# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6aprc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H104 Cl6 Co2 N8' _chemical_formula_weight 1700.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 13.595(5) _cell_length_b 15.962(5) _cell_length_c 20.831(5) _cell_angle_alpha 90.352(5) _cell_angle_beta 90.037(5) _cell_angle_gamma 112.077(5) _cell_volume 4189(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour 'red block' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8826 _exptl_absorpt_correction_T_max 0.9271 _exptl_absorpt_process_details 'SADABS 2.05 (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22683 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_unetI/netI 0.1598 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15993 _reflns_number_gt 8934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.1139P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15993 _refine_ls_number_parameters 1026 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1492 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2388 _refine_ls_wR_factor_gt 0.1974 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 -0.13719(8) 0.15687(7) 0.91009(5) 0.0267(3) Uani 1 1 d . . . N1 N -0.2378(5) 0.1973(4) 0.9560(3) 0.0279(16) Uani 1 1 d . . . N2 N -0.0177(5) 0.2496(5) 0.9538(3) 0.0330(17) Uani 1 1 d . . . N3 N -0.0378(5) 0.1199(4) 0.8609(3) 0.0280(16) Uani 1 1 d . . . N4 N -0.2575(5) 0.0633(4) 0.8663(3) 0.0295(16) Uani 1 1 d . . . C1 C -0.3461(6) 0.1520(5) 0.9622(4) 0.0273(19) Uani 1 1 d . . . C2 C -0.3875(6) 0.2091(6) 0.9988(4) 0.034(2) Uani 1 1 d . . . C3 C -0.3044(6) 0.2870(5) 1.0145(4) 0.031(2) Uani 1 1 d . . . C4 C -0.2119(6) 0.2778(5) 0.9898(4) 0.0296(19) Uani 1 1 d . . . C5 C -0.1069(6) 0.3348(6) 1.0057(4) 0.033(2) Uani 1 1 d . . . H5 H -0.0978 0.3891 1.0282 0.040 Uiso 1 1 calc R . . C6 C -0.0209(6) 0.3196(5) 0.9923(4) 0.0278(19) Uani 1 1 d . . . C7 C 0.0850(6) 0.3735(5) 1.0173(4) 0.0279(19) Uani 1 1 d . . . C8 C 0.1513(6) 0.3319(6) 0.9946(4) 0.034(2) Uani 1 1 d . . . C9 C 0.0882(6) 0.2581(5) 0.9544(4) 0.0273(18) Uani 1 1 d . . . C10 C 0.1273(6) 0.2042(5) 0.9182(4) 0.0296(19) Uani 1 1 d . . . H10 H 0.1988 0.2103 0.9251 0.036 Uiso 1 1 calc R . . C11 C 0.0681(6) 0.1419(5) 0.8724(4) 0.0282(19) Uani 1 1 d . . . C12 C 0.1129(6) 0.0987(5) 0.8256(4) 0.0286(19) Uani 1 1 d . . . C13 C 0.0347(6) 0.0501(6) 0.7851(4) 0.0299(19) Uani 1 1 d . . . C14 C -0.0623(7) 0.0612(6) 0.8080(4) 0.036(2) Uani 1 1 d . . . C15 C -0.1610(6) 0.0156(6) 0.7845(4) 0.034(2) Uani 1 1 d . . . H15 H -0.1670 -0.0166 0.7453 0.041 Uiso 1 1 calc R . . C16 C -0.2531(6) 0.0126(5) 0.8133(4) 0.0277(18) Uani 1 1 d . . . C17 C -0.3554(6) -0.0525(6) 0.7967(4) 0.035(2) Uani 1 1 d . . . C18 C -0.4252(5) -0.0434(5) 0.8409(4) 0.0284(19) Uani 1 1 d . . . C19 C -0.3666(5) 0.0304(5) 0.8846(4) 0.0231(17) Uani 1 1 d . . . C20 C -0.4027(6) 0.0671(5) 0.9345(4) 0.0260(18) Uani 1 1 d . . . C21 C -0.5034(6) 0.1966(6) 1.0115(4) 0.037(2) Uani 1 1 d . . . H21A H -0.5058 0.2402 1.0449 0.044 Uiso 1 1 calc R . . H21B H -0.5427 0.1348 1.0277 0.044 Uiso 1 1 calc R . . C22 C -0.5573(7) 0.2114(6) 0.9501(5) 0.046(2) Uani 1 1 d . . . H22A H -0.6321 0.1996 0.9589 0.070 Uiso 1 1 calc R . . H22B H -0.5523 0.1700 0.9164 0.070 Uiso 1 1 calc R . . H22C H -0.5217 0.2739 0.9358 0.070 Uiso 1 1 calc R . . C23 C -0.3068(7) 0.3677(6) 1.0513(5) 0.046(3) Uani 1 1 d . . . H23A H -0.3725 0.3775 1.0404 0.055 Uiso 1 1 calc R . . H23B H -0.2456 0.4222 1.0384 0.055 Uiso 1 1 calc R . . C24 C -0.3027(9) 0.3550(7) 1.1234(5) 0.065(3) Uani 1 1 d . . . H24A H -0.3009 0.4098 1.1457 0.097 Uiso 1 1 calc R . . H24B H -0.2387 0.3435 1.1343 0.097 Uiso 1 1 calc R . . H24C H -0.3657 0.3036 1.1368 0.097 Uiso 1 1 calc R . . C25 C 0.1085(7) 0.4516(6) 1.0636(5) 0.040(2) Uani 1 1 d . . . H25A H 0.1849 0.4901 1.0610 0.048 Uiso 1 1 calc R . . H25B H 0.0678 0.4886 1.0503 0.048 Uiso 1 1 calc R . . C26 C 0.0818(8) 0.4235(7) 1.1319(5) 0.057(3) Uani 1 1 d . . . H26A H 0.1008 0.4774 1.1594 0.086 Uiso 1 1 calc R . . H26B H 0.1216 0.3867 1.1456 0.086 Uiso 1 1 calc R . . H26C H 0.0055 0.3881 1.1355 0.086 Uiso 1 1 calc R . . C27 C 0.2676(6) 0.3602(6) 1.0055(5) 0.042(2) Uani 1 1 d . . . H27A H 0.2831 0.3060 1.0160 0.050 Uiso 1 1 calc R . . H27B H 0.2879 0.4012 1.0433 0.050 Uiso 1 1 calc R . . C28 C 0.3362(7) 0.4077(6) 0.9490(5) 0.052(3) Uani 1 1 d . . . H28A H 0.4110 0.4211 0.9592 0.078 Uiso 1 1 calc R . . H28B H 0.3261 0.4642 0.9403 0.078 Uiso 1 1 calc R . . H28C H 0.3158 0.3684 0.9109 0.078 Uiso 1 1 calc R . . C29 C 0.2273(6) 0.1085(6) 0.8230(4) 0.033(2) Uani 1 1 d . . . H29A H 0.2535 0.1085 0.8674 0.040 Uiso 1 1 calc R . . H29B H 0.2318 0.0554 0.8003 0.040 Uiso 1 1 calc R . . C30 C 0.2985(6) 0.1931(6) 0.7900(5) 0.044(2) Uani 1 1 d . . . H30A H 0.3717 0.1958 0.7906 0.067 Uiso 1 1 calc R . . H30B H 0.2951 0.2461 0.8124 0.067 Uiso 1 1 calc R . . H30C H 0.2750 0.1926 0.7454 0.067 Uiso 1 1 calc R . . C31 C 0.0362(7) -0.0072(7) 0.7280(5) 0.053(3) Uani 1 1 d . . . H31A H -0.0281 -0.0634 0.7284 0.064 Uiso 1 1 calc R . . H31B H 0.0989 -0.0244 0.7309 0.064 Uiso 1 1 calc R . . C32 C 0.0403(9) 0.0421(9) 0.6650(6) 0.081(4) Uani 1 1 d . . . H32A H 0.0459 0.0042 0.6291 0.121 Uiso 1 1 calc R . . H32B H 0.1022 0.0991 0.6652 0.121 Uiso 1 1 calc R . . H32C H -0.0245 0.0547 0.6602 0.121 Uiso 1 1 calc R . . C33 C -0.3803(7) -0.1171(7) 0.7387(4) 0.044(2) Uani 1 1 d . . . H33A H -0.3248 -0.1431 0.7352 0.052 Uiso 1 1 calc R . . H33B H -0.4491 -0.1676 0.7458 0.052 Uiso 1 1 calc R . . C34 C -0.3857(7) -0.0710(7) 0.6761(5) 0.054(3) Uani 1 1 d . . . H34A H -0.4193 -0.1169 0.6430 0.080 Uiso 1 1 calc R . . H34B H -0.3138 -0.0332 0.6625 0.080 Uiso 1 1 calc R . . H34C H -0.4275 -0.0332 0.6823 0.080 Uiso 1 1 calc R . . C35 C -0.5448(6) -0.0931(6) 0.8340(4) 0.039(2) Uani 1 1 d . . . H35A H -0.5594 -0.1415 0.8013 0.046 Uiso 1 1 calc R . . H35B H -0.5743 -0.1218 0.8754 0.046 Uiso 1 1 calc R . . C36 C -0.5998(6) -0.0297(6) 0.8145(4) 0.036(2) Uani 1 1 d . . . H36A H -0.6760 -0.0645 0.8089 0.054 Uiso 1 1 calc R . . H36B H -0.5699 -0.0003 0.7740 0.054 Uiso 1 1 calc R . . H36C H -0.5891 0.0163 0.8480 0.054 Uiso 1 1 calc R . . C37 C -0.5092(6) 0.0107(6) 0.9653(4) 0.032(2) Uani 1 1 d . . . H37A H -0.5569 0.0448 0.9645 0.038 Uiso 1 1 calc R . . H37B H -0.5436 -0.0462 0.9408 0.038 Uiso 1 1 calc R . . Co2 Co 0.36387(8) 0.67130(7) 0.58409(5) 0.0248(3) Uani 1 1 d . . . N1A N 0.2442(5) 0.5839(4) 0.6309(3) 0.0258(15) Uani 1 1 d . . . N2A N 0.4644(5) 0.6378(4) 0.6348(3) 0.0262(15) Uani 1 1 d . . . N3A N 0.4834(5) 0.7594(4) 0.5389(3) 0.0284(16) Uani 1 1 d . . . N4A N 0.2627(4) 0.7076(4) 0.5362(3) 0.0246(15) Uani 1 1 d . . . C1A C 0.1395(6) 0.5507(5) 0.6139(4) 0.0288(19) Uani 1 1 d . . . C2A C 0.0783(6) 0.4874(5) 0.6638(4) 0.0269(18) Uani 1 1 d . . . C3A C 0.1482(6) 0.4859(5) 0.7099(4) 0.0296(19) Uani 1 1 d . . . C4A C 0.2520(6) 0.5424(5) 0.6865(4) 0.0270(18) Uani 1 1 d . . . C5A C 0.3462(6) 0.5461(5) 0.7152(4) 0.0290(19) Uani 1 1 d . . . H5A H 0.3419 0.5188 0.7561 0.035 Uiso 1 1 calc R . . C6A C 0.4450(6) 0.5868(6) 0.6881(4) 0.0300(19) Uani 1 1 d . . . C7A C 0.5396(6) 0.5746(6) 0.7111(4) 0.033(2) Uani 1 1 d . . . C8A C 0.6145(6) 0.6183(5) 0.6694(4) 0.031(2) Uani 1 1 d . . . C9A C 0.5712(6) 0.6590(5) 0.6221(4) 0.0289(19) Uani 1 1 d . . . C10A C 0.6247(6) 0.7142(5) 0.5733(4) 0.0278(19) Uani 1 1 d . . . H10A H 0.6944 0.7171 0.5644 0.033 Uiso 1 1 calc R . . C11A C 0.5863(6) 0.7656(5) 0.5363(4) 0.0272(18) Uani 1 1 d . . . C12A C 0.6471(6) 0.8374(6) 0.4945(4) 0.034(2) Uani 1 1 d . . . C13A C 0.5832(6) 0.8781(5) 0.4726(4) 0.031(2) Uani 1 1 d . . . C14A C 0.4813(6) 0.8275(5) 0.4994(4) 0.0291(19) Uani 1 1 d . . . C15A C 0.3868(6) 0.8397(5) 0.4837(4) 0.0301(19) Uani 1 1 d . . . H15A H 0.3932 0.8934 0.4617 0.036 Uiso 1 1 calc R . . C16A C 0.2879(6) 0.7810(5) 0.4975(4) 0.0269(19) Uani 1 1 d . . . C17A C 0.1902(6) 0.7851(6) 0.4693(4) 0.032(2) Uani 1 1 d . . . C18A C 0.1091(6) 0.7106(5) 0.4879(4) 0.0290(19) Uani 1 1 d . . . C19A C 0.1532(6) 0.6589(5) 0.5302(4) 0.0232(17) Uani 1 1 d . . . C20A C 0.0965(5) 0.5791(5) 0.5615(4) 0.0245(18) Uani 1 1 d . . . C21A C -0.0404(5) 0.4414(6) 0.6724(5) 0.040(2) Uani 1 1 d . . . H21C H -0.0551 0.3989 0.7088 0.048 Uiso 1 1 calc R . . H21D H -0.0719 0.4059 0.6332 0.048 Uiso 1 1 calc R . . C22A C -0.0923(7) 0.5099(6) 0.6851(5) 0.044(2) Uani 1 1 d . . . H22D H -0.1675 0.4778 0.6952 0.067 Uiso 1 1 calc R . . H22E H -0.0859 0.5470 0.6468 0.067 Uiso 1 1 calc R . . H22F H -0.0567 0.5490 0.7213 0.067 Uiso 1 1 calc R . . C23A C 0.1254(6) 0.4347(6) 0.7720(5) 0.041(2) Uani 1 1 d . . . H23C H 0.0614 0.4393 0.7918 0.049 Uiso 1 1 calc R . . H23D H 0.1857 0.4630 0.8019 0.049 Uiso 1 1 calc R . . C24A C 0.1079(7) 0.3366(7) 0.7630(5) 0.050(3) Uani 1 1 d . . . H24D H 0.0906 0.3057 0.8044 0.075 Uiso 1 1 calc R . . H24E H 0.1726 0.3316 0.7459 0.075 Uiso 1 1 calc R . . H24F H 0.0492 0.3086 0.7329 0.075 Uiso 1 1 calc R . . C25A C 0.5432(6) 0.5225(7) 0.7699(5) 0.048(3) Uani 1 1 d . . . H25C H 0.5999 0.4983 0.7645 0.058 Uiso 1 1 calc R . . H25D H 0.4750 0.4703 0.7735 0.058 Uiso 1 1 calc R . . C26A C 0.5632(9) 0.5768(8) 0.8325(5) 0.072(4) Uani 1 1 d . . . H26D H 0.5539 0.5359 0.8689 0.109 Uiso 1 1 calc R . . H26E H 0.5126 0.6071 0.8360 0.109 Uiso 1 1 calc R . . H26F H 0.6357 0.6221 0.8327 0.109 Uiso 1 1 calc R . . C27A C 0.7305(6) 0.6270(6) 0.6694(4) 0.036(2) Uani 1 1 d . . . H27C H 0.7524 0.6213 0.6248 0.044 Uiso 1 1 calc R . . H27D H 0.7370 0.5769 0.6946 0.044 Uiso 1 1 calc R . . C28A C 0.8052(6) 0.7175(7) 0.6979(5) 0.050(3) Uani 1 1 d . . . H28D H 0.8777 0.7187 0.6993 0.074 Uiso 1 1 calc R . . H28E H 0.7822 0.7245 0.7415 0.074 Uiso 1 1 calc R . . H28F H 0.8032 0.7671 0.6711 0.074 Uiso 1 1 calc R . . C29A C 0.7634(6) 0.8595(6) 0.4797(4) 0.038(2) Uani 1 1 d . . . H29C H 0.7745 0.8021 0.4735 0.046 Uiso 1 1 calc R . . H29D H 0.7807 0.8930 0.4388 0.046 Uiso 1 1 calc R . . C30A C 0.8397(6) 0.9148(6) 0.5308(5) 0.052(3) Uani 1 1 d . . . H30D H 0.9126 0.9259 0.5176 0.078 Uiso 1 1 calc R . . H30E H 0.8247 0.8816 0.5714 0.078 Uiso 1 1 calc R . . H30F H 0.8311 0.9726 0.5366 0.078 Uiso 1 1 calc R . . C31A C 0.6084(7) 0.9541(6) 0.4273(4) 0.036(2) Uani 1 1 d . . . H31C H 0.6830 0.9957 0.4338 0.044 Uiso 1 1 calc R . . H31D H 0.5622 0.9881 0.4363 0.044 Uiso 1 1 calc R . . C32A C 0.5928(9) 0.9213(7) 0.3577(4) 0.055(3) Uani 1 1 d . . . H32D H 0.6085 0.9733 0.3291 0.082 Uiso 1 1 calc R . . H32E H 0.5191 0.8798 0.3512 0.082 Uiso 1 1 calc R . . H32F H 0.6407 0.8899 0.3481 0.082 Uiso 1 1 calc R . . C33A C 0.1879(6) 0.8558(6) 0.4238(4) 0.038(2) Uani 1 1 d . . . H33C H 0.2507 0.9118 0.4318 0.045 Uiso 1 1 calc R . . H33D H 0.1238 0.8694 0.4322 0.045 Uiso 1 1 calc R . . C34A C 0.1875(9) 0.8277(7) 0.3532(5) 0.060(3) Uani 1 1 d . . . H34D H 0.1836 0.8758 0.3256 0.090 Uiso 1 1 calc R . . H34E H 0.1260 0.7719 0.3450 0.090 Uiso 1 1 calc R . . H34F H 0.2528 0.8175 0.3439 0.090 Uiso 1 1 calc R . . C35A C -0.0030(6) 0.6945(6) 0.4714(4) 0.036(2) Uani 1 1 d . . . H35C H -0.0398 0.6309 0.4574 0.043 Uiso 1 1 calc R . . H35D H -0.0047 0.7340 0.4353 0.043 Uiso 1 1 calc R . . C36A C -0.0620(6) 0.7142(6) 0.5299(5) 0.046(3) Uani 1 1 d . . . H36D H -0.1362 0.7009 0.5183 0.069 Uiso 1 1 calc R . . H36E H -0.0279 0.7780 0.5423 0.069 Uiso 1 1 calc R . . H36F H -0.0590 0.6761 0.5659 0.069 Uiso 1 1 calc R . . C37A C -0.0066(6) 0.5177(5) 0.5327(4) 0.0293(19) Uani 1 1 d . . . H37C H -0.0548 0.5509 0.5291 0.035 Uiso 1 1 calc R . . H37D H -0.0401 0.4659 0.5617 0.035 Uiso 1 1 calc R . . C38 C -0.1775(7) 0.1047(6) 1.0758(5) 0.046(2) Uani 1 1 d . . . H38 H -0.2393 0.1172 1.0846 0.055 Uiso 1 1 calc R . . C39 C -0.0868(9) 0.1496(7) 1.1088(5) 0.051(3) Uani 1 1 d . . . H39 H -0.0860 0.1925 1.1408 0.061 Uiso 1 1 calc R . . C40 C 0.0089(7) 0.1330(6) 1.0960(4) 0.039(2) Uani 1 1 d . . . C41 C 0.0032(7) 0.0663(5) 1.0481(4) 0.0296(19) Uani 1 1 d . . . C42 C -0.0925(6) 0.0203(6) 1.0140(4) 0.032(2) Uani 1 1 d . . . C43 C -0.1815(7) 0.0401(6) 1.0288(4) 0.036(2) Uani 1 1 d . . . H43 H -0.2462 0.0092 1.0065 0.044 Uiso 1 1 calc R . . C44 C 0.1040(9) 0.1806(6) 1.1292(5) 0.050(3) Uani 1 1 d . . . H44 H 0.1067 0.2249 1.1606 0.060 Uiso 1 1 calc R . . C45 C 0.1934(8) 0.1623(7) 1.1158(5) 0.052(3) Uani 1 1 d . . . H45 H 0.2576 0.1930 1.1386 0.063 Uiso 1 1 calc R . . C46 C 0.1892(7) 0.0983(6) 1.0683(5) 0.042(2) Uani 1 1 d . . . H46 H 0.2523 0.0879 1.0595 0.050 Uiso 1 1 calc R . . C47 C 0.0983(6) 0.0491(5) 1.0335(4) 0.034(2) Uani 1 1 d . . . C38A C 0.4049(6) 0.5186(6) 0.4867(4) 0.0303(19) Uani 1 1 d . . . C39A C 0.3181(6) 0.5386(6) 0.4736(4) 0.034(2) Uani 1 1 d . . . H39A H 0.2558 0.5119 0.4986 0.040 Uiso 1 1 calc R . . C40A C 0.3185(7) 0.5976(6) 0.4242(4) 0.038(2) Uani 1 1 d . . . H40A H 0.2562 0.6096 0.4160 0.045 Uiso 1 1 calc R . . C41A C 0.4056(7) 0.6379(6) 0.3880(4) 0.037(2) Uani 1 1 d . . . H41A H 0.4041 0.6773 0.3544 0.045 Uiso 1 1 calc R . . C42A C 0.4988(7) 0.6216(6) 0.4001(4) 0.034(2) Uani 1 1 d . . . C43A C 0.5912(7) 0.6655(6) 0.3652(4) 0.036(2) Uani 1 1 d . . . H43A H 0.5913 0.7067 0.3325 0.043 Uiso 1 1 calc R . . C44A C 0.6808(7) 0.6499(6) 0.3774(5) 0.040(2) Uani 1 1 d . . . H44A H 0.7425 0.6796 0.3525 0.049 Uiso 1 1 calc R . . C45A C 0.6838(7) 0.5908(6) 0.4261(5) 0.039(2) Uani 1 1 d . . . H45A H 0.7478 0.5819 0.4345 0.047 Uiso 1 1 calc R . . C46A C 0.5940(6) 0.5451(5) 0.4624(4) 0.0289(19) Uani 1 1 d . . . C47A C 0.5013(6) 0.5626(5) 0.4498(4) 0.0263(18) Uani 1 1 d . . . C48 C -0.3041(6) 0.2726(6) 0.8259(5) 0.046(3) Uani 1 1 d . . . H48 H -0.3201 0.2460 0.8698 0.055 Uiso 1 1 calc R . . Cl1 Cl -0.3882(2) 0.1949(2) 0.77124(16) 0.0702(8) Uani 1 1 d . . . Cl2 Cl -0.17004(19) 0.2951(2) 0.80956(14) 0.0635(8) Uani 1 1 d . . . Cl3 Cl -0.3296(3) 0.3730(2) 0.82542(19) 0.0842(10) Uani 1 1 d . . . C49 C 0.2060(7) 0.7694(6) 0.6772(5) 0.044(2) Uani 1 1 d . . . H49 H 0.1803 0.7184 0.6456 0.053 Uiso 1 1 calc R . . Cl4 Cl 0.34506(18) 0.81736(18) 0.67394(13) 0.0548(7) Uani 1 1 d . . . Cl5 Cl 0.1550(2) 0.85072(19) 0.65536(17) 0.0700(9) Uani 1 1 d . . . Cl6 Cl 0.1632(3) 0.7275(2) 0.75259(15) 0.0838(10) 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 0.0152(5) 0.0330(6) 0.0353(7) 0.0036(5) 0.0020(5) 0.0130(5) N1 0.027(4) 0.026(4) 0.033(4) 0.005(3) -0.002(3) 0.013(3) N2 0.028(4) 0.041(4) 0.037(4) 0.010(3) 0.002(3) 0.020(3) N3 0.024(4) 0.031(4) 0.031(4) 0.006(3) 0.000(3) 0.013(3) N4 0.015(3) 0.040(4) 0.040(4) 0.005(3) 0.002(3) 0.019(3) C1 0.016(4) 0.028(5) 0.044(5) 0.004(4) 0.006(4) 0.016(3) C2 0.025(4) 0.035(5) 0.047(5) -0.002(4) 0.001(4) 0.018(4) C3 0.029(5) 0.028(5) 0.045(5) 0.004(4) 0.008(4) 0.020(4) C4 0.024(4) 0.033(5) 0.035(5) 0.012(4) 0.004(4) 0.015(4) C5 0.031(5) 0.033(5) 0.035(5) -0.003(4) 0.001(4) 0.013(4) C6 0.020(4) 0.033(5) 0.034(5) 0.011(4) 0.003(4) 0.014(4) C7 0.026(4) 0.025(4) 0.035(5) 0.007(4) 0.004(4) 0.011(3) C8 0.026(4) 0.035(5) 0.040(5) 0.009(4) 0.004(4) 0.010(4) C9 0.019(4) 0.032(5) 0.033(5) 0.006(4) 0.000(4) 0.011(3) C10 0.013(4) 0.039(5) 0.040(5) 0.004(4) 0.003(4) 0.013(3) C11 0.021(4) 0.028(4) 0.037(5) 0.011(4) 0.002(4) 0.012(3) C12 0.011(4) 0.040(5) 0.038(5) 0.013(4) 0.009(4) 0.013(3) C13 0.022(4) 0.034(5) 0.037(5) -0.003(4) 0.001(4) 0.015(4) C14 0.033(5) 0.032(5) 0.046(6) -0.010(4) 0.001(4) 0.016(4) C15 0.027(5) 0.040(5) 0.038(5) -0.003(4) 0.001(4) 0.015(4) C16 0.020(4) 0.034(5) 0.034(5) -0.003(4) -0.004(4) 0.017(4) C17 0.025(4) 0.044(5) 0.043(5) -0.011(4) -0.005(4) 0.019(4) C18 0.009(4) 0.033(5) 0.041(5) -0.004(4) -0.010(3) 0.005(3) C19 0.009(3) 0.029(4) 0.034(5) 0.001(4) 0.002(3) 0.010(3) C20 0.021(4) 0.028(4) 0.032(5) 0.003(4) 0.002(4) 0.013(3) C21 0.026(4) 0.050(6) 0.041(5) -0.001(4) 0.004(4) 0.023(4) C22 0.027(5) 0.054(6) 0.066(7) 0.006(5) -0.003(5) 0.023(4) C23 0.022(4) 0.038(5) 0.074(7) -0.013(5) 0.005(5) 0.007(4) C24 0.083(8) 0.061(7) 0.049(7) -0.031(6) 0.003(6) 0.027(6) C25 0.031(5) 0.032(5) 0.055(6) 0.000(4) 0.006(4) 0.010(4) C26 0.062(7) 0.044(6) 0.054(7) -0.005(5) -0.006(6) 0.007(5) C27 0.015(4) 0.057(6) 0.058(6) -0.005(5) -0.011(4) 0.017(4) C28 0.029(5) 0.042(6) 0.083(8) 0.004(5) 0.016(5) 0.011(4) C29 0.020(4) 0.046(5) 0.042(5) 0.000(4) 0.003(4) 0.021(4) C30 0.021(4) 0.056(6) 0.062(7) 0.004(5) 0.010(4) 0.020(4) C31 0.034(5) 0.074(8) 0.057(7) -0.019(6) 0.007(5) 0.026(5) C32 0.050(7) 0.125(11) 0.063(8) -0.024(8) 0.010(6) 0.028(7) C33 0.025(5) 0.060(6) 0.047(6) -0.010(5) 0.001(4) 0.017(4) C34 0.051(6) 0.053(6) 0.046(6) 0.001(5) 0.000(5) 0.007(5) C35 0.031(5) 0.046(6) 0.041(5) -0.005(4) -0.004(4) 0.017(4) C36 0.011(4) 0.050(6) 0.050(6) 0.006(4) -0.001(4) 0.013(4) C37 0.027(4) 0.030(5) 0.037(5) 0.000(4) 0.002(4) 0.010(4) Co2 0.0139(5) 0.0293(6) 0.0336(6) 0.0024(5) -0.0015(5) 0.0108(4) N1A 0.024(4) 0.027(4) 0.031(4) 0.000(3) -0.007(3) 0.014(3) N2A 0.018(3) 0.033(4) 0.033(4) 0.002(3) 0.003(3) 0.015(3) N3A 0.022(4) 0.032(4) 0.036(4) -0.006(3) -0.006(3) 0.015(3) N4A 0.009(3) 0.034(4) 0.036(4) -0.002(3) 0.001(3) 0.014(3) C1A 0.024(4) 0.023(4) 0.040(5) 0.002(4) 0.002(4) 0.010(3) C2A 0.018(4) 0.037(5) 0.029(4) 0.006(4) 0.001(3) 0.014(3) C3A 0.020(4) 0.038(5) 0.036(5) 0.000(4) -0.005(4) 0.017(4) C4A 0.027(4) 0.021(4) 0.035(5) 0.000(4) -0.002(4) 0.011(3) C5A 0.024(4) 0.027(5) 0.036(5) 0.006(4) -0.005(4) 0.010(3) C6A 0.016(4) 0.044(5) 0.031(5) 0.001(4) -0.001(3) 0.012(4) C7A 0.026(4) 0.038(5) 0.043(5) 0.006(4) -0.006(4) 0.023(4) C8A 0.018(4) 0.039(5) 0.043(5) -0.002(4) -0.004(4) 0.018(4) C9A 0.012(4) 0.036(5) 0.041(5) -0.005(4) 0.001(4) 0.011(3) C10A 0.011(4) 0.033(5) 0.043(5) -0.005(4) 0.000(4) 0.013(3) C11A 0.014(4) 0.028(4) 0.035(5) -0.001(4) -0.002(3) 0.002(3) C12A 0.019(4) 0.030(5) 0.048(5) 0.004(4) 0.003(4) 0.003(4) C13A 0.020(4) 0.029(5) 0.044(5) 0.005(4) 0.006(4) 0.009(3) C14A 0.019(4) 0.027(4) 0.044(5) 0.000(4) 0.002(4) 