell_length_b 21.62584(18) _cell_length_c 22.16086(19) _cell_angle_alpha 90.00 _cell_angle_beta 102.5923(9) _cell_angle_gamma 90.00 _cell_volume 5515.64(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34750 _cell_measurement_theta_min 2.9714 _cell_measurement_theta_max 32.6932 _exptl_crystal_description blocks _exptl_crystal_colour Brown _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2860 _exptl_absorpt_coefficient_mu 3.174 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.511 _exptl_absorpt_correction_T_max 0.741 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67792 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 32.77 _reflns_number_total 18599 _reflns_number_gt 14055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18599 _refine_ls_number_parameters 629 _refine_ls_number_restraints 435 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0548 _refine_ls_wR_factor_gt 0.0530 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.41176(2) 0.412749(12) 0.621617(12) 0.01714(5) Uani 1 1 d . . . Co2 Co 0.52657(2) 0.500344(12) 0.720069(12) 0.01815(5) Uani 1 1 d . . . Co3 Co 0.39676(2) 0.377078(13) 0.764035(13) 0.02106(6) Uani 1 1 d D . . I1 I 0.613094(11) 0.481360(6) 0.604854(6) 0.02338(3) Uani 1 1 d . . . I2 I 0.225795(11) 0.354429(6) 0.670432(7) 0.02566(3) Uani 1 1 d . A . I3 I 0.397764(13) 0.482124(7) 0.821174(7) 0.02836(4) Uani 1 1 d . A . I4 I 0.45721(5) 0.28271(3) 0.83188(3) 0.03701(12) Uani 0.973(3) 1 d PD A 1 I4' I 0.4789(8) 0.2970(7) 0.8483(7) 0.026(2) Uiso 0.027(3) 1 d PD A 2 O1 O 0.51587(11) 0.39988(6) 0.71570(6) 0.0172(3) Uani 1 1 d . A . C1 C 0.61580(16) 0.36346(9) 0.72678(9) 0.0189(4) Uani 1 1 d . . . C2 C 0.61847(17) 0.30861(9) 0.69417(9) 0.0219(4) Uani 1 1 d . A . C3 C 0.51343(18) 0.28512(9) 0.64988(10) 0.0241(4) Uani 1 1 d . . . H3A H 0.5316 0.2442 0.6344 0.029 Uiso 1 1 calc R A . H3B H 0.4502 0.2793 0.6723 0.029 Uiso 1 1 calc R . . N4 N 0.47099(15) 0.32656(8) 0.59598(8) 0.0202(3) Uani 1 1 d D A . H4 H 0.5329(13) 0.3340(12) 0.5795(10) 0.037(7) Uiso 1 1 d D . . C5 C 0.39005(19) 0.29102(10) 0.54815(10) 0.0260(4) Uani 1 1 d . . . H5A H 0.3233 0.2780 0.5656 0.031 Uiso 1 1 calc R A . H5B H 0.4303 0.2530 0.5392 0.031 Uiso 1 1 calc R . . C6 C 0.34296(18) 0.32446(10) 0.48722(9) 0.0244(4) Uani 1 1 d . A . C7 C 0.25981(18) 0.37677(10) 0.49483(10) 0.0253(4) Uani 1 1 d . . . H7A H 0.2225 0.3923 0.4532 0.030 Uiso 1 1 calc R A . H7B H 0.1978 0.3593 0.5134 0.030 Uiso 1 1 calc R . . N8 N 0.31196(14) 0.43007(7) 0.53295(7) 0.0189(3) Uani 1 1 d D A . H8 H 0.3577(17) 0.4502(10) 0.5119(9) 0.031(6) Uiso 1 1 d D . . C9 C 0.21486(17) 0.47249(9) 0.53797(9) 0.0222(4) Uani 1 1 d . . . H9A H 0.1687 0.4532 0.5653 0.027 Uiso 1 1 calc R A . H9B H 0.1633 0.4772 0.4965 0.027 Uiso 1 1 calc R . . C10 C 0.25279(16) 0.53532(9) 0.56262(9) 0.0195(4) Uani 1 1 d . A . C11 C 0.32227(15) 0.54392(9) 0.62215(8) 0.0165(4) Uani 1 1 d . . . O11 O 0.37103(11) 0.49522(6) 0.65724(6) 0.0165(3) Uani 1 1 d . A . C12 C 0.33643(16) 0.60453(9) 0.64498(9) 0.0185(4) Uani 1 1 d . A . C13 C 0.39674(17) 0.61760(9) 0.71017(9) 0.0209(4) Uani 1 1 d . . . H13A H 0.3930 0.6625 0.7182 0.025 Uiso 1 1 calc R A . H13B H 0.3561 0.5957 0.7385 0.025 Uiso 1 1 calc R . . N14 N 0.52046(14) 0.59769(8) 0.72314(7) 0.0194(3) Uani 1 1 d D A . H14 H 0.5461(18) 0.6101(10) 0.6897(6) 0.027(6) Uiso 1 1 d D . . C15 C 0.58409(18) 0.62823(10) 0.78014(10) 0.0255(4) Uani 1 1 d . . . H15A H 0.5468 0.6170 0.8146 0.031 Uiso 1 1 calc R A . H15B H 0.5771 0.6736 0.7744 0.031 Uiso 1 1 calc R . . C16 C 0.71284(19) 0.61133(10) 0.79834(10) 0.0276(4) Uani 1 1 d . A . C17 C 0.7297(2) 0.54559(10) 0.82436(10) 0.0289(5) Uani 1 1 d . . . H17A H 0.8130 0.5398 0.8437 0.035 Uiso 1 1 calc R A . H17B H 0.6857 0.5415 0.8574 0.035 Uiso 1 1 calc R . . N18 N 0.69301(14) 0.49500(8) 0.77865(8) 0.0215(3) Uani 1 1 d D A . H18 H 0.7432(18) 0.4952(13) 0.7534(10) 0.048(8) Uiso 1 1 d D . . C19 C 0.70995(18) 0.43529(10) 0.81328(10) 0.0245(4) Uani 1 1 d . . . H19A H 0.6465 0.4301 0.8356 0.029 Uiso 1 1 calc R A . H19B H 0.7841 0.4370 0.8444 0.029 Uiso 1 1 calc R . . C20 C 0.71182(17) 0.38025(9) 0.77239(9) 0.0224(4) Uani 1 1 d . A . C21 C 0.81088(18) 0.34305(10) 0.78280(10) 0.0276(5) Uani 1 1 d . . . H21A H 0.8762 0.3552 0.8137 0.033 Uiso 1 1 calc R A . C22 C 0.81813(19) 0.28953(11) 0.75022(10) 0.0285(5) Uani 1 1 d . A . C23 C 0.71895(19) 0.27317(10) 0.70636(10) 0.0268(5) Uani 1 1 d . . . H23A H 0.7202 0.2360 0.6837 0.032 Uiso 1 1 calc R A . C24 C 0.9287(2) 0.24986(12) 0.76052(11) 0.0353(6) Uani 1 1 d D . . C25 C 1.0357(3) 0.28483(17) 0.80374(16) 0.0428(9) Uani 0.775(4) 1 d PD A 1 H25A H 1.0485 0.3245 0.7849 0.064 Uiso 0.775(4) 1 calc PR A 1 H25B H 1.1057 0.2593 0.8084 0.064 Uiso 0.775(4) 1 calc PR A 1 H25C H 1.0185 0.2921 0.8445 0.064 Uiso 0.775(4) 1 calc PR A 1 C26 C 0.9669(3) 0.24130(16) 0.69960(15) 0.0385(8) Uani 0.775(4) 1 d PD A 1 H26A H 0.9769 0.2819 0.6818 0.058 Uiso 0.775(4) 1 calc PR A 1 H26B H 0.9076 0.2178 0.6708 0.058 Uiso 0.775(4) 1 calc PR A 1 H26C H 1.0407 0.2188 0.7071 0.058 Uiso 0.775(4) 1 calc PR A 1 C27 C 0.9126(3) 0.19126(16) 0.7906(2) 0.0505(12) Uani 0.775(4) 1 d PD A 1 H27A H 0.8883 0.1995 0.8294 0.076 Uiso 0.775(4) 1 calc PR A 1 H27B H 0.9860 0.1683 0.7994 0.076 Uiso 0.775(4) 1 calc PR A 1 H27C H 0.8528 0.1668 0.7632 0.076 Uiso 0.775(4) 1 calc PR A 1 C25' C 1.0156(8) 0.2779(5) 0.7405(5) 0.033(2) Uiso 0.225(4) 1 d PD A 2 H25D H 0.9862 0.2940 0.6987 0.049 Uiso 0.225(4) 1 calc PR A 2 H25E H 1.0778 0.2480 0.7399 0.049 Uiso 0.225(4) 1 calc PR A 2 H25F H 1.0461 0.3121 0.7684 0.049 Uiso 0.225(4) 1 calc PR A 2 C26' C 0.8952(9) 0.1833(4) 0.7202(5) 0.037(3) Uiso 0.225(4) 1 d PD A 2 H26D H 0.8306 0.1628 0.7335 0.056 Uiso 0.225(4) 1 calc PR A 2 H26E H 0.9631 0.1560 0.7279 0.056 Uiso 0.225(4) 1 calc PR A 2 H26F H 0.8726 0.1927 0.6760 0.056 Uiso 0.225(4) 1 calc PR A 2 C27' C 0.9483(9) 0.2233(5) 0.8266(4) 0.033(2) Uiso 0.225(4) 1 d PD A 2 H27D H 0.8758 0.2051 0.8331 0.050 Uiso 0.225(4) 1 calc PR A 2 H27E H 0.9727 0.2566 0.8567 0.050 Uiso 0.225(4) 1 calc PR A 2 H27F H 1.0087 0.1914 0.8321 0.050 Uiso 0.225(4) 1 calc PR A 2 C28 C 0.44185(19) 0.34740(10) 0.45839(10) 0.0272(5) Uani 1 1 d . . . H28A H 0.4094 0.3685 0.4193 0.041 Uiso 1 1 calc R A . H28B H 0.4888 0.3121 0.4505 0.041 Uiso 1 1 calc R . . H28C H 0.4908 0.3762 0.4868 0.041 Uiso 1 1 calc R . . C29 C 0.2689(2) 0.27732(11) 0.44419(11) 0.0352(5) Uani 1 1 d . . . H29A H 0.2367 0.2968 0.4042 0.053 Uiso 1 1 calc R A . H29B H 0.2054 0.2630 0.4627 0.053 Uiso 1 1 calc R . . H29C H 0.3174 0.2420 0.4381 0.053 Uiso 1 1 calc R . . C30 C 0.20736(17) 0.58630(10) 0.52751(9) 0.0226(4) Uani 1 1 d . . . H30A H 0.1615 0.5793 0.4872 0.027 Uiso 1 1 calc R A . C31 C 0.22525(17) 0.64702(9) 0.54810(9) 0.0216(4) Uani 1 1 d . A . C32 C 0.28934(17) 0.65434(9) 0.60774(10) 0.0225(4) Uani 1 1 d . . . H32A H 0.3019 0.6950 0.6241 0.027 Uiso 1 1 calc R A . C33 C 0.17519(19) 0.70085(10) 0.50613(10) 0.0281(5) Uani 1 1 d . . . C34 C 0.2328(3) 0.70127(14) 0.44970(12) 0.0494(7) Uani 1 1 d . A . H34A H 0.3169 0.7066 0.4639 0.074 Uiso 1 1 calc R . . H34B H 0.2011 0.7354 0.4221 0.074 Uiso 1 1 calc R . . H34C H 0.2170 0.6620 0.4274 0.074 Uiso 1 1 calc R . . C35 C 0.0443(2) 0.69319(14) 0.48370(14) 0.0517(8) Uani 1 1 d . A . H35A H 0.0073 0.6938 0.5192 0.077 Uiso 1 1 calc R . . H35B H 0.0278 0.6537 0.4619 0.077 Uiso 1 1 calc R . . H35C H 0.0136 0.7272 0.4556 0.077 Uiso 1 1 calc R . . C36 C 0.1991(3) 0.76332(11) 0.53844(13) 0.0450(7) Uani 1 1 d . A . H36A H 0.2830 0.7688 0.5532 0.068 Uiso 1 1 calc R . . H36B H 0.1611 0.7648 0.5736 0.068 Uiso 1 1 calc R . . H36C H 0.1684 0.7964 0.5092 0.068 Uiso 1 1 calc R . . C37 C 0.7721(2) 0.61969(12) 0.74397(12) 0.0367(6) Uani 1 1 d . . . H37A H 0.7366 0.5917 0.7103 0.055 Uiso 1 1 calc R A . H37B H 0.8550 0.6102 0.7574 0.055 Uiso 1 1 calc R . . H37C H 0.7626 0.6625 0.7293 0.055 Uiso 1 1 calc R . . C38 C 0.7674(2) 0.65516(12) 0.85135(12) 0.0447(6) Uani 1 1 d . . . H38A H 0.7293 0.6493 0.8861 0.067 Uiso 1 1 calc R A . H38B H 0.7572 0.6981 0.8369 0.067 Uiso 1 1 calc R . . H38C H 0.8505 0.6461 0.8648 0.067 Uiso 1 1 calc R . . O40 O 0.93304(16) 0.47923(9) 0.74309(9) 0.0475(5) Uani 1 1 d . . . C41 C 1.0393(3) 0.51205(17) 0.74999(17) 0.0645(9) Uani 1 1 d . . . H41A H 1.1028 0.4886 0.7769 0.077 Uiso 1 1 calc R . . H41B H 1.0329 0.5528 0.7693 0.077 Uiso 1 1 calc R . . C42 C 1.0650(3) 0.52053(15) 0.68762(18) 0.0724(11) Uani 1 1 d . . . H42A H 1.1439 0.5054 0.6868 0.087 Uiso 1 1 calc R . . H42B H 1.0588 0.5646 0.6752 0.087 Uiso 1 1 calc R . . C43 C 0.9716(3) 0.48151(15) 0.64529(15) 0.0555(8) Uani 1 1 d . . . H43A H 0.9085 0.5079 0.6217 0.067 Uiso 1 1 calc R . . H43B H 1.0052 0.4567 0.6160 0.067 Uiso 1 1 calc R . . C44 C 0.9284(2) 0.44103(13) 0.69020(12) 0.0407(6) Uani 1 1 d . . . H44A H 0.8479 0.4272 0.6729 0.049 Uiso 1 1 calc R . . H44B H 0.9788 0.4042 0.7009 0.049 Uiso 1 1 calc R . . O50 O 0.0684(9) 0.4422(5) 0.8973(4) 0.134(4) Uiso 0.432(4) 1 d PDU B 1 C51 C -0.0118(13) 0.4521(9) 0.9377(7) 0.149(6) Uiso 0.432(4) 1 d PDU B 1 H51A H -0.0922 0.4406 0.9171 0.179 Uiso 0.432(4) 1 calc PR B 1 H51B H -0.0106 0.4956 0.9517 0.179 Uiso 0.432(4) 1 calc PR B 1 C52 C 0.0383(11) 0.4077(7) 0.9921(5) 0.113(4) Uiso 0.432(4) 1 d PDU B 1 H52A H 0.0540 0.4304 1.0319 0.135 Uiso 0.432(4) 1 calc PR B 1 H52B H -0.0174 0.3740 0.9943 0.135 Uiso 0.432(4) 1 calc PR B 1 C53 C 0.1464(15) 0.3826(10) 0.9796(7) 0.165(7) Uiso 0.432(4) 1 d PDU B 1 H53A H 0.2110 0.3910 1.0155 0.198 Uiso 0.432(4) 1 calc PR B 1 H53B H 0.1389 0.3372 0.9744 0.198 Uiso 0.432(4) 1 calc PR B 1 C54 C 0.1734(9) 0.4096(6) 0.9243(5) 0.079(3) Uiso 0.432(4) 1 d PDU B 1 H54A H 0.2404 0.4381 0.9349 0.095 Uiso 0.432(4) 1 calc PR B 1 H54B H 0.1907 0.3772 0.8961 0.095 Uiso 0.432(4) 1 calc PR B 1 O50' O -0.0197(9) 0.4119(6) 0.9382(6) 0.110(4) Uiso 0.320(7) 1 d PDU C 2 C51' C 0.0635(12) 0.3738(6) 0.9771(6) 0.078(4) Uiso 0.320(7) 1 d PDU C 2 H51C H 0.0803 0.3360 0.9553 0.094 Uiso 0.320(7) 1 calc PR C 2 H51D H 0.0383 0.3620 1.0152 0.094 Uiso 0.320(7) 1 calc PR C 2 C52' C 0.1680(15) 0.4178(12) 0.9906(10) 0.167(9) Uiso 0.320(7) 1 d PDU C 2 H52C H 0.2425 0.3952 1.0026 0.201 Uiso 0.320(7) 1 calc PR C 2 H52D H 0.1619 0.4483 1.0231 0.201 Uiso 0.320(7) 1 calc PR C 2 C53' C 0.1535(15) 0.4485(11) 0.9263(10) 0.170(9) Uiso 0.320(7) 1 d PDU C 2 H53C H 0.2041 0.4853 0.9281 0.204 Uiso 0.320(7) 1 calc PR C 2 H53D H 0.1713 0.4191 0.8955 0.204 Uiso 0.320(7) 1 calc PR C 2 C54' C 0.0287(15) 0.4662(8) 0.9115(10) 0.127(7) Uiso 0.320(7) 1 d PDU C 2 H54C H 0.0146 0.5053 0.9319 0.152 Uiso 0.320(7) 1 calc PR C 2 H54D H -0.0024 0.4697 0.8663 0.152 Uiso 0.320(7) 1 calc PR C 2 O50" O 0.1814(18) 0.4078(14) 0.9764(13) 0.203(11) Uiso 0.248(7) 1 d PDU D 3 C51" C 0.130(2) 0.3960(15) 0.9095(11) 0.164(12) Uiso 0.248(7) 1 d PDU D 3 H51E H 0.1364 0.4321 0.8830 0.196 Uiso 0.248(7) 1 calc PR D 3 H51F H 0.1624 0.3588 0.8936 0.196 Uiso 0.248(7) 1 calc PR D 3 C52" C 0.009(2) 0.3864(12) 0.9178(11) 0.147(10) Uiso 0.248(7) 1 d PDU D 3 H52E H -0.0002 0.3439 0.9326 0.177 Uiso 0.248(7) 1 calc PR D 3 H52F H -0.0475 0.3925 0.8780 0.177 Uiso 0.248(7) 1 calc PR D 3 C53" C -0.011(2) 0.4334(13) 0.9650(12) 0.161(10) Uiso 0.248(7) 1 d PDU D 3 H53E H -0.0533 0.4144 0.9944 0.194 Uiso 0.248(7) 1 calc PR D 3 H53F H -0.0576 0.4687 0.9444 0.194 Uiso 0.248(7) 1 calc PR D 3 C54" C 0.109(3) 0.4549(15) 0.9986(14) 0.234(19) Uiso 0.248(7) 1 d PD D 3 H54E H 0.1270 0.4971 0.9860 0.280 Uiso 0.248(7) 1 calc PR D 3 H54F H 0.1189 0.4534 1.0441 0.280 Uiso 0.248(7) 1 calc PR D 3 O60 O 0.4445(8) 0.6404(3) 0.9179(3) 0.070(2) Uiso 0.404(4) 1 d PDU E 1 C61 C 0.5273(8) 0.6083(6) 0.9644(6) 0.085(4) Uiso 0.404(4) 1 d PDU E 1 H61A H 0.5970 0.6337 0.9809 0.103 Uiso 0.404(4) 1 calc PR E 1 H61B H 0.5509 0.5682 0.9492 0.103 Uiso 0.404(4) 1 calc PR E 1 C62 C 0.4517(12) 0.5999(8) 1.0112(5) 0.106(5) Uiso 0.404(4) 1 d PDU E 1 H62A H 0.4822 0.5663 1.0406 0.128 Uiso 0.404(4) 1 calc PR E 1 H62B H 0.4485 0.6385 1.0347 0.128 Uiso 0.404(4) 1 calc PR E 1 C63 C 0.3366(10) 0.5840(6) 0.9745(6) 0.080(3) Uiso 0.404(4) 1 d PDU E 1 H63A H 0.2750 0.5937 0.9971 0.096 Uiso 0.404(4) 1 calc PR E 1 H63B H 0.3319 0.5397 0.9630 0.096 Uiso 0.404(4) 1 calc PR E 1 C64 C 0.3273(8) 0.6259(4) 0.9170(4) 0.0465(19) Uiso 0.404(4) 1 d PDU E 1 H64A H 0.2908 0.6037 0.8787 0.056 Uiso 0.404(4) 1 calc PR E 1 H64B H 0.2818 0.6637 0.9205 0.056 Uiso 0.404(4) 1 calc PR E 1 O60' O 0.3783(10) 0.6437(5) 0.9266(5) 0.100(3) Uiso 0.367(7) 1 d PDU F 2 C61' C 0.4953(10) 0.6246(6) 0.9416(6) 0.066(3) Uiso 0.367(7) 1 d PDU F 2 H61C H 0.5491 0.6592 0.9392 0.079 Uiso 0.367(7) 1 calc PR F 2 H61D H 0.5103 0.5902 0.9149 0.079 Uiso 0.367(7) 1 calc PR F 2 C62' C 0.5032(9) 0.6044(7) 1.0056(5) 0.086(4) Uiso 0.367(7) 1 d PDU F 2 H62C H 0.5387 0.6373 1.0348 0.103 Uiso 0.367(7) 1 calc PR F 2 H62D H 0.5519 0.5668 1.0144 0.103 Uiso 0.367(7) 1 calc PR F 2 C63' C 0.3806(8) 0.5907(4) 1.0132(4) 0.051(2) Uiso 0.367(7) 1 d PDU F 2 H63C H 0.3764 0.5489 1.0308 0.061 Uiso 0.367(7) 1 calc PR F 2 H63D H 0.3562 0.6214 1.0410 0.061 Uiso 0.367(7) 1 calc PR F 2 C64' C 0.3044(10) 0.5947(9) 0.9496(7) 0.109(5) Uiso 0.367(7) 1 d PDU F 2 H64C H 0.2250 0.6094 0.9498 0.130 Uiso 0.367(7) 1 calc PR F 2 H64D H 0.3008 0.5553 0.9264 0.130 Uiso 0.367(7) 1 calc PR F 2 O60" O 0.2811(13) 0.6148(8) 0.9203(8) 0.116(6) Uiso 0.229(7) 1 d PDU G 3 C61" C 0.3891(15) 0.6342(8) 0.9041(6) 0.060(4) Uiso 0.229(7) 1 d PDU G 3 H61E H 0.3816 0.6750 0.8833 0.072 Uiso 0.229(7) 1 calc PR G 3 H61F H 0.4180 0.6033 0.8782 0.072 Uiso 0.229(7) 1 calc PR G 3 C62" C 0.4631(15) 0.6373(9) 0.9685(8) 0.091(6) Uiso 0.229(7) 1 d PDU G 3 H62E H 0.4427 0.6733 0.9917 0.109 Uiso 0.229(7) 1 calc PR G 3 H62F H 0.5469 0.6388 0.9682 0.109 Uiso 0.229(7) 1 calc PR G 3 C63" C 0.4289(15) 0.5745(9) 0.9954(9) 0.090(6) Uiso 0.229(7) 1 d PDU G 3 H63E H 0.4636 0.5388 0.9781 0.108 Uiso 0.229(7) 1 calc PR G 3 H63F H 0.4531 0.5736 1.0411 0.108 Uiso 0.229(7) 1 calc PR G 3 C64" C 0.2989(15) 0.5749(11) 0.9745(11) 0.105(8) Uiso 0.229(7) 1 d PDU G 3 H64E H 0.2684 0.5327 0.9635 0.127 Uiso 0.229(7) 1 calc PR G 3 H64F H 0.2616 0.5921 1.0067 0.127 Uiso 0.229(7) 1 calc PR G 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02001(12) 0.01386(12) 0.01804(12) -0.00035(10) 0.00525(10) 0.00190(10) Co2 0.01791(12) 0.01500(12) 0.02047(13) 0.00025(10) 0.00182(10) 0.00122(10) Co3 0.02381(13) 0.01951(14) 0.02241(14) 0.00372(11) 0.01058(11) 0.00173(11) I1 0.02250(6) 0.02561(7) 0.02432(7) 0.00283(5) 0.01011(5) -0.00189(5) I2 0.02099(6) 0.02517(7) 0.03219(7) 0.00166(6) 0.00876(5) -0.00252(5) I3 0.03677(8) 0.02580(7) 0.02543(7) -0.00161(6) 0.01315(6) 0.00359(6) I4 0.05476(15) 0.02706(16) 0.0321(2) 0.01294(13) 0.01582(16) 0.00588(14) O1 0.0165(6) 0.0161(6) 0.0203(6) 0.0026(5) 0.0071(5) 0.0036(5) C1 0.0201(9) 0.0166(9) 0.0223(9) 0.0066(7) 0.0095(8) 0.0053(7) C2 0.0253(10) 0.0203(10) 0.0218(10) 0.0045(8) 0.0089(8) 0.0056(8) C3 0.0318(11) 0.0146(9) 0.0278(11) 0.0021(8) 0.0107(9) 0.0044(8) N4 0.0246(9) 0.0168(8) 0.0206(8) -0.0006(6) 0.0079(7) 0.0006(7) C5 0.0320(11) 0.0178(10) 0.0292(11) -0.0041(8) 0.0087(9) -0.0012(8) C6 0.0294(11) 0.0212(10) 0.0230(10) -0.0081(8) 0.0064(9) -0.0025(8) C7 0.0271(10) 0.0246(11) 0.0229(10) -0.0076(8) 0.0027(8) -0.0022(8) N8 0.0205(8) 0.0168(8) 0.0202(8) -0.0015(6) 0.0062(7) -0.0005(6) C9 0.0202(9) 0.0223(10) 0.0225(10) -0.0010(8) 0.0010(8) 0.0023(8) C10 0.0190(9) 0.0189(9) 0.0214(9) -0.0005(7) 0.0062(8) 0.0015(7) C11 0.0145(8) 0.0177(9) 0.0181(9) 0.0019(7) 0.0055(7) 0.0024(7) O11 0.0181(6) 0.0135(6) 0.0180(6) 0.0009(5) 0.0041(5) 0.0026(5) C12 0.0165(9) 0.0180(9) 0.0216(9) 0.0014(7) 0.0055(7) 0.0033(7) C13 0.0216(9) 0.0183(9) 0.0226(10) -0.0015(8) 0.0046(8) 0.0046(8) N14 0.0200(8) 0.0185(8) 0.0189(8) -0.0002(6) 0.0026(7) 0.0008(6) C15 0.0281(11) 0.0216(10) 0.0245(10) -0.0050(8) 0.0004(9) -0.0002(8) C16 0.0263(11) 0.0202(10) 0.0320(11) -0.0042(9) -0.0030(9) -0.0043(8) C17 0.0281(11) 0.0266(12) 0.0273(11) -0.0037(9) -0.0045(9) -0.0008(9) N18 0.0206(8) 0.0195(8) 0.0237(9) 0.0011(7) 0.0032(7) 0.0016(6) C19 0.0226(10) 0.0235(11) 0.0244(10) 0.0036(8) -0.0015(8) 0.0041(8) C20 0.0223(10) 0.0201(10) 0.0255(10) 0.0055(8) 0.0064(8) 0.0039(8) C21 0.0207(10) 0.0309(12) 0.0318(11) 0.0084(9) 0.0070(9) 0.0080(9) C22 0.0286(11) 0.0304(12) 0.0288(11) 0.0128(9) 0.0114(9) 0.0157(9) C23 0.0345(12) 0.0221(11) 0.0276(11) 0.0040(8) 0.0150(10) 0.0116(9) C24 0.0340(12) 0.0414(14) 0.0327(12) 0.0133(11) 0.0120(10) 0.0231(11) C25 0.0261(16) 0.050(2) 0.048(2) 0.0026(17) -0.0012(14) 0.0177(15) C26 0.0275(15) 0.044(2) 0.0463(19) 0.0082(16) 0.0138(14) 0.0137(14) C27 0.0414(19) 0.0339(19) 0.083(3) 0.035(2) 0.028(2) 0.0222(16) C28 0.0304(11) 0.0307(12) 0.0229(10) -0.0065(9) 0.0110(9) -0.0022(9) C29 0.0388(13) 0.0288(12) 0.0372(13) -0.0158(10) 0.0066(11) -0.0052(10) C30 0.0218(10) 0.0248(11) 0.0199(9) 0.0031(8) 0.0013(8) 0.0040(8) C31 0.0200(9) 0.0198(10) 0.0254(10) 0.0042(8) 0.0057(8) 0.0050(8) C32 0.0211(9) 0.0175(10) 0.0302(11) 0.0012(8) 0.0088(8) 0.0027(7) C33 0.0297(11) 0.0226(11) 0.0304(12) 0.0090(9) 0.0030(9) 0.0067(9) C34 0.0660(19) 0.0468(17) 0.0397(15) 0.0214(13) 0.0205(14) 0.0160(14) C35 0.0317(14) 0.0438(17) 0.072(2) 0.0190(15) -0.0061(13) 0.0081(12) C36 0.0582(17) 0.0214(12) 0.0503(16) 0.0077(11) 0.0005(14) 0.0105(12) C37 0.0273(12) 0.0324(13) 0.0507(15) -0.0002(11) 0.0090(11) -0.0086(10) C38 0.0456(15) 0.0303(14) 0.0473(15) -0.0086(12) -0.0140(12) -0.0067(11) O40 0.0359(10) 0.0601(13) 0.0514(12) -0.0003(10) 0.0201(9) 0.0004(9) C41 0.0438(17) 0.071(2) 0.080(2) -0.0138(19) 0.0169(17) -0.0023(16) C42 0.088(3) 0.0382(18) 0.110(3) -0.0015(18) 0.063(2) -0.0093(17) C43 0.0472(17) 0.069(2) 0.0559(18) 0.0209(16) 0.0246(15) 0.0209(15) C44 0.0281(12) 0.0442(15) 0.0515(16) 0.0036(13) 0.0122(12) 0.0076(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O11 2.0494(13) . ? Co1 N8 2.0925(17) . ? Co1 N4 2.1114(16) . ? Co1 O1 2.1945(13) . ? Co1 I1 2.8916(3) . ? Co1 I2 2.9333(3) . ? Co1 Co2 2.9822(4) . ? Co2 O11 2.0497(13) . ? Co2 N18 2.1072(17) . ? Co2 N14 2.1080(17) . ? Co2 O1 2.1773(13) . ? Co2 I1 2.9774(3) . ? Co2 I3 2.9944(3) . ? Co3 O1 2.0049(12) . ? Co3 I4 2.5429(3) . ? Co3 I4' 2.575(8) . ? Co3 I3 2.5996(3) . ? Co3 I2 2.6046(3) . ? O1 C1 1.394(2) . ? C1 C20 1.392(3) . ? C1 C2 1.393(3) . ? C2 C23 1.387(3) . ? C2 C3 1.492(3) . ? C3 N4 1.490(3) . ? N4 C5 1.478(3) . ? C5 C6 1.526(3) . ? C6 C28 1.529(3) . ? C6 C7 1.530(3) . ? C6 C29 1.532(3) . ? C7 N8 1.481(3) . ? N8 C9 1.490(2) . ? C9 C10 1.496(3) . ? C10 C30 1.388(3) . ? C10 C11 1.405(3) . ? C11 O11 1.360(2) . ? C11 C12 1.402(3) . ? C12 C32 1.396(3) . ? C12 C13 1.492(3) . ? C13 N14 1.488(2) . ? N14 C15 1.477(3) . ? C15 C16 1.528(3) . ? C16 C37 1.530(3) . ? C16 C17 1.531(3) . ? C16 C38 1.537(3) . ? C17 N18 1.490(3) . ? N18 C19 1.493(3) . ? C19 C20 1.499(3) . ? C20 C21 1.396(3) . ? C21 C22 1.377(3) . ? C22 C23 1.394(3) . ? C22 C24 1.536(3) . ? C24 C25' 1.347(8) . ? C24 C27 1.463(4) . ? C24 C26 1.525(4) . ? C24 C27' 1.543(8) . ? C24 C25 1.598(4) . ? C24 C26' 1.694(9) . ? C30 C31 1.391(3) . ? C31 C32 1.381(3) . ? C31 C33 1.526(3) . ? C33 C35 1.524(3) . ? C33 C36 1.526(3) . ? C33 C34 1.548(3) . ? O40 C41 1.419(4) . ? O40 C44 1.425(3) . ? C41 C42 1.490(5) . ? C42 C43 1.535(5) . ? C43 C44 1.496(4) . ? O50 C54 1.438(11) . ? O50 C51 1.452(12) . ? C51 C52 1.554(12) . ? C52 C53 1.467(12) . ? C53 C54 1.454(12) . ? O50' C51' 1.420(12) . ? O50' C54' 1.484(13) . ? C51' C52' 1.534(14) . ? C52' C53' 1.548(14) . ? C53' C54' 1.486(14) . ? O50" C54" 1.477(16) . ? O50" C51" 1.497(15) . ? C51" C52" 1.490(14) . ? C52" C53" 1.517(15) . ? C53" C54" 1.53(3) . ? O60 C64 1.413(10) . ? O60 C61 1.435(10) . ? C61 C62 1.519(12) . ? C62 C63 1.462(12) . ? C63 C64 1.548(11) . ? O60' C61' 1.409(12) . ? O60' C64' 1.528(12) . ? C61' C62' 1.468(11) . ? C62' C63' 1.520(11) . ? C63' C64' 1.500(12) . ? O60" C64" 1.456(14) . ? O60" C61" 1.458(13) . ? C61" C62" 1.503(14) . ? C62" C63" 1.571(13) . ? C63" C64" 1.501(14) . ? 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 O11 Co1 N8 94.30(6) . . ? O11 Co1 N4 172.29(6) . . ? N8 Co1 N4 93.25(6) . . ? O11 Co1 O1 82.76(5) . . ? N8 Co1 O1 176.93(6) . . ? N4 Co1 O1 89.67(6) . . ? O11 Co1 I1 82.58(4) . . ? N8 Co1 I1 95.56(4) . . ? N4 Co1 I1 95.12(5) . . ? O1 Co1 I1 83.23(3) . . ? O11 Co1 I2 88.58(4) . . ? N8 Co1 I2 96.35(4) . . ? N4 Co1 I2 92.15(4) . . ? O1 Co1 I2 84.46(3) . . ? I1 Co1 I2 165.654(11) . . ? O11 Co1 Co2 43.32(4) . . ? N8 Co1 Co2 130.24(5) . . ? N4 Co1 Co2 129.31(5) . . ? O1 Co1 Co2 46.75(4) . . ? I1 Co1 Co2 60.891(8) . . ? I2 Co1 Co2 105.069(9) . . ? O11 Co2 N18 172.27(6) . . ? O11 Co2 N14 92.53(6) . . ? N18 Co2 N14 93.94(7) . . ? O11 Co2 O1 83.18(5) . . ? N18 Co2 O1 90.56(6) . . ? N14 Co2 O1 174.83(6) . . ? O11 Co2 I1 80.40(3) . . ? N18 Co2 I1 94.21(5) . . ? N14 Co2 I1 100.71(4) . . ? O1 Co2 I1 81.47(3) . . ? O11 Co2 Co1 43.32(4) . . ? N18 Co2 Co1 128.99(5) . . ? N14 Co2 Co1 130.15(5) . . ? O1 Co2 Co1 47.23(4) . . ? I1 Co2 Co1 58.051(7) . . ? O11 Co2 I3 88.65(3) . . ? N18 Co2 I3 95.05(5) . . ? N14 Co2 I3 94.63(4) . . ? O1 Co2 I3 82.42(3) . . ? I1 Co2 I3 161.460(11) . . ? Co1 Co2 I3 103.910(10) . . ? O1 Co3 I4 111.99(4) . . ? O1 Co3 I4' 110.84(18) . . ? O1 Co3 I3 96.66(4) . . ? I4 Co3 I3 116.26(2) . . ? I4' Co3 I3 105.9(4) . . ? O1 Co3 I2 97.56(4) . . ? I4 Co3 I2 112.86(2) . . ? I4' Co3 I2 123.7(4) . . ? I3 Co3 I2 118.217(11) . . ? Co1 I1 Co2 61.058(8) . . ? Co3 I2 Co1 72.646(8) . . ? Co3 I3 Co2 72.525(8) . . ? C1 O1 Co3 115.52(10) . . ? C1 O1 Co2 121.15(11) . . ? Co3 O1 Co2 105.20(5) . . ? C1 O1 Co1 121.03(11) . . ? Co3 O1 Co1 103.11(6) . . ? Co2 O1 Co1 86.02(5) . . ? C20 C1 C2 119.48(18) . . ? C20 C1 O1 120.23(17) . . ? C2 C1 O1 120.24(18) . . ? C23 C2 C1 119.0(2) . . ? C23 C2 C3 119.43(19) . . ? C1 C2 C3 121.46(18) . . ? N4 C3 C2 114.09(17) . . ? C5 N4 C3 108.28(16) . . ? C5 N4 Co1 116.89(13) . . ? C3 N4 Co1 112.85(12) . . ? N4 C5 C6 116.21(17) . . ? C5 C6 C28 111.09(18) . . ? C5 C6 C7 111.78(16) . . ? C28 C6 C7 111.82(18) . . ? C5 C6 C29 106.46(18) . . ? C28 C6 C29 109.80(17) . . ? C7 C6 C29 105.59(18) . . ? N8 C7 C6 116.22(17) . . ? C7 N8 C9 106.94(15) . . ? C7 N8 Co1 118.34(13) . . ? C9 N8 Co1 108.91(12) . . ? N8 C9 C10 114.39(16) . . ? C30 C10 C11 119.73(18) . . ? C30 C10 C9 117.94(18) . . ? C11 C10 C9 121.99(18) . . ? O11 C11 C12 121.02(17) . . ? O11 C11 C10 121.44(17) . . ? C12 C11 C10 117.51(17) . . ? C11 O11 Co1 123.98(11) . . ? C11 O11 Co2 123.42(11) . . ? Co1 O11 Co2 93.36(5) . . ? C32 C12 C11 120.47(18) . . ? C32 C12 C13 118.07(18) . . ? C11 C12 C13 121.39(17) . . ? N14 C13 C12 111.88(15) . . ? C15 N14 C13 109.25(15) . . ? C15 N14 Co2 117.37(13) . . ? C13 N14 Co2 108.77(12) . . ? N14 C15 C16 114.14(17) . . ? C15 C16 C37 111.23(19) . . ? C15 C16 C17 111.22(18) . . ? C37 C16 C17 111.24(19) . . ? C15 C16 C38 106.28(19) . . ? C37 C16 C38 110.0(2) . . ? C17 C16 C38 106.64(19) . . ? N18 C17 C16 115.54(17) . . ? C17 N18 C19 107.40(16) . . ? C17 N18 Co2 118.19(13) . . ? C19 N18 Co2 111.49(12) . . ? N18 C19 C20 113.20(16) . . ? C1 C20 C21 119.28(19) . . ? C1 C20 C19 121.96(17) . . ? C21 C20 C19 118.67(19) . . ? C22 C21 C20 122.9(2) . . ? C21 C22 C23 116.15(19) . . ? C21 C22 C24 122.6(2) . . ? C23 C22 C24 121.2(2) . . ? C2 C23 C22 123.2(2) . . ? C27 C24 C26 113.0(3) . . ? C25' C24 C22 112.4(5) . . ? C27 C24 C22 111.2(2) . . ? C26 C24 C22 110.0(2) . . ? C25' C24 C27' 120.9(6) . . ? C22 C24 C27' 107.2(4) . . ? C27 C24 C25 107.5(3) . . ? C26 C24 C25 103.9(2) . . ? C22 C24 C25 111.0(2) . . ? C25' C24 C26' 108.4(5) . . ? C22 C24 C26' 107.7(4) . . ? C27' C24 C26' 98.8(5) . . ? C10 C30 C31 123.61(19) . . ? C32 C31 C30 115.74(18) . . ? C32 C31 C33 123.64(19) . . ? C30 C31 C33 120.62(19) . . ? C31 C32 C12 122.77(19) . . ? C35 C33 C36 108.6(2) . . ? C35 C33 C31 110.21(19) . . ? C36 C33 C31 112.46(19) . . ? C35 C33 C34 109.2(2) . . ? C36 C33 C34 107.8(2) . . ? C31 C33 C34 108.49(18) . . ? C41 O40 C44 104.6(2) . . ? O40 C41 C42 108.4(3) . . ? C41 C42 C43 103.6(2) . . ? C44 C43 C42 102.6(3) . . ? O40 C44 C43 104.5(2) . . ? C54 O50 C51 115.7(8) . . ? O50 C51 C52 101.5(7) . . ? C53 C52 C51 106.3(7) . . ? C54 C53 C52 111.7(8) . . ? O50 C54 C53 102.8(7) . . ? C51' O50' C54' 115.3(8) . . ? O50' C51' C52' 100.2(8) . . ? C51' C52' C53' 99.4(10) . . ? C54' C53' C52' 102.7(10) . . ? O50' C54' C53' 99.0(9) . . ? C54" O50" C51" 108.0(14) . . ? C52" C51" O50" 95.5(11) . . ? C51" C52" C53" 106.9(11) . . ? C52" C53" C54" 105.6(9) . . ? O50" C54" C53" 99.8(11) . . ? C64 O60 C61 114.3(6) . . ? O60 C61 C62 98.0(7) . . ? C63 C62 C61 105.1(8) . . ? C62 C63 C64 102.1(7) . . ? O60 C64 C63 103.0(6) . . ? C61' O60' C64' 108.6(9) . . ? O60' C61' C62' 99.6(7) . . ? C61' C62' C63' 107.7(7) . . ? C64' C63' C62' 105.9(7) . . ? C63' C64' O60' 94.8(7) . . ? C64" O60" C61" 113.4(10) . . ? O60" C61" C62" 97.9(9) . . ? C61" C62" C63" 100.3(10) . . ? C64" C63" C62" 102.0(9) . . ? O60" C64" C63" 102.2(8) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.796 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.084 #===END data_1b _database_code_depnum_ccdc_archive 'CCDC 825191' #TrackingRef '- kember et al_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H54 Br4 Co3 N4 O2, 3(C4 H8 O)' _chemical_formula_sum 'C46 H78 Br4 Co3 N4 O5' _chemical_formula_weight 1263.55 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.69346(15) _cell_length_b 20.8757(3) _cell_length_c 22.0206(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.0342(12) _cell_angle_gamma 90.00 _cell_volume 5257.30(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21167 _cell_measurement_theta_min 2.9944 _cell_measurement_theta_max 32.6221 _exptl_crystal_description blocks _exptl_crystal_colour Teal _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2572 _exptl_absorpt_coefficient_mu 4.021 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.288 _exptl_absorpt_correction_T_max 0.414 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57484 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 32.70 _reflns_number_total 17821 _reflns_number_gt 10690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17821 _refine_ls_number_parameters 624 _refine_ls_number_restraints 561 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.40535(3) 0.409327(13) 0.611817(13) 0.01815(7) Uani 1 1 d . . . Co2 Co 0.52250(3) 0.491844(14) 0.714860(14) 0.01950(7) Uani 1 1 d . . . Co3 Co 0.37908(3) 0.367610(14) 0.750798(14) 0.02314(7) Uani 1 1 d . . . Br1 Br 0.59823(2) 0.474790(11) 0.604537(11) 0.02581(6) Uani 1 1 d . . . Br2 Br 0.22883(2) 0.352804(11) 0.657467(11) 0.02727(6) Uani 1 1 d . . . Br3 Br 0.39707(2) 0.468141(11) 0.807081(11) 0.02802(6) Uani 1 1 d . . . Br4 Br 0.42929(3) 0.275478(13) 0.812036(12) 0.04323(8) Uani 1 1 d . . . O1 O 0.50601(12) 0.38941(7) 0.70513(6) 0.0171(3) Uani 1 1 d . . . C1 C 0.60257(19) 0.34936(10) 0.71425(10) 0.0187(5) Uani 1 1 d . . . C2 C 0.6010(2) 0.29412(10) 0.67872(10) 0.0214(5) Uani 1 1 d . . . C3 C 0.4928(2) 0.27397(10) 0.63329(10) 0.0237(5) Uani 1 1 d . . . H3A H 0.5065 0.2316 0.6160 0.028 Uiso 1 1 calc R . . H3B H 0.4279 0.2693 0.6555 0.028 Uiso 1 1 calc R . . N4 N 0.45755(16) 0.32033(9) 0.58126(8) 0.0198(4) Uani 1 1 d D . . H4 H 0.5210(11) 0.3264(10) 0.5648(9) 0.019(6) Uiso 1 1 d D . . C5 C 0.3742(2) 0.28762(10) 0.53115(10) 0.0241(5) Uani 1 1 d . . . H5A H 0.3045 0.2752 0.5474 0.029 Uiso 1 1 calc R . . H5B H 0.4111 0.2477 0.5203 0.029 Uiso 1 1 calc R . . C6 C 0.33382(19) 0.32631(11) 0.47224(10) 0.0224(5) Uani 1 1 d . . . C7 C 0.2530(2) 0.38105(11) 0.48236(10) 0.0255(5) Uani 1 1 d . . . H7A H 0.2180 0.3997 0.4414 0.031 Uiso 1 1 calc R . . H7B H 0.1883 0.3628 0.4996 0.031 Uiso 1 1 calc R . . N8 N 0.30715(16) 0.43352(8) 0.52378(8) 0.0198(4) Uani 1 1 d D . . H8 H 0.3508(16) 0.4549(9) 0.5013(8) 0.023(6) Uiso 1 1 d D . . C9 C 0.2108(2) 0.47697(10) 0.53217(11) 0.0256(5) Uani 1 1 d . . . H9A H 0.1639 0.4551 0.5586 0.031 Uiso 1 1 calc R . . H9B H 0.1591 0.4846 0.4911 0.031 Uiso 1 1 calc R . . C10 C 0.2503(2) 0.54022(11) 0.56086(10) 0.0229(5) Uani 1 1 d . . . C11 C 0.31971(19) 0.54489(10) 0.62104(10) 0.0194(5) Uani 1 1 d . . . O11 O 0.36557(12) 0.49224(7) 0.65255(7) 0.0189(3) Uani 1 1 d . . . C12 C 0.33564(19) 