plementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jun Tao' _publ_contact_author_email TAOJUN@XMU.EDU.CN _publ_section_title ; Structure and magnetic property of a mixed-valence nonanuclear cobalt complex with a square-pyramidal CoII5 core ; loop_ _publ_author_name 'Zhong-Quan Jia.' 'Xiao-Jun Sun.' 'Li-Li Hu.' 'Jun Tao.' 'Rong-Bin Huan.' 'Lan-Sun Zheng.' # Attachment 'crystal_data-revised.cif' #============================================================ data_1 _database_code_depnum_ccdc_archive 'CCDC 720927' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H116 Cl2 Co9 N8 O28' _chemical_formula_weight 2383.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.6238(16) _cell_length_b 9.4814(4) _cell_length_c 33.395(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.339(5) _cell_angle_gamma 90.00 _cell_volume 9746.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7147 _cell_measurement_theta_min 2.4972 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4900 _exptl_absorpt_coefficient_mu 1.627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93795 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20988 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9324 _reflns_number_gt 7147 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The hydrogen atoms on O1W cannot be fixed. Although the structure contains accessible voids as calculated by PLATON, no additional molecules were found in the structure. We think that it may be due to the existence of unidentified solvate which could not be modeled satisfactorily. ; _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^)+(0.0185P)^2^+109.4782P] 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 9324 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1289 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _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 0.5000 -0.08281(11) 0.2500 0.0161(2) Uani 1 2 d S . . Co2 Co 0.53791(2) 0.10087(8) 0.19906(2) 0.01385(17) Uani 1 1 d . . . Co3 Co 0.62057(2) 0.13266(8) 0.18158(2) 0.01478(17) Uani 1 1 d . . . Co4 Co 0.43010(2) 0.09847(8) 0.19252(2) 0.01411(17) Uani 1 1 d . . . Co5 Co 0.38541(2) 0.13295(8) 0.10000(2) 0.01579(17) Uani 1 1 d . . . Cl1 Cl 0.5000 -0.3245(2) 0.2500 0.0296(5) Uani 1 2 d S . . Cl2 Cl 0.5000 0.22091(19) 0.2500 0.0173(4) Uani 1 2 d S . . N1 N 0.59178(15) 0.2619(5) 0.13775(14) 0.0158(10) Uani 1 1 d . . . O1 O 0.64596(13) 0.0254(4) 0.14876(12) 0.0211(9) Uani 1 1 d . . . O2 O 0.59103(12) 