0.012(3) C15A 0.022(4) 0.026(5) 0.043(5) 0.004(4) 0.000(4) 0.010(3) C16A 0.015(4) 0.016(4) 0.048(5) 0.004(4) 0.005(4) 0.003(3) C17A 0.020(4) 0.040(5) 0.037(5) 0.000(4) -0.002(4) 0.013(4) C18A 0.017(4) 0.034(5) 0.038(5) 0.006(4) -0.004(4) 0.012(3) C19A 0.017(4) 0.027(4) 0.029(4) 0.000(3) -0.002(3) 0.013(3) C20A 0.012(4) 0.030(4) 0.035(5) 0.000(4) 0.002(3) 0.013(3) C21A 0.006(4) 0.063(6) 0.046(6) 0.016(5) 0.005(4) 0.007(4) C22A 0.033(5) 0.061(6) 0.045(6) 0.002(5) 0.012(4) 0.025(5) C23A 0.025(4) 0.048(6) 0.051(6) 0.005(5) -0.002(4) 0.015(4) C24A 0.050(6) 0.061(7) 0.047(6) 0.015(5) 0.001(5) 0.029(5) C25A 0.015(4) 0.071(7) 0.065(7) 0.016(5) -0.008(4) 0.025(4) C26A 0.071(8) 0.105(10) 0.029(6) 0.016(6) -0.018(5) 0.019(7) C27A 0.021(4) 0.049(6) 0.044(5) 0.012(4) 0.001(4) 0.020(4) C28A 0.017(4) 0.075(7) 0.050(6) -0.018(5) -0.006(4) 0.011(4) C29A 0.026(5) 0.043(5) 0.040(5) 0.006(4) 0.003(4) 0.006(4) C30A 0.018(4) 0.041(6) 0.090(8) -0.003(5) 0.003(5) 0.003(4) C31A 0.025(4) 0.035(5) 0.047(6) 0.003(4) 0.005(4) 0.008(4) C32A 0.078(8) 0.044(6) 0.034(6) 0.011(5) 0.005(5) 0.013(5) C33A 0.026(4) 0.031(5) 0.062(6) 0.016(4) -0.004(4) 0.018(4) C34A 0.070(7) 0.063(7) 0.048(7) 0.024(5) -0.007(5) 0.026(6) C35A 0.018(4) 0.038(5) 0.056(6) 0.001(4) -0.008(4) 0.014(4) C36A 0.019(4) 0.049(6) 0.076(7) -0.005(5) -0.011(5) 0.021(4) C37A 0.012(4) 0.034(5) 0.044(5) -0.005(4) -0.001(4) 0.011(3) C38 0.036(5) 0.053(6) 0.061(7) 0.012(5) 0.004(5) 0.031(5) C39 0.085(8) 0.042(6) 0.044(6) 0.015(5) 0.020(6) 0.044(6) C40 0.047(6) 0.040(5) 0.041(5) 0.004(4) -0.006(5) 0.028(4) C41 0.040(5) 0.021(4) 0.033(5) 0.007(4) -0.004(4) 0.017(4) C42 0.023(4) 0.034(5) 0.038(5) 0.017(4) 0.005(4) 0.012(4) C43 0.032(5) 0.040(5) 0.043(5) 0.015(4) 0.011(4) 0.020(4) C44 0.082(8) 0.045(6) 0.038(6) -0.002(5) -0.019(6) 0.041(6) C45 0.057(7) 0.040(6) 0.060(7) -0.003(5) -0.026(5) 0.019(5) C46 0.025(5) 0.031(5) 0.071(7) 0.004(5) -0.014(5) 0.012(4) C47 0.027(5) 0.031(5) 0.047(6) 0.002(4) -0.003(4) 0.016(4) C38A 0.022(4) 0.036(5) 0.036(5) 0.000(4) 0.000(4) 0.014(4) C39A 0.016(4) 0.039(5) 0.049(6) -0.010(4) -0.002(4) 0.014(4) C40A 0.035(5) 0.043(5) 0.043(6) -0.010(4) -0.009(4) 0.024(4) C41A 0.034(5) 0.045(5) 0.041(5) 0.003(4) -0.001(4) 0.025(4) C42A 0.039(5) 0.029(5) 0.031(5) -0.001(4) 0.004(4) 0.009(4) C43A 0.038(5) 0.031(5) 0.044(6) 0.000(4) -0.004(4) 0.019(4) C44A 0.038(5) 0.035(5) 0.044(6) 0.001(4) 0.016(4) 0.009(4) C45A 0.030(5) 0.032(5) 0.058(6) -0.006(4) 0.003(5) 0.016(4) C46A 0.017(4) 0.032(5) 0.036(5) -0.006(4) 0.003(4) 0.007(3) C47A 0.013(4) 0.023(4) 0.042(5) 0.002(4) -0.002(4) 0.006(3) C48 0.021(4) 0.058(6) 0.056(6) 0.020(5) -0.001(4) 0.013(4) Cl1 0.0507(15) 0.0651(19) 0.087(2) -0.0079(16) -0.0149(15) 0.0128(13) Cl2 0.0317(13) 0.083(2) 0.0682(18) 0.0295(15) 0.0067(12) 0.0125(13) Cl3 0.080(2) 0.061(2) 0.117(3) -0.0008(18) -0.018(2) 0.0312(17) C49 0.051(6) 0.038(6) 0.047(6) -0.005(5) -0.007(5) 0.020(5) Cl4 0.0353(13) 0.0661(17) 0.0651(17) -0.0223(14) -0.0152(12) 0.0216(12) Cl5 0.0504(16) 0.0570(17) 0.113(2) 0.0053(16) -0.0065(16) 0.0322(14) Cl6 0.114(3) 0.075(2) 0.061(2) 0.0122(16) 0.0331(19) 0.0337(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 N3 1.955(6) . ? Co1 N2 1.959(7) . ? Co1 N1 1.965(7) . ? Co1 N4 1.970(7) . ? N1 C1 1.382(9) . ? N1 C4 1.384(11) . ? N2 C6 1.384(10) . ? N2 C9 1.395(9) . ? N3 C11 1.368(9) . ? N3 C14 1.397(11) . ? N4 C16 1.381(10) . ? N4 C19 1.428(9) . ? C1 C20 1.403(11) . ? C1 C2 1.451(11) . ? C2 C3 1.367(12) . ? C2 C21 1.536(10) . ? C3 C4 1.417(10) . ? C3 C23 1.505(12) . ? C4 C5 1.413(11) . ? C5 C6 1.310(10) . ? C5 H5 0.9500 . ? C6 C7 1.466(11) . ? C7 C8 1.387(11) . ? C7 C25 1.507(12) . ? C8 C9 1.433(12) . ? C8 C27 1.489(11) . ? C9 C10 1.388(11) . ? C10 C11 1.390(12) . ? C10 H10 0.9500 . ? C11 C12 1.449(11) . ? C12 C13 1.346(11) . ? C12 C29 1.506(10) . ? C13 C14 1.474(11) . ? C13 C31 1.502(12) . ? C14 C15 1.353(11) . ? C15 C16 1.372(10) . ? C15 H15 0.9500 . ? C16 C17 1.429(11) . ? C17 C18 1.369(11) . ? C17 C33 1.537(12) . ? C18 C19 1.460(11) . ? C18 C35 1.525(10) . ? C19 C20 1.368(10) . ? C20 C37 1.533(11) . ? C21 C22 1.536(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.520(14) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.498(13) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.521(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.505(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.524(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.516(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.523(11) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C37 1.528(16) 2_457 ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? Co2 N3A 1.950(7) . ? Co2 N2A 1.956(6) . ? Co2 N4A 1.957(6) . ? Co2 N1A 1.964(6) . ? N1A C4A 1.362(10) . ? N1A C1A 1.365(9) . ? N2A C6A 1.348(10) . ? N2A C9A 1.388(9) . ? N3A C11A 1.366(9) . ? N3A C14A 1.376(10) . ? N4A C16A 1.360(10) . ? N4A C19A 1.402(9) . ? C1A C20A 1.394(11) . ? C1A C2A 1.474(11) . ? C2A C3A 1.357(10) . ? C2A C21A 1.513(10) . ? C3A C4A 1.447(11) . ? C3A C23A 1.503(12) . ? C4A C5A 1.393(10) . ? C5A C6A 1.376(10) . ? C5A H5A 0.9500 . ? C6A C7A 1.452(10) . ? C7A C8A 1.325(11) . ? C7A C25A 1.496(12) . ? C8A C9A 1.426(11) . ? C8A C27A 1.530(10) . ? C9A C10A 1.366(11) . ? C10A C11A 1.368(11) . ? C10A H10A 0.9500 . ? C11A C12A 1.434(11) . ? C12A C13A 1.346(11) . ? C12A C29A 1.517(11) . ? C13A C14A 1.431(11) . ? C13A C31A 1.477(11) . ? C14A C15A 1.408(10) . ? C15A C16A 1.351(10) . ? C15A H15A 0.9500 . ? C16A C17A 1.476(11) . ? C17A C18A 1.342(11) . ? C17A C33A 1.486(11) . ? C18A C19A 1.482(10) . ? C18A C35A 1.487(10) . ? C19A C20A 1.384(10) . ? C20A C37A 1.497(10) . ? C21A C22A 1.530(12) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23A C24A 1.504(13) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A C26A 1.528(15) . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C27A C28A 1.535(12) . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A C30A 1.512(13) . ? C29A H29C 0.9900 . ? C29A H29D 0.9900 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31A C32A 1.525(13) . ? C31A H31C 0.9900 . ? C31A H31D 0.9900 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33A C34A 1.535(13) . ? C33A H33C 0.9900 . ? C33A H33D 0.9900 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? C35A C36A 1.553(12) . ? C35A H35C 0.9900 . ? C35A H35D 0.9900 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 0.9800 . ? C37A C37A 1.506(16) 2_566 ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C38 C39 1.355(14) . ? C38 C43 1.404(13) . ? C38 H38 0.9500 . ? C39 C40 1.446(12) . ? C39 H39 0.9500 . ? C40 C44 1.409(13) . ? C40 C41 1.435(12) . ? C41 C42 1.418(11) . ? C41 C47 1.451(11) . ? C42 C43 1.395(11) . ? C42 C47 1.460(12) 2_557 ? C43 H43 0.9500 . ? C44 C45 1.381(14) . ? C44 H44 0.9500 . ? C45 C46 1.403(14) . ? C45 H45 0.9500 . ? C46 C47 1.391(12) . ? C46 H46 0.9500 . ? C47 C42 1.460(12) 2_557 ? C38A C39A 1.362(11) . ? C38A C47A 1.455(11) . ? C38A C46A 1.477(11) 2_666 ? C39A C40A 1.397(12) . ? C39A H39A 0.9500 . ? C40A C41A 1.348(12) . ? C40A H40A 0.9500 . ? C41A C42A 1.410(11) . ? C41A H41A 0.9500 . ? C42A C43A 1.394(11) . ? C42A C47A 1.412(11) . ? C43A C44A 1.355(12) . ? C43A H43A 0.9500 . ? C44A C45A 1.401(12) . ? C44A H44A 0.9500 . ? C45A C46A 1.390(11) . ? C45A H45A 0.9500 . ? C46A C47A 1.414(10) . ? C46A C38A 1.477(11) 2_666 ? C48 Cl1 1.749(10) . ? C48 Cl2 1.754(9) . ? C48 Cl3 1.763(10) . ? C48 H48 1.0000 . ? C49 Cl6 1.724(10) . ? C49 Cl5 1.748(9) . ? C49 Cl4 1.754(10) . ? C49 H49 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 N2 89.9(3) . . ? N3 Co1 N1 177.3(3) . . ? N2 Co1 N1 90.6(3) . . ? N3 Co1 N4 90.2(3) . . ? N2 Co1 N4 179.8(3) . . ? N1 Co1 N4 89.4(3) . . ? C1 N1 C4 106.6(6) . . ? C1 N1 Co1 127.7(5) . . ? C4 N1 Co1 125.6(5) . . ? C6 N2 C9 105.3(7) . . ? C6 N2 Co1 127.2(5) . . ? C9 N2 Co1 127.5(6) . . ? C11 N3 C14 105.7(7) . . ? C11 N3 Co1 127.8(6) . . ? C14 N3 Co1 126.4(5) . . ? C16 N4 C19 105.5(6) . . ? C16 N4 Co1 127.1(5) . . ? C19 N4 Co1 127.3(5) . . ? N1 C1 C20 123.7(7) . . ? N1 C1 C2 108.1(7) . . ? C20 C1 C2 128.1(7) . . ? C3 C2 C1 108.1(7) . . ? C3 C2 C21 122.3(7) . . ? C1 C2 C21 129.1(8) . . ? C2 C3 C4 106.4(7) . . ? C2 C3 C23 128.3(7) . . ? C4 C3 C23 125.3(8) . . ? N1 C4 C5 123.8(7) . . ? N1 C4 C3 110.7(7) . . ? C5 C4 C3 124.8(8) . . ? C6 C5 C4 126.0(8) . . ? C6 C5 H5 117.0 . . ? C4 C5 H5 117.0 . . ? C5 C6 N2 125.0(8) . . ? C5 C6 C7 124.3(8) . . ? N2 C6 C7 110.7(6) . . ? C8 C7 C6 105.8(7) . . ? C8 C7 C25 129.6(8) . . ? C6 C7 C25 124.4(7) . . ? C7 C8 C9 107.1(7) . . ? C7 C8 C27 127.6(8) . . ? C9 C8 C27 125.2(8) . . ? C10 C9 N2 123.9(7) . . ? C10 C9 C8 124.9(7) . . ? N2 C9 C8 111.1(7) . . ? C9 C10 C11 123.9(7) . . ? C9 C10 H10 118.1 . . ? C11 C10 H10 118.1 . . ? N3 C11 C10 124.9(7) . . ? N3 C11 C12 110.6(7) . . ? C10 C11 C12 124.2(7) . . ? C13 C12 C11 108.0(7) . . ? C13 C12 C29 126.7(8) . . ? C11 C12 C29 125.3(8) . . ? C12 C13 C14 106.1(7) . . ? C12 C13 C31 130.8(7) . . ? C14 C13 C31 123.1(8) . . ? C15 C14 N3 125.5(7) . . ? C15 C14 C13 124.8(8) . . ? N3 C14 C13 109.5(7) . . ? C14 C15 C16 124.7(8) . . ? C14 C15 H15 117.6 . . ? C16 C15 H15 117.6 . . ? C15 C16 N4 124.6(7) . . ? C15 C16 C17 123.2(8) . . ? N4 C16 C17 111.7(7) . . ? C18 C17 C16 106.7(7) . . ? C18 C17 C33 127.7(7) . . ? C16 C17 C33 125.6(7) . . ? C17 C18 C19 108.2(6) . . ? C17 C18 C35 122.0(7) . . ? C19 C18 C35 128.9(7) . . ? C20 C19 N4 122.5(7) . . ? C20 C19 C18 129.7(7) . . ? N4 C19 C18 107.8(6) . . ? C19 C20 C1 124.4(7) . . ? C19 C20 C37 118.8(7) . . ? C1 C20 C37 116.7(7) . . ? C2 C21 C22 111.1(7) . . ? C2 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C2 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 C24 111.8(8) . . ? C3 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C3 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C7 113.9(8) . . ? C26 C25 H25A 108.8 . . ? C7 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? C7 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C28 114.6(8) . . ? C8 C27 H27A 108.6 . . ? C28 C27 H27A 108.6 . . ? C8 C27 H27B 108.6 . . ? C28 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C12 113.6(7) . . ? C30 C29 H29A 108.8 . . ? C12 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? C12 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C13 C31 C32 111.9(9) . . ? C13 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? C13 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C17 112.8(8) . . ? C34 C33 H33A 109.0 . . ? C17 C33 H33A 109.0 . . ? C34 C33 H33B 109.0 . . ? C17 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C18 111.9(7) . . ? C36 C35 H35A 109.2 . . ? C18 C35 H35A 109.2 . . ? C36 C35 H35B 109.2 . . ? C18 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C37 C37 C20 109.5(8) 2_457 . ? C37 C37 H37A 109.8 2_457 . ? C20 C37 H37A 109.8 . . ? C37 C37 H37B 109.8 2_457 . ? C20 C37 H37B 109.8 . . ? H37A C37 H37B 108.2 . . ? N3A Co2 N2A 89.0(3) . . ? N3A Co2 N4A 91.4(3) . . ? N2A Co2 N4A 177.8(3) . . ? N3A Co2 N1A 179.1(3) . . ? N2A Co2 N1A 90.7(3) . . ? N4A Co2 N1A 88.8(3) . . ? C4A N1A C1A 106.9(6) . . ? C4A N1A Co2 125.3(5) . . ? C1A N1A Co2 127.8(5) . . ? C6A N2A C9A 104.9(6) . . ? C6A N2A Co2 128.0(5) . . ? C9A N2A Co2 127.1(5) . . ? C11A N3A C14A 104.0(6) . . ? C11A N3A Co2 128.7(5) . . ? C14A N3A Co2 127.2(5) . . ? C16A N4A C19A 107.4(6) . . ? C16A N4A Co2 125.7(5) . . ? C19A N4A Co2 126.7(5) . . ? N1A C1A C20A 125.3(7) . . ? N1A C1A C2A 108.8(7) . . ? C20A C1A C2A 125.6(7) . . ? C3A C2A C1A 107.2(7) . . ? C3A C2A C21A 122.1(7) . . ? C1A C2A C21A 130.0(7) . . ? C2A C3A C4A 105.8(7) . . ? C2A C3A C23A 128.2(7) . . ? C4A C3A C23A 126.0(7) . . ? N1A C4A C5A 125.7(7) . . ? N1A C4A C3A 111.0(7) . . ? C5A C4A C3A 123.0(7) . . ? C6A C5A C4A 124.1(8) . . ? C6A C5A H5A 117.9 . . ? C4A C5A H5A 117.9 . . ? N2A C6A C5A 124.2(7) . . ? N2A C6A C7A 111.8(7) . . ? C5A C6A C7A 123.8(7) . . ? C8A C7A C6A 104.8(7) . . ? C8A C7A C25A 131.0(7) . . ? C6A C7A C25A 124.2(7) . . ? C7A C8A C9A 109.3(7) . . ? C7A C8A C27A 127.6(8) . . ? C9A C8A C27A 123.1(7) . . ? C10A C9A N2A 123.8(7) . . ? C10A C9A C8A 127.0(7) . . ? N2A C9A C8A 109.2(7) . . ? C9A C10A C11A 125.5(7) . . ? C9A C10A H10A 117.3 . . ? C11A C10A H10A 117.3 . . ? N3A C11A C10A 123.0(7) . . ? N3A C11A C12A 110.5(7) . . ? C10A C11A C12A 126.3(7) . . ? C13A C12A C11A 108.2(7) . . ? C13A C12A C29A 128.6(8) . . ? C11A C12A C29A 123.3(8) . . ? C12A C13A C14A 104.9(7) . . ? C12A C13A C31A 128.5(7) . . ? C14A C13A C31A 126.5(7) . . ? N3A C14A C15A 122.7(7) . . ? N3A C14A C13A 112.4(7) . . ? C15A C14A C13A 124.7(7) . . ? C16A C15A C14A 125.1(8) . . ? C16A C15A H15A 117.4 . . ? C14A C15A H15A 117.4 . . ? C15A C16A N4A 126.2(7) . . ? C15A C16A C17A 124.1(7) . . ? N4A C16A C17A 109.6(6) . . ? C18A C17A C16A 107.3(7) . . ? C18A C17A C33A 128.1(7) . . ? C16A C17A C33A 124.3(7) . . ? C17A C18A C19A 107.5(7) . . ? C17A C18A C35A 122.2(7) . . ? C19A C18A C35A 130.1(7) . . ? C20A C19A N4A 125.3(7) . . ? C20A C19A C18A 126.6(7) . . ? N4A C19A C18A 108.0(6) . . ? C19A C20A C1A 121.2(7) . . ? C19A C20A C37A 118.3(7) . . ? C1A C20A C37A 120.1(7) . . ? C2A C21A C22A 111.6(7) . . ? C2A C21A H21C 109.3 . . ? C22A C21A H21C 109.3 . . ? C2A C21A H21D 109.3 . . ? C22A C21A H21D 109.3 . . ? H21C C21A H21D 108.0 . . ? C21A C22A H22D 109.5 . . ? C21A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C21A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C3A C23A C24A 112.5(8) . . ? C3A C23A H23C 109.1 . . ? C24A C23A H23C 109.1 . . ? C3A C23A H23D 109.1 . . ? C24A C23A H23D 109.1 . . ? H23C C23A H23D 107.8 . . ? C23A C24A H24D 109.5 . . ? C23A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C7A C25A C26A 114.8(8) . . ? C7A C25A H25C 108.6 . . ? C26A C25A H25C 108.6 . . ? C7A C25A H25D 108.6 . . ? C26A C25A H25D 108.6 . . ? H25C C25A H25D 107.5 . . ? C25A C26A H26D 109.5 . . ? C25A C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C25A C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C8A C27A C28A 112.3(7) . . ? C8A C27A H27C 109.2 . . ? C28A C27A H27C 109.2 . . ? C8A C27A H27D 109.2 . . ? C28A C27A H27D 109.2 . . ? H27C C27A H27D 107.9 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C30A C29A C12A 114.7(8) . . ? C30A C29A H29C 108.6 . . ? C12A C29A H29C 108.6 . . ? C30A C29A H29D 108.6 . . ? C12A C29A H29D 108.6 . . ? H29C C29A H29D 107.6 . . ? C29A C30A H30D 109.5 . . ? C29A C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C29A C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C13A C31A C32A 111.7(8) . . ? C13A C31A H31C 109.3 . . ? C32A C31A H31C 109.3 . . ? C13A C31A H31D 109.3 . . ? C32A C31A H31D 109.3 . . ? H31C C31A H31D 107.9 . . ? C31A C32A H32D 109.5 . . ? C31A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C31A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C17A C33A C34A 113.1(7) . . ? C17A C33A H33C 109.0 . . ? C34A C33A H33C 109.0 . . ? C17A C33A H33D 109.0 . . ? C34A C33A H33D 109.0 . . ? H33C C33A H33D 107.8 . . ? C33A C34A H34D 109.5 . . ? C33A C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? C33A C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? C18A C35A C36A 111.0(7) . . ? C18A C35A H35C 109.4 . . ? C36A C35A H35C 109.4 . . ? C18A C35A H35D 109.4 . . ? C36A C35A H35D 109.4 . . ? H35C C35A H35D 108.0 . . ? C35A C36A H36D 109.5 . . ? C35A C36A H36E 109.5 . . ? H36D C36A H36E 109.5 . . ? C35A C36A H36F 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? C20A C37A C37A 112.9(7) . 2_566 ? C20A C37A H37C 109.0 . . ? C37A C37A H37C 109.0 2_566 . ? C20A C37A H37D 109.0 . . ? C37A C37A H37D 109.0 2_566 . ? H37C C37A H37D 107.8 . . ? C39 C38 C43 120.9(8) . . ? C39 C38 H38 119.6 . . ? C43 C38 H38 119.6 . . ? C38 C39 C40 120.9(9) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C44 C40 C41 121.3(8) . . ? C44 C40 C39 121.2(9) . . ? C41 C40 C39 117.5(9) . . ? C42 C41 C40 120.7(8) . . ? C42 C41 C47 120.5(8) . . ? C40 C41 C47 118.8(8) . . ? C43 C42 C41 118.6(8) . . ? C43 C42 C47 121.1(8) . 2_557 ? C41 C42 C47 120.3(7) . 2_557 ? C42 C43 C38 121.4(9) . . ? C42 C43 H43 119.3 . . ? C38 C43 H43 119.3 . . ? C45 C44 C40 119.3(9) . . ? C45 C44 H44 120.4 . . ? C40 C44 H44 120.4 . . ? C44 C45 C46 119.9(9) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C47 C46 C45 123.9(8) . . ? C47 C46 H46 118.1 . . ? C45 C46 H46 118.1 . . ? C46 C47 C41 116.8(8) . . ? C46 C47 C42 124.0(7) . 2_557 ? C41 C47 C42 119.1(7) . 2_557 ? C39A C38A C47A 118.8(8) . . ? C39A C38A C46A 122.8(7) . 2_666 ? C47A C38A C46A 118.5(7) . 2_666 ? C38A C39A C40A 121.6(8) . . ? C38A C39A H39A 119.2 . . ? C40A C39A H39A 119.2 . . ? C41A C40A C39A 121.1(8) . . ? C41A C40A H40A 119.4 . . ? C39A C40A H40A 119.4 . . ? C40A C41A C42A 120.1(8) . . ? C40A C41A H41A 120.0 . . ? C42A C41A H41A 120.0 . . ? C43A C42A C41A 121.0(8) . . ? C43A C42A C47A 118.7(8) . . ? C41A C42A C47A 120.3(8) . . ? C44A C43A C42A 120.7(8) . . ? C44A C43A H43A 119.6 . . ? C42A C43A H43A 119.6 . . ? C43A C44A C45A 121.0(8) . . ? C43A C44A H44A 119.5 . . ? C45A C44A H44A 119.5 . . ? C46A C45A C44A 120.7(8) . . ? C46A C45A H45A 119.7 . . ? C44A C45A H45A 119.7 . . ? C45A C46A C47A 117.8(8) . . ? C45A C46A C38A 121.5(7) . 2_666 ? C47A C46A C38A 120.7(7) . 