0.60607(10) 0.64799(10) 0.0204(5) Uani 1 1 d . . . C13 C 0.39633(19) 0.61434(11) 0.71397(10) 0.0230(5) Uani 1 1 d . . . H13A H 0.3544 0.5897 0.7410 0.028 Uiso 1 1 calc R . . H13B H 0.3945 0.6601 0.7255 0.028 Uiso 1 1 calc R . . N14 N 0.52024(16) 0.59219(9) 0.72456(8) 0.0203(4) Uani 1 1 d D . . H14 H 0.5459(18) 0.6066(10) 0.6913(6) 0.025(7) Uiso 1 1 d D . . C15 C 0.5865(2) 0.61929(11) 0.78304(10) 0.0252(5) Uani 1 1 d . . . H15A H 0.5494 0.6053 0.8174 0.030 Uiso 1 1 calc R . . H15B H 0.5813 0.6666 0.7806 0.030 Uiso 1 1 calc R . . C16 C 0.7156(2) 0.60003(11) 0.79852(11) 0.0278(5) Uani 1 1 d . . . C17 C 0.7291(2) 0.53080(11) 0.82142(11) 0.0292(6) Uani 1 1 d . . . H17A H 0.8125 0.5230 0.8401 0.035 Uiso 1 1 calc R . . H17B H 0.6844 0.5254 0.8546 0.035 Uiso 1 1 calc R . . N18 N 0.68930(16) 0.48130(9) 0.77287(9) 0.0221(4) Uani 1 1 d D . . H18 H 0.7398(13) 0.4822(10) 0.7472(7) 0.014(6) Uiso 1 1 d D . . C19 C 0.7015(2) 0.41751(10) 0.80459(10) 0.0244(5) Uani 1 1 d . . . H19A H 0.6365 0.4119 0.8266 0.029 Uiso 1 1 calc R . . H19B H 0.7757 0.4167 0.8360 0.029 Uiso 1 1 calc R . . C20 C 0.70076(19) 0.36267(10) 0.76027(10) 0.0217(5) Uani 1 1 d . . . C21 C 0.7974(2) 0.32228(11) 0.76778(11) 0.0255(5) Uani 1 1 d . . . H21A H 0.8643 0.3322 0.7989 0.031 Uiso 1 1 calc R . . C22 C 0.7996(2) 0.26855(11) 0.73184(11) 0.0262(5) Uani 1 1 d . A . C23 C 0.6991(2) 0.25490(11) 0.68827(10) 0.0251(5) Uani 1 1 d . . . H23A H 0.6971 0.2172 0.6639 0.030 Uiso 1 1 calc R . . C24 C 0.9100(2) 0.22623(12) 0.74015(12) 0.0321(6) Uani 1 1 d D . . C25 C 1.0062(2) 0.26442(15) 0.72005(16) 0.0490(9) Uani 0.947(3) 1 d PDU A 1 H25A H 1.0255 0.3019 0.7470 0.074 Uiso 0.947(3) 1 calc PR A 1 H25B H 0.9795 0.2785 0.6770 0.074 Uiso 0.947(3) 1 calc PR A 1 H25C H 1.0759 0.2375 0.7232 0.074 Uiso 0.947(3) 1 calc PR A 1 C26 C 0.8881(2) 0.16550(13) 0.69946(14) 0.0426(8) Uani 0.947(3) 1 d PDU A 1 H26A H 0.8217 0.1418 0.7090 0.064 Uiso 0.947(3) 1 calc PR A 1 H26B H 0.9580 0.1383 0.7080 0.064 Uiso 0.947(3) 1 calc PR A 1 H26C H 0.8707 0.1778 0.6555 0.064 Uiso 0.947(3) 1 calc PR A 1 C27 C 0.9480(2) 0.20510(14) 0.80724(12) 0.0398(8) Uani 0.947(3) 1 d PDU A 1 H27A H 0.9562 0.2427 0.8344 0.060 Uiso 0.947(3) 1 calc PR A 1 H27B H 1.0232 0.1828 0.8128 0.060 Uiso 0.947(3) 1 calc PR A 1 H27C H 0.8891 0.1762 0.8178 0.060 Uiso 0.947(3) 1 calc PR A 1 C25' C 0.954(4) 0.224(2) 0.6788(11) 0.038(7) Uiso 0.053(3) 1 d PDU A 2 H25D H 1.0027 0.2617 0.6761 0.057 Uiso 0.053(3) 1 calc PR A 2 H25E H 0.8869 0.2239 0.6436 0.057 Uiso 0.053(3) 1 calc PR A 2 H25F H 1.0002 0.1851 0.6776 0.057 Uiso 0.053(3) 1 calc PR A 2 C26' C 0.910(5) 0.1605(11) 0.7670(18) 0.056(8) Uiso 0.053(3) 1 d PDU A 2 H26D H 0.8817 0.1627 0.8059 0.084 Uiso 0.053(3) 1 calc PR A 2 H26E H 0.9892 0.1431 0.7752 0.084 Uiso 0.053(3) 1 calc PR A 2 H26F H 0.8578 0.1328 0.7375 0.084 Uiso 0.053(3) 1 calc PR A 2 C27' C 1.005(4) 0.266(2) 0.7856(15) 0.051(8) Uiso 0.053(3) 1 d PDU A 2 H27D H 0.9764 0.3101 0.7890 0.076 Uiso 0.053(3) 1 calc PR A 2 H27E H 1.0772 0.2680 0.7693 0.076 Uiso 0.053(3) 1 calc PR A 2 H27F H 1.0218 0.2463 0.8266 0.076 Uiso 0.053(3) 1 calc PR A 2 C28 C 0.4377(2) 0.35058(12) 0.44678(11) 0.0304(6) Uani 1 1 d . . . H28A H 0.4092 0.3721 0.4069 0.046 Uiso 1 1 calc R . . H28B H 0.4875 0.3143 0.4408 0.046 Uiso 1 1 calc R . . H28C H 0.4830 0.3809 0.4763 0.046 Uiso 1 1 calc R . . C29 C 0.2587(2) 0.28167(12) 0.42501(11) 0.0333(6) Uani 1 1 d . . . H29A H 0.2296 0.3051 0.3863 0.050 Uiso 1 1 calc R . . H29B H 0.1924 0.2661 0.4417 0.050 Uiso 1 1 calc R . . H29C H 0.3060 0.2452 0.4167 0.050 Uiso 1 1 calc R . . C30 C 0.2078(2) 0.59590(11) 0.52843(10) 0.0256(5) Uani 1 1 d . . . H30A H 0.1630 0.5918 0.4873 0.031 Uiso 1 1 calc R . . C31 C 0.2280(2) 0.65654(11) 0.55355(11) 0.0238(5) Uani 1 1 d . . . C32 C 0.29105(19) 0.66030(11) 0.61393(10) 0.0230(5) Uani 1 1 d . . . H32A H 0.3046 0.7012 0.6330 0.028 Uiso 1 1 calc R . . C33 C 0.1808(2) 0.71543(11) 0.51459(11) 0.0306(6) Uani 1 1 d . . . C34 C 0.2420(3) 0.72058(14) 0.46016(13) 0.0517(8) Uani 1 1 d . . . H34A H 0.3263 0.7259 0.4759 0.078 Uiso 1 1 calc R . . H34B H 0.2115 0.7577 0.4346 0.078 Uiso 1 1 calc R . . H34C H 0.2277 0.6815 0.4350 0.078 Uiso 1 1 calc R . . C35 C 0.0491(2) 0.70935(14) 0.49109(15) 0.0533(9) Uani 1 1 d . . . H35A H 0.0101 0.7098 0.5264 0.080 Uiso 1 1 calc R . . H35B H 0.0316 0.6690 0.4683 0.080 Uiso 1 1 calc R . . H35C H 0.0208 0.7454 0.4635 0.080 Uiso 1 1 calc R . . C36 C 0.2040(3) 0.77708(12) 0.55289(13) 0.0463(8) Uani 1 1 d . . . H36A H 0.2884 0.7826 0.5678 0.070 Uiso 1 1 calc R . . H36B H 0.1659 0.7744 0.5885 0.070 Uiso 1 1 calc R . . H36C H 0.1725 0.8137 0.5269 0.070 Uiso 1 1 calc R . . C37 C 0.7724(2) 0.61073(12) 0.74269(12) 0.0349(6) Uani 1 1 d . . . H37A H 0.7361 0.5823 0.7087 0.052 Uiso 1 1 calc R . . H37B H 0.8562 0.6014 0.7546 0.052 Uiso 1 1 calc R . . H37C H 0.7613 0.6554 0.7290 0.052 Uiso 1 1 calc R . . C38 C 0.7746(2) 0.64277(12) 0.85296(12) 0.0422(7) Uani 1 1 d . . . H38A H 0.7358 0.6368 0.8880 0.063 Uiso 1 1 calc R . . H38B H 0.7683 0.6877 0.8399 0.063 Uiso 1 1 calc R . . H38C H 0.8572 0.6310 0.8657 0.063 Uiso 1 1 calc R . . O40 O 0.92796(19) 0.46241(11) 0.73460(11) 0.0607(6) Uani 1 1 d . . . C41 C 1.0431(3) 0.48434(16) 0.75116(15) 0.0566(9) Uani 1 1 d . . . H41A H 1.0961 0.4486 0.7677 0.068 Uiso 1 1 calc R . . H41B H 1.0496 0.5177 0.7837 0.068 Uiso 1 1 calc R . . C42 C 1.0756(3) 0.51148(15) 0.69441(17) 0.0652(10) Uani 1 1 d . . . H42A H 1.1520 0.4946 0.6890 0.078 Uiso 1 1 calc R . . H42B H 1.0793 0.5588 0.6963 0.078 Uiso 1 1 calc R . . C43 C 0.9773(4) 0.4890(2) 0.64259(17) 0.0817(13) Uani 1 1 d . . . H43A H 0.9232 0.5246 0.6268 0.098 Uiso 1 1 calc R . . H43B H 1.0082 0.4707 0.6078 0.098 Uiso 1 1 calc R . . C44 C 0.9185(3) 0.4392(2) 0.67339(17) 0.0717(11) Uani 1 1 d . . . H44A H 0.8355 0.4344 0.6522 0.086 Uiso 1 1 calc R . . H44B H 0.9582 0.3973 0.6735 0.086 Uiso 1 1 calc R . . O50 O 0.0267(10) 0.4306(7) 0.8904(4) 0.127(3) Uiso 0.351(3) 1 d PDU B 1 C51 C 0.0003(17) 0.4591(8) 0.9449(7) 0.132(4) Uiso 0.351(3) 1 d PDU B 1 H51A H -0.0853 0.4624 0.9411 0.158 Uiso 0.351(3) 1 calc PR B 1 H51B H 0.0347 0.5025 0.9514 0.158 Uiso 0.351(3) 1 calc PR B 1 C52 C 0.0524(18) 0.4160(9) 0.9971(5) 0.119(4) Uiso 0.351(3) 1 d PDU B 1 H52A H 0.1097 0.4398 1.0286 0.143 Uiso 0.351(3) 1 calc PR B 1 H52B H -0.0093 0.3989 1.0173 0.143 Uiso 0.351(3) 1 calc PR B 1 C53 C 0.1098(18) 0.3640(7) 0.9709(6) 0.132(3) Uiso 0.351(3) 1 d PDU B 1 H53A H 0.0702 0.3229 0.9754 0.158 Uiso 0.351(3) 1 calc PR B 1 H53B H 0.1924 0.3605 0.9931 0.158 Uiso 0.351(3) 1 calc PR B 1 C54 C 0.1037(18) 0.3786(8) 0.9017(6) 0.124(3) Uiso 0.351(3) 1 d PDU B 1 H54A H 0.1816 0.3903 0.8940 0.149 Uiso 0.351(3) 1 calc PR B 1 H54B H 0.0729 0.3415 0.8753 0.149 Uiso 0.351(3) 1 calc PR B 1 O50' O -0.0124(15) 0.4142(9) 0.9280(11) 0.124(3) Uiso 0.204(5) 1 d PDU C 2 C51' C 0.061(2) 0.3916(14) 0.9867(11) 0.121(4) Uiso 0.204(5) 1 d PDU C 2 H51C H 0.0356 0.3489 0.9984 0.145 Uiso 0.204(5) 1 calc PR C 2 H51D H 0.0598 0.4221 1.0210 0.145 Uiso 0.204(5) 1 calc PR C 2 C52' C 0.180(2) 0.3888(15) 0.9702(15) 0.126(4) Uiso 0.204(5) 1 d PDU C 2 H52C H 0.1915 0.3472 0.9508 0.151 Uiso 0.204(5) 1 calc PR C 2 H52D H 0.2425 0.3950 1.0075 0.151 Uiso 0.204(5) 1 calc PR C 2 C53' C 0.1773(16) 0.4435(15) 0.9245(13) 0.134(4) Uiso 0.204(5) 1 d PDU C 2 H53C H 0.2338 0.4772 0.9424 0.161 Uiso 0.204(5) 1 calc PR C 2 H53D H 0.1973 0.4279 0.8855 0.161 Uiso 0.204(5) 1 calc PR C 2 C54' C 0.0549(16) 0.4692(11) 0.9122(14) 0.126(4) Uiso 0.204(5) 1 d PDU C 2 H54C H 0.0484 0.5066 0.9389 0.151 Uiso 0.204(5) 1 calc PR C 2 H54D H 0.0284 0.4816 0.8681 0.151 Uiso 0.204(5) 1 calc PR C 2 O50" O 0.1840(9) 0.4023(6) 0.9753(5) 0.150(3) Uiso 0.445(5) 1 d PDU D 3 C51" C 0.1578(9) 0.3988(7) 0.9059(5) 0.107(3) Uiso 0.445(5) 1 d PDU D 3 H51E H 0.2022 0.3641 0.8906 0.128 Uiso 0.445(5) 1 calc PR D 3 H51F H 0.1729 0.4400 0.8868 0.128 Uiso 0.445(5) 1 calc PR D 3 C52" C 0.0285(10) 0.3838(7) 0.8954(6) 0.129(3) Uiso 0.445(5) 1 d PDU D 3 H52E H 0.0158 0.3379 0.9032 0.155 Uiso 0.445(5) 1 calc PR D 3 H52F H -0.0111 0.3943 0.8523 0.155 Uiso 0.445(5) 1 calc PR D 3 C53" C -0.0175(10) 0.4256(6) 0.9414(6) 0.115(3) Uiso 0.445(5) 1 d PDU D 3 H53E H -0.0686 0.4010 0.9635 0.138 Uiso 0.445(5) 1 calc PR D 3 H53F H -0.0609 0.4630 0.9207 0.138 Uiso 0.445(5) 1 calc PR D 3 C54" C 0.1060(13) 0.4476(7) 0.9891(6) 0.138(3) Uiso 0.445(5) 1 d PDU D 3 H54E H 0.1291 0.4916 0.9799 0.165 Uiso 0.445(5) 1 calc PR D 3 H54F H 0.0992 0.4450 1.0331 0.165 Uiso 0.445(5) 1 calc PR D 3 O60 O 0.4132(10) 0.6025(4) 0.9284(3) 0.083(2) Uiso 0.468(4) 1 d PDU E 1 C61 C 0.5174(6) 0.6165(4) 0.9675(3) 0.0495(17) Uiso 0.468(4) 1 d PDU E 1 H61A H 0.5517 0.6562 0.9542 0.059 Uiso 0.468(4) 1 calc PR E 1 H61B H 0.5739 0.5810 0.9685 0.059 Uiso 0.468(4) 1 calc PR E 1 C62 C 0.4880(9) 0.6252(4) 1.0286(3) 0.063(2) Uiso 0.468(4) 1 d PDU E 1 H62A H 0.4620 0.6697 1.0335 0.076 Uiso 0.468(4) 1 calc PR E 1 H62B H 0.5565 0.6159 1.0622 0.076 Uiso 0.468(4) 1 calc PR E 1 C63 C 0.3914(10) 0.5789(5) 1.0301(4) 0.058(2) Uiso 0.468(4) 1 d PDU E 1 H63A H 0.3371 0.5956 1.0554 0.069 Uiso 0.468(4) 1 calc PR E 1 H63B H 0.4223 0.5369 1.0470 0.069 Uiso 0.468(4) 1 calc PR E 1 C64 C 0.3324(11) 0.5737(7) 0.9630(5) 0.085(3) Uiso 0.468(4) 1 d PDU E 1 H64A H 0.3173 0.5283 0.9510 0.102 Uiso 0.468(4) 1 calc PR E 1 H64B H 0.2570 0.5971 0.9549 0.102 Uiso 0.468(4) 1 calc PR E 1 O60' O 0.4595(15) 0.5905(6) 0.9310(5) 0.093(3) Uiso 0.239(9) 1 d PDU F 2 C61' C 0.4888(15) 0.6420(7) 0.9717(6) 0.042(3) Uiso 0.239(9) 1 d PDU F 2 H61C H 0.4224 0.6717 0.9703 0.051 Uiso 0.239(9) 1 calc PR F 2 H61D H 0.5576 0.6659 0.9640 0.051 Uiso 0.239(9) 1 calc PR F 2 C62' C 0.5161(16) 0.6044(8) 1.0309(6) 0.060(3) Uiso 0.239(9) 1 d PDU F 2 H62C H 0.5307 0.6326 1.0679 0.072 Uiso 0.239(9) 1 calc PR F 2 H62D H 0.5837 0.5755 1.0324 0.072 Uiso 0.239(9) 1 calc PR F 2 C63' C 0.401(2) 0.5673(11) 1.0245(8) 0.072(4) Uiso 0.239(9) 1 d PDU F 2 H63C H 0.4136 0.5259 1.0467 0.086 Uiso 0.239(9) 1 calc PR F 2 H63D H 0.3425 0.5925 1.0409 0.086 Uiso 0.239(9) 1 calc PR F 2 C64' C 0.3629(19) 0.5573(10) 0.9560(8) 0.092(4) Uiso 0.239(9) 1 d PDU F 2 H64C H 0.2859 0.5775 0.9397 0.111 Uiso 0.239(9) 1 calc PR F 2 H64D H 0.3585 0.5112 0.9454 0.111 Uiso 0.239(9) 1 calc PR F 2 O60" O 0.3014(13) 0.5677(7) 0.9546(6) 0.113(3) Uiso 0.293(9) 1 d PDU G 3 C61" C 0.3574(17) 0.6139(8) 0.9237(5) 0.095(3) Uiso 0.293(9) 1 d PDU G 3 H61E H 0.3025 0.6490 0.9077 0.114 Uiso 0.293(9) 1 calc PR G 3 H61F H 0.3839 0.5940 0.8883 0.114 Uiso 0.293(9) 1 calc PR G 3 C62" C 0.4589(11) 0.6392(6) 0.9693(6) 0.048(3) Uiso 0.293(9) 1 d PDU G 3 H62E H 0.4503 0.6858 0.9754 0.057 Uiso 0.293(9) 1 calc PR G 3 H62F H 0.5324 0.6316 0.9548 0.057 Uiso 0.293(9) 1 calc PR G 3 C63" C 0.4598(13) 0.6035(7) 1.0287(5) 0.059(3) Uiso 0.293(9) 1 d PDU G 3 H63E H 0.5287 0.5748 1.0386 0.070 Uiso 0.293(9) 1 calc PR G 3 H63F H 0.4629 0.6338 1.0635 0.070 Uiso 0.293(9) 1 calc PR G 3 C64" C 0.3501(14) 0.5655(7) 1.0184(6) 0.069(3) Uiso 0.293(9) 1 d PDU G 3 H64E H 0.3670 0.5207 1.0320 0.083 Uiso 0.293(9) 1 calc PR G 3 H64F H 0.2952 0.5840 1.0424 0.083 Uiso 0.293(9) 1 calc PR G 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02066(16) 0.01657(15) 0.01736(14) -0.00003(11) 0.00430(12) 0.00075(12) Co2 0.01962(16) 0.01767(16) 0.02054(15) -0.00017(12) 0.00265(13) -0.00087(12) Co3 0.02632(18) 0.02274(17) 0.02270(16) 0.00186(13) 0.01046(14) -0.00284(13) Br1 0.02569(12) 0.02826(13) 0.02571(12) 0.00265(9) 0.01046(10) -0.00496(10) Br2 0.02247(12) 0.03023(13) 0.03030(13) -0.00021(10) 0.00824(10) -0.00652(10) Br3 0.03524(14) 0.02826(13) 0.02322(12) -0.00226(10) 0.01223(10) 0.00022(10) Br4 0.0699(2) 0.02973(15) 0.03454(15) 0.01174(11) 0.02124(14) 0.00107(13) O1 0.0169(8) 0.0165(8) 0.0192(7) 0.0020(6) 0.0070(6) 0.0004(6) C1 0.0195(11) 0.0184(11) 0.0193(11) 0.0068(9) 0.0070(9) 0.0015(9) C2 0.0264(12) 0.0210(12) 0.0184(11) 0.0055(9) 0.0086(10) 0.0025(9) C3 0.0304(13) 0.0152(11) 0.0256(12) 0.0013(9) 0.0062(10) 0.0016(9) N4 0.0220(10) 0.0193(10) 0.0188(9) 0.0007(7) 0.0056(8) -0.0004(8) C5 0.0285(13) 0.0207(12) 0.0231(11) -0.0028(9) 0.0058(10) -0.0021(9) C6 0.0251(12) 0.0242(12) 0.0183(11) -0.0040(9) 0.0052(10) -0.0015(9) C7 0.0244(13) 0.0286(14) 0.0224(12) -0.0045(10) 0.0018(10) -0.0005(10) N8 0.0226(10) 0.0176(10) 0.0197(9) -0.0002(7) 0.0057(8) 0.0007(8) C9 0.0231(12) 0.0261(13) 0.0253(12) -0.0036(10) -0.0002(10) 0.0041(10) C10 0.0232(12) 0.0230(13) 0.0229(11) -0.0017(9) 0.0059(10) 0.0035(9) C11 0.0170(11) 0.0204(12) 0.0222(11) 0.0030(9) 0.0077(9) 0.0009(9) O11 0.0205(8) 0.0155(8) 0.0204(8) 0.0012(6) 0.0039(6) 0.0015(6) C12 0.0191(11) 0.0208(12) 0.0231(11) -0.0007(9) 0.0090(10) 0.0021(9) C13 0.0226(12) 0.0202(12) 0.0267(12) -0.0006(9) 0.0064(10) 0.0028(9) N14 0.0217(10) 0.0202(10) 0.0195(9) -0.0024(8) 0.0057(8) -0.0021(8) C15 0.0315(14) 0.0227(13) 0.0208(11) -0.0052(9) 0.0041(10) -0.0022(10) C16 0.0278(13) 0.0261(13) 0.0270(12) -0.0071(10) -0.0002(11) -0.0063(10) C17 0.0314(14) 0.0272(14) 0.0251(12) -0.0045(10) -0.0031(11) -0.0010(10) N18 0.0212(10) 0.0238(11) 0.0213(10) -0.0024(8) 0.0043(8) -0.0043(8) C19 0.0246(13) 0.0240(13) 0.0229(12) 0.0030(9) 0.0011(10) -0.0012(10) C20 0.0221(12) 0.0221(12) 0.0211(11) 0.0038(9) 0.0051(10) 0.0008(9) C21 0.0198(12) 0.0286(13) 0.0276(12) 0.0047(10) 0.0039(10) 0.0013(10) C22 0.0257(13) 0.0292(14) 0.0263(12) 0.0093(10) 0.0114(11) 0.0089(10) C23 0.0317(14) 0.0223(12) 0.0236(12) 0.0044(9) 0.0108(11) 0.0078(10) C24 0.0253(13) 0.0358(15) 0.0368(14) 0.0081(11) 0.0103(12) 0.0116(11) C25 0.0317(16) 0.0450(19) 0.077(2) 0.0163(16) 0.0262(17) 0.0120(13) C26 0.0367(17) 0.0375(17) 0.0536(19) -0.0004(14) 0.0091(15) 0.0195(13) C27 0.0312(16) 0.0456(18) 0.0426(17) 0.0100(14) 0.0077(14) 0.0165(13) C28 0.0320(14) 0.0370(15) 0.0238(12) -0.0009(10) 0.0097(11) 0.0001(11) C29 0.0345(15) 0.0372(15) 0.0264(13) -0.0109(11) 0.0021(12) 0.0003(11) C30 0.0284(13) 0.0256(13) 0.0219(12) 0.0029(9) 0.0035(10) 0.0055(10) C31 0.0217(12) 0.0215(13) 0.0302(13) 0.0049(10) 0.0103(10) 0.0048(9) C32 0.0216(12) 0.0197(12) 0.0298(13) -0.0013(9) 0.0105(10) 0.0021(9) C33 0.0328(14) 0.0255(14) 0.0340(14) 0.0106(10) 0.0083(12) 0.0074(10) C34 0.068(2) 0.0476(19) 0.0449(17) 0.0235(14) 0.0255(16) 0.0196(15) C35 0.0377(17) 0.0430(18) 0.072(2) 0.0167(16) -0.0060(16) 0.0117(13) C36 0.060(2) 0.0242(15) 0.0526(18) 0.0100(13) 0.0067(16) 0.0098(13) C37 0.0271(14) 0.0345(15) 0.0432(16) -0.0007(12) 0.0078(12) -0.0105(11) C38 0.0450(17) 0.0363(16) 0.0379(16) -0.0118(12) -0.0081(14) -0.0095(13) O40 0.0433(13) 0.0834(17) 0.0619(15) -0.0127(12) 0.0261(11) -0.0162(11) C41 0.053(2) 0.059(2) 0.058(2) -0.0072(17) 0.0120(18) -0.0036(16) C42 0.080(3) 0.0374(19) 0.093(3) -0.0056(18) 0.050(2) -0.0134(17) C43 0.088(3) 0.110(3) 0.052(2) 0.029(2) 0.024(2) 0.046(3) C44 0.0348(19) 0.113(3) 0.069(3) -0.031(2) 0.0124(18) -0.0065(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O11 2.0471(14) . ? Co1 N8 2.0986(18) . ? Co1 N4 2.1091(18) . ? Co1 O1 2.1844(14) . ? Co1 Br1 2.6704(4) . ? Co1 Br2 2.7438(4) . ? Co1 Co2 2.9490(4) . ? Co2 O11 2.0494(14) . ? Co2 N14 2.1064(18) . ? Co2 N18 2.1085(18) . ? Co2 O1 2.1538(14) . ? Co2 Br1 2.7767(4) . ? Co2 Br3 2.7860(4) . ? Co3 O1 2.0109(14) . ? Co3 Br4 2.3521(4) . ? Co3 Br3 2.4240(4) . ? Co3 Br2 2.4291(4) . ? O1 C1 1.386(2) . ? C1 C2 1.392(3) . ? C1 C20 1.392(3) . ? C2 C23 1.389(3) . ? C2 C3 1.500(3) . ? C3 N4 1.491(3) . ? N4 C5 1.479(3) . ? C5 C6 1.517(3) . ? C6 C28 1.526(3) . ? C6 C7 1.529(3) . ? C6 C29 1.530(3) . ? C7 N8 1.481(3) . ? N8 C9 1.487(3) . ? C9 C10 1.495(3) . ? C10 C30 1.400(3) . ? C10 C11 1.406(3) . ? C11 O11 1.350(2) . ? C11 C12 1.404(3) . ? C12 C32 1.398(3) . ? C12 C13 1.488(3) . ? C13 N14 1.492(3) . ? N14 C15 1.470(3) . ? C15 C16 1.530(3) . ? C16 C17 1.528(3) . ? C16 C37 1.531(3) . ? C16 C38 1.538(3) . ? C17 N18 1.490(3) . ? N18 C19 1.497(3) . ? C19 C20 1.503(3) . ? C20 C21 1.391(3) . ? C21 C22 1.376(3) . ? C22 C23 1.383(3) . ? C22 C24 1.543(3) . ? C24 C26' 1.494(15) . ? C24 C27 1.517(3) . ? C24 C25 1.519(4) . ? C24 C26 1.543(4) . ? C24 C25' 1.544(15) . ? C24 C27' 1.576(15) . ? C30 C31 1.382(3) . ? C31 C32 1.382(3) . ? C31 C33 1.534(3) . ? C33 C34 1.523(4) . ? C33 C35 1.525(3) . ? C33 C36 1.532(4) . ? O40 C41 1.397(4) . ? O40 C44 1.415(4) . ? C41 C42 1.492(5) . ? C42 C43 1.515(5) . ? C43 C44 1.486(5) . ? O50 C54 1.399(12) . ? O50 C51 1.428(12) . ? C51 C52 1.487(12) . ? C52 C53 1.458(12) . ? C53 C54 1.542(12) . ? O50' C51' 1.471(15) . ? O50' C54' 1.475(14) . ? C51' C52' 1.508(14) . ? C52' C53' 1.520(14) . ? C53' C54' 1.498(14) . ? O50" C54" 1.390(11) . ? O50" C51" 1.497(11) . ? C51" C52" 1.514(11) . ? C52" C53" 1.517(13) . ? C53" C54" 1.663(16) . ? O60 C61 1.370(10) . ? O60 C64 1.460(9) . ? C61 C62 1.467(9) . ? C62 C63 1.493(9) . ? C63 C64 1.500(10) . ? O60' C61' 1.395(13) . ? O60' C64' 1.523(13) . ? C61' C62' 1.498(12) . ? C62' C63' 1.533(13) . ? C63' C64' 1.495(13) . ? O60" C64" 1.403(12) . ? O60" C61" 1.417(12) . ? C61" C62" 1.483(12) . ? C62" C63" 1.504(11) . ? C63" C64" 1.485(11) . ? 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 O11 Co1 N8 94.06(6) . . ? O11 Co1 N4 172.70(6) . . ? N8 Co1 N4 93.22(7) . . ? O11 Co1 O1 82.87(5) . . ? N8 Co1 O1 176.89(6) . . ? N4 Co1 O1 89.85(6) . . ? O11 Co1 Br1 82.27(4) . . ? N8 Co1 Br1 97.34(5) . . ? N4 Co1 Br1 97.32(5) . . ? O1 Co1 Br1 81.82(4) . . ? O11 Co1 Br2 86.91(4) . . ? N8 Co1 Br2 97.67(5) . . ? N4 Co1 Br2 91.60(5) . . ? O1 Co1 Br2 82.68(4) . . ? Br1 Co1 Br2 162.059(14) . . ? O11 Co1 Co2 43.99(4) . . ? N8 Co1 Co2 130.33(5) . . ? N4 Co1 Co2 129.88(5) . . ? O1 Co1 Co2 46.74(4) . . ? Br1 Co1 Co2 58.975(10) . . ? Br2 Co1 Co2 103.507(12) . . ? O11 Co2 N14 92.04(6) . . ? O11 Co2 N18 172.79(7) . . ? N14 Co2 N18 94.13(7) . . ? O11 Co2 O1 83.58(5) . . ? N14 Co2 O1 174.12(7) . . ? N18 Co2 O1 90.51(6) . . ? O11 Co2 Br1 79.58(4) . . ? N14 Co2 Br1 103.26(5) . . ? N18 Co2 Br1 95.35(5) . . ? O1 Co2 Br1 79.86(4) . . ? O11 Co2 Br3 87.41(4) . . ? N14 Co2 Br3 94.76(5) . . ? N18 Co2 Br3 95.79(5) . . ? O1 Co2 Br3 81.16(4) . . ? Br1 Co2 Br3 158.027(14) . . ? O11 Co2 Co1 43.93(4) . . ? N14 Co2 Co1 130.19(5) . . ? N18 Co2 Co1 128.89(5) . . ? O1 Co2 Co1 47.61(4) . . ? Br1 Co2 Co1 55.502(9) . . ? Br3 Co2 Co1 103.086(12) . . ? O1 Co3 Br4 110.47(4) . . ? O1 Co3 Br3 93.75(4) . . ? Br4 Co3 Br3 115.477(15) . . ? O1 Co3 Br2 94.86(4) . . ? Br4 Co3 Br2 115.536(15) . . ? Br3 Co3 Br2 120.870(15) . . ? Co1 Br1 Co2 65.522(10) . . ? Co3 Br2 Co1 77.795(11) . . ? Co3 Br3 Co2 77.516(11) . . ? C1 O1 Co3 117.07(12) . . ? C1 O1 Co2 122.10(12) . . ? Co3 O1 Co2 103.59(6) . . ? C1 O1 Co1 120.95(12) . . ? Co3 O1 Co1 101.79(6) . . ? Co2 O1 Co1 85.65(5) . . ? O1 C1 C2 120.27(19) . . ? O1 C1 C20 120.58(19) . . ? C2 C1 C20 119.1(2) . . ? C23 C2 C1 119.3(2) . . ? C23 C2 C3 119.4(2) . . ? C1 C2 C3 121.1(2) . . ? N4 C3 C2 112.96(18) . . ? C5 N4 C3 107.90(17) . . ? C5 N4 Co1 117.08(14) . . ? C3 N4 Co1 112.25(13) . . ? N4 C5 C6 115.55(18) . . ? C5 C6 C28 111.19(19) . . ? C5 C6 C7 111.39(18) . . ? C28 C6 C7 111.64(19) . . ? C5 C6 C29 106.81(19) . . ? C28 C6 C29 109.90(19) . . ? C7 C6 C29 105.64(18) . . ? N8 C7 C6 116.40(18) . . ? C7 N8 C9 106.86(17) . . ? C7 N8 Co1 118.19(14) . . ? C9 N8 Co1 108.34(13) . . ? N8 C9 C10 114.60(19) . . ? C30 C10 C11 119.8(2) . . ? C30 C10 C9 118.2(2) . . ? C11 C10 C9 121.8(2) . . ? O11 C11 C12 121.32(19) . . ? O11 C11 C10 121.17(19) . . ? C12 C11 C10 117.46(19) . . ? C11 O11 Co1 124.43(13) . . ? C11 O11 Co2 123.49(13) . . ? Co1 O11 Co2 92.09(6) . . ? C32 C12 C11 120.6(2) . . ? C32 C12 C13 118.6(2) . . ? C11 C12 C13 120.83(19) . . ? C12 C13 N14 111.50(18) . . ? C15 N14 C13 109.55(17) . . ? C15 N14 Co2 117.13(14) . . ? C13 N14 Co2 108.94(13) . . ? N14 C15 C16 114.14(19) . . ? C17 C16 C15 110.6(2) . . ? C17 C16 C37 111.8(2) . . ? C15 C16 C37 110.9(2) . . ? C17 C16 C38 107.0(2) . . ? C15 C16 C38 106.4(2) . . ? C37 C16 C38 110.0(2) . . ? N18 C17 C16 115.09(19) . . ? C17 N18 C19 107.29(17) . . ? C17 N18 Co2 118.25(14) . . ? C19 N18 Co2 111.22(13) . . ? N18 C19 C20 112.81(18) . . ? C21 C20 C1 119.4(2) . . ? C21 C20 C19 119.3(2) . . ? C1 C20 C19 121.1(2) . . ? C22 C21 C20 122.5(2) . . ? C21 C22 C23 116.8(2) . . ? C21 C22 C24 120.9(2) . . ? C23 C22 C24 122.2(2) . . ? C22 C23 C2 122.6(2) . . ? C26' C24 C27 51.1(16) . . ? C26' C24 C25 131(2) . . ? C27 C24 C25 110.6(2) . . ? C26' C24 C26 57.4(16) . . ? C27 C24 C26 107.8(2) . . ? C25 C24 C26 107.8(2) . . ? C26' C24 C22 120(2) . . ? C27 C24 C22 110.5(2) . . ? C25 C24 C22 108.5(2) . . ? C26 C24 C22 111.6(2) . . ? C26' C24 C25' 110.4(14) . . ? C27 C24 C25' 139.5(18) . . ? C25 C24 C25' 50.1(15) . . ? C26 C24 C25' 60.8(15) . . ? C22 C24 C25' 109.6(17) . . ? C26' C24 C27' 107.3(14) . . ? C27 C24 C27' 60.8(15) . . ? C25 C24 C27' 55.7(15) . . ? C26 C24 C27' 144.7(19) . . ? C22 C24 C27' 103.5(19) . . ? C25' C24 C27' 104.5(13) . . ? C31 C30 C10 122.9(2) . . ? C32 C31 C30 116.7(2) . . ? C32 C31 C33 123.4(2) . . ? C30 C31 C33 119.9(2) . . ? C31 C32 C12 122.3(2) . . ? C34 C33 C35 110.3(2) . . ? C34 C33 C36 108.4(2) . . ? C35 C33 C36 107.9(2) . . ? C34 C33 C31 108.9(2) . . ? C35 C33 C31 110.1(2) . . ? C36 C33 C31 111.3(2) . . ? C41 O40 C44 103.9(2) . . ? O40 C41 C42 107.8(3) . . ? C41 C42 C43 103.1(3) . . ? C44 C43 C42 102.9(3) . . ? O40 C44 C43 104.1(3) . . ? C54 O50 C51 114.7(8) . . ? O50 C51 C52 105.9(8) . . ? C53 C52 C51 106.9(7) . . ? C52 C53 C54 108.3(7) . . ? O50 C54 C53 102.9(8) . . ? C51' O50' C54' 102.5(12) . . ? O50' C51' C52' 101.4(11) . . ? C51' C52' C53' 103.9(9) . . ? C54' C53' C52' 105.8(8) . . ? O50' C54' C53' 102.4(10) . . ? C54" O50" C51" 104.6(9) . . ? O50" C51" C52" 98.8(7) . . ? C51" C52" C53" 105.1(7) . . ? C52" C53" C54" 101.5(7) . . ? O50" C54" C53" 101.4(8) . . ? C61 O60 C64 110.4(6) . . ? O60 C61 C62 104.8(6) . . ? C61 C62 C63 105.3(6) . . ? C62 C63 C64 102.6(6) . . ? O60 C64 C63 105.7(6) . . ? C61' O60' C64' 102.7(10) . . ? O60' C61' C62' 97.8(10) . . ? C61' C62' C63' 99.2(9) . . ? C64' C63' C62' 103.6(8) . . ? C63' C64' O60' 102.3(8) . . ? C64" O60" C61" 111.8(9) . . ? O60" C61" C62" 107.7(8) . . ? C61" C62" C63" 105.7(7) . . ? C64" C63" C62" 106.5(7) . . ? O60" C64" C63" 107.0(8) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.612 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.084 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 825192' #TrackingRef '- kember et al_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H108 Cl5 Co4 K N8 O4, 7.5(C H2 Cl2)' _chemical_formula_sum 'C75.50 H123 Cl20 Co4 K N8 O4' _chemical_formula_weight 2190.64 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' 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 23.2374(5) _cell_length_b 30.6555(6) _cell_length_c 14.1318(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10066.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16492 _cell_measurement_theta_min 3.0076 _cell_measurement_theta_max 30.2542 _exptl_crystal_description prisms _exptl_crystal_colour 'Dark pink' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4524 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32133 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 30.33 _reflns_number_total 13312 _reflns_number_gt 10248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0353P)^2^+36.8466P] 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 SHELXL _refine_ls_extinction_coef 0.00035(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13312 _refine_ls_number_parameters 623 _refine_ls_number_restraints 166 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.57238(2) 0.632085(15) 0.46348(3) 0.01748(11) Uani 1 1 d . . . Co2 Co 0.46741(2) 0.664822(16) 0.55679(3) 0.01780(11) Uani 1 1 d . . . Cl1 Cl 0.48342(4) 0.58333(3) 0.52934(7) 0.02373(18) Uani 1 1 d . . . Cl2 Cl 0.64704(4) 0.68053(3) 0.40830(7) 0.02531(19) Uani 1 1 d . . . Cl3 Cl 0.45604(5) 0.7500 0.57574(9) 0.0215(2) Uani 1 2 d S . . O1 O 0.55495(10) 0.66312(8) 0.59401(17) 0.0190(5) Uani 1 1 d . . . C1 C 0.57272(15) 0.64659(11) 0.6782(3) 0.0192(7) Uani 1 1 d . . . C2 C 0.62415(15) 0.62258(12) 0.6862(3) 0.0196(7) Uani 1 1 d . . . C3 C 0.66279(15) 0.61504(13) 0.6029(3) 0.0213(7) Uani 1 1 d . . . H3A H 0.6756 0.6435 0.5775 0.026 Uiso 1 1 calc R . . H3B H 0.6974 0.5989 0.6239 0.026 Uiso 1 1 calc R . . N4 N 0.63356(12) 0.58994(10) 0.5265(2) 0.0184(6) Uani 1 1 d D . . H4 H 0.6165(17) 0.5663(9) 0.552(3) 0.028(12) Uiso 1 1 d D . . C5 C 0.67751(15) 0.56968(12) 0.4644(3) 0.0220(7) Uani 1 1 d . . . H5A H 0.7009 0.5494 0.5029 0.026 Uiso 1 1 calc R . . H5B H 0.7035 0.5929 0.4409 0.026 Uiso 1 1 calc R . . C6 C 0.65372(16) 0.54491(12) 0.3800(3) 0.0216(7) Uani 1 1 d . . . C7 C 0.62817(16) 0.57582(13) 0.3062(3) 0.0236(8) Uani 1 1 d . . . H7A H 0.6570 0.5986 0.2915 0.028 Uiso 1 1 calc R . . H7B H 0.6212 0.5591 0.2473 0.028 Uiso 1 1 calc R . . N8 N 0.57382(13) 0.59747(10) 0.3344(2) 0.0186(6) Uani 1 1 d D . . H8 H 0.5433(12) 0.5794(12) 0.337(3) 0.032(12) Uiso 1 1 d D . . C9 C 0.55651(16) 0.62810(12) 0.2579(3) 0.0212(7) Uani 1 1 d . . . H9A H 0.5656 0.6149 0.1957 0.025 Uiso 1 1 calc R . . H9B H 0.5790 0.6554 0.2638 0.025 Uiso 1 1 calc R . . C10 C 0.49366(15) 0.63864(11) 0.2617(3) 0.0194(7) Uani 1 1 d . . . C11 C 0.46832(15) 0.65798(11) 0.3424(3) 0.0187(7) Uani 1 1 d . . . O11 O 0.49969(10) 0.66866(8) 0.41881(17) 0.0177(5) Uani 1 1 d . . . C12 C 0.40867(15) 0.66649(12) 0.3372(3) 0.0195(7) Uani 1 1 d . . . C13 C 0.37741(16) 0.68785(12) 0.4175(3) 0.0230(7) Uani 1 1 d . . . H13A H 0.3937 0.7173 0.4279 0.028 Uiso 1 1 calc R . . H13B H 0.3364 0.6913 0.4002 0.028 Uiso 1 1 calc R . . N14 N 0.38140(13) 0.66246(10) 0.5073(2) 0.0197(6) Uani 1 1 d D . . H14 H 0.373(2) 0.6346(6) 0.492(4) 0.056(17) Uiso 1 1 d D . . C15 C 0.33354(15) 0.67606(13) 0.5697(3) 0.0244(8) Uani 1 1 d . . . H15A H 0.2968 0.6677 0.5393 0.029 Uiso 1 1 calc R . . H15B H 0.3340 0.7083 0.5748 0.029 Uiso 1 1 calc R . . C16 C 0.33473(15) 0.65686(13) 0.6696(3) 0.0247(8) Uani 1 1 d . . . C17 C 0.38419(15) 0.67530(13) 0.7272(3) 0.0236(8) Uani 1 1 d . . . H17A H 0.3838 0.7075 0.7211 0.028 Uiso 1 1 calc R . . H17B H 0.3777 0.6682 0.7946 0.028 Uiso 1 1 calc R . . N18 N 0.44200(13) 0.65917(10) 0.6996(2) 0.0195(6) Uani 1 1 d D . . H18 H 0.4426(16) 0.6307(3) 0.715(3) 0.011(9) Uiso 1 1 d D . . C19 C 0.48665(16) 0.67971(13) 0.7603(3) 0.0226(7) Uani 1 1 d . . . H19A H 0.4717 0.6825 0.8257 0.027 Uiso 1 1 calc R . . H19B H 0.4950 0.7094 0.7365 0.027 Uiso 1 1 calc R . . C20 C 0.54118(15) 0.65350(12) 0.7615(3) 0.0214(7) Uani 1 1 d . . . C21 C 0.55909(16) 0.63527(13) 0.8465(3) 0.0245(8) Uani 1 1 d . . . H21A H 0.5364 0.6403 0.9013 0.029 Uiso 1 1 calc R . . C22 C 0.60862(16) 0.60997(13) 0.8557(3) 0.0245(8) Uani 1 1 d . . . C23 C 0.64014(15) 0.60488(12) 0.7730(3) 0.0215(7) Uani 1 1 d . . . H23A H 0.6747 0.5883 0.7758 0.026 Uiso 1 1 calc R . . C24 C 0.62603(17) 0.59020(15) 0.9508(3) 0.0302(9) Uani 1 1 d . . . C25 C 0.6439(3) 0.6275(2) 1.0177(4) 0.0580(16) Uani 1 1 d . . . H25A H 0.6121 0.6483 1.0237 0.087 Uiso 1 1 calc R . . H25B H 0.6777 0.6425 0.9918 0.087 Uiso 1 1 calc R . . H25C H 0.6533 0.6155 1.0801 0.087 Uiso 1 1 calc R . . C26 C 0.57612(19) 0.56538(17) 0.9947(3) 0.0380(10) Uani 1 1 d . . . H26A H 0.5649 0.5414 0.9529 0.057 Uiso 1 1 calc R . . H26B H 0.5434 0.5852 1.0034 0.057 Uiso 1 1 calc R . . H26C H 0.5879 0.5536 1.0562 0.057 Uiso 1 1 calc R . . C27 C 0.6763(2) 0.5579(2) 0.9410(4) 0.0500(14) Uani 1 1 d . . . H27A H 0.6650 0.5340 0.8987 0.075 Uiso 1 1 calc R . . H27B H 0.6860 0.5460 1.0034 0.075 Uiso 1 1 calc R . . H27C H 0.7098 0.5730 0.9146 0.075 Uiso 1 1 calc R . . C28 C 0.61015(18) 0.50999(13) 0.4106(3) 0.0289(8) Uani 1 1 d . . . H28A H 0.6278 0.4909 0.4580 0.043 Uiso 1 1 calc R . . H28B H 0.5987 0.4926 0.3555 0.043 Uiso 1 1 calc R . . H28C H 0.5761 0.5241 0.4378 0.043 Uiso 1 1 calc R . . C29 C 0.70528(19) 0.52251(15) 0.3321(3) 0.0343(10) Uani 1 1 d . . . H29A H 0.7234 0.5023 0.3767 0.051 Uiso 1 1 calc R . . H29B H 0.7333 0.5446 0.3125 0.051 Uiso 1 1 calc R . . H29C H 0.6920 0.5064 0.2764 0.051 Uiso 1 1 calc R . . C30 C 0.46061(16) 0.62891(12) 0.1823(3) 0.0227(7) Uani 1 1 d . . . H30A H 0.4790 0.6155 0.1298 0.027 Uiso 1 1 calc R . . C31 C 0.40201(16) 0.63792(13) 0.1759(3) 0.0231(7) Uani 1 1 d . . . C32 C 0.37738(16) 0.65690(12) 0.2561(3) 0.0226(7) Uani 1 1 d . . . H32A H 0.3375 0.6635 0.2552 0.027 Uiso 1 1 calc R . . C33 C 0.36723(18) 0.62621(15) 0.0871(3) 0.0295(9) Uani 1 1 d . . . C34 C 0.3988(2) 0.6420(2) -0.0014(3) 0.0584(17) Uani 1 1 d . . . H34A H 0.3764 0.6343 -0.0577 0.088 Uiso 1 1 calc R . . H34B H 0.4367 0.6281 -0.0048 0.088 Uiso 1 1 calc R . . H34C H 0.4035 0.6738 0.0016 0.088 Uiso 1 1 calc R . . C35 C 0.3077(2) 0.6466(2) 0.0879(4) 0.0482(13) Uani 1 1 d . . . H35A H 0.2865 0.6365 0.1437 0.072 Uiso 1 1 calc R . . H35B H 0.2869 0.6381 0.0305 0.072 Uiso 1 1 calc R . . H35C H 0.3113 0.6785 0.0901 0.072 Uiso 1 1 calc R . . C36 C 0.3607(3) 0.57670(19) 0.0805(5) 0.0660(19) Uani 1 1 d . . . H36A H 0.3407 0.5659 0.1369 0.099 Uiso 1 1 calc R . . H36B H 0.3988 0.5632 0.0764 0.099 Uiso 1 1 calc R . . H36C H 0.3383 0.5693 0.0240 0.099 Uiso 1 1 calc R . . C37 C 0.33633(19) 0.60658(14) 0.6663(4) 0.0348(10) Uani 1 1 d . . . H37A H 0.3715 0.5970 0.6341 0.052 Uiso 1 1 calc R . . H37B H 0.3026 0.5958 0.6317 0.052 Uiso 1 1 calc R . . H37C H 0.3359 0.5950 0.7309 0.052 Uiso 1 1 calc R . . C38 C 0.27899(17) 0.67228(16) 0.7183(3) 0.0347(10) Uani 1 1 d . . . H38A H 0.2782 0.7042 0.7198 0.052 Uiso 1 1 calc R . . H38B H 0.2777 0.6609 0.7831 0.052 Uiso 1 1 calc R . . H38C H 0.2456 0.6615 0.6829 0.052 Uiso 1 1 calc R . . K1 K 0.56813(7) 0.7500 0.47897(16) 0.0559(5) Uani 1 2 d S . 