0.2337(4) 0.21382(11) 0.0157(8) Uani 1 1 d . . . O3 O 0.50744(13) 0.2304(4) 0.14893(12) 0.0190(9) Uani 1 1 d . . . H3 H 0.4817 0.2434 0.1492 0.023 Uiso 1 1 d R . . C1 C 0.63700(18) 0.0396(6) 0.10781(18) 0.0201(13) Uani 1 1 d . . . C2 C 0.6511(2) -0.0672(7) 0.0857(2) 0.0297(15) Uani 1 1 d . . . H2A H 0.6639 -0.1481 0.1002 0.036 Uiso 1 1 calc R . . C3 C 0.6463(2) -0.0543(8) 0.0436(2) 0.0369(17) Uani 1 1 d . . . H3A H 0.6565 -0.1256 0.0303 0.044 Uiso 1 1 calc R . . C4 C 0.6264(2) 0.0631(8) 0.0204(2) 0.0379(18) Uani 1 1 d . . . H4A H 0.6243 0.0727 -0.0079 0.045 Uiso 1 1 calc R . . C5 C 0.6101(2) 0.1636(7) 0.0398(2) 0.0330(16) Uani 1 1 d . . . H5A H 0.5961 0.2414 0.0243 0.040 Uiso 1 1 calc R . . C6 C 0.61400(19) 0.1527(6) 0.08327(18) 0.0218(13) Uani 1 1 d . . . C7 C 0.59317(19) 0.2585(6) 0.10009(18) 0.0207(13) Uani 1 1 d . . . H7A H 0.5794 0.3313 0.0820 0.025 Uiso 1 1 calc R . . C8 C 0.56841(19) 0.3791(6) 0.15076(18) 0.0195(12) Uani 1 1 d . . . C9 C 0.52003(19) 0.3558(6) 0.13285(19) 0.0204(12) Uani 1 1 d . . . H9A H 0.5052 0.4357 0.1400 0.024 Uiso 1 1 calc R . . H9B H 0.5113 0.3499 0.1022 0.024 Uiso 1 1 calc R . . C10 C 0.5844(2) 0.3760(6) 0.19918(18) 0.0207(12) Uani 1 1 d . . . H10A H 0.6115 0.4279 0.2100 0.025 Uiso 1 1 calc R . . H10B H 0.5632 0.4209 0.2096 0.025 Uiso 1 1 calc R . . C11 C 0.5782(2) 0.5235(6) 0.1355(2) 0.0267(14) Uani 1 1 d . . . H11A H 0.5683 0.5251 0.1050 0.040 Uiso 1 1 calc R . . H11B H 0.6090 0.5404 0.1461 0.040 Uiso 1 1 calc R . . H11C H 0.5635 0.5955 0.1457 0.040 Uiso 1 1 calc R . . N2 N 0.64572(15) 0.0104(5) 0.22871(14) 0.0163(10) Uani 1 1 d . . . O4 O 0.66666(13) 0.2634(4) 0.19686(12) 0.0226(9) Uani 1 1 d . . . O5 O 0.57272(12) 0.0029(4) 0.16734(12) 0.0156(8) Uani 1 1 d . . . O6 O 0.56359(12) -0.0214(4) 0.25369(11) 0.0140(8) Uani 1 1 d . . . C12 C 0.69453(17) 0.2761(6) 0.23495(18) 0.0180(12) Uani 1 1 d . . . C13 C 0.7187(2) 0.4021(7) 0.2458(2) 0.0286(14) Uani 1 1 d . . . H13A H 0.7140 0.4735 0.2257 0.034 Uiso 1 1 calc R . . C14 C 0.7487(2) 0.4216(7) 0.2849(2) 0.0334(16) Uani 1 1 d . . . H14A H 0.7635 0.5069 0.2912 0.040 Uiso 1 1 calc R . . C15 C 0.7576(2) 0.3162(7) 0.3158(2) 0.0367(17) Uani 1 1 d . . . H15A H 0.7784 0.3300 0.3423 0.044 Uiso 1 1 calc R . . C16 C 0.7351(2) 0.1920(7) 0.3062(2) 0.0316(15) Uani 1 1 d . . . H16A H 0.7412 0.1205 0.3264 0.038 Uiso 1 1 calc R . . C17 C 0.70316(19) 0.1698(6) 0.26663(19) 0.0207(13) Uani 1 1 d . . . C18 C 0.67878(19) 0.0406(6) 0.26044(18) 0.0210(13) Uani 1 1 d . . . H18A H 0.6881 -0.0272 0.2817 0.025 Uiso 1 1 calc R . . C19 C 0.62165(18) -0.1235(5) 0.22759(17) 0.0170(12) Uani 1 1 d . . . C20 C 0.58967(19) -0.1325(6) 0.18242(18) 0.0200(12) Uani 1 1 d . . . H20A H 0.6042 -0.1714 0.1639 0.024 Uiso 1 1 calc R . . H20B H 0.5660 -0.1952 0.1819 0.024 Uiso 1 1 calc R . . C21 C 0.59800(19) -0.1216(6) 0.26052(18) 0.0199(12) Uani 1 1 d . . . H21A H 0.5862 -0.2150 0.2615 0.024 Uiso 1 1 calc R . . H21B H 0.6193 -0.1035 0.2882 0.024 Uiso 1 1 calc R . . C22 C 0.6521(2) -0.2504(6) 0.2370(2) 0.0246(14) Uani 1 1 d . . . H22A H 0.6670 -0.2545 0.2167 0.037 Uiso 1 1 calc R . . H22B H 0.6355 -0.3352 0.2354 0.037 Uiso 1 1 calc R . . H22C H 0.6729 -0.2415 0.2650 0.037 Uiso 1 1 calc R . . N3 N 0.34561(15) 0.2574(5) 0.11225(14) 0.0168(10) Uani 1 1 d . . . O7 O 0.34394(13) 0.0265(4) 0.05920(12) 0.0232(9) Uani 1 1 d . . . O8 O 0.42847(12) 0.2347(4) 0.14402(12) 0.0158(8) Uani 1 1 d . . . O9 O 0.38527(13) 0.2240(4) 0.20583(12) 0.0198(9) Uani 1 1 d . . . H9 H 0.3947 0.2404 0.2323 0.024 Uiso 1 1 d R . . C23 C 0.3023(2) 0.0479(6) 0.04616(19) 0.0230(13) Uani 1 1 d . . . C24 C 0.2758(2) -0.0390(7) 0.0138(2) 0.0330(16) Uani 1 1 d . . . H24A H 0.2885 -0.1106 0.0029 0.040 Uiso 1 1 calc R . . C25 C 0.2316(3) -0.0211(8) -0.0022(2) 0.045(2) Uani 1 1 d . . . H25A H 0.2150 -0.0803 -0.0237 0.054 Uiso 1 1 calc R . . C26 C 0.2113(2) 0.0830(9) 0.0130(3) 0.051(2) Uani 1 1 d . . . H26A H 0.1814 0.0946 0.0019 0.061 Uiso 1 1 calc R . . C27 C 0.2358(2) 0.1687(8) 0.0447(3) 0.0438(19) Uani 1 1 d . . . H27A H 0.2220 0.2386 0.0551 0.053 Uiso 1 1 calc R . . C28 C 0.2814(2) 0.1543(7) 0.0621(2) 0.0286(14) Uani 1 1 d . . . C29 C 0.3046(2) 0.2523(6) 0.0941(2) 0.0232(13) Uani 1 1 d . . . H29A H 0.2881 0.3189 0.1024 0.028 Uiso 1 1 calc R . . C30 C 0.36575(19) 0.3735(6) 0.14265(18) 0.0209(12) Uani 1 1 d . . . C31 C 0.41350(18) 0.3752(6) 0.14540(19) 0.0204(12) Uani 1 1 d . . . H31A H 0.4167 0.4291 0.1219 0.025 Uiso 1 1 calc R . . H31B H 0.4308 0.4202 0.1716 0.025 Uiso 1 1 calc R . . C32 C 0.3614(2) 0.3446(6) 0.18591(18) 0.0209(13) Uani 1 1 d . . . H32A H 0.3716 0.4261 0.2040 0.025 Uiso 1 1 calc R . . H32B H 0.3310 0.3309 0.1826 0.025 Uiso 1 1 calc R . . C33 C 0.3450(2) 0.5160(6) 0.1274(2) 0.0276(14) Uani 1 1 d . . . H33A H 0.3151 0.5139 0.1258 0.041 Uiso 1 1 calc R . . H33B H 0.3468 0.5359 0.0999 0.041 Uiso 1 1 calc R . . H33C H 0.3600 0.5879 0.1470 0.041 Uiso 1 1 calc R . . N4 N 0.57148(16) 0.0109(5) 0.40714(15) 0.0171(10) Uani 1 1 d . . . O10 