2_666 ? C42A C47A C46A 121.0(7) . . ? C42A C47A C38A 118.1(7) . . ? C46A C47A C38A 120.9(7) . . ? Cl1 C48 Cl2 111.7(6) . . ? Cl1 C48 Cl3 109.7(5) . . ? Cl2 C48 Cl3 110.8(5) . . ? Cl1 C48 H48 108.1 . . ? Cl2 C48 H48 108.1 . . ? Cl3 C48 H48 108.1 . . ? Cl6 C49 Cl5 111.1(5) . . ? Cl6 C49 Cl4 111.0(5) . . ? Cl5 C49 Cl4 109.2(5) . . ? Cl6 C49 H49 108.5 . . ? Cl5 C49 H49 108.5 . . ? Cl4 C49 H49 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Co1 N1 C1 95(6) . . . . ? N2 Co1 N1 C1 -164.6(7) . . . . ? N4 Co1 N1 C1 15.2(7) . . . . ? N3 Co1 N1 C4 -86(6) . . . . ? N2 Co1 N1 C4 14.2(6) . . . . ? N4 Co1 N1 C4 -166.0(6) . . . . ? N3 Co1 N2 C6 168.5(7) . . . . ? N1 Co1 N2 C6 -8.9(7) . . . . ? N4 Co1 N2 C6 -96(100) . . . . ? N3 Co1 N2 C9 -13.3(7) . . . . ? N1 Co1 N2 C9 169.3(7) . . . . ? N4 Co1 N2 C9 82(100) . . . . ? N2 Co1 N3 C11 14.3(6) . . . . ? N1 Co1 N3 C11 114(6) . . . . ? N4 Co1 N3 C11 -165.5(6) . . . . ? N2 Co1 N3 C14 -169.1(7) . . . . ? N1 Co1 N3 C14 -69(6) . . . . ? N4 Co1 N3 C14 11.1(7) . . . . ? N3 Co1 N4 C16 -11.2(6) . . . . ? N2 Co1 N4 C16 -107(100) . . . . ? N1 Co1 N4 C16 166.2(6) . . . . ? N3 Co1 N4 C19 165.4(6) . . . . ? N2 Co1 N4 C19 70(100) . . . . ? N1 Co1 N4 C19 -17.3(6) . . . . ? C4 N1 C1 C20 180.0(7) . . . . ? Co1 N1 C1 C20 -1.0(11) . . . . ? C4 N1 C1 C2 2.5(9) . . . . ? Co1 N1 C1 C2 -178.5(5) . . . . ? N1 C1 C2 C3 -0.5(10) . . . . ? C20 C1 C2 C3 -177.8(8) . . . . ? N1 C1 C2 C21 171.0(8) . . . . ? C20 C1 C2 C21 -6.4(15) . . . . ? C1 C2 C3 C4 -1.7(10) . . . . ? C21 C2 C3 C4 -173.9(8) . . . . ? C1 C2 C3 C23 179.1(9) . . . . ? C21 C2 C3 C23 6.9(15) . . . . ? C1 N1 C4 C5 167.0(7) . . . . ? Co1 N1 C4 C5 -12.1(11) . . . . ? C1 N1 C4 C3 -3.6(9) . . . . ? Co1 N1 C4 C3 177.4(5) . . . . ? C2 C3 C4 N1 3.3(10) . . . . ? C23 C3 C4 N1 -177.4(8) . . . . ? C2 C3 C4 C5 -167.1(8) . . . . ? C23 C3 C4 C5 12.1(13) . . . . ? N1 C4 C5 C6 -1.2(13) . . . . ? C3 C4 C5 C6 168.0(8) . . . . ? C4 C5 C6 N2 7.5(14) . . . . ? C4 C5 C6 C7 -170.9(8) . . . . ? C9 N2 C6 C5 -178.4(8) . . . . ? Co1 N2 C6 C5 0.1(12) . . . . ? C9 N2 C6 C7 0.3(8) . . . . ? Co1 N2 C6 C7 178.8(5) . . . . ? C5 C6 C7 C8 176.6(8) . . . . ? N2 C6 C7 C8 -2.0(9) . . . . ? C5 C6 C7 C25 2.2(13) . . . . ? N2 C6 C7 C25 -176.5(7) . . . . ? C6 C7 C8 C9 2.8(9) . . . . ? C25 C7 C8 C9 176.9(8) . . . . ? C6 C7 C8 C27 179.4(8) . . . . ? C25 C7 C8 C27 -6.6(15) . . . . ? C6 N2 C9 C10 -175.7(7) . . . . ? Co1 N2 C9 C10 5.9(11) . . . . ? C6 N2 C9 C8 1.6(9) . . . . ? Co1 N2 C9 C8 -176.9(5) . . . . ? C7 C8 C9 C10 174.3(8) . . . . ? C27 C8 C9 C10 -2.3(13) . . . . ? C7 C8 C9 N2 -2.9(9) . . . . ? C27 C8 C9 N2 -179.5(8) . . . . ? N2 C9 C10 C11 6.8(13) . . . . ? C8 C9 C10 C11 -170.0(8) . . . . ? C14 N3 C11 C10 175.1(8) . . . . ? Co1 N3 C11 C10 -7.7(11) . . . . ? C14 N3 C11 C12 1.4(9) . . . . ? Co1 N3 C11 C12 178.5(5) . . . . ? C9 C10 C11 N3 -5.9(13) . . . . ? C9 C10 C11 C12 167.0(8) . . . . ? N3 C11 C12 C13 0.1(9) . . . . ? C10 C11 C12 C13 -173.7(8) . . . . ? N3 C11 C12 C29 179.3(7) . . . . ? C10 C11 C12 C29 5.5(12) . . . . ? C11 C12 C13 C14 -1.4(9) . . . . ? C29 C12 C13 C14 179.4(8) . . . . ? C11 C12 C13 C31 179.7(9) . . . . ? C29 C12 C13 C31 0.5(15) . . . . ? C11 N3 C14 C15 172.8(8) . . . . ? Co1 N3 C14 C15 -4.4(13) . . . . ? C11 N3 C14 C13 -2.2(9) . . . . ? Co1 N3 C14 C13 -179.4(5) . . . . ? C12 C13 C14 C15 -172.8(9) . . . . ? C31 C13 C14 C15 6.3(14) . . . . ? C12 C13 C14 N3 2.3(10) . . . . ? C31 C13 C14 N3 -178.7(8) . . . . ? N3 C14 C15 C16 -7.4(14) . . . . ? C13 C14 C15 C16 166.9(8) . . . . ? C14 C15 C16 N4 7.3(13) . . . . ? C14 C15 C16 C17 -164.0(9) . . . . ? C19 N4 C16 C15 -172.7(8) . . . . ? Co1 N4 C16 C15 4.5(11) . . . . ? C19 N4 C16 C17 -0.5(8) . . . . ? Co1 N4 C16 C17 176.7(5) . . . . ? C15 C16 C17 C18 171.5(8) . . . . ? N4 C16 C17 C18 -0.9(9) . . . . ? C15 C16 C17 C33 -10.5(13) . . . . ? N4 C16 C17 C33 177.1(8) . . . . ? C16 C17 C18 C19 1.8(9) . . . . ? C33 C17 C18 C19 -176.2(8) . . . . ? C16 C17 C18 C35 171.9(7) . . . . ? C33 C17 C18 C35 -6.1(14) . . . . ? C16 N4 C19 C20 -177.5(7) . . . . ? Co1 N4 C19 C20 5.3(10) . . . . ? C16 N4 C19 C18 1.5(8) . . . . ? Co1 N4 C19 C18 -175.7(5) . . . . ? C17 C18 C19 C20 176.8(8) . . . . ? C35 C18 C19 C20 7.6(14) . . . . ? C17 C18 C19 N4 -2.1(9) . . . . ? C35 C18 C19 N4 -171.3(8) . . . . ? N4 C19 C20 C1 16.8(12) . . . . ? C18 C19 C20 C1 -162.0(8) . . . . ? N4 C19 C20 C37 -159.7(7) . . . . ? C18 C19 C20 C37 21.5(12) . . . . ? N1 C1 C20 C19 -19.3(13) . . . . ? C2 C1 C20 C19 157.7(8) . . . . ? N1 C1 C20 C37 157.3(7) . . . . ? C2 C1 C20 C37 -25.7(12) . . . . ? C3 C2 C21 C22 100.3(10) . . . . ? C1 C2 C21 C22 -70.1(11) . . . . ? C2 C3 C23 C24 85.2(12) . . . . ? C4 C3 C23 C24 -93.9(11) . . . . ? C8 C7 C25 C26 -94.0(11) . . . . ? C6 C7 C25 C26 79.0(11) . . . . ? C7 C8 C27 C28 -102.7(11) . . . . ? C9 C8 C27 C28 73.2(11) . . . . ? C13 C12 C29 C30 97.1(10) . . . . ? C11 C12 C29 C30 -82.0(10) . . . . ? C12 C13 C31 C32 -100.5(12) . . . . ? C14 C13 C31 C32 80.7(11) . . . . ? C18 C17 C33 C34 100.2(11) . . . . ? C16 C17 C33 C34 -77.4(11) . . . . ? C17 C18 C35 C36 -106.6(9) . . . . ? C19 C18 C35 C36 61.3(11) . . . . ? C19 C20 C37 C37 114.6(9) . . . 2_457 ? C1 C20 C37 C37 -62.1(11) . . . 2_457 ? N3A Co2 N1A C4A -56(17) . . . . ? N2A Co2 N1A C4A 13.8(6) . . . . ? N4A Co2 N1A C4A -164.0(6) . . . . ? N3A Co2 N1A C1A 126(16) . . . . ? N2A Co2 N1A C1A -163.9(7) . . . . ? N4A Co2 N1A C1A 18.3(7) . . . . ? N3A Co2 N2A C6A 168.0(7) . . . . ? N4A Co2 N2A C6A 66(7) . . . . ? N1A Co2 N2A C6A -11.2(7) . . . . ? N3A Co2 N2A C9A -14.6(7) . . . . ? N4A Co2 N2A C9A -116(7) . . . . ? N1A Co2 N2A C9A 166.3(7) . . . . ? N2A Co2 N3A C11A 16.3(7) . . . . ? N4A Co2 N3A C11A -165.9(7) . . . . ? N1A Co2 N3A C11A 87(17) . . . . ? N2A Co2 N3A C14A -167.2(7) . . . . ? N4A Co2 N3A C14A 10.6(7) . . . . ? N1A Co2 N3A C14A -97(17) . . . . ? N3A Co2 N4A C16A -10.2(7) . . . . ? N2A Co2 N4A C16A 91(7) . . . . ? N1A Co2 N4A C16A 168.9(7) . . . . ? N3A Co2 N4A C19A 163.0(6) . . . . ? N2A Co2 N4A C19A -96(7) . . . . ? N1A Co2 N4A C19A -17.9(6) . . . . ? C4A N1A C1A C20A 176.4(8) . . . . ? Co2 N1A C1A C20A -5.6(12) . . . . ? C4A N1A C1A C2A 2.4(8) . . . . ? Co2 N1A C1A C2A -179.5(5) . . . . ? N1A C1A C2A C3A 1.2(9) . . . . ? C20A C1A C2A C3A -172.8(8) . . . . ? N1A C1A C2A C21A 171.8(8) . . . . ? C20A C1A C2A C21A -2.2(14) . . . . ? C1A C2A C3A C4A -4.0(9) . . . . ? C21A C2A C3A C4A -175.5(8) . . . . ? C1A C2A C3A C23A 177.6(8) . . . . ? C21A C2A C3A C23A 6.1(14) . . . . ? C1A N1A C4A C5A 169.5(8) . . . . ? Co2 N1A C4A C5A -8.6(11) . . . . ? C1A N1A C4A C3A -5.0(9) . . . . ? Co2 N1A C4A C3A 176.9(5) . . . . ? C2A C3A C4A N1A 5.8(9) . . . . ? C23A C3A C4A N1A -175.8(8) . . . . ? C2A C3A C4A C5A -169.0(8) . . . . ? C23A C3A C4A C5A 9.5(13) . . . . ? N1A C4A C5A C6A -5.5(14) . . . . ? C3A C4A C5A C6A 168.4(8) . . . . ? C9A N2A C6A C5A -175.6(8) . . . . ? Co2 N2A C6A C5A 2.2(13) . . . . ? C9A N2A C6A C7A 0.4(9) . . . . ? Co2 N2A C6A C7A 178.2(5) . . . . ? C4A C5A C6A N2A 8.9(14) . . . . ? C4A C5A C6A C7A -166.6(8) . . . . ? N2A C6A C7A C8A -1.0(10) . . . . ? C5A C6A C7A C8A 175.0(8) . . . . ? N2A C6A C7A C25A 178.9(8) . . . . ? C5A C6A C7A C25A -5.1(14) . . . . ? C6A C7A C8A C9A 1.2(10) . . . . ? C25A C7A C8A C9A -178.7(9) . . . . ? C6A C7A C8A C27A -179.1(8) . . . . ? C25A C7A C8A C27A 0.9(16) . . . . ? C6A N2A C9A C10A -176.6(8) . . . . ? Co2 N2A C9A C10A 5.5(12) . . . . ? C6A N2A C9A C8A 0.4(9) . . . . ? Co2 N2A C9A C8A -177.5(5) . . . . ? C7A C8A C9A C10A 175.8(8) . . . . ? C27A C8A C9A C10A -3.9(14) . . . . ? C7A C8A C9A N2A -1.1(10) . . . . ? C27A C8A C9A N2A 179.2(7) . . . . ? N2A C9A C10A C11A 9.5(14) . . . . ? C8A C9A C10A C11A -166.9(8) . . . . ? C14A N3A C11A C10A 174.4(8) . . . . ? Co2 N3A C11A C10A -8.4(12) . . . . ? C14A N3A C11A C12A -0.5(9) . . . . ? Co2 N3A C11A C12A 176.7(6) . . . . ? C9A C10A C11A N3A -8.1(13) . . . . ? C9A C10A C11A C12A 166.0(8) . . . . ? N3A C11A C12A C13A 2.0(10) . . . . ? C10A C11A C12A C13A -172.8(8) . . . . ? N3A C11A C12A C29A -177.9(8) . . . . ? C10A C11A C12A C29A 7.4(14) . . . . ? C11A C12A C13A C14A -2.4(10) . . . . ? C29A C12A C13A C14A 177.4(9) . . . . ? C11A C12A C13A C31A -178.5(9) . . . . ? C29A C12A C13A C31A 1.3(16) . . . . ? C11A N3A C14A C15A 173.9(8) . . . . ? Co2 N3A C14A C15A -3.3(12) . . . . ? C11A N3A C14A C13A -1.1(9) . . . . ? Co2 N3A C14A C13A -178.3(6) . . . . ? C12A C13A C14A N3A 2.3(10) . . . . ? C31A C13A C14A N3A 178.4(8) . . . . ? C12A C13A C14A C15A -172.6(8) . . . . ? C31A C13A C14A C15A 3.6(15) . . . . ? N3A C14A C15A C16A -9.4(14) . . . . ? C13A C14A C15A C16A 165.0(9) . . . . ? C14A C15A C16A N4A 9.9(14) . . . . ? C14A C15A C16A C17A -166.7(8) . . . . ? C19A N4A C16A C15A -171.9(8) . . . . ? Co2 N4A C16A C15A 2.4(12) . . . . ? C19A N4A C16A C17A 5.1(9) . . . . ? Co2 N4A C16A C17A 179.4(5) . . . . ? C15A C16A C17A C18A 172.6(8) . . . . ? N4A C16A C17A C18A -4.5(10) . . . . ? C15A C16A C17A C33A -1.9(14) . . . . ? N4A C16A C17A C33A -179.0(8) . . . . ? C16A C17A C18A C19A 1.9(9) . . . . ? C33A C17A C18A C19A 176.1(8) . . . . ? C16A C17A C18A C35A 176.5(8) . . . . ? C33A C17A C18A C35A -9.3(15) . . . . ? C16A N4A C19A C20A 179.4(8) . . . . ? Co2 N4A C19A C20A 5.2(11) . . . . ? C16A N4A C19A C18A -3.9(8) . . . . ? Co2 N4A C19A C18A -178.1(5) . . . . ? C17A C18A C19A C20A 177.7(8) . . . . ? C35A C18A C19A C20A 3.8(14) . . . . ? C17A C18A C19A N4A 1.1(9) . . . . ? C35A C18A C19A N4A -172.9(8) . . . . ? N4A C19A C20A C1A 15.4(12) . . . . ? C18A C19A C20A C1A -160.7(8) . . . . ? N4A C19A C20A C37A -156.7(7) . . . . ? C18A C19A C20A C37A 27.2(11) . . . . ? N1A C1A C20A C19A -15.3(12) . . . . ? C2A C1A C20A C19A 157.7(8) . . . . ? N1A C1A C20A C37A 156.7(7) . . . . ? C2A C1A C20A C37A -30.4(12) . . . . ? C3A C2A C21A C22A 105.6(9) . . . . ? C1A C2A C21A C22A -63.8(12) . . . . ? C2A C3A C23A C24A 78.9(11) . . . . ? C4A C3A C23A C24A -99.2(10) . . . . ? C8A C7A C25A C26A 94.1(12) . . . . ? C6A C7A C25A C26A -85.8(11) . . . . ? C7A C8A C27A C28A -99.4(11) . . . . ? C9A C8A C27A C28A 80.2(11) . . . . ? C13A C12A C29A C30A 99.9(12) . . . . ? C11A C12A C29A C30A -80.3(11) . . . . ? C12A C13A C31A C32A 86.8(12) . . . . ? C14A C13A C31A C32A -88.4(11) . . . . ? C18A C17A C33A C34A -79.6(12) . . . . ? C16A C17A C33A C34A 93.8(10) . . . . ? C17A C18A C35A C36A -102.8(10) . . . . ? C19A C18A C35A C36A 70.4(11) . . . . ? C19A C20A C37A C37A 62.6(11) . . . 2_566 ? C1A C20A C37A C37A -109.6(10) . . . 2_566 ? C43 C38 C39 C40 0.8(14) . . . . ? C38 C39 C40 C44 178.7(8) . . . . ? C38 C39 C40 C41 -1.2(13) . . . . ? C44 C40 C41 C42 -178.6(8) . . . . ? C39 C40 C41 C42 1.3(12) . . . . ? C44 C40 C41 C47 -0.8(12) . . . . ? C39 C40 C41 C47 179.1(7) . . . . ? C40 C41 C42 C43 -1.1(12) . . . . ? C47 C41 C42 C43 -178.9(7) . . . . ? C40 C41 C42 C47 -178.3(7) . . . 2_557 ? C47 C41 C42 C47 3.9(13) . . . 2_557 ? C41 C42 C43 C38 0.7(12) . . . . ? C47 C42 C43 C38 177.9(8) 2_557 . . . ? C39 C38 C43 C42 -0.6(14) . . . . ? C41 C40 C44 C45 -0.5(13) . . . . ? C39 C40 C44 C45 179.6(9) . . . . ? C40 C44 C45 C46 1.5(14) . . . . ? C44 C45 C46 C47 -1.2(15) . . . . ? C45 C46 C47 C41 -0.1(13) . . . . ? C45 C46 C47 C42 -177.2(9) . . . 2_557 ? C42 C41 C47 C46 178.8(7) . . . . ? C40 C41 C47 C46 1.0(12) . . . . ? C42 C41 C47 C42 -3.9(13) . . . 2_557 ? C40 C41 C47 C42 178.3(7) . . . 2_557 ? C47A C38A C39A C40A 2.3(13) . . . . ? C46A C38A C39A C40A -178.6(8) 2_666 . . . ? C38A C39A C40A C41A -0.8(14) . . . . ? C39A C40A C41A C42A -0.7(14) . . . . ? C40A C41A C42A C43A -177.2(8) . . . . ? C40A C41A C42A C47A 0.5(13) . . . . ? C41A C42A C43A C44A 179.5(9) . . . . ? C47A C42A C43A C44A 1.8(13) . . . . ? C42A C43A C44A C45A -1.2(14) . . . . ? C43A C44A C45A C46A 1.3(14) . . . . ? C44A C45A C46A C47A -2.0(13) . . . . ? C44A C45A C46A C38A 179.0(8) . . . 2_666 ? C43A C42A C47A C46A -2.5(12) . . . . ? C41A C42A C47A C46A 179.7(8) . . . . ? C43A C42A C47A C38A 178.8(8) . . . . ? C41A C42A C47A C38A 1.0(12) . . . . ? C45A C46A C47A C42A 2.6(12) . . . . ? C38A C46A C47A C42A -178.4(8) 2_666 . . . ? C45A C46A C47A C38A -178.7(8) . . . . ? C38A C46A C47A C38A 0.2(13) 2_666 . . . ? C39A C38A C47A C42A -2.4(12) . . . . ? C46A C38A C47A C42A 178.5(7) 2_666 . . . ? C39A C38A C47A C46A 178.9(8) . . . . ? C46A C38A C47A C46A -0.2(13) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.942 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 958598' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_16julcm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H122 Co2 N8 O4' _chemical_formula_weight 1497.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9193(12) _cell_length_b 12.4194(13) _cell_length_c 14.3773(15) _cell_angle_alpha 88.565(2) _cell_angle_beta 66.974(2) _cell_angle_gamma 83.038(2) _cell_volume 1943.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9552 _exptl_absorpt_correction_T_max 0.9715 _exptl_absorpt_process_details 'SADABS 2.05 (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10444 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_unetI/netI 0.0527 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7086 _reflns_number_gt 5938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0779P)^2^+0.9080P] 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 7086 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 1.12128(3) 1.12288(3) 1.36359(2) 0.01836(13) Uani 1 1 d . . . O1 O 1.27023(18) 1.22451(17) 1.33591(14) 0.0354(5) Uani 1 1 d . . . N1 N 1.02969(18) 1.23927(16) 1.31788(15) 0.0187(4) Uani 1 1 d . . . N2 N 1.19898(18) 1.05774(16) 1.22633(15) 0.0201(4) Uani 1 1 d . . . N3 N 1.20565(18) 1.00146(16) 1.41099(15) 0.0194(4) Uani 1 1 d . . . N4 N 1.03627(18) 1.18349(16) 1.50130(15) 0.0179(4) Uani 1 1 d . . . C1 C 0.9700(2) 1.33749(19) 1.36639(18) 0.0184(5) Uani 1 1 d . . . C2 C 0.9156(2) 1.4013(2) 1.30413(19) 0.0213(5) Uani 1 1 d . . . C3 C 0.9443(2) 1.3403(2) 1.21898(19) 0.0229(5) Uani 1 1 d . . . C4 C 1.0176(2) 1.2429(2) 1.22622(18) 0.0213(5) Uani 1 1 d . . . C5 C 1.0808(2) 1.1689(2) 1.14634(19) 0.0250(6) Uani 1 1 d . . . H5A H 1.0605 1.1758 1.0887 0.030 Uiso 1 1 calc R . . C6 C 1.1704(2) 1.0865(2) 1.14413(18) 0.0231(5) Uani 1 1 d . . . C7 C 1.2527(3) 1.0239(2) 1.05492(19) 0.0278(6) Uani 1 1 d . . . C8 C 1.3330(2) 0.9584(2) 1.08293(19) 0.0245(6) Uani 1 1 d . . . C9 C 1.2972(2) 0.9779(2) 1.19028(18) 0.0226(5) Uani 1 1 d . . . C10 C 1.3491(2) 0.9195(2) 1.24949(19) 0.0234(5) Uani 1 1 d . . . H10A H 1.4215 0.8710 1.2163 0.028 Uiso 1 1 calc R . . C11 C 1.3027(2) 0.9269(2) 1.35393(19) 0.0220(5) Uani 1 1 d . . . C12 C 1.3435(2) 0.8546(2) 1.41777(19) 0.0216(5) Uani 1 1 d . . . C13 C 1.2677(2) 0.8840(2) 1.51524(19) 0.0220(5) Uani 1 1 d . . . C14 C 1.1833(2) 0.97511(19) 1.50942(18) 0.0203(5) Uani 1 1 d . . . C15 C 1.0979(2) 1.0336(2) 1.59236(18) 0.0218(5) Uani 1 1 d . . . H15A H 1.0819 1.0034 1.6570 0.026 Uiso 1 1 calc R . . C16 C 1.0335(2) 1.1337(2) 1.58836(18) 0.0187(5) Uani 1 1 d . . . C17 C 0.9686(2) 1.2044(2) 1.67528(18) 0.0191(5) Uani 1 1 d . . . C18 C 0.9360(2) 1.3013(2) 1.64061(18) 0.0191(5) Uani 1 1 d . . . C19 C 0.9782(2) 1.28748(19) 1.53056(18) 0.0177(5) Uani 1 1 d . . . C20 C 0.9603(2) 1.36542(19) 1.46414(17) 0.0178(5) Uani 1 1 d . . . C21 C 0.8287(2) 1.5054(2) 1.3284(2) 0.0257(6) Uani 1 1 d . . . H21A H 0.8134 1.5279 1.2674 0.031 Uiso 1 1 calc R . . H21B H 0.8683 1.5631 1.3457 0.031 Uiso 1 1 calc R . . C22 C 0.7056(3) 1.4956(2) 1.4158(2) 0.0323(6) Uani 1 1 d . . . H22A H 0.6543 1.5659 1.4290 0.048 Uiso 1 1 calc R . . H22B H 0.7199 1.4733 1.4766 0.048 Uiso 1 1 calc R . . H22C H 0.6638 1.4412 1.3980 0.048 Uiso 1 1 calc R . . C23 C 0.9025(3) 1.3658(2) 1.13337(19) 0.0287(6) Uani 1 1 d . . . H23A H 0.9606 1.3251 1.0717 0.034 Uiso 1 1 calc R . . H23B H 0.9038 1.4442 1.1193 0.034 Uiso 1 1 calc R . . C24 C 0.7733(3) 1.3364(3) 1.1579(2) 0.0419(8) Uani 1 1 d . . . H24A H 0.7518 1.3497 1.0991 0.063 Uiso 1 1 calc R . . H24B H 0.7144 1.3811 1.2155 0.063 Uiso 1 1 calc R . . H24C H 0.7707 1.2596 1.1749 0.063 Uiso 1 1 calc R . . C25 C 1.2458(3) 1.0317(2) 0.9527(2) 0.0361(7) Uani 1 1 d . . . H25A H 1.2117 1.1064 0.9445 0.043 Uiso 1 1 calc R . . H25B H 1.3298 1.0176 0.8998 0.043 Uiso 1 1 calc R . . C26 C 1.1678(5) 0.9531(4) 0.9384(3) 0.0747(14) Uani 1 1 d . . . H26A H 1.1564 0.9681 0.8753 0.112 Uiso 1 1 calc R . . H26B H 1.0877 0.9607 0.9953 0.112 Uiso 1 1 calc R . . H26C H 1.2083 0.8790 0.9354 0.112 Uiso 1 1 calc R . . C27 C 1.4366(2) 0.8763(2) 1.0192(2) 0.0297(6) Uani 1 1 d . . . H27A H 1.5054 0.8750 1.0416 0.036 Uiso 1 1 calc R . . H27B H 1.4663 0.8991 0.9479 0.036 Uiso 1 1 calc R . . C28 C 1.4000(3) 0.7625(2) 1.0247(2) 0.0319(6) Uani 1 1 d . . . H28A H 1.4720 0.7119 0.9852 0.048 Uiso 1 1 calc R . . H28B H 1.3367 0.7618 0.9972 0.048 Uiso 1 1 calc R . . H28C H 1.3676 0.7404 1.0954 0.048 Uiso 1 1 calc R . . C29 C 1.4509(2) 0.7669(2) 1.3819(2) 0.0257(6) Uani 1 1 d . . . H29A H 1.4495 0.7278 1.3233 0.031 Uiso 1 1 calc R . . H29B H 1.4413 0.7142 1.4365 0.031 Uiso 1 1 calc R . . C30 C 1.5752(3) 0.8087(2) 1.3515(2) 0.0372(7) Uani 1 1 d . . . H30A H 1.6404 0.7473 1.3311 0.056 Uiso 1 1 calc R . . H30B H 1.5773 0.8479 1.4090 0.056 Uiso 1 1 calc R . . H30C H 1.5877 0.8578 1.2948 0.056 Uiso 1 1 calc R . . C31 C 1.2746(2) 0.8404(2) 1.61070(19) 0.0254(6) Uani 1 1 d . . . H31A H 1.3170 0.7653 1.5979 0.030 Uiso 1 1 calc R . . H31B H 1.1904 0.8378 1.6620 0.030 Uiso 1 1 calc R . . C32 C 1.3433(3) 0.9102(2) 1.6519(2) 0.0318(6) Uani 1 1 d . . . H32A H 1.3502 0.8769 1.7123 0.048 Uiso 1 1 calc R . . H32B H 1.2981 0.9830 1.6695 0.048 Uiso 1 1 calc R . . H32C H 1.4256 0.9152 1.6002 0.048 Uiso 1 1 calc R . . C33 C 0.9479(2) 1.1755(2) 1.78210(18) 0.0229(5) Uani 1 1 d . . . H33A H 0.9489 1.0959 1.7886 0.028 Uiso 1 1 calc R . . H33B H 0.8656 1.2096 1.8277 0.028 Uiso 1 1 calc R . . C34 C 1.0450(3) 1.2122(2) 1.8156(2) 0.0344(7) Uani 1 1 d . . . H34A H 1.0266 1.1923 1.8860 0.052 Uiso 1 1 calc R . . H34B H 1.0440 1.2911 1.8099 0.052 Uiso 1 1 calc R . . H34C H 1.1263 1.1766 1.7724 0.052 Uiso 1 1 calc R . . C35 C 0.8534(2) 1.3932(2) 1.70987(18) 0.0218(5) Uani 1 1 d . . . H35A H 0.8850 1.4628 1.6842 0.026 Uiso 1 1 calc R . . H35B H 0.8542 1.3834 1.7782 0.026 Uiso 1 1 calc R . . C36 C 0.7218(2) 1.3972(2) 