1 C40 C 0.4976(2) 0.46616(14) 0.2379(3) 0.0355(10) Uani 1 1 d . . . H40A H 0.4622 0.4503 0.2197 0.043 Uiso 1 1 calc R . . H40B H 0.5041 0.4616 0.3064 0.043 Uiso 1 1 calc R . . Cl4 Cl 0.48878(6) 0.52207(4) 0.21534(10) 0.0450(3) Uani 1 1 d . . . Cl5 Cl 0.55653(6) 0.44513(4) 0.17373(10) 0.0492(3) Uani 1 1 d . . . C50 C 0.3672(2) 0.55261(15) 0.3533(3) 0.0383(10) Uani 1 1 d . . . H50A H 0.3981 0.5526 0.4017 0.046 Uiso 1 1 calc R . . H50B H 0.3805 0.5703 0.2989 0.046 Uiso 1 1 calc R . . Cl6 Cl 0.35345(7) 0.49837(4) 0.31574(9) 0.0489(3) Uani 1 1 d . . . Cl7 Cl 0.30449(6) 0.57589(5) 0.40119(11) 0.0565(4) Uani 1 1 d . . . C60 C 0.7371(3) 0.7500 0.5383(6) 0.0496(18) Uani 1 2 d S A 2 H60A H 0.7303 0.7761 0.4986 0.059 Uiso 0.50 1 calc PR A 2 H60B H 0.7303 0.7239 0.4986 0.059 Uiso 0.50 1 calc PR A 2 Cl8 Cl 0.80997(8) 0.7500 0.57698(16) 0.0587(5) Uani 1 2 d S A 2 Cl9 Cl 0.68883(9) 0.7500 0.63117(15) 0.0615(6) Uani 1 2 d S A 2 C70 C 0.4833(5) 0.7493(3) 0.1583(7) 0.052(3) Uiso 0.388(5) 1 d PDU B -3 H70A H 0.4576 0.7250 0.1769 0.062 Uiso 0.388(5) 1 calc PR B -3 H70B H 0.4626 0.7770 0.1703 0.062 Uiso 0.388(5) 1 calc PR B -3 Cl10 Cl 0.5460(3) 0.748(3) 0.2277(5) 0.059(5) Uani 0.388(5) 1 d PDU B -3 Cl11 Cl 0.4985(3) 0.7452(10) 0.0386(3) 0.103(5) Uani 0.388(5) 1 d PDU B -3 C75 C 0.4694(11) 0.7516(3) 0.1828(15) 0.039(6) Uiso 0.112(5) 1 d PDU B -4 H75A H 0.4555 0.7254 0.2169 0.047 Uiso 0.112(5) 1 calc PR B -4 H75B H 0.4497 0.7775 0.2090 0.047 Uiso 0.112(5) 1 calc PR B -4 Cl12 Cl 0.5442(11) 0.7568(13) 0.1959(18) 0.070(6) Uani 0.112(5) 1 d PDU B -4 Cl13 Cl 0.4551(11) 0.747(2) 0.0620(11) 0.100(6) Uani 0.112(5) 1 d PDU B -4 C80 C 0.7034(4) 0.7417(3) 0.2256(7) 0.029(3) Uiso 0.343(3) 1 d PDU C -5 H80A H 0.6897 0.7632 0.1784 0.035 Uiso 0.343(3) 1 calc PR C -5 H80B H 0.6760 0.7411 0.2793 0.035 Uiso 0.343(3) 1 calc PR C -5 Cl14 Cl 0.7723(3) 0.7548(4) 0.2643(4) 0.076(2) Uani 0.343(3) 1 d PDU C -5 Cl15 Cl 0.7099(2) 0.6898(2) 0.1745(4) 0.0800(17) Uani 0.343(3) 1 d PDU C -5 C85 C 0.7230(14) 0.7152(8) 0.173(2) 0.051(7) Uiso 0.157(3) 1 d PDU C -6 H85A H 0.6894 0.7064 0.2113 0.061 Uiso 0.157(3) 1 calc PR C -6 H85B H 0.7364 0.6896 0.1360 0.061 Uiso 0.157(3) 1 calc PR C -6 Cl16 Cl 0.7773(9) 0.7349(7) 0.2438(12) 0.098(3) Uani 0.157(3) 1 d PDU C -6 Cl17 Cl 0.7043(5) 0.7581(5) 0.0963(7) 0.084(3) Uani 0.157(3) 1 d PDU C -6 C90 C 0.6483(13) 0.7756(7) 0.883(2) 0.078(11) Uiso 0.183(2) 1 d PDU D -7 H90A H 0.6227 0.7951 0.9196 0.094 Uiso 0.183(2) 1 calc PR D -7 H90B H 0.6658 0.7930 0.8313 0.094 Uiso 0.183(2) 1 calc PR D -7 Cl18 Cl 0.7026(3) 0.7560(5) 0.9569(6) 0.052(3) Uani 0.183(2) 1 d PDU D -7 Cl19 Cl 0.6084(3) 0.7341(3) 0.8350(6) 0.0591(19) Uani 0.183(2) 1 d PDU D -7 C95 C 0.6337(8) 0.7627(3) 0.992(2) 0.087(14) Uiso 0.067(2) 1 d PDU D -8 H95A H 0.6356 0.7468 1.0528 0.104 Uiso 0.067(2) 1 calc PR D -8 H95B H 0.6312 0.7943 1.0060 0.104 Uiso 0.067(2) 1 calc PR D -8 Cl20 Cl 0.5730(5) 0.7463(3) 0.9293(10) 0.043(3) Uiso 0.067(2) 1 d PDU D -8 Cl21 Cl 0.6953(7) 0.7522(3) 0.9258(15) 0.052(3) Uiso 0.067(2) 1 d PDU D -8 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0174(2) 0.0172(2) 0.0178(2) -0.00108(19) 0.00055(18) 0.00081(17) Co2 0.0161(2) 0.0199(2) 0.0174(2) -0.00018(19) 0.00176(18) -0.00057(17) Cl1 0.0252(4) 0.0184(4) 0.0277(5) 0.0007(3) 0.0029(4) -0.0012(3) Cl2 0.0220(4) 0.0214(4) 0.0325(5) 0.0008(4) 0.0036(4) -0.0038(3) Cl3 0.0238(6) 0.0164(5) 0.0242(6) 0.000 0.0020(5) 0.000 O1 0.0197(11) 0.0196(12) 0.0177(12) 0.0006(10) 0.0009(10) -0.0010(9) C1 0.0194(16) 0.0189(16) 0.0191(17) -0.0011(13) -0.0016(14) -0.0036(13) C2 0.0182(16) 0.0210(17) 0.0195(18) -0.0012(14) -0.0013(13) -0.0040(13) C3 0.0179(16) 0.0254(18) 0.0205(18) -0.0033(15) -0.0023(14) 0.0000(13) N4 0.0174(13) 0.0190(14) 0.0189(15) -0.0008(12) 0.0007(11) -0.0017(11) C5 0.0179(16) 0.0256(17) 0.0225(18) -0.0012(15) 0.0004(14) 0.0033(13) C6 0.0225(17) 0.0187(16) 0.0236(19) -0.0006(14) -0.0009(14) 0.0029(13) C7 0.0217(17) 0.0276(19) 0.0215(19) -0.0009(15) 0.0032(15) 0.0028(14) N8 0.0192(14) 0.0170(13) 0.0198(15) 0.0017(12) 0.0023(12) 0.0012(11) C9 0.0228(17) 0.0239(17) 0.0170(17) 0.0030(14) 0.0030(14) 0.0029(14) C10 0.0213(16) 0.0179(16) 0.0189(17) 0.0029(14) 0.0010(14) 0.0014(13) C11 0.0219(16) 0.0150(15) 0.0193(17) 0.0051(13) 0.0000(14) -0.0008(13) O11 0.0165(11) 0.0189(12) 0.0176(12) -0.0007(10) 0.0004(9) 0.0003(9) C12 0.0194(16) 0.0195(16) 0.0196(17) 0.0008(14) 0.0025(13) 0.0015(13) C13 0.0234(17) 0.0240(18) 0.0217(19) -0.0020(15) -0.0011(15) 0.0055(14) N14 0.0183(13) 0.0195(14) 0.0214(15) -0.0038(12) 0.0009(12) 0.0006(11) C15 0.0170(16) 0.0309(19) 0.025(2) -0.0020(16) 0.0032(14) 0.0033(14) C16 0.0171(16) 0.0268(19) 0.030(2) -0.0005(16) 0.0074(15) -0.0015(14) C17 0.0202(17) 0.0287(19) 0.0220(19) -0.0003(15) 0.0054(14) 0.0022(14) N18 0.0186(14) 0.0166(14) 0.0232(16) -0.0002(12) 0.0022(12) 0.0013(11) C19 0.0247(17) 0.0258(18) 0.0174(17) -0.0032(15) -0.0007(14) 0.0031(14) C20 0.0203(17) 0.0238(17) 0.0199(18) -0.0020(14) -0.0022(14) -0.0016(14) C21 0.0217(17) 0.030(2) 0.0213(18) -0.0033(16) 0.0009(14) -0.0020(15) C22 0.0224(17) 0.0301(19) 0.0211(19) 0.0007(16) -0.0039(15) -0.0036(15) C23 0.0179(16) 0.0246(18) 0.0222(19) -0.0015(15) -0.0022(14) -0.0016(14) C24 0.0254(19) 0.043(2) 0.022(2) 0.0045(18) -0.0031(16) 0.0006(17) C25 0.073(4) 0.072(4) 0.028(3) 0.003(3) -0.017(3) -0.025(3) C26 0.033(2) 0.052(3) 0.028(2) 0.015(2) -0.0006(18) -0.001(2) C27 0.037(2) 0.078(4) 0.036(3) 0.022(3) -0.001(2) 0.019(3) C28 0.034(2) 0.0197(17) 0.033(2) -0.0017(16) -0.0032(18) -0.0005(15) C29 0.034(2) 0.039(2) 0.030(2) -0.0092(19) 0.0003(18) 0.0160(19) C30 0.0280(18) 0.0241(17) 0.0160(17) -0.0001(14) 0.0010(14) 0.0007(15) C31 0.0263(18) 0.0252(18) 0.0177(18) 0.0015(15) -0.0017(14) -0.0031(15) C32 0.0203(17) 0.0245(18) 0.0231(19) 0.0016(15) -0.0014(14) 0.0016(14) C33 0.0283(19) 0.039(2) 0.0212(19) 0.0003(17) -0.0048(16) -0.0019(17) C34 0.041(3) 0.113(5) 0.021(2) 0.010(3) -0.004(2) -0.008(3) C35 0.036(2) 0.072(4) 0.037(3) -0.014(3) -0.013(2) 0.005(2) C36 0.094(5) 0.047(3) 0.057(4) -0.004(3) -0.042(4) -0.010(3) C37 0.033(2) 0.027(2) 0.044(3) 0.0015(19) 0.005(2) -0.0074(17) C38 0.0217(19) 0.048(3) 0.034(2) -0.003(2) 0.0101(17) -0.0005(18) K1 0.0379(8) 0.0221(6) 0.1079(15) 0.000 0.0365(9) 0.000 C40 0.041(2) 0.027(2) 0.038(3) 0.0016(19) -0.003(2) -0.0028(18) Cl4 0.0493(7) 0.0278(5) 0.0580(8) 0.0014(5) -0.0059(6) -0.0043(5) Cl5 0.0479(7) 0.0444(7) 0.0554(8) -0.0004(6) 0.0025(6) 0.0044(5) C50 0.048(3) 0.032(2) 0.036(2) 0.0020(19) 0.003(2) -0.008(2) Cl6 0.0742(9) 0.0289(5) 0.0436(7) 0.0009(5) -0.0004(6) -0.0108(6) Cl7 0.0497(7) 0.0553(8) 0.0645(9) -0.0207(7) 0.0151(7) -0.0140(6) C60 0.034(3) 0.060(5) 0.055(5) 0.000 -0.010(3) 0.000 Cl8 0.0429(10) 0.0722(14) 0.0611(13) 0.000 -0.0118(9) 0.000 Cl9 0.0504(11) 0.0891(16) 0.0451(11) 0.000 -0.0038(9) 0.000 Cl10 0.0591(18) 0.037(14) 0.081(4) 0.002(7) -0.007(2) 0.000(6) Cl11 0.141(5) 0.099(13) 0.069(3) -0.012(5) 0.009(3) -0.037(10) Cl12 0.076(7) 0.041(14) 0.093(11) 0.002(8) -0.010(8) 0.002(9) Cl13 0.132(9) 0.098(14) 0.070(7) -0.009(11) -0.001(7) -0.037(14) Cl14 0.071(2) 0.077(5) 0.079(3) -0.027(4) 0.021(2) -0.050(3) Cl15 0.081(3) 0.096(4) 0.063(3) -0.024(3) 0.021(2) -0.025(3) Cl16 0.093(5) 0.103(7) 0.097(6) -0.006(6) 0.028(5) -0.023(6) Cl17 0.090(5) 0.095(7) 0.066(4) -0.002(5) 0.014(4) -0.024(5) Cl18 0.048(3) 0.051(7) 0.056(4) 0.007(4) -0.013(3) -0.002(3) Cl19 0.058(4) 0.056(4) 0.064(4) -0.008(3) -0.003(3) -0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N8 2.111(3) . ? Co1 O1 2.115(3) . ? Co1 N4 2.117(3) . ? Co1 O11 2.123(2) . ? Co1 Cl2 2.4132(10) . ? Co1 Cl1 2.7155(10) . ? Co1 Co2 2.9490(7) . ? Co2 O11 2.092(2) . ? Co2 O1 2.102(2) . ? Co2 N18 2.110(3) . ? Co2 N14 2.119(3) . ? Co2 Cl1 2.5554(10) . ? Co2 Cl3 2.6381(5) . ? Cl2 K1 2.9823(14) . ? Cl3 Co2 2.6381(5) 7_575 ? Cl3 K1 2.9420(19) . ? O1 C1 1.357(4) . ? O1 K1 3.135(3) . ? C1 C20 1.403(5) . ? C1 C2 1.408(5) . ? C2 C23 1.391(5) . ? C2 C3 1.498(5) . ? C3 N4 1.490(5) . ? N4 C5 1.483(5) . ? C5 C6 1.518(5) . ? C6 C7 1.529(5) . ? C6 C28 1.536(5) . ? C6 C29 1.538(5) . ? C7 N8 1.481(5) . ? N8 C9 1.487(5) . ? C9 C10 1.497(5) . ? C10 C30 1.393(5) . ? C10 C11 1.414(5) . ? C11 O11 1.343(4) . ? C11 C12 1.412(5) . ? O11 K1 3.077(3) . ? C12 C32 1.388(5) . ? C12 C13 1.499(5) . ? C13 N14 1.491(5) . ? N14 C15 1.479(5) . ? C15 C16 1.531(6) . ? C16 C17 1.517(5) . ? C16 C38 1.541(5) . ? C16 C37 1.543(6) . ? C17 N18 1.483(4) . ? N18 C19 1.486(5) . ? C19 C20 1.500(5) . ? C20 C21 1.388(5) . ? C21 C22 1.394(5) . ? C22 C23 1.388(5) . ? C22 C24 1.529(5) . ? C24 C26 1.520(6) . ? C24 C27 1.538(6) . ? C24 C25 1.542(7) . ? C30 C31 1.392(5) . ? C31 C32 1.397(5) . ? C31 C33 1.536(5) . ? C33 C35 1.518(6) . ? C33 C36 1.528(7) . ? C33 C34 1.528(6) . ? K1 Cl2 2.9823(14) 7_575 ? K1 O11 3.077(3) 7_575 ? K1 O1 3.135(3) 7_575 ? C40 Cl4 1.755(4) . ? C40 Cl5 1.764(5) . ? C50 Cl7 1.759(5) . ? C50 Cl6 1.775(5) . ? C60 Cl9 1.727(8) . ? C60 Cl8 1.779(7) . ? C70 Cl11 1.731(10) . ? C70 Cl10 1.759(10) . ? C75 Cl13 1.746(15) . ? C75 Cl12 1.754(15) . ? C80 Cl14 1.740(9) . ? C80 Cl15 1.754(10) . ? C85 Cl16 1.725(16) . ? C85 Cl17 1.754(16) . ? C90 Cl19 1.715(15) . ? C90 Cl18 1.745(15) . ? C95 Cl20 1.740(16) . ? C95 Cl21 1.741(16) . ? 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 N8 Co1 O1 169.46(11) . . ? N8 Co1 N4 92.64(12) . . ? O1 Co1 N4 92.08(11) . . ? N8 Co1 O11 91.21(11) . . ? O1 Co1 O11 82.49(9) . . ? N4 Co1 O11 168.91(11) . . ? N8 Co1 Cl2 91.07(9) . . ? O1 Co1 Cl2 98.20(7) . . ? N4 Co1 Cl2 91.65(8) . . ? O11 Co1 Cl2 98.68(7) . . ? N8 Co1 Cl1 91.81(9) . . ? O1 Co1 Cl1 78.63(7) . . ? N4 Co1 Cl1 91.79(8) . . ? O11 Co1 Cl1 77.69(7) . . ? Cl2 Co1 Cl1 175.41(4) . . ? N8 Co1 Co2 124.80(8) . . ? O1 Co1 Co2 45.44(7) . . ? N4 Co1 Co2 125.10(8) . . ? O11 Co1 Co2 45.19(7) . . ? Cl2 Co1 Co2 121.98(3) . . ? Cl1 Co1 Co2 53.44(2) . . ? O11 Co2 O1 83.55(9) . . ? O11 Co2 N18 175.05(11) . . ? O1 Co2 N18 91.69(11) . . ? O11 Co2 N14 91.85(11) . . ? O1 Co2 N14 174.13(11) . . ? N18 Co2 N14 92.82(12) . . ? O11 Co2 Cl1 82.03(7) . . ? O1 Co2 Cl1 82.69(7) . . ? N18 Co2 Cl1 96.07(8) . . ? N14 Co2 Cl1 93.08(9) . . ? O11 Co2 Cl3 94.29(7) . . ? O1 Co2 Cl3 95.51(7) . . ? N18 Co2 Cl3 87.49(9) . . ? N14 Co2 Cl3 88.45(9) . . ? Cl1 Co2 Cl3 176.05(4) . . ? O11 Co2 Co1 46.04(7) . . ? O1 Co2 Co1 45.80(7) . . ? N18 Co2 Co1 129.15(8) . . ? N14 Co2 Co1 128.38(9) . . ? Cl1 Co2 Co1 58.60(2) . . ? Cl3 Co2 Co1 117.71(3) . . ? Co2 Cl1 Co1 67.96(3) . . ? Co1 Cl2 K1 83.64(3) . . ? Co2 Cl3 Co2 163.60(6) 7_575 . ? Co2 Cl3 K1 82.19(3) 7_575 . ? Co2 Cl3 K1 82.19(3) . . ? C1 O1 Co2 121.5(2) . . ? C1 O1 Co1 122.6(2) . . ? Co2 O1 Co1 88.75(9) . . ? C1 O1 K1 137.9(2) . . ? Co2 O1 K1 86.77(9) . . ? Co1 O1 K1 84.90(8) . . ? O1 C1 C20 121.3(3) . . ? O1 C1 C2 121.6(3) . . ? C20 C1 C2 117.0(3) . . ? C23 C2 C1 120.1(3) . . ? C23 C2 C3 118.2(3) . . ? C1 C2 C3 121.7(3) . . ? N4 C3 C2 112.1(3) . . ? C5 N4 C3 109.3(3) . . ? C5 N4 Co1 118.0(2) . . ? C3 N4 Co1 107.2(2) . . ? N4 C5 C6 115.1(3) . . ? C5 C6 C7 111.6(3) . . ? C5 C6 C28 111.6(3) . . ? C7 C6 C28 111.6(3) . . ? C5 C6 C29 106.6(3) . . ? C7 C6 C29 106.2(3) . . ? C28 C6 C29 109.0(3) . . ? N8 C7 C6 115.1(3) . . ? C7 N8 C9 108.5(3) . . ? C7 N8 Co1 118.1(2) . . ? C9 N8 Co1 107.9(2) . . ? N8 C9 C10 111.9(3) . . ? C30 C10 C11 120.7(3) . . ? C30 C10 C9 117.5(3) . . ? C11 C10 C9 121.8(3) . . ? O11 C11 C12 122.0(3) . . ? O11 C11 C10 121.6(3) . . ? C12 C11 C10 116.3(3) . . ? C11 O11 Co2 122.7(2) . . ? C11 O11 Co1 122.8(2) . . ? Co2 O11 Co1 88.77(9) . . ? C11 O11 K1 134.4(2) . . ? Co2 O11 K1 88.48(9) . . ? Co1 O11 K1 86.25(8) . . ? C32 C12 C11 121.2(3) . . ? C32 C12 C13 117.6(3) . . ? C11 C12 C13 121.1(3) . . ? N14 C13 C12 112.7(3) . . ? C15 N14 C13 108.2(3) . . ? C15 N14 Co2 120.2(2) . . ? C13 N14 Co2 108.8(2) . . ? N14 C15 C16 115.3(3) . . ? C17 C16 C15 111.4(3) . . ? C17 C16 C38 106.5(3) . . ? C15 C16 C38 106.2(3) . . ? C17 C16 C37 111.7(3) . . ? C15 C16 C37 110.9(4) . . ? C38 C16 C37 109.9(3) . . ? N18 C17 C16 114.9(3) . . ? C17 N18 C19 109.8(3) . . ? C17 N18 Co2 118.5(2) . . ? C19 N18 Co2 108.8(2) . . ? N18 C19 C20 111.7(3) . . ? C21 C20 C1 120.6(3) . . ? C21 C20 C19 118.6(3) . . ? C1 C20 C19 120.8(3) . . ? C20 C21 C22 123.5(4) . . ? C23 C22 C21 114.8(4) . . ? C23 C22 C24 123.8(3) . . ? C21 C22 C24 121.4(4) . . ? C22 C23 C2 123.9(3) . . ? C26 C24 C22 110.8(3) . . ? C26 C24 C27 107.1(4) . . ? C22 C24 C27 112.2(4) . . ? C26 C24 C25 109.1(4) . . ? C22 C24 C25 108.4(4) . . ? C27 C24 C25 109.2(4) . . ? C10 C30 C31 123.3(4) . . ? C30 C31 C32 115.5(3) . . ? C30 C31 C33 121.4(3) . . ? C32 C31 C33 123.0(3) . . ? C12 C32 C31 122.9(3) . . ? C35 C33 C36 108.6(4) . . ? C35 C33 C34 108.2(4) . . ? C36 C33 C34 108.3(5) . . ? C35 C33 C31 112.1(4) . . ? C36 C33 C31 109.5(4) . . ? C34 C33 C31 110.0(4) . . ? Cl3 K1 Cl2 134.43(3) . 7_575 ? Cl3 K1 Cl2 134.43(3) . . ? Cl2 K1 Cl2 91.13(5) 7_575 . ? Cl3 K1 O11 70.78(5) . . ? Cl2 K1 O11 143.50(9) 7_575 . ? Cl2 K1 O11 69.31(5) . . ? Cl3 K1 O11 70.78(5) . 7_575 ? Cl2 K1 O11 69.31(5) 7_575 7_575 ? Cl2 K1 O11 143.50(9) . 7_575 ? O11 K1 O11 108.25(11) . 7_575 ? Cl3 K1 O1 70.88(5) . 7_575 ? Cl2 K1 O1 68.11(5) 7_575 7_575 ? Cl2 K1 O1 147.17(8) . 7_575 ? O11 K1 O1 141.36(8) . 7_575 ? O11 K1 O1 53.45(6) 7_575 7_575 ? Cl3 K1 O1 70.88(5) . . ? Cl2 K1 O1 147.17(8) 7_575 . ? Cl2 K1 O1 68.11(5) . . ? O11 K1 O1 53.45(6) . . ? O11 K1 O1 141.36(8) 7_575 . ? O1 K1 O1 116.30(11) 7_575 . ? Cl4 C40 Cl5 110.8(3) . . ? Cl7 C50 Cl6 110.2(3) . . ? Cl9 C60 Cl8 112.6(5) . . ? Cl11 C70 Cl10 111.9(7) . . ? Cl13 C75 Cl12 107.4(13) . . ? Cl14 C80 Cl15 105.0(6) . . ? Cl16 C85 Cl17 106.1(12) . . ? Cl19 C90 Cl18 111.8(12) . . ? Cl20 C95 Cl21 109.9(14) . . ? _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.968 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.096 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 825193' #TrackingRef '- kember et al_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H108 Cl5 Co4 K N8 O4, 8(C H2 Cl2)' _chemical_formula_sum 'C76 H124 Cl21 Co4 K N8 O4' _chemical_formula_weight 2233.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.78965(15) _cell_length_b 31.1301(4) _cell_length_c 27.4398(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.1289(13) _cell_angle_gamma 90.00 _cell_volume 10013.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16761 _cell_measurement_theta_min 2.1509 _cell_measurement_theta_max 72.3392 _exptl_crystal_description blocks _exptl_crystal_colour Pink _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4608 _exptl_absorpt_coefficient_mu 11.008 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.150 _exptl_absorpt_correction_T_max 0.448 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36036 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 72.56 _reflns_number_total 18582 _reflns_number_gt 13181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0823P)^2^+45.4461P] 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 18582 _refine_ls_number_parameters 1054 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.1075 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.2113 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.35443(8) 0.24869(3) 0.20798(3) 0.0273(2) Uani 1 1 d . A . Co2 Co 0.54867(8) 0.28519(3) 0.27025(3) 0.0274(2) Uani 1 1 d . A . Co3 Co 0.35934(8) 0.48989(3) 0.21008(3) 0.0266(2) Uani 1 1 d . A . Co4 Co 0.55129(8) 0.45139(3) 0.27170(3) 0.0267(2) Uani 1 1 d . A . Cl1 Cl 0.52452(13) 0.20329(5) 0.25913(6) 0.0340(3) Uani 1 1 d . . . Cl2 Cl 0.21916(14) 0.29723(5) 0.16691(6) 0.0381(3) Uani 1 1 d . A . Cl3 Cl 0.55412(12) 0.36846(5) 0.27418(5) 0.0320(3) Uani 1 1 d . A . Cl4 Cl 0.52815(13) 0.53372(5) 0.26126(5) 0.0335(3) Uani 1 1 d . . . Cl5 Cl 0.22415(14) 0.44237(5) 0.16768(6) 0.0381(3) Uani 1 1 d . A . O1 O 0.5009(3) 0.28408(13) 0.19393(15) 0.0291(9) Uani 1 1 d . A . C1 C 0.5720(5) 0.27014(19) 0.1612(2) 0.0279(12) Uani 1 1 d . . . C2 C 0.5314(5) 0.2485(2) 0.1182(2) 0.0311(13) Uani 1 1 d . . . C3 C 0.4075(6) 0.2382(2) 0.1062(2) 0.0344(14) Uani 1 1 d . . . H3A H 0.3631 0.2652 0.1031 0.041 Uiso 1 1 calc R . . H3B H 0.3963 0.2231 0.0744 0.041 Uiso 1 1 calc R . . N4 N 0.3644(4) 0.21085(16) 0.14466(17) 0.0273(10) Uani 1 1 d . . . H4A H 0.4182 0.1908 0.1527 0.033 Uiso 1 1 calc R . . C5 C 0.2609(5) 0.1875(2) 0.1237(2) 0.0334(14) Uani 1 1 d . . . H5A H 0.2808 0.1698 0.0959 0.040 Uiso 1 1 calc R . . H5B H 0.2032 0.2088 0.1105 0.040 Uiso 1 1 calc R . . C6 C 0.2074(5) 0.1586(2) 0.1596(2) 0.0330(14) Uani 1 1 d . . . C7 C 0.1506(5) 0.1850(2) 0.1966(2) 0.0314(13) Uani 1 1 d . . . H7A H 0.0997 0.2063 0.1786 0.038 Uiso 1 1 calc R . . H7B H 0.1022 0.1657 0.2142 0.038 Uiso 1 1 calc R . . N8 N 0.2294(4) 0.20829(15) 0.23355(18) 0.0266(10) Uani 1 1 d . . . H8A H 0.2668 0.1882 0.2527 0.032 Uiso 1 1 calc R . . C9 C 0.1613(5) 0.2341(2) 0.2656(2) 0.0312(13) Uani 1 1 d . . . H9A H 0.0913 0.2180 0.2713 0.037 Uiso 1 1 calc R . . H9B H 0.1379 0.2614 0.2490 0.037 Uiso 1 1 calc R . . C10 C 0.2291(5) 0.2434(2) 0.3139(2) 0.0285(13) Uani 1 1 d . . . C11 C 0.3316(5) 0.26653(18) 0.3170(2) 0.0246(12) Uani 1 1 d . . . O11 O 0.3747(3) 0.28115(13) 0.27604(14) 0.0257(8) Uani 1 1 d . . . C12 C 0.3859(5) 0.27573(19) 0.3640(2) 0.0278(12) Uani 1 1 d . . . C13 C 0.4921(5) 0.3023(2) 0.3713(2) 0.0315(13) Uani 1 1 d . . . H13A H 0.5151 0.3058 0.4068 0.038 Uiso 1 1 calc R . . H13B H 0.4765 0.3311 0.3570 0.038 Uiso 1 1 calc R . . N14 N 0.5878(4) 0.28193(17) 0.34789(18) 0.0288(11) Uani 1 1 d . . . H14C H 0.5873 0.2539 0.3558 0.035 Uiso 1 1 calc R . . C15 C 0.6979(5) 0.2991(2) 0.3699(2) 0.0350(14) Uani 1 1 d . . . H15A H 0.7057 0.2929 0.4055 0.042 Uiso 1 1 calc R . . H15B H 0.6969 0.3307 0.3660 0.042 Uiso 1 1 calc R . . C16 C 0.8027(5) 0.2813(2) 0.3482(3) 0.0361(15) Uani 1 1 d . . . C17 C 0.8113(5) 0.2989(2) 0.2979(2) 0.0342(14) Uani 1 1 d . . . H17A H 0.8050 0.3306 0.2992 0.041 Uiso 1 1 calc R . . H17B H 0.8879 0.2920 0.2883 0.041 Uiso 1 1 calc R . . N18 N 0.7238(4) 0.28252(16) 0.25905(17) 0.0273(10) Uani 1 1 d . . . H18A H 0.7400 0.2546 0.2550 0.033 Uiso 1 1 calc R . . C19 C 0.7406(6) 0.3040(2) 0.2120(2) 0.0349(14) Uani 1 1 d . . . H19A H 0.8233 0.3076 0.2097 0.042 Uiso 1 1 calc R . . H19B H 0.7056 0.3329 0.2113 0.042 Uiso 1 1 calc R . . C20 C 0.6892(5) 0.2789(2) 0.1688(2) 0.0301(13) Uani 1 1 d . . . C21 C 0.7625(6) 0.2657(2) 0.1343(2) 0.0325(13) Uani 1 1 d . . . H21A H 0.8416 0.2720 0.1405 0.039 Uiso 1 1 calc R . . C22 C 0.7239(6) 0.2438(2) 0.0918(2) 0.0362(15) Uani 1 1 d . . . C23 C 0.6065(6) 0.2357(2) 0.0847(2) 0.0336(14) Uani 1 1 d . . . H23A H 0.5764 0.2210 0.0559 0.040 Uiso 1 1 calc R . . C24 C 0.8028(6) 0.2305(3) 0.0534(3) 0.0437(17) Uani 1 1 d . . . C25 C 0.7852(9) 0.1839(3) 0.0394(4) 0.078(3) Uani 1 1 d . . . H25A H 0.8363 0.1761 0.0149 0.117 Uiso 1 1 calc R . . H25B H 0.7059 0.1794 0.0258 0.117 Uiso 1 1 calc R . . H25C H 0.8021 0.1659 0.0686 0.117 Uiso 1 1 calc R . . C26 C 0.7764(9) 0.2589(4) 0.0082(3) 0.073(3) Uani 1 1 d . . . H26A H 0.8257 0.2507 -0.0169 0.110 Uiso 1 1 calc R . . H26B H 0.7902 0.2891 0.0172 0.110 Uiso 1 1 calc R . . H26C H 0.6963 0.2552 -0.0049 0.110 Uiso 1 1 calc R . . C27 C 0.9281(7) 0.2371(4) 0.0729(3) 0.070(3) Uani 1 1 d . . . H27A H 0.9768 0.2282 0.0479 0.105 Uiso 1 1 calc R . . H27B H 0.9463 0.2198 0.1025 0.105 Uiso 1 1 calc R . . H27C H 0.9416 0.2675 0.0807 0.105 Uiso 1 1 calc R . . C28 C 0.2938(6) 0.1268(2) 0.1842(3) 0.0397(15) Uani 1 1 d . . . H28A H 0.2566 0.1087 0.2070 0.060 Uiso 1 1 calc R . . H28B H 0.3569 0.1426 0.2023 0.060 Uiso 1 1 calc R . . H28C H 0.3235 0.1088 0.1592 0.060 Uiso 1 1 calc R . . C29 C 0.1118(6) 0.1332(2) 0.1296(3) 0.0431(16) Uani 1 1 d . . . H29A H 0.0552 0.1532 0.1139 0.065 Uiso 1 1 calc R . . H29B H 0.0751 0.1140 0.1515 0.065 Uiso 1 1 calc R . . H29C H 0.1444 0.1162 0.1045 0.065 Uiso 1 1 calc R . . C30 C 0.1868(5) 0.2286(2) 0.3568(2) 0.0302(13) Uani 1 1 d . . . H30A H 0.1175 0.2129 0.3537 0.036 Uiso 1 1 calc R . . C31 C 0.2417(5) 0.23592(19) 0.4037(2) 0.0287(13) Uani 1 1 d . . . C32 C 0.3405(5) 0.2600(2) 0.4059(2) 0.0312(13) Uani 1 1 d . . . H32A H 0.3796 0.2662 0.4372 0.037 Uiso 1 1 calc R . . C33 C 0.1970(6) 0.2172(2) 0.4502(2) 0.0345(14) Uani 1 1 d . . . C34 C 0.2886(7) 0.1874(3) 0.4759(3) 0.061(2) Uani 1 1 d . . . H34A H 0.3041 0.1639 0.4538 0.091 Uiso 1 1 calc R . . H34B H 0.2613 0.1755 0.5056 0.091 Uiso 1 1 calc R . . H34C H 0.3588 0.2037 0.4848 0.091 Uiso 1 1 calc R . . C35 C 0.1754(8) 0.2541(3) 0.4847(3) 0.056(2) Uani 1 1 d . . . H35A H 0.1170 0.2733 0.4686 0.083 Uiso 1 1 calc R . . H35B H 0.2463 0.2702 0.4929 0.083 Uiso 1 1 calc R . . H35C H 0.1492 0.2425 0.5148 0.083 Uiso 1 1 calc R . . C36 C 0.0874(7) 0.1924(3) 0.4390(3) 0.056(2) Uani 1 1 d . . . H36A H 0.0292 0.2112 0.4221 0.083 Uiso 1 1 calc R . . H36B H 0.0612 0.1822 0.4697 0.083 Uiso 1 1 calc R . . H36C H 0.1004 0.1678 0.4181 0.083 Uiso 1 1 calc R . . C37 C 0.8072(6) 0.2324(2) 0.3504(3) 0.0416(16) Uani 1 1 d . . . H37A H 0.8750 0.2223 0.3361 0.062 Uiso 1 1 calc R . . H37B H 0.7387 0.2206 0.3318 0.062 Uiso 1 1 calc R . . H37C H 0.8106 0.2230 0.3846 0.062 Uiso 1 1 calc R . . C38 C 0.9078(6) 0.2998(2) 0.3814(3) 0.0421(16) Uani 1 1 d . . . H38A H 0.9784 0.2899 0.3692 0.063 Uiso 1 1 calc R . . H38B H 0.9054 0.2899 0.4152 0.063 Uiso 1 1 calc R . . H38C H 0.9051 0.3313 0.3806 0.063 Uiso 1 1 calc R . . O41 O 0.3770(3) 0.45632(13) 0.27732(14) 0.0254(8) Uani 1 1 d . . . C41 C 0.3330(5) 0.4707(2) 0.3181(2) 0.0274(12) Uani 1 1 d . . . C42 C 0.2311(5) 0.4942(2) 0.3148(2) 0.0293(13) Uani 1 1 d . . . C43 C 0.1648(5) 0.5044(2) 0.2665(2) 0.0318(13) Uani 1 1 d . . . H43A H 0.1412 0.4773 0.2495 0.038 Uiso 1 1 calc R . . H43B H 0.0950 0.5205 0.2722 0.038 Uiso 1 1 calc R . . N44 N 0.2327(4) 0.53027(16) 0.23491(17) 0.0264(10) Uani 1 1 d . . . H44A H 0.2695 0.5503 0.2542 0.032 Uiso 1 1 calc R . . C45 C 0.1543(5) 0.5535(2) 0.1982(2) 0.0331(14) Uani 1 1 d . . . H45A H 0.1053 0.5727 0.2157 0.040 Uiso 1 1 calc R . . H45B H 0.1039 0.5323 0.1798 0.040 Uiso 1 1 calc R . . C46 C 0.2128(5) 0.5806(2) 0.1611(2) 0.0319(13) Uani 1 1 d . . . C47 C 0.2693(5) 0.5514(2) 0.1259(2) 0.0329(14) Uani 1 1 d . . . H47A H 0.2128 0.5297 0.1126 0.040 Uiso 1 1 calc R . . H47B H 0.2899 0.5689 0.0981 0.040 Uiso 1 1 calc R . . N48 N 0.3732(4) 0.52864(16) 0.14815(17) 0.0280(10) Uani 1 1 d . . . H48A H 0.4264 0.5487 0.1568 0.034 Uiso 1 1 calc R . . C49 C 0.4163(5) 0.5019(2) 0.1091(2) 0.0315(13) Uani 1 1 d . . . H49A H 0.4067 0.5178 0.0777 0.038 Uiso 1 1 calc R . . H49B H 0.3707 0.4752 0.1049 0.038 Uiso 1 1 calc R . . C50 C 0.5402(5) 0.49058(19) 0.1215(2) 0.0290(13) Uani 1 1 d . . . C51 C 0.5778(5) 0.46669(18) 0.1633(2) 0.0244(11) Uani 1 1 d . . . O51 O 0.5050(3) 0.45351(13) 0.19550(14) 0.0288(9) Uani 1 1 d . A . C52 C 0.6944(6) 0.4565(2) 0.1709(2) 0.0310(13) Uani 1 1 d . . . C53 C 0.7426(5) 0.4310(2) 0.2143(2) 0.0309(13) Uani 1 1 d . . . H53A H 0.8250 0.4261 0.2124 0.037 Uiso 1 1 calc R . . H53B H 0.7046 0.4026 0.2138 0.037 Uiso 1 1 calc R . . N54 N 0.7267(4) 0.45351(16) 0.26116(18) 0.0286(11) Uani 1 1 d . . . H54A H 0.7433 0.4813 0.2565 0.034 Uiso 1 1 calc R . . C55 C 0.8130(6) 0.4377(2) 0.3002(2) 0.0371(15) Uani 1 1 d . . . H55A H 0.8896 0.4449 0.2910 0.045 Uiso 1 1 calc R . . H55B H 0.8075 0.4060 0.3015 0.045 Uiso 1 1 calc R . . C56 C 0.8036(5) 0.4552(2) 0.3511(2) 0.0330(14) Uani 1 1 d . . . C57 C 0.6981(5) 0.4382(2) 0.3718(2) 0.0346(14) Uani 1 1 d . . . H57A H 0.6973 0.4065 0.3687 0.041 Uiso 1 1 calc R . . H57B H 0.7042 0.4451 0.4072 0.041 Uiso 1 1 calc R . . N58 N 0.5879(4) 0.45509(17) 0.34855(18) 0.0304(11) Uani 1 1 d . . . H58A H 0.5867 0.4832 0.3562 0.036 Uiso 1 1 calc R . . C59 C 0.4927(5) 0.4350(2) 0.3719(2) 0.0301(13) Uani 1 1 d . . . H59A H 0.5162 0.4311 0.4074 0.036 Uiso 1 1 calc R . . H59B H 0.4766 0.4062 0.3574 0.036 Uiso 1 1 calc R . . C60 C 0.3864(5) 0.4615(2) 0.3653(2) 0.0283(12) Uani 1 1 d . . . C61 C 0.3414(6) 0.4770(2) 0.4066(2) 0.0316(13) Uani 1 1 d . . . H61A H 0.3799 0.4704 0.4379 0.038 Uiso 1 1 calc R . . C62 C 0.2416(5) 0.5019(2) 0.4042(2) 0.0306(13) Uani 1 1 d . . . C63 C 0.1880(5) 0.5093(2) 0.3575(2) 0.0323(13) Uani 1 1 d . . . H63A H 0.1190 0.5253 0.3541 0.039 Uiso 1 1 calc R . . C64 C 0.1991(6) 0.5204(2) 0.4509(2) 0.0355(15) Uani 1 1 d . . . C65 C 0.0895(7) 0.5472(3) 0.4396(3) 0.0492(19) Uani 1 1 d . . . H65A H 0.1046 0.5714 0.4183 0.074 Uiso 1 1 calc R . . H65B H 0.0650 0.5582 0.4703 0.074 Uiso 1 1 calc R . . H65C H 0.0292 0.5291 0.4230 0.074 Uiso 1 1 calc R . . C66 C 0.1719(7) 0.4834(3) 0.4847(3) 0.0470(18) Uani 1 1 d . . . H66A H 0.1134 0.4648 0.4675 0.071 Uiso 1 1 calc R . . H66B H 0.1437 0.4951 0.5143 0.071 Uiso 1 1 calc R . . H66C H 0.2412 0.4666 0.4939 0.071 Uiso 1 1 calc R . . C67 C 0.2902(7) 0.5494(3) 0.4776(3) 0.053(2) Uani 1 1 d . . . H67A H 0.3075 0.5730 0.4559 0.079 Uiso 1 1 calc R . . H67B H 0.3596 0.5327 0.4868 0.079 Uiso 1 1 calc R . . H67C H 0.2619 0.5612 0.5071 0.079 Uiso 1 1 calc R . . C68 C 0.2972(6) 0.6122(2) 0.1871(2) 0.0355(14) Uani 1 1 d . . . H68A H 0.3336 0.6288 0.1627 0.053 Uiso 1 1 calc R . . H68B H 0.3555 0.5964 0.2080 0.053 Uiso 1 1 calc R . . H68C H 0.2568 0.6317 0.2073 0.053 Uiso 1 1 calc R . . C69 C 0.1184(6) 0.6056(2) 0.1306(3) 0.0418(16) Uani 1 1 d . . . H69A H 0.1520 0.6230 0.1061 0.063 Uiso 1 1 calc R . . H69B H 0.0793 0.6243 0.1521 0.063 Uiso 1 1 calc R . . H69C H 0.0636 0.5853 0.1140 0.063 Uiso 1 1 calc R . . C70 C 0.6167(5) 0.5032(2) 0.0892(2) 0.0318(13) Uani 1 1 d . . . H70A H 0.5883 0.5192 0.0611 0.038 Uiso 1 1 calc R . . C71 C 0.7339(6) 0.4937(2) 0.0956(2) 0.0317(13) Uani 1 1 d . . . C72 C 0.7691(5) 0.4702(2) 0.1376(2) 0.0302(13) Uani 1 1 d . . . H72A H 0.8477 0.4630 0.1440 0.036 Uiso 1 1 calc R . . C73 C 0.8139(6) 0.5089(2) 0.0590(2) 0.0390(15) Uani 1 1 d . . . C74 C 0.8148(8) 0.5592(3) 0.0582(4) 0.062(2) Uani 1 1 d . . . H74A H 0.7375 0.5698 0.0483 0.093 Uiso 1 1 calc R . . H74B H 0.8663 0.5693 0.0349 0.093 Uiso 1 1 calc R . . H74C H 0.8411 0.5701 0.0910 0.093 Uiso 1 1 calc R . . C75 C 0.9383(7) 0.4959(3) 0.0745(3) 0.054(2) Uani 1 1 d . . . H75A H 0.9442 0.4645 0.0756 0.082 Uiso 1 1 calc R . . H75B H 0.9627 0.5077 0.1071 0.082 Uiso 1 1 calc R . . H75C H 0.9872 0.5072 0.0508 0.082 Uiso 1 1 calc R . . C76 C 0.7774(8) 0.4911(4) 0.0088(3) 0.076(3) Uani 1 1 d . . . H76A H 0.7773 0.4597 0.0102 0.114 Uiso 1 1 calc R . . H76B H 0.8307 0.5007 -0.0141 0.114 Uiso 1 1 calc R . . H76C H 0.7005 0.5014 -0.0025 0.114 Uiso 1 1 calc R . . C77 C 0.8073(6) 0.5046(2) 0.3514(3) 0.0418(16) Uani 1 1 d . . . H77A H 0.8770 0.5144 0.3383 0.063 Uiso 1 1 calc R . . H77B H 0.8067 0.5151 0.3851 0.063 Uiso 1 1 calc R . . H77C H 0.7405 0.5159 0.3310 0.063 Uiso 1 1 calc R . . C78 C 0.9080(6) 0.4382(3) 0.3847(3) 0.0427(16) Uani 1 1 d . . . H78A H 0.9068 0.4067 0.3848 0.064 Uiso 1 1 calc R . . H78B