O 0.61165(14) 0.2660(4) 0.44077(13) 0.0253(10) Uani 1 1 d . . . O11 O 0.61550(12) 0.0030(4) 0.35645(12) 0.0161(8) Uani 1 1 d . . . O12 O 0.51863(12) -0.0215(4) 0.31389(11) 0.0140(8) Uani 1 1 d . . . C34 C 0.58118(19) 0.2707(7) 0.45802(18) 0.0230(13) Uani 1 1 d . . . C35 C 0.5797(2) 0.3890(7) 0.4831(2) 0.0329(15) Uani 1 1 d . . . H35A H 0.5996 0.4616 0.4860 0.039 Uiso 1 1 calc R . . C36 C 0.5492(2) 0.3990(7) 0.5032(2) 0.0358(16) Uani 1 1 d . . . H36A H 0.5493 0.4779 0.5198 0.043 Uiso 1 1 calc R . . C37 C 0.5186(2) 0.2951(7) 0.4996(2) 0.0362(17) Uani 1 1 d . . . H37A H 0.4982 0.3035 0.5133 0.043 Uiso 1 1 calc R . . C38 C 0.5190(2) 0.1795(7) 0.4752(2) 0.0318(15) Uani 1 1 d . . . H38A H 0.4986 0.1087 0.4726 0.038 Uiso 1 1 calc R . . C39 C 0.5494(2) 0.1648(6) 0.45407(18) 0.0235(13) Uani 1 1 d . . . C40 C 0.5473(2) 0.0393(6) 0.42958(18) 0.0211(13) Uani 1 1 d . . . H40A H 0.5265 -0.0275 0.4299 0.025 Uiso 1 1 calc R . . C41 C 0.56545(19) -0.1242(6) 0.38302(17) 0.0174(12) Uani 1 1 d . . . C42 C 0.60507(19) -0.1318(6) 0.36794(18) 0.0182(12) Uani 1 1 d . . . H42A H 0.6297 -0.1697 0.3905 0.022 Uiso 1 1 calc R . . H42B H 0.5988 -0.1947 0.3437 0.022 Uiso 1 1 calc R . . C43 C 0.52262(18) -0.1252(6) 0.34617(17) 0.0190(12) Uani 1 1 d . . . H43A H 0.5188 -0.2177 0.3331 0.023 Uiso 1 1 calc R . . H43B H 0.4991 -0.1113 0.3575 0.023 Uiso 1 1 calc R . . C44 C 0.5654(2) -0.2515(6) 0.41144(19) 0.0248(14) Uani 1 1 d . . . H44A H 0.5920 -0.2532 0.4350 0.037 Uiso 1 1 calc R . . H44B H 0.5628 -0.3369 0.3953 0.037 Uiso 1 1 calc R . . H44C H 0.5413 -0.2441 0.4218 0.037 Uiso 1 1 calc R . . O1W O 0.5427(2) -0.1176(8) 0.0844(2) 0.078(2) Uani 1 1 d . . . O13 O 0.6974(2) -0.1158(8) 0.3510(2) 0.077(2) Uani 1 1 d . . . H13 H 0.6765 -0.0864 0.3587 0.093 Uiso 1 1 d R . . C45 C 0.7324(3) -0.1725(9) 0.3851(3) 0.055(2) Uani 1 1 d . . . H45A H 0.7213 -0.2340 0.4023 0.067 Uiso 1 1 calc R . . H45B H 0.7486 -0.0968 0.4030 0.067 Uiso 1 1 calc R . . C46 C 0.7607(4) -0.2515(12) 0.3676(4) 0.093(4) Uani 1 1 d . . . H46A H 0.7845 -0.2900 0.3903 0.140 Uiso 1 1 calc R . . H46B H 0.7717 -0.1898 0.3508 0.140 Uiso 1 1 calc R . . H46C H 0.7446 -0.3267 0.3502 0.140 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 0.0194(6) 0.0142(6) 0.0162(5) 0.000 0.0081(4) 0.000 Co2 0.0163(4) 0.0116(4) 0.0154(4) -0.0003(3) 0.0076(3) -0.0006(3) Co3 0.0162(4) 0.0161(4) 0.0141(4) -0.0021(3) 0.0077(3) -0.0021(3) Co4 0.0176(4) 0.0120(4) 0.0138(4) 0.0010(3) 0.0068(3) 0.0003(3) Co5 0.0164(4) 