1.7166(2) 0.0275(6) Uani 1 1 d . . . H36A H 0.6696 1.4557 1.7638 0.041 Uiso 1 1 calc R . . H36B H 0.6910 1.3278 1.7408 0.041 Uiso 1 1 calc R . . H36C H 0.7204 1.4107 1.6496 0.041 Uiso 1 1 calc R . . C37 C 0.9425(2) 1.48444(19) 1.49368(18) 0.0188(5) Uani 1 1 d . . . H37A H 0.8700 1.4992 1.5580 0.023 Uiso 1 1 calc R . . H37B H 0.9273 1.5292 1.4409 0.023 Uiso 1 1 calc R . . C38 C 1.3276(2) 1.2796(2) 1.2441(2) 0.0291(6) Uani 1 1 d . . . H38A H 1.2777 1.3491 1.2432 0.035 Uiso 1 1 calc R . . H38B H 1.3382 1.2343 1.1849 0.035 Uiso 1 1 calc R . . C39 C 1.4517(2) 1.2996(2) 1.2429(2) 0.0326(6) Uani 1 1 d . . . H39A H 1.5142 1.2361 1.2143 0.039 Uiso 1 1 calc R . . H39B H 1.4809 1.3646 1.2039 0.039 Uiso 1 1 calc R . . C40 C 1.4220(3) 1.3170(2) 1.3547(2) 0.0336(7) Uani 1 1 d . . . H40A H 1.3886 1.3933 1.3764 0.040 Uiso 1 1 calc R . . H40B H 1.4957 1.2975 1.3703 0.040 Uiso 1 1 calc R . . C41 C 1.3254(3) 1.2404(3) 1.4052(2) 0.0344(7) Uani 1 1 d . . . H41A H 1.3643 1.1704 1.4194 0.041 Uiso 1 1 calc R . . H41B H 1.2631 1.2729 1.4696 0.041 Uiso 1 1 calc R . . O1S O 0.5875(2) 1.52773(19) 1.07871(16) 0.0435(5) Uani 1 1 d . . . C1S C 0.6265(3) 1.6093(3) 1.1240(3) 0.0479(8) Uani 1 1 d . . . H1SA H 0.6478 1.5786 1.1800 0.057 Uiso 1 1 calc R . . H1SB H 0.5600 1.6701 1.1514 0.057 Uiso 1 1 calc R . . C2S C 0.7374(4) 1.6484(3) 1.0426(3) 0.0647(11) Uani 1 1 d . . . H2SA H 0.7152 1.7195 1.0175 0.078 Uiso 1 1 calc R . . H2SB H 0.8020 1.6558 1.0684 0.078 Uiso 1 1 calc R . . C3S C 0.7806(4) 1.5624(3) 0.9602(3) 0.0574(10) Uani 1 1 d . . . H3SA H 0.8178 1.5938 0.8925 0.069 Uiso 1 1 calc R . . H3SB H 0.8409 1.5054 0.9694 0.069 Uiso 1 1 calc R . . C4S C 0.6646(3) 1.5192(3) 0.9741(2) 0.0366(7) Uani 1 1 d . . . H4SA H 0.6237 1.5614 0.9344 0.044 Uiso 1 1 calc R . . H4SB H 0.6818 1.4424 0.9506 0.044 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 0.0227(2) 0.0152(2) 0.01744(19) -0.00010(13) -0.00820(14) -0.00188(13) O1 0.0421(12) 0.0473(13) 0.0272(10) 0.0144(9) -0.0198(9) -0.0257(10) N1 0.0226(10) 0.0157(10) 0.0187(10) 0.0004(8) -0.0083(8) -0.0051(8) N2 0.0241(11) 0.0155(11) 0.0206(10) -0.0002(8) -0.0084(8) -0.0027(8) N3 0.0223(10) 0.0147(10) 0.0208(10) -0.0010(8) -0.0080(8) -0.0014(8) N4 0.0198(10) 0.0140(10) 0.0203(10) 0.0011(8) -0.0084(8) -0.0022(8) C1 0.0184(12) 0.0146(12) 0.0222(12) 0.0030(10) -0.0073(10) -0.0052(9) C2 0.0235(13) 0.0194(13) 0.0242(13) 0.0056(10) -0.0118(10) -0.0068(10) C3 0.0288(14) 0.0220(13) 0.0221(13) 0.0034(10) -0.0140(11) -0.0053(11) C4 0.0267(13) 0.0212(13) 0.0173(12) 0.0033(10) -0.0096(10) -0.0052(10) C5 0.0336(14) 0.0245(14) 0.0194(12) 0.0012(10) -0.0122(11) -0.0073(11) C6 0.0306(14) 0.0188(13) 0.0196(12) -0.0006(10) -0.0084(10) -0.0066(11) C7 0.0360(15) 0.0243(14) 0.0203(13) -0.0004(11) -0.0070(11) -0.0069(12) C8 0.0291(14) 0.0223(14) 0.0189(12) -0.0010(10) -0.0046(10) -0.0073(11) C9 0.0247(13) 0.0186(13) 0.0224(13) -0.0020(10) -0.0057(10) -0.0056(10) C10 0.0225(13) 0.0200(13) 0.0249(13) -0.0031(10) -0.0070(10) 0.0008(10) C11 0.0210(12) 0.0176(13) 0.0269(13) -0.0004(10) -0.0083(10) -0.0036(10) C12 0.0236(13) 0.0146(12) 0.0281(13) 0.0003(10) -0.0114(10) -0.0032(10) C13 0.0247(13) 0.0163(12) 0.0281(13) 0.0017(10) -0.0133(11) -0.0037(10) C14 0.0227(12) 0.0148(12) 0.0237(12) 0.0013(10) -0.0094(10) -0.0024(10) C15 0.0246(13) 0.0218(13) 0.0201(12) 0.0047(10) -0.0097(10) -0.0046(10) C16 0.0176(12) 0.0182(12) 0.0217(12) 0.0000(10) -0.0089(10) -0.0032(9) C17 0.0194(12) 0.0184(12) 0.0198(12) 0.0018(10) -0.0072(9) -0.0049(10) C18 0.0205(12) 0.0181(12) 0.0193(12) -0.0003(10) -0.0086(10) -0.0022(10) C19 0.0177(12) 0.0159(12) 0.0203(12) -0.0006(9) -0.0079(9) -0.0033(9) C20 0.0177(12) 0.0165(12) 0.0197(12) -0.0001(9) -0.0077(9) -0.0029(9) C21 0.0361(15) 0.0191(13) 0.0292(14) 0.0026(11) -0.0214(12) -0.0007(11) C22 0.0317(15) 0.0296(16) 0.0375(16) -0.0027(12) -0.0179(13) 0.0048(12) C23 0.0367(15) 0.0276(15) 0.0264(14) 0.0038(12) -0.0184(12) -0.0003(12) C24 0.054(2) 0.0433(19) 0.0464(18) 0.0129(15) -0.0369(16) -0.0148(15) C25 0.0484(18) 0.0344(17) 0.0191(13) -0.0046(12) -0.0090(12) 0.0049(14) C26 0.135(4) 0.063(3) 0.056(2) 0.012(2) -0.066(3) -0.031(3) C27 0.0306(15) 0.0300(15) 0.0204(13) -0.0025(11) -0.0021(11) -0.0010(12) C28 0.0344(15) 0.0262(15) 0.0273(14) -0.0007(12) -0.0054(12) 0.0024(12) C29 0.0271(14) 0.0192(13) 0.0303(14) 0.0009(11) -0.0125(11) 0.0033(11) C30 0.0299(15) 0.0310(16) 0.0500(18) 0.0005(14) -0.0158(13) -0.0005(12) C31 0.0294(14) 0.0191(13) 0.0273(14) 0.0052(11) -0.0120(11) 0.0008(11) C32 0.0396(16) 0.0268(15) 0.0337(15) 0.0007(12) -0.0199(13) -0.0023(12) C33 0.0276(13) 0.0209(13) 0.0179(12) 0.0011(10) -0.0067(10) -0.0016(10) C34 0.0464(17) 0.0366(17) 0.0290(14) 0.0089(13) -0.0226(13) -0.0122(14) C35 0.0271(13) 0.0172(13) 0.0198(12) -0.0007(10) -0.0082(10) -0.0012(10) C36 0.0260(14) 0.0261(14) 0.0261(14) 0.0012(11) -0.0059(11) -0.0021(11) C37 0.0212(12) 0.0156(12) 0.0219(12) 0.0018(10) -0.0110(10) -0.0019(10) C38 0.0317(15) 0.0290(15) 0.0263(14) 0.0051(11) -0.0096(11) -0.0094(12) C39 0.0248(14) 0.0336(16) 0.0364(16) 0.0013(13) -0.0079(12) -0.0066(12) C40 0.0303(15) 0.0357(16) 0.0400(16) -0.0047(13) -0.0187(13) -0.0045(12) C41 0.0315(15) 0.0487(19) 0.0288(15) 0.0043(13) -0.0169(12) -0.0097(13) O1S 0.0396(12) 0.0493(14) 0.0383(12) -0.0011(10) -0.0101(10) -0.0100(10) C1S 0.050(2) 0.045(2) 0.0464(19) -0.0117(16) -0.0194(16) 0.0066(16) C2S 0.057(2) 0.051(2) 0.084(3) -0.011(2) -0.023(2) -0.0149(19) C3S 0.060(2) 0.072(3) 0.0405(19) 0.0094(18) -0.0168(17) -0.023(2) C4S 0.0385(16) 0.0330(17) 0.0329(16) 0.0013(13) -0.0088(13) -0.0019(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 1.958(2) . ? Co1 N1 1.961(2) . ? Co1 N3 1.966(2) . ? Co1 N2 1.969(2) . ? Co1 O1 2.2065(19) . ? O1 C41 1.420(3) . ? O1 C38 1.428(3) . ? N1 C4 1.379(3) . ? N1 C1 1.387(3) . ? N2 C9 1.375(3) . ? N2 C6 1.380(3) . ? N3 C14 1.372(3) . ? N3 C11 1.380(3) . ? N4 C16 1.373(3) . ? N4 C19 1.381(3) . ? C1 C20 1.413(3) . ? C1 C2 1.464(3) . ? C2 C3 1.358(4) . ? C2 C21 1.511(4) . ? C3 C4 1.431(4) . ? C3 C23 1.511(3) . ? C4 C5 1.392(3) . ? C5 C6 1.377(4) . ? C6 C7 1.447(4) . ? C7 C8 1.355(4) . ? C7 C25 1.503(4) . ? C8 C9 1.450(3) . ? C8 C27 1.504(4) . ? C9 C10 1.380(4) . ? C10 C11 1.383(4) . ? C11 C12 1.444(4) . ? C12 C13 1.367(4) . ? C12 C29 1.505(3) . ? C13 C14 1.445(3) . ? C13 C31 1.491(3) . ? C14 C15 1.378(3) . ? C15 C16 1.392(3) . ? C16 C17 1.438(3) . ? C17 C18 1.361(3) . ? C17 C33 1.499(3) . ? C18 C19 1.468(3) . ? C18 C35 1.510(3) . ? C19 C20 1.399(3) . ? C20 C37 1.515(3) . ? C21 C22 1.530(4) . ? C23 C24 1.528(4) . ? C25 C26 1.497(5) . ? C27 C28 1.521(4) . ? C29 C30 1.524(4) . ? C31 C32 1.534(4) . ? C33 C34 1.535(4) . ? C35 C36 1.528(4) . ? C37 C37 1.546(5) 2_788 ? C38 C39 1.523(4) . ? C39 C40 1.520(4) . ? C40 C41 1.529(4) . ? O1S C4S 1.421(3) . ? O1S C1S 1.432(4) . ? C1S C2S 1.507(5) . ? C2S C3S 1.505(5) . ? C3S C4S 1.483(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N1 88.65(8) . . ? N4 Co1 N3 91.21(8) . . ? N1 Co1 N3 176.87(8) . . ? N4 Co1 N2 176.88(8) . . ? N1 Co1 N2 91.01(8) . . ? N3 Co1 N2 88.97(8) . . ? N4 Co1 O1 90.56(8) . . ? N1 Co1 O1 90.40(8) . . ? N3 Co1 O1 92.73(8) . . ? N2 Co1 O1 92.55(8) . . ? C41 O1 C38 110.8(2) . . ? C41 O1 Co1 124.66(16) . . ? C38 O1 Co1 124.46(15) . . ? C4 N1 C1 105.1(2) . . ? C4 N1 Co1 126.48(17) . . ? C1 N1 Co1 128.28(16) . . ? C9 N2 C6 105.2(2) . . ? C9 N2 Co1 127.57(17) . . ? C6 N2 Co1 127.17(17) . . ? C14 N3 C11 104.8(2) . . ? C14 N3 Co1 127.02(16) . . ? C11 N3 Co1 128.18(17) . . ? C16 N4 C19 105.72(19) . . ? C16 N4 Co1 126.26(16) . . ? C19 N4 Co1 127.71(16) . . ? N1 C1 C20 122.9(2) . . ? N1 C1 C2 110.1(2) . . ? C20 C1 C2 126.9(2) . . ? C3 C2 C1 106.1(2) . . ? C3 C2 C21 122.9(2) . . ? C1 C2 C21 130.5(2) . . ? C2 C3 C4 107.6(2) . . ? C2 C3 C23 127.3(2) . . ? C4 C3 C23 125.1(2) . . ? N1 C4 C5 124.6(2) . . ? N1 C4 C3 111.0(2) . . ? C5 C4 C3 124.0(2) . . ? C6 C5 C4 125.3(2) . . ? C5 C6 N2 124.0(2) . . ? C5 C6 C7 125.2(2) . . ? N2 C6 C7 110.7(2) . . ? C8 C7 C6 106.6(2) . . ? C8 C7 C25 128.3(2) . . ? C6 C7 C25 125.1(3) . . ? C7 C8 C9 106.8(2) . . ? C7 C8 C27 128.3(2) . . ? C9 C8 C27 124.8(2) . . ? N2 C9 C10 124.6(2) . . ? N2 C9 C8 110.6(2) . . ? C10 C9 C8 124.7(2) . . ? C9 C10 C11 124.4(2) . . ? N3 C11 C10 123.8(2) . . ? N3 C11 C12 111.1(2) . . ? C10 C11 C12 125.1(2) . . ? C13 C12 C11 106.5(2) . . ? C13 C12 C29 127.7(2) . . ? C11 C12 C29 125.8(2) . . ? C12 C13 C14 106.3(2) . . ? C12 C13 C31 128.5(2) . . ? C14 C13 C31 125.0(2) . . ? N3 C14 C15 124.3(2) . . ? N3 C14 C13 111.4(2) . . ? C15 C14 C13 124.0(2) . . ? C14 C15 C16 124.8(2) . . ? N4 C16 C15 125.1(2) . . ? N4 C16 C17 111.2(2) . . ? C15 C16 C17 123.2(2) . . ? C18 C17 C16 106.9(2) . . ? C18 C17 C33 128.0(2) . . ? C16 C17 C33 125.1(2) . . ? C17 C18 C19 106.4(2) . . ? C17 C18 C35 122.9(2) . . ? C19 C18 C35 129.8(2) . . ? N4 C19 C20 124.1(2) . . ? N4 C19 C18 109.7(2) . . ? C20 C19 C18 126.1(2) . . ? C19 C20 C1 122.2(2) . . ? C19 C20 C37 119.0(2) . . ? C1 C20 C37 118.6(2) . . ? C2 C21 C22 113.3(2) . . ? C3 C23 C24 112.0(2) . . ? C26 C25 C7 112.4(3) . . ? C8 C27 C28 113.1(2) . . ? C12 C29 C30 113.9(2) . . ? C13 C31 C32 111.7(2) . . ? C17 C33 C34 112.7(2) . . ? C18 C35 C36 111.1(2) . . ? C20 C37 C37 110.4(2) . 2_788 ? O1 C38 C39 105.2(2) . . ? C40 C39 C38 101.8(2) . . ? C39 C40 C41 102.9(2) . . ? O1 C41 C40 106.3(2) . . ? C4S O1S C1S 108.1(2) . . ? O1S C1S C2S 107.2(3) . . ? C3S C2S C1S 104.7(3) . . ? C4S C3S C2S 101.9(3) . . ? O1S C4S C3S 108.0(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.993 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 940536' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12octa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H92 Cl6 Co2 I4 N8' _chemical_formula_weight 1955.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _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 14.7397(7) _cell_length_b 18.4955(9) _cell_length_c 14.3836(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.3920(10) _cell_angle_gamma 90.00 _cell_volume 3879.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.0 _exptl_crystal_description Block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 2.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7267 _exptl_absorpt_correction_T_max 0.8046 _exptl_absorpt_process_details 'SADABS 2.05 (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27648 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_unetI/netI 0.0656 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7212 _reflns_number_gt 5430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0560P)^2^+16.2125P] 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 7212 _refine_ls_number_parameters 468 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.75688(5) 0.10712(4) 0.15214(5) 0.00794(19) Uani 1 1 d . . . I1 I 0.79644(3) -0.02105(2) 0.20078(3) 0.01815(13) Uani 1 1 d . . . I2 I 0.94052(3) -0.00144(3) 0.41681(4) 0.03436(16) Uani 1 1 d . . . N1 N 0.7538(3) 0.0961(3) 0.0183(3) 0.0093(10) Uani 1 1 d . . . N2 N 0.6239(3) 0.0972(3) 0.1382(3) 0.0105(11) Uani 1 1 d . . . N3 N 0.7553(3) 0.1382(3) 0.2801(3) 0.0079(10) Uani 1 1 d . . . N4 N 0.8856(3) 0.1327(3) 0.1594(3) 0.0099(11) Uani 1 1 d . . . C1 C 0.8263(4) 0.0834(3) -0.0302(4) 0.0112(13) Uani 1 1 d . . . C2 C 0.7941(4) 0.0855(3) -0.1319(4) 0.0136(13) Uani 1 1 d . . . C3 C 0.7032(4) 0.0973(3) -0.1417(4) 0.0139(13) Uani 1 1 d . . . C4 C 0.6771(4) 0.0994(3) -0.0507(4) 0.0112(13) Uani 1 1 d . . . C5 C 0.5881(4) 0.0982(3) -0.0316(4) 0.0138(13) Uani 1 1 d . . . H5A H 0.5405 0.0999 -0.0838 0.017 Uiso 1 1 calc R . . C6 C 0.5624(4) 0.0946(3) 0.0555(4) 0.0106(13) Uani 1 1 d . . . C7 C 0.4698(4) 0.0867(3) 0.0756(5) 0.0158(14) Uani 1 1 d . . . C8 C 0.4751(4) 0.0811(3) 0.1694(4) 0.0138(13) Uani 1 1 d . . . C9 C 0.5711(4) 0.0887(3) 0.2087(4) 0.0115(13) Uani 1 1 d . . . C10 C 0.6038(4) 0.0971(3) 0.3026(4) 0.0141(13) Uani 1 1 d . . . H10A H 0.5653 0.0828 0.3467 0.017 Uiso 1 1 calc R . . C11 C 0.6884(4) 0.1248(3) 0.3367(4) 0.0105(13) Uani 1 1 d . . . C12 C 0.7151(4) 0.1524(3) 0.4294(4) 0.0151(14) Uani 1 1 d . . . C13 C 0.7963(4) 0.1862(3) 0.4301(4) 0.0129(13) Uani 1 1 d . . . C14 C 0.8224(4) 0.1745(3) 0.3379(4) 0.0119(13) Uani 1 1 d . . . C15 C 0.9075(4) 0.1900(3) 0.3141(4) 0.0142(13) Uani 1 1 d . . . H15A H 0.9481 0.2186 0.3565 0.017 Uiso 1 1 calc R . . C16 C 0.9376(4) 0.1670(3) 0.2331(4) 0.0117(13) Uani 1 1 d . . . C17 C 1.0329(4) 0.1702(4) 0.2182(4) 0.0154(14) Uani 1 1 d . . . C18 C 1.0382(4) 0.1341(3) 0.1363(4) 0.0137(13) Uani 1 1 d . . . C19 C 0.9455(4) 0.1112(3) 0.0994(4) 0.0112(13) Uani 1 1 d . . . C20 C 0.9166(4) 0.0781(3) 0.0128(4) 0.0134(13) Uani 1 1 d . . . C21 C 0.8502(4) 0.0869(4) -0.2115(4) 0.0190(15) Uani 1 1 d . . . H21A H 0.9155 0.0942 -0.1853 0.023 Uiso 1 1 calc R . . H21B H 0.8305 0.1286 -0.2527 0.023 Uiso 1 1 calc R . . C22 C 0.8416(5) 0.0181(4) -0.2707(5) 0.0281(17) Uani 1 1 d . . . H22A H 0.8751 0.0241 -0.3242 0.042 Uiso 1 1 calc R . . H22B H 0.7767 0.0088 -0.2937 0.042 Uiso 1 1 calc R . . H22C H 0.8673 -0.0227 -0.2322 0.042 Uiso 1 1 calc R . . C23 C 0.6394(4) 0.1146(4) -0.2300(4) 0.0191(15) Uani 1 1 d . . . H23A H 0.5806 0.0890 -0.2293 0.023 Uiso 1 1 calc R . . H23B H 0.6665 0.0972 -0.2850 0.023 Uiso 1 1 calc R . . C24 C 0.6216(6) 0.1951(4) -0.2397(5) 0.0348(19) Uani 1 1 d . . . H24A H 0.5767 0.2042 -0.2958 0.052 Uiso 1 1 calc R . . H24B H 0.6790 0.2202 -0.2457 0.052 Uiso 1 1 calc R . . H24C H 0.5975 0.2129 -0.1840 0.052 Uiso 1 1 calc R . . C25 C 0.3873(4) 0.0895(4) 0.0015(5) 0.0187(15) Uani 1 1 d . . . H25A H 0.3335 0.0707 0.0279 0.022 Uiso 1 1 calc R . . H25B H 0.3975 0.0577 -0.0514 0.022 Uiso 1 1 calc R . . C26 C 0.3667(4) 0.1660(4) -0.0353(5) 0.0276(17) Uani 1 1 d . . . H26A H 0.3146 0.1649 -0.0861 0.041 Uiso 1 1 calc R . . H26B H 0.4206 0.1856 -0.0592 0.041 Uiso 1 1 calc R . . H26C H 0.3517 0.1968 0.0158 0.041 Uiso 1 1 calc R . . C27 C 0.3990(4) 0.0785(4) 0.2284(5) 0.0251(17) Uani 1 1 d . . . H27A H 0.4190 0.0491 0.2852 0.030 Uiso 1 1 calc R . . H27B H 0.3450 0.0545 0.1923 0.030 Uiso 1 1 calc R . . C28 C 0.3714(5) 0.1533(4) 0.2579(5) 0.0327(19) Uani 1 1 d . . . H28A H 0.3245 0.1488 0.2992 0.049 Uiso 1 1 calc R . . H28B H 0.3468 0.1813 0.2020 0.049 Uiso 1 1 calc R . . H28C H 0.4252 0.1781 0.2915 0.049 Uiso 1 1 calc R . . C29 C 0.6567(4) 0.1485(4) 0.5068(4) 0.0186(14) Uani 1 1 d . . . H29A H 0.6967 0.1527 0.5682 0.022 Uiso 1 1 calc R . . H29B H 0.6263 0.1007 0.5047 0.022 Uiso 1 1 calc R . . C30 C 0.5843(5) 0.2073(4) 0.4996(5) 0.0273(17) Uani 1 1 d . . . H30A H 0.5450 0.1999 0.5482 0.041 Uiso 1 1 calc R . . H30B H 0.5469 0.2054 0.4374 0.041 Uiso 1 1 calc R . . H30C H 0.6142 0.2547 0.5084 0.041 Uiso 1 1 calc R . . C31 C 0.8510(4) 0.2261(4) 0.5082(4) 0.0199(15) Uani 1 1 d . . . H31A H 0.8091 0.2457 0.5499 0.024 Uiso 1 1 calc R . . H31B H 0.8817 0.2674 0.4821 0.024 Uiso 1 1 calc R . . C32 C 0.9232(5) 0.1793(4) 0.5662(5) 0.0248(16) Uani 1 1 d . . . H32A H 0.9524 0.2069 0.6207 0.037 Uiso 1 1 calc R . . H32B H 0.9697 0.1650 0.5275 0.037 Uiso 1 1 calc R . . H32C H 0.8941 0.1360 0.5878 0.037 Uiso 1 1 calc R . . C33 C 1.1091(4) 0.2059(4) 0.2821(5) 0.0207(15) Uani 1 1 d . . . H33A H 1.0945 0.2045 0.3471 0.025 Uiso 1 1 calc R . . H33B H 1.1661 0.1778 0.2810 0.025 Uiso 1 1 calc R . . C34 C 1.1258(6) 0.2817(5) 0.2570(6) 0.045(2) Uani 1 1 d . . . H34A H 1.1771 0.3013 0.3009 0.068 Uiso 1 1 calc R . . H34B H 1.0706 0.3105 0.2607 0.068 Uiso 1 1 calc R . . H34C H 1.1409 0.2837 0.1929 0.068 Uiso 1 1 calc R . . C35 C 1.1216(4) 0.1328(4) 0.0870(5) 0.0178(14) Uani 1 1 d . . . H35A H 1.1289 0.0839 0.0613 0.021 Uiso 1 1 calc R . . H35B H 1.1768 0.1434 0.1330 0.021 Uiso 1 1 calc R . . C36 C 1.1147(5) 0.1879(4) 0.0071(5) 0.0248(16) Uani 1 1 d . . . H36A H 1.1707 0.1863 -0.0220 0.037 Uiso 1 1 calc R . . H36B H 1.1072 0.2365 0.0322 0.037 Uiso 1 1 calc R . . H36C H 1.0617 0.1763 -0.0400 0.037 Uiso 1 1 calc R . . C37 C 0.9831(4) 0.0313(3) -0.0326(4) 0.0144(13) Uani 1 1 d . . . H37A H 1.0359 0.0609 -0.0453 0.017 Uiso 1 1 calc R . . H37B H 0.9519 0.0121 -0.0933 0.017 Uiso 1 1 calc R . . C1S C 0.6694(6) -0.0878(5) 0.4143(7) 0.052(2) Uani 1 1 d . A 1 H1SA H 0.7006 -0.0465 0.3870 0.062 Uiso 1 1 calc R A 1 Cl1 Cl 0.5777(3) -0.05633(19) 0.4643(4) 0.0749(15) Uani 0.762(3) 1 d P A 1 Cl2 Cl 0.7486(2) -0.1348(2) 0.4962(3) 0.0837(14) Uani 0.762(3) 1 d P A 1 Cl3 Cl 0.6262(3) -0.1505(2) 0.3233(3) 0.0747(12) Uani 0.762(3) 1 d P A 1 Cl1A Cl 0.6919(14) -0.0735(11) 0.3408(15) 0.034(6) Uiso 0.095(5) 1 d P B 2 Cl2A Cl 0.598(2) -0.100(2) 0.489(2) 0.072(10) Uiso 0.095(5) 1 d P B 2 Cl3A Cl 0.726(2) -0.1565(15) 0.410(2) 0.057(8) Uiso 0.095(5) 1 d P B 2 Cl1B Cl 0.7100(18) -0.0533(16) 0.5286(19) 0.105(9) Uiso 0.143(6) 1 d P C 3 Cl2B Cl 0.679(2) -0.1601(15) 0.369(2) 0.090(9) Uiso 0.143(6) 1 d P C 3 Cl3B Cl 0.556(2) -0.0664(18) 0.406(2) 0.099(11) Uiso 0.143(6) 1 d P C 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 0.0049(4) 0.0123(4) 0.0068(4) -0.0026(3) 0.0013(3) -0.0004(3) I1 0.0198(2) 0.0149(2) 0.0186(2) -0.00002(18) -0.00103(17) 0.00149(17) I2 0.0297(3) 0.0293(3) 0.0452(3) 0.0070(2) 0.0093(2) 0.0094(2) N1 0.009(3) 0.011(3) 0.008(3) -0.002(2) 0.002(2) -0.0021(19) N2 0.008(3) 0.014(3) 0.009(3) -0.004(2) 0.001(2) 0.000(2) N3 0.006(2) 0.013(3) 0.006(2) -0.002(2) 0.002(2) 0.0004(19) N4 0.011(3) 0.011(3) 0.007(2) -0.001(2) 0.001(2) 0.000(2) C1 0.015(3) 0.011(3) 0.009(3) -0.003(2) 0.005(2) -0.001(2) C2 0.020(3) 0.014(3) 0.008(3) -0.003(3) 0.006(3) -0.002(3) C3 0.014(3) 0.019(4) 0.008(3) -0.003(3) -0.001(2) 0.000(3) C4 0.011(3) 0.012(3) 0.009(3) -0.001(2) -0.004(2) 0.002(2) C5 0.008(3) 0.018(4) 0.014(3) -0.002(3) -0.005(3) 0.004(2) C6 0.007(3) 0.010(3) 0.015(3) -0.001(2) 0.003(2) 0.002(2) C7 0.010(3) 0.013(3) 0.024(4) -0.006(3) 