H 0.9050 0.4488 0.4181 0.064 Uiso 1 1 calc R . . H78C H 0.9784 0.4482 0.3723 0.064 Uiso 1 1 calc R . . K1 K 0.40206(14) 0.36917(5) 0.17493(7) 0.0501(4) Uani 1 1 d . . . C80 C 0.5789(11) 0.3942(5) 0.0476(6) 0.064(3) Uani 0.665(4) 1 d PDU A 1 H80A H 0.6108 0.3853 0.0173 0.077 Uiso 0.665(4) 1 calc PR A 1 H80B H 0.6263 0.4180 0.0626 0.077 Uiso 0.665(4) 1 calc PR A 1 Cl8A Cl 0.5828(4) 0.35122(15) 0.08809(19) 0.0760(13) Uani 0.665(4) 1 d PDU A 1 Cl8B Cl 0.4360(5) 0.41242(16) 0.0329(2) 0.0984(17) Uani 0.665(4) 1 d PDU A 1 C80' C 0.541(2) 0.3962(13) 0.047(3) 0.065(6) Uiso 0.192(6) 1 d PDU A 2 H80C H 0.5535 0.3981 0.0119 0.078 Uiso 0.192(6) 1 calc PR A 2 H80D H 0.5837 0.4197 0.0648 0.078 Uiso 0.192(6) 1 calc PR A 2 Cl8C Cl 0.5890(18) 0.3464(7) 0.0707(8) 0.084(4) Uiso 0.192(6) 1 d PDU A 2 Cl8D Cl 0.3939(14) 0.4012(6) 0.0532(7) 0.082(4) Uiso 0.192(6) 1 d PDU A 2 C80" C 0.494(4) 0.4061(19) 0.023(2) 0.065(6) Uiso 0.143(5) 1 d PDU A 3 H80E H 0.4394 0.4027 -0.0064 0.078 Uiso 0.143(5) 1 calc PR A 3 H80F H 0.5029 0.4371 0.0307 0.078 Uiso 0.143(5) 1 calc PR A 3 Cl8E Cl 0.4437(17) 0.3786(7) 0.0736(7) 0.085(3) Uiso 0.143(5) 1 d PDU A 3 Cl8F Cl 0.627(2) 0.3839(9) 0.0131(9) 0.113(8) Uiso 0.143(5) 1 d PD A 3 C90 C 0.5250(6) 0.0754(2) 0.1175(3) 0.0408(16) Uani 1 1 d . . . H90A H 0.5074 0.0735 0.1519 0.049 Uiso 1 1 calc R . . H90B H 0.5988 0.0609 0.1152 0.049 Uiso 1 1 calc R . . Cl9A Cl 0.53692(16) 0.12954(6) 0.10144(8) 0.0511(4) Uani 1 1 d . . . Cl9B Cl 0.41748(17) 0.04913(6) 0.07918(8) 0.0555(5) Uani 1 1 d . . . C100 C 0.7515(6) 0.1644(2) 0.1904(3) 0.0412(16) Uani 1 1 d . . . H10A H 0.7345 0.1810 0.1597 0.049 Uiso 1 1 calc R . . H10B H 0.6816 0.1637 0.2074 0.049 Uiso 1 1 calc R . . Cl0A Cl 0.86249(15) 0.18975(6) 0.22813(8) 0.0517(4) Uani 1 1 d . . . Cl0B Cl 0.79156(18) 0.11124(6) 0.17630(7) 0.0522(4) Uani 1 1 d . . . C110 C 0.2458(6) 0.0738(2) 0.3057(3) 0.0419(16) Uani 1 1 d . . . H11A H 0.2646 0.0575 0.3365 0.050 Uiso 1 1 calc R . . H11B H 0.3148 0.0747 0.2880 0.050 Uiso 1 1 calc R . . Cl1A Cl 0.20503(19) 0.12667(6) 0.31953(7) 0.0553(5) Uani 1 1 d . . . Cl1B Cl 0.13399(16) 0.04772(6) 0.26901(8) 0.0534(5) Uani 1 1 d . . . C120 C 0.4735(6) 0.1626(2) 0.3809(3) 0.0434(16) Uani 1 1 d . . . H12A H 0.4919 0.1655 0.3467 0.052 Uiso 1 1 calc R . . H12B H 0.4004 0.1776 0.3837 0.052 Uiso 1 1 calc R . . Cl2A Cl 0.58203(18) 0.18642(7) 0.42099(8) 0.0592(5) Uani 1 1 d . . . Cl2B Cl 0.45880(16) 0.10751(6) 0.39511(8) 0.0525(5) Uani 1 1 d . . . C130 C 0.0260(7) 0.3733(3) 0.1082(3) 0.058(2) Uani 1 1 d . . . H13C H 0.0488 0.3991 0.1280 0.069 Uiso 1 1 calc R . . H13D H 0.0649 0.3482 0.1247 0.069 Uiso 1 1 calc R . . Cl3A Cl -0.1210(2) 0.36632(8) 0.10715(12) 0.0831(8) Uani 1 1 d . . . Cl3B Cl 0.0723(4) 0.37898(12) 0.05170(12) 0.1194(13) Uani 1 1 d . . . C140 C 0.1800(7) 0.3690(3) 0.2681(3) 0.055(2) Uani 1 1 d . . . H14A H 0.2188 0.3434 0.2563 0.066 Uiso 1 1 calc R . . H14B H 0.2179 0.3948 0.2564 0.066 Uiso 1 1 calc R . . Cl4A Cl 0.0363(2) 0.36869(11) 0.24290(11) 0.0865(8) Uani 1 1 d . . . Cl4B Cl 0.1950(3) 0.36892(10) 0.33183(9) 0.0994(10) Uani 1 1 d . . . C150 C 0.2091(14) 0.3666(4) 0.4497(4) 0.108(5) Uani 1 1 d . . . H15C H 0.2033 0.3925 0.4285 0.129 Uiso 1 1 calc R . . H15D H 0.2005 0.3411 0.4282 0.129 Uiso 1 1 calc R . . Cl5A Cl 0.0986(4) 0.36735(10) 0.48731(15) 0.1157(12) Uani 1 1 d . . . Cl5B Cl 0.3475(4) 0.36551(11) 0.48412(14) 0.1168(12) 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 Co1 0.0298(5) 0.0290(5) 0.0234(5) -0.0011(4) 0.0048(4) -0.0005(4) Co2 0.0263(5) 0.0330(5) 0.0231(4) 0.0012(4) 0.0042(4) 0.0016(4) Co3 0.0290(5) 0.0290(5) 0.0219(4) 0.0018(4) 0.0041(4) 0.0006(4) Co4 0.0269(5) 0.0318(5) 0.0217(4) -0.0001(4) 0.0035(4) 0.0005(4) Cl1 0.0366(7) 0.0304(7) 0.0358(7) 0.0005(6) 0.0071(6) 0.0030(6) Cl2 0.0417(8) 0.0336(8) 0.0383(8) 0.0017(7) 0.0013(7) 0.0049(6) Cl3 0.0389(7) 0.0263(7) 0.0317(7) 0.0002(6) 0.0084(6) 0.0015(6) Cl4 0.0382(8) 0.0310(7) 0.0315(7) -0.0022(6) 0.0056(6) -0.0046(6) Cl5 0.0405(8) 0.0362(8) 0.0368(8) -0.0009(7) 0.0001(7) -0.0056(7) O1 0.028(2) 0.034(2) 0.026(2) -0.0017(17) 0.0062(17) -0.0021(17) C1 0.033(3) 0.028(3) 0.024(3) 0.002(2) 0.005(2) 0.001(2) C2 0.037(3) 0.033(3) 0.024(3) 0.004(2) 0.008(3) -0.001(3) C3 0.039(3) 0.041(4) 0.024(3) 0.000(3) 0.006(3) -0.002(3) N4 0.032(3) 0.028(3) 0.021(2) 0.002(2) 0.001(2) 0.002(2) C5 0.036(3) 0.038(4) 0.025(3) -0.003(3) 0.000(3) -0.005(3) C6 0.032(3) 0.034(3) 0.032(3) 0.000(3) 0.003(3) -0.004(3) C7 0.027(3) 0.037(3) 0.030(3) -0.005(3) 0.003(2) -0.001(3) N8 0.031(3) 0.022(2) 0.026(2) 0.000(2) 0.002(2) 0.001(2) C9 0.027(3) 0.039(4) 0.028(3) -0.001(3) 0.005(2) 0.002(3) C10 0.030(3) 0.034(3) 0.023(3) 0.005(2) 0.009(2) 0.005(3) C11 0.027(3) 0.025(3) 0.023(3) -0.005(2) 0.008(2) 0.006(2) O11 0.029(2) 0.027(2) 0.0218(19) -0.0025(16) 0.0058(16) -0.0007(16) C12 0.030(3) 0.028(3) 0.026(3) -0.002(2) 0.006(2) 0.002(2) C13 0.037(3) 0.031(3) 0.027(3) -0.003(3) 0.007(3) -0.002(3) N14 0.025(2) 0.029(3) 0.031(3) 0.000(2) -0.002(2) 0.000(2) C15 0.037(3) 0.038(4) 0.029(3) 0.000(3) -0.002(3) 0.000(3) C16 0.030(3) 0.036(4) 0.042(4) 0.008(3) 0.005(3) 0.000(3) C17 0.034(3) 0.034(3) 0.036(3) -0.001(3) 0.007(3) -0.003(3) N18 0.026(2) 0.028(3) 0.026(2) -0.004(2) -0.004(2) 0.002(2) C19 0.035(3) 0.039(4) 0.032(3) 0.004(3) 0.005(3) -0.004(3) C20 0.035(3) 0.032(3) 0.025(3) 0.003(2) 0.007(2) 0.002(3) C21 0.035(3) 0.033(3) 0.031(3) 0.000(3) 0.010(3) 0.002(3) C22 0.041(4) 0.038(4) 0.030(3) 0.002(3) 0.010(3) 0.003(3) C23 0.047(4) 0.033(3) 0.022(3) -0.002(3) 0.009(3) 0.000(3) C24 0.048(4) 0.051(4) 0.035(4) -0.003(3) 0.016(3) 0.000(3) C25 0.088(7) 0.056(6) 0.098(8) -0.023(5) 0.057(6) -0.004(5) C26 0.095(7) 0.091(7) 0.039(4) 0.006(5) 0.033(5) 0.013(6) C27 0.050(5) 0.106(8) 0.057(5) -0.025(5) 0.020(4) 0.011(5) C28 0.044(4) 0.036(4) 0.041(4) 0.001(3) 0.011(3) -0.001(3) C29 0.040(4) 0.047(4) 0.041(4) -0.009(3) 0.001(3) -0.008(3) C30 0.034(3) 0.029(3) 0.028(3) -0.001(3) 0.010(3) 0.004(3) C31 0.035(3) 0.026(3) 0.026(3) -0.002(2) 0.012(2) 0.003(2) C32 0.035(3) 0.030(3) 0.029(3) 0.000(3) 0.006(3) 0.003(3) C33 0.037(3) 0.040(4) 0.028(3) 0.003(3) 0.011(3) 0.002(3) C34 0.057(5) 0.064(5) 0.063(5) 0.040(5) 0.017(4) 0.012(4) C35 0.066(5) 0.063(5) 0.040(4) 0.000(4) 0.021(4) 0.000(4) C36 0.053(5) 0.070(6) 0.045(4) 0.009(4) 0.010(4) -0.016(4) C37 0.045(4) 0.036(4) 0.043(4) 0.004(3) -0.001(3) 0.002(3) C38 0.031(3) 0.050(4) 0.043(4) -0.001(3) -0.006(3) -0.002(3) O41 0.025(2) 0.032(2) 0.0197(18) 0.0006(16) 0.0029(15) 0.0003(16) C41 0.034(3) 0.031(3) 0.018(3) 0.001(2) 0.008(2) -0.002(2) C42 0.030(3) 0.033(3) 0.025(3) 0.003(2) 0.005(2) -0.003(3) C43 0.026(3) 0.041(4) 0.028(3) 0.002(3) 0.007(2) -0.001(3) N44 0.026(2) 0.029(3) 0.024(2) 0.000(2) 0.0027(19) -0.002(2) C45 0.024(3) 0.043(4) 0.032(3) 0.005(3) 0.001(2) 0.002(3) C46 0.033(3) 0.032(3) 0.031(3) 0.000(3) 0.003(3) -0.001(3) C47 0.027(3) 0.040(4) 0.030(3) 0.009(3) -0.005(2) 0.003(3) N48 0.030(3) 0.030(3) 0.024(2) -0.003(2) 0.002(2) 0.001(2) C49 0.038(3) 0.036(3) 0.020(3) 0.001(2) 0.001(2) 0.003(3) C50 0.036(3) 0.029(3) 0.022(3) -0.010(2) 0.002(2) -0.001(3) C51 0.031(3) 0.023(3) 0.020(3) 0.003(2) 0.004(2) 0.000(2) O51 0.026(2) 0.037(2) 0.024(2) 0.0013(17) 0.0047(16) -0.0032(17) C52 0.038(3) 0.029(3) 0.026(3) -0.002(2) 0.002(3) 0.002(3) C53 0.034(3) 0.030(3) 0.029(3) -0.002(3) 0.006(3) 0.006(3) N54 0.028(3) 0.030(3) 0.028(2) 0.003(2) -0.001(2) 0.003(2) C55 0.031(3) 0.041(4) 0.038(4) -0.004(3) 0.002(3) 0.002(3) C56 0.033(3) 0.033(3) 0.032(3) 0.007(3) -0.002(3) -0.001(3) C57 0.036(3) 0.037(4) 0.029(3) 0.003(3) -0.005(3) 0.000(3) N58 0.028(3) 0.033(3) 0.029(3) 0.005(2) 0.002(2) 0.004(2) C59 0.037(3) 0.030(3) 0.024(3) 0.003(2) 0.006(2) 0.001(3) C60 0.033(3) 0.028(3) 0.025(3) 0.001(2) 0.008(2) -0.001(2) C61 0.040(3) 0.037(3) 0.018(3) 0.001(2) 0.007(2) -0.001(3) C62 0.032(3) 0.040(4) 0.021(3) -0.002(3) 0.011(2) -0.004(3) C63 0.032(3) 0.034(3) 0.033(3) -0.002(3) 0.014(3) 0.001(3) C64 0.038(4) 0.044(4) 0.026(3) -0.005(3) 0.014(3) 0.000(3) C65 0.053(4) 0.061(5) 0.036(4) 0.000(3) 0.018(3) 0.015(4) C66 0.056(4) 0.059(5) 0.029(3) 0.006(3) 0.016(3) 0.005(4) C67 0.053(5) 0.068(5) 0.038(4) -0.016(4) 0.012(3) -0.010(4) C68 0.037(3) 0.032(3) 0.038(3) -0.001(3) 0.004(3) -0.003(3) C69 0.045(4) 0.042(4) 0.038(4) 0.002(3) 0.003(3) 0.008(3) C70 0.040(3) 0.033(3) 0.021(3) -0.001(2) 0.001(3) -0.001(3) C71 0.040(3) 0.031(3) 0.026(3) -0.005(3) 0.010(3) -0.002(3) C72 0.032(3) 0.031(3) 0.029(3) -0.007(3) 0.008(2) 0.002(3) C73 0.039(4) 0.049(4) 0.032(3) 0.005(3) 0.014(3) 0.004(3) C74 0.065(6) 0.060(5) 0.066(6) 0.011(4) 0.028(5) 0.000(4) C75 0.043(4) 0.067(5) 0.055(5) 0.010(4) 0.015(4) 0.001(4) C76 0.068(6) 0.134(10) 0.029(4) -0.017(5) 0.019(4) -0.032(6) C77 0.043(4) 0.038(4) 0.043(4) 0.001(3) -0.003(3) -0.004(3) C78 0.035(4) 0.055(4) 0.037(4) -0.001(3) -0.006(3) 0.003(3) K1 0.0501(9) 0.0353(8) 0.0627(10) 0.0007(8) -0.0035(7) -0.0005(7) C80 0.066(6) 0.054(5) 0.073(6) -0.006(5) 0.015(6) 0.007(5) Cl8A 0.091(3) 0.057(2) 0.083(3) 0.025(2) 0.022(2) 0.0226(18) Cl8B 0.109(3) 0.076(3) 0.099(3) -0.033(2) -0.043(3) 0.035(3) C90 0.039(4) 0.034(4) 0.047(4) -0.005(3) -0.001(3) 0.004(3) Cl9A 0.0515(10) 0.0372(9) 0.0660(11) 0.0053(9) 0.0128(8) 0.0020(8) Cl9B 0.0515(11) 0.0488(11) 0.0638(12) 0.0130(9) -0.0041(9) -0.0074(8) C100 0.051(4) 0.033(4) 0.040(4) -0.005(3) 0.004(3) 0.007(3) Cl0A 0.0391(9) 0.0489(10) 0.0669(12) -0.0087(9) 0.0055(8) 0.0026(8) Cl0B 0.0706(12) 0.0360(9) 0.0505(10) -0.0028(8) 0.0084(9) 0.0076(9) C110 0.049(4) 0.036(4) 0.041(4) -0.001(3) 0.005(3) 0.006(3) Cl1A 0.0780(13) 0.0380(9) 0.0508(10) 0.0031(8) 0.0113(9) 0.0124(9) Cl1B 0.0406(9) 0.0521(11) 0.0670(12) -0.0076(9) 0.0030(8) 0.0038(8) C120 0.043(4) 0.035(4) 0.052(4) 0.006(3) 0.007(3) 0.000(3) Cl2A 0.0546(11) 0.0496(11) 0.0722(13) 0.0029(10) 0.0014(10) -0.0071(9) Cl2B 0.0549(10) 0.0328(9) 0.0722(12) -0.0001(9) 0.0186(9) 0.0010(8) C130 0.048(4) 0.063(5) 0.059(5) 0.005(4) -0.008(4) 0.000(4) Cl3A 0.0553(12) 0.0586(13) 0.133(2) 0.0022(15) -0.0006(13) -0.0047(11) Cl3B 0.172(4) 0.118(3) 0.0784(19) -0.0183(18) 0.061(2) 0.010(2) C140 0.068(5) 0.046(4) 0.055(5) 0.003(4) 0.023(4) 0.001(4) Cl4A 0.0547(12) 0.113(2) 0.0950(19) 0.0032(17) 0.0204(12) 0.0041(14) Cl4B 0.167(3) 0.0823(18) 0.0497(12) 0.0021(13) 0.0157(16) -0.004(2) C150 0.193(15) 0.062(7) 0.062(6) -0.004(6) -0.016(8) -0.005(8) Cl5A 0.168(4) 0.0666(17) 0.117(3) -0.0025(18) 0.035(2) 0.009(2) Cl5B 0.162(3) 0.0732(19) 0.112(3) -0.0151(18) 0.000(2) -0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.113(5) . ? Co1 N8 2.113(5) . ? Co1 O11 2.114(4) . ? Co1 O1 2.118(4) . ? Co1 Cl2 2.3903(18) . ? Co1 Cl1 2.7179(18) . ? Co1 Co2 2.9358(14) . ? Co2 O11 2.077(4) . ? Co2 O1 2.110(4) . ? Co2 N18 2.122(5) . ? Co2 N14 2.134(5) . ? Co2 Cl1 2.5799(18) . ? Co2 Cl3 2.5948(18) . ? Co3 N48 2.105(5) . ? Co3 O41 2.111(4) . ? Co3 N44 2.119(5) . ? Co3 O51 2.130(4) . ? Co3 Cl5 2.3848(18) . ? Co3 Cl4 2.6828(18) . ? Co3 Co4 2.9325(14) . ? Co4 O41 2.083(4) . ? Co4 O51 2.105(4) . ? Co4 N58 2.110(5) . ? Co4 N54 2.120(5) . ? Co4 Cl3 2.5828(18) . ? Co4 Cl4 2.5900(18) . ? Cl2 K1 3.100(2) . ? Cl3 K1 3.097(2) . ? Cl5 K1 3.089(2) . ? O1 C1 1.364(7) . ? O1 K1 2.918(5) . ? C1 C2 1.397(9) . ? C1 C20 1.402(9) . ? C2 C23 1.400(9) . ? C2 C3 1.497(9) . ? C3 N4 1.486(8) . ? N4 C5 1.483(8) . ? C5 C6 1.519(9) . ? C6 C7 1.518(9) . ? C6 C28 1.526(9) . ? C6 C29 1.540(9) . ? C7 N8 1.487(8) . ? N8 C9 1.487(8) . ? C9 C10 1.501(8) . ? C10 C11 1.400(8) . ? C10 C30 1.405(8) . ? C11 O11 1.362(7) . ? C11 C12 1.406(8) . ? C12 C32 1.407(8) . ? C12 C13 1.495(9) . ? C13 N14 1.497(8) . ? N14 C15 1.472(8) . ? C15 C16 1.532(9) . ? C16 C17 1.499(9) . ? C16 C37 1.523(10) . ? C16 C38 1.567(9) . ? C17 N18 1.491(8) . ? N18 C19 1.486(8) . ? C19 C20 1.492(9) . ? C20 C21 1.409(9) . ? C21 C22 1.386(9) . ? C22 C23 1.400(10) . ? C22 C24 1.536(9) . ? C24 C25 1.510(12) . ? C24 C26 1.527(12) . ? C24 C27 1.531(12) . ? C30 C31 1.395(9) . ? C31 C32 1.382(9) . ? C31 C33 1.546(8) . ? C33 C36 1.508(10) . ? C33 C35 1.529(10) . ? C33 C34 1.538(10) . ? O41 C41 1.359(7) . ? C41 C42 1.402(9) . ? C41 C60 1.407(8) . ? C42 C63 1.406(8) . ? C42 C43 1.498(8) . ? C43 N44 1.479(8) . ? N44 C45 1.482(8) . ? C45 C46 1.540(9) . ? C46 C68 1.520(9) . ? C46 C47 1.530(9) . ? C46 C69 1.532(9) . ? C47 N48 1.489(7) . ? N48 C49 1.487(8) . ? C49 C50 1.506(9) . ? C50 C70 1.387(9) . ? C50 C51 1.399(8) . ? C51 O51 1.360(7) . ? C51 C52 1.405(9) . ? O51 K1 2.922(4) . ? C52 C72 1.402(9) . ? C52 C53 1.491(9) . ? C53 N54 1.494(8) . ? N54 C55 1.480(8) . ? C55 C56 1.515(9) . ? C56 C57 1.517(9) . ? C56 C77 1.539(9) . ? C56 C78 1.551(9) . ? C57 N58 1.481(8) . ? N58 C59 1.488(8) . ? C59 C60 1.496(9) . ? C60 C61 1.387(8) . ? C61 C62 1.405(9) . ? C62 C63 1.386(9) . ? C62 C64 1.537(8) . ? C64 C67 1.530(10) . ? C64 C66 1.534(10) . ? C64 C65 1.542(10) . ? C70 C71 1.406(9) . ? C71 C72 1.390(9) . ? C71 C73 1.526(9) . ? C73 C76 1.503(10) . ? C73 C75 1.536(10) . ? C73 C74 1.568(11) . ? K1 Cl8E 2.890(19) . ? K1 Cl8A 3.408(5) . ? K1 Cl8D 3.479(18) . ? C80 Cl8A 1.737(11) . ? C80 Cl8B 1.781(11) . ? C80' Cl8C 1.752(18) . ? C80' Cl8D 1.766(17) . ? C80" Cl8F 1.761(18) . ? C80" Cl8E 1.780(18) . ? C90 Cl9A 1.750(7) . ? C90 Cl9B 1.760(7) . ? C100 Cl0A 1.766(7) . ? C100 Cl0B 1.775(7) . ? C110 Cl1A 1.766(7) . ? C110 Cl1B 1.769(8) . ? C120 Cl2A 1.760(8) . ? C120 Cl2B 1.770(7) . ? C130 Cl3B 1.706(9) . ? C130 Cl3A 1.744(8) . ? C140 Cl4B 1.740(9) . ? C140 Cl4A 1.759(9) . ? C150 Cl5A 1.746(16) . ? C150 Cl5B 1.796(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N8 92.48(19) . . ? N4 Co1 O11 169.06(18) . . ? N8 Co1 O11 90.48(17) . . ? N4 Co1 O1 91.28(18) . . ? N8 Co1 O1 168.78(18) . . ? O11 Co1 O1 83.95(16) . . ? N4 Co1 Cl2 93.30(14) . . ? N8 Co1 Cl2 94.53(14) . . ? O11 Co1 Cl2 96.96(12) . . ? O1 Co1 Cl2 95.81(13) . . ? N4 Co1 Cl1 91.84(14) . . ? N8 Co1 Cl1 91.23(14) . . ? O11 Co1 Cl1 77.57(12) . . ? O1 Co1 Cl1 78.09(12) . . ? Cl2 Co1 Cl1 172.11(7) . . ? N4 Co1 Co2 125.88(14) . . ? N8 Co1 Co2 124.43(14) . . ? O11 Co1 Co2 45.03(11) . . ? O1 Co1 Co2 45.91(11) . . ? Cl2 Co1 Co2 117.99(6) . . ? Cl1 Co1 Co2 54.13(4) . . ? N4 Co1 K1 108.77(14) . . ? N8 Co1 K1 140.32(14) . . ? O11 Co1 K1 75.00(11) . . ? O1 Co1 K1 47.11(12) . . ? Cl2 Co1 K1 52.39(5) . . ? Cl1 Co1 K1 120.12(5) . . ? Co2 Co1 K1 69.00(4) . . ? O11 Co2 O1 85.06(15) . . ? O11 Co2 N18 173.08(18) . . ? O1 Co2 N18 90.94(17) . . ? O11 Co2 N14 91.76(17) . . ? O1 Co2 N14 175.29(18) . . ? N18 Co2 N14 91.87(19) . . ? O11 Co2 Cl1 81.48(12) . . ? O1 Co2 Cl1 81.49(12) . . ? N18 Co2 Cl1 92.35(14) . . ? N14 Co2 Cl1 94.61(15) . . ? O11 Co2 Cl3 94.45(12) . . ? O1 Co2 Cl3 93.47(12) . . ? N18 Co2 Cl3 91.43(14) . . ? N14 Co2 Cl3 90.24(15) . . ? Cl1 Co2 Cl3 173.74(6) . . ? O11 Co2 Co1 46.06(11) . . ? O1 Co2 Co1 46.14(11) . . ? N18 Co2 Co1 127.69(14) . . ? N14 Co2 Co1 129.41(14) . . ? Cl1 Co2 Co1 58.62(4) . . ? Cl3 Co2 Co1 115.16(5) . . ? O11 Co2 K1 74.09(11) . . ? O1 Co2 K1 45.91(12) . . ? N18 Co2 K1 107.04(14) . . ? N14 Co2 K1 136.32(14) . . ? Cl1 Co2 K1 122.63(5) . . ? Cl3 Co2 K1 51.35(4) . . ? Co1 Co2 K1 67.23(4) . . ? N48 Co3 O41 168.66(18) . . ? N48 Co3 N44 92.18(19) . . ? O41 Co3 N44 91.12(17) . . ? N48 Co3 O51 91.10(18) . . ? O41 Co3 O51 83.97(15) . . ? N44 Co3 O51 170.22(18) . . ? N48 Co3 Cl5 93.85(15) . . ? O41 Co3 Cl5 96.75(12) . . ? N44 Co3 Cl5 93.89(14) . . ? O51 Co3 Cl5 95.08(12) . . ? N48 Co3 Cl4 90.80(14) . . ? O41 Co3 Cl4 78.23(11) . . ? N44 Co3 Cl4 92.22(14) . . ? O51 Co3 Cl4 78.52(12) . . ? Cl5 Co3 Cl4 172.18(7) . . ? N48 Co3 Co4 125.31(14) . . ? O41 Co3 Co4 45.25(11) . . ? N44 Co3 Co4 125.72(14) . . ? O51 Co3 Co4 45.82(11) . . ? Cl5 Co3 Co4 117.53(6) . . ? Cl4 Co3 Co4 54.72(4) . . ? N48 Co3 K1 109.09(14) . . ? O41 Co3 K1 74.79(11) . . ? N44 Co3 K1 139.48(14) . . ? O51 Co3 K1 46.98(11) . . ? Cl5 Co3 K1 51.89(5) . . ? Cl4 Co3 K1 120.53(5) . . ? Co4 Co3 K1 68.84(4) . . ? O41 Co4 O51 85.29(15) . . ? O41 Co4 N58 91.15(17) . . ? O51 Co4 N58 174.12(19) . . ? O41 Co4 N54 173.01(18) . . ? O51 Co4 N54 90.97(18) . . ? N58 Co4 N54 92.08(19) . . ? O41 Co4 Cl3 94.69(12) . . ? O51 Co4 Cl3 93.37(12) . . ? N58 Co4 Cl3 91.58(15) . . ? N54 Co4 Cl3 91.41(15) . . ? O41 Co4 Cl4 80.92(12) . . ? O51 Co4 Cl4 81.15(12) . . ? N58 Co4 Cl4 93.69(15) . . ? N54 Co4 Cl4 92.69(15) . . ? Cl3 Co4 Cl4 173.20(6) . . ? O41 Co4 Co3 46.03(11) . . ? O51 Co4 Co3 46.54(12) . . ? N58 Co4 Co3 128.08(14) . . ? N54 Co4 Co3 127.79(14) . . ? Cl3 Co4 Co3 115.52(5) . . ? Cl4 Co4 Co3 57.73(4) . . ? O41 Co4 K1 74.11(11) . . ? O51 Co4 K1 45.97(12) . . ? N58 Co4 K1 137.21(15) . . ? N54 Co4 K1 107.37(14) . . ? Cl3 Co4 K1 51.36(4) . . ? Cl4 Co4 K1 122.08(5) . . ? Co3 Co4 K1 67.51(4) . . ? Co2 Cl1 Co1 67.25(5) . . ? Co1 Cl2 K1 89.96(6) . . ? Co4 Cl3 Co2 175.75(7) . . ? Co4 Cl3 K1 87.99(6) . . ? Co2 Cl3 K1 87.77(6) . . ? Co4 Cl4 Co3 67.55(5) . . ? Co3 Cl5 K1 90.71(6) . . ? C1 O1 Co2 122.8(4) . . ? C1 O1 Co1 121.7(4) . . ? Co2 O1 Co1 87.95(16) . . ? C1 O1 K1 115.6(3) . . ? Co2 O1 K1 102.80(16) . . ? Co1 O1 K1 100.77(15) . . ? O1 C1 C2 122.0(5) . . ? O1 C1 C20 120.3(5) . . ? C2 C1 C20 117.6(6) . . ? C1 C2 C23 120.4(6) . . ? C1 C2 C3 121.8(6) . . ? C23 C2 C3 117.7(6) . . ? N4 C3 C2 111.5(5) . . ? C5 N4 C3 109.6(5) . . ? C5 N4 Co1 118.4(4) . . ? C3 N4 Co1 108.5(4) . . ? N4 C5 C6 114.8(5) . . ? C7 C6 C5 110.9(5) . . ? C7 C6 C28 112.1(5) . . ? C5 C6 C28 111.6(5) . . ? C7 C6 C29 106.6(5) . . ? C5 C6 C29 106.8(5) . . ? C28 C6 C29 108.6(6) . . ? N8 C7 C6 115.6(5) . . ? C7 N8 C9 109.1(5) . . ? C7 N8 Co1 118.1(4) . . ? C9 N8 Co1 108.4(4) . . ? N8 C9 C10 110.9(5) . . ? C11 C10 C30 119.8(6) . . ? C11 C10 C9 122.0(5) . . ? C30 C10 C9 118.2(6) . . ? O11 C11 C10 121.1(5) . . ? O11 C11 C12 121.0(5) . . ? C10 C11 C12 117.9(5) . . ? C11 O11 Co2 122.9(3) . . ? C11 O11 Co1 123.6(3) . . ? Co2 O11 Co1 88.91(15) . . ? C11 C12 C32 120.1(6) . . ? C11 C12 C13 121.9(5) . . ? C32 C12 C13 118.0(5) . . ? C12 C13 N14 111.6(5) . . ? C15 N14 C13 110.0(5) . . ? C15 N14 Co2 118.7(4) . . ? C13 N14 Co2 108.4(4) . . ? N14 C15 C16 114.9(5) . . ? C17 C16 C37 113.3(6) . . ? C17 C16 C15 111.3(5) . . ? C37 C16 C15 111.9(6) . . ? C17 C16 C38 105.9(5) . . ? C37 C16 C38 108.9(6) . . ? C15 C16 C38 105.1(6) . . ? N18 C17 C16 115.1(5) . . ? C19 N18 C17 108.8(5) . . ? C19 N18 Co2 109.3(4) . . ? C17 N18 Co2 119.5(4) . . ? N18 C19 C20 112.0(5) . . ? C1 C20 C21 120.6(6) . . ? C1 C20 C19 122.1(5) . . ? C21 C20 C19 117.3(6) . . ? C22 C21 C20 122.6(6) . . ? C21 C22 C23 115.9(6) . . ? C21 C22 C24 122.8(6) . . ? C23 C22 C24 121.3(6) . . ? C22 C23 C2 122.9(6) . . ? C25 C24 C26 109.9(8) . . ? C25 C24 C27 108.5(8) . . ? C26 C24 C27 108.2(8) . . ? C25 C24 C22 110.8(6) . . ? C26 C24 C22 108.5(6) . . ? C27 C24 C22 110.9(6) . . ? C31 C30 C10 123.3(6) . . ? C32 C31 C30 115.8(6) . . ? C32 C31 C33 121.9(6) . . ? C30 C31 C33 122.3(6) . . ? C31 C32 C12 123.0(6) . . ? C36 C33 C35 108.3(6) . . ? C36 C33 C34 109.3(7) . . ? C35 C33 C34 108.9(7) . . ? C36 C33 C31 112.7(6) . . ? C35 C33 C31 108.8(6) . . ? C34 C33 C31 108.8(5) . . ? C41 O41 Co4 123.5(3) . . ? C41 O41 Co3 123.2(4) . . ? Co4 O41 Co3 88.71(15) . . ? O41 C41 C42 121.2(5) . . ? O41 C41 C60 121.2(5) . . ? C42 C41 C60 117.6(5) . . ? C41 C42 C63 120.2(6) . . ? C41 C42 C43 122.1(5) . . ? C63 C42 C43 117.7(6) . . ? N44 C43 C42 111.7(5) . . ? C43 N44 C45 109.1(5) . . ? C43 N44 Co3 108.0(4) . . ? C45 N44 Co3 118.7(4) . . ? N44 C45 C46 115.2(5) . . ? C68 C46 C47 111.9(5) . . ? C68 C46 C69 109.2(5) . . ? C47 C46 C69 107.2(5) . . ? C68 C46 C45 111.2(5) . . ? C47 C46 C45 110.3(5) . . ? C69 C46 C45 106.7(5) . . ? N48 C47 C46 114.8(5) . . ? C49 N48 C47 107.5(5) . . ? C49 N48 Co3 108.8(4) . . ? C47 N48 Co3 118.1(4) . . ? N48 C49 C50 111.6(5) . . ? C70 C50 C51 120.2(6) . . ? C70 C50 C49 118.2(5) . . ? C51 C50 C49 121.6(5) . . ? O51 C51 C50 121.8(5) . . ? O51 C51 C52 120.7(5) . . ? C50 C51 C52 117.5(5) . . ? C51 O51 Co4 122.7(3) . . ? C51 O51 Co3 122.6(4) . . ? Co4 O51 Co3 87.64(15) . . ? C51 O51 K1 115.1(3) . . ? Co4 O51 K1 102.83(16) . . ? Co3 O51 K1 100.81(15) . . ? C72 C52 C51 120.4(6) . . ? C72 C52 C53 118.0(6) . . ? C51 C52 C53 121.5(5) . . ? C52 C53 N54 111.4(5) . . ? C55 N54 C53 109.1(5) . . ? C55 N54 Co4 119.7(4) . . ? C53 N54 Co4 108.5(4) . . ? N54 C55 C56 115.9(5) . . ? C55 C56 C57 111.3(5) . . ? C55 C56 C77 111.0(6) . . ? C57 C56 C77 111.8(6) . . ? C55 C56 C78 107.0(5) . . ? C57 C56 C78 106.8(5) . . ? C77 C56 C78 108.6(6) . . ? N58 C57 C56 115.5(5) . . ? C57 N58 C59 109.4(5) . . ? C57 N58 Co4 119.2(4) . . ? C59 N58 Co4 108.9(4) . . ? N58 C59 C60 112.1(5) . . ? C61 C60 C41 120.5(6) . . ? C61 C60 C59 118.8(5) . . ? C41 C60 C59 120.7(5) . . ? C60 C61 C62 123.0(6) . . ? C63 C62 C61 115.5(5) . . ? C63 C62 C64 123.5(6) . . ? C61 C62 C64 120.9(5) . . ? C62 C63 C42 123.1(6) . . ? C67 C64 C66 109.6(6) . . ? C67 C64 C62 110.2(5) . . ? C66 C64 C62 109.3(6) . . ? C67 C64 C65 107.9(6) . . ? C66 C64 C65 107.7(6) . . ? C62 C64 C65 112.1(6) . . ? C50 C70 C71 123.9(6) . . ? C72 C71 C70 114.7(6) . . ? C72 C71 C73 124.0(6) . . ? C70 C71 C73 121.3(6) . . ? C71 C72 C52 123.2(6) . . ? C76 C73 C71 110.7(6) . . ? C76 C73 C75 109.2(7) . . ? C71 C73 C75 112.0(6) . . ? C76 C73 C74 110.9(7) . . ? C71 C73 C74 109.0(6) . . ? C75 C73 C74 105.0(7) . . ? Cl8E K1 O1 99.1(4) . . ? Cl8E K1 O51 89.1(4) . . ? O1 K1 O51 129.15(12) . . ? Cl8E K1 Cl5 92.7(4) . . ? O1 K1 Cl5 159.47(11) . . ? O51 K1 Cl5 67.34(9) . . ? Cl8E K1 Cl3 134.8(4) . . ? O1 K1 Cl3 69.74(9) . . ? O51 K1 Cl3 69.33(9) . . ? Cl5 K1 Cl3 112.79(7) . . ? Cl8E K1 Cl2 101.2(4) . . ? O1 K1 Cl2 67.57(9) . . ? O51 K1 Cl2 159.08(11) . . ? Cl5 K1 Cl2 93.78(6) . . ? Cl3 K1 Cl2 112.97(7) . . ? Cl8E K1 Cl8A 33.0(4) . . ? O1 K1 Cl8A 73.05(11) . . ? O51 K1 Cl8A 90.26(13) . . ? Cl5 K1 Cl8A 123.16(9) . . ? Cl3 K1 Cl8A 105.50(10) . . ? Cl2 K1 Cl8A 108.31(11) . . ? Cl8E K1 Cl8D 15.6(4) . . ? O1 K1 Cl8D 113.7(3) . . ? O51 K1 Cl8D 84.0(3) . . ? Cl5 K1 Cl8D 77.1(3) . . ? Cl3 K1 Cl8D 143.2(3) . . ? Cl2 K1 Cl8D 101.0(3) . . ? Cl8A K1 Cl8D 48.0(3) . . ? Cl8E K1 Co1 111.3(4) . . ? O1 K1 Co1 32.12(8) . . ? O51 K1 Co1 152.04(10) . . ? Cl5 K1 Co1 127.49(6) . . ? Cl3 K1 Co1 82.72(5) . . ? Cl2 K1 Co1 37.65(4) . . ? Cl8A K1 Co1 96.94(9) . . ? Cl8D K1 Co1 120.5(3) . . ? Cl8E K1 Co3 100.3(4) . . ? O1 K1 Co3 152.16(10) . . ? O51 K1 Co3 32.21(8) . . ? Cl5 K1 Co3 37.40(4) . . ? Cl3 K1 Co3 82.42(5) . . ? Cl2 K1 Co3 127.04(6) . . ? Cl8A K1 Co3 115.78(10) . . ? Cl8D K1 Co3 88.3(3) . . ? Co1 K1 Co3 146.64(5) . . ? Cl8E K1 Co2 126.5(4) . . ? O1 K1 Co2 31.29(8) . . ? O51 K1 Co2 108.81(9) . . ? Cl5 K1 Co2 140.77(7) . . ? Cl3 K1 Co2 40.88(4) . . ? Cl2 K1 Co2 79.71(5) . . ? Cl8A K1 Co2 95.28(8) . . ? Cl8D K1 Co2 142.1(3) . . ? Co1 K1 Co2 43.77(3) . . ? Co3 K1 Co2 121.86(5) . . ? Cl8E K1 Co4 118.0(4) . . ? O1 K1 Co4 109.05(9) . . ? O51 K1 Co4 31.20(8) . . ? Cl5 K1 Co4 79.43(5) . . ? Cl3 K1 Co4 40.65(4) . . ? Cl2 K1 Co4 140.34(7) . . ? Cl8A K1 Co4 107.96(11) . . ? Cl8D K1 Co4 115.0(3) . . ? Co1 K1 Co4 121.89(5) . . ? Co3 K1 Co4 43.65(3) . . ? Co2 K1 Co4 81.52(4) . . ? Cl8A C80 Cl8B 110.5(8) . . ? C80 Cl8A K1 110.1(5) . . ? Cl8C C80' Cl8D 109.0(15) . . ? C80' Cl8D K1 98(2) . . ? Cl8F C80" Cl8E 108.2(16) . . ? C80" Cl8E K1 154(3) . . ? Cl9A C90 Cl9B 111.7(4) . . ? Cl0A C100 Cl0B 110.3(4) . . ? Cl1A C110 Cl1B 110.3(4) . . ? Cl2A C120 Cl2B 110.7(4) . . ? Cl3B C130 Cl3A 114.3(5) . . ? Cl4B C140 Cl4A 112.6(5) . . ? Cl5A C150 Cl5B 112.5(7) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 66.65 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.533 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.107 #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 825194' #TrackingRef '- kember et al_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H54 Cl3 Co2 N4 O2, C6 H16 N, 2(C H2 Cl2)' _chemical_formula_sum 'C42 H74 Cl7 Co2 N5 O2' _chemical_formula_weight 1047.07 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4425(2) _cell_length_b 21.5810(3) _cell_length_c 16.8129(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.0867(14) _cell_angle_gamma 90.00 _cell_volume 5059.69(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 32048 _cell_measurement_theta_min 2.8611 _cell_measurement_theta_max 32.9877 _exptl_crystal_description blocks _exptl_crystal_colour Pink _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69133 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 33.06 _reflns_number_total 17566 _reflns_number_gt 12400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17566 _refine_ls_number_parameters 543 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.668473(12) 0.527161(8) 0.315977(11) 0.01711(4) Uani 1 1 d . . . Co2 Co 0.701506(13) 0.417762(8) 0.221622(11) 0.01802(4) Uani 1 1 d . . . Cl1 Cl 0.58187(2) 0.515913(14) 0.15996(2) 0.02051(6) Uani 1 1 d . . . Cl2 Cl 0.75504(3) 0.531802(16) 0.46340(2) 0.02836(8) Uani 1 1 d . . . Cl3 Cl 0.80765(3) 0.333660(16) 0.27810(2) 0.02748(8) Uani 1 1 d . . . O1 O 0.78373(6) 0.49519(4) 0.27257(6) 0.01782(18) Uani 1 1 d . . . C1 C 0.83217(8) 0.53109(6) 0.23208(8) 0.0165(2) Uani 1 1 d . . . C2 C 0.84835(9) 0.59463(6) 0.25095(8) 0.0187(2) Uani 1 1 d . . . C3 C 0.81196(9) 0.62454(6) 0.31738(9) 0.0209(3) Uani 1 1 d . . . H3A H 0.8414 0.6039 0.3706 0.025 Uiso 1 1 calc R . . H3B H 0.8318 0.6686 0.3225 0.025 Uiso 1 1 calc R . . N4 N 0.70586(8) 0.62091(5) 0.30051(7) 0.0172(2) Uani 1 1 d D . . H4 H 0.6820(10) 0.6296(7) 0.2467(3) 0.026(4) Uiso 1 1 d D . . C5 C 0.67332(10) 0.66989(6) 0.34864(9) 0.0215(3) Uani 1 1 d . . . H5A H 0.6919 0.7107 0.3306 0.026 Uiso 1 1 calc R . . H5B H 0.7076 0.6647 0.4074 0.026 Uiso 1 1 calc R . . C6 C 0.56573(9) 0.67068(6) 0.34126(9) 0.0207(3) Uani 1 1 d . . . C7 C 0.53569(10) 0.61491(6) 0.38486(9) 0.0225(3) Uani 1 1 d . . . H7A H 0.5777 0.6130 0.4417 0.027 Uiso 1 1 calc R . . H7B H 0.4693 0.6218 0.3890 0.027 Uiso 1 1 calc R . . N8 N 0.53960(8) 0.55435(5) 0.34459(7) 0.0188(2) Uani 1 1 d D . . H8 H 0.4931(8) 0.5554(8) 0.2971(5) 0.029(4) Uiso 1 1 d D . . C9 C 0.51196(10) 0.50519(6) 0.39612(9) 0.0229(3) Uani 1 1 d . . . H9A H 0.4600 0.5210 0.4191 0.027 Uiso 1 1 calc R . . H9B H 0.5677 0.4955 0.4428 0.027 Uiso 1 1 calc R . . C10 C 0.47881(10) 0.44711(6) 0.34853(8) 0.0205(3) Uani 1 1 d . . . C11 C 0.53995(9) 0.41406(6) 0.30998(8) 0.0183(2) Uani 1 1 d . . . O11 O 0.62979(7) 0.43308(4) 0.31452(6) 0.01890(18) Uani 1 1 d . . . C12 C 0.50206(10) 0.35939(6) 0.26770(8) 0.0201(3) Uani 1 1 d . . . C13 C 0.56161(10) 0.32027(6) 0.22630(9) 0.0217(3) Uani 1 1 d . . . H13A H 0.6192 0.3055 0.2680 0.026 Uiso 1 1 calc R . . H13B H 0.5241 0.2835 0.2014 0.026 Uiso 1 1 calc R . . N14 N 0.59185(8) 0.35515(5) 0.16151(7) 0.0182(2) Uani 1 1 d D . . H14 H 0.5407(6) 0.3776(6) 0.1348(8) 0.018(4) Uiso 1 1 d D . . C15 C 0.61378(10) 0.31113(6) 0.10190(9) 0.0207(3) Uani 1 1 d . . . H15A H 0.5551 0.2871 0.0767 0.025 Uiso 1 1 calc R . . H15B H 0.6628 0.2815 0.1322 0.025 Uiso 1 1 calc R . . C16 C 0.65011(9) 0.34043(6) 0.03305(8) 0.0186(2) Uani 1 1 d . . . C17 C 0.75141(10) 0.36630(6) 0.06543(8) 0.0204(3) Uani 1 1 d . . . H17A H 0.7926 0.3335 0.0976 0.025 Uiso 1 1 calc R . . H17B H 0.7771 0.3763 0.0178 0.025 Uiso 1 1 calc R . . N18 N 0.75900(8) 0.42195(5) 0.11750(7) 0.0172(2) Uani 1 1 d D . . H18 H 0.7269(9) 0.4519(5) 0.0842(8) 0.019(4) Uiso 1 1 d D . . C19 C 0.86152(9) 0.43965(6) 0.14737(9) 0.0206(3) Uani 1 1 d . . . H19A H 0.8944 0.4314 0.1036 0.025 Uiso 1 1 calc R . . H19B H 0.8925 0.4139 0.1958 0.025 Uiso 1 1 calc R . . C20 C 0.87266(9) 0.50679(6) 0.17082(8) 0.0184(2) Uani 1 1 d . . . C21 C 0.92414(9) 0.54479(6) 0.13048(9) 0.0219(3) Uani 1 1 d . . . H21A H 0.9502 0.5269 0.0894 0.026 Uiso 1 1 calc R . . C22 C 0.93902(9) 0.60753(6) 0.14760(9) 0.0226(3) Uani 1 1 d . . . C23 C 0.90007(9) 0.63066(6) 0.20938(9) 0.0218(3) Uani 1 1 d . . . H23A H 0.9095 0.6732 0.2237 0.026 Uiso 1 1 calc R . . C24 C 0.99508(11) 0.64939(7) 0.10331(11) 0.0319(3) Uani 1 1 d . . . C25 C 1.08959(15) 0.66845(11) 0.16647(16) 0.0660(7) Uani 1 1 d . . . H25A H 1.1275 0.6313 0.1867 0.099 Uiso 1 1 calc R . . H25B H 1.0746 0.6901 0.2128 0.099 Uiso 1 1 calc R . . H25C H 1.1264 0.6959 0.1398 0.099 Uiso 1 1 calc R . . C26 C 1.01807(19) 0.61802(10) 0.03060(16) 0.0651(7) Uani 1 1 d . . . H26A H 0.9583 0.6064 -0.0096 0.098 