0.0173(4) 0.0144(4) 0.0018(3) 0.0062(3) -0.0001(3) Cl1 0.0391(13) 0.0138(11) 0.0376(13) 0.000 0.0147(10) 0.000 Cl2 0.0215(10) 0.0127(10) 0.0195(10) 0.000 0.0090(8) 0.000 N1 0.017(2) 0.014(2) 0.019(2) -0.0023(19) 0.009(2) -0.0051(19) O1 0.023(2) 0.025(2) 0.017(2) -0.0003(17) 0.0097(18) 0.0035(17) O2 0.021(2) 0.012(2) 0.0158(19) -0.0019(15) 0.0084(17) -0.0033(16) O3 0.016(2) 0.018(2) 0.025(2) 0.0069(16) 0.0098(18) -0.0002(16) C1 0.012(3) 0.030(3) 0.020(3) -0.006(2) 0.007(2) -0.003(2) C2 0.023(3) 0.039(4) 0.025(3) -0.006(3) 0.005(3) 0.013(3) C3 0.030(4) 0.056(5) 0.023(3) -0.016(3) 0.007(3) 0.012(3) C4 0.035(4) 0.065(5) 0.015(3) -0.007(3) 0.010(3) 0.009(4) C5 0.035(4) 0.044(4) 0.021(3) 0.002(3) 0.012(3) 0.008(3) C6 0.021(3) 0.026(3) 0.020(3) -0.004(2) 0.009(2) -0.002(3) C7 0.023(3) 0.021(3) 0.019(3) 0.001(2) 0.008(3) -0.003(2) C8 0.027(3) 0.013(3) 0.023(3) -0.002(2) 0.015(3) -0.002(2) C9 0.026(3) 0.012(3) 0.026(3) 0.005(2) 0.011(3) 0.005(2) C10 0.030(3) 0.012(3) 0.023(3) -0.004(2) 0.013(3) -0.003(2) C11 0.038(4) 0.016(3) 0.031(4) 0.001(3) 0.018(3) -0.005(3) N2 0.019(3) 0.016(2) 0.017(2) -0.0022(19) 0.010(2) 0.0023(19) O4 0.026(2) 0.024(2) 0.019(2) -0.0013(17) 0.0102(19) -0.0083(18) O5 0.016(2) 0.014(2) 0.017(2) -0.0025(15) 0.0060(16) 0.0003(16) O6 0.014(2) 0.012(2) 0.0181(19) -0.0013(15) 0.0087(16) 0.0008(15) C12 0.010(3) 0.023(3) 0.024(3) -0.005(2) 0.010(2) -0.003(2) C13 0.024(3) 0.030(4) 0.036(4) -0.005(3) 0.015(3) -0.006(3) C14 0.021(3) 0.037(4) 0.043(4) -0.016(3) 0.013(3) -0.015(3) C15 0.028(4) 0.044(4) 0.032(4) -0.008(3) 0.003(3) -0.011(3) C16 0.031(4) 0.036(4) 0.026(3) 0.001(3) 0.006(3) 0.001(3) C17 0.018(3) 0.021(3) 0.024(3) -0.004(2) 0.009(2) 0.000(2) C18 0.023(3) 0.023(3) 0.018(3) 0.001(2) 0.010(3) 0.005(3) C19 0.022(3) 0.008(3) 0.022(3) 0.000(2) 0.009(2) 0.001(2) C20 0.022(3) 0.014(3) 0.027(3) -0.004(2) 0.012(3) 0.000(2) C21 0.022(3) 0.019(3) 0.023(3) 0.003(2) 0.013(2) 0.001(2) C22 0.028(3) 0.015(3) 0.033(4) -0.003(3) 0.014(3) 0.003(3) N3 0.019(3) 0.018(3) 0.015(2) 0.0058(19) 0.008(2) 0.0008(19) O7 0.019(2) 0.032(2) 0.018(2) -0.0049(18) 0.0054(18) -0.0015(18) O8 0.017(2) 0.013(2) 0.018(2) 0.0021(15) 0.0052(16) 0.0008(15) O9 0.027(2) 0.020(2) 0.0133(19) 0.0040(16) 0.0082(17) 0.0077(18) C23 0.023(3) 0.024(3) 0.021(3) 0.006(2) 0.006(3) -0.005(3) C24 0.034(4) 0.033(4) 0.026(3) -0.001(3) 0.003(3) -0.004(3) C25 0.039(4) 0.047(5) 0.035(4) -0.002(3) -0.006(3) -0.014(4) C26 0.021(4) 0.052(5) 0.068(6) -0.001(4) -0.002(4) -0.004(4) C27 