0.002(3) -0.002(2) C8 0.005(3) 0.016(3) 0.020(3) -0.006(3) 0.000(3) -0.001(2) C9 0.010(3) 0.008(3) 0.019(3) -0.003(3) 0.006(3) -0.004(2) C10 0.012(3) 0.018(4) 0.014(3) 0.001(3) 0.007(3) 0.001(2) C11 0.014(3) 0.005(3) 0.013(3) -0.001(2) 0.006(3) 0.006(2) C12 0.018(3) 0.013(3) 0.014(3) -0.002(3) 0.002(3) 0.003(3) C13 0.015(3) 0.015(3) 0.009(3) 0.003(3) 0.003(3) 0.000(2) C14 0.016(3) 0.009(3) 0.010(3) -0.005(2) 0.002(3) 0.001(2) C15 0.013(3) 0.010(3) 0.019(3) -0.006(3) 0.000(3) -0.005(2) C16 0.009(3) 0.013(3) 0.013(3) -0.001(3) 0.001(2) -0.001(2) C17 0.011(3) 0.023(4) 0.012(3) 0.002(3) 0.001(3) -0.003(3) C18 0.009(3) 0.019(4) 0.013(3) 0.002(3) 0.001(3) 0.003(2) C19 0.009(3) 0.013(3) 0.011(3) 0.002(3) 0.000(2) 0.002(2) C20 0.009(3) 0.016(3) 0.016(3) 0.001(3) 0.005(3) 0.001(2) C21 0.022(4) 0.026(4) 0.010(3) 0.005(3) 0.002(3) 0.000(3) C22 0.030(4) 0.037(5) 0.019(4) 0.001(3) 0.011(3) 0.003(3) C23 0.021(4) 0.028(4) 0.008(3) -0.004(3) -0.001(3) -0.002(3) C24 0.047(5) 0.039(5) 0.014(4) 0.001(3) -0.010(3) 0.009(4) C25 0.011(3) 0.027(4) 0.018(4) -0.002(3) 0.001(3) -0.004(3) C26 0.011(4) 0.037(5) 0.033(4) -0.005(4) -0.003(3) 0.006(3) C27 0.007(3) 0.044(5) 0.026(4) -0.007(3) 0.009(3) -0.012(3) C28 0.014(4) 0.052(5) 0.035(4) -0.016(4) 0.012(3) -0.001(3) C29 0.024(4) 0.022(4) 0.013(3) 0.000(3) 0.011(3) -0.003(3) C30 0.027(4) 0.036(5) 0.022(4) -0.003(3) 0.014(3) 0.003(3) C31 0.025(4) 0.019(4) 0.016(4) -0.005(3) 0.004(3) -0.004(3) C32 0.031(4) 0.028(4) 0.015(4) -0.002(3) 0.002(3) -0.004(3) C33 0.009(3) 0.035(4) 0.019(4) -0.011(3) 0.006(3) -0.005(3) C34 0.039(5) 0.059(6) 0.032(5) -0.005(4) -0.012(4) -0.022(4) C35 0.005(3) 0.027(4) 0.022(4) -0.005(3) 0.004(3) -0.003(3) C36 0.018(4) 0.036(4) 0.022(4) -0.002(3) 0.010(3) -0.002(3) C37 0.012(3) 0.018(4) 0.013(3) -0.004(3) 0.003(3) 0.002(2) C1S 0.057(6) 0.042(6) 0.061(6) 0.002(5) 0.024(5) 0.000(4) Cl1 0.091(3) 0.0302(19) 0.125(4) 0.014(2) 0.087(3) 0.0122(19) Cl2 0.046(2) 0.106(3) 0.099(3) 0.052(3) 0.008(2) 0.0044(19) Cl3 0.077(3) 0.076(3) 0.075(3) -0.019(2) 0.024(2) -0.037(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.930(5) . ? Co1 N3 1.931(5) . ? Co1 N4 1.943(5) . ? Co1 N2 1.950(5) . ? Co1 I1 2.5158(9) . ? I2 I2 2.7530(11) 3_756 ? N1 C1 1.379(7) . ? N1 C4 1.393(7) . ? N2 C9 1.375(7) . ? N2 C6 1.387(7) . ? N3 C14 1.372(7) . ? N3 C11 1.390(7) . ? N4 C16 1.370(7) . ? N4 C19 1.381(7) . ? C1 C20 1.387(8) . ? C1 C2 1.470(8) . ? C2 C3 1.345(8) . ? C2 C21 1.508(8) . ? C3 C4 1.418(8) . ? C3 C23 1.499(8) . ? C4 C5 1.379(8) . ? C5 C6 1.363(8) . ? C5 H5A 0.9500 . ? C6 C7 1.443(8) . ? C7 C8 1.345(9) . ? C7 C25 1.496(9) . ? C8 C9 1.452(8) . ? C8 C27 1.502(8) . ? C9 C10 1.375(8) . ? C10 C11 1.370(8) . ? C10 H10A 0.9500 . ? C11 C12 1.428(8) . ? C12 C13 1.349(8) . ? C12 C29 1.505(8) . ? C13 C14 1.449(8) . ? C13 C31 1.480(8) . ? C14 C15 1.378(8) . ? C15 C16 1.373(8) . ? C15 H15A 0.9500 . ? C16 C17 1.453(8) . ? C17 C18 1.365(9) . ? C17 C33 1.498(8) . ? C18 C19 1.455(8) . ? C18 C35 1.508(8) . ? C19 C20 1.397(8) . ? C20 C37 1.525(8) . ? C21 C22 1.525(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.515(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.527(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.520(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.517(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.522(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.478(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.527(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C37 1.528(12) 3_755 ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C1S Cl1 1.721(9) . ? C1S Cl2 1.762(10) . ? C1S Cl3 1.795(10) . ? C1S H1SA 1.0000 . ? Cl1A Cl3A 1.86(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N3 168.5(2) . . ? N1 Co1 N4 87.69(19) . . ? N3 Co1 N4 91.36(19) . . ? N1 Co1 N2 90.6(2) . . ? N3 Co1 N2 88.53(19) . . ? N4 Co1 N2 170.9(2) . . ? N1 Co1 I1 98.57(15) . . ? N3 Co1 I1 92.88(14) . . ? N4 Co1 I1 91.71(14) . . ? N2 Co1 I1 97.42(15) . . ? C1 N1 C4 104.8(5) . . ? C1 N1 Co1 128.0(4) . . ? C4 N1 Co1 127.2(4) . . ? C9 N2 C6 105.0(4) . . ? C9 N2 Co1 127.1(4) . . ? C6 N2 Co1 127.8(4) . . ? C14 N3 C11 104.0(5) . . ? C14 N3 Co1 128.0(4) . . ? C11 N3 Co1 127.8(4) . . ? C16 N4 C19 106.3(5) . . ? C16 N4 Co1 125.8(4) . . ? C19 N4 Co1 127.2(4) . . ? N1 C1 C20 123.4(5) . . ? N1 C1 C2 109.7(5) . . ? C20 C1 C2 126.5(5) . . ? C3 C2 C1 106.3(5) . . ? C3 C2 C21 124.4(6) . . ? C1 C2 C21 128.6(5) . . ? C2 C3 C4 107.9(5) . . ? C2 C3 C23 128.0(6) . . ? C4 C3 C23 123.7(5) . . ? C5 C4 N1 123.7(5) . . ? C5 C4 C3 125.3(5) . . ? N1 C4 C3 110.8(5) . . ? C6 C5 C4 125.8(6) . . ? C6 C5 H5A 117.1 . . ? C4 C5 H5A 117.1 . . ? C5 C6 N2 123.5(5) . . ? C5 C6 C7 126.0(5) . . ? N2 C6 C7 110.5(5) . . ? C8 C7 C6 106.9(5) . . ? C8 C7 C25 129.8(6) . . ? C6 C7 C25 123.2(6) . . ? C7 C8 C9 107.1(5) . . ? C7 C8 C27 129.1(6) . . ? C9 C8 C27 123.3(6) . . ? C10 C9 N2 123.8(5) . . ? C10 C9 C8 125.1(5) . . ? N2 C9 C8 110.4(5) . . ? C11 C10 C9 124.4(6) . . ? C11 C10 H10A 117.8 . . ? C9 C10 H10A 117.8 . . ? C10 C11 N3 122.9(5) . . ? C10 C11 C12 125.5(5) . . ? N3 C11 C12 111.1(5) . . ? C13 C12 C11 107.2(5) . . ? C13 C12 C29 128.2(6) . . ? C11 C12 C29 124.3(6) . . ? C12 C13 C14 106.1(5) . . ? C12 C13 C31 128.3(6) . . ? C14 C13 C31 125.5(5) . . ? N3 C14 C15 123.6(5) . . ? N3 C14 C13 111.4(5) . . ? C15 C14 C13 124.7(5) . . ? C16 C15 C14 124.4(6) . . ? C16 C15 H15A 117.8 . . ? C14 C15 H15A 117.8 . . ? N4 C16 C15 125.9(5) . . ? N4 C16 C17 110.4(5) . . ? C15 C16 C17 123.5(5) . . ? C18 C17 C16 106.6(5) . . ? C18 C17 C33 127.8(6) . . ? C16 C17 C33 125.6(6) . . ? C17 C18 C19 106.8(5) . . ? C17 C18 C35 124.5(6) . . ? C19 C18 C35 127.6(6) . . ? N4 C19 C20 122.9(5) . . ? N4 C19 C18 109.8(5) . . ? C20 C19 C18 127.0(5) . . ? C1 C20 C19 121.0(5) . . ? C1 C20 C37 118.9(5) . . ? C19 C20 C37 120.0(5) . . ? C2 C21 C22 113.5(6) . . ? C2 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C2 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 C24 111.5(5) . . ? C3 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C3 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 C25 C26 112.3(5) . . ? C7 C25 H25A 109.2 . . ? C26 C25 H25A 109.2 . . ? C7 C25 H25B 109.2 . . ? C26 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C28 112.4(6) . . ? C8 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C8 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C12 C29 C30 112.8(5) . . ? C12 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? C12 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C13 C31 C32 113.1(6) . . ? C13 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? C13 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C17 113.9(6) . . ? C34 C33 H33A 108.8 . . ? C17 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? C17 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C18 C35 C36 112.0(5) . . ? C18 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? C18 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C20 C37 C37 109.8(6) . 3_755 ? C20 C37 H37A 109.7 . . ? C37 C37 H37A 109.7 3_755 . ? C20 C37 H37B 109.7 . . ? C37 C37 H37B 109.7 3_755 . ? H37A C37 H37B 108.2 . . ? Cl1 C1S Cl2 111.8(6) . . ? Cl1 C1S Cl3 107.9(6) . . ? Cl2 C1S Cl3 107.3(5) . . ? Cl1 C1S H1SA 109.9 . . ? Cl2 C1S H1SA 109.9 . . ? Cl3 C1S H1SA 109.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.178 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.156 _database_code_depnum_ccdc_archive 'CCDC 940533' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12mayam _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126 H150 Cl2 Co2 N16 O8' _chemical_formula_weight 2205.38 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 13.595(5) _cell_length_b 14.481(5) _cell_length_c 16.835(6) _cell_angle_alpha 85.952(7) _cell_angle_beta 70.336(7) _cell_angle_gamma 70.463(6) _cell_volume 2938.2(18) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 0.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9437 _exptl_absorpt_correction_T_max 0.9619 _exptl_absorpt_process_details 'SADABS 2.05 (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15780 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_unetI/netI 0.1006 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10666 _reflns_number_gt 6737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0903P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10666 _refine_ls_number_parameters 692 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1809 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 0.75843(4) 0.25611(3) 0.72585(3) 0.02400(16) Uani 1 1 d . . . N1 N 0.9154(2) 0.1841(2) 0.70005(18) 0.0249(7) Uani 1 1 d . . . N2 N 0.7794(2) 0.3745(2) 0.75789(18) 0.0246(7) Uani 1 1 d . . . N3 N 0.5995(2) 0.3278(2) 0.75600(18) 0.0257(7) Uani 1 1 d . . . N4 N 0.7388(2) 0.1367(2) 0.69441(18) 0.0245(7) Uani 1 1 d . . . N5 N 0.7362(2) 0.2172(2) 0.84020(18) 0.0258(7) Uani 1 1 d . . . N6 N 0.7656(3) 0.1339(2) 0.9488(2) 0.0351(8) Uani 1 1 d . . . N7 N 0.7853(2) 0.2941(2) 0.60995(19) 0.0263(7) Uani 1 1 d . . . N8 N 0.7802(3) 0.3131(2) 0.4804(2) 0.0360(8) Uani 1 1 d . . . C1 C 0.9746(3) 0.0931(2) 0.6579(2) 0.0249(8) Uani 1 1 d . . . C2 C 1.0820(3) 0.0560(2) 0.6699(2) 0.0265(8) Uani 1 1 d . . . C3 C 1.0873(3) 0.1262(3) 0.7168(2) 0.0279(9) Uani 1 1 d . . . C4 C 0.9845(3) 0.2066(3) 0.7324(2) 0.0264(8) Uani 1 1 d . . . C5 C 0.9639(3) 0.2981(3) 0.7676(2) 0.0274(8) Uani 1 1 d . . . H5A H 1.0177 0.3061 0.7882 0.033 Uiso 1 1 calc R . . C6 C 0.8700(3) 0.3785(2) 0.7745(2) 0.0265(8) Uani 1 1 d . . . C7 C 0.8544(3) 0.4775(3) 0.7999(2) 0.0282(9) Uani 1 1 d . . . C8 C 0.7520(3) 0.5326(3) 0.7996(2) 0.0302(9) Uani 1 1 d . . . C9 C 0.7050(3) 0.4676(2) 0.7748(2) 0.0255(8) Uani 1 1 d . . . C10 C 0.5954(3) 0.4935(2) 0.7785(2) 0.0271(8) Uani 1 1 d . . . H10A H 0.5530 0.5612 0.7837 0.033 Uiso 1 1 calc R . . C11 C 0.5447(3) 0.4263(3) 0.7752(2) 0.0287(9) Uani 1 1 d . . . C12 C 0.4265(3) 0.4479(3) 0.7986(2) 0.0312(9) Uani 1 1 d . . . C13 C 0.4095(3) 0.3615(3) 0.7976(3) 0.0342(9) Uani 1 1 d . . . C14 C 0.5182(3) 0.2868(3) 0.7697(2) 0.0286(9) Uani 1 1 d . . . C15 C 0.5367(3) 0.1898(3) 0.7513(2) 0.0292(9) Uani 1 1 d . . . H15A H 0.4743 0.1682 0.7668 0.035 Uiso 1 1 calc R . . C16 C 0.6399(3) 0.1218(3) 0.7117(2) 0.0274(8) Uani 1 1 d . . . C17 C 0.6559(3) 0.0299(3) 0.6733(2) 0.0281(8) Uani 1 1 d . . . C18 C 0.7658(3) -0.0086(3) 0.6279(2) 0.0270(8) Uani 1 1 d . . . C19 C 0.8188(3) 0.0574(2) 0.6422(2) 0.0257(8) Uani 1 1 d . . . C20 C 0.9321(3) 0.0425(2) 0.6174(2) 0.0254(8) Uani 1 1 d . . . C21 C 1.1657(3) -0.0460(3) 0.6501(2) 0.0296(9) Uani 1 1 d . . . H21A H 1.1301 -0.0905 0.6381 0.036 Uiso 1 1 calc R . . H21B H 1.1864 -0.0689 0.7009 0.036 Uiso 1 1 calc R . . C22 C 1.2709(3) -0.0549(3) 0.5758(3) 0.0373(10) Uani 1 1 d . . . H22A H 1.3264 -0.1192 0.5749 0.056 Uiso 1 1 calc R . . H22B H 1.2999 -0.0032 0.5818 0.056 Uiso 1 1 calc R . . H22C H 1.2542 -0.0480 0.5230 0.056 Uiso 1 1 calc R . . C23 C 1.1753(3) 0.1214(3) 0.7531(2) 0.0319(9) Uani 1 1 d . . . H23A H 1.1938 0.1826 0.7416 0.038 Uiso 1 1 calc R . . H23B H 1.2428 0.0661 0.7246 0.038 Uiso 1 1 calc R . . C24 C 1.1401(4) 0.1079(3) 0.8476(3) 0.0497(12) Uani 1 1 d . . . H24A H 1.1984 0.1096 0.8689 0.074 Uiso 1 1 calc R . . H24B H 1.1279 0.0446 0.8590 0.074 Uiso 1 1 calc R . . H24C H 1.0714 0.1609 0.8759 0.074 Uiso 1 1 calc R . . C25 C 0.9363(3) 0.5111(3) 0.8205(3) 0.0370(10) Uani 1 1 d . . . H25A H 0.9865 0.4551 0.8404 0.044 Uiso 1 1 calc R . . H25B H 0.8963 0.5620 0.8671 0.044 Uiso 1 1 calc R . . C26 C 1.0051(4) 0.5530(3) 0.7448(3) 0.0530(13) Uani 1 1 d . . . H26A H 1.0543 0.5773 0.7621 0.079 Uiso 1 1 calc R . . H26B H 0.9557 0.6070 0.7237 0.079 Uiso 1 1 calc R . . H26C H 1.0494 0.5014 0.7001 0.079 Uiso 1 1 calc R . . C27 C 0.6915(3) 0.6395(3) 0.8271(3) 0.0334(9) Uani 1 1 d . . . H27A H 0.6424 0.6693 0.7935 0.040 Uiso 1 1 calc R . . H27B H 0.7458 0.6744 0.8163 0.040 Uiso 1 1 calc R . . C28 C 0.6226(4) 0.6516(3) 0.9209(3) 0.0483(12) Uani 1 1 d . . . H28A H 0.5832 0.7214 0.9368 0.072 Uiso 1 1 calc R . . H28B H 0.6714 0.6241 0.9544 0.072 Uiso 1 1 calc R . . H28C H 0.5689 0.6169 0.9317 0.072 Uiso 1 1 calc R . . C29 C 0.3409(3) 0.5484(3) 0.8233(3) 0.0427(11) Uani 1 1 d . . . H29A H 0.2761 0.5515 0.8075 0.051 Uiso 1 1 calc R . . H29B H 0.3723 0.5979 0.7914 0.051 Uiso 1 1 calc R . . C30 C 0.3031(4) 0.5737(3) 0.9172(3) 0.0613(14) Uani 1 1 d . . . H30A H 0.2516 0.6411 0.9295 0.092 Uiso 1 1 calc R . . H30B H 0.3675 0.5677 0.9338 0.092 Uiso 1 1 calc R . . H30C H 0.2659 0.5284 0.9490 0.092 Uiso 1 1 calc R . . C31 C 0.3012(3) 0.3441(3) 0.8142(3) 0.0464(12) Uani 1 1 d . . . H31A H 0.3071 0.2779 0.8360 0.056 Uiso 1 1 calc R . . H31B H 0.2422 0.3926 0.8581 0.056 Uiso 1 1 calc R . . C32 C 0.2699(4) 0.3524(3) 0.7359(3) 0.0577(14) Uani 1 1 d . . . H32A H 0.1977 0.3435 0.7497 0.086 Uiso 1 1 calc R . . H32B H 0.3258 0.3018 0.6935 0.086 Uiso 1 1 calc R . . H32C H 0.2656 0.4174 0.7134 0.086 Uiso 1 1 calc R . . C33 C 0.5650(3) -0.0108(3) 0.6804(2) 0.0331(9) Uani 1 1 d . . . H33A H 0.5082 0.0078 0.7370 0.040 Uiso 1 1 calc R . . H33B H 0.5961 -0.0833 0.6751 0.040 Uiso 1 1 calc R . . C34 C 0.5102(3) 0.0254(3) 0.6137(3) 0.0455(11) Uani 1 1 d . . . H34A H 0.4491 -0.0001 0.6234 0.068 Uiso 1 1 calc R . . H34B H 0.5646 0.0025 0.5576 0.068 Uiso 1 1 calc R . . H34C H 0.4815 0.0973 0.6172 0.068 Uiso 1 1 calc R . . C35 C 0.8168(3) -0.1078(3) 0.5803(3) 0.0352(10) Uani 1 1 d . . . H35A H 0.8775 -0.1052 0.5282 0.042 Uiso 1 1 calc R . . H35B H 0.7601 -0.1220 0.5634 0.042 Uiso 1 1 calc R . . C36 C 0.8623(4) -0.1906(3) 0.6326(3) 0.0483(12) Uani 1 1 d . . . H36A H 0.8866 -0.2536 0.6019 0.072 Uiso 1 1 calc R . . H36B H 0.8044 -0.1898 0.6866 0.072 Uiso 1 1 calc R . . H36C H 0.9253 -0.1816 0.6431 0.072 Uiso 1 1 calc R . . C37 C 1.0113(3) -0.0222(3) 0.5399(2) 0.0297(9) Uani 1 1 d . . . H37A H 1.0031 -0.0880 0.5459 0.036 Uiso 1 1 calc R . . H37B H 1.0884 -0.0300 0.5350 0.036 Uiso 1 1 calc R . . C38 C 0.7922(3) 0.1331(3) 0.8652(2) 0.0314(9) Uani 1 1 d . . . H38A H 0.8445 0.0793 0.8282 0.038 Uiso 1 1 calc R . . C39 C 0.6860(3) 0.2230(3) 0.9812(2) 0.0332(9) Uani 1 1 d . . . H39A H 0.6505 0.2443 1.0390 0.040 Uiso 1 1 calc R . . C40 C 0.6688(3) 0.2736(3) 0.9140(2) 0.0313(9) Uani 1 1 d . . . H40A H 0.6183 0.3381 0.9168 0.038 Uiso 1 1 calc R . . C41 C 0.8121(4) 0.0545(3) 0.9984(3) 0.0495(12) Uani 1 1 d . . . H41A H 0.8687 0.0000 0.9603 0.074 Uiso 1 1 calc R . . H41B H 0.7530 0.0316 1.0360 0.074 Uiso 1 1 calc R . . H41C H 0.8455 0.0788 1.0321 0.074 Uiso 1 1 calc R . . C42 C 0.7390(3) 0.2810(3) 0.5563(3) 0.0345(9) Uani 1 1 d . . . H42A H 0.6826 0.2519 0.5702 0.041 Uiso 1 1 calc R . . C43 C 0.8579(4) 0.3488(3) 0.4848(3) 0.0450(11) Uani 1 1 d . . . H43A H 0.9019 0.3770 0.4404 0.054 Uiso 1 1 calc R . . C44 C 0.8617(4) 0.3369(3) 0.5642(3) 0.0430(11) Uani 1 1 d . . . H44A H 0.9097 0.3553 0.5850 0.052 Uiso 1 1 calc R . . C45 C 0.7447(4) 0.3146(3) 0.4065(3) 0.0504(12) Uani 1 1 d . . . H45A H 0.6915 0.2793 0.4184 0.076 Uiso 1 1 calc R . . H45B H 0.8092 0.2828 0.3574 0.076 Uiso 1 1 calc R . . H45C H 0.7098 0.3827 0.3946 0.076 Uiso 1 1 calc R . . Cl1 Cl 0.63401(8) 0.19200(7) 0.22864(6) 0.0375(3) Uani 1 1 d . . . O1 O 0.7429(2) 0.1889(2) 0.1750(2) 0.0596(9) Uani 1 1 d . . . O2 O 0.5555(2) 0.24957(19) 0.19046(17) 0.0402(7) Uani 1 1 d . . . O3 O 0.6122(3) 0.2356(3) 0.3072(2) 0.0947(15) Uani 1 1 d . . . O4 O 0.6320(3) 0.0961(2) 0.2356(3) 0.0852(13) Uani 1 1 d . . . C1S C 0.9871(3) 0.1943(4) 0.1505(4) 0.093(2) Uani 1 1 d G . . H1SA H 0.9116 0.1989 0.1750 0.112 Uiso 1 1 calc R . . C2S C 1.0644(5) 0.1367(3) 0.1864(2) 0.0828(19) Uani 1 1 d G . . H2SA H 1.0416 0.1019 0.2353 0.099 Uiso 1 1 calc R . . C3S C 1.1749(4) 0.1301(3) 0.1506(3) 0.085(2) Uani 1 1 d G . . H3SA H 1.2277 0.0907 0.1751 0.102 Uiso 1 1 calc R . . C4S C 1.2082(3) 0.1811(4) 0.0791(3) 0.094(3) Uani 1 1 d G . . H4SA H 1.2837 0.1765 0.0546 0.113 Uiso 1 1 calc R . . C5S C 1.1309(6) 0.2387(3) 0.0432(2) 0.103(3) Uani 1 1 d G . . H5SA H 1.1536 0.2735 -0.0057 0.124 Uiso 1 1 calc R . . C6S C 1.0204(5) 0.2453(3) 0.0790(4) 0.104(3) Uani 1 1 d G . . H6SA H 0.9676 0.2847 0.0545 0.125 Uiso 1 1 calc R . . C7S C 0.3315(4) 0.3165(4) 0.4019(3) 0.0562(13) Uani 1 1 d . . . H7SA H 0.3841 0.3168 0.3479 0.067 Uiso 1 1 calc R . . C8S C 0.2290(4) 0.3879(4) 0.4250(3) 0.0589(13) Uani 1 1 d . . . H8SA H 0.2114 0.4380 0.3875 0.071 Uiso 1 1 calc R . . C9S C 0.1514(4) 0.3865(4) 0.5033(3) 0.0628(14) Uani 1 1 d . . . H9SA H 0.0806 0.4358 0.5199 0.075 Uiso 1 1 calc R . . C10S C 0.1774(4) 0.3139(4) 0.5565(3) 0.0539(13) Uani 1 1 d . . . H10B H 0.1240 0.3122 0.6097 0.065 Uiso 1 1 calc R . . C11S C 0.2823(5) 0.2417(4) 0.5332(3) 0.0579(13) Uani 1 1 d . . . H11A H 0.2999 0.1916 0.5707 0.069 Uiso 1 1 calc R . . C12S C 0.3589(4) 0.2437(4) 0.4566(3) 0.0563(13) Uani 1 1 d . . . H12A H 0.4306 0.1957 0.4408 0.068 Uiso 1 1 calc R . . C13S C 0.4378(4) 0.4383(3) 0.5154(3) 0.0517(12) Uani 1 1 d . . . H13A H 0.3943 0.3964 0.5266 0.062 Uiso 1 1 calc R . . C14S C 0.4874(4) 0.4486(3) 0.5730(3) 0.0475(11) Uani 1 1 d . . . H14A H 0.4794 0.4124 0.6228 0.057 Uiso 1 1 calc R . . C15S C 0.5481(4) 0.5114(3) 0.5576(3) 0.0505(12) Uani 1 1 d . . . H15B H 0.5803 0.5199 0.5975 0.061 Uiso 1 1 calc R . . C16S C 0.5210(4) 0.0627(3) 1.0456(3) 0.0512(12) Uani 1 1 d . . . H16A H 0.5362 0.1047 1.0774 0.061 Uiso 1 1 calc R . . C17S C 0.5292(4) 0.0793(3) 0.9635(3) 0.0453(11) Uani 1 1 d . . . H17A H 0.5483 0.1343 0.9377 0.054 Uiso 1 1 calc R . . C18S C 0.5098(4) 0.0163(3) 0.9179(3) 0.0548(13) Uani 1 1 d . . . H18A H 0.5178 0.0272 0.8601 0.066 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 0.0196(3) 0.0170(3) 0.0302(3) -0.0041(2) -0.0054(2) -0.0014(2) N1 0.0213(16) 0.0193(15) 