Uiso 1 1 calc R . . H26B H 1.0563 0.5808 0.0493 0.098 Uiso 1 1 calc R . . H26C H 1.0545 0.6465 0.0048 0.098 Uiso 1 1 calc R . . C27 C 0.93957(16) 0.70867(9) 0.07422(14) 0.0559(6) Uani 1 1 d . . . H27A H 0.8793 0.6985 0.0338 0.084 Uiso 1 1 calc R . . H27B H 0.9780 0.7359 0.0487 0.084 Uiso 1 1 calc R . . H27C H 0.9257 0.7298 0.1214 0.084 Uiso 1 1 calc R . . C28 C 0.50803(10) 0.67520(7) 0.25123(9) 0.0276(3) Uani 1 1 d . . . H28A H 0.5201 0.6384 0.2213 0.041 Uiso 1 1 calc R . . H28B H 0.5275 0.7124 0.2262 0.041 Uiso 1 1 calc R . . H28C H 0.4395 0.6777 0.2485 0.041 Uiso 1 1 calc R . . C29 C 0.54657(11) 0.72847(7) 0.38776(11) 0.0308(3) Uani 1 1 d . . . H29A H 0.5836 0.7259 0.4455 0.046 Uiso 1 1 calc R . . H29B H 0.4781 0.7309 0.3851 0.046 Uiso 1 1 calc R . . H29C H 0.5658 0.7656 0.3625 0.046 Uiso 1 1 calc R . . C30 C 0.38598(10) 0.42639(6) 0.34268(9) 0.0238(3) Uani 1 1 d . . . H30A H 0.3473 0.4493 0.3701 0.029 Uiso 1 1 calc R . . C31 C 0.34704(10) 0.37384(7) 0.29866(9) 0.0240(3) Uani 1 1 d . . . C32 C 0.40815(10) 0.34128(6) 0.26241(9) 0.0227(3) Uani 1 1 d . . . H32A H 0.3847 0.3047 0.2324 0.027 Uiso 1 1 calc R . . C33 C 0.24308(11) 0.35432(7) 0.29174(10) 0.0304(3) Uani 1 1 d . . . C34 C 0.17442(14) 0.40685(11) 0.25653(19) 0.0696(8) Uani 1 1 d . . . H34A H 0.1922 0.4439 0.2909 0.104 Uiso 1 1 calc R . . H34B H 0.1089 0.3946 0.2557 0.104 Uiso 1 1 calc R . . H34C H 0.1779 0.4160 0.2003 0.104 Uiso 1 1 calc R . . C35 C 0.23325(15) 0.33754(10) 0.37716(12) 0.0506(5) Uani 1 1 d . . . H35A H 0.2518 0.3731 0.4141 0.076 Uiso 1 1 calc R . . H35B H 0.2751 0.3023 0.3987 0.076 Uiso 1 1 calc R . . H35C H 0.1665 0.3264 0.3737 0.076 Uiso 1 1 calc R . . C36 C 0.21338(14) 0.29775(11) 0.23660(14) 0.0552(6) Uani 1 1 d . . . H36A H 0.2181 0.3074 0.1808 0.083 Uiso 1 1 calc R . . H36B H 0.1471 0.2866 0.2348 0.083 Uiso 1 1 calc R . . H36C H 0.2559 0.2629 0.2587 0.083 Uiso 1 1 calc R . . C37 C 0.58078(10) 0.38962(6) -0.01339(9) 0.0246(3) Uani 1 1 d . . . H37A H 0.5762 0.4235 0.0243 0.037 Uiso 1 1 calc R . . H37B H 0.5173 0.3711 -0.0353 0.037 Uiso 1 1 calc R . . H37C H 0.6044 0.4059 -0.0589 0.037 Uiso 1 1 calc R . . C38 C 0.65744(11) 0.28804(7) -0.02672(9) 0.0274(3) Uani 1 1 d . . . H38A H 0.6803 0.3049 -0.0723 0.041 Uiso 1 1 calc R . . H38B H 0.5942 0.2692 -0.0484 0.041 Uiso 1 1 calc R . . H38C H 0.7026 0.2566 0.0024 0.041 Uiso 1 1 calc R . . N40 N 0.84921(10) 0.40576(6) 0.51445(8) 0.0312(3) Uani 1 1 d D . . H40 H 0.8175(11) 0.4416(4) 0.5000(10) 0.032(5) Uiso 1 1 d D . . C41 C 0.78077(13) 0.35289(8) 0.48716(11) 0.0400(4) Uani 1 1 d . . . H41A H 0.8120 0.3139 0.5112 0.048 Uiso 1 1 calc R . . H41B H 0.7656 0.3492 0.4264 0.048 Uiso 1 1 calc R . . C42 C 0.68883(15) 0.36130(10) 0.51262(13) 0.0514(5) Uani 1 1 d . . . H42A H 0.6466 0.3258 0.4937 0.077 Uiso 1 1 calc R . . H42B H 0.6569 0.3994 0.4880 0.077 Uiso 1 1 calc R . . H42C H 0.7033 0.3642 0.5728 0.077 Uiso 1 1 calc R . . C43 C 0.92500(13) 0.40773(8) 0.46790(12) 0.0403(4) Uani 1 1 d . . . H43A H 0.8933 0.4132 0.4086 0.048 Uiso 1 1 calc R . . H43B H 0.9662 0.4444 0.4863 0.048 Uiso 1 1 calc R . . C44 C 0.98750(14) 0.35119(10) 0.47825(15) 0.0567(6) Uani 1 1 d . . . H44A H 1.0344 0.3559 0.4458 0.085 Uiso 1 1 calc R . . H44B H 0.9477 0.3146 0.4592 0.085 Uiso 1 1 calc R . . H44C H 1.0212 0.3461 0.5365 0.085 Uiso 1 1 calc R . . C45 C 0.88827(16) 0.40907(9) 0.60598(11) 0.0489(5) Uani 1 1 d . . . H45A H 0.9310 0.3731 0.6245 0.059 Uiso 1 1 calc R . . H45B H 0.8344 0.4059 0.6321 0.059 Uiso 1 1 calc R . . C46 C 0.94299(16) 0.46732(10) 0.63486(14) 0.0630(7) Uani 1 1 d . . . H46A H 0.9668 0.4665 0.6950 0.094 Uiso 1 1 calc R . . H46B H 0.9007 0.5032 0.6183 0.094 Uiso 1 1 calc R . . H46C H 0.9973 0.4704 0.6102 0.094 Uiso 1 1 calc R . . C50 C 0.68756(11) 0.63668(7) 0.05145(9) 0.0295(3) Uani 1 1 d . . . H50A H 0.6457 0.6031 0.0623 0.035 Uiso 1 1 calc R . . H50B H 0.7544 0.6213 0.0663 0.035 Uiso 1 1 calc R . . Cl51 Cl 0.67863(3) 0.701842(18) 0.11246(3) 0.03595(9) Uani 1 1 d . . . Cl52 Cl 0.65296(3) 0.65639(2) -0.05443(3) 0.04472(11) Uani 1 1 d . . . C60 C 0.32802(11) 0.49387(7) 0.14625(10) 0.0324(3) Uani 1 1 d . . . H60A H 0.3317 0.4553 0.1789 0.039 Uiso 1 1 calc R . . H60B H 0.3899 0.4992 0.1320 0.039 Uiso 1 1 calc R . . Cl61 Cl 0.23408(3) 0.48765(2) 0.05489(3) 0.04474(11) Uani 1 1 d . . . Cl62 Cl 0.30804(3) 0.55767(2) 0.20553(3) 0.04888(12) 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 Co1 0.01981(9) 0.01528(8) 0.01681(9) -0.00127(6) 0.00581(7) 0.00162(6) Co2 0.02258(9) 0.01586(8) 0.01651(9) -0.00206(6) 0.00666(7) -0.00018(6) Cl1 0.02168(15) 0.02105(15) 0.01779(15) 0.00121(11) 0.00333(11) 0.00272(11) Cl2 0.03652(19) 0.02505(17) 0.01892(17) -0.00093(13) -0.00100(13) 0.00500(13) Cl3 0.03395(19) 0.02373(16) 0.02284(17) 0.00347(13) 0.00396(13) 0.00795(13) O1 0.0199(4) 0.0160(4) 0.0179(5) -0.0010(3) 0.0055(3) 0.0018(3) C1 0.0122(5) 0.0185(6) 0.0174(6) -0.0005(5) 0.0013(4) 0.0007(4) C2 0.0150(6) 0.0186(6) 0.0219(7) -0.0028(5) 0.0034(5) 0.0015(4) C3 0.0182(6) 0.0201(6) 0.0245(7) -0.0061(5) 0.0056(5) -0.0018(5) N4 0.0184(5) 0.0166(5) 0.0170(5) -0.0035(4) 0.0051(4) 0.0021(4) C5 0.0229(7) 0.0170(6) 0.0253(7) -0.0068(5) 0.0077(5) 0.0007(5) C6 0.0220(6) 0.0162(6) 0.0243(7) -0.0037(5) 0.0068(5) 0.0022(5) C7 0.0260(7) 0.0208(7) 0.0239(7) -0.0046(5) 0.0122(5) 0.0016(5) N8 0.0236(6) 0.0175(5) 0.0166(6) -0.0014(4) 0.0074(4) 0.0013(4) C9 0.0303(7) 0.0220(7) 0.0203(7) -0.0001(5) 0.0139(6) 0.0001(5) C10 0.0267(7) 0.0187(6) 0.0185(7) 0.0020(5) 0.0103(5) 0.0010(5) C11 0.0231(6) 0.0184(6) 0.0139(6) 0.0038(5) 0.0059(5) 0.0001(5) O11 0.0216(5) 0.0180(4) 0.0178(5) 0.0002(3) 0.0063(4) -0.0007(3) C12 0.0273(7) 0.0173(6) 0.0175(6) 0.0021(5) 0.0090(5) -0.0005(5) C13 0.0288(7) 0.0168(6) 0.0222(7) 0.0008(5) 0.0114(5) -0.0016(5) N14 0.0231(6) 0.0150(5) 0.0176(6) 0.0005(4) 0.0073(4) 0.0018(4) C15 0.0278(7) 0.0136(6) 0.0225(7) -0.0030(5) 0.0098(5) -0.0002(5) C16 0.0230(6) 0.0155(6) 0.0172(6) -0.0024(5) 0.0050(5) 0.0007(5) C17 0.0244(7) 0.0177(6) 0.0204(7) -0.0052(5) 0.0081(5) 0.0019(5) N18 0.0190(5) 0.0142(5) 0.0179(5) -0.0024(4) 0.0040(4) 0.0017(4) C19 0.0189(6) 0.0197(6) 0.0241(7) -0.0049(5) 0.0073(5) 0.0005(5) C20 0.0164(6) 0.0189(6) 0.0188(7) -0.0038(5) 0.0028(5) 0.0007(4) C21 0.0184(6) 0.0244(7) 0.0237(7) -0.0024(5) 0.0070(5) 0.0010(5) C22 0.0173(6) 0.0221(7) 0.0292(8) -0.0005(5) 0.0075(5) -0.0004(5) C23 0.0186(6) 0.0180(6) 0.0285(7) -0.0021(5) 0.0057(5) 0.0005(5) C24 0.0297(8) 0.0258(8) 0.0469(10) 0.0010(7) 0.0220(7) -0.0022(6) C25 0.0389(11) 0.0709(16) 0.092(2) 0.0055(13) 0.0230(11) -0.0215(10) C26 0.0956(18) 0.0437(12) 0.0827(17) -0.0068(11) 0.0711(15) -0.0133(11) C27 0.0690(14) 0.0399(11) 0.0777(16) 0.0230(10) 0.0527(12) 0.0139(9) C28 0.0272(7) 0.0246(7) 0.0289(8) 0.0022(6) 0.0034(6) 0.0050(5) C29 0.0304(8) 0.0230(7) 0.0420(9) -0.0093(6) 0.0147(7) 0.0032(6) C30 0.0288(7) 0.0234(7) 0.0233(7) 0.0038(5) 0.0140(6) 0.0010(5) C31 0.0265(7) 0.0248(7) 0.0233(7) 0.0061(5) 0.0108(5) -0.0021(5) C32 0.0284(7) 0.0199(6) 0.0208(7) 0.0022(5) 0.0084(5) -0.0047(5) C33 0.0291(8) 0.0311(8) 0.0349(9) 0.0025(6) 0.0153(6) -0.0053(6) C34 0.0271(10) 0.0598(14) 0.122(2) 0.0352(14) 0.0204(12) 0.0025(9) C35 0.0550(12) 0.0595(13) 0.0471(12) -0.0020(9) 0.0310(9) -0.0255(10) C36 0.0366(10) 0.0738(15) 0.0584(14) -0.0272(11) 0.0182(9) -0.0236(9) C37 0.0253(7) 0.0250(7) 0.0217(7) 0.0031(5) 0.0029(5) 0.0019(5) C38 0.0354(8) 0.0244(7) 0.0238(8) -0.0088(5) 0.0102(6) -0.0038(6) N40 0.0399(8) 0.0255(7) 0.0257(7) -0.0011(5) 0.0038(6) 0.0048(5) C41 0.0536(11) 0.0290(8) 0.0359(10) -0.0041(7) 0.0087(8) -0.0049(7) C42 0.0527(12) 0.0485(12) 0.0537(13) -0.0012(9) 0.0153(10) -0.0079(9) C43 0.0398(10) 0.0388(10) 0.0417(11) -0.0085(8) 0.0096(8) 0.0002(7) C44 0.0348(10) 0.0539(12) 0.0761(16) -0.0210(11) 0.0048(10) 0.0074(9) C45 0.0616(13) 0.0538(12) 0.0245(9) -0.0028(8) -0.0010(8) 0.0081(9) C46 0.0685(15) 0.0539(13) 0.0448(13) -0.0144(10) -0.0242(10) 0.0195(10) C50 0.0309(8) 0.0313(8) 0.0256(8) 0.0033(6) 0.0059(6) 0.0051(6) Cl51 0.0469(2) 0.0303(2) 0.0325(2) 0.00420(15) 0.01366(17) 0.00988(16) Cl52 0.0444(3) 0.0615(3) 0.0259(2) 0.00586(19) 0.00488(17) 0.0100(2) C60 0.0302(8) 0.0297(8) 0.0345(9) 0.0084(6) 0.0032(6) 0.0011(6) Cl61 0.0455(3) 0.0438(2) 0.0369(2) 0.00837(19) -0.00369(19) -0.00152(18) Cl62 0.0431(3) 0.0404(2) 0.0562(3) -0.0069(2) 0.0004(2) 0.00384(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.1005(9) . ? Co1 O11 2.1043(9) . ? Co1 N8 2.1227(11) . ? Co1 N4 2.1273(11) . ? Co1 Cl2 2.4705(4) . ? Co1 Cl1 2.6070(4) . ? Co1 Co2 2.9516(2) . ? Co2 O1 2.0992(9) . ? Co2 O11 2.1128(9) . ? Co2 N18 2.1258(12) . ? Co2 N14 2.1266(11) . ? Co2 Cl3 2.4059(4) . ? Co2 Cl1 2.7595(4) . ? O1 C1 1.3420(15) . ? C1 C20 1.4111(18) . ? C1 C2 1.4132(18) . ? C2 C23 1.3866(19) . ? C2 C3 1.4986(19) . ? C3 N4 1.4860(16) . ? N4 C5 1.4803(16) . ? C5 C6 1.5264(19) . ? C6 C28 1.529(2) . ? C6 C7 1.5297(19) . ? C6 C29 1.5349(19) . ? C7 N8 1.4799(17) . ? N8 C9 1.4884(17) . ? C9 C10 1.4972(19) . ? C10 C30 1.3923(19) . ? C10 C11 1.4164(18) . ? C11 O11 1.3440(16) . ? C11 C12 1.4121(18) . ? C12 C32 1.3919(19) . ? C12 C13 1.4996(18) . ? C13 N14 1.4804(17) . ? N14 C15 1.4739(16) . ? C15 C16 1.5268(19) . ? C16 C37 1.5272(18) . ? C16 C17 1.5277(18) . ? C16 C38 1.5345(18) . ? C17 N18 1.4735(16) . ? N18 C19 1.4843(17) . ? C19 C20 1.4994(18) . ? C20 C21 1.3956(19) . ? C21 C22 1.3893(19) . ? C22 C23 1.396(2) . ? C22 C24 1.530(2) . ? C24 C26 1.508(3) . ? C24 C27 1.521(2) . ? C24 C25 1.551(3) . ? C30 C31 1.390(2) . ? C31 C32 1.387(2) . ? C31 C33 1.534(2) . ? C33 C34 1.521(3) . ? C33 C35 1.523(2) . ? C33 C36 1.525(2) . ? N40 C45 1.497(2) . ? N40 C41 1.501(2) . ? N40 C43 1.503(2) . ? C41 C42 1.508(3) . ? C43 C44 1.501(2) . ? C45 C46 1.497(3) . ? C50 Cl51 1.7651(16) . ? C50 Cl52 1.7710(16) . ? C60 Cl62 1.7671(18) . ? C60 Cl61 1.7700(17) . ? 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 O11 84.90(4) . . ? O1 Co1 N8 172.07(4) . . ? O11 Co1 N8 91.35(4) . . ? O1 Co1 N4 91.18(4) . . ? O11 Co1 N4 172.43(4) . . ? N8 Co1 N4 91.74(4) . . ? O1 Co1 Cl2 97.01(3) . . ? O11 Co1 Cl2 96.56(3) . . ? N8 Co1 Cl2 90.35(3) . . ? N4 Co1 Cl2 90.33(3) . . ? O1 Co1 Cl1 80.55(3) . . ? O11 Co1 Cl1 80.91(3) . . ? N8 Co1 Cl1 91.97(3) . . ? N4 Co1 Cl1 92.07(3) . . ? Cl2 Co1 Cl1 176.607(13) . . ? O1 Co1 Co2 45.33(2) . . ? O11 Co1 Co2 45.70(3) . . ? N8 Co1 Co2 128.08(3) . . ? N4 Co1 Co2 127.83(3) . . ? Cl2 Co1 Co2 117.468(11) . . ? Cl1 Co1 Co2 59.141(8) . . ? O1 Co2 O11 84.72(4) . . ? O1 Co2 N18 90.08(4) . . ? O11 Co2 N18 166.88(4) . . ? O1 Co2 N14 166.40(4) . . ? O11 Co2 N14 90.17(4) . . ? N18 Co2 N14 92.17(4) . . ? O1 Co2 Cl3 101.82(3) . . ? O11 Co2 Cl3 102.17(3) . . ? N18 Co2 Cl3 90.67(3) . . ? N14 Co2 Cl3 91.57(3) . . ? O1 Co2 Cl1 76.98(3) . . ? O11 Co2 Cl1 77.18(3) . . ? N18 Co2 Cl1 89.92(3) . . ? N14 Co2 Cl1 89.61(3) . . ? Cl3 Co2 Cl1 178.660(14) . . ? O1 Co2 Co1 45.36(2) . . ? O11 Co2 Co1 45.46(2) . . ? N18 Co2 Co1 124.12(3) . . ? N14 Co2 Co1 124.00(3) . . ? Cl3 Co2 Co1 124.529(11) . . ? Cl1 Co2 Co1 54.193(8) . . ? Co1 Cl1 Co2 66.666(9) . . ? C1 O1 Co2 124.52(8) . . ? C1 O1 Co1 123.48(8) . . ? Co2 O1 Co1 89.31(3) . . ? O1 C1 C20 121.71(11) . . ? O1 C1 C2 121.59(12) . . ? C20 C1 C2 116.66(12) . . ? C23 C2 C1 120.68(12) . . ? C23 C2 C3 118.26(12) . . ? C1 C2 C3 121.04(12) . . ? N4 C3 C2 112.29(11) . . ? C5 N4 C3 108.44(10) . . ? C5 N4 Co1 119.05(8) . . ? C3 N4 Co1 107.99(8) . . ? N4 C5 C6 115.13(11) . . ? C5 C6 C28 111.24(12) . . ? C5 C6 C7 111.23(11) . . ? C28 C6 C7 112.03(11) . . ? C5 C6 C29 106.40(11) . . ? C28 C6 C29 109.17(12) . . ? C7 C6 C29 106.49(12) . . ? N8 C7 C6 115.23(11) . . ? C7 N8 C9 108.37(10) . . ? C7 N8 Co1 119.21(8) . . ? C9 N8 Co1 108.59(8) . . ? N8 C9 C10 112.49(11) . . ? C30 C10 C11 120.62(12) . . ? C30 C10 C9 118.35(12) . . ? C11 C10 C9 121.03(12) . . ? O11 C11 C12 121.71(12) . . ? O11 C11 C10 121.86(12) . . ? C12 C11 C10 116.42(12) . . ? C11 O11 Co1 123.01(8) . . ? C11 O11 Co2 124.20(8) . . ? Co1 O11 Co2 88.84(4) . . ? C32 C12 C11 120.68(12) . . ? C32 C12 C13 118.64(12) . . ? C11 C12 C13 120.67(12) . . ? N14 C13 C12 111.72(11) . . ? C15 N14 C13 109.24(10) . . ? C15 N14 Co2 117.87(8) . . ? C13 N14 Co2 107.41(8) . . ? N14 C15 C16 115.20(10) . . ? C15 C16 C37 111.50(11) . . ? C15 C16 C17 111.56(11) . . ? C37 C16 C17 111.58(11) . . ? C15 C16 C38 106.70(11) . . ? C37 C16 C38 108.97(11) . . ? C17 C16 C38 106.24(11) . . ? N18 C17 C16 115.20(10) . . ? C17 N18 C19 108.91(10) . . ? C17 N18 Co2 118.03(8) . . ? C19 N18 Co2 107.54(8) . . ? N18 C19 C20 111.52(10) . . ? C21 C20 C1 120.72(12) . . ? C21 C20 C19 118.32(12) . . ? C1 C20 C19 120.97(12) . . ? C22 C21 C20 123.04(13) . . ? C21 C22 C23 115.60(13) . . ? C21 C22 C24 123.21(13) . . ? C23 C22 C24 121.19(12) . . ? C2 C23 C22 123.28(12) . . ? C26 C24 C27 109.01(17) . . ? C26 C24 C22 112.68(14) . . ? C27 C24 C22 110.59(13) . . ? C26 C24 C25 109.50(17) . . ? C27 C24 C25 107.06(16) . . ? C22 C24 C25 107.84(15) . . ? C31 C30 C10 123.25(13) . . ? C32 C31 C30 115.56(13) . . ? C32 C31 C33 123.33(13) . . ? C30 C31 C33 121.10(13) . . ? C31 C32 C12 123.40(13) . . ? C34 C33 C35 109.44(17) . . ? C34 C33 C36 107.96(17) . . ? C35 C33 C36 107.59(15) . . ? C34 C33 C31 110.54(13) . . ? C35 C33 C31 108.86(14) . . ? C36 C33 C31 112.38(14) . . ? C45 N40 C41 113.12(14) . . ? C45 N40 C43 113.79(14) . . ? C41 N40 C43 111.92(13) . . ? N40 C41 C42 112.34(15) . . ? C44 C43 N40 114.47(17) . . ? N40 C45 C46 113.55(17) . . ? Cl51 C50 Cl52 110.40(8) . . ? Cl62 C60 Cl61 110.35(9) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.601 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.065 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 825195' #TrackingRef '- kember et al_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H54 Cl3 Co2 N4 O2, C9 H17 N2, C4 H8 O, 0.5(C6 H14)' _chemical_formula_sum 'C50 H86 Cl3 Co2 N6 O3' _chemical_formula_weight 1043.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4636(4) _cell_length_b 15.6121(6) _cell_length_c 15.8197(5) _cell_angle_alpha 69.978(3) _cell_angle_beta 71.369(3) _cell_angle_gamma 85.244(3) _cell_volume 2739.42(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14146 _cell_measurement_theta_min 3.2207 _cell_measurement_theta_max 32.8905 _exptl_crystal_description blocks _exptl_crystal_colour Pink _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1114 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.779 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32068 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 32.97 _reflns_number_total 18033 _reflns_number_gt 11966 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18033 _refine_ls_number_parameters 684 _refine_ls_number_restraints 416 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.577882(16) 0.691521(14) 0.562312(14) 0.02151(5) Uani 1 1 d . . . Co2 Co 0.818892(16) 0.740649(15) 0.460390(14) 0.02471(6) Uani 1 1 d . . . Cl1 Cl 0.72101(3) 0.56799(3) 0.51834(3) 0.03078(9) Uani 1 1 d . . . Cl2 Cl 0.46314(3) 0.81358(3) 0.60293(3) 0.02816(8) Uani 1 1 d . . . Cl3 Cl 0.89103(4) 0.89050(3) 0.41757(3) 0.03826(10) Uani 1 1 d . . . O1 O 0.66830(8) 0.76890(7) 0.42496(7) 0.0227(2) Uani 1 1 d . . . C1 C 0.65043(12) 0.76859(10) 0.34577(10) 0.0212(3) Uani 1 1 d . . . C2 C 0.54068(12) 0.75570(10) 0.34338(10) 0.0213(3) Uani 1 1 d . . . C3 C 0.43979(12) 0.73789(10) 0.43043(10) 0.0230(3) Uani 1 1 d . . . H3A H 0.4272 0.7925 0.4502 0.028 Uiso 1 1 calc R . . H3B H 0.3719 0.7274 0.4152 0.028 Uiso 1 1 calc R . . N4 N 0.45332(10) 0.65778(8) 0.51042(9) 0.0208(2) Uani 1 1 d D . . H4 H 0.4825(12) 0.6109(7) 0.4904(10) 0.021(4) Uiso 1 1 d D . . C5 C 0.33966(12) 0.62551(11) 0.57788(11) 0.0248(3) Uani 1 1 d . . . H5A H 0.2959 0.6052 0.5455 0.030 Uiso 1 1 calc R . . H5B H 0.3002 0.6776 0.5953 0.030 Uiso 1 1 calc R . . C6 C 0.33877(12) 0.54794(10) 0.66828(11) 0.0245(3) Uani 1 1 d . . . C7 C 0.38060(12) 0.58058(11) 0.73315(11) 0.0259(3) Uani 1 1 d . . . H7A H 0.3413 0.6370 0.7388 0.031 Uiso 1 1 calc R . . H7B H 0.3593 0.5338 0.7970 0.031 Uiso 1 1 calc R . . N8 N 0.50431(10) 0.59901(9) 0.70077(9) 0.0229(3) Uani 1 1 d D . . H8 H 0.5413(13) 0.5469(6) 0.7012(13) 0.033(5) Uiso 1 1 d D . . C9 C 0.53409(12) 0.63137(12) 0.76865(11) 0.0273(3) Uani 1 1 d . . . H9A H 0.4872 0.5973 0.8339 0.033 Uiso 1 1 calc R . . H9B H 0.5170 0.6968 0.7559 0.033 Uiso 1 1 calc R . . C10 C 0.65652(13) 0.61870(12) 0.76123(11) 0.0277(3) Uani 1 1 d . . . C11 C 0.74152(12) 0.66509(11) 0.67696(11) 0.0250(3) Uani 1 1 d . . . O11 O 0.71574(8) 0.71982(7) 0.60028(7) 0.0248(2) Uani 1 1 d . . . C12 C 0.85425(13) 0.65242(12) 0.67836(11) 0.0296(3) Uani 1 1 d . . . C13 C 0.95020(13) 0.70232(13) 0.59356(11) 0.0321(4) Uani 1 1 d . . . H13A H 0.9401 0.7689 0.5787 0.038 Uiso 1 1 calc R . . H13B H 1.0225 0.6876 0.6082 0.038 Uiso 1 1 calc R . . N14 N 0.95562(10) 0.67705(10) 0.50968(9) 0.0276(3) Uani 1 1 d D . . H14 H 0.9400(15) 0.6167(3) 0.5307(13) 0.037(5) Uiso 1 1 d D . . C15 C 1.07146(13) 0.69526(14) 0.44234(12) 0.0350(4) Uani 1 1 d . . . H15A H 1.1247 0.6586 0.4745 0.042 Uiso 1 1 calc R . . H15B H 1.0918 0.7604 0.4248 0.042 Uiso 1 1 calc R . . C16 C 1.08748(13) 0.67390(13) 0.35176(11) 0.0325(4) Uani 1 1 d . . . C17 C 1.02754(12) 0.74197(13) 0.28795(12) 0.0320(4) Uani 1 1 d . . . H17A H 1.0494 0.8044 0.2803 0.038 Uiso 1 1 calc R . . H17B H 1.0551 0.7351 0.2246 0.038 Uiso 1 1 calc R . . N18 N 0.90262(10) 0.73292(9) 0.32200(9) 0.0257(3) Uani 1 1 d D . . H18 H 0.8850(13) 0.6764(4) 0.3266(12) 0.023(4) Uiso 1 1 d D . . C19 C 0.85854(12) 0.80505(11) 0.25314(11) 0.0286(3) Uani 1 1 d . . . H19A H 0.9089 0.8123 0.1883 0.034 Uiso 1 1 calc R . . H19B H 0.8602 0.8636 0.2641 0.034 Uiso 1 1 calc R . . C20 C 0.73951(12) 0.78444(10) 0.26004(10) 0.0243(3) Uani 1 1 d . . . C21 C 0.71914(13) 0.78473(11) 0.17822(11) 0.0277(3) Uani 1 1 d . . . H21A H 0.7815 0.7943 0.1221 0.033 Uiso 1 1 calc R . . C22 C 0.61186(13) 0.77174(11) 0.17510(11) 0.0278(3) Uani 1 1 d . A . C23 C 0.52457(13) 0.75809(10) 0.25931(11) 0.0256(3) Uani 1 1 d . . . H23A H 0.4497 0.7499 0.2598 0.031 Uiso 1 1 calc R . . C24 C 0.58840(15) 0.77185(14) 0.08548(12) 0.0421(5) Uani 1 1 d D . . C25 C 0.5115(3) 0.8499(3) 0.0580(2) 0.0904(13) Uani 0.900(5) 1 d PDU A 1 H25A H 0.5490 0.9078 0.0449 0.136 Uiso 0.900(5) 1 calc PR A 1 H25B H 0.4404 0.8421 0.1100 0.136 Uiso 0.900(5) 1 calc PR A 1 H25C H 0.4953 0.8501 0.0012 0.136 Uiso 0.900(5) 1 calc PR A 1 C26 C 0.6954(2) 0.7793(3) 0.00429(17) 0.0625(9) Uani 0.900(5) 1 d PDU A 1 H26A H 0.7340 0.8381 -0.0142 0.094 Uiso 0.900(5) 1 calc PR A 1 H26B H 0.6764 0.7747 -0.0496 0.094 Uiso 0.900(5) 1 calc PR A 1 H26C H 0.7454 0.7298 0.0239 0.094 Uiso 0.900(5) 1 calc PR A 1 C27 C 0.5258(3) 0.6817(2) 0.10679(18) 0.0666(10) Uani 0.900(5) 1 d PDU A 1 H27A H 0.5700 0.6299 0.1320 0.100 Uiso 0.900(5) 1 calc PR A 1 H27B H 0.5167 0.6793 0.0484 0.100 Uiso 0.900(5) 1 calc PR A 1 H27C H 0.4511 0.6788 0.1535 0.100 Uiso 0.900(5) 1 calc PR A 1 C25' C 0.594(2) 0.8737(9) 0.0214(18) 0.067(6) Uiso 0.100(5) 1 d PDU A 2 H25D H 0.6564 0.9057 0.0250 0.101 Uiso 0.100(5) 1 calc PR A 2 H25E H 0.5227 0.9023 0.0431 0.101 Uiso 0.100(5) 1 calc PR A 2 H25F H 0.6081 0.8771 -0.0442 0.101 Uiso 0.100(5) 1 calc PR A 2 C26' C 0.6842(17) 0.7247(17) 0.031(2) 0.072(6) Uiso 0.100(5) 1 d PDU A 2 H26D H 0.7497 0.7669 -0.0047 0.108 Uiso 0.100(5) 1 calc PR A 2 H26E H 0.6584 0.7063 -0.0128 0.108 Uiso 0.100(5) 1 calc PR A 2 H26F H 0.7058 0.6706 0.0757 0.108 Uiso 0.100(5) 1 calc PR A 2 C27' C 0.4762(13) 0.7329(16) 0.0976(17) 0.057(5) Uiso 0.100(5) 1 d PDU A 2 H27D H 0.4214 0.7817 0.0916 0.085 Uiso 0.100(5) 1 calc PR A 2 H27E H 0.4490 0.6863 0.1603 0.085 Uiso 0.100(5) 1 calc PR A 2 H27F H 0.4850 0.7053 0.0488 0.085 Uiso 0.100(5) 1 calc PR A 2 C28 C 0.40579(14) 0.46773(11) 0.64692(12) 0.0310(3) Uani 1 1 d . . . H28A H 0.4853 0.4870 0.6128 0.046 Uiso 1 1 calc R . . H28B H 0.3745 0.4465 0.6078 0.046 Uiso 1 1 calc R . . H28C H 0.4007 0.4181 0.7064 0.046 Uiso 1 1 calc R . . C29 C 0.21413(13) 0.51612(13) 0.72143(13) 0.0363(4) Uani 1 1 d . . . H29A H 0.1697 0.5672 0.7354 0.054 Uiso 1 1 calc R . . H29B H 0.2094 0.4664 0.7808 0.054 Uiso 1 1 calc R . . H29C H 0.1840 0.4945 0.6820 0.054 Uiso 1 1 calc R . . C30 C 0.68446(14) 0.55838(13) 0.83870(11) 0.0330(4) Uani 1 1 d . . . H30A H 0.6250 0.5273 0.8938 0.040 Uiso 1 1 calc R . . C31 C 0.79580(14) 0.54182(14) 0.83871(12) 0.0361(4) Uani 1 1 d . B . C32 C 0.87833(14) 0.59177(13) 0.75738(12) 0.0355(4) Uani 1 1 d . . . H32A H 0.9554 0.5841 0.7556 0.043 Uiso 1 1 calc R . . C33 C 0.82312(16) 0.47340(16) 0.92575(12) 0.0483(5) Uani 1 1 d D . . C34 C 0.7482(3) 0.3837(3) 0.9637(3) 0.0882(15) Uani 0.780(5) 1 d PDU B 1 H34A H 0.7544 0.3619 0.9111 0.132 Uiso 0.780(5) 1 calc PR B 1 H34B H 0.6690 0.3965 0.9918 0.132 Uiso 0.780(5) 1 calc PR B 1 H34C H 0.7746 0.3368 1.0117 0.132 Uiso 0.780(5) 1 calc PR B 1 C35 C 0.7954(3) 0.5133(3) 1.0033(2) 0.0771(12) Uani 0.780(5) 1 d PDU B 1 H35A H 0.8401 0.5699 0.9812 0.116 Uiso 0.780(5) 1 calc PR B 1 H35B H 0.8134 0.4698 1.0582 0.116 Uiso 0.780(5) 1 calc PR B 1 H35C H 0.7145 0.5263 1.0214 0.116 Uiso 0.780(5) 1 calc PR B 1 C36 C 0.9441(3) 0.4443(3) 0.9024(2) 0.0763(14) Uani 0.780(5) 1 d PDU B 1 H36A H 0.9948 0.4975 0.8809 0.115 Uiso 0.780(5) 1 calc PR B 1 H36B H 0.9599 0.4175 0.8522 0.115 Uiso 0.780(5) 1 calc PR B 1 H36C H 0.9564 0.3991 0.9590 0.115 Uiso 0.780(5) 1 calc PR B 1 C34' C 0.7236(7) 0.4355(8) 1.0027(7) 0.055(3) Uiso 0.220(5) 1 d PDU B 2 H34D H 0.6957 0.4785 1.0373 0.083 Uiso 0.220(5) 1 calc PR B 2 H34E H 0.7416 0.3781 1.0455 0.083 Uiso 0.220(5) 1 calc PR B 2 H34F H 0.6652 0.4240 0.9783 0.083 Uiso 0.220(5) 1 calc PR B 2 C35' C 0.8861(10) 0.5370(7) 0.9597(9) 0.069(3) Uiso 0.220(5) 1 d PDU B 2 H35D H 0.9348 0.5832 0.9040 0.104 Uiso 0.220(5) 1 calc PR B 2 H35E H 0.9323 0.4989 0.9974 0.104 Uiso 0.220(5) 1 calc PR B 2 H35F H 0.8291 0.5671 0.9981 0.104 Uiso 0.220(5) 1 calc PR B 2 C36' C 0.9086(10) 0.4099(8) 0.8941(9) 0.060(3) Uiso 0.220(5) 1 d PDU B 2 H36D H 0.9835 0.4405 0.8651 0.089 Uiso 0.220(5) 1 calc PR B 2 H36E H 0.8891 0.3911 0.8475 0.089 Uiso 0.220(5) 1 calc PR B 2 H36F H 0.9097 0.3560 0.9486 0.089 Uiso 0.220(5) 1 calc PR B 2 C37 C 1.05187(15) 0.57652(13) 0.37246(13) 0.0402(4) Uani 1 1 d . . . H37A H 1.0641 0.5655 0.3128 0.060 Uiso 1 1 calc R . . H37B H 0.9714 0.5666 0.4095 0.060 Uiso 1 1 calc R . . H37C H 1.0970 0.5345 0.4085 0.060 Uiso 1 1 calc R . . C38 C 1.21549(14) 0.68785(16) 0.29760(13) 0.0473(5) Uani 1 1 d . . . H38A H 1.2312 0.6745 0.2387 0.071 Uiso 1 1 calc R . . H38B H 1.2580 0.6468 0.3369 0.071 Uiso 1 1 calc R . . H38C H 1.2385 0.7512 0.2828 0.071 Uiso 1 1 calc R . . N41 N 0.55747(13) 0.93084(9) 0.70991(10) 0.0331(3) Uani 1 1 d . . . C42 C 0.44998(17) 0.91119(13) 0.78646(13) 0.0431(4) Uani 1 1 d . . . H42A H 0.4639 0.9028 0.8470 0.052 Uiso 1 1 calc R . . H42B H 0.4159 0.8537 0.7921 0.052 Uiso 1 1 calc R . . C43 C 0.36796(17) 0.98769(14) 0.76884(13) 0.0434(4) Uani 1 1 d . . . H43A H 0.2918 0.9684 0.8151 0.052 Uiso 1 1 calc R . . H43B H 0.3938 1.0421 0.7765 0.052 Uiso 1 1 calc R . . C44 C 0.36263(15) 1.01057(12) 0.66979(13) 0.0356(4) Uani 1 1 d . . . H44A H 0.3301 0.9580 0.6637 0.043 Uiso 1 1 calc R . . H44B H 0.3138 1.0634 0.6553 0.043 Uiso 1 1 calc R . . N45 N 0.47701(13) 1.03216(9) 0.60440(10) 0.0316(3) Uani 1 1 d D . . H45 H 0.4899(15) 1.0735(9) 0.5460(5) 0.034(5) Uiso 1 1 d D . . C46 C 0.56622(15) 0.99056(11) 0.62440(12) 0.0305(3) Uani 1 1 d . . . C47 C 0.67841(16) 1.01327(13) 0.55036(13) 0.0397(4) Uani 1 1 d . . . H47A H 0.6683 1.0591 0.4924 0.048 Uiso 1 1 calc R . . H47B H 0.7076 0.9577 0.5349 0.048 Uiso 1 1 calc R . . C48 C 0.76714(18) 1.05040(15) 0.57817(16) 0.0524(5) Uani 1 1 d . . . H48A H 0.8254 1.0864 0.5198 0.063 Uiso 1 1 calc R . . H48B H 0.7300 1.0922 0.6132 0.063 Uiso 1 1 calc R . . C49 C 0.82561(19) 0.97684(17) 0.63911(17) 0.0586(6) Uani 1 1 d . . . H49A H 0.8636 0.9356 0.6036 0.070 Uiso 1 1 calc R . . H49B H 0.8850 1.0064 0.6498 0.070 Uiso 1 1 calc R . . C50 C 0.74712(19) 0.92002(16) 0.73449(16) 0.0545(6) Uani 1 1 d . . . H50A H 0.7921 0.8741 0.7685 0.065 Uiso 1 1 calc R . . H50B H 0.7143 0.9602 0.7724 0.065 Uiso 1 1 calc R . . C51 C 0.65143(17) 0.87135(13) 0.72766(14) 0.0424(4) Uani 1 1 d . . . H51A H 0.6819 0.8454 0.6759 0.051 Uiso 1 1 calc R . . H51B H 0.6218 0.8200 0.7874 0.051 Uiso 1 1 calc R . . C61 C 1.2222(7) 0.9434(7) 0.0611(8) 0.071(3) Uiso 0.356(4) 1 d PDU C -1 H61A H 1.2520 0.9518 0.1082 0.106 Uiso 0.356(4) 1 calc PR C -1 H61B H 1.2743 0.9729 -0.0025 0.106 Uiso 0.356(4) 1 calc PR C -1 H61C H 1.2150 0.8781 0.0723 0.106 Uiso 0.356(4) 1 calc PR C -1 C62 C 1.1113(6) 0.9841(5) 0.0690(6) 0.0461(16) Uiso 0.356(4) 1 d PDU C -1 H62A H 1.0602 0.9522 0.1333 0.055 Uiso 0.356(4) 1 calc PR C -1 H62B H 1.1196 1.0483 0.0643 0.055 Uiso 0.356(4) 1 calc PR C -1 C63 C 1.0574(9) 0.9841(8) 0.0045(9) 0.067(3) Uiso 0.356(4) 1 d PDU C -1 H63A H 1.0461 0.9196 0.0116 0.081 Uiso 0.356(4) 1 calc PR C -1 H63B H 1.1107 1.0129 -0.0597 0.081 Uiso 0.356(4) 1 calc PR C -1 C64 C 0.9451(9) 1.0296(8) 0.0072(9) 0.063(3) Uiso 0.356(4) 1 d PDU C -1 H64A H 0.8959 1.0020 0.0732 0.075 Uiso 0.356(4) 1 calc PR C -1 H64B H 0.9599 1.0935 -0.0005 0.075 Uiso 0.356(4) 1 calc PR C -1 C65 C 0.8782(9) 1.0352(9) -0.0464(9) 0.102(4) Uiso 0.356(4) 1 d PDU C -1 H65A H 0.8552 0.9714 -0.0327 0.123 Uiso 0.356(4) 1 calc PR C -1 H65B H 0.9291 1.0559 -0.1126 0.123 Uiso 0.356(4) 1 calc PR C -1 C66 C 0.7779(8) 1.0863(8) -0.0483(8) 0.084(3) Uiso 0.356(4) 1 d PDU C -1 H66A H 0.7510 1.0809 -0.0982 0.126 Uiso 0.356(4) 1 calc PR C -1 H66B H 0.7948 1.1505 -0.0612 0.126 Uiso 0.356(4) 1 calc PR C -1 H66C H 0.7192 1.0624 0.0130 0.126 Uiso 0.356(4) 1 calc PR C -1 C61' C 1.2154(16) 0.9369(15) 0.1082(18) 0.078(6) Uiso 0.144(4) 1 d PDU C -2 H61D H 1.2395 0.9420 0.1596 0.117 Uiso 0.144(4) 1 calc PR C -2 H61E H 1.2748 0.9630 0.0477 0.117 Uiso 0.144(4) 1 calc PR C -2 H61F H 1.2020 0.8724 0.1191 0.117 Uiso 0.144(4) 1 calc PR C -2 C62' C 1.1149(17) 0.9845(18) 0.1059(18) 0.100(7) Uiso 0.144(4) 1 d PDU C -2 H62C H 1.0567 0.9451 0.1619 0.120 Uiso 0.144(4) 1 calc PR C -2 H62D H 1.1251 1.0383 0.1224 0.120 Uiso 0.144(4) 1 calc PR C -2 C63' C 1.0594(19) 1.018(2) 0.0399(19) 0.123(7) Uiso 0.144(4) 1 d PDU C -2 H63C H 1.0737 0.9718 0.0079 0.148 Uiso 0.144(4) 1 calc PR C -2 H63D H 1.1076 1.0717 -0.0064 0.148 Uiso 0.144(4) 1 calc PR C -2 C64' C 0.9498(19) 1.046(2) 0.038(2) 0.127(8) Uiso 0.144(4) 1 d PDU C -2 H64C H 0.9083 0.9868 0.0691 0.152 Uiso 0.144(4) 1 calc PR C -2 H64D H 0.9290 1.0753 0.0873 0.152 Uiso 0.144(4) 1 calc PR C -2 C65' C 0.8840(16) 1.0920(15) -0.0139(15) 0.085(6) Uiso 0.144(4) 1 d PDU C -2 H65C H 0.9018 1.0582 -0.0593 0.102 Uiso 0.144(4) 1 calc PR C -2 H65D H 0.9318 1.1484 -0.0493 0.102 Uiso 0.144(4) 1 calc PR C -2 C66' C 0.7859(16) 1.1271(16) -0.0270(17) 0.085(6) Uiso 0.144(4) 1 d PDU C -2 H66D H 0.7553 1.0910 -0.0544 0.128 Uiso 0.144(4) 1 calc PR C -2 H66E H 0.7995 1.1903 -0.0701 0.128 Uiso 0.144(4) 1 calc PR C -2 H66F H 0.7315 1.1256 0.0340 0.128 Uiso 0.144(4) 1 calc PR C -2 O70 O 0.1073(9) 0.7210(5) 0.8367(5) 0.090(2) Uiso 0.308(3) 1 d PDU D 1 C71 C 0.0895(10) 0.7365(7) 0.7459(7) 0.080(3) Uiso 0.308(3) 1 d PDU D 1 H71A H 0.1495 0.7081 0.7066 0.096 Uiso 0.308(3) 1 calc PR D 1 H71B H 0.0150 0.7108 0.7552 0.096 Uiso 0.308(3) 1 calc PR D 1 C72 C 0.094(2) 0.8335(9) 0.7023(11) 0.137(7) Uiso 0.308(3) 1 d PDU D 1 H72A H 0.1601 0.8519 0.6441 0.164 Uiso 0.308(3) 1 calc PR D 1 H72B H 0.0247 0.8536 0.6844 0.164 Uiso 0.308(3) 1 calc PR D 1 C73 C 0.1038(16) 0.8755(7) 0.7656(10) 0.115(4) Uiso 0.308(3) 1 d PDU D 1 H73A H 0.1672 0.9211 0.7334 0.138 Uiso 0.308(3) 1 calc PR D 1 H73B H 0.0333 0.9077 0.7852 0.138 Uiso 0.308(3) 1 calc PR D 1 C74 C 0.1228(13) 0.8109(8) 0.8452(8) 0.093(3) Uiso 0.308(3) 1 d PDU D 1 H74A H 0.0680 0.8167 0.9039 0.112 Uiso 0.308(3) 1 calc PR D 1 H74B H 0.2005 0.8183 0.8461 0.112 Uiso 0.308(3) 1 calc PR D 1 O70' O 0.0364(9) 0.8842(5) 0.7867(7) 0.079(3) Uiso 0.256(5) 1 d PDU E 2 C71' C 0.0162(13) 0.7987(8) 0.8729(8) 0.084(4) Uiso 0.256(5) 1 d PDU E 2 H71C H 0.0708 0.7966 0.9073 0.101 Uiso 0.256(5) 1 calc PR E 2 H71D H -0.0616 0.7966 0.9165 0.101 Uiso 0.256(5) 1 calc PR E 2 C72' C 0.0319(14) 0.7251(7) 0.8378(8) 0.081(4) Uiso 