0.020(4) 0.038(4) 0.063(5) -0.002(4) -0.001(4) 0.005(3) C28 0.024(3) 0.027(4) 0.032(4) 0.006(3) 0.007(3) -0.004(3) C29 0.022(3) 0.020(3) 0.029(3) 0.004(3) 0.011(3) 0.003(3) C30 0.026(3) 0.016(3) 0.022(3) 0.002(2) 0.009(2) 0.001(2) C31 0.023(3) 0.013(3) 0.024(3) 0.002(2) 0.006(2) -0.001(2) C32 0.024(3) 0.020(3) 0.020(3) 0.003(2) 0.008(2) 0.009(2) C33 0.037(4) 0.019(3) 0.028(3) 0.006(3) 0.012(3) 0.007(3) N4 0.022(3) 0.014(2) 0.017(2) -0.0004(19) 0.010(2) 0.003(2) O10 0.027(2) 0.026(2) 0.026(2) -0.0086(18) 0.013(2) -0.0034(18) O11 0.016(2) 0.017(2) 0.017(2) -0.0013(16) 0.0082(16) 0.0012(16) O12 0.017(2) 0.0112(19) 0.0156(19) 0.0052(15) 0.0077(16) 0.0036(15) C34 0.020(3) 0.031(4) 0.018(3) -0.001(3) 0.006(2) 0.004(3) C35 0.041(4) 0.029(4) 0.029(3) -0.009(3) 0.012(3) -0.001(3) C36 0.047(4) 0.030(4) 0.034(4) -0.012(3) 0.018(3) 0.008(3) C37 0.046(4) 0.040(4) 0.034(4) -0.002(3) 0.027(3) 0.013(3) C38 0.040(4) 0.032(4) 0.031(4) 0.002(3) 0.022(3) 0.004(3) C39 0.034(4) 0.023(3) 0.017(3) 0.001(2) 0.012(3) 0.004(3) C40 0.025(3) 0.022(3) 0.020(3) 0.003(2) 0.011(3) -0.001(2) C41 0.026(3) 0.012(3) 0.017(3) 0.003(2) 0.010(2) 0.002(2) C42 0.024(3) 0.010(3) 0.023(3) 0.001(2) 0.012(2) 0.005(2) C43 0.022(3) 0.016(3) 0.020(3) 0.002(2) 0.009(2) -0.005(2) C44 0.038(4) 0.016(3) 0.023(3) 0.004(2) 0.013(3) 0.002(3) O1W 0.063(4) 0.105(6) 0.066(4) -0.018(4) 0.022(4) -0.006(4) O13 0.059(4) 0.121(6) 0.055(4) 0.010(4) 0.023(3) 0.025(4) C45 0.054(5) 0.056(6) 0.055(5) 0.000(4) 0.016(5) 0.005(4) C46 0.069(7) 0.099(9) 0.116(10) -0.012(7) 0.037(7) 0.039(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 O12 2.098(4) 2_655 ? Co1 O12 2.098(4) . ? Co1 O6 2.118(4) . ? Co1 O6 2.118(4) 2_655 ? Co1 Cl1 2.292(2) . ? Co1 Co2 2.9750(9) . ? Co1 Co2 2.9750(9) 2_655 ? Co1 Co4 2.9899(9) 2_655 ? Co1 Co4 2.9899(9) . ? Co2 O5 2.018(4) . ? Co2 O3 2.049(4) . ? Co2 O2 2.065(4) . ? Co2 O6 2.089(4) . ? Co2 O12 2.099(4) 2_655 ? Co2 Cl2 2.6670(10) . ? Co2 Co3 2.9574(10) . ? Co3 O1 1.877(4) . ? Co3 O4 1.884(4) . ? Co3 N1 1.902(5) . ? Co3 N2 1.908(5) . ? Co3 O5 1.920(4) . ? Co3 O2 1.922(4) . ? Co4 O11 2.024(4) 2_655 ? Co4 O9 2.045(4) . ? Co4 O8 2.059(4) . ? Co4 O6 2.078(4) 2_655 ? Co4 O12 2.091(4) 2_655 ? Co4 Cl2 2.7080(11) . ? Co4 Co5 2.9658(10) . ? Co5 O7 1.867(4) . ? Co5 O10 1.882(4) 2_655 ? Co5 N4 1.896(5) 2_655 ? Co5 N3 1.897(5) . ? Co5 O11 1.914(4) 2_655 ? Co5 O8 1.923(4) . ? Cl2 Co2 2.6670(10) 2_655 ? Cl2 Co4 2.7080(11) 2_655 ? N1 C7 1.274(7) . ? N1 C8 1.491(7) . ? O1 