0.0282(17) -0.0048(12) -0.0048(13) -0.0016(13) N2 0.0203(15) 0.0186(15) 0.0308(18) -0.0040(13) -0.0060(13) -0.0028(12) N3 0.0219(16) 0.0192(15) 0.0307(18) -0.0054(13) -0.0041(13) -0.0035(13) N4 0.0219(16) 0.0184(15) 0.0294(17) -0.0034(12) -0.0081(13) -0.0014(12) N5 0.0207(15) 0.0197(16) 0.0310(18) -0.0049(13) -0.0034(13) -0.0031(13) N6 0.0380(19) 0.0272(18) 0.034(2) 0.0019(14) -0.0112(16) -0.0041(15) N7 0.0236(16) 0.0184(15) 0.0326(18) -0.0029(13) -0.0093(14) -0.0006(13) N8 0.042(2) 0.0302(18) 0.0290(19) 0.0007(14) -0.0124(16) -0.0023(16) C1 0.0209(18) 0.0213(19) 0.026(2) -0.0036(15) -0.0052(15) -0.0008(15) C2 0.0220(19) 0.0202(18) 0.031(2) -0.0032(15) -0.0058(16) -0.0009(15) C3 0.0236(19) 0.0229(19) 0.032(2) -0.0016(16) -0.0083(17) -0.0021(16) C4 0.0199(18) 0.0231(19) 0.031(2) -0.0022(15) -0.0056(16) -0.0026(15) C5 0.0234(19) 0.0256(19) 0.033(2) -0.0044(16) -0.0099(16) -0.0066(16) C6 0.0237(19) 0.0178(18) 0.033(2) -0.0029(15) -0.0065(16) -0.0033(15) C7 0.026(2) 0.0224(19) 0.032(2) -0.0065(16) -0.0051(17) -0.0059(16) C8 0.029(2) 0.023(2) 0.038(2) -0.0040(16) -0.0104(18) -0.0075(16) C9 0.0249(19) 0.0183(18) 0.028(2) -0.0032(15) -0.0053(16) -0.0036(15) C10 0.0237(19) 0.0161(18) 0.033(2) -0.0003(15) -0.0064(16) 0.0010(15) C11 0.025(2) 0.0196(19) 0.034(2) -0.0018(16) -0.0073(17) -0.0008(16) C12 0.0186(19) 0.026(2) 0.043(2) -0.0078(17) -0.0070(17) -0.0022(16) C13 0.0195(19) 0.027(2) 0.048(3) -0.0087(18) -0.0039(18) -0.0028(16) C14 0.0173(18) 0.0244(19) 0.036(2) -0.0064(16) -0.0034(16) -0.0013(15) C15 0.0229(19) 0.0222(19) 0.040(2) -0.0026(16) -0.0070(17) -0.0071(16) C16 0.0220(19) 0.0224(19) 0.033(2) -0.0030(16) -0.0051(16) -0.0049(15) C17 0.027(2) 0.0224(19) 0.031(2) -0.0048(15) -0.0068(17) -0.0040(16) C18 0.027(2) 0.0212(19) 0.032(2) -0.0023(15) -0.0111(17) -0.0048(16) C19 0.0234(19) 0.0189(18) 0.031(2) -0.0015(15) -0.0106(16) 0.0003(15) C20 0.0210(18) 0.0187(18) 0.030(2) -0.0029(15) -0.0077(16) 0.0016(15) C21 0.025(2) 0.025(2) 0.032(2) -0.0057(16) -0.0095(17) 0.0023(16) C22 0.027(2) 0.033(2) 0.045(3) -0.0067(18) -0.0123(19) 0.0002(18) C23 0.029(2) 0.0219(19) 0.043(2) -0.0042(17) -0.0158(18) -0.0010(16) C24 0.054(3) 0.044(3) 0.050(3) -0.002(2) -0.030(2) -0.001(2) C25 0.030(2) 0.028(2) 0.050(3) -0.0100(18) -0.015(2) -0.0021(17) C26 0.039(3) 0.046(3) 0.076(4) -0.001(2) -0.015(2) -0.019(2) C27 0.028(2) 0.0180(19) 0.051(3) -0.0064(17) -0.0134(19) -0.0030(16) C28 0.040(3) 0.036(2) 0.055(3) -0.023(2) -0.008(2) 0.001(2) C29 0.024(2) 0.023(2) 0.072(3) -0.012(2) -0.011(2) 0.0003(17) C30 0.048(3) 0.035(3) 0.078(4) -0.020(2) -0.004(3) 0.002(2) C31 0.024(2) 0.026(2) 0.074(3) -0.015(2) -0.003(2) 0.0002(18) C32 0.033(3) 0.044(3) 0.096(4) -0.012(3) -0.020(3) -0.011(2) C33 0.026(2) 0.026(2) 0.040(2) -0.0088(17) -0.0037(18) -0.0047(16) C34 0.034(2) 0.054(3) 0.054(3) -0.003(2) -0.018(2) -0.017(2) C35 0.028(2) 0.029(2) 0.042(3) -0.0104(18) -0.0050(18) -0.0065(17) C36 0.051(3) 0.026(2) 0.056(3) -0.006(2) -0.011(2) -0.004(2) C37 0.0219(19) 0.026(2) 0.034(2) -0.0095(16) -0.0071(17) 0.0005(16) C38 0.034(2) 0.023(2) 0.028(2) -0.0043(16) -0.0046(17) -0.0023(17) C39 0.041(2) 0.027(2) 0.028(2) -0.0061(16) -0.0084(18) -0.0070(18) C40 0.025(2) 0.024(2) 0.033(2) -0.0073(17) -0.0023(17) -0.0006(16) C41 0.061(3) 0.036(2) 0.038(3) 0.005(2) -0.015(2) -0.002(2) C42 0.033(2) 0.030(2) 0.037(2) -0.0006(18) -0.0107(19) -0.0063(18) C43 0.040(3) 0.050(3) 0.038(3) 0.007(2) -0.005(2) -0.015(2) C44 0.043(3) 0.051(3) 0.042(3) 0.015(2) -0.015(2) -0.025(2) C45 0.072(3) 0.040(3) 0.040(3) 0.004(2) -0.028(2) -0.011(2) Cl1 0.0307(5) 0.0320(5) 0.0432(6) 0.0033(4) -0.0130(5) -0.0015(4) O1 0.0311(17) 0.067(2) 0.076(2) 0.0058(18) -0.0118(16) -0.0169(16) O2 0.0352(16) 0.0341(16) 0.0432(17) -0.0001(13) -0.0165(13) 0.0023(13) O3 0.085(3) 0.120(4) 0.046(2) -0.024(2) -0.032(2) 0.024(3) O4 0.053(2) 0.039(2) 0.170(4) 0.042(2) -0.047(3) -0.0215(17) C1S 0.044(3) 0.117(6) 0.116(6) -0.072(5) -0.005(4) -0.028(4) C2S 0.095(5) 0.068(4) 0.071(4) -0.026(3) 0.006(4) -0.038(4) C3S 0.065(4) 0.082(5) 0.093(5) -0.048(4) -0.021(4) 0.002(3) C4S 0.063(4) 0.108(6) 0.104(6) -0.066(5) 0.020(4) -0.051(4) C5S 0.151(8) 0.072(5) 0.067(4) -0.018(4) 0.002(5) -0.047(5) C6S 0.120(7) 0.084(5) 0.096(6) -0.030(4) -0.062(5) 0.014(5) C7S 0.063(3) 0.059(3) 0.052(3) -0.008(3) -0.013(3) -0.030(3) C8S 0.067(4) 0.064(3) 0.045(3) 0.008(2) -0.013(3) -0.027(3) C9S 0.057(3) 0.059(3) 0.064(4) -0.008(3) -0.009(3) -0.019(3) C10S 0.060(3) 0.052(3) 0.048(3) -0.004(2) -0.008(3) -0.025(3) C11S 0.079(4) 0.051(3) 0.052(3) -0.004(2) -0.019(3) -0.033(3) C12S 0.055(3) 0.046(3) 0.073(4) -0.013(3) -0.021(3) -0.020(2) C13S 0.061(3) 0.042(3) 0.058(3) -0.001(2) -0.019(3) -0.023(2) C14S 0.061(3) 0.037(3) 0.047(3) 0.003(2) -0.020(2) -0.017(2) C15S 0.061(3) 0.044(3) 0.053(3) -0.002(2) -0.026(3) -0.018(2) C16S 0.062(3) 0.045(3) 0.050(3) -0.007(2) -0.012(2) -0.028(2) C17S 0.050(3) 0.037(2) 0.046(3) 0.003(2) -0.007(2) -0.020(2) C18S 0.080(4) 0.048(3) 0.041(3) 0.007(2) -0.018(3) -0.029(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 N5 1.919(3) . ? Co1 N7 1.936(3) . ? Co1 N1 1.945(3) . ? Co1 N3 1.959(3) . ? Co1 N2 1.968(3) . ? Co1 N4 1.968(3) . ? N1 C4 1.363(4) . ? N1 C1 1.387(4) . ? N2 C9 1.368(4) . ? N2 C6 1.371(4) . ? N3 C14 1.370(5) . ? N3 C11 1.374(4) . ? N4 C16 1.365(4) . ? N4 C19 1.392(4) . ? N5 C38 1.328(4) . ? N5 C40 1.388(4) . ? N6 C38 1.329(5) . ? N6 C39 1.379(5) . ? N6 C41 1.468(5) . ? N7 C42 1.318(5) . ? N7 C44 1.371(5) . ? N8 C42 1.330(5) . ? N8 C43 1.346(5) . ? N8 C45 1.475(5) . ? C1 C20 1.399(5) . ? C1 C2 1.455(5) . ? C2 C3 1.365(5) . ? C2 C21 1.509(5) . ? C3 C4 1.444(5) . ? C3 C23 1.496(5) . ? C4 C5 1.392(5) . ? C5 C6 1.387(5) . ? C5 H5A 0.9500 . ? C6 C7 1.450(5) . ? C7 C8 1.355(5) . ? C7 C25 1.499(5) . ? C8 C9 1.452(5) . ? C8 C27 1.510(5) . ? C9 C10 1.389(5) . ? C10 C11 1.382(5) . ? C10 H10A 0.9500 . ? C11 C12 1.446(5) . ? C12 C13 1.348(5) . ? C12 C29 1.507(5) . ? C13 C14 1.453(5) . ? C13 C31 1.507(5) . ? C14 C15 1.380(5) . ? C15 C16 1.387(5) . ? C15 H15A 0.9500 . ? C16 C17 1.438(5) . ? C17 C18 1.364(5) . ? C17 C33 1.506(5) . ? C18 C19 1.449(5) . ? C18 C35 1.520(5) . ? C19 C20 1.397(5) . ? C20 C37 1.513(4) . ? C21 C22 1.524(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.518(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.528(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.529(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.519(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.501(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.520(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.522(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C37 1.530(7) 2_756 ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9500 . ? C39 C40 1.348(5) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9500 . ? C43 C44 1.352(6) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? Cl1 O4 1.395(3) . ? Cl1 O3 1.401(3) . ? Cl1 O2 1.427(3) . ? Cl1 O1 1.439(3) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S H1SA 0.9500 . ? C2S C3S 1.3900 . ? C2S H2SA 0.9500 . ? C3S C4S 1.3900 . ? C3S H3SA 0.9500 . ? C4S C5S 1.3900 . ? C4S H4SA 0.9500 . ? C5S C6S 1.3900 . ? C5S H5SA 0.9500 . ? C6S H6SA 0.9500 . ? C7S C8S 1.375(7) . ? C7S C12S 1.389(7) . ? C7S H7SA 0.9500 . ? C8S C9S 1.388(7) . ? C8S H8SA 0.9500 . ? C9S C10S 1.365(7) . ? C9S H9SA 0.9500 . ? C10S C11S 1.401(7) . ? C10S H10B 0.9500 . ? C11S C12S 1.364(7) . ? C11S H11A 0.9500 . ? C12S H12A 0.9500 . ? C13S C15S 1.373(6) 2_666 ? C13S C14S 1.396(6) . ? C13S H13A 0.9500 . ? C14S C15S 1.379(6) . ? C14S H14A 0.9500 . ? C15S C13S 1.373(6) 2_666 ? C15S H15B 0.9500 . ? C16S C17S 1.360(6) . ? C16S C18S 1.382(6) 2_657 ? C16S H16A 0.9500 . ? C17S C18S 1.375(6) . ? C17S H17A 0.9500 . ? C18S C16S 1.382(6) 2_657 ? C18S H18A 0.9500 . ? 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 N5 Co1 N7 178.37(12) . . ? N5 Co1 N1 88.27(12) . . ? N7 Co1 N1 90.14(12) . . ? N5 Co1 N3 89.74(12) . . ? N7 Co1 N3 91.84(12) . . ? N1 Co1 N3 178.00(12) . . ? N5 Co1 N2 88.45(12) . . ? N7 Co1 N2 91.17(12) . . ? N1 Co1 N2 90.54(12) . . ? N3 Co1 N2 89.20(12) . . ? N5 Co1 N4 91.11(12) . . ? N7 Co1 N4 89.25(12) . . ? N1 Co1 N4 88.90(12) . . ? N3 Co1 N4 91.34(12) . . ? N2 Co1 N4 179.30(12) . . ? C4 N1 C1 106.3(3) . . ? C4 N1 Co1 125.4(2) . . ? C1 N1 Co1 127.5(2) . . ? C9 N2 C6 105.5(3) . . ? C9 N2 Co1 127.9(2) . . ? C6 N2 Co1 126.4(2) . . ? C14 N3 C11 105.3(3) . . ? C14 N3 Co1 125.9(2) . . ? C11 N3 Co1 128.6(2) . . ? C16 N4 C19 106.4(3) . . ? C16 N4 Co1 125.6(2) . . ? C19 N4 Co1 127.6(2) . . ? C38 N5 C40 105.1(3) . . ? C38 N5 Co1 126.5(2) . . ? C40 N5 Co1 128.0(3) . . ? C38 N6 C39 107.9(3) . . ? C38 N6 C41 126.5(3) . . ? C39 N6 C41 125.6(3) . . ? C42 N7 C44 104.5(3) . . ? C42 N7 Co1 128.3(3) . . ? C44 N7 Co1 127.1(3) . . ? C42 N8 C43 106.7(3) . . ? C42 N8 C45 127.3(4) . . ? C43 N8 C45 126.0(4) . . ? N1 C1 C20 124.4(3) . . ? N1 C1 C2 109.3(3) . . ? C20 C1 C2 126.1(3) . . ? C3 C2 C1 106.9(3) . . ? C3 C2 C21 123.7(3) . . ? C1 C2 C21 128.5(3) . . ? C2 C3 C4 106.6(3) . . ? C2 C3 C23 128.7(3) . . ? C4 C3 C23 124.6(3) . . ? N1 C4 C5 124.6(3) . . ? N1 C4 C3 110.8(3) . . ? C5 C4 C3 124.3(3) . . ? C6 C5 C4 124.4(3) . . ? C6 C5 H5A 117.8 . . ? C4 C5 H5A 117.8 . . ? N2 C6 C5 124.0(3) . . ? N2 C6 C7 111.1(3) . . ? C5 C6 C7 124.9(3) . . ? C8 C7 C6 105.9(3) . . ? C8 C7 C25 127.6(3) . . ? C6 C7 C25 126.6(3) . . ? C7 C8 C9 107.2(3) . . ? C7 C8 C27 127.6(3) . . ? C9 C8 C27 125.0(3) . . ? N2 C9 C10 124.7(3) . . ? N2 C9 C8 110.3(3) . . ? C10 C9 C8 124.5(3) . . ? C11 C10 C9 123.8(3) . . ? C11 C10 H10A 118.1 . . ? C9 C10 H10A 118.1 . . ? N3 C11 C10 124.2(3) . . ? N3 C11 C12 110.6(3) . . ? C10 C11 C12 124.9(3) . . ? C13 C12 C11 106.8(3) . . ? C13 C12 C29 127.9(3) . . ? C11 C12 C29 125.2(3) . . ? C12 C13 C14 106.5(3) . . ? C12 C13 C31 127.9(3) . . ? C14 C13 C31 125.4(3) . . ? N3 C14 C15 124.8(3) . . ? N3 C14 C13 110.6(3) . . ? C15 C14 C13 124.3(3) . . ? C14 C15 C16 124.6(3) . . ? C14 C15 H15A 117.7 . . ? C16 C15 H15A 117.7 . . ? N4 C16 C15 125.4(3) . . ? N4 C16 C17 110.5(3) . . ? C15 C16 C17 123.6(3) . . ? C18 C17 C16 107.0(3) . . ? C18 C17 C33 128.1(3) . . ? C16 C17 C33 124.9(3) . . ? C17 C18 C19 107.0(3) . . ? C17 C18 C35 123.1(3) . . ? C19 C18 C35 129.7(3) . . ? N4 C19 C20 123.0(3) . . ? N4 C19 C18 109.1(3) . . ? C20 C19 C18 127.6(3) . . ? C19 C20 C1 121.6(3) . . ? C19 C20 C37 120.3(3) . . ? C1 C20 C37 117.9(3) . . ? C2 C21 C22 115.0(3) . . ? C2 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? C2 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 C24 112.6(3) . . ? C3 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C3 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 C25 C26 112.4(3) . . ? C7 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? C7 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C28 111.2(3) . . ? C8 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C8 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C12 C29 C30 112.5(4) . . ? C12 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? C12 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C13 111.9(4) . . ? C32 C31 H31A 109.2 . . ? C13 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? C13 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C17 C33 C34 113.0(3) . . ? C17 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? C17 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C18 C35 C36 112.5(3) . . ? C18 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? C18 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C20 C37 C37 110.8(3) . 2_756 ? C20 C37 H37A 109.5 . . ? C37 C37 H37A 109.5 2_756 . ? C20 C37 H37B 109.5 . . ? C37 C37 H37B 109.5 2_756 . ? H37A C37 H37B 108.1 . . ? N5 C38 N6 111.3(3) . . ? N5 C38 H38A 124.3 . . ? N6 C38 H38A 124.3 . . ? C40 C39 N6 105.9(3) . . ? C40 C39 H39A 127.1 . . ? N6 C39 H39A 127.1 . . ? C39 C40 N5 109.7(3) . . ? C39 C40 H40A 125.1 . . ? N5 C40 H40A 125.1 . . ? N6 C41 H41A 109.5 . . ? N6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N7 C42 N8 112.4(4) . . ? N7 C42 H42A 123.8 . . ? N8 C42 H42A 123.8 . . ? N8 C43 C44 107.2(4) . . ? N8 C43 H43A 126.4 . . ? C44 C43 H43A 126.4 . . ? C43 C44 N7 109.2(4) . . ? C43 C44 H44A 125.4 . . ? N7 C44 H44A 125.4 . . ? N8 C45 H45A 109.5 . . ? N8 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N8 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O4 Cl1 O3 111.9(3) . . ? O4 Cl1 O2 110.1(2) . . ? O3 Cl1 O2 109.8(2) . . ? O4 Cl1 O1 107.9(2) . . ? O3 Cl1 O1 108.5(3) . . ? O2 Cl1 O1 108.62(19) . . ? C2S C1S C6S 120.0 . . ? C2S C1S H1SA 120.0 . . ? C6S C1S H1SA 120.0 . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2SA 120.0 . . ? C1S C2S H2SA 120.0 . . ? C4S C3S C2S 120.0 . . ? C4S C3S H3SA 120.0 . . ? C2S C3S H3SA 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4SA 120.0 . . ? C3S C4S H4SA 120.0 . . ? C4S C5S C6S 120.0 . . ? C4S C5S H5SA 120.0 . . ? C6S C5S H5SA 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6SA 120.0 . . ? C1S C6S H6SA 120.0 . . ? C8S C7S C12S 120.8(5) . . ? C8S C7S H7SA 119.6 . . ? C12S C7S H7SA 119.6 . . ? C7S C8S C9S 119.6(5) . . ? C7S C8S H8SA 120.2 . . ? C9S C8S H8SA 120.2 . . ? C10S C9S C8S 119.7(5) . . ? C10S C9S H9SA 120.2 . . ? C8S C9S H9SA 120.2 . . ? C9S C10S C11S 120.6(5) . . ? C9S C10S H10B 119.7 . . ? C11S C10S H10B 119.7 . . ? C12S C11S C10S 119.8(5) . . ? C12S C11S H11A 120.1 . . ? C10S C11S H11A 120.1 . . ? C11S C12S C7S 119.5(5) . . ? C11S C12S H12A 120.2 . . ? C7S C12S H12A 120.2 . . ? C15S C13S C14S 120.1(4) 2_666 . ? C15S C13S H13A 120.0 2_666 . ? C14S C13S H13A 120.0 . . ? C15S C14S C13S 119.8(4) . . ? C15S C14S H14A 120.1 . . ? C13S C14S H14A 120.1 . . ? C13S C15S C14S 120.1(4) 2_666 . ? C13S C15S H15B 119.9 2_666 . ? C14S C15S H15B 119.9 . . ? C17S C16S C18S 118.9(4) . 2_657 ? C17S C16S H16A 120.6 . . ? C18S C16S H16A 120.6 2_657 . ? C16S C17S C18S 119.7(4) . . ? C16S C17S H17A 120.1 . . ? C18S C17S H17A 120.1 . . ? C17S C18S C16S 121.4(4) . 2_657 ? C17S C18S H18A 119.3 . . ? C16S C18S H18A 119.3 2_657 . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.692 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 940532' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_13janc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H116 Cl20 Co2 N12' _chemical_formula_weight 2312.91 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 24.574(4) _cell_length_b 11.2196(15) _cell_length_c 20.890(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.473(3) _cell_angle_gamma 90.00 _cell_volume 5395.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 27.8 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2388 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 0.9348 _exptl_absorpt_process_details 'SADABS 2.05 (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28550 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_unetI/netI 0.0882 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10027 _reflns_number_gt 6799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0868P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10027 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 0.20993(2) 0.09057(4) 0.58436(2) 0.01664(16) Uani 1 1 d . . . N1 N 0.15535(14) 0.0707(3) 0.63179(15) 0.0164(7) Uani 1 1 d . . . N2 N 0.24909(14) 0.2201(3) 0.64458(15) 0.0175(7) Uani 1 1 d . . . N3 N 0.26433(14) 0.1072(3) 0.53580(15) 0.0195(7) Uani 1 1 d . . . N4 N 0.17255(14) -0.0427(3) 0.52591(15) 0.0162(7) Uani 1 1 d . . . N5 N 0.26274(14) -0.0236(3) 0.64646(15) 0.0184(7) Uani 1 1 d . . . N6 N 0.15703(14) 0.2065(3) 0.52287(15) 0.0197(8) Uani 1 1 d . . . C1 C 0.10066(17) 0.0197(3) 0.60683(18) 0.0169(8) Uani 1 1 d . . . C1S C 0.4985(2) 0.0676(4) 0.8462(2) 0.0338(11) Uani 1 1 d . . . H1SA H 0.4917 0.0043 0.8120 0.041 Uiso 1 1 calc R . . C2 C 0.07309(17) 0.0305(3) 0.65768(18) 0.0177(8) Uani 1 1 d . . . C2S C 0.4501(2) -0.3279(5) 0.5868(3) 0.0441(13) Uani 1 1 d . . . H2SA H 0.4745 -0.2844 0.6274 0.053 Uiso 1 1 calc R . . C3 C 0.11191(17) 0.0883(3) 0.71258(18) 0.0168(8) Uani 1 1 d . . . C3S C 0.1189(2) 0.5823(4) 0.7101(2) 0.0304(11) Uani 1 1 d . . . H3SA H 0.0808 0.6035 0.7120 0.036 Uiso 1 1 calc R . . C4 C 0.16195(17) 0.1163(3) 0.69527(18) 0.0176(9) Uani 1 1 d . . . C5 C 0.20602(17) 0.1927(3) 0.73184(19) 0.0201(9) Uani 1 1 d . . . H5A H 0.2095 0.2094 0.7767 0.024 Uiso 1 1 calc R . . C6 C 0.24510(17) 0.2460(3) 0.70702(19) 0.0195(9) Uani 1 1 d . . . C7 C 0.28089(17) 0.3483(3) 0.73696(19) 0.0203(9) Uani 1 1 d . . . C8 C 0.30547(19) 0.3850(3) 0.6914(2) 0.0237(9) Uani 1 1 d . . . C9 C 0.28647(17) 0.3028(3) 0.6341(2) 0.0199(9) Uani 1 1 d . . . C10 C 0.30671(17) 0.2996(4) 0.5804(2) 0.0220(9) Uani 1 1 d . . . H10A H 0.3266 0.3659 0.5732 0.026 Uiso 1 1 calc R . . C11 C 0.29914(17) 0.2031(4) 0.53624(19) 0.0206(9) Uani 1 1 d . . . C12 C 0.33290(17) 0.1795(4) 0.49316(19) 0.0212(9) Uani 1 1 d . . . C13 C 0.32046(17) 0.0653(4) 0.4704(2) 0.0230(9) Uani 1 1 d . . . C14 C 0.27756(17) 0.0203(3) 0.49695(18) 0.0194(9) Uani 1 1 d . . . C15 C 0.25021(18) -0.0885(4) 0.48259(19) 0.0221(9) Uani 1 1 d . . . H15A H 0.2667 -0.1467 0.4634 0.027 Uiso 1 1 calc R . . C16 C 0.20021(17) -0.1179(3) 0.49457(18) 0.0182(9) Uani 1 1 d . . . C17 C 0.16436(17) -0.2207(3) 0.46797(19) 0.0189(9) Uani 1 1 d . . . C18 C 0.11293(17) -0.2032(3) 0.47829(18) 0.0170(8) Uani 1 1 d . . . C19 C 0.11867(17) -0.0908(3) 0.51545(18) 0.0163(8) Uani 1 1 d . . . C20 C 0.08000(17) -0.0449(3) 0.54525(18) 0.0174(8) Uani 1 1 d . . . C21 C 0.01860(17) -0.0263(3) 0.65945(19) 0.0203(9) Uani 1 1 d . . . H21A H -0.0122 -0.0142 0.6158 0.024 Uiso 1 1 calc R . . H21B H 0.0071 0.0122 0.6943 0.024 Uiso 1 1 calc R . . C22 C 0.02608(19) -0.1597(3) 0.6744(2) 0.0246(10) Uani 1 1 d . . . H22A H -0.0072 -0.1897 0.6832 0.037 Uiso 1 1 calc R . . H22B H 0.0604 -0.1729 0.7137 0.037 Uiso 1 1 calc R . . H22C H 0.0298 -0.2003 0.6357 0.037 Uiso 1 1 calc R . . C23 C 0.10524(18) 0.1153(4) 0.77932(19) 0.0226(9) Uani 1 1 d . . . H23A H 0.0651 0.1363 0.7713 0.027 Uiso 1 1 calc R . . H23B H 0.1291 0.1838 0.7998 0.027 Uiso 1 1 calc R . . C24 C 0.12241(19) 0.0111(4) 0.8292(2) 0.0270(10) Uani 1 1 d . . . H24A H 0.1189 0.0342 0.8719 0.041 Uiso 1 1 calc R . . H24B H 0.1619 -0.0112 0.8367 0.041 Uiso 1 1 calc R . . H24C H 0.0973 -0.0554 0.8106 0.041 Uiso 1 1 calc R . . C25 C 0.28619(19) 0.4031(4) 0.8046(2) 0.0263(10) Uani 1 1 d . . . H25A H 0.2477 0.4106 0.8072 0.032 Uiso 1 1 calc R . . H25B H 0.3022 0.4826 0.8069 0.032 Uiso 1 1 calc R . . C26 C 0.3242(2) 0.3319(4) 0.8660(2) 0.0351(11) Uani 1 1 d . . . H26A H 0.3232 0.3679 0.9072 0.053 Uiso 1 1 calc R . . H26B H 0.3635 0.3312 0.8666 0.053 Uiso 1 1 calc R . . H26C H 0.3100 0.2516 0.8629 0.053 Uiso 1 1 calc R . . C27 C 0.34611(19) 0.4877(4) 0.6979(2) 0.0298(10) Uani 1 1 d . . . H27A H 0.3315 0.5561 0.7152 0.036 Uiso 1 1 calc R . . H27B H 0.3461 0.5081 0.6528 0.036 Uiso 1 1 calc R . . C28 C 0.4076(2) 0.4647(5) 0.7438(3) 0.0503(14) Uani 1 1 d . . . H28A H 0.4299 0.5365 0.7487 0.075 Uiso 1 1 calc R . . H28B H 0.4242 0.4036 0.7243 0.075 Uiso 1 1 calc R . . H28C H 0.4080 0.4393 0.7879 0.075 Uiso 1 1 calc R . . C29 C 0.37411(19) 0.2646(4) 0.4800(2) 0.0277(10) Uani 1 1 d . . . H29A H 0.4033 0.2199 0.4687 0.033 Uiso 1 1 calc R . . H29B H 0.3938 0.3090 0.5215 0.033 Uiso 1 1 calc R . . C30 C 0.3453(2) 0.3519(5) 0.4227(3) 0.0498(14) Uani 1 1 d . . . H30A H 0.3745 0.4004 0.4147 0.075 Uiso 1 1 calc R . . H30B H 0.3190 0.4019 0.4353 0.075 Uiso 1 1 calc R . . H30C H 0.3243 0.3088 0.3818 0.075 Uiso 1 1 calc R . . C31 C 0.34351(18) -0.0011(4) 0.42323(19) 0.0237(9) Uani 1 1 d . . . H31A H 0.3495 -0.0839 0.4373 0.028 Uiso 1 1 calc R . . H31B H 0.3808 0.0322 0.4263 0.028 Uiso 1 1 calc R . . C32 C 0.3023(2) 0.0053(4) 0.3498(2) 0.0329(11) Uani 1 1 d . . . H32A H 0.3192 -0.0348 0.3207 0.049 Uiso 1 1 calc R . . H32B H 0.2953 0.0873 0.3361 0.049 Uiso 1 1 calc R . . H32C H 0.2662 -0.0324 0.3460 0.049 Uiso 1 1 calc R . . C33 C 0.18239(19) -0.3286(4) 0.4385(2) 0.0254(10) Uani 1 1 d . . . H33A H 0.2052 -0.3040 0.4112 0.030 Uiso 1 1 calc R . . H33B H 0.1480 -0.3691 0.4086 0.030 Uiso 1 1 calc R . . C34 C 0.2182(2) -0.4158(4) 0.4939(2) 0.0376(12) Uani 1 1 d . . . H34A H 0.2269 -0.4856 0.4727 0.056 Uiso 1 1 calc R . . H34B H 0.1964 -0.4381 0.5222 0.056 Uiso 1 1 calc R . . H34C H 0.2538 -0.3781 0.5214 0.056 Uiso 1 1 calc R . . C35 C 0.06500(17) -0.2936(3) 0.46122(19) 0.0209(9) Uani 1 1 d . . . H35A H 0.0417 -0.2783 0.4895 0.025 Uiso 1 1 calc R . . H35B H 0.0822 -0.3720 0.4731 0.025 Uiso 1 1 calc R . . C36 C 0.02453(19) -0.2954(4) 0.3859(2) 0.0266(10) Uani 1 1 d . . . H36A H -0.0041 -0.3569 0.3794 0.040 Uiso 1 1 calc R . . H36B H 0.0469 -0.3108 0.3573 0.040 Uiso 1 1 calc R . . H36C H 0.0055 -0.2196 0.3741 0.040 Uiso 1 1 calc R . . C37 C 0.01521(16) -0.0613(3) 0.50945(19) 0.0175(9) Uani 1 1 d . . . H37A H -0.0008 -0.1041 0.5392 0.021 Uiso 1 1 calc R . . H37B H 0.0081 -0.1082 0.4683 0.021 Uiso 1 1 calc R . . C38 C 0.24391(19) -0.1265(3) 0.6643(2) 0.0221(9) Uani 1 1 d . . . H38A H 0.2041 -0.1403 0.6499 0.027 Uiso 1 1 calc R . . C39 C 0.28099(19) -0.2120(4) 0.7028(2) 0.0283(10) Uani 1 1 d . . . H39A H 0.2664 -0.2816 0.7148 0.034 Uiso 1 1 calc R . . C40 C 0.34015(19) -0.1935(4) 0.7235(2) 0.0283(10) Uani 1 1 d . . . H40A H 0.3660 -0.2510 0.7488 0.034 Uiso 1 1 calc R . . C41 C 0.36022(19) -0.0879(4) 0.7060(2) 0.0255(10) Uani 1 1 d . . . H41A H 0.3998 -0.0729 0.7192 0.031 Uiso 1 1 calc R . . C42 C 0.32038(17) -0.0053(3) 0.66856(19) 0.0201(9) Uani 1 1 d . . . H42A H 0.3340 0.0667 0.6580 0.024 Uiso 1 1 calc R . . C43 C 0.14816(18) 0.2090(4) 0.45529(19) 0.0230(9) Uani 1 1 d . . . H43A H 0.1687 0.1560 0.4381 0.028 Uiso 1 1 calc R . . C44 C 0.11010(19) 0.2865(4) 0.4111(2) 0.0272(10) Uani 1 1 d . . . H44A H 0.1047 0.2845 0.3648 0.033 Uiso 1 1 calc R . . C45 C 0.08008(19) 0.3664(4) 0.4352(2) 0.0274(10) Uani 1 1 d . . . H45A H 0.0543 0.4198 0.4059 0.033 Uiso 1 1 calc R . . C46 C 0.08905(19) 0.3660(4) 0.5045(2) 0.0249(10) Uani 1 1 d . . . H46A H 0.0692 0.4193 0.5225 0.030 Uiso 1 1 calc R . . C47 C 0.12762(18) 0.2856(3) 0.5464(2) 0.0207(9) Uani 1 1 d . . . H47A H 0.1335 0.2863 0.5928 0.025 Uiso 1 1 calc R . . Cl1S Cl 0.45621(7) -0.48261(14) 0.60412(8) 0.0659(4) Uani 1 1 d . . . Cl1 Cl 0.0000 0.56768(13) 0.7500 0.0272(3) Uani 1 2 d S . . Cl2 Cl 0.5000 -0.19295(14) 0.7500 0.0301(4) Uani 1 2 d S . . Cl2S Cl 0.47339(8) -0.29488(15) 0.51745(9) 0.0717(5) Uani 1 1 d . . . Cl3S Cl 0.37785(6) -0.28247(14) 0.56589(7) 0.0553(4) Uani 1 1 d . . . Cl4S Cl 0.55285(5) 0.16303(12) 0.83973(6) 0.0443(3) Uani 1 1 d . . . Cl5S Cl 0.52065(7) 0.00246(13) 0.92834(7) 0.0573(4) Uani 1 1 d . . . Cl6S Cl 0.43361(5) 0.14697(12) 0.83142(7) 0.0449(3) Uani 1 1 d . . . Cl7S Cl 0.12750(6) 0.42669(11) 0.71647(6) 0.0435(3) Uani 1 1 d . . . Cl8S Cl 0.12319(6) 0.63161(12) 0.63181(6) 0.0495(4) Uani 1 1 d . . . Cl9S Cl 0.17375(5) 0.65358(11) 0.77817(6) 0.0413(3) 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 0.0140(3) 0.0204(3) 0.0155(3) -0.0006(2) 0.0052(2) -0.0008(2) N1 0.0157(18) 0.0191(17) 0.0150(16) 0.0003(13) 0.0060(14) -0.0019(14) N2 0.0146(18) 0.0196(17) 0.0164(17) -0.0011(13) 0.0030(14) -0.0014(15) N3 0.0163(18) 0.0248(19) 0.0171(17) -0.0011(14) 0.0056(14) -0.0013(15) N4 0.0165(18) 0.0187(17) 0.0143(16) -0.0019(13) 0.0063(14) -0.0007(15) N5 0.0141(18) 0.0222(18) 0.0193(17) -0.0033(14) 0.0065(14) -0.0008(15) N6 0.0213(19) 0.0219(18) 0.0170(17) -0.0013(13) 0.0080(14) -0.0036(15) C1 0.018(2) 0.016(2) 0.0166(19) 0.0008(15) 0.0053(16) 0.0020(17) C1S 0.030(3) 0.039(3) 0.034(3) -0.002(2) 0.012(2) 0.001(2) C2 0.020(2) 0.019(2) 0.0156(19) 0.0012(15) 0.0078(17) 0.0043(18) C2S 0.034(3) 0.054(3) 0.046(3) -0.014(2) 0.016(2) -0.005(3) C3 0.017(2) 0.018(2) 0.0146(19) 0.0012(15) 0.0048(16) -0.0003(17) C3S 0.028(3) 0.032(3) 0.028(2) -0.0041(19) 0.007(2) 0.003(2) C4 0.021(2) 0.017(2) 0.015(2) 0.0022(15) 0.0063(17) 0.0020(17) C5 0.017(2) 0.028(2) 0.014(2) -0.0015(16) 0.0042(17) 0.0021(18) C6 0.016(2) 0.024(2) 0.017(2) -0.0044(16) 0.0039(17) 0.0001(18) C7 0.014(2) 0.022(2) 0.022(2) -0.0006(17) 0.0030(17) 0.0009(18) C8 0.023(2) 0.018(2) 0.030(2) 0.0001(17) 0.0092(19) -0.0004(18) C9 0.017(2) 0.015(2) 0.027(2) 0.0017(16) 0.0063(18) -0.0007(17) C10 0.016(2) 0.021(2) 0.028(2) 0.0057(17) 0.0066(18) 0.0003(18) C11 0.017(2) 0.025(2) 0.019(2) 0.0069(17) 0.0051(17) 0.0023(18) C12 0.016(2) 0.027(2) 0.020(2) 0.0055(17) 0.0059(17) 0.0009(18) C13 0.014(2) 0.033(2) 0.019(2) 0.0015(17) 0.0028(17) -0.0005(19) C14 0.017(2) 0.025(2) 0.015(2) -0.0002(16) 0.0030(17) 0.0011(18) C15 0.020(2) 0.028(2) 0.020(2) 0.0005(17) 0.0102(18) 0.0054(19) C16 0.017(2) 0.023(2) 0.0143(19) 0.0015(16) 0.0053(17) 0.0030(18) C17 0.019(2) 0.021(2) 0.016(2) 0.0000(16) 0.0062(17) 0.0000(18) C18 0.017(2) 0.018(2) 0.0166(19) -0.0001(15) 0.0065(17) -0.0024(17) C19 0.012(2) 0.018(2) 0.017(2) 0.0016(15) 0.0036(16) -0.0003(17) C20 0.020(2) 0.016(2) 0.0151(19) 0.0032(15) 0.0047(17) -0.0008(17) C21 0.019(2) 0.026(2) 0.018(2) -0.0046(16) 0.0080(17) -0.0002(18) C22 0.029(3) 0.026(2) 0.020(2) -0.0031(17) 0.0113(19) -0.003(2) C23 0.019(2) 0.034(2) 0.017(2) -0.0044(17) 0.0081(17) -0.0059(19) C24 0.027(3) 0.038(3) 0.019(2) -0.0004(18) 0.0113(19) -0.001(2) C25 0.025(2) 0.026(2) 0.028(2) -0.0079(18) 0.0099(19) -0.003(2) C26 0.039(3) 0.035(3) 0.029(2) -0.007(2) 0.010(2) 0.002(2) C27 0.029(3) 0.025(2) 0.039(3) -0.0060(19) 0.016(2) -0.006(2) C28 0.034(3) 0.055(3) 0.054(3) -0.001(3) 0.004(3) -0.019(3) C29 0.027(3) 0.034(3) 0.027(2) 0.0032(19) 0.016(2) 0.000(2) C30 0.042(3) 0.048(3) 0.062(4) 0.029(3) 0.021(3) 0.006(3) C31 0.023(2) 0.029(2) 0.022(2) -0.0003(17) 0.0122(18) 0.0000(19) C32 0.037(3) 0.036(3) 0.030(2) -0.004(2) 0.017(2) 0.004(2) C33 0.023(2) 0.024(2) 0.033(2) -0.0075(18) 0.0128(19) -0.0049(19) C34 0.032(3) 0.028(3) 0.051(3) -0.005(2) 0.012(2) 0.005(2) C35 0.019(2) 0.020(2) 0.025(2) -0.0044(17) 0.0087(18) -0.0011(18) C36 0.024(2) 0.024(2) 0.031(2) -0.0060(18) 0.0069(19) -0.001(2) C37 0.016(2) 0.020(2) 0.0157(19) -0.0005(15) 0.0054(17) -0.0016(17) C38 0.019(2) 0.023(2) 0.022(2) -0.0016(17) 0.0045(18) -0.0035(19) C39 0.026(3) 0.023(2) 0.035(2) 0.0024(19) 0.009(2) -0.005(2) C40 0.024(3) 0.025(2) 0.028(2) 0.0018(18) -0.0010(19) 0.004(2) C41 0.017(2) 0.027(2) 0.030(2) -0.0057(18) 0.0049(19) -0.0029(19) C42 0.020(2) 0.018(2) 0.022(2) -0.0040(16) 0.0073(18) -0.0042(18) C43 0.022(2) 0.028(2) 0.020(2) -0.0028(17) 0.0083(18) -0.0022(19) C44 0.031(3) 0.030(2) 0.019(2) 0.0013(18) 0.0068(19) -0.001(2) C45 0.023(2) 0.023(2) 0.028(2) 0.0057(18) -0.0007(19) 0.001(2) C46 0.026(2) 0.022(2) 0.029(2) -0.0018(18) 0.0109(19) -0.0001(19) C47 0.024(2) 0.020(2) 0.021(2) -0.0001(16) 0.0111(18) 0.0005(18) Cl1S 0.0708(11) 0.0582(10) 0.0670(10) -0.0064(7) 0.0221(9) -0.0029(8) Cl1 0.0278(8) 0.0301(8) 0.0263(8) 0.000 0.0129(7) 0.000 Cl2 0.0184(8) 0.0360(9) 0.0327(8) 0.000 0.0051(6) 0.000 Cl2S 0.0702(11) 0.0817(11) 0.0848(11) -0.0160(9) 0.0542(10) -0.0218(9) Cl3S 0.0362(8) 0.0901(11) 0.0402(7) 0.0029(7) 0.0141(6) -0.0010(8) Cl4S 0.0284(7) 0.0626(9) 0.0434(7) -0.0029(6) 0.0143(6) -0.0076(6) Cl5S 0.0656(10) 0.0635(9) 0.0387(7) 0.0108(6) 0.0133(7) -0.0009(8) Cl6S 0.0298(7) 0.0554(8) 0.0547(8) -0.0029(6) 0.0213(6) 0.0041(6) Cl7S 0.0361(7) 0.0336(7) 0.0527(8) -0.0048(5) 0.0052(6) 0.0075(6) Cl8S 0.0577(9) 0.0612(9) 0.0345(7) -0.0005(6) 0.0224(6) 0.0093(7) Cl9S 0.0338(7) 0.0498(8) 0.0403(7) -0.0155(6) 0.0128(6) -0.0044(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.939(3) . ? Co1 N2 1.943(3) . ? Co1 N4 1.946(3) . ? Co1 N3 1.949(3) . ? Co1 N5 1.957(3) . ? Co1 N6 1.965(3) . ? N1 C4 1.377(5) . ? N1 C1 1.384(5) . ? N2 C6 1.373(5) . ? N2 C9 1.376(5) . ? N3 C11 1.373(5) . ? N3 C14 1.378(5) . ? N4 C19 1.375(5) . ? N4 C16 1.383(5) . ? N5 C42 1.343(5) . ? N5 C38 1.343(5) . ? N6 C47 1.342(5) . ? N6 C43 1.351(5) . ? C1 C20 1.407(5) . ? C1 C2 1.451(5) . ? C1S Cl4S 1.753(5) . ? C1S Cl6S 1.757(5) . ? C1S Cl5S 1.766(5) . ? C1S H1SA 0.9800 . ? C2 C3 1.371(5) . ? C2 C21 1.495(5) . ? C2S Cl3S 1.750(5) . ? C2S Cl1S 1.768(6) . ? C2S Cl2S 1.773(5) . ? C2S H2SA 0.9800 . ? C3 C4 1.433(5) . ? C3 C23 1.491(5) . ? C3S Cl7S 1.758(4) . ? C3S Cl8S 1.765(4) . ? C3S Cl9S 1.770(4) . ? C3S H3SA 0.9800 . ? C4 C5 1.383(5) . ? C5 C6 1.377(5) . ? C5 H5A 0.9300 . ? C6 C7 1.448(5) . ? C7 C8 1.358(6) . ? C7 C25 1.505(5) . ? C8 C9 1.452(5) . ? C8 C27 1.499(6) . ? C9 C10 1.378(6) . ? C10 C11 1.392(6) . ? C10 H10A 0.9300 . ? C11 C12 1.446(6) . ? C12 C13 1.364(6) . ? C12 C29 1.486(6) . ? C13 C14 1.443(6) . ? C13 C31 1.496(5) . ? C14 C15 1.375(5) . ? C15 C16 1.377(6) . ? C15 H15A 0.9300 . ? C16 C17 1.440(5) . ? C17 C18 1.368(5) . ? C17 C33 1.494(5) . ? C18 C19 1.462(5) . ? C18 C35 1.499(5) . ? C19 C20 1.404(5) . ? C20 C37 1.515(5) . ? C21 C22 1.526(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.525(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.522(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.502(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.516(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.517(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.535(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.540(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C37 1.549(7) 3_556 ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.373(6) . ? C38 H38A 0.9300 . ? C39 C40 1.380(6) . ? C39 H39A 0.9300 . ? C40 C41 1.381(6) . ? C40 H40A 0.9300 . ? C41 C42 1.375(6) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C44 1.370(6) . ? C43 H43A 0.9300 . ? C44 C45 1.365(6) . ? C44 H44A 0.9300 . ? C45 C46 1.386(6) . ? C45 H45A 0.9300 . ? C46 C47 1.377(6) . ? C46 H46A 0.9300 . ? C47 H47A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N2 91.70(13) . . ? N1 Co1 N4 88.47(13) . . ? N2 Co1 N4 178.16(14) . . ? N1 Co1 N3 178.78(13) . . ? N2 Co1 N3 89.47(13) . . ? N4 Co1 N3 90.35(13) . . ? N1 Co1 N5 90.16(13) . . ? N2 Co1 N5 89.83(13) . . ? N4 Co1 N5 88.34(13) . . ? N3 Co1 N5 89.50(13) . . ? N1 Co1 N6 89.57(13) . . ? N2 Co1 N6 89.58(13) . . ? N4 Co1 N6 92.25(13) . . ? N3 Co1 N6 90.79(13) . . ? N5 Co1 N6 179.35(13) . . ? C4 N1 C1 106.8(3) . . ? C4 N1 Co1 125.4(3) . . ? C1 N1 Co1 127.5(2) . . ? C6 N2 C9 106.4(3) . . ? C6 N2 Co1 126.1(3) . . ? C9 N2 Co1 127.5(3) . . ? C11 N3 C14 106.5(3) . . ? C11 N3 Co1 127.6(3) . . ? C14 N3 Co1 125.8(3) . . ? C19 N4 C16 106.9(3) . . ? C19 N4 Co1 128.2(3) . . ? C16 N4 Co1 124.3(3) . . ? C42 N5 C38 117.4(3) . . ? C42 N5 Co1 120.2(3) . . ? C38 N5 Co1 122.2(3) . . ? C47 N6 C43 117.2(3) . . ? C47 N6 Co1 121.1(3) . . ? C43 N6 Co1 121.6(3) . . ? N1 C1 C20 123.3(4) . . ? N1 C1 C2 109.3(3) . . ? C20 C1 C2 126.9(4) . . ? Cl4S C1S Cl6S 110.2(3) . . ? Cl4S C1S Cl5S 110.1(3) . . ? Cl6S C1S Cl5S 109.5(3) . . ? Cl4S C1S H1SA 109.0 . . ? Cl6S C1S H1SA 109.0 . . ? Cl5S C1S H1SA 109.0 . . ? C3 C2 C1 106.6(3) . . ? C3 C2 C21 123.2(3) . . ? C1 C2 C21 129.3(3) . . ? Cl3S C2S Cl1S 110.1(3) . . ? Cl3S C2S Cl2S 108.9(3) . . ? Cl1S C2S Cl2S 110.1(3) . . ? Cl3S C2S H2SA 109.3 . . ? Cl1S C2S H2SA 109.3 . . ? Cl2S C2S H2SA 109.3 . . ? C2 C3 C4 107.5(3) . . ? C2 C3 C23 127.3(4) . . ? C4 C3 C23 125.2(3) . . ? Cl7S C3S Cl8S 109.7(2) . . ? Cl7S C3S Cl9S 110.5(2) . . ? Cl8S C3S Cl9S 109.1(3) . . ? Cl7S C3S H3SA 109.2 . . ? Cl8S C3S H3SA 109.2 . . ? Cl9S C3S H3SA 109.2 . . ? N1 C4 C5 124.6(4) . . ? N1 C4 C3 109.8(3) . . ? C5 C4 C3 124.9(3) . . ? C6 C5 C4 125.1(4) . . ? C6 C5 H5A 117.4 . . ? C4 C5 H5A 117.4 . . ? N2 C6 C5 123.8(3) . . ? N2 C6 C7 110.1(3) . . ? C5 C6 C7 125.4(4) . . ? C8 C7 C6 106.8(3) . . ? C8 C7 C25 128.4(4) . . ? C6 C7 C25 124.7(4) . . ? C7 C8 C9 106.9(4) . . ? C7 C8 C27 128.0(4) . . ? C9 C8 C27 125.1(4) . . ? N2 C9 C10 124.3(4) . . ? N2 C9 C8 109.8(3) . . ? C10 C9 C8 125.7(4) . . ? C9 C10 C11 123.9(4) . . ? C9 C10 H10A 118.1 . . ? C11 C10 H10A 118.1 . . ? N3 C11 C10 123.6(4) . . ? N3 C11 C12 110.1(3) . . ? C10 C11 C12 125.6(4) . . ? C13 C12 C11 106.4(4) . . ? C13 C12 C29 128.6(4) . . ? C11 C12 C29 125.1(4) . . ? C12 C13 C14 107.4(4) . . ? C12 C13 C31 127.4(4) . . ? C14 C13 C31 125.1(4) . . ? C15 C14 N3 124.0(4) . . ? C15 C14 C13 126.4(4) . . ? N3 C14 C13 109.5(3) . . ? C14 C15 C16 124.9(4) . . ? C14 C15 H15A 117.6 . . ? C16 C15 H15A 117.6 . . ? C15 C16 N4 123.9(4) . . ? C15 C16 C17 125.9(4) . . ? N4 C16 C17 109.6(3) . . ? C18 C17 C16 107.4(3) . . ? C18 C17 C33 127.2(4) . . ? C16 C17 C33 125.4(4) . . ? C17 C18 C19 106.5(3) . . ? C17 C18 C35 123.9(3) . . ? C19 C18 C35 129.1(3) . . ? N4 C19 C20 123.3(3) . . ? N4 C19 C18 109.4(3) . . ? C20 C19 C18 126.7(4) . . ? C19 C20 C1 120.7(4) . . ? C19 C20 C37 119.6(3) . . ? C1 C20 C37 119.6(3) . . ? C2 C21 C22 112.2(3) . . ? C2 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C2 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 C24 112.9(3) . . ? C3 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? C3 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 C25 C26 113.7(3) . . ? C7 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? C7 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C28 114.5(4) . . ? C8 C27 H27A 108.6 . . ? C28 C27 H27A 108.6 . . ? C8 C27 H27B 108.6 . . ? C28 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C12 C29 C30 113.7(4) . . ? C12 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? C12 C29 H29B 108.8 . . ? C30 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C13 C31 C32 111.7(4) . . ? C13 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? C13 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C17 C33 C34 112.3(3) . . ? C17 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? C17 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C18 C35 C36 115.2(3) . . ? C18 C35 H35A 108.5 . . ? C36 C35 H35A 108.5 . . ? C18 C35 H35B 108.5 . . ? C36 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C20 C37 C37 110.4(4) . 3_556 ? C20 C37 H37A 109.6 . . ? C37 C37 H37A 109.6 3_556 . ? C20 C37 H37B 109.6 . . ? C37 C37 H37B 109.6 3_556 . ? H37A C37 H37B 108.1 . . ? N5 C38 C39 122.7(4) . . ? N5 C38 H38A 118.6 . . ? C39 C38 H38A 118.6 . . ? C38 C39 C40 119.3(4) . . ? C38 C39 H39A 120.4 . . ? C40 C39 H39A 120.4 . . ? C39 C40 C41 118.7(4) . . ? C39 C40 H40A 120.6 . . ? C41 C40 H40A 120.6 . . ? C42 C41 C40 118.6(4) . . ? C42 C41 H41A 120.7 . . ? C40 C41 H41A 120.7 . . ? N5 C42 C41 123.2(4) . . ? N5 C42 H42A 118.4 . . ? C41 C42 H42A 118.4 . . ? N6 C43 C44 122.6(4) . . ? N6 C43 H43A 118.7 . . ? C44 C43 H43A 118.7 . . ? C45 C44 C43 119.9(4) . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C44 C45 C46 118.3(4) . . ? C44 C45 H45A 120.9 . . ? C46 C45 H45A 120.9 . . ? C47 C46 C45 119.2(4) . . ? C47 C46 H46A 120.4 . . ? C45 C46 H46A 120.4 . . ? N6 C47 C46 122.7(4) . . ? N6 C47 H47A 118.6 . . ? C46 C47 H47A 118.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.983 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 940534' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_16decc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H114 Cl14 Co2 N18' _chemical_formula_weight 2158.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 22.991(3) _cell_length_b 13.454(2) _cell_length_c 18.836(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.454(2) _cell_angle_gamma 90.00 _cell_volume 5459.