0.256(5) 1 d PDU E 2 H72C H -0.0348 0.7152 0.8207 0.098 Uiso 0.256(5) 1 calc PR E 2 H72D H 0.0463 0.6681 0.8846 0.098 Uiso 0.256(5) 1 calc PR E 2 C73' C 0.1301(17) 0.7553(10) 0.7551(13) 0.134(7) Uiso 0.256(5) 1 d PDU E 2 H73C H 0.1354 0.7210 0.7116 0.161 Uiso 0.256(5) 1 calc PR E 2 H73D H 0.2003 0.7471 0.7731 0.161 Uiso 0.256(5) 1 calc PR E 2 C74' C 0.1121(19) 0.8526(10) 0.7104(9) 0.103(5) Uiso 0.256(5) 1 d PDU E 2 H74C H 0.0765 0.8609 0.6605 0.124 Uiso 0.256(5) 1 calc PR E 2 H74D H 0.1851 0.8875 0.6814 0.124 Uiso 0.256(5) 1 calc PR E 2 O70" O 0.0470(11) 0.8466(8) 0.7215(8) 0.082(3) Uiso 0.226(5) 1 d PDU F 3 C71" C 0.1563(15) 0.795(2) 0.7194(16) 0.116(8) Uiso 0.226(5) 1 d PDU F 3 H71E H 0.1436 0.7291 0.7313 0.139 Uiso 0.226(5) 1 calc PR F 3 H71F H 0.2159 0.8204 0.6579 0.139 Uiso 0.226(5) 1 calc PR F 3 C72" C 0.1860(12) 0.8071(15) 0.7940(13) 0.110(6) Uiso 0.226(5) 1 d PDU F 3 H72E H 0.1800 0.7481 0.8459 0.132 Uiso 0.226(5) 1 calc PR F 3 H72F H 0.2650 0.8310 0.7707 0.132 Uiso 0.226(5) 1 calc PR F 3 C73" C 0.1137(10) 0.8673(10) 0.8264(9) 0.073(4) Uiso 0.226(5) 1 d PDU F 3 H73E H 0.1372 0.9307 0.7846 0.087 Uiso 0.226(5) 1 calc PR F 3 H73F H 0.1115 0.8611 0.8913 0.087 Uiso 0.226(5) 1 calc PR F 3 C74" C -0.0005(9) 0.8428(13) 0.8253(10) 0.082(4) Uiso 0.226(5) 1 d PDU F 3 H74E H -0.0581 0.8891 0.8350 0.098 Uiso 0.226(5) 1 calc PR F 3 H74F H -0.0296 0.7814 0.8699 0.098 Uiso 0.226(5) 1 calc PR F 3 O70* O 0.1702(9) 0.7651(10) 0.8042(8) 0.085(4) Uiso 0.209(5) 1 d PDU G 4 C71* C 0.0682(11) 0.7713(12) 0.8794(8) 0.076(4) Uiso 0.209(5) 1 d PDU G 4 H71G H 0.0672 0.7259 0.9413 0.091 Uiso 0.209(5) 1 calc PR G 4 H71H H 0.0610 0.8331 0.8844 0.091 Uiso 0.209(5) 1 calc PR G 4 C72* C -0.0181(10) 0.7514(12) 0.8476(9) 0.084(5) Uiso 0.209(5) 1 d PDU G 4 H72G H -0.0213 0.6856 0.8565 0.100 Uiso 0.209(5) 1 calc PR G 4 H72H H -0.0930 0.7692 0.8818 0.100 Uiso 0.209(5) 1 calc PR G 4 C73* C 0.0148(12) 0.8044(15) 0.7505(10) 0.105(6) Uiso 0.209(5) 1 d PDU G 4 H73G H 0.0036 0.8700 0.7419 0.126 Uiso 0.209(5) 1 calc PR G 4 H73H H -0.0293 0.7857 0.7172 0.126 Uiso 0.209(5) 1 calc PR G 4 C74* C 0.1355(12) 0.7862(15) 0.7150(9) 0.065(4) Uiso 0.209(5) 1 d PDU G 4 H74G H 0.1778 0.8401 0.6636 0.078 Uiso 0.209(5) 1 calc PR G 4 H74H H 0.1466 0.7334 0.6922 0.078 Uiso 0.209(5) 1 calc PR G 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01689(9) 0.02817(11) 0.01933(10) -0.00780(8) -0.00532(7) -0.00039(8) Co2 0.01637(9) 0.03583(12) 0.02236(11) -0.01040(9) -0.00582(8) 0.00054(8) Cl1 0.02707(18) 0.0368(2) 0.0341(2) -0.01722(17) -0.01303(16) 0.00841(16) Cl2 0.03174(19) 0.02760(18) 0.02631(19) -0.01155(15) -0.00881(15) 0.00483(15) Cl3 0.0323(2) 0.0382(2) 0.0441(3) -0.01488(19) -0.00867(18) -0.00612(18) O1 0.0183(5) 0.0303(5) 0.0201(5) -0.0084(4) -0.0063(4) -0.0003(4) C1 0.0209(7) 0.0213(7) 0.0206(7) -0.0058(6) -0.0072(6) 0.0028(6) C2 0.0196(6) 0.0213(7) 0.0212(7) -0.0042(6) -0.0073(6) 0.0018(5) C3 0.0184(6) 0.0282(7) 0.0216(7) -0.0066(6) -0.0078(6) 0.0031(6) N4 0.0165(5) 0.0230(6) 0.0211(6) -0.0071(5) -0.0041(5) 0.0016(5) C5 0.0164(6) 0.0310(8) 0.0247(8) -0.0079(6) -0.0049(6) 0.0003(6) C6 0.0192(7) 0.0285(8) 0.0236(7) -0.0074(6) -0.0041(6) -0.0027(6) C7 0.0177(7) 0.0339(8) 0.0225(7) -0.0083(6) -0.0025(6) -0.0003(6) N8 0.0180(6) 0.0294(7) 0.0216(6) -0.0097(5) -0.0058(5) 0.0018(5) C9 0.0208(7) 0.0421(9) 0.0196(7) -0.0127(7) -0.0046(6) 0.0006(6) C10 0.0224(7) 0.0416(9) 0.0228(8) -0.0153(7) -0.0077(6) 0.0028(7) C11 0.0238(7) 0.0350(8) 0.0213(7) -0.0149(6) -0.0084(6) 0.0029(6) O11 0.0202(5) 0.0348(6) 0.0213(5) -0.0107(5) -0.0073(4) 0.0008(4) C12 0.0220(7) 0.0487(10) 0.0234(8) -0.0178(7) -0.0082(6) 0.0016(7) C13 0.0217(7) 0.0538(11) 0.0264(8) -0.0178(8) -0.0101(6) -0.0003(7) N14 0.0182(6) 0.0428(8) 0.0221(7) -0.0121(6) -0.0051(5) -0.0007(6) C15 0.0171(7) 0.0593(11) 0.0289(9) -0.0156(8) -0.0064(6) 0.0006(7) C16 0.0177(7) 0.0538(11) 0.0241(8) -0.0131(7) -0.0046(6) 0.0042(7) C17 0.0166(7) 0.0505(10) 0.0250(8) -0.0100(7) -0.0042(6) 0.0007(7) N18 0.0169(6) 0.0343(7) 0.0242(7) -0.0075(6) -0.0061(5) -0.0001(5) C19 0.0207(7) 0.0375(9) 0.0223(8) -0.0040(7) -0.0058(6) -0.0005(6) C20 0.0205(7) 0.0294(8) 0.0197(7) -0.0043(6) -0.0064(6) 0.0015(6) C21 0.0242(7) 0.0337(8) 0.0188(7) -0.0035(6) -0.0044(6) 0.0013(6) C22 0.0274(8) 0.0339(8) 0.0204(7) -0.0052(6) -0.0097(6) 0.0018(7) C23 0.0222(7) 0.0304(8) 0.0234(8) -0.0053(6) -0.0102(6) 0.0003(6) C24 0.0356(9) 0.0684(13) 0.0229(8) -0.0128(9) -0.0121(7) -0.0011(9) C25 0.097(3) 0.133(3) 0.0500(17) -0.0225(18) -0.0533(19) 0.045(2) C26 0.0506(14) 0.113(3) 0.0233(11) -0.0237(14) -0.0047(10) -0.0197(15) C27 0.0630(17) 0.109(3) 0.0403(14) -0.0365(15) -0.0123(12) -0.0280(18) C28 0.0341(9) 0.0261(8) 0.0324(9) -0.0083(7) -0.0116(7) 0.0004(7) C29 0.0241(8) 0.0459(10) 0.0320(9) -0.0064(8) -0.0039(7) -0.0105(7) C30 0.0259(8) 0.0531(11) 0.0196(8) -0.0123(7) -0.0066(6) 0.0015(7) C31 0.0288(8) 0.0614(12) 0.0206(8) -0.0153(8) -0.0112(7) 0.0087(8) C32 0.0226(7) 0.0642(12) 0.0250(8) -0.0201(8) -0.0101(6) 0.0067(8) C33 0.0323(9) 0.0868(16) 0.0212(8) -0.0115(9) -0.0118(7) 0.0113(10) C34 0.098(3) 0.075(3) 0.081(3) 0.018(2) -0.058(2) -0.006(2) C35 0.085(3) 0.121(3) 0.0275(14) -0.0243(17) -0.0268(16) 0.026(2) C36 0.0482(18) 0.120(3) 0.0308(15) 0.0020(18) -0.0098(13) 0.035(2) C37 0.0343(9) 0.0513(11) 0.0357(10) -0.0177(9) -0.0113(8) 0.0140(8) C38 0.0205(8) 0.0856(16) 0.0318(10) -0.0192(10) -0.0047(7) 0.0083(9) N41 0.0427(8) 0.0311(7) 0.0288(7) -0.0094(6) -0.0162(7) 0.0026(6) C42 0.0538(12) 0.0443(11) 0.0262(9) -0.0060(8) -0.0118(8) 0.0000(9) C43 0.0489(11) 0.0467(11) 0.0329(10) -0.0168(8) -0.0072(8) 0.0037(9) C44 0.0388(9) 0.0322(9) 0.0373(10) -0.0140(8) -0.0123(8) 0.0052(7) N45 0.0400(8) 0.0275(7) 0.0275(7) -0.0080(6) -0.0127(6) 0.0033(6) C46 0.0417(9) 0.0279(8) 0.0281(8) -0.0140(7) -0.0141(7) 0.0022(7) C47 0.0414(10) 0.0462(11) 0.0313(9) -0.0121(8) -0.0136(8) 0.0080(8) C48 0.0447(12) 0.0567(13) 0.0494(13) -0.0072(10) -0.0148(10) -0.0102(10) C49 0.0466(12) 0.0714(16) 0.0605(15) -0.0132(12) -0.0284(11) -0.0033(11) C50 0.0572(13) 0.0633(14) 0.0503(13) -0.0125(11) -0.0338(11) 0.0033(11) C51 0.0514(12) 0.0384(10) 0.0416(11) -0.0095(8) -0.0257(9) 0.0077(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.0772(10) . ? Co1 O11 2.1155(10) . ? Co1 N8 2.1201(13) . ? Co1 N4 2.1465(12) . ? Co1 Cl2 2.4267(4) . ? Co1 Cl1 2.6345(5) . ? Co2 O1 2.0969(10) . ? Co2 O11 2.1011(10) . ? Co2 N14 2.1299(13) . ? Co2 N18 2.1441(14) . ? Co2 Cl3 2.3696(5) . ? Co2 Cl1 2.7809(5) . ? O1 C1 1.3423(17) . ? C1 C20 1.410(2) . ? C1 C2 1.4131(19) . ? C2 C23 1.395(2) . ? C2 C3 1.498(2) . ? C3 N4 1.4871(18) . ? N4 C5 1.4778(18) . ? C5 C6 1.523(2) . ? C6 C28 1.522(2) . ? C6 C7 1.526(2) . ? C6 C29 1.541(2) . ? C7 N8 1.4800(18) . ? N8 C9 1.4845(19) . ? C9 C10 1.494(2) . ? C10 C30 1.392(2) . ? C10 C11 1.410(2) . ? C11 O11 1.3411(18) . ? C11 C12 1.409(2) . ? C12 C32 1.390(2) . ? C12 C13 1.500(2) . ? C13 N14 1.489(2) . ? N14 C15 1.476(2) . ? C15 C16 1.529(2) . ? C16 C37 1.514(3) . ? C16 C17 1.524(2) . ? C16 C38 1.544(2) . ? C17 N18 1.4774(18) . ? N18 C19 1.4821(19) . ? C19 C20 1.506(2) . ? C20 C21 1.395(2) . ? C21 C22 1.388(2) . ? C22 C23 1.386(2) . ? C22 C24 1.536(2) . ? C24 C27' 1.500(12) . ? C24 C26 1.507(3) . ? C24 C25 1.517(3) . ? C24 C26' 1.530(13) . ? C24 C27 1.547(3) . ? C24 C25' 1.558(12) . ? C30 C31 1.390(2) . ? C31 C32 1.386(2) . ? C31 C33 1.544(2) . ? C33 C34' 1.426(8) . ? C33 C36' 1.481(9) . ? C33 C35 1.492(4) . ? C33 C36 1.504(3) . ? C33 C34 1.574(4) . ? C33 C35' 1.629(9) . ? N41 C46 1.330(2) . ? N41 C42 1.460(2) . ? N41 C51 1.471(2) . ? C42 C43 1.517(3) . ? C43 C44 1.505(3) . ? C44 N45 1.454(2) . ? N45 C46 1.312(2) . ? C46 C47 1.485(2) . ? C47 C48 1.531(3) . ? C48 C49 1.527(3) . ? C49 C50 1.518(3) . ? C50 C51 1.517(3) . ? C61 C62 1.460(9) . ? C62 C63 1.390(10) . ? C63 C64 1.510(7) . ? C64 C65 1.346(10) . ? C65 C66 1.429(10) . ? C61' C62' 1.407(13) . ? C62' C63' 1.367(15) . ? C63' C64' 1.408(13) . ? C64' C65' 1.333(12) . ? C65' C66' 1.345(12) . ? O70 C71 1.458(10) . ? O70 C74 1.489(11) . ? C71 C72 1.431(12) . ? C72 C73 1.407(13) . ? C73 C74 1.394(11) . ? O70' C74' 1.481(14) . ? O70' C71' 1.515(11) . ? C71' C72' 1.414(11) . ? C72' C73' 1.443(13) . ? C73' C74' 1.472(13) . ? O70" C71" 1.524(15) . ? O70" C74" 1.539(13) . ? C71" C72" 1.420(13) . ? C72" C73" 1.360(13) . ? C73" C74" 1.511(12) . ? O70* C71* 1.461(12) . ? O70* C74* 1.527(13) . ? C71* C72* 1.419(12) . ? C72* C73* 1.413(13) . ? C73* C74* 1.468(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 O1 Co1 O11 85.80(4) . . ? O1 Co1 N8 171.82(5) . . ? O11 Co1 N8 90.98(4) . . ? O1 Co1 N4 89.65(4) . . ? O11 Co1 N4 172.91(4) . . ? N8 Co1 N4 92.80(5) . . ? O1 Co1 Cl2 96.82(3) . . ? O11 Co1 Cl2 94.95(3) . . ? N8 Co1 Cl2 90.94(4) . . ? N4 Co1 Cl2 90.98(3) . . ? O1 Co1 Cl1 81.08(3) . . ? O11 Co1 Cl1 79.20(3) . . ? N8 Co1 Cl1 90.94(4) . . ? N4 Co1 Cl1 94.74(3) . . ? Cl2 Co1 Cl1 173.885(15) . . ? O1 Co2 O11 85.67(4) . . ? O1 Co2 N14 165.36(5) . . ? O11 Co2 N14 90.48(4) . . ? O1 Co2 N18 88.85(4) . . ? O11 Co2 N18 166.12(5) . . ? N14 Co2 N18 91.65(5) . . ? O1 Co2 Cl3 100.59(3) . . ? O11 Co2 Cl3 100.74(3) . . ? N14 Co2 Cl3 94.00(4) . . ? N18 Co2 Cl3 92.80(4) . . ? O1 Co2 Cl1 77.26(3) . . ? O11 Co2 Cl1 76.03(3) . . ? N14 Co2 Cl1 88.11(4) . . ? N18 Co2 Cl1 90.33(4) . . ? Cl3 Co2 Cl1 176.175(17) . . ? Co1 Cl1 Co2 65.732(11) . . ? C1 O1 Co1 125.81(8) . . ? C1 O1 Co2 127.50(9) . . ? Co1 O1 Co2 89.61(4) . . ? O1 C1 C20 121.69(12) . . ? O1 C1 C2 121.59(13) . . ? C20 C1 C2 116.68(13) . . ? C23 C2 C1 120.19(13) . . ? C23 C2 C3 118.54(12) . . ? C1 C2 C3 121.26(13) . . ? N4 C3 C2 112.71(12) . . ? C5 N4 C3 108.32(11) . . ? C5 N4 Co1 118.36(9) . . ? C3 N4 Co1 108.95(8) . . ? N4 C5 C6 115.10(12) . . ? C28 C6 C5 111.55(13) . . ? C28 C6 C7 111.46(12) . . ? C5 C6 C7 111.47(13) . . ? C28 C6 C29 108.49(13) . . ? C5 C6 C29 106.67(12) . . ? C7 C6 C29 106.93(13) . . ? N8 C7 C6 114.44(12) . . ? C7 N8 C9 109.31(12) . . ? C7 N8 Co1 117.73(9) . . ? C9 N8 Co1 108.38(9) . . ? N8 C9 C10 111.55(13) . . ? C30 C10 C11 120.92(14) . . ? C30 C10 C9 118.36(14) . . ? C11 C10 C9 120.71(14) . . ? O11 C11 C12 121.98(14) . . ? O11 C11 C10 121.46(13) . . ? C12 C11 C10 116.55(14) . . ? C11 O11 Co2 124.06(9) . . ? C11 O11 Co1 122.60(9) . . ? Co2 O11 Co1 88.46(4) . . ? C32 C12 C11 120.47(15) . . ? C32 C12 C13 119.07(14) . . ? C11 C12 C13 120.44(14) . . ? N14 C13 C12 111.26(13) . . ? C15 N14 C13 109.49(12) . . ? C15 N14 Co2 118.22(10) . . ? C13 N14 Co2 107.40(10) . . ? N14 C15 C16 114.56(13) . . ? C37 C16 C17 111.62(14) . . ? C37 C16 C15 112.03(14) . . ? C17 C16 C15 111.47(15) . . ? C37 C16 C38 109.23(15) . . ? C17 C16 C38 106.43(14) . . ? C15 C16 C38 105.71(13) . . ? N18 C17 C16 115.21(13) . . ? C17 N18 C19 108.04(12) . . ? C17 N18 Co2 116.86(10) . . ? C19 N18 Co2 108.35(10) . . ? N18 C19 C20 112.92(12) . . ? C21 C20 C1 120.88(13) . . ? C21 C20 C19 118.04(13) . . ? C1 C20 C19 121.04(13) . . ? C22 C21 C20 122.96(14) . . ? C23 C22 C21 115.67(14) . . ? C23 C22 C24 120.90(14) . . ? C21 C22 C24 123.43(14) . . ? C22 C23 C2 123.60(13) . . ? C26 C24 C25 110.4(2) . . ? C27' C24 C26' 109.7(10) . . ? C27' C24 C22 117.4(9) . . ? C26 C24 C22 112.56(15) . . ? C25 C24 C22 108.86(18) . . ? C26' C24 C22 109.5(11) . . ? C26 C24 C27 107.6(2) . . ? C25 C24 C27 108.0(2) . . ? C22 C24 C27 109.35(16) . . ? C27' C24 C25' 106.9(10) . . ? C26' C24 C25' 106.5(10) . . ? C22 C24 C25' 106.2(10) . . ? C31 C30 C10 122.70(15) . . ? C32 C31 C30 115.73(15) . . ? C32 C31 C33 123.21(15) . . ? C30 C31 C33 121.04(15) . . ? C31 C32 C12 123.41(15) . . ? C34' C33 C36' 118.1(6) . . ? C35 C33 C36 111.0(2) . . ? C34' C33 C31 112.5(5) . . ? C36' C33 C31 108.9(6) . . ? C35 C33 C31 109.8(2) . . ? C36 C33 C31 112.48(17) . . ? C35 C33 C34 107.7(3) . . ? C36 C33 C34 106.0(3) . . ? C31 C33 C34 109.77(17) . . ? C34' C33 C35' 106.2(6) . . ? C36' C33 C35' 106.6(6) . . ? C31 C33 C35' 103.3(5) . . ? C46 N41 C42 121.90(15) . . ? C46 N41 C51 121.15(15) . . ? C42 N41 C51 116.31(14) . . ? N41 C42 C43 111.37(14) . . ? C44 C43 C42 108.84(15) . . ? N45 C44 C43 108.31(14) . . ? C46 N45 C44 122.89(14) . . ? N45 C46 N41 121.02(16) . . ? N45 C46 C47 118.69(15) . . ? N41 C46 C47 120.26(15) . . ? C46 C47 C48 114.42(16) . . ? C49 C48 C47 114.13(18) . . ? C50 C49 C48 114.57(19) . . ? C51 C50 C49 113.72(17) . . ? N41 C51 C50 113.49(16) . . ? C63 C62 C61 118.4(8) . . ? C62 C63 C64 120.2(9) . . ? C65 C64 C63 129.6(10) . . ? C64 C65 C66 128.2(11) . . ? C63' C62' C61' 135(2) . . ? C62' C63' C64' 138(2) . . ? C65' C64' C63' 148(3) . . ? C64' C65' C66' 155(2) . . ? C71 O70 C74 108.7(6) . . ? C72 C71 O70 104.9(7) . . ? C73 C72 C71 109.9(8) . . ? C74 C73 C72 110.7(8) . . ? C73 C74 O70 105.1(7) . . ? C74' O70' C71' 102.6(7) . . ? C72' C71' O70' 105.6(8) . . ? C71' C72' C73' 102.5(9) . . ? C72' C73' C74' 104.6(10) . . ? C73' C74' O70' 106.4(8) . . ? C71" O70" C74" 102.7(9) . . ? C72" C71" O70" 102.9(8) . . ? C73" C72" C71" 108.2(9) . . ? C72" C73" C74" 105.0(9) . . ? C73" C74" O70" 92.3(8) . . ? C71* O70* C74* 106.6(7) . . ? C72* C71* O70* 101.6(9) . . ? C73* C72* C71* 103.7(9) . . ? C72* C73* C74* 104.4(9) . . ? C73* C74* O70* 101.0(7) . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.467 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.057 #===END data_3c _database_code_depnum_ccdc_archive 'CCDC 825196' #TrackingRef '- kember et al_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H54 Cl3 Co2 N4 O2, C8 H16 N3' _chemical_formula_sum 'C42 H70 Cl3 Co2 N7 O2' _chemical_formula_weight 929.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0900(2) _cell_length_b 20.2875(3) _cell_length_c 15.7020(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.0816(15) _cell_angle_gamma 90.00 _cell_volume 4662.54(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11516 _cell_measurement_theta_min 2.1759 _cell_measurement_theta_max 72.4071 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 7.478 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.359 _exptl_absorpt_correction_T_max 0.824 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22211 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 72.56 _reflns_number_total 9062 _reflns_number_gt 7530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0657P)^2^+0.4120P] 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 SHELXL _refine_ls_extinction_coef 0.00030(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9062 _refine_ls_number_parameters 577 _refine_ls_number_restraints 202 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.83880(3) 0.04630(2) 0.66889(3) 0.02911(11) Uani 1 1 d . . . Co2 Co 0.81155(3) -0.05446(2) 0.79677(2) 0.02776(11) Uani 1 1 d . . . Cl1 Cl 0.88962(4) 0.07077(3) 0.83733(4) 0.03506(14) Uani 1 1 d . . . Cl2 Cl 0.78259(4) 0.02456(3) 0.51115(4) 0.03898(15) Uani 1 1 d . . . Cl3 Cl 0.74702(4) -0.16256(3) 0.76118(4) 0.03860(15) Uani 1 1 d . . . O1 O 0.72558(11) 0.00888(9) 0.70792(11) 0.0300(4) Uani 1 1 d . . . C1 C 0.65938(16) 0.04637(13) 0.72650(16) 0.0306(5) Uani 1 1 d . . . C2 C 0.63502(17) 0.10821(14) 0.68584(17) 0.0343(5) Uani 1 1 d . . . C3 C 0.68106(17) 0.13601(14) 0.61896(17) 0.0360(6) Uani 1 1 d . . . H3A H 0.6679 0.1070 0.5667 0.043 Uiso 1 1 calc R . . H3B H 0.6546 0.1799 0.6003 0.043 Uiso 1 1 calc R . . N4 N 0.78132(14) 0.14281(11) 0.65149(14) 0.0316(4) Uani 1 1 d D . . H4 H 0.793(2) 0.1586(15) 0.7067(8) 0.046(9) Uiso 1 1 d D . . C5 C 0.81477(17) 0.18896(14) 0.59275(17) 0.0353(6) Uani 1 1 d . . . H5A H 0.7874 0.2328 0.5971 0.042 Uiso 1 1 calc R . . H5B H 0.7921 0.1735 0.5315 0.042 Uiso 1 1 calc R . . C6 C 0.91835(18) 0.19709(13) 0.61112(17) 0.0359(6) Uani 1 1 d . . . C7 C 0.96499(18) 0.13480(13) 0.58852(17) 0.0359(6) Uani 1 1 d . . . H7A H 0.9339 0.1212 0.5281 0.043 Uiso 1 1 calc R . . H7B H 1.0289 0.1459 0.5886 0.043 Uiso 1 1 calc R . . N8 N 0.96608(14) 0.07812(11) 0.64744(14) 0.0311(4) Uani 1 1 d D . . H8 H 0.9998(18) 0.0897(16) 0.7008(9) 0.045(9) Uiso 1 1 d D . . C9 C 1.00891(18) 0.02057(14) 0.61370(18) 0.0356(6) Uani 1 1 d . . . H9A H 1.0594 0.0364 0.5889 0.043 Uiso 1 1 calc R . . H9B H 0.9630 -0.0008 0.5658 0.043 Uiso 1 1 calc R . . C10 C 1.04532(18) -0.02911(13) 0.68380(17) 0.0332(5) Uani 1 1 d . . . C11 C 0.98745(16) -0.05885(12) 0.73113(16) 0.0288(5) Uani 1 1 d . . . O11 O 0.89779(11) -0.04506(8) 0.71273(11) 0.0296(4) Uani 1 1 d . . . C12 C 1.02823(17) -0.10382(12) 0.79726(16) 0.0304(5) Uani 1 1 d . . . C13 C 0.97418(18) -0.13904(13) 0.85215(17) 0.0335(5) Uani 1 1 d . . . H13A H 0.9312 -0.1700 0.8144 0.040 Uiso 1 1 calc R . . H13B H 1.0165 -0.1653 0.8977 0.040 Uiso 1 1 calc R . . N14 N 0.92155(13) -0.09314(10) 0.89558(13) 0.0287(4) Uani 1 1 d D . . H14 H 0.9571(16) -0.0589(9) 0.9192(18) 0.033(8) Uiso 1 1 d D . . C15 C 0.90010(17) -0.12737(13) 0.97110(16) 0.0331(5) Uani 1 1 d . . . H15A H 0.9583 -0.1373 1.0142 0.040 Uiso 1 1 calc R . . H15B H 0.8708 -0.1700 0.9503 0.040 Uiso 1 1 calc R . . C16 C 0.83806(16) -0.09020(13) 1.01848(16) 0.0322(5) Uani 1 1 d . . . C17 C 0.74063(16) -0.08575(14) 0.96167(16) 0.0322(5) Uani 1 1 d . . . H17A H 0.7212 -0.1301 0.9380 0.039 Uiso 1 1 calc R . . H17B H 0.6997 -0.0723 0.9992 0.039 Uiso 1 1 calc R . . N18 N 0.72911(14) -0.03918(11) 0.88790(13) 0.0287(4) Uani 1 1 d D . . H18 H 0.7426(19) 0.0016(6) 0.9097(18) 0.035(8) Uiso 1 1 d D . . C19 C 0.63258(16) -0.03814(14) 0.83674(17) 0.0336(5) Uani 1 1 d . . . H19A H 0.5920 -0.0437 0.8771 0.040 Uiso 1 1 calc R . . H19B H 0.6217 -0.0755 0.7949 0.040 Uiso 1 1 calc R . . C20 C 0.60971(16) 0.02523(14) 0.78705(16) 0.0330(5) Uani 1 1 d . . . C21 C 0.53874(17) 0.06318(14) 0.80335(18) 0.0369(6) Uani 1 1 d . . . H21A H 0.5066 0.0472 0.8441 0.044 Uiso 1 1 calc R . . C22 C 0.51287(17) 0.12339(15) 0.76262(18) 0.0376(6) Uani 1 1 d . A . C23 C 0.56376(17) 0.14457(14) 0.70485(18) 0.0372(6) Uani 1 1 d . . . H23A H 0.5492 0.1860 0.6768 0.045 Uiso 1 1 calc R . . C24 C 0.43217(19) 0.16359(15) 0.77740(19) 0.0459(7) Uani 1 1 d D . . C25 C 0.3906(5) 0.1366(3) 0.8485(4) 0.0530(15) Uani 0.691(4) 1 d PDU A 1 H25A H 0.3631 0.0935 0.8305 0.079 Uiso 0.691(4) 1 calc PR A 1 H25B H 0.3435 0.1670 0.8581 0.079 Uiso 0.691(4) 1 calc PR A 1 H25C H 0.4383 0.1318 0.9030 0.079 Uiso 0.691(4) 1 calc PR A 1 C26 C 0.4677(4) 0.23477(19) 0.8109(4) 0.0479(12) Uani 0.691(4) 1 d PDU A 1 H26A H 0.5290 0.2313 0.8499 0.072 Uiso 0.691(4) 1 calc PR A 1 H26B H 0.4261 0.2544 0.8429 0.072 Uiso 0.691(4) 1 calc PR A 1 H26C H 0.4699 0.2626 0.7604 0.072 Uiso 0.691(4) 1 calc PR A 1 C27 C 0.3622(4) 0.1734(4) 0.6908(4) 0.0774(19) Uani 0.691(4) 1 d PDU A 1 H27A H 0.3380 0.1305 0.6674 0.116 Uiso 0.691(4) 1 calc PR A 1 H27B H 0.3912 0.1951 0.6489 0.116 Uiso 0.691(4) 1 calc PR A 1 H27C H 0.3121 0.2010 0.7003 0.116 Uiso 0.691(4) 1 calc PR A 1 C25' C 0.4141(13) 0.1420(12) 0.8659(7) 0.040(4) Uiso 0.242(8) 1 d PDU A 2 H25D H 0.3872 0.0977 0.8599 0.060 Uiso 0.242(8) 1 calc PR A 2 H25E H 0.3719 0.1731 0.8831 0.060 Uiso 0.242(8) 1 calc PR A 2 H25F H 0.4719 0.1414 0.9110 0.060 Uiso 0.242(8) 1 calc PR A 2 C26' C 0.4429(13) 0.2374(4) 0.7763(15) 0.058(4) Uiso 0.242(8) 1 d PDU A 2 H26D H 0.4012 0.2555 0.7236 0.088 Uiso 0.242(8) 1 calc PR A 2 H26E H 0.5060 0.2484 0.7758 0.088 Uiso 0.242(8) 1 calc PR A 2 H26F H 0.4284 0.2563 0.8287 0.088 Uiso 0.242(8) 1 calc PR A 2 C27' C 0.3462(9) 0.1417(9) 0.7062(9) 0.053(4) Uiso 0.242(8) 1 d PDU A 2 H27D H 0.3439 0.0935 0.7030 0.080 Uiso 0.242(8) 1 calc PR A 2 H27E H 0.3494 0.1597 0.6491 0.080 Uiso 0.242(8) 1 calc PR A 2 H27F H 0.2911 0.1583 0.7216 0.080 Uiso 0.242(8) 1 calc PR A 2 C25" C 0.423(3) 0.174(3) 0.8716(12) 0.060(6) Uiso 0.067(8) 1 d PDU A 3 H25G H 0.3964 0.1344 0.8913 0.090 Uiso 0.067(8) 1 calc PR A 3 H25H H 0.3835 0.2119 0.8734 0.090 Uiso 0.067(8) 1 calc PR A 3 H25I H 0.4836 0.1820 0.9104 0.090 Uiso 0.067(8) 1 calc PR A 3 C26" C 0.425(3) 0.2303(13) 0.731(3) 0.046(9) Uiso 0.067(8) 1 d PDU A 3 H26G H 0.3855 0.2259 0.6713 0.068 Uiso 0.067(8) 1 calc PR A 3 H26H H 0.4857 0.2449 0.7274 0.068 Uiso 0.067(8) 1 calc PR A 3 H26I H 0.3982 0.2627 0.7636 0.068 Uiso 0.067(8) 1 calc PR A 3 C27" C 0.349(2) 0.122(2) 0.729(3) 0.052(9) Uiso 0.067(8) 1 d PDU A 3 H27G H 0.3662 0.0752 0.7310 0.077 Uiso 0.067(8) 1 calc PR A 3 H27H H 0.3294 0.1361 0.6675 0.077 Uiso 0.067(8) 1 calc PR A 3 H27I H 0.2985 0.1278 0.7574 0.077 Uiso 0.067(8) 1 calc PR A 3 C28 C 0.9586(2) 0.21863(15) 0.70586(19) 0.0438(6) Uani 1 1 d . . . H28A H 1.0249 0.2235 0.7159 0.066 Uiso 1 1 calc R . . H28B H 0.9449 0.1853 0.7460 0.066 Uiso 1 1 calc R . . H28C H 0.9316 0.2609 0.7165 0.066 Uiso 1 1 calc R . . C29 C 0.9349(2) 0.25100(15) 0.5482(2) 0.0458(7) Uani 1 1 d . . . H29A H 0.9089 0.2372 0.4875 0.069 Uiso 1 1 calc R . . H29B H 1.0007 0.2583 0.5572 0.069 Uiso 1 1 calc R . . H29C H 0.9055 0.2920 0.5599 0.069 Uiso 1 1 calc R . . C30 C 1.13721(18) -0.04606(13) 0.69995(18) 0.0365(6) Uani 1 1 d . . . H30A H 1.1739 -0.0255 0.6662 0.044 Uiso 1 1 calc R . . C31 C 1.17753(18) -0.09184(14) 0.76351(18) 0.0372(6) Uani 1 1 d . B . C32 C 1.12113(17) -0.11905(13) 0.81180(17) 0.0340(5) Uani 1 1 d . . . H32A H 1.1468 -0.1495 0.8570 0.041 Uiso 1 1 calc R . . C33 C 1.27819(19) -0.11117(15) 0.7767(2) 0.0516(8) Uani 1 1 d D . . C34 C 1.3368(5) -0.0508(3) 0.7871(7) 0.062(2) Uani 0.513(4) 1 d PDU B 1 H34A H 1.3402 -0.0348 0.7291 0.092 Uiso 0.513(4) 1 calc PR B 1 H34B H 1.3984 -0.0616 0.8217 0.092 Uiso 0.513(4) 1 calc PR B 1 H34C H 1.3103 -0.0165 0.8173 0.092 Uiso 0.513(4) 1 calc PR B 1 C35 C 1.2861(5) -0.1505(4) 0.6910(4) 0.0518(18) Uani 0.513(4) 1 d PDU B 1 H35A H 1.2272 -0.1491 0.6475 0.078 Uiso 0.513(4) 1 calc PR B 1 H35B H 1.3027 -0.1964 0.7064 0.078 Uiso 0.513(4) 1 calc PR B 1 H35C H 1.3331 -0.1301 0.6662 0.078 Uiso 0.513(4) 1 calc PR B 1 C36 C 1.3088(5) -0.1607(4) 0.8498(5) 0.0494(18) Uani 0.513(4) 1 d PDU B 1 H36A H 1.2971 -0.2054 0.8261 0.074 Uiso 0.513(4) 1 calc PR B 1 H36B H 1.2749 -0.1535 0.8949 0.074 Uiso 0.513(4) 1 calc PR B 1 H36C H 1.3744 -0.1552 0.8758 0.074 Uiso 0.513(4) 1 calc PR B 1 C34' C 1.3363(10) -0.0748(8) 0.7243(10) 0.067(4) Uiso 0.248(6) 1 d PDU B 2 H34D H 1.3162 -0.0871 0.6622 0.100 Uiso 0.248(6) 1 calc PR B 2 H34E H 1.4007 -0.0869 0.7467 0.100 Uiso 0.248(6) 1 calc PR B 2 H34F H 1.3293 -0.0272 0.7303 0.100 Uiso 0.248(6) 1 calc PR B 2 C35' C 1.2987(12) -0.1838(4) 0.7842(11) 0.076(5) Uiso 0.248(6) 1 d PD B 2 H35D H 1.2738 -0.2050 0.7274 0.114 Uiso 0.248(6) 1 calc PR B 2 H35E H 1.2707 -0.2032 0.8285 0.114 Uiso 0.248(6) 1 calc PR B 2 H35F H 1.3650 -0.1904 0.8017 0.114 Uiso 0.248(6) 1 calc PR B 2 C36' C 1.3240(11) -0.0847(8) 0.8743(6) 0.074(5) Uiso 0.248(6) 1 d PD B 2 H36D H 1.2788 -0.0594 0.8961 0.111 Uiso 0.248(6) 1 calc PR B 2 H36E H 1.3762 -0.0563 0.8727 0.111 Uiso 0.248(6) 1 calc PR B 2 H36F H 1.3449 -0.1222 0.9133 0.111 Uiso 0.248(6) 1 calc PR B 2 C34" C 1.3355(12) -0.0543(7) 0.7545(11) 0.043(4) Uiso 0.239(8) 1 d PDU B 3 H34G H 1.3284 -0.0524 0.6908 0.064 Uiso 0.239(8) 1 calc PR B 3 H34H H 1.4000 -0.0614 0.7837 0.064 Uiso 0.239(8) 1 calc PR B 3 H34I H 1.3148 -0.0126 0.7747 0.064 Uiso 0.239(8) 1 calc PR B 3 C35" C 1.2786(17) -0.1649(8) 0.7059(10) 0.064(5) Uiso 0.239(8) 1 d PDU B 3 H35G H 1.2336 -0.1535 0.6516 0.096 Uiso 0.239(8) 1 calc PR B 3 H35H H 1.2630 -0.2077 0.7273 0.096 Uiso 0.239(8) 1 calc PR B 3 H35I H 1.3395 -0.1673 0.6944 0.096 Uiso 0.239(8) 1 calc PR B 3 C36" C 1.3203(13) -0.1405(8) 0.8661(7) 0.048(4) Uiso 0.239(8) 1 d PDU B 3 H36G H 1.3178 -0.1887 0.8621 0.073 Uiso 0.239(8) 1 calc PR B 3 H36H H 1.2864 -0.1255 0.9083 0.073 Uiso 0.239(8) 1 calc PR B 3 H36I H 1.3841 -0.1264 0.8856 0.073 Uiso 0.239(8) 1 calc PR B 3 C37 C 0.87558(19) -0.02217(15) 1.04943(18) 0.0404(6) Uani 1 1 d . . . H37A H 0.8771 0.0052 0.9984 0.061 Uiso 1 1 calc R . . H37B H 0.9376 -0.0266 1.0868 0.061 Uiso 1 1 calc R . . H37C H 0.8362 -0.0014 1.0830 0.061 Uiso 1 1 calc R . . C38 C 0.83548(19) -0.13180(17) 1.09979(18) 0.0446(7) Uani 1 1 d . . . H38A H 0.7964 -0.1101 1.1329 0.067 Uiso 1 1 calc R . . H38B H 0.8975 -0.1362 1.1371 0.067 Uiso 1 1 calc R . . H38C H 0.8109 -0.1756 1.0811 0.067 Uiso 1 1 calc R . . N41 N 0.6183(2) -0.20416(15) 0.56035(17) 0.0577(7) Uani 1 1 d . . . C42 C 0.6329(3) -0.27072(18) 0.5912(2) 0.0599(9) Uani 1 1 d . . . H42A H 0.5763 -0.2966 0.5698 0.072 Uiso 1 1 calc R . . H42B H 0.6483 -0.2712 0.6562 0.072 Uiso 1 1 calc R . . C43 C 0.7101(3) -0.3020(2) 0.5589(3) 0.0742(12) Uani 1 1 d . . . H43A H 0.7266 -0.3451 0.5881 0.089 Uiso 1 1 calc R . . H43B H 0.6905 -0.3095 0.4948 0.089 Uiso 1 1 calc R . . C44 C 0.7904(3) -0.25719(16) 0.5793(2) 0.0580(9) Uani 1 1 d . . . H44A H 0.8152 -0.2554 0.6437 0.070 Uiso 1 1 calc R . . H44B H 0.8386 -0.2751 0.5529 0.070 Uiso 1 1 calc R . . N45 N 0.76720(19) -0.19124(13) 0.54648(17) 0.0494(6) Uani 1 1 d . . . C46 C 0.6838(2) -0.16456(16) 0.54643(17) 0.0443(7) Uani 1 1 d . . . N47 N 0.66990(19) -0.10223(14) 0.52645(18) 0.0543(7) Uani 1 1 d . . . H47 H 0.7157 -0.0785 0.5141 0.082 Uiso 1 1 calc R . . C48 C 0.5819(2) -0.0693(2) 0.5233(3) 0.0623(9) Uani 1 1 d . . . H48A H 0.5925 -0.0221 0.5388 0.075 Uiso 1 1 calc R . . H48B H 0.5419 -0.0721 0.4633 0.075 Uiso 1 1 calc R . . C49 C 0.5377(3) -0.1018(3) 0.5861(3) 0.0762(12) Uani 1 1 d . . . H49A H 0.4756 -0.0833 0.5792 0.091 Uiso 1 1 calc R . . H49B H 0.5731 -0.0922 0.6466 0.091 Uiso 1 1 calc R . . C50 C 0.5308(2) -0.1742(2) 0.5733(3) 0.0721(12) Uani 1 1 d . . . H50A H 0.4805 -0.1842 0.5214 0.087 Uiso 1 1 calc R . . H50B H 0.5155 -0.1947 0.6251 0.087 Uiso 1 1 calc R . . C51 C 0.8404(2) -0.14764(17) 0.5387(2) 0.0546(8) Uani 1 1 d . . . H51A H 0.8214 -0.1217 0.4847 0.082 Uiso 1 1 calc R . . H51B H 0.8945 -0.1737 0.5367 0.082 Uiso 1 1 calc R . . H51C H 0.8550 -0.1179 0.5894 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0295(2) 0.0320(2) 0.0285(2) 0.00449(16) 0.01207(16) 0.00243(16) Co2 0.0275(2) 0.0320(2) 0.0255(2) 0.00270(15) 0.00970(15) 0.00123(16) Cl1 0.0377(3) 0.0356(3) 0.0315(3) -0.0005(2) 0.0077(2) 0.0015(2) Cl2 0.0465(3) 0.0432(4) 0.0285(3) 0.0014(3) 0.0116(2) -0.0043(3) Cl3 0.0433(3) 0.0375(3) 0.0344(3) -0.0056(2) 0.0083(2) -0.0082(3) O1 0.0270(8) 0.0356(9) 0.0295(8) 0.0032(7) 0.0107(7) 0.0020(7) C1 0.0242(11) 0.0393(14) 0.0285(12) 0.0022(10) 0.0070(9) 0.0011(10) C2 0.0286(12) 0.0437(15) 0.0319(12) 0.0054(11) 0.0098(10) 0.0032(11) C3 0.0320(12) 0.0419(15) 0.0350(13) 0.0115(11) 0.0099(10) 0.0066(11) N4 0.0333(11) 0.0338(11) 0.0299(10) 0.0052(9) 0.0117(8) 0.0030(9) C5 0.0372(13) 0.0352(14) 0.0366(13) 0.0107(11) 0.0147(11) 0.0044(11) C6 0.0379(14) 0.0358(14) 0.0364(13) 0.0043(11) 0.0137(11) 0.0007(11) C7 0.0375(13) 0.0378(14) 0.0373(13) 0.0081(11) 0.0186(11) 0.0012(11) N8 0.0323(11) 0.0329(11) 0.0313(11) 0.0040(9) 0.0138(9) 0.0025(9) C9 0.0397(13) 0.0389(14) 0.0345(13) 0.0044(11) 0.0211(11) 0.0048(11) C10 0.0373(13) 0.0328(13) 0.0331(13) 0.0015(10) 0.0155(11) 0.0048(11) C11 0.0288(12) 0.0305(12) 0.0301(12) -0.0037(10) 0.0131(10) 0.0027(10) O11 0.0308(8) 0.0322(9) 0.0290(8) 0.0025(7) 0.0133(7) 0.0023(7) C12 0.0342(12) 0.0285(12) 0.0317(12) -0.0008(10) 0.0139(10) 0.0032(10) C13 0.0369(13) 0.0318(13) 0.0353(13) 0.0034(11) 0.0155(11) 0.0055(11) N14 0.0309(10) 0.0307(11) 0.0266(10) 0.0001(8) 0.0108(8) -0.0004(8) C15 0.0306(12) 0.0388(14) 0.0313(12) 0.0067(11) 0.0103(10) 0.0015(11) C16 0.0315(12) 0.0396(14) 0.0264(11) 0.0028(10) 0.0092(10) 0.0003(11) C17 0.0293(12) 0.0396(14) 0.0291(12) 0.0047(10) 0.0099(10) -0.0015(10) N18 0.0280(10) 0.0327(11) 0.0269(10) 0.0003(8) 0.0094(8) -0.0014(8) C19 0.0250(11) 0.0436(15) 0.0333(13) 0.0062(11) 0.0091(10) -0.0015(10) C20 0.0280(12) 0.0400(14) 0.0317(13) 0.0026(11) 0.0084(10) 0.0003(11) C21 0.0293(13) 0.0468(16) 0.0381(14) 0.0047(12) 0.0150(11) 0.0021(11) C22 0.0296(12) 0.0444(15) 0.0406(14) 0.0013(12) 0.0123(11) 0.0047(11) C23 0.0322(13) 0.0418(15) 0.0390(14) 0.0070(12) 0.0113(11) 0.0076(11) C24 0.0379(14) 0.0547(18) 0.0499(16) 0.0024(14) 0.0200(13) 0.0118(13) C25 0.049(4) 0.042(3) 0.080(3) -0.009(3) 0.040(3) -0.001(3) C26 0.052(3) 0.040(2) 0.062(3) 0.013(2) 0.033(3) 0.0130(19) C27 0.050(3) 0.111(5) 0.065(3) -0.015(3) 0.004(2) 0.037(3) C28 0.0471(16) 0.0402(16) 0.0451(16) -0.0009(13) 0.0132(13) -0.0057(13) C29 0.0469(16) 0.0405(16) 0.0558(18) 0.0127(14) 0.0240(14) -0.0004(13) C30 0.0343(13) 