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9210 _exptl_absorpt_correction_T_max 0.9593 _exptl_absorpt_process_details 'SADABS 2.05 (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10101 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_unetI/netI 0.0799 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10101 _reflns_number_gt 6850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _refine_special_details ; The asymmetric unit also contains an uncoordinated pyrazine molecule with 50% occupancy. ISOR restraints were placed on atoms C4S and C5S belongs to the same uncoordinated pyrazine. The structure also contains solvent accessible voids of 240 cub. Ang per unit cell which can be correlated to a chloroform solvent molecule. 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^)+(0.1165P)^2^+5.7179P] 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 10101 _refine_ls_number_parameters 627 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2163 _refine_ls_wR_factor_gt 0.1897 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.033 _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 0.28841(3) 0.10096(5) 0.33126(4) 0.02237(19) Uani 1 1 d . . . N1 N 0.35318(18) 0.0293(3) 0.3087(2) 0.0249(9) Uani 1 1 d . . . N2 N 0.22499(18) 0.0209(3) 0.2574(2) 0.0232(9) Uani 1 1 d . . . N3 N 0.22294(18) 0.1747(3) 0.3513(2) 0.0239(9) Uani 1 1 d . . . N4 N 0.35231(18) 0.1803(3) 0.4054(2) 0.0235(9) Uani 1 1 d . . . N5 N 0.28648(18) 0.1980(3) 0.2527(2) 0.0255(9) Uani 1 1 d . . . N6 N 0.2852(2) 0.3315(3) 0.1382(3) 0.0377(11) Uani 1 1 d . . . N7 N 0.29132(18) 0.0066(3) 0.4112(2) 0.0232(9) Uani 1 1 d . . . N8 N 0.2980(2) -0.1271(3) 0.5271(2) 0.0338(10) Uani 1 1 d . . . C1 C 0.4156(2) 0.0221(4) 0.3522(3) 0.0276(11) Uani 1 1 d . . . C2 C 0.4466(2) -0.0404(4) 0.3134(3) 0.0331(12) Uani 1 1 d . . . C3 C 0.4033(2) -0.0638(4) 0.2445(3) 0.0315(12) Uani 1 1 d . . . C4 C 0.3454(2) -0.0241(4) 0.2439(3) 0.0280(11) Uani 1 1 d . . . C5 C 0.2884(2) -0.0506(4) 0.1901(3) 0.0281(11) Uani 1 1 d . . . H5A H 0.2879 -0.0796 0.1439 0.034 Uiso 1 1 calc R . . C6 C 0.2325(2) -0.0366(4) 0.2009(3) 0.0264(11) Uani 1 1 d . . . C7 C 0.1746(2) -0.0851(4) 0.1575(3) 0.0295(11) Uani 1 1 d . . . C8 C 0.1330(2) -0.0585(4) 0.1894(3) 0.0276(11) Uani 1 1 d . . . C9 C 0.1640(2) 0.0107(3) 0.2500(3) 0.0240(10) Uani 1 1 d . . . C10 C 0.1347(2) 0.0666(4) 0.2893(3) 0.0271(11) Uani 1 1 d . . . H10A H 0.0941 0.0479 0.2863 0.032 Uiso 1 1 calc R . . C11 C 0.1618(2) 0.1481(4) 0.3326(3) 0.0286(11) Uani 1 1 d . . . C12 C 0.1288(2) 0.2245(4) 0.3573(3) 0.0348(13) Uani 1 1 d . . . C13 C 0.1698(2) 0.2986(4) 0.3881(3) 0.0309(12) Uani 1 1 d . . . C14 C 0.2289(2) 0.2654(4) 0.3871(3) 0.0261(11) Uani 1 1 d . . . C15 C 0.2854(2) 0.3113(4) 0.4236(3) 0.0289(11) Uani 1 1 d . . . H15A H 0.2847 0.3772 0.4415 0.035 Uiso 1 1 calc R . . C16 C 0.3423(2) 0.2685(4) 0.4360(3) 0.0256(11) Uani 1 1 d . . . C17 C 0.4005(2) 0.3046(4) 0.4887(3) 0.0295(11) Uani 1 1 d . . . C18 C 0.4441(2) 0.2358(4) 0.4921(3) 0.0306(12) Uani 1 1 d . . . C19 C 0.4145(2) 0.1568(4) 0.4391(3) 0.0271(11) Uani 1 1 d . . . C20 C 0.4431(2) 0.0747(4) 0.4196(3) 0.0295(12) Uani 1 1 d . . . C21 C 0.5144(3) -0.0653(4) 0.3345(4) 0.0427(15) Uani 1 1 d . . . H21A H 0.5188 -0.1235 0.3046 0.051 Uiso 1 1 calc R . . H21B H 0.5314 -0.0838 0.3888 0.051 Uiso 1 1 calc R . . C22 C 0.5521(2) 0.0213(4) 0.3205(3) 0.0343(12) Uani 1 1 d . . . H22A H 0.5956 0.0012 0.3340 0.052 Uiso 1 1 calc R . . H22B H 0.5493 0.0782 0.3515 0.052 Uiso 1 1 calc R . . H22C H 0.5355 0.0399 0.2668 0.052 Uiso 1 1 calc R . . C23 C 0.4112(3) -0.1217(4) 0.1802(4) 0.0399(14) Uani 1 1 d . . . H23A H 0.4535 -0.1100 0.1793 0.048 Uiso 1 1 calc R . . H23B H 0.3811 -0.0970 0.1317 0.048 Uiso 1 1 calc R . . C24 C 0.4015(4) -0.2335(4) 0.1864(4) 0.0574(18) Uani 1 1 d . . . H24A H 0.4064 -0.2675 0.1429 0.086 Uiso 1 1 calc R . . H24B H 0.3597 -0.2456 0.1871 0.086 Uiso 1 1 calc R . . H24C H 0.4323 -0.2589 0.2333 0.086 Uiso 1 1 calc R . . C25 C 0.1681(3) -0.1582(4) 0.0946(3) 0.0360(13) Uani 1 1 d . . . H25A H 0.1940 -0.1359 0.0653 0.043 Uiso 1 1 calc R . . H25B H 0.1244 -0.1592 0.0599 0.043 Uiso 1 1 calc R . . C26 C 0.1874(4) -0.2628(5) 0.1238(4) 0.0593(19) Uani 1 1 d . . . H26A H 0.1827 -0.3073 0.0810 0.089 Uiso 1 1 calc R . . H26B H 0.1611 -0.2861 0.1516 0.089 Uiso 1 1 calc R . . H26C H 0.2309 -0.2625 0.1577 0.089 Uiso 1 1 calc R . . C27 C 0.0660(2) -0.0873(4) 0.1651(3) 0.0382(13) Uani 1 1 d . . . H27A H 0.0525 -0.0861 0.2095 0.046 Uiso 1 1 calc R . . H27B H 0.0610 -0.1561 0.1451 0.046 Uiso 1 1 calc R . . C28 C 0.0257(3) -0.0184(6) 0.1051(4) 0.064(2) Uani 1 1 d . . . H28A H -0.0177 -0.0396 0.0903 0.096 Uiso 1 1 calc R . . H28B H 0.0387 -0.0201 0.0608 0.096 Uiso 1 1 calc R . . H28C H 0.0298 0.0495 0.1252 0.096 Uiso 1 1 calc R . . C29 C 0.0615(3) 0.2193(5) 0.3496(4) 0.0498(17) Uani 1 1 d . . . H29A H 0.0457 0.2876 0.3500 0.060 Uiso 1 1 calc R . . H29B H 0.0376 0.1890 0.3001 0.060 Uiso 1 1 calc R . . C30 C 0.0509(4) 0.1609(9) 0.4108(6) 0.105(3) Uani 1 1 d . . . H30A H 0.0062 0.1535 0.3997 0.158 Uiso 1 1 calc R . . H30B H 0.0697 0.1955 0.4592 0.158 Uiso 1 1 calc R . . H30C H 0.0699 0.0950 0.4138 0.158 Uiso 1 1 calc R . . C31 C 0.1582(3) 0.3969(4) 0.4186(3) 0.0355(13) Uani 1 1 d . . . H31A H 0.1156 0.4192 0.3888 0.043 Uiso 1 1 calc R . . H31B H 0.1874 0.4466 0.4114 0.043 Uiso 1 1 calc R . . C32 C 0.1656(3) 0.3940(5) 0.5025(4) 0.0529(17) Uani 1 1 d . . . H32A H 0.1575 0.4601 0.5187 0.079 Uiso 1 1 calc R . . H32B H 0.2080 0.3737 0.5326 0.079 Uiso 1 1 calc R . . H32C H 0.1361 0.3462 0.5100 0.079 Uiso 1 1 calc R . . C33 C 0.4078(3) 0.3966(4) 0.5358(3) 0.0354(13) Uani 1 1 d . . . H33A H 0.3741 0.4439 0.5100 0.042 Uiso 1 1 calc R . . H33B H 0.4479 0.4288 0.5415 0.042 Uiso 1 1 calc R . . C34 C 0.4057(3) 0.3715(5) 0.6133(3) 0.0498(16) Uani 1 1 d . . . H34A H 0.4201 0.4288 0.6471 0.075 Uiso 1 1 calc R . . H34B H 0.4327 0.3143 0.6342 0.075 Uiso 1 1 calc R . . H34C H 0.3630 0.3552 0.6088 0.075 Uiso 1 1 calc R . . C35 C 0.5122(2) 0.2556(5) 0.5344(3) 0.0430(15) Uani 1 1 d . . . H35A H 0.5320 0.1944 0.5612 0.052 Uiso 1 1 calc R . . H35B H 0.5164 0.3077 0.5730 0.052 Uiso 1 1 calc R . . C36 C 0.5459(3) 0.2890(4) 0.4820(3) 0.0377(13) Uani 1 1 d . . . H36A H 0.5893 0.3034 0.5119 0.057 Uiso 1 1 calc R . . H36B H 0.5260 0.3489 0.4547 0.057 Uiso 1 1 calc R . . H36C H 0.5440 0.2360 0.4456 0.057 Uiso 1 1 calc R . . C37 C 0.5041(2) 0.0380(4) 0.4753(3) 0.0366(13) Uani 1 1 d . . . H37A H 0.5297 0.0113 0.4470 0.044 Uiso 1 1 calc R . . H37B H 0.5268 0.0947 0.5062 0.044 Uiso 1 1 calc R . . C38 C 0.2333(2) 0.2259(4) 0.1988(3) 0.0325(12) Uani 1 1 d . . . H38A H 0.1949 0.2001 0.1991 0.039 Uiso 1 1 calc R . . C39 C 0.2340(3) 0.2916(4) 0.1432(3) 0.0404(14) Uani 1 1 d . . . H39A H 0.1953 0.3095 0.1060 0.048 Uiso 1 1 calc R . . C40 C 0.3373(3) 0.3047(4) 0.1934(3) 0.0364(13) Uani 1 1 d . . . H40A H 0.3753 0.3333 0.1942 0.044 Uiso 1 1 calc R . . C41 C 0.3390(2) 0.2375(4) 0.2494(3) 0.0290(11) Uani 1 1 d . . . H41A H 0.3777 0.2191 0.2860 0.035 Uiso 1 1 calc R . . C42 C 0.2977(2) -0.0909(3) 0.4030(3) 0.0253(11) Uani 1 1 d . . . H42A H 0.3002 -0.1154 0.3569 0.030 Uiso 1 1 calc R . . C43 C 0.3009(2) -0.1571(4) 0.4608(3) 0.0297(11) Uani 1 1 d . . . H43A H 0.3051 -0.2260 0.4529 0.036 Uiso 1 1 calc R . . C44 C 0.2914(2) -0.0294(4) 0.5336(3) 0.0307(12) Uani 1 1 d . . . H44A H 0.2886 -0.0046 0.5795 0.037 Uiso 1 1 calc R . . C45 C 0.2883(2) 0.0373(4) 0.4771(3) 0.0274(11) Uani 1 1 d . . . H45A H 0.2839 0.1062 0.4852 0.033 Uiso 1 1 calc R . . Cl1 Cl 0.26842(9) -0.50210(14) 0.27101(11) 0.0657(5) Uani 1 1 d . . . C1S C 0.3292(3) -0.4428(4) 0.3416(3) 0.0405(14) Uani 1 1 d . . . H1SA H 0.3199 -0.4438 0.3897 0.049 Uiso 1 1 calc R . . Cl2 Cl 0.33634(8) -0.31847(11) 0.31744(9) 0.0508(4) Uani 1 1 d . . . Cl3 Cl 0.39983(8) -0.50649(12) 0.35737(9) 0.0508(4) Uani 1 1 d . . . C2S C 0.1548(3) -0.2276(5) -0.1086(4) 0.0486(16) Uani 1 1 d . . . H2SA H 0.1919 -0.1998 -0.0678 0.058 Uiso 1 1 calc R . . Cl4 Cl 0.14062(9) -0.34962(13) -0.08322(11) 0.0659(5) Uani 1 1 d . . . Cl5 Cl 0.17017(9) -0.23407(15) -0.19307(9) 0.0629(5) Uani 1 1 d . . . Cl6 Cl 0.08990(8) -0.15113(12) -0.11900(10) 0.0532(4) Uani 1 1 d . . . Cl Cl 0.28045(6) -0.41286(8) 0.48840(7) 0.0281(3) Uani 1 1 d . . . N2S N 0.0921(5) 0.1338(15) -0.3680(8) 0.109(7) Uani 0.50 1 d P . . N1S N 0.0364(4) 0.0437(7) -0.2806(5) 0.033(2) Uani 0.50 1 d P . . C3S C 0.0202(6) 0.1315(12) -0.3135(7) 0.057(4) Uani 0.50 1 d P . . H3SA H -0.0133 0.1660 -0.3062 0.068 Uiso 0.50 1 calc PR . . C4S C 0.0500(6) 0.1755(10) -0.3580(8) 0.053(3) Uani 0.50 1 d PU . . H4SA H 0.0368 0.2386 -0.3805 0.064 Uiso 0.50 1 calc PR . . C5S C 0.1101(6) 0.0370(12) -0.3386(8) 0.062(4) Uani 0.50 1 d PU . . H5SA H 0.1398 -0.0021 -0.3508 0.074 Uiso 0.50 1 calc PR . . C6S C 0.0798(7) 0.0047(10) -0.2901(8) 0.067(5) Uani 0.50 1 d P . . H6SA H 0.0952 -0.0541 -0.2619 0.080 Uiso 0.50 1 calc PR . . 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 0.0254(4) 0.0152(3) 0.0263(4) 0.0028(3) 0.0087(3) 0.0009(3) N1 0.028(2) 0.019(2) 0.029(2) 0.0055(17) 0.0105(18) 0.0030(17) N2 0.027(2) 0.017(2) 0.026(2) 0.0028(17) 0.0103(18) 0.0016(17) N3 0.024(2) 0.015(2) 0.029(2) 0.0022(17) 0.0052(17) 0.0008(16) N4 0.026(2) 0.016(2) 0.026(2) 0.0075(17) 0.0054(17) -0.0004(16) N5 0.026(2) 0.019(2) 0.032(2) 0.0010(18) 0.0099(18) 0.0004(17) N6 0.047(3) 0.027(2) 0.040(3) 0.008(2) 0.016(2) 0.001(2) N7 0.024(2) 0.017(2) 0.028(2) -0.0004(17) 0.0093(18) -0.0027(16) N8 0.045(3) 0.025(2) 0.033(3) 0.0027(19) 0.015(2) -0.003(2) C1 0.028(3) 0.018(2) 0.037(3) 0.013(2) 0.011(2) 0.004(2) C2 0.031(3) 0.018(3) 0.053(4) 0.009(2) 0.018(3) 0.003(2) C3 0.037(3) 0.016(2) 0.049(3) 0.008(2) 0.025(3) 0.004(2) C4 0.036(3) 0.018(2) 0.033(3) 0.008(2) 0.016(2) 0.003(2) C5 0.041(3) 0.019(3) 0.027(3) 0.003(2) 0.016(2) 0.001(2) C6 0.032(3) 0.021(3) 0.025(3) 0.003(2) 0.008(2) 0.000(2) C7 0.037(3) 0.024(3) 0.025(3) 0.005(2) 0.008(2) -0.002(2) C8 0.033(3) 0.023(3) 0.025(3) 0.001(2) 0.008(2) 0.000(2) C9 0.034(3) 0.013(2) 0.027(3) 0.0047(19) 0.012(2) 0.001(2) C10 0.028(3) 0.018(2) 0.036(3) 0.001(2) 0.012(2) -0.006(2) C11 0.026(3) 0.022(3) 0.037(3) -0.001(2) 0.010(2) 0.003(2) C12 0.032(3) 0.029(3) 0.045(3) -0.007(2) 0.015(3) 0.002(2) C13 0.036(3) 0.020(3) 0.036(3) 0.000(2) 0.011(2) 0.004(2) C14 0.029(3) 0.019(2) 0.029(3) 0.000(2) 0.008(2) 0.002(2) C15 0.037(3) 0.015(2) 0.034(3) 0.005(2) 0.012(2) -0.002(2) C16 0.028(3) 0.021(3) 0.028(3) 0.001(2) 0.011(2) -0.007(2) C17 0.033(3) 0.033(3) 0.025(3) 0.002(2) 0.013(2) -0.008(2) C18 0.029(3) 0.043(3) 0.021(3) 0.002(2) 0.010(2) -0.007(2) C19 0.028(3) 0.029(3) 0.025(3) 0.010(2) 0.010(2) 0.001(2) C20 0.023(3) 0.032(3) 0.032(3) 0.015(2) 0.008(2) 0.000(2) C21 0.034(3) 0.026(3) 0.069(4) 0.005(3) 0.019(3) 0.005(2) C22 0.033(3) 0.031(3) 0.043(3) -0.005(2) 0.018(3) -0.001(2) C23 0.043(3) 0.028(3) 0.061(4) 0.000(3) 0.033(3) 0.005(2) C24 0.088(5) 0.027(3) 0.071(5) -0.004(3) 0.045(4) 0.001(3) C25 0.047(3) 0.035(3) 0.027(3) -0.008(2) 0.013(3) -0.008(3) C26 0.096(6) 0.034(4) 0.059(4) -0.011(3) 0.041(4) -0.003(4) C27 0.033(3) 0.037(3) 0.042(3) -0.011(3) 0.011(3) -0.012(2) C28 0.034(4) 0.084(6) 0.062(5) 0.016(4) 0.002(3) -0.009(3) C29 0.032(3) 0.042(4) 0.080(5) -0.026(3) 0.026(3) -0.003(3) C30 0.067(6) 0.135(9) 0.137(9) -0.014(7) 0.066(6) -0.024(6) C31 0.036(3) 0.018(3) 0.052(3) -0.005(2) 0.014(3) 0.002(2) C32 0.072(5) 0.037(4) 0.059(4) -0.012(3) 0.034(4) 0.001(3) C33 0.039(3) 0.030(3) 0.032(3) 0.004(2) 0.006(2) -0.008(2) C34 0.084(5) 0.033(3) 0.033(3) -0.004(3) 0.020(3) 0.001(3) C35 0.029(3) 0.066(4) 0.032(3) -0.005(3) 0.008(2) -0.005(3) C36 0.035(3) 0.027(3) 0.053(4) 0.001(3) 0.016(3) -0.005(2) C37 0.031(3) 0.038(3) 0.038(3) 0.017(3) 0.008(2) 0.007(2) C38 0.030(3) 0.027(3) 0.036(3) 0.007(2) 0.006(2) 0.000(2) C39 0.045(4) 0.032(3) 0.035(3) 0.010(3) 0.003(3) 0.006(3) C40 0.044(3) 0.027(3) 0.043(3) 0.006(2) 0.022(3) -0.001(2) C41 0.034(3) 0.020(3) 0.037(3) 0.005(2) 0.016(2) 0.000(2) C42 0.027(3) 0.017(2) 0.030(3) 0.001(2) 0.008(2) -0.003(2) C43 0.036(3) 0.017(3) 0.034(3) -0.001(2) 0.011(2) -0.002(2) C44 0.041(3) 0.023(3) 0.027(3) 0.001(2) 0.010(2) -0.002(2) C45 0.032(3) 0.018(2) 0.032(3) -0.002(2) 0.010(2) -0.002(2) Cl1 0.0669(12) 0.0487(10) 0.0702(12) -0.0189(9) 0.0099(9) -0.0070(8) C1S 0.049(4) 0.035(3) 0.041(3) -0.001(3) 0.019(3) -0.002(3) Cl2 0.0655(10) 0.0359(8) 0.0515(9) 0.0048(7) 0.0213(8) -0.0022(7) Cl3 0.0591(10) 0.0491(9) 0.0494(9) 0.0066(7) 0.0256(8) 0.0095(8) C2S 0.056(4) 0.046(4) 0.046(4) -0.008(3) 0.020(3) -0.005(3) Cl4 0.0695(12) 0.0443(10) 0.0797(13) 0.0061(9) 0.0207(10) -0.0025(8) Cl5 0.0767(12) 0.0674(12) 0.0447(9) -0.0062(8) 0.0214(9) 0.0089(9) Cl6 0.0561(10) 0.0406(9) 0.0626(10) -0.0064(8) 0.0205(8) -0.0015(7) Cl 0.0407(7) 0.0146(6) 0.0325(7) 0.0024(5) 0.0171(6) -0.0011(5) N2S 0.027(6) 0.205(19) 0.086(10) 0.068(11) 0.007(6) -0.050(9) N1S 0.033(5) 0.034(5) 0.039(5) 0.017(4) 0.020(4) 0.010(4) C3S 0.052(8) 0.079(11) 0.040(7) -0.007(7) 0.016(6) 0.021(7) C4S 0.045(5) 0.050(5) 0.067(5) 0.004(4) 0.024(4) 0.022(4) C5S 0.047(5) 0.061(5) 0.070(5) 0.019(4) 0.012(4) 0.008(4) C6S 0.077(11) 0.041(8) 0.057(9) 0.042(7) -0.008(8) -0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.941(4) . ? Co1 N3 1.947(4) . ? Co1 N2 1.950(4) . ? Co1 N4 1.953(4) . ? Co1 N7 1.953(4) . ? Co1 N5 1.963(4) . ? N1 C4 1.373(6) . ? N1 C1 1.386(6) . ? N2 C9 1.366(6) . ? N2 C6 1.376(6) . ? N3 C11 1.373(6) . ? N3 C14 1.377(6) . ? N4 C16 1.373(6) . ? N4 C19 1.384(6) . ? N5 C41 1.340(6) . ? N5 C38 1.341(6) . ? N6 C39 1.328(7) . ? N6 C40 1.332(7) . ? N7 C45 1.333(6) . ? N7 C42 1.334(6) . ? N8 C44 1.334(7) . ? N8 C43 1.335(7) . ? C1 C20 1.396(7) . ? C1 C2 1.454(7) . ? C2 C3 1.369(8) . ? C2 C21 1.506(7) . ? C3 C4 1.430(7) . ? C3 C23 1.503(7) . ? C4 C5 1.395(7) . ? C5 C6 1.381(7) . ? C6 C7 1.452(7) . ? C7 C8 1.345(7) . ? C7 C25 1.506(7) . ? C8 C9 1.452(7) . ? C8 C27 1.496(7) . ? C9 C10 1.384(7) . ? C10 C11 1.378(7) . ? C11 C12 1.448(7) . ? C12 C13 1.356(7) . ? C12 C29 1.503(7) . ? C13 C14 1.436(7) . ? C13 C31 1.503(7) . ? C14 C15 1.385(7) . ? C15 C16 1.373(7) . ? C16 C17 1.442(7) . ? C17 C18 1.351(7) . ? C17 C33 1.498(7) . ? C18 C19 1.454(7) . ? C18 C35 1.513(7) . ? C19 C20 1.398(7) . ? C20 C37 1.511(7) . ? C21 C22 1.528(7) . ? C23 C24 1.531(8) . ? C25 C26 1.520(8) . ? C27 C28 1.505(9) . ? C29 C30 1.483(11) . ? C31 C32 1.531(8) . ? C33 C34 1.515(8) . ? C35 C36 1.519(8) . ? C37 C37 1.440(10) 3_656 ? C38 C39 1.375(7) . ? C40 C41 1.379(7) . ? C42 C43 1.389(7) . ? C44 C45 1.373(7) . ? Cl1 C1S 1.748(6) . ? C1S Cl2 1.757(6) . ? C1S Cl3 1.768(6) . ? C2S Cl5 1.748(6) . ? C2S Cl6 1.766(7) . ? C2S Cl4 1.771(7) . ? N2S C4S 1.19(2) . ? N2S C5S 1.42(2) . ? N1S C6S 1.195(18) . ? N1S C3S 1.325(17) . ? C3S C4S 1.39(2) . ? C5S C6S 1.40(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N3 178.45(17) . . ? N1 Co1 N2 90.54(17) . . ? N3 Co1 N2 89.08(16) . . ? N1 Co1 N4 89.15(17) . . ? N3 Co1 N4 91.24(16) . . ? N2 Co1 N4 179.58(17) . . ? N1 Co1 N7 91.38(16) . . ? N3 Co1 N7 90.12(16) . . ? N2 Co1 N7 90.37(16) . . ? N4 Co1 N7 89.36(16) . . ? N1 Co1 N5 88.96(16) . . ? N3 Co1 N5 89.55(16) . . ? N2 Co1 N5 90.88(16) . . ? N4 Co1 N5 89.39(16) . . ? N7 Co1 N5 178.70(17) . . ? C4 N1 C1 106.0(4) . . ? C4 N1 Co1 125.7(3) . . ? C1 N1 Co1 128.3(3) . . ? C9 N2 C6 105.4(4) . . ? C9 N2 Co1 127.9(3) . . ? C6 N2 Co1 126.7(3) . . ? C11 N3 C14 105.9(4) . . ? C11 N3 Co1 127.5(3) . . ? C14 N3 Co1 126.5(3) . . ? C16 N4 C19 107.6(4) . . ? C16 N4 Co1 125.3(3) . . ? C19 N4 Co1 127.0(3) . . ? C41 N5 C38 116.9(4) . . ? C41 N5 Co1 121.0(3) . . ? C38 N5 Co1 122.1(3) . . ? C39 N6 C40 114.4(5) . . ? C45 N7 C42 117.1(4) . . ? C45 N7 Co1 121.2(3) . . ? C42 N7 Co1 121.7(3) . . ? C44 N8 C43 115.3(4) . . ? N1 C1 C20 123.3(4) . . ? N1 C1 C2 109.4(4) . . ? C20 C1 C2 127.2(5) . . ? C3 C2 C1 106.7(4) . . ? C3 C2 C21 122.8(5) . . ? C1 C2 C21 129.8(5) . . ? C2 C3 C4 106.8(5) . . ? C2 C3 C23 129.1(5) . . ? C4 C3 C23 124.2(5) . . ? N1 C4 C5 125.2(5) . . ? N1 C4 C3 110.9(5) . . ? C5 C4 C3 123.1(5) . . ? C6 C5 C4 123.0(5) . . ? N2 C6 C5 124.5(4) . . ? N2 C6 C7 110.5(4) . . ? C5 C6 C7 124.9(5) . . ? C8 C7 C6 106.5(4) . . ? C8 C7 C25 129.4(5) . . ? C6 C7 C25 123.8(5) . . ? C7 C8 C9 106.9(4) . . ? C7 C8 C27 127.7(5) . . ? C9 C8 C27 125.3(5) . . ? N2 C9 C10 124.3(4) . . ? N2 C9 C8 110.5(4) . . ? C10 C9 C8 124.9(5) . . ? C11 C10 C9 123.1(5) . . ? N3 C11 C10 124.7(4) . . ? N3 C11 C12 109.7(4) . . ? C10 C11 C12 125.2(5) . . ? C13 C12 C11 107.2(4) . . ? C13 C12 C29 127.9(5) . . ? C11 C12 C29 124.9(5) . . ? C12 C13 C14 106.6(4) . . ? C12 C13 C31 128.4(5) . . ? C14 C13 C31 125.0(5) . . ? N3 C14 C15 123.6(4) . . ? N3 C14 C13 110.4(4) . . ? C15 C14 C13 125.6(5) . . ? C16 C15 C14 124.8(5) . . ? N4 C16 C15 125.5(4) . . ? N4 C16 C17 109.2(4) . . ? C15 C16 C17 125.1(5) . . ? C18 C17 C16 107.2(5) . . ? C18 C17 C33 127.6(5) . . ? C16 C17 C33 124.8(5) . . ? C17 C18 C19 107.9(4) . . ? C17 C18 C35 121.3(5) . . ? C19 C18 C35 129.9(5) . . ? N4 C19 C20 124.5(5) . . ? N4 C19 C18 107.9(4) . . ? C20 C19 C18 127.4(5) . . ? C1 C20 C19 122.3(4) . . ? C1 C20 C37 118.7(5) . . ? C19 C20 C37 118.9(5) . . ? C2 C21 C22 112.4(4) . . ? C3 C23 C24 112.7(5) . . ? C7 C25 C26 112.6(5) . . ? C8 C27 C28 111.6(5) . . ? C30 C29 C12 113.1(6) . . ? C13 C31 C32 113.7(5) . . ? C17 C33 C34 110.7(4) . . ? C18 C35 C36 112.2(4) . . ? C37 C37 C20 112.4(6) 3_656 . ? N5 C38 C39 120.4(5) . . ? N6 C39 C38 124.1(5) . . ? N6 C40 C41 123.4(5) . . ? N5 C41 C40 120.7(5) . . ? N7 C42 C43 121.1(5) . . ? N8 C43 C42 122.2(5) . . ? N8 C44 C45 123.3(5) . . ? N7 C45 C44 120.9(5) . . ? Cl1 C1S Cl2 111.1(3) . . ? Cl1 C1S Cl3 110.5(3) . . ? Cl2 C1S Cl3 109.9(3) . . ? Cl5 C2S Cl6 111.1(4) . . ? Cl5 C2S Cl4 108.3(3) . . ? Cl6 C2S Cl4 110.0(3) . . ? C4S N2S C5S 120.9(13) . . ? C6S N1S C3S 115.7(11) . . ? N1S C3S C4S 123.1(12) . . ? N2S C4S C3S 119.7(14) . . ? C6S C5S N2S 113.3(14) . . ? N1S C6S C5S 126.5(12) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.122 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 940535'