0.0398(15) 0.0412(14) 0.0039(11) 0.0201(11) 0.0023(11) C31 0.0336(13) 0.0392(14) 0.0422(14) 0.0012(12) 0.0154(11) 0.0054(11) C32 0.0346(13) 0.0340(13) 0.0354(13) 0.0024(11) 0.0120(10) 0.0058(11) C33 0.0326(14) 0.0556(19) 0.072(2) 0.0204(17) 0.0229(14) 0.0084(13) C34 0.032(3) 0.065(5) 0.085(6) 0.009(4) 0.007(4) -0.009(3) C35 0.038(3) 0.065(4) 0.062(4) 0.010(3) 0.032(3) 0.022(3) C36 0.028(3) 0.054(4) 0.063(4) 0.014(4) 0.006(3) 0.006(3) C37 0.0384(14) 0.0497(17) 0.0323(13) -0.0062(12) 0.0073(11) -0.0023(12) C38 0.0410(14) 0.0633(19) 0.0322(13) 0.0126(13) 0.0142(11) 0.0043(14) N41 0.0638(17) 0.0678(19) 0.0385(13) 0.0020(13) 0.0066(12) -0.0282(15) C42 0.077(2) 0.057(2) 0.0481(18) -0.0084(16) 0.0195(17) -0.0334(18) C43 0.111(3) 0.054(2) 0.068(2) -0.0163(19) 0.040(2) -0.025(2) C44 0.085(2) 0.0409(17) 0.057(2) -0.0055(15) 0.0357(18) -0.0060(17) N45 0.0606(16) 0.0473(15) 0.0434(13) -0.0048(11) 0.0187(12) -0.0135(13) C46 0.0521(17) 0.0536(18) 0.0264(13) -0.0038(12) 0.0081(11) -0.0162(14) N47 0.0560(16) 0.0549(17) 0.0519(15) 0.0045(13) 0.0126(12) -0.0120(13) C48 0.0462(18) 0.070(2) 0.068(2) 0.0059(19) 0.0086(16) -0.0044(17) C49 0.052(2) 0.109(4) 0.065(2) 0.013(2) 0.0097(18) -0.001(2) C50 0.0394(18) 0.103(3) 0.069(2) 0.028(2) 0.0020(16) -0.0163(19) C51 0.0591(19) 0.0483(18) 0.066(2) -0.0043(16) 0.0334(17) -0.0063(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 Co1 O1 2.0931(16) . ? Co1 O11 2.0985(17) . ? Co1 N8 2.129(2) . ? Co1 N4 2.132(2) . ? Co1 Cl2 2.4549(7) . ? Co1 Cl1 2.6159(7) . ? Co2 O11 2.0752(16) . ? Co2 O1 2.0975(17) . ? Co2 N14 2.127(2) . ? Co2 N18 2.1349(19) . ? Co2 Cl3 2.4095(7) . ? Co2 Cl1 2.8077(8) . ? O1 C1 1.343(3) . ? C1 C20 1.413(3) . ? C1 C2 1.415(4) . ? C2 C23 1.395(4) . ? C2 C3 1.503(3) . ? C3 N4 1.481(3) . ? N4 C5 1.486(3) . ? C5 C6 1.528(4) . ? C6 C28 1.527(4) . ? C6 C7 1.529(4) . ? C6 C29 1.534(4) . ? C7 N8 1.474(3) . ? N8 C9 1.493(3) . ? C9 C10 1.495(4) . ? C10 C30 1.391(4) . ? C10 C11 1.412(3) . ? C11 O11 1.342(3) . ? C11 C12 1.406(4) . ? C12 C32 1.399(3) . ? C12 C13 1.504(3) . ? C13 N14 1.492(3) . ? N14 C15 1.477(3) . ? C15 C16 1.529(3) . ? C16 C17 1.526(3) . ? C16 C37 1.526(4) . ? C16 C38 1.539(4) . ? C17 N18 1.472(3) . ? N18 C19 1.483(3) . ? C19 C20 1.500(4) . ? C20 C21 1.392(4) . ? C21 C22 1.390(4) . ? C22 C23 1.391(4) . ? C22 C24 1.530(4) . ? C24 C26' 1.507(8) . ? C24 C25 1.510(5) . ? C24 C27 1.518(5) . ? C24 C26" 1.530(9) . ? C24 C25" 1.533(9) . ? C24 C25' 1.544(8) . ? C24 C27" 1.553(9) . ? C24 C27' 1.557(8) . ? C24 C26 1.585(5) . ? C30 C31 1.390(4) . ? C31 C32 1.385(4) . ? C31 C33 1.533(4) . ? C33 C34 1.496(6) . ? C33 C35' 1.504(8) . ? C33 C36 1.510(5) . ? C33 C36" 1.514(8) . ? C33 C34' 1.531(7) . ? C33 C34" 1.533(8) . ? C33 C35" 1.558(8) . ? C33 C35 1.595(6) . ? C33 C36' 1.611(8) . ? N41 C46 1.332(4) . ? N41 C42 1.434(5) . ? N41 C50 1.511(5) . ? C42 C43 1.518(6) . ? C43 C44 1.486(5) . ? C44 N45 1.446(4) . ? N45 C46 1.370(4) . ? N45 C51 1.443(4) . ? C46 N47 1.307(4) . ? N47 C48 1.477(5) . ? C48 C49 1.474(5) . ? C49 C50 1.484(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O11 83.97(7) . . ? O1 Co1 N8 171.23(8) . . ? O11 Co1 N8 89.58(7) . . ? O1 Co1 N4 92.00(7) . . ? O11 Co1 N4 168.55(7) . . ? N8 Co1 N4 93.20(8) . . ? O1 Co1 Cl2 97.12(5) . . ? O11 Co1 Cl2 100.79(5) . . ? N8 Co1 Cl2 89.91(6) . . ? N4 Co1 Cl2 90.33(6) . . ? O1 Co1 Cl1 80.34(5) . . ? O11 Co1 Cl1 80.76(5) . . ? N8 Co1 Cl1 92.78(6) . . ? N4 Co1 Cl1 88.01(6) . . ? Cl2 Co1 Cl1 176.91(3) . . ? O11 Co2 O1 84.43(6) . . ? O11 Co2 N14 89.94(7) . . ? O1 Co2 N14 163.27(8) . . ? O11 Co2 N18 166.09(8) . . ? O1 Co2 N18 89.42(7) . . ? N14 Co2 N18 92.48(8) . . ? O11 Co2 Cl3 102.52(5) . . ? O1 Co2 Cl3 104.69(5) . . ? N14 Co2 Cl3 91.89(6) . . ? N18 Co2 Cl3 91.10(6) . . ? O11 Co2 Cl1 76.57(5) . . ? O1 Co2 Cl1 75.76(5) . . ? N14 Co2 Cl1 87.62(6) . . ? N18 Co2 Cl1 89.85(6) . . ? Cl3 Co2 Cl1 178.96(3) . . ? Co1 Cl1 Co2 66.126(18) . . ? C1 O1 Co1 124.16(15) . . ? C1 O1 Co2 125.10(14) . . ? Co1 O1 Co2 90.00(6) . . ? O1 C1 C20 121.2(2) . . ? O1 C1 C2 122.0(2) . . ? C20 C1 C2 116.8(2) . . ? C23 C2 C1 120.1(2) . . ? C23 C2 C3 117.6(2) . . ? C1 C2 C3 122.3(2) . . ? N4 C3 C2 113.7(2) . . ? C3 N4 C5 108.50(19) . . ? C3 N4 Co1 107.96(17) . . ? C5 N4 Co1 117.98(15) . . ? N4 C5 C6 115.9(2) . . ? C28 C6 C5 111.1(2) . . ? C28 C6 C7 111.5(2) . . ? C5 C6 C7 112.0(2) . . ? C28 C6 C29 109.6(2) . . ? C5 C6 C29 105.9(2) . . ? C7 C6 C29 106.5(2) . . ? N8 C7 C6 115.8(2) . . ? C7 N8 C9 109.11(18) . . ? C7 N8 Co1 117.59(16) . . ? C9 N8 Co1 107.71(16) . . ? N8 C9 C10 112.3(2) . . ? C30 C10 C11 121.0(2) . . ? C30 C10 C9 118.2(2) . . ? C11 C10 C9 120.8(2) . . ? O11 C11 C12 122.1(2) . . ? O11 C11 C10 121.2(2) . . ? C12 C11 C10 116.7(2) . . ? C11 O11 Co2 126.81(15) . . ? C11 O11 Co1 125.42(15) . . ? Co2 O11 Co1 90.47(6) . . ? C32 C12 C11 120.3(2) . . ? C32 C12 C13 117.6(2) . . ? C11 C12 C13 122.0(2) . . ? N14 C13 C12 112.9(2) . . ? C15 N14 C13 108.58(19) . . ? C15 N14 Co2 118.33(15) . . ? C13 N14 Co2 107.73(15) . . ? N14 C15 C16 116.0(2) . . ? C17 C16 C37 111.3(2) . . ? C17 C16 C15 111.2(2) . . ? C37 C16 C15 112.2(2) . . ? C17 C16 C38 107.6(2) . . ? C37 C16 C38 108.3(2) . . ? C15 C16 C38 106.0(2) . . ? N18 C17 C16 114.2(2) . . ? C17 N18 C19 110.36(19) . . ? C17 N18 Co2 117.24(15) . . ? C19 N18 Co2 107.14(15) . . ? N18 C19 C20 111.4(2) . . ? C21 C20 C1 120.9(2) . . ? C21 C20 C19 117.9(2) . . ? C1 C20 C19 121.2(2) . . ? C22 C21 C20 122.9(2) . . ? C21 C22 C23 115.7(2) . . ? C21 C22 C24 122.9(2) . . ? C23 C22 C24 121.3(2) . . ? C22 C23 C2 123.5(3) . . ? C25 C24 C27 112.7(4) . . ? C26' C24 C22 115.9(8) . . ? C25 C24 C22 114.1(3) . . ? C27 C24 C22 109.9(3) . . ? C26" C24 C22 111.6(16) . . ? C26" C24 C25" 109.2(12) . . ? C22 C24 C25" 118.7(19) . . ? C26' C24 C25' 109.6(9) . . ? C22 C24 C25' 107.8(9) . . ? C26" C24 C27" 106.9(11) . . ? C22 C24 C27" 102.3(18) . . ? C25" C24 C27" 107.2(11) . . ? C26' C24 C27' 110.3(8) . . ? C22 C24 C27' 107.1(7) . . ? C25' C24 C27' 105.5(7) . . ? C25 C24 C26 104.7(3) . . ? C27 C24 C26 106.4(4) . . ? C22 C24 C26 108.6(3) . . ? C31 C30 C10 122.6(2) . . ? C32 C31 C30 116.1(2) . . ? C32 C31 C33 123.0(2) . . ? C30 C31 C33 120.9(2) . . ? C31 C32 C12 123.2(2) . . ? C34 C33 C36 113.4(5) . . ? C35' C33 C34' 112.3(8) . . ? C36" C33 C34" 112.0(8) . . ? C34 C33 C31 110.2(4) . . ? C35' C33 C31 116.1(7) . . ? C36 C33 C31 112.5(3) . . ? C36" C33 C31 113.9(8) . . ? C34' C33 C31 118.9(7) . . ? C34" C33 C31 111.8(8) . . ? C36" C33 C35" 108.2(8) . . ? C34" C33 C35" 105.3(8) . . ? C31 C33 C35" 105.0(10) . . ? C34 C33 C35 109.7(5) . . ? C36 C33 C35 103.7(5) . . ? C31 C33 C35 106.8(3) . . ? C35' C33 C36' 102.7(7) . . ? C34' C33 C36' 100.4(7) . . ? C31 C33 C36' 103.0(6) . . ? C46 N41 C42 124.3(3) . . ? C46 N41 C50 119.1(3) . . ? C42 N41 C50 113.7(3) . . ? N41 C42 C43 110.4(3) . . ? C44 C43 C42 108.9(3) . . ? N45 C44 C43 112.0(3) . . ? C46 N45 C51 118.7(3) . . ? C46 N45 C44 120.6(3) . . ? C51 N45 C44 118.3(3) . . ? N47 C46 N41 122.7(3) . . ? N47 C46 N45 118.4(3) . . ? N41 C46 N45 118.7(3) . . ? C46 N47 C48 122.4(3) . . ? C49 C48 N47 109.0(3) . . ? C48 C49 C50 112.4(4) . . ? C49 C50 N41 112.5(3) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 72.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.580 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.055 #===END data_4a _database_code_depnum_ccdc_archive 'CCDC 825197' #TrackingRef '- kember et al_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H60 Cl2 Co2 N6 O2, 2(C4 H8 O)' _chemical_formula_sum 'C46 H76 Cl2 Co2 N6 O4' _chemical_formula_weight 965.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3806(4) _cell_length_b 13.8405(4) _cell_length_c 15.7508(6) _cell_angle_alpha 96.278(3) _cell_angle_beta 96.347(3) _cell_angle_gamma 91.870(3) _cell_volume 2448.45(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 7009 _cell_measurement_theta_min 2.8389 _cell_measurement_theta_max 72.3266 _exptl_crystal_description 'platy needles' _exptl_crystal_colour 'Pale red' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 6.675 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.357 _exptl_absorpt_correction_T_max 0.795 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17348 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 72.48 _reflns_number_total 9185 _reflns_number_gt 6422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.1054P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9185 _refine_ls_number_parameters 626 _refine_ls_number_restraints 448 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 1.012 _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 Co1 Co 0.17287(5) 0.17746(4) 0.25704(4) 0.03508(17) Uani 1 1 d . . . Co2 Co 0.34718(5) 0.22294(4) 0.14274(4) 0.03520(17) Uani 1 1 d . . . Cl1 Cl 0.38028(8) 0.26485(8) 0.31722(7) 0.0496(2) Uani 1 1 d . . . Cl2 Cl 0.30087(8) 0.18115(7) -0.00993(6) 0.0433(2) Uani 1 1 d . . . O1 O 0.2808(2) 0.09580(18) 0.18348(17) 0.0361(6) Uani 1 1 d . . . C1 C 0.3403(3) 0.0181(3) 0.2048(3) 0.0367(8) Uani 1 1 d . . . C2 C 0.2996(3) -0.0432(3) 0.2620(3) 0.0425(9) Uani 1 1 d . . . C3 C 0.1918(4) -0.0226(3) 0.3059(3) 0.0468(10) Uani 1 1 d . . . H3A H 0.1212 -0.0332 0.2626 0.056 Uiso 1 1 calc R . . H3B H 0.1847 -0.0696 0.3483 0.056 Uiso 1 1 calc R . . N4 N 0.1920(3) 0.0770(2) 0.3504(2) 0.0418(8) Uani 1 1 d D . . H4 H 0.2670(16) 0.096(3) 0.371(3) 0.056(14) Uiso 1 1 d D . . C5 C 0.1099(4) 0.0812(3) 0.4170(3) 0.0478(10) Uani 1 1 d . . . H5A H 0.1400 0.0400 0.4615 0.057 Uiso 1 1 calc R . . H5B H 0.0322 0.0521 0.3901 0.057 Uiso 1 1 calc R . . C6 C 0.0906(4) 0.1819(3) 0.4614(3) 0.0503(10) Uani 1 1 d . . . C7 C 0.0214(4) 0.2445(3) 0.4010(3) 0.0475(10) Uani 1 1 d . . . H7A H -0.0503 0.2062 0.3733 0.057 Uiso 1 1 calc R . . H7B H -0.0052 0.3015 0.4362 0.057 Uiso 1 1 calc R . . N8 N 0.0842(3) 0.2799(2) 0.3331(2) 0.0372(7) Uani 1 1 d D . . H8 H 0.139(3) 0.324(2) 0.361(2) 0.036(11) Uiso 1 1 d D . . C9 C 0.0003(3) 0.3294(3) 0.2746(3) 0.0401(9) Uani 1 1 d . . . H9A H -0.0530 0.3677 0.3095 0.048 Uiso 1 1 calc R . . H9B H -0.0491 0.2794 0.2355 0.048 Uiso 1 1 calc R . . C10 C 0.0598(3) 0.3958(3) 0.2219(3) 0.0362(8) Uani 1 1 d . . . C11 C 0.1534(3) 0.3672(3) 0.1745(2) 0.0336(8) Uani 1 1 d . . . O11 O 0.1865(2) 0.27478(17) 0.16780(17) 0.0354(5) Uani 1 1 d . . . C12 C 0.2092(3) 0.4376(3) 0.1329(2) 0.0352(8) Uani 1 1 d . . . C13 C 0.3120(3) 0.4157(3) 0.0827(3) 0.0383(8) Uani 1 1 d . . . H13A H 0.2831 0.3736 0.0291 0.046 Uiso 1 1 calc R . . H13B H 0.3445 0.4774 0.0663 0.046 Uiso 1 1 calc R . . N14 N 0.4087(3) 0.3669(2) 0.1306(2) 0.0370(7) Uani 1 1 d D . . H14 H 0.423(4) 0.394(3) 0.1856(9) 0.042(11) Uiso 1 1 d D . . C15 C 0.5181(3) 0.3765(3) 0.0887(3) 0.0421(9) Uani 1 1 d . . . H15A H 0.5423 0.4464 0.0934 0.051 Uiso 1 1 calc R . . H15B H 0.4995 0.3534 0.0267 0.051 Uiso 1 1 calc R . . C16 C 0.6232(3) 0.3215(3) 0.1248(3) 0.0442(9) Uani 1 1 d . . . C17 C 0.6033(3) 0.2108(3) 0.1012(3) 0.0445(9) Uani 1 1 d . . . H17A H 0.5782 0.1980 0.0386 0.053 Uiso 1 1 calc R . . H17B H 0.6800 0.1802 0.1127 0.053 Uiso 1 1 calc R . . N18 N 0.5154(3) 0.1626(2) 0.1467(2) 0.0401(7) Uani 1 1 d D . . H18 H 0.540(3) 0.163(3) 0.2031(6) 0.038(11) Uiso 1 1 d D . . C19 C 0.4984(3) 0.0584(3) 0.1099(3) 0.0432(9) Uani 1 1 d . . . H19A H 0.5760 0.0334 0.0975 0.052 Uiso 1 1 calc R . . H19B H 0.4464 0.0540 0.0548 0.052 Uiso 1 1 calc R . . C20 C 0.4451(3) -0.0051(3) 0.1684(3) 0.0406(9) Uani 1 1 d . . . C21 C 0.4979(4) -0.0921(3) 0.1828(3) 0.0476(10) Uani 1 1 d . . . H21A H 0.5658 -0.1085 0.1551 0.057 Uiso 1 1 calc R . . C22 C 0.4557(4) -0.1565(3) 0.2361(3) 0.0505(10) Uani 1 1 d . A . C23 C 0.3578(4) -0.1287(3) 0.2759(3) 0.0503(10) Uani 1 1 d . . . H23A H 0.3288 -0.1693 0.3145 0.060 Uiso 1 1 calc R . . C24 C 0.5146(4) -0.2536(3) 0.2466(3) 0.0623(13) Uani 1 1 d D . . C25 C 0.4946(12) -0.3186(9) 0.1618(6) 0.082(3) Uani 0.76(2) 1 d PDU A 1 H25A H 0.4102 -0.3373 0.1486 0.123 Uiso 0.76(2) 1 calc PR A 1 H25B H 0.5400 -0.3772 0.1662 0.123 Uiso 0.76(2) 1 calc PR A 1 H25C H 0.5205 -0.2835 0.1160 0.123 Uiso 0.76(2) 1 calc PR A 1 C26 C 0.6517(7) -0.2313(6) 0.2645(7) 0.082(3) Uani 0.76(2) 1 d PDU A 1 H26A H 0.6761 -0.1874 0.2243 0.123 Uiso 0.76(2) 1 calc PR A 1 H26B H 0.6929 -0.2922 0.2568 0.123 Uiso 0.76(2) 1 calc PR A 1 H26C H 0.6716 -0.2005 0.3236 0.123 Uiso 0.76(2) 1 calc PR A 1 C27 C 0.4794(12) -0.3002(8) 0.3201(8) 0.094(3) Uani 0.76(2) 1 d PDU A 1 H27A H 0.3937 -0.3142 0.3121 0.141 Uiso 0.76(2) 1 calc PR A 1 H27B H 0.5009 -0.2564 0.3732 0.141 Uiso 0.76(2) 1 calc PR A 1 H27C H 0.5203 -0.3611 0.3240 0.141 Uiso 0.76(2) 1 calc PR A 1 C25' C 0.523(3) -0.309(3) 0.1573(11) 0.047(6) Uiso 0.24(2) 1 d PDU A 2 H25D H 0.4446 -0.3346 0.1315 0.071 Uiso 0.24(2) 1 calc PR A 2 H25E H 0.5757 -0.3638 0.1635 0.071 Uiso 0.24(2) 1 calc PR A 2 H25F H 0.5558 -0.2654 0.1201 0.071 Uiso 0.24(2) 1 calc PR A 2 C26' C 0.6319(16) -0.250(3) 0.2987(18) 0.091(7) Uiso 0.24(2) 1 d PDU A 2 H26D H 0.6215 -0.2612 0.3578 0.137 Uiso 0.24(2) 1 calc PR A 2 H26E H 0.6708 -0.1853 0.2991 0.137 Uiso 0.24(2) 1 calc PR A 2 H26F H 0.6810 -0.2996 0.2737 0.137 Uiso 0.24(2) 1 calc PR A 2 C27' C 0.428(2) -0.3212(18) 0.2880(16) 0.064(6) Uiso 0.24(2) 1 d PDU A 2 H27D H 0.3465 -0.3161 0.2611 0.095 Uiso 0.24(2) 1 calc PR A 2 H27E H 0.4317 -0.3006 0.3499 0.095 Uiso 0.24(2) 1 calc PR A 2 H27F H 0.4507 -0.3888 0.2788 0.095 Uiso 0.24(2) 1 calc PR A 2 C28 C 0.2087(5) 0.2324(4) 0.5002(3) 0.0661(13) Uani 1 1 d . . . H28A H 0.2514 0.1906 0.5382 0.099 Uiso 1 1 calc R . . H28B H 0.1943 0.2943 0.5332 0.099 Uiso 1 1 calc R . . H28C H 0.2563 0.2449 0.4540 0.099 Uiso 1 1 calc R . . C29 C 0.0142(5) 0.1665(4) 0.5336(3) 0.0691(14) Uani 1 1 d . . . H29A H -0.0616 0.1341 0.5089 0.104 Uiso 1 1 calc R . . H29B H 0.0001 0.2296 0.5646 0.104 Uiso 1 1 calc R . . H29C H 0.0554 0.1258 0.5736 0.104 Uiso 1 1 calc R . . C30 C 0.0173(3) 0.4892(3) 0.2184(3) 0.0388(8) Uani 1 1 d . . . H30A H -0.0468 0.5070 0.2498 0.047 Uiso 1 1 calc R . . C31 C 0.0639(3) 0.5567(3) 0.1715(3) 0.0411(9) Uani 1 1 d . B . C32 C 0.1631(3) 0.5300(3) 0.1316(3) 0.0398(8) Uani 1 1 d . . . H32A H 0.2010 0.5764 0.1023 0.048 Uiso 1 1 calc R . . C33 C 0.0079(4) 0.6548(3) 0.1629(3) 0.0511(10) Uani 1 1 d D . . C34 C -0.1094(8) 0.6650(8) 0.1960(8) 0.081(3) Uani 0.531(7) 1 d PDU B 1 H34A H -0.1015 0.6555 0.2571 0.122 Uiso 0.531(7) 1 calc PR B 1 H34B H -0.1663 0.6160 0.1639 0.122 Uiso 0.531(7) 1 calc PR B 1 H34C H -0.1375 0.7301 0.1889 0.122 Uiso 0.531(7) 1 calc PR B 1 C35 C 0.0955(9) 0.7365(6) 0.2051(7) 0.082(3) Uani 0.531(7) 1 d PDU B 1 H35A H 0.1111 0.7311 0.2668 0.123 Uiso 0.531(7) 1 calc PR B 1 H35B H 0.0620 0.7995 0.1965 0.123 Uiso 0.531(7) 1 calc PR B 1 H35C H 0.1696 0.7314 0.1790 0.123 Uiso 0.531(7) 1 calc PR B 1 C36 C -0.0088(9) 0.6705(7) 0.0651(5) 0.068(3) Uani 0.531(7) 1 d PDU B 1 H36A H -0.0018 0.6084 0.0300 0.102 Uiso 0.531(7) 1 calc PR B 1 H36B H 0.0523 0.7175 0.0537 0.102 Uiso 0.531(7) 1 calc PR B 1 H36C H -0.0872 0.6955 0.0505 0.102 Uiso 0.531(7) 1 calc PR B 1 C34' C -0.1212(7) 0.6338(8) 0.1262(7) 0.058(3) Uiso 0.469(7) 1 d PDU B 2 H34D H -0.1668 0.6148 0.1715 0.087 Uiso 0.469(7) 1 calc PR B 2 H34E H -0.1263 0.5808 0.0792 0.087 Uiso 0.469(7) 1 calc PR B 2 H34F H -0.1534 0.6923 0.1045 0.087 Uiso 0.469(7) 1 calc PR B 2 C35' C 0.0073(9) 0.7105(8) 0.2541(6) 0.061(3) Uiso 0.469(7) 1 d PDU B 2 H35D H 0.0229 0.6655 0.2975 0.091 Uiso 0.469(7) 1 calc PR B 2 H35E H -0.0702 0.7381 0.2590 0.091 Uiso 0.469(7) 1 calc PR B 2 H35F H 0.0688 0.7631 0.2633 0.091 Uiso 0.469(7) 1 calc PR B 2 C36' C 0.0687(11) 0.7192(10) 0.1094(8) 0.082(3) Uiso 0.469(7) 1 d PDU B 2 H36D H 0.1321 0.7587 0.1458 0.122 Uiso 0.469(7) 1 calc PR B 2 H36E H 0.0114 0.7620 0.0836 0.122 Uiso 0.469(7) 1 calc PR B 2 H36F H 0.1026 0.6792 0.0638 0.122 Uiso 0.469(7) 1 calc PR B 2 C37 C 0.6524(4) 0.3484(4) 0.2212(3) 0.0585(12) Uani 1 1 d . . . H37A H 0.5854 0.3289 0.2505 0.088 Uiso 1 1 calc R . . H37B H 0.6681 0.4189 0.2335 0.088 Uiso 1 1 calc R . . H37C H 0.7227 0.3147 0.2417 0.088 Uiso 1 1 calc R . . C38 C 0.7289(4) 0.3514(4) 0.0781(3) 0.0554(11) Uani 1 1 d . . . H38A H 0.7460 0.4217 0.0909 0.083 Uiso 1 1 calc R . . H38B H 0.7091 0.3350 0.0159 0.083 Uiso 1 1 calc R . . H38C H 0.7986 0.3166 0.0977 0.083 Uiso 1 1 calc R . . N40 N 0.0149(3) 0.1131(2) 0.1825(2) 0.0413(7) Uani 1 1 d . . . C41 C -0.0039(3) 0.1248(3) 0.1002(3) 0.0409(9) Uani 1 1 d . . . H41A H 0.0440 0.1654 0.0718 0.049 Uiso 1 1 calc R . . N42 N -0.1005(3) 0.0711(3) 0.0616(2) 0.0455(8) Uani 1 1 d . . . C43 C -0.1453(4) 0.0225(3) 0.1229(3) 0.0540(11) Uani 1 1 d . . . H43A H -0.2128 -0.0211 0.1151 0.065 Uiso 1 1 calc R . . C44 C -0.0738(4) 0.0491(3) 0.1968(3) 0.0502(10) Uani 1 1 d . . . H44A H -0.0835 0.0268 0.2507 0.060 Uiso 1 1 calc R . . C45 C -0.1511(4) 0.0672(4) -0.0286(3) 0.0610(12) Uani 1 1 d . . . H45A H -0.2127 0.1148 -0.0337 0.091 Uiso 1 1 calc R . . H45B H -0.1858 0.0018 -0.0485 0.091 Uiso 1 1 calc R . . H45C H -0.0887 0.0824 -0.0639 0.091 Uiso 1 1 calc R . . O50 O 0.1555(6) 0.4785(7) 0.4407(4) 0.103(2) Uani 0.785(14) 1 d PDU C 1 C51 C 0.2402(7) 0.5319(9) 0.4018(5) 0.092(3) Uani 0.785(14) 1 d PDU C 1 H51A H 0.2163 0.5994 0.3970 0.110 Uiso 0.785(14) 1 calc PR C 1 H51B H 0.2510 0.5000 0.3439 0.110 Uiso 0.785(14) 1 calc PR C 1 C52 C 0.3491(7) 0.5301(10) 0.4619(6) 0.099(3) Uani 0.785(14) 1 d PDU C 1 H52A H 0.4002 0.4782 0.4410 0.118 Uiso 0.785(14) 1 calc PR C 1 H52B H 0.3942 0.5933 0.4679 0.118 Uiso 0.785(14) 1 calc PR C 1 C53 C 0.3102(9) 0.5109(9) 0.5448(7) 0.108(3) Uani 0.785(14) 1 d PDU C 1 H53A H 0.3389 0.5638 0.5906 0.130 Uiso 0.785(14) 1 calc PR C 1 H53B H 0.3393 0.4485 0.5619 0.130 Uiso 0.785(14) 1 calc PR C 1 C54 C 0.1755(10) 0.5067(9) 0.5281(6) 0.107(3) Uani 0.785(14) 1 d PDU C 1 H54A H 0.1401 0.4585 0.5610 0.129 Uiso 0.785(14) 1 calc PR C 1 H54B H 0.1433 0.5712 0.5432 0.129 Uiso 0.785(14) 1 calc PR C 1 O50' O 0.1502(17) 0.539(3) 0.4548(17) 0.097(5) Uiso 0.215(14) 1 d PDU C 2 C51' C 0.239(3) 0.584(3) 0.413(2) 0.101(6) Uiso 0.215(14) 1 d PDU C 2 H51C H 0.2555 0.6533 0.4372 0.121 Uiso 0.215(14) 1 calc PR C 2 H51D H 0.2158 0.5814 0.3504 0.121 Uiso 0.215(14) 1 calc PR C 2 C52' C 0.344(2) 0.526(3) 0.432(3) 0.099(6) Uiso 0.215(14) 1 d PDU C 2 H52C H 0.3532 0.4769 0.3823 0.119 Uiso 0.215(14) 1 calc PR C 2 H52D H 0.4173 0.5677 0.4448 0.119 Uiso 0.215(14) 1 calc PR C 2 C53' C 0.320(3) 0.477(3) 0.508(3) 0.103(6) Uiso 0.215(14) 1 d PDU C 2 H53C H 0.3883 0.4853 0.5532 0.124 Uiso 0.215(14) 1 calc PR C 2 H53D H 0.3008 0.4063 0.4919 0.124 Uiso 0.215(14) 1 calc PR C 2 C54' C 0.214(3) 0.528(3) 0.5377(16) 0.111(6) Uiso 0.215(14) 1 d PDU C 2 H54C H 0.1685 0.4879 0.5718 0.133 Uiso 0.215(14) 1 calc PR C 2 H54D H 0.2376 0.5918 0.5714 0.133 Uiso 0.215(14) 1 calc PR C 2 O60 O 0.7082(10) 0.0404(8) 0.3624(7) 0.132(3) Uani 0.650(10) 1 d PDU D 1 C61 C 0.5999(18) 0.0382(11) 0.4100(16) 0.105(3) Uani 0.650(10) 1 d PDU D 1 H61A H 0.5266 0.0305 0.3693 0.126 Uiso 0.650(10) 1 calc PR D 1 H61B H 0.6019 -0.0158 0.4464 0.126 Uiso 0.650(10) 1 calc PR D 1 C62 C 0.6068(15) 0.1334(10) 0.4634(11) 0.100(3) Uani 0.650(10) 1 d PDU D 1 H62A H 0.6517 0.1296 0.5203 0.121 Uiso 0.650(10) 1 calc PR D 1 H62B H 0.5268 0.1560 0.4716 0.121 Uiso 0.650(10) 1 calc PR D 1 C63 C 0.6697(9) 0.1993(7) 0.4132(7) 0.083(3) Uani 0.650(10) 1 d PDU D 1 H63A H 0.6171 0.2512 0.3962 0.100 Uiso 0.650(10) 1 calc PR D 1 H63B H 0.7406 0.2304 0.4490 0.100 Uiso 0.650(10) 1 calc PR D 1 C64 C 0.7034(9) 0.1458(6) 0.3393(6) 0.078(2) Uani 0.650(10) 1 d PDU D 1 H64A H 0.7818 0.1697 0.3267 0.094 Uiso 0.650(10) 1 calc PR D 1 H64B H 0.6447 0.1503 0.2888 0.094 Uiso 0.650(10) 1 calc PR D 1 O60' O 0.6841(19) 0.0468(16) 0.3385(13) 0.128(4) Uiso 0.350(10) 1 d PDU D 2 C61' C 0.600(3) 0.0211(19) 0.405(3) 0.107(5) Uiso 0.350(10) 1 d PDU D 2 H61C H 0.5219 -0.0051 0.3756 0.128 Uiso 0.350(10) 1 calc PR D 2 H61D H 0.6345 -0.0270 0.4412 0.128 Uiso 0.350(10) 1 calc PR D 2 C62' C 0.589(2) 0.115(2) 0.456(2) 0.096(5) Uiso 0.350(10) 1 d PDU D 2 H62C H 0.5793 0.1064 0.5158 0.115 Uiso 0.350(10) 1 calc PR D 2 H62D H 0.5206 0.1495 0.4310 0.115 Uiso 0.350(10) 1 calc PR D 2 C63' C 0.7020(18) 0.1720(14) 0.4510(15) 0.102(5) Uiso 0.350(10) 1 d PDU D 2 H63C H 0.6869 0.2290 0.4192 0.122 Uiso 0.350(10) 1 calc PR D 2 H63D H 0.7409 0.1949 0.5094 0.122 Uiso 0.350(10) 1 calc PR D 2 C64' C 0.7757(12) 0.1042(11) 0.4056(10) 0.067(4) Uiso 0.350(10) 1 d PDU D 2 H64C H 0.8159 0.0611 0.4447 0.080 Uiso 0.350(10) 1 calc PR D 2 H64D H 0.8358 0.1390 0.3779 0.080 Uiso 0.350(10) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0338(3) 0.0319(3) 0.0412(3) 0.0077(2) 0.0067(3) 0.0072(2) Co2 0.0293(3) 0.0319(3) 0.0457(4) 0.0058(3) 0.0073(2) 0.0065(2) Cl1 0.0416(5) 0.0581(6) 0.0478(5) 0.0028(5) 0.0032(4) 0.0006(4) Cl2 0.0456(5) 0.0389(5) 0.0448(5) 0.0029(4) 0.0033(4) 0.0056(4) O1 0.0345(12) 0.0322(12) 0.0437(14) 0.0076(11) 0.0076(11) 0.0101(10) C1 0.0370(19) 0.0310(18) 0.042(2) 0.0035(16) 0.0015(16) 0.0095(14) C2 0.045(2) 0.037(2) 0.045(2) 0.0071(17) 0.0013(18) 0.0112(16) C3 0.051(2) 0.0328(19) 0.061(3) 0.0156(19) 0.014(2) 0.0093(16) N4 0.0449(19) 0.0345(16) 0.049(2) 0.0109(15) 0.0084(16) 0.0092(14) C5 0.051(2) 0.046(2) 0.051(2) 0.0158(19) 0.0142(19) 0.0072(18) C6 0.062(3) 0.046(2) 0.047(2) 0.0130(19) 0.014(2) 0.011(2) C7 0.053(2) 0.043(2) 0.052(2) 0.0112(19) 0.022(2) 0.0106(18) N8 0.0376(16) 0.0346(16) 0.0423(18) 0.0084(14) 0.0120(14) 0.0056(13) C9 0.0329(18) 0.040(2) 0.049(2) 0.0083(17) 0.0077(17) 0.0139(15) C10 0.0317(17) 0.0359(19) 0.043(2) 0.0096(16) 0.0064(16) 0.0061(14) C11 0.0302(17) 0.0297(17) 0.041(2) 0.0053(15) 0.0018(15) 0.0090(14) O11 0.0318(12) 0.0288(12) 0.0475(15) 0.0070(11) 0.0088(11) 0.0064(9) C12 0.0311(17) 0.0329(18) 0.042(2) 0.0062(15) 0.0052(15) 0.0053(14) C13 0.0375(19) 0.0330(18) 0.047(2) 0.0100(16) 0.0093(17) 0.0073(15) N14 0.0323(15) 0.0353(16) 0.0443(18) 0.0049(14) 0.0075(14) 0.0025(12) C15 0.0387(19) 0.038(2) 0.051(2) 0.0053(17) 0.0150(18) 0.0010(15) C16 0.0290(18) 0.051(2) 0.054(2) 0.0065(19) 0.0093(17) 0.0000(16) C17 0.0300(18) 0.049(2) 0.058(2) 0.010(2) 0.0132(17) 0.0111(16) N18 0.0351(16) 0.0407(17) 0.0465(19) 0.0053(15) 0.0109(15) 0.0087(13) C19 0.0354(19) 0.042(2) 0.054(2) 0.0045(18) 0.0079(17) 0.0139(16) C20 0.0383(19) 0.040(2) 0.043(2) 0.0032(17) 0.0013(17) 0.0093(16) C21 0.047(2) 0.043(2) 0.053(2) 0.0044(19) 0.0049(19) 0.0206(18) C22 0.060(3) 0.045(2) 0.049(2) 0.0092(19) 0.003(2) 0.023(2) C23 0.065(3) 0.039(2) 0.049(2) 0.0135(19) 0.005(2) 0.0176(19) C24 0.086(3) 0.049(3) 0.054(3) 0.012(2) 0.006(3) 0.037(2) C25 0.103(9) 0.041(4) 0.100(7) 0.000(4) 0.003(5) 0.022(5) C26 0.088(5) 0.074(5) 0.088(6) 0.028(4) -0.007(5) 0.052(4) C27 0.122(7) 0.076(5) 0.103(6) 0.054(5) 0.040(6) 0.062(5) C28 0.090(4) 0.061(3) 0.046(3) 0.005(2) 0.001(3) 0.004(3) C29 0.099(4) 0.058(3) 0.060(3) 0.022(2) 0.035(3) 0.020(3) C30 0.0356(19) 0.0378(19) 0.045(2) 0.0058(16) 0.0070(16) 0.0132(15) C31 0.043(2) 0.0353(19) 0.047(2) 0.0054(17) 0.0075(17) 0.0111(16) C32 0.041(2) 0.0327(18) 0.048(2) 0.0092(16) 0.0101(17) 0.0084(15) C33 0.056(2) 0.038(2) 0.063(3) 0.014(2) 0.015(2) 0.0170(18) C34 0.084(6) 0.063(6) 0.110(8) 0.031(6) 0.042(6) 0.035(5) C35 0.106(7) 0.039(5) 0.094(7) -0.003(5) -0.006(6) 0.012(5) C36 0.077(6) 0.060(5) 0.070(6) 0.021(5) 0.003(5) 0.036(5) C37 0.041(2) 0.076(3) 0.056(3) 0.003(2) 0.001(2) -0.003(2) C38 0.035(2) 0.064(3) 0.071(3) 0.014(2) 0.018(2) 0.0000(19) N40 0.0360(16) 0.0379(17) 0.050(2) 0.0036(15) 0.0070(14) 0.0017(13) C41 0.0345(18) 0.0371(19) 0.050(2) 0.0013(17) 0.0047(17) 0.0032(15) N42 0.0351(16) 0.0433(18) 0.055(2) -0.0041(16) -0.0021(15) 0.0073(14) C43 0.039(2) 0.042(2) 0.081(3) 0.006(2) 0.006(2) 0.0014(17) C44 0.039(2) 0.050(2) 0.063(3) 0.013(2) 0.007(2) -0.0016(18) C45 0.055(3) 0.055(3) 0.067(3) -0.009(2) -0.003(2) 0.004(2) O50 0.110(4) 0.089(5) 0.105(4) -0.008(4) 0.028(4) -0.036(3) C51 0.096(5) 0.093(6) 0.082(5) 0.003(4) -0.005(4) -0.004(4) C52 0.091(5) 0.109(6) 0.089(6) 0.007(6) -0.014(5) 0.005(4) C53 0.134(6) 0.091(6) 0.095(6) 0.013(5) -0.006(5) -0.007(5) C54 0.133(7) 0.084(5) 0.111(6) 0.014(5) 0.035(6) 0.001(5) O60 0.118(5) 0.139(6) 0.134(6) -0.001(5) 0.013(5) 0.009(5) C61 0.099(6) 0.107(7) 0.109(7) -0.009(6) 0.037(6) -0.017(6) C62 0.103(7) 0.108(7) 0.090(6) 0.000(6) 0.019(6) 0.013(6) C63 0.078(5) 0.079(5) 0.088(6) 0.003(5) -0.003(5) 0.004(4) C64 0.082(5) 0.065(5) 0.091(6) 0.005(4) 0.034(4) -0.008(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 Co1 O1 2.061(3) . ? Co1 O11 2.065(3) . ? Co1 N8 2.110(3) . ? Co1 N4 2.131(3) . ? Co1 N40 2.145(3) . ? Co1 Cl1 2.6461(11) . ? Co1 Co2 2.9204(8) . ? Co2 O11 2.049(2) . ? Co2 O1 2.085(3) . ? Co2 N18 2.111(3) . ? Co2 N14 2.126(3) . ? Co2 Cl2 2.4064(11) . ? Co2 Cl1 2.7275(12) . ? O1 C1 1.343(4) . ? C1 C2 1.407(6) . ? C1 C20 1.410(5) . ? C2 C23 1.400(5) . ? C2 C3 1.495(6) . ? C3 N4 1.477(5) . ? N4 C5 1.477(5) . ? C5 C6 1.524(6) . ? C6 C28 1.527(7) . ? C6 C7 1.528(6) . ? C6 C29 1.535(6) . ? C7 N8 1.468(5) . ? N8 C9 1.489(5) . ? C9 C10 1.498(5) . ? C10 C30 1.400(5) . ? C10 C11 1.409(5) . ? C11 O11 1.342(4) . ? C11 C12 1.404(5) . ? C12 C32 1.400(5) . ? C12 C13 1.504(5) . ? C13 N14 1.487(5) . ? N14 C15 1.481(5) . ? C15 C16 1.529(6) . ? C16 C37 1.520(7) . ? C16 C17 1.539(6) . ? C16 C38 1.546(6) . ? C17 N18 1.477(5) . ? N18 C19 1.493(5) . ? C19 C20 1.502(6) . ? C20 C21 1.393(5) . ? C21 C22 1.398(6) . ? C22 C23 1.383(6) . ? C22 C24 1.538(6) . ? C24 C27 1.472(8) . ? C24 C26' 1.485(13) . ? C24 C25 1.516(9) . ? C24 C25' 1.544(14) . ? C24 C26 1.569(9) . ? C24 C27' 1.580(13) . ? C30 C31 1.381(6) . ? C31 C32 1.392(5) . ? C31 C33 1.531(5) . ? C33 C34 1.492(9) . ? C33 C36' 1.496(10) . ? C33 C34' 1.525(9) . ? C33 C35 1.526(9) . ? C33 C35' 1.555(9) . ? C33 C36 1.571(9) . ? N40 C41 1.319(5) . ? N40 C44 1.376(5) . ? C41 N42 1.353(5) . ? N42 C43 1.369(6) . ? N42 C45 1.467(6) . ? C43 C44 1.353(7) . ? O50 C54 1.381(10) . ? O50 C51 1.427(9) . ? C51 C52 1.476(10) . ? C52 C53 1.471(10) . ? C53 C54 1.524(11) . ? O50' C51' 1.434(17) . ? O50' C54' 1.449(17) . ? C51' C52' 1.487(15) . ? C52' C53' 1.487(15) . ? C53' C54' 1.508(16) . ? O60 C61 1.513(11) . ? O60 C64 1.543(12) . ? C61 C62 1.478(12) . ? C62 C63 1.486(12) . ? C63 C64 1.406(10) . ? O60' C64' 1.534(16) . ? O60' C61' 1.553(16) . ? C61' C62' 1.471(15) . ? C62' C63' 1.494(14) . ? C63' C64' 1.460(14) . ? 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 O11 83.86(10) . . ? O1 Co1 N8 170.42(11) . . ? O11 Co1 N8 90.38(11) . . ? O1 Co1 N4 89.58(12) . . ? O11 Co1 N4 169.88(11) . . ? N8 Co1 N4 95.04(13) . . ? O1 Co1 N40 92.59(12) . . ? O11 Co1 N40 89.58(12) . . ? N8 Co1 N40 95.02(13) . . ? N4 Co1 N40 98.43(13) . . ? O1 Co1 Cl1 80.33(8) . . ? O11 Co1 Cl1 79.99(7) . . ? N8 Co1 Cl1 91.16(9) . . ? N4 Co1 Cl1 91.34(10) . . ? N40 Co1 Cl1 167.92(10) . . ? O1 Co1 Co2 45.55(7) . . ? O11 Co1 Co2 44.56(7) . . ? N8 Co1 Co2 125.79(9) . . ? N4 Co1 Co2 126.03(9) . . ? N40 Co1 Co2 109.71(10) . . ? Cl1 Co1 Co2 58.43(3) . . ? O11 Co2 O1 83.63(9) . . ? O11 Co2 N18 166.75(12) . . ? O1 Co2 N18 88.80(11) . . ? O11 Co2 N14 89.53(11) . . ? O1 Co2 N14 166.60(12) . . ? N18 Co2 N14 95.58(12) . . ? O11 Co2 Cl2 97.83(8) . . ? O1 Co2 Cl2 98.68(8) . . ? N18 Co2 Cl2 94.05(10) . . ? N14 Co2 Cl2 93.65(10) . . ? O11 Co2 Cl1 78.27(8) . . ? O1 Co2 Cl1 77.97(8) . . ? N18 Co2 Cl1 89.54(10) . . ? N14 Co2 Cl1 89.38(10) . . ? Cl2 Co2 Cl1 175.06(4) . . ? O11 Co2 Co1 44.99(7) . . ? O1 Co2 Co1 44.88(7) . . ? N18 Co2 Co1 123.17(10) . . ? N14 Co2 Co1 123.56(9) . . ? Cl2 Co2 Co1 119.33(3) . . ? Cl1 Co2 Co1 55.75(3) . . ? Co1 Cl1 Co2 65.82(3) . . ? C1 O1 Co1 127.2(2) . . ? C1 O1 Co2 128.1(2) . . ? Co1 O1 Co2 89.56(10) . . ? O1 C1 C2 121.6(3) . . ? O1 C1 C20 120.2(3) . . ? C2 C1 C20 118.1(3) . . ? C23 C2 C1 119.8(4) . . ? C23 C2 C3 118.2(4) . . ? C1 C2 C3 121.9(3) . . ? N4 C3 C2 114.1(3) . . ? C3 N4 C5 110.5(3) . . ? C3 N4 Co1 109.0(3) . . ? C5 N4 Co1 118.3(2) . . ? N4 C5 C6 116.2(3) . . ? C5 C6 C28 110.5(4) . . ? C5 C6 C7 112.0(4) . . ? C28 C6 C7 111.2(4) . . ? C5 C6 C29 106.5(4) . . ? C28 C6 C29 109.3(4) . . ? C7 C6 C29 107.0(4) . . ? N8 C7 C6 116.7(3) . . ? C7 N8 C9 109.4(3) . . ? C7 N8 Co1 117.6(2) . . ? C9 N8 Co1 108.1(2) . . ? N8 C9 C10 113.7(3) . . ? C30 C10 C11 119.3(3) . . ? C30 C10 C9 117.7(3) . . ? C11 C10 C9 123.0(3) . . ? O11 C11 C12 120.9(3) . . ? O11 C11 C10 120.8(3) . . ? C12 C11 C10 118.2(3) . . ? C11 O11 Co2 128.4(2) . . ? C11 O11 Co1 126.5(2) . . ? Co2 O11 Co1 90.45(9) . . ? C32 C12 C11 119.7(3) . . ? C32 C12 C13 117.4(3) . . ? C11 C12 C13 122.6(3) . . ? N14 C13 C12 113.6(3) . . ? C15 N14 C13 109.1(3) . . ? C15 N14 Co2 116.5(2) . . ? C13 N14 Co2 108.3(2) . . ? N14 C15 C16 115.7(3) . . ? C37 C16 C15 111.6(4) . . ? C37 C16 C17 111.8(4) . . ? C15 C16 C17 111.6(3) . . ? C37 C16 C38 109.8(3) . . ? C15 C16 C38 106.0(3) . . ? C17 C16 C38 105.7(3) . . ? N18 C17 C16 116.0(3) . . ? C17 N18 C19 108.8(3) . . ? C17 N18 Co2 116.2(2) . . ? C19 N18 Co2 107.8(2) . . ? N18 C19 C20 113.3(3) . . ? C21 C20 C1 119.6(4) . . ? C21 C20 C19 118.3(4) . . ? C1 C20 C19 122.0(3) . . ? C20 C21 C22 123.0(4) . . ? C23 C22 C21 116.2(4) . . ? C23 C22 C24 123.0(4) . . ? C21 C22 C24 120.7(4) . . ? C22 C23 C2 123.0(4) . . ? C27 C24 C25 113.8(7) . . ? C27 C24 C22 113.2(5) . . ? C26' C24 C22 117.3(15) . . ? C25 C24 C22 109.3(6) . . ? C26' C24 C25' 109.2(12) . . ? C22 C24 C25' 109.8(16) . . ? C27 C24 C26 106.7(5) . . ? C25 C24 C26 105.9(6) . . ? C22 C24 C26 107.5(4) . . ? C26' C24 C27' 107.9(11) . . ? C22 C24 C27' 108.3(11) . . ? C25' C24 C27' 103.5(11) . . ? C31 C30 C10 123.2(3) . . ? C30 C31 C32 116.3(3) . . ? C30 C31 C33 121.5(3) . . ? C32 C31 C33 122.1(4) . . ? C31 C32 C12 122.6(4) . . ? C36' C33 C34' 110.6(6) . . ? C34 C33 C35 111.0(6) . . ? C34 C33 C31 115.3(5) . . ? C36' C33 C31 114.8(6) . . ? C34' C33 C31 107.4(5) . . ? C35 C33 C31 109.2(5) . . ? C36' C33 C35' 108.1(6) . . ? C34' C33 C35' 106.6(6) . . ? C31 C33 C35' 108.9(5) . . ? C34 C33 C36 107.7(6) . . ? C35 C33 C36 104.7(6) . . ? C31 C33 C36 108.4(5) . . ? C41 N40 C44 105.6(3) . . ? C41 N40 Co1 119.1(3) . . ? C44 N40 Co1 134.8(3) . . ? N40 C41 N42 111.0(4) . . ? C41 N42 C43 107.3(4) . . ? C41 N42 C45 126.9(4) . . ? C43 N42 C45 125.7(4) . . ? C44 C43 N42 106.1(4) . . ? C43 C44 N40 110.0(4) . . ? C54 O50 C51 106.8(7) . . ? O50 C51 C52 102.9(6) . . ? C53 C52 C51 106.1(6) . . ? C52 C53 C54 104.1(6) . . ? O50 C54 C53 102.4(7) . . ? C51' O50' C54' 101.6(16) . . ? O50' C51' C52' 103.0(13) . . ? C53' C52' C51' 105.1(9) . . ? C52' C53' C54' 103.1(10) . . ? O50' C54' C53' 99.3(13) . . ? C61 O60 C64 98.8(11) . . ? C62 C61 O60 104.2(7) . . ? C61 C62 C63 104.0(8) . . ? C64 C63 C62 109.7(7) . . ? C63 C64 O60 104.2(7) . . ? C64' O60' C61' 94.8(16) . . ? C62' C61' O60' 102.8(12) . . ? C61' C62' C63' 105.5(9) . . ? C64' C63' C62' 105.2(9) . . ? C63' C64' O60' 101.9(10) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.027 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.076 #===END data_4b _database_code_depnum_ccdc_archive 'CCDC 825198' #TrackingRef '- kember et al_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H64 Cl2 Co2 N6 O2, 4.5(C H2 Cl2)' _chemical_formula_sum 'C45.50 H73 Cl11 Co2 N6 O2' _chemical_formula_weight 1243.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 35.3728(13) _cell_length_b 20.4934(4) _cell_length_c 19.9836(6) _cell_angle_alpha 90.00 _cell_angle_beta 124.046(5) _cell_angle_gamma 90.00 _cell_volume 12003.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24056 _cell_measurement_theta_min 2.9222 _cell_measurement_theta_max 31.8205 _exptl_crystal_description needles _exptl_crystal_colour Pink _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5160 _exptl_absorpt_coefficient_mu 1.082 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.716 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57096 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 31.83 _reflns_number_total 18252 _reflns_number_gt 11576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0761P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18252 _refine_ls_number_parameters 721 _refine_ls_number_restraints 436 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1258 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.668388(10) 0.391402(15) 0.608294(17) 0.01872(7) Uani 1 1 d . . . Co2 Co 0.649241(10) 0.397706(15) 0.445129(16) 0.01859(7) Uani 1 1 d . . . Cl1 Cl 0.711642(19) 0.31836(3) 0.56016(3) 0.02495(12) Uani 1 1 d . . . Cl2 Cl 0.592426(18) 0.47625(3) 0.35538(3) 0.02426(12) Uani 1 1 d . . . O1 O 0.61467(5) 0.35993(7) 0.49502(8) 0.0184(3) Uani 1 1 d . . . C1 C 0.59520(7) 0.30102(11) 0.47893(12) 0.0178(4) Uani 1 1 d . . . C2 C 0.59289(7) 0.26469(11) 0.53656(12) 0.0201(4) Uani 1 1 d . . . C3 C 0.61221(8) 0.29034(12) 0.62027(13) 0.0228(5) Uani 1 1 d . . . H3A H 0.5946 0.3293 0.6166 0.027 Uiso 1 1 calc R . . H3B H 0.6085 0.2568 0.6518 0.027 Uiso 1 1 calc R . . N4 N 0.66133(6) 0.30816(10) 0.66392(10) 0.0209(4) Uani 1 1 d D . . H4 H 0.6753(8) 0.2770(9) 0.6536(14) 0.028(7) Uiso 1 1 d D . . C5 C 0.68213(8) 0.30508(13) 0.75255(13) 0.0265(5) Uani 1 1 d . . . H5A H 0.6800 0.2596 0.7669 0.032 Uiso 1 1 calc R . . H5B H 0.6639 0.3328 0.7650 0.032 Uiso 1 1 calc R . . C6 C 0.73158(8) 0.32661(13) 0.80554(13) 0.0275(5) Uani 1 1 d . . . C7 C 0.73633(9) 0.39956(13) 0.79511(13) 0.0280(5) Uani 1 1 d . . . H7A H 0.7136 0.4236 0.7996 0.034 Uiso 1 1 calc R . . H7B H 0.7670 0.4140 0.8401 0.034 Uiso 1 1 calc R . . N8 N 0.73022(7) 0.41784(10) 0.71773(11) 0.0223(4) Uani 1 1 d D . . H8 H 0.7530(5) 0.3964(10) 0.7197(14) 0.019(6) Uiso 1 1 d D . . C9 C 0.73598(8) 0.48937(12) 0.71486(13) 0.0257(5) Uani 1 1 d . . . H9A H 0.7593 0.5055 0.7698 0.031 Uiso 1 1 calc R . . H9B H 0.7068 0.5117 0.6962 0.031 Uiso 1 1 calc R . . C10 C 0.75039(8) 0.50544(12) 0.65872(13) 0.0232(5) Uani 1 1 d . . . C11 C 0.72153(7) 0.48989(11) 0.57598(13) 0.0202(4) Uani 1 1 d . . . O11 O 0.68116(5) 0.46068(8) 0.54536(8) 0.0200(3) Uani 1 1 d . . . C12 C 0.73695(8) 0.50831(11) 0.52692(13) 0.0228(4) Uani 1 1 d . . . C13 C 0.70798(8) 0.49669(11) 0.43710(13) 0.0228(5) Uani 1 1 d . . . H13A H 0.6796 0.5225 0.4129 0.027 Uiso 1 1 calc R . . H13B H 0.7246 0.5123 0.4136 0.027 Uiso 1 1 calc R . . N14 N 0.69596(6) 0.42680(9) 0.41574(10) 0.0192(4) Uani 1 1 d D . . H14 H 0.7213(5) 0.4023(10) 0.4451(12) 0.018(6) Uiso 1 1 d D . . C15 C 0.68139(8) 0.41818(11) 0.33083(12) 0.0220(4) Uani 1 1 d . . . H15A H 0.7072 0.4301 0.3269 0.026 Uiso 1 1 calc R . . H15B H 0.6562 0.4491 0.2966 0.026 Uiso 1 1 calc R . . C16 C 0.66537(8) 0.34925(11) 0.29629(12) 0.0213(4) Uani 1 1 d . . . C17 C 0.61935(8) 0.33326(12) 0.28222(12) 0.0222(5) Uani 1 1 d . . . H17A H 0.5980 0.3695 0.2516 0.027 Uiso 1 1 calc R . . H17B H 0.6070 0.2936 0.2483 0.027 Uiso 1 1 calc R . . N18 N 0.62082(6) 0.32232(9) 0.35722(10) 0.0193(4) Uani 1 1 d D . . H18 H 0.6390(6) 0.2881(6) 0.3848(11) 0.006(5) Uiso 1 1 d D . . C19 C 0.57389(7) 0.30832(12) 0.33523(12) 0.0217(4) Uani 1 1 d . . . H19A H 0.5576 0.2817 0.2854 0.026 Uiso 1 1 calc R . . H19B H 0.5571 0.3499 0.3237 0.026 Uiso 1 1 calc R . . C20 C 0.57391(7) 0.27278(11) 0.40090(12) 0.0205(4) Uani 1 1 d . . . C21 C 0.55262(8) 0.21272(12) 0.38460(13) 0.0243(5) Uani 1 1 d . . . H21A H 0.5388 0.1953 0.3318 0.029 Uiso 1 1 calc R . . C22 C 0.55031(8) 0.17646(12) 0.44095(14) 0.0257(5) Uani 1 1 d . A . C23 C 0.57109(7) 0.20469(12) 0.51695(13) 0.0235(5) Uani 1 1 d . . . H23A H 0.5703 0.1817 0.5575 0.028 Uiso 1 1 calc R . . C24 C 0.52608(10) 0.10985(14) 0.41953(16) 0.0381(6) Uani 1 1 d D . . C25 C 0.47550(15) 0.1205(3) 0.3530(3) 0.0652(16) Uani 0.719(5) 1 d PDU A 1 H25A H 0.4716 0.1630 0.3275 0.098 Uiso 0.719(5) 1 calc PR A 1 H25B H 0.4576 0.1192 0.3767 0.098 Uiso 0.719(5) 1 calc PR A 1 H25C H 0.4650 0.0859 0.3123 0.098 Uiso 0.719(5) 1 calc PR A 1 C26 C 0.54590(18) 0.0655(2) 0.3846(3) 0.0567(13) Uani 0.719(5) 1 d PDU A 1 H26A H 0.5330 0.0777 0.3284 0.085 Uiso 0.719(5) 1 calc PR A 1 H26B H 0.5382 0.0200 0.3869 0.085 Uiso 0.719(5) 1 calc PR A 1 H26C H 0.5791 0.0705 0.4163 0.085 Uiso 0.719(5) 1 calc PR A 1 C27 C 0.5312(2) 0.0773(3) 0.4910(3) 0.0717(18) Uani 0.719(5) 1 d PDU A 1 H27A H 0.5068 0.0920 0.4968 0.108 Uiso 0.719(5) 1 calc PR A 1 H27B H 0.5609 0.0886 0.5397 0.108 Uiso 0.719(5) 1 calc PR A 1 H27C H 0.5292 0.0299 0.4833 0.108 Uiso 0.719(5) 1 calc PR A 1 C25' C 0.5071(4) 0.0853(7) 0.3377(5) 0.056(3) Uiso 0.281(5) 1 d PDU A 2 H25D H 0.4858 0.1174 0.2982 0.084 Uiso 0.281(5) 1 calc PR A 2 H25E H 0.4911 0.0442 0.3300 0.084 Uiso 0.281(5) 1 calc PR A 2 H25F H 0.5319 0.0780 0.3302 0.084 Uiso 0.281(5) 1 calc PR A 2 C26' C 0.5610(4) 0.0592(7) 0.4812(7) 0.064(3) Uiso 0.281(5) 1 d PDU A 2 H26D H 0.5638 0.0640 0.5326 0.096 Uiso 0.281(5) 1 calc PR A 2 H26E H 0.5908 0.0667 0.4897 0.096 Uiso 0.281(5) 1 calc PR A 2 H26F H 0.5504 0.0150 0.4601 0.096 Uiso 0.281(5) 1 calc PR A 2 C27' C 0.4875(4) 0.1138(7) 0.4327(8) 0.064(3) Uiso 0.281(5) 1 d PDU A 2 H27D H 0.4640 0.1439 0.3932 0.096 Uiso 0.281(5) 1 calc PR A 2 H27E H 0.4997 0.1297 0.4874 0.096 Uiso 0.281(5) 1 calc PR A 2 H27F H 0.4742 0.0704 0.4258 0.096 Uiso 0.281(5) 1 calc PR A 2 C28 C 0.76212(9) 0.28506(14) 0.79055(15) 0.0351(6) Uani 1 1 d . . . H28A H 0.7527 0.2907 0.7345 0.053 Uiso 1 1 calc R . . H28B H 0.7592 0.2390 0.8003 0.053 Uiso 1 1 calc R . . H28C H 0.7939 0.2989 0.8272 0.053 Uiso 1 1 calc R . . C29 C 0.74633(10) 0.31756(16) 0.89393(14) 0.0414(7) Uani 1 1 d . . . H29A H 0.7444 0.2713 0.9040 0.062 Uiso 1 1 calc R . . H29B H 0.7262 0.3430 0.9031 0.062 Uiso 1 1 calc R . . H29C H 0.7778 0.3327 0.9307 0.062 Uiso 1 1 calc R . . C30 C 0.79226(8) 0.53546(12) 0.68993(14) 0.0270(5) Uani 1 1 d . . . H30A H 0.8108 0.5447 0.7461 0.032 Uiso 1 1 calc R . . C31 C 0.80825(8) 0.55260(12) 0.64252(15) 0.0277(5) Uani 1 1 d . B . C32 C 0.77872(8) 0.53855(12) 0.56042(14) 0.0251(5) Uani 1 1 d . . . H32A H 0.7879 0.5505 0.5255 0.030 Uiso 1 1 calc R . . C33 C 0.85511(9) 0.58386(14) 0.67683(15) 0.0342(6) Uani 1 1 d D . . C34 C 0.88336(12) 0.5407(2) 0.6602(3) 0.0611(12) Uani 0.861(4) 1 d PDU B 1 H34A H 0.8698 0.5394 0.6019 0.092 Uiso 0.861(4) 1 calc PR B 1 H34B H 0.8843 0.4965 0.6797 0.092 Uiso 0.861(4) 1 calc PR B 1 H34C H 0.9144 0.5581 0.6880 0.092 Uiso 0.861(4) 1 calc PR B 1 C35 C 0.88135(14) 0.5949(3) 0.7682(2) 0.0687(14) Uani 0.861(4) 1 d PDU B 1 H35A H 0.8746 0.6386 0.7788 0.103 Uiso 0.861(4) 1 calc PR B 1 H35B H 0.9142 0.5910 0.7922 0.103 Uiso 0.861(4) 1 calc PR B 1 H35C H 0.8721 0.5621 0.7920 0.103 Uiso 0.861(4) 1 calc PR B 1 C36 C 0.84874(14) 0.65052(19) 0.6372(3) 0.0623(12) Uani 0.861(4) 1 d PDU B 1 H36A H 0.8265 0.6467 0.5787 0.093 Uiso 0.861(4) 1 calc PR B 1 H36B H 0.8780 0.6655 0.6482 0.093 Uiso 0.861(4) 1 calc PR B 1 H36C H 0.8376 0.6820 0.6593 0.093 Uiso 0.861(4) 1 calc PR B 1 C34' C 0.8629(9) 0.5891(12) 0.6093(11) 0.062(5) Uiso 0.139(4) 1 d PDU B 2 H34D H 0.8340 0.5996 0.5584 0.092 Uiso 0.139(4) 1 calc PR B 2 H34E H 0.8745 0.5475 0.6038 0.092 Uiso 0.139(4) 1 calc PR B 2 H34F H 0.8851 0.6237 0.6223 0.092 Uiso 0.139(4) 1 calc PR B 2 C35' C 0.8902(8) 0.5410(10) 0.7446(11) 0.061(5) Uiso 0.139(4) 1 d PDU B 2 H35D H 0.8782 0.4966 0.7368 0.092 Uiso 0.139(4) 1 calc PR B 2 H35E H 0.8972 0.5582 0.7962 0.092 Uiso 0.139(4) 1 calc PR B 2 H35F H 0.9181 0.5404 0.7451 0.092 Uiso 0.139(4) 1 calc PR B 2 C36' C 0.8558(10) 0.6513(8) 0.7073(14) 0.067(5) Uiso 0.139(4) 1 d PDU B 2 H36D H 0.8367 0.6804 0.6614 0.100 Uiso 0.139(4) 1 calc PR B 2 H36E H 0.8872 0.6677 0.7390 0.100 Uiso 0.139(4) 1 calc PR B 2 H36F H 0.8440 0.6496 0.7415 0.100 Uiso 0.139(4) 1 calc PR B 2 C37 C 0.70142(8) 0.29822(12) 0.34984(14) 0.0267(5) Uani 1 1 d . . . H37A H 0.7060 0.2977 0.4030 0.040 Uiso 1 1 calc R . . H37B H 0.7302 0.3091 0.3561 0.040 Uiso 1 1 calc R . . H37C H 0.6911 0.2551 0.3248 0.040 Uiso 1 1 calc R . . C38 C 0.65850(9) 0.34925(13) 0.21319(14) 0.0299(5) Uani 1 1 d . . . H38A H 0.6483 0.3060 0.1885 0.045 Uiso 1 1 calc R . . H38B H 0.6874 0.3599 0.2197 0.045 Uiso 1 1 calc R . . H38C H 0.6354 0.3818 0.1783 0.045 Uiso 1 1 calc R . . N40 N 0.62293(6) 0.45578(9) 0.61341(10) 0.0207(4) Uani 1 1 d . . . C41 C 0.61064(7) 0.45821(11) 0.66651(12) 0.0212(4) Uani 1 1 d . . . H41A H 0.6268 0.4309 0.7127 0.025 Uiso 1 1 calc R . . C42 C 0.57700(7) 0.49668(12) 0.65917(13) 0.0217(4) Uani 1 1 d . . . H42A H 0.5698 0.4944 0.6984 0.026 Uiso 1 1 calc R . . C43 C 0.55291(7) 0.53989(11) 0.59329(13) 0.0209(4) Uani 1 1 d . . . C44 C 0.56519(7) 0.53741(12) 0.53703(13) 0.0231(5) Uani 1 1 d . . . H44A H 0.5501 0.5647 0.4907 0.028 Uiso 1 1 calc R . . C45 C 0.59867(8) 0.49596(12) 0.54892(13) 0.0229(5) Uani 1 1 d . . . H45A H 0.6054 0.4953 0.5091 0.028 Uiso 1 1 calc R . . N46 N 0.52102(7) 0.58168(11) 0.58482(12) 0.0299(5) Uani 1 1 d . . . C47 C 0.50263(9) 0.57713(16) 0.63378(16) 0.0390(7) Uani 1 1 d . . . H47A H 0.5012 0.5312 0.6459 0.058 Uiso 1 1 calc R . . H47B H 0.4719 0.5960 0.6042 0.058 Uiso 1 1 calc R . . H47C H 0.5224 0.6011 0.6843 0.058 Uiso 1 1 calc R . . C48 C 0.49950(10) 0.62780(16) 0.51859(18) 0.0438(7) Uani 1 1 d . . . H48A H 0.5230 0.6520 0.5175 0.066 Uiso 1 1 calc R . . H48B H 0.4808 0.6583 0.5259 0.066 Uiso 1 1 calc R . . H48C H 0.4801 0.6042 0.4675 0.066 Uiso 1 1 calc R . . C50 C 0.6314(2) 0.6279(3) 0.4550(3) 0.0504(15) Uani 0.638(3) 1 d PDU C 1 H50A H 0.6026 0.6342 0.4515 0.060 Uiso 0.638(3) 1 calc PR C 1 H50B H 0.6361 0.5805 0.4529 0.060 Uiso 0.638(3) 1 calc PR C 1 Cl3 Cl 0.62790(18) 0.6673(3) 0.3735(3) 0.1076(15) Uani 0.638(3) 1 d PDU C 1 Cl4 Cl 0.67620(12) 0.65980(13) 0.54401(12) 0.1218(12) Uani 0.638(3) 1 d PDU C 1 C50' C 0.6452(8) 0.6265(10) 0.4611(9) 0.074(5) Uiso 0.276(3) 1 d PDU D 2 H50C H 0.6311 0.5836 0.4566 0.088 Uiso 0.276(3) 1 calc PR D 2 H50D H 0.6782 0.6193 0.4863 0.088 Uiso 0.276(3) 1 calc PR D 2 Cl3' Cl 0.6212(3) 0.6585(5) 0.3650(5) 0.0607(15) Uiso 0.276(3) 1 d PDU D 2 Cl4' Cl 0.6382(2) 0.6765(2) 0.5232(3) 0.0826(15) Uiso 0.276(3) 1 d PDU D 2 C50" C 0.6557(15) 0.631(2) 0.536(4) 0.088(5) Uiso 0.086(2) 1 d PDU E 3 H50E H 0.6435 0.5872 0.5144 0.106 Uiso 0.086(2) 1 calc PR E 3 H50F H 0.6740 0.6293 0.5959 0.106 Uiso 0.086(2) 1 calc PR E 3 Cl3" Cl 0.6887(6) 0.6593(11) 0.5024(14) 0.121(4) Uiso 0.086(2) 1 d PDU E 3 Cl4" Cl 0.6120(5) 0.6872(6) 0.5005(8) 0.068(3) Uiso 0.086(2) 1 d PDU E 3 C55 C 0.82599(9) 0.35190(14) 0.45008(16) 0.0355(6) Uani 1 1 d . . . H55A H 0.8121 0.3138 0.4590 0.043 Uiso 1 1 calc R . . H55B H 0.8596 0.3478 0.4866 0.043 Uiso 1 1 calc R . . Cl5 Cl 0.80949(3) 0.35286(4) 0.34890(4) 0.04566(18) Uani 1 1 d . . . Cl6 Cl 0.80821(3) 0.42425(5) 0.47240(5) 0.0589(2) Uani 1 1 d . . . C60 C 0.82875(10) 0.38004(15) 0.66683(19) 0.0407(7) Uani 1 1 d . . . H60A H 0.8235 0.4257 0.6476 0.049 Uiso 1 1 calc R . . H60B H 0.7998 0.3557 0.6325 0.049 Uiso 1 1 calc R . . Cl7 Cl 0.87113(3) 0.34489(4) 0.65787(5) 0.04972(19) Uani 1 1 d . . . Cl8 Cl 0.84509(3) 0.37841(5) 0.76760(5) 0.0626(2) Uani 1 1 d . . . C65 C 0.5029(14) 0.5872(3) 0.2437(17) 0.050(4) Uani 0.50 1 d PD F -1 H65A H 0.4772 0.5561 0.2135 0.059 Uiso 0.50 1 calc PR F -1 H65B H 0.5316 0.5620 0.2697 0.059 Uiso 0.50 1 calc PR F -1 Cl9 Cl 0.5012(4) 0.6435(4) 0.1760(6) 0.0792(18) Uani 0.50 1 d PD F -1 Cl10 Cl 0.4994(4) 0.6250(4) 0.3188(5) 0.0705(15) Uani 0.50 1 d PD F -1 C70 C 0.5366(7) 0.8275(15) 0.3948(16) 0.181(8) Uiso 0.269(5) 1 d PDU G -1 H70A H 0.5512 0.8545 0.4443 0.218 Uiso 0.269(5) 1 calc PR G -1 H70B H 0.5596 0.7993 0.3957 0.218 Uiso 0.269(5) 1 calc PR G -1 Cl11 Cl 0.5058(5) 0.8734(7) 0.3077(10) 0.223(5) Uiso 0.269(5) 1 d PDU G -1 Cl12 Cl 0.4880(2) 0.7820(3) 0.3777(4) 0.104(2) Uiso 0.269(5) 1 d PDU G -1 C70' C 0.5038(12) 0.7924(12) 0.3232(13) 0.149(8) Uiso 0.231(5) 1 d PDU G -2 H70C H 0.5240 0.7605 0.3210 0.179 Uiso 0.231(5) 1 calc PR G -2 H70D H 0.4727 0.7732 0.2917 0.179 Uiso 0.231(5) 1 calc PR G -2 Cl13 Cl 0.5019(3) 0.8568(3) 0.2717(4) 0.095(2) Uiso 0.231(5) 1 d PDU G -2 Cl14 Cl 0.5205(7) 0.7938(8) 0.4248(9) 0.242(6) Uiso 0.231(5) 1 d PDU G -2 C75 C 0.6056(6) 0.8175(7) 0.5460(11) 0.079(5) Uiso 0.238(2) 1 d PDU H 4 H75A H 0.6333 0.7921 0.5620 0.094 Uiso 0.238(2) 1 calc PR H 4 H75B H 0.6078 0.8255 0.5968 0.094 Uiso 0.238(2) 1 calc PR H 4 Cl15 Cl 0.6162(2) 0.8886(3) 0.5245(3) 0.0879(17) Uiso 0.238(2) 1 d PDU H 4 Cl16 Cl 0.5661(3) 0.7647(5) 0.5014(6) 0.170(4) Uiso 0.238(2) 1 d PDU H 4 C75' C 0.5938(6) 0.9115(8) 0.5245(14) 0.048(5) Uiso 0.146(4) 1 d PDU I 5 H75C H 0.5781 0.9094 0.5529 0.058 Uiso 0.146(4) 1 calc PR I 5 H75D H 0.5709 0.9253 0.4682 0.058 Uiso 0.146(4) 1 calc PR I 5 Cl17 Cl 0.6370(2) 0.9716(4) 0.5716(4) 0.064(2) Uiso 0.146(4) 1 d PDU I 5 Cl18 Cl 0.6112(3) 0.8403(6) 0.5228(5) 0.081(3) Uiso 0.146(4) 1 d PDU I 5 C75" C 0.5922(7) 0.8828(9) 0.5055(14) 0.034(4) Uiso 0.116(4) 1 d PDU J 6 H75E H 0.5750 0.8840 0.5312 0.041 Uiso 0.116(4) 1 calc PR J 6 H75F H 0.5709 0.8961 0.4484 0.041 Uiso 0.116(4) 1 calc PR J 6 Cl19 Cl 0.6353(4) 0.9386(7) 0.5524(7) 0.079(3) Uiso 0.116(4) 1 d PDU J 6 Cl20 Cl 0.6090(5) 0.8052(8) 0.5078(9) 0.106(4) Uiso 0.116(4) 1 d PDU J 6 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02032(15) 0.02130(16) 0.01666(13) 0.00144(11) 0.01166(12) 0.00390(12) Co2 0.02008(15) 0.02156(16) 0.01743(14) 0.00069(11) 0.01252(12) 0.00218(11) Cl1 0.0232(3) 0.0265(3) 0.0254(3) 0.0048(2) 0.0138(2) 0.0087(2) Cl2 0.0252(3) 0.0260(3) 0.0222(2) 0.0048(2) 0.0137(2) 0.0073(2) O1 0.0201(8) 0.0181(8) 0.0185(7) 0.0013(6) 0.0117(6) 0.0028(6) C1 0.0131(9) 0.0216(11) 0.0198(10) 0.0027(8) 0.0099(8) 0.0054(8) C2 0.0170(10) 0.0242(11) 0.0199(10) 0.0031(8) 0.0107(9) 0.0037(8) C3 0.0240(11) 0.0270(12) 0.0210(10) 0.0027(9) 0.0148(9) 0.0020(9) N4 0.0226(10) 0.0249(10) 0.0156(8) 0.0027(7) 0.0110(8) 0.0058(8) C5 0.0332(13) 0.0297(13) 0.0172(10) 0.0039(9) 0.0145(10) 0.0039(10) C6 0.0282(12) 0.0335(14) 0.0167(10) 0.0030(9) 0.0101(10) 0.0043(10) C7 0.0315(13) 0.0354(14) 0.0162(10) -0.0017(9) 0.0128(10) -0.0007(10) N8 0.0254(10) 0.0270(10) 0.0182(8) -0.0011(7) 0.0144(8) 0.0020(8) C9 0.0296(12) 0.0278(13) 0.0232(11) -0.0061(9) 0.0170(10) -0.0014(10) C10 0.0264(12) 0.0236(12) 0.0229(10) -0.0009(9) 0.0158(10) 0.0017(9) C11 0.0219(11) 0.0166(10) 0.0267(11) 0.0008(8) 0.0165(9) 0.0038(8) O11 0.0190(7) 0.0234(8) 0.0198(7) 0.0002(6) 0.0123(6) 0.0019(6) C12 0.0261(11) 0.0213(11) 0.0249(11) 0.0004(9) 0.0167(10) 0.0020(9) C13 0.0259(12) 0.0214(11) 0.0243(10) 0.0026(9) 0.0160(10) 0.0018(9) N14 0.0210(9) 0.0211(10) 0.0177(8) 0.0040(7) 0.0123(8) 0.0058(7) C15 0.0262(12) 0.0251(12) 0.0190(10) 0.0040(9) 0.0153(9) 0.0030(9) C16 0.0240(11) 0.0241(12) 0.0189(10) 0.0030(8) 0.0138(9) 0.0061(9) C17 0.0242(11) 0.0291(12) 0.0150(9) 0.0000(8) 0.0122(9) 0.0039(9) N18 0.0191(9) 0.0239(10) 0.0175(8) 0.0028(7) 0.0120(8) 0.0045(7) C19 0.0200(11) 0.0269(12) 0.0183(10) 0.0004(8) 0.0107(9) 0.0007(9) C20 0.0178(10) 0.0250(12) 0.0207(10) 0.0010(8) 0.0120(9) 0.0033(8) C21 0.0210(11) 0.0280(12) 0.0230(11) -0.0024(9) 0.0118(9) -0.0005(9) C22 0.0198(11) 0.0290(13) 0.0279(11) -0.0014(9) 0.0130(10) -0.0035(9) C23 0.0206(11) 0.0281(12) 0.0253(11) 0.0042(9) 0.0150(9) 0.0019(9) C24 0.0395(15) 0.0370(16) 0.0378(14) -0.0047(12) 0.0217(13) -0.0159(12) C25 0.039(3) 0.067(3) 0.072(3) -0.010(3) 0.020(2) -0.026(2) C26 0.078(3) 0.031(2) 0.077(3) -0.013(2) 0.053(3) -0.015(2) C27 0.108(4) 0.057(3) 0.056(3) -0.008(2) 0.049(3) -0.050(3) C28 0.0311(14) 0.0384(15) 0.0295(12) 0.0057(11) 0.0131(11) 0.0102(11) C29 0.0450(17) 0.0501(18) 0.0195(12) 0.0058(11) 0.0123(12) -0.0008(14) C30 0.0297(12) 0.0272(13) 0.0252(11) -0.0063(9) 0.0160(10) -0.0019(10) C31 0.0277(12) 0.0243(12) 0.0355(12) -0.0057(10) 0.0204(11) -0.0030(10) C32 0.0294(12) 0.0219(12) 0.0318(12) 0.0000(9) 0.0218(11) 0.0003(9) C33 0.0309(14) 0.0374(15) 0.0379(14) -0.0097(11) 0.0215(12) -0.0100(11) C34 0.0325(19) 0.065(3) 0.091(3) -0.027(2) 0.038(2) -0.0131(18) C35 0.044(2) 0.115(4) 0.046(2) -0.031(2) 0.0241(18) -0.044(2) C36 0.051(2) 0.042(2) 0.084(3) -0.001(2) 0.032(2) -0.0192(18) C37 0.0260(12) 0.0254(12) 0.0321(12) 0.0031(10) 0.0184(10) 0.0072(9) C38 0.0388(14) 0.0346(14) 0.0254(11) -0.0002(10) 0.0235(11) 0.0032(11) N40 0.0221(9) 0.0234(10) 0.0189(8) 0.0011(7) 0.0129(8) 0.0042(7) C41 0.0232(11) 0.0234(11) 0.0181(10) 0.0007(8) 0.0122(9) 0.0034(9) C42 0.0215(11) 0.0285(12) 0.0189(10) -0.0028(9) 0.0136(9) 0.0007(9) C43 0.0158(10) 0.0253(12) 0.0211(10) -0.0048(8) 0.0100(9) -0.0002(8) C44 0.0221(11) 0.0276(12) 0.0203(10) 0.0027(9) 0.0124(9) 0.0046(9) C45 0.0251(11) 0.0270(12) 0.0210(10) 0.0003(9) 0.0155(10) 0.0034(9) N46 0.0210(10) 0.0421(13) 0.0296(10) 0.0024(9) 0.0160(9) 0.0116(9) C47 0.0291(14) 0.061(2) 0.0359(14) -0.0018(13) 0.0235(12) 0.0120(13) C48 0.0399(16) 0.0474(18) 0.0470(16) 0.0091(14) 0.0262(14) 0.0241(14) C50 0.071(4) 0.043(3) 0.054(3) -0.017(2) 0.045(3) -0.015(3) Cl3 0.150(3) 0.113(3) 0.0899(19) 0.0169(17) 0.086(2) -0.019(2) Cl4 0.140(2) 0.0987(17) 0.0668(12) -0.0271(11) 0.0211(14) -0.0287(16) C55 0.0324(14) 0.0346(15) 0.0404(14) -0.0022(12) 0.0209(12) 0.0064(11) Cl5 0.0606(5) 0.0392(4) 0.0477(4) 0.0097(3) 0.0368(4) 0.0130(3) Cl6 0.0425(4) 0.0588(5) 0.0629(5) -0.0201(4) 0.0218(4) 0.0150(4) C60 0.0386(16) 0.0348(16) 0.0562(18) 0.0049(13) 0.0312(15) 0.0064(12) Cl7 0.0484(4) 0.0384(4) 0.0762(5) 0.0001(4) 0.0434(4) 0.0062(3) Cl8 0.0540(5) 0.0840(7) 0.0596(5) 0.0129(5) 0.0379(4) 0.0172(5) C65 0.041(8) 0.040(3) 0.051(7) -0.002(5) 0.016(4) 0.005(5) Cl9 0.096(3) 0.080(4) 0.0603(18) 0.010(2) 0.0425(17) -0.010(3) Cl10 0.086(2) 0.080(4) 0.062(3) 0.014(3) 0.051(2) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.0819(14) . ? Co1 O11 2.1066(15) . ? Co1 N8 2.1224(19) . ? Co1 N4 2.1259(19) . ? Co1 N40 2.1261(18) . ? Co1 Cl1 2.6748(6) . ? Co1 Co2 2.9384(4) . ? Co2 O11 2.1024(15) . ? Co2 O1 2.1105(15) . ? Co2 N18 2.1228(19) . ? Co2 N14 2.1254(18) . ? Co2 Cl2 2.4105(6) . ? Co2 Cl1 2.6681(6) . ? O1 C1 1.337(3) . ? C1 C2 1.412(3) . ? C1 C20 1.421(3) . ? C2 C23 1.386(3) . ? C2 C3 1.504(3) . ? C3 N4 1.489(3) . ? N4 C5 1.491(3) . ? C5 C6 1.517(3) . ? C6 C28 1.531(4) . ? C6 C7 1.532(4) . ? C6 C29 1.547(3) . ? C7 N8 1.484(3) . ? N8 C9 1.485(3) . ? C9 C10 1.506(3) . ? C10 C30 1.388(3) . ? C10 C11 1.410(3) . ? C11 O11 1.339(3) . ? C11 C12 1.414(3) . ? C12 C32 1.381(3) . ? C12 C13 1.506(3) . ? C13 N14 1.487(3) . ? N14 C15 1.482(3) . ? C15 C16 1.534(3) . ? C16 C17 1.524(3) . ? C16 C37 1.529(3) . ? C16 C38 1.538(3) . ? C17 N18 1.487(3) . ? N18 C19 1.488(3) . ? C19 C20 1.501(3) . ? C20 C21 1.383(3) . ? C21 C22 1.389(3) . ? C22 C23 1.390(3) . ? C22 C24 1.539(4) . ? C24 C25' 1.466(9) . ? C24 C27 1.492(5) . ? C24 C27' 1.528(10) . ? C24 C26 1.533(5) . ? C24 C25 1.534(5) . ? C24 C26' 1.555(10) . ? C30 C31 1.393(3) . ? C31 C32 1.395(3) . ? C31 C33 1.535(3) . ? C33 C36' 1.504(13) . ? C33 C34 1.505(4) . ? C33 C35' 1.505(12) . ? C33 C34' 1.524(12) . ? C33 C36 1.531(5) . ? C33 C35 1.532(4) . ? N40 C41 1.354(3) . ? N40 C45 1.355(3) . ? C41 C42 1.365(3) . ? C42 C43 1.410(3) . ? C43 N46 1.349(3) . ? C43 C44 1.415(3) . ? C44 C45 1.366(3) . ? N46 C48 1.448(3) . ? N46 C47 1.450(3) . ? C50 Cl4 1.717(6) . ? C50 Cl3 1.757(6) . ? C50' Cl4' 1.731(14) . ? C50' Cl3' 1.737(14) . ? C50" Cl4" 1.727(17) . ? C50" Cl3" 1.739(17) . ? C55 Cl6 1.763(3) . ? C55 Cl5 1.763(3) . ? C60 Cl8 1.757(3) . ? C60 Cl7 1.761(3) . ? C65 Cl10 1.753(11) . ? C65 Cl9 1.753(10) . ? C70 Cl11 1.725(18) . ? C70 Cl12 1.811(19) . ? C70' Cl13 1.652(18) . ? C70' Cl14 1.767(18) . ? C75 Cl16 1.589(9) . ? C75 Cl15 1.620(9) . ? C75' Cl18 1.591(16) . ? C75' Cl17 1.769(16) . ? C75" Cl20 1.690(17) . ? C75" Cl19 1.707(17) . ? 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 O11 85.98(6) . . ? O1 Co1 N8 170.47(7) . . ? O11 Co1 N8 90.08(7) . . ? O1 Co1 N4 90.98(7) . . ? O11 Co1 N4 168.60(7) . . ? N8 Co1 N4 91.21(7) . . ? O1 Co1 N40 89.43(6) . . ? O11 Co1 N40 91.79(7) . . ? N8 Co1 N40 99.38(7) . . ? N4 Co1 N40 99.17(7) . . ? O1 Co1 Cl1 78.07(4) . . ? O11 Co1 Cl1 78.78(4) . . ? N8 Co1 Cl1 92.66(5) . . ? N4 Co1 Cl1 89.84(5) . . ? N40 Co1 Cl1 164.75(5) . . ? O1 Co1 Co2 45.90(4) . . ? O11 Co1 Co2 45.67(4) . . ? N8 Co1 Co2 126.62(5) . . ? N4 Co1 Co2 126.44(5) . . ? N40 Co1 Co2 108.38(5) . . ? Cl1 Co1 Co2 56.526(14) . . ? O11 Co2 O1 85.37(6) . . ? O11 Co2 N18 171.16(6) . . ? O1 Co2 N18 89.59(6) . . ? O11 Co2 N14 90.29(6) . . ? O1 Co2 N14 168.29(6) . . ? N18 Co2 N14 93.25(7) . . ? O11 Co2 Cl2 94.49(4) . . ? O1 Co2 Cl2 97.71(4) . . ? N18 Co2 Cl2 93.38(5) . . ? N14 Co2 Cl2 93.47(5) . . ? O11 Co2 Cl1 79.01(4) . . ? O1 Co2 Cl1 77.77(4) . . ? N18 Co2 Cl1 92.84(5) . . ? N14 Co2 Cl1 90.74(5) . . ? Cl2 Co2 Cl1 172.28(2) . . ? O11 Co2 Co1 45.78(4) . . ? O1 Co2 Co1 45.10(4) . . ? N18 Co2 Co1 126.48(5) . . ? N14 Co2 Co1 125.95(5) . . ? Cl2 Co2 Co1 115.667(18) . . ? Cl1 Co2 Co1 56.744(14) . . ? Co2 Cl1 Co1 66.730(15) . . ? C1 O1 Co1 125.09(12) . . ? C1 O1 Co2 125.05(12) . . ? Co1 O1 Co2 89.00(6) . . ? O1 C1 C2 122.51(19) . . ? O1 C1 C20 121.13(19) . . ? C2 C1 C20 116.3(2) . . ? C23 C2 C1 121.0(2) . . ? C23 C2 C3 117.32(19) . . ? C1 C2 C3 121.7(2) . . ? N4 C3 C2 113.09(17) . . ? C3 N4 C5 108.89(17) . . ? C3 N4 Co1 109.31(13) . . ? C5 N4 Co1 122.06(15) . . ? N4 C5 C6 115.23(19) . . ? C5 C6 C28 111.5(2) . . ? C5 C6 C7 111.1(2) . . ? C28 C6 C7 111.9(2) . . ? C5 C6 C29 106.4(2) . . ? C28 C6 C29 109.4(2) . . ? C7 C6 C29 106.2(2) . . ? N8 C7 C6 115.16(19) . . ? C7 N8 C9 110.26(17) . . ? C7 N8 Co1 118.29(15) . . ? C9 N8 Co1 107.25(14) . . ? N8 C9 C10 110.84(18) . . ? C30 C10 C11 121.1(2) . . ? C30 C10 C9 118.9(2) . . ? C11 C10 C9 120.0(2) . . ? O11 C11 C10 121.58(19) . . ? O11 C11 C12 121.95(19) . . ? C10 C11 C12 116.4(2) . . ? C11 O11 Co2 125.18(13) . . ? C11 O11 Co1 123.97(13) . . ? Co2 O11 Co1 88.55(6) . . ? C32 C12 C11 120.5(2) . . ? C32 C12 C13 118.6(2) . . ? C11 C12 C13 121.0(2) . . ? N14 C13 C12 112.88(18) . . ? C15 N14 C13 107.68(17) . . ? C15 N14 Co2 117.20(14) . . ? C13 N14 Co2 109.42(13) . . ? N14 C15 C16 115.39(18) . . ? C17 C16 C37 111.60(19) . . ? C17 C16 C15 111.60(18) . . ? C37 C16 C15 111.20(19) . . ? C17 C16 C38 107.10(18) . . ? C37 C16 C38 108.76(19) . . ? C15 C16 C38 106.32(18) . . ? N18 C17 C16 114.54(17) . . ? C17 N18 C19 109.13(16) . . ? C17 N18 Co2 117.22(14) . . ? C19 N18 Co2 108.53(13) . . ? N18 C19 C20 112.41(17) . . ? C21 C20 C1 120.3(2) . . ? C21 C20 C19 119.49(19) . . ? C1 C20 C19 120.2(2) . . ? C20 C21 C22 123.8(2) . . ? C21 C22 C23 115.3(2) . . ? C21 C22 C24 121.7(2) . . ? C23 C22 C24 123.0(2) . . ? C2 C23 C22 123.3(2) . . ? C25' C24 C27 130.5(6) . . ? C25' C24 C27' 108.4(7) . . ? C27 C24 C27' 60.1(5) . . ? C25' C24 C26 47.9(5) . . ? C27 C24 C26 109.2(4) . . ? C27' C24 C26 142.0(6) . . ? C25' C24 C25 59.9(5) . . ? C27 C24 C25 110.5(4) . . ? C27' C24 C25 54.6(5) . . ? C26 C24 C25 107.4(3) . . ? C25' C24 C22 116.7(6) . . ? C27 C24 C22 112.3(3) . . ? C27' C24 C22 108.4(6) . . ? C26 C24 C22 109.1(3) . . ? C25 C24 C22 108.2(3) . . ? C25' C24 C26' 108.6(7) . . ? C27 C24 C26' 47.7(5) . . ? C27' C24 C26' 106.8(7) . . ? C26 C24 C26' 66.5(5) . . ? C25 C24 C26' 143.7(6) . . ? C22 C24 C26' 107.5(6) . . ? C10 C30 C31 122.9(2) . . ? C30 C31 C32 115.2(2) . . ? C30 C31 C33 123.3(2) . . ? C32 C31 C33 121.5(2) . . ? C12 C32 C31 123.8(2) . . ? C36' C33 C34 140.1(11) . . ? C36' C33 C35' 110.6(10) . . ? C34 C33 C35' 62.7(9) . . ? C36' C33 C34' 108.9(10) . . ? C34 C33 C34' 51.3(9) . . ? C35' C33 C34' 111.8(10) . . ? C36' C33 C36 49.8(9) . . ? C34 C33 C36 109.5(3) . . ? C35' C33 C36 142.6(11) . . ? C34' C33 C36 61.7(9) . . ? C36' C33 C35 61.3(9) . . ? C34 C33 C35 108.4(3) . . ? C35' C33 C35 50.9(9) . . ? C34' C33 C35 139.1(11) . . ? C36 C33 C35 107.5(3) . . ? C36' C33 C31 109.5(11) . . ? C34 C33 C31 109.9(2) . . ? C35' C33 C31 107.4(11) . . ? C34' C33 C31 108.6(11) . . ? C36 C33 C31 109.4(3) . . ? C35 C33 C31 112.1(2) . . ? C41 N40 C45 114.37(18) . . ? C41 N40 Co1 130.07(15) . . ? C45 N40 Co1 115.12(14) . . ? N40 C41 C42 125.4(2) . . ? C41 C42 C43 119.87(19) . . ? N46 C43 C42 122.8(2) . . ? N46 C43 C44 122.0(2) . . ? C42 C43 C44 115.2(2) . . ? C45 C44 C43 120.4(2) . . ? N40 C45 C44 124.7(2) . . ? C43 N46 C48 120.3(2) . . ? C43 N46 C47 122.3(2) . . ? C48 N46 C47 117.0(2) . . ? Cl4 C50 Cl3 109.3(4) . . ? Cl4' C50' Cl3' 113.1(11) . . ? Cl4" C50" Cl3" 105.1(14) . . ? Cl6 C55 Cl5 110.18(15) . . ? Cl8 C60 Cl7 110.87(16) . . ? Cl10 C65 Cl9 112.5(4) . . ? Cl11 C70 Cl12 95.4(11) . . ? Cl13 C70' Cl14 125.0(16) . . ? Cl16 C75 Cl15 136.4(12) . . ? Cl18 C75' Cl17 114.8(12) . . ? Cl20 C75" Cl19 115.0(13) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 29.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.798 _refine_diff_density_min -0.876 _refine_diff_density_rms 0.096 #===END