C1 1.307(7) . ? O2 C10 1.427(6) . ? O3 C9 1.420(6) . ? C1 C6 1.406(8) . ? C1 C2 1.415(8) . ? C2 C3 1.368(9) . ? C3 C4 1.388(10) . ? C4 C5 1.356(9) . ? C5 C6 1.418(8) . ? C6 C7 1.427(8) . ? C8 C9 1.507(8) . ? C8 C10 1.526(8) . ? C8 C11 1.531(8) . ? N2 C18 1.269(7) . ? N2 C19 1.487(7) . ? O4 C12 1.301(7) . ? O5 C20 1.422(7) . ? O6 C21 1.430(7) . ? O6 Co4 2.078(4) 2_655 ? C12 C13 1.410(8) . ? C12 C17 1.420(8) . ? C13 C14 1.362(9) . ? C14 C15 1.396(10) . ? C15 C16 1.368(9) . ? C16 C17 1.401(9) . ? C17 C18 1.439(8) . ? C19 C22 1.525(8) . ? C19 C20 1.526(8) . ? C19 C21 1.539(7) . ? N3 C29 1.275(8) . ? N3 C30 1.494(7) . ? O7 C23 1.297(7) . ? O8 C31 1.424(6) . ? O9 C32 1.419(7) . ? C23 C24 1.406(9) . ? C23 C28 1.418(9) . ? C24 C25 1.372(10) . ? C25 C26 1.374(11) . ? C26 C27 1.362(11) . ? C27 C28 1.415(9) . ? C28 C29 1.427(9) . ? C30 C33 1.521(8) . ? C30 C32 1.523(8) . ? C30 C31 1.530(8) . ? N4 C40 1.284(7) . ? N4 C41 1.492(7) . ? N4 Co5 1.896(5) 2_655 ? O10 C34 1.304(7) . ? O10 Co5 1.882(4) 2_655 ? O11 C42 1.409(6) . ? O11 Co5 1.914(4) 2_655 ? O11 Co4 2.024(4) 2_655 ? O12 C43 1.433(6) . ? O12 Co4 2.091(4) 2_655 ? O12 Co2 2.099(4) 2_655 ? C34 C35 1.410(8) . ? C34 C39 1.418(9) . ? C35 C36 1.375(9) . ? C36 C37 1.378(10) . ? C37 C38 1.367(9) . ? C38 C39 1.402(8) . ? C39 C40 1.432(8) . ? C41 C43 1.526(8) . ? C41 C44 1.536(7) . ? C41 C42 1.536(7) . ? O13 C45 1.425(10) . ? C45 C46 1.454(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Co1 O12 147.82(19) 2_655 . ? O12 Co1 O6 86.06(14) 2_655 . ? O12 Co1 O6 85.21(14) . . ? O12 Co1 O6 85.21(14) 2_655 2_655 ? O12 Co1 O6 86.06(14) . 2_655 ? O6 Co1 O6 148.1(2) . 2_655 ? O12 Co1 Cl1 106.09(10) 2_655 . ? O12 Co1 Cl1 106.09(10) . . ? O6 Co1 Cl1 105.94(10) . . ? O6 Co1 Cl1 105.94(10) 2_655 . ? O12 Co1 Co2 44.89(10) 2_655 . ? O12 Co1 Co2 112.58(10) . . ? O6 Co1 Co2 44.59(10) . . ? O6 Co1 Co2 112.99(10) 2_655 . ? Cl1 Co1 Co2 125.83(2) . . ? O12 Co1 Co2 112.58(10) 2_655 2_655 ? O12 Co1 Co2 44.89(10) . 2_655 ? O6 Co1 Co2 112.99(10) . 2_655 ? O6 Co1 Co2 44.59(10) 2_655 2_655 ? Cl1 Co1 Co2 125.83(2) . 2_655 ? Co2 Co1 Co2 108.34(4) . 2_655 ? O12 Co1 Co4 113.34(10) 2_655 2_655 ? O12 Co1 Co4 44.38(10) . 2_655 ? O6 Co1 Co4 44.01(10) . 2_655 ? O6 Co1 Co4 113.79(10) 2_655 2_655 ? Cl1 Co1 Co4 125.09(2) . 2_655 ? Co2 Co1 Co4 69.97(3) . 2_655 ? Co2 Co1 Co4 70.70(3) 2_655 2_655 ? O12 Co1 Co4 44.38(10) 2_655 . ? O12 Co1 Co4 113.34(10) . . ? O6 Co1 Co4 113.79(10) . . ? O6 Co1 Co4 44.01(10) 2_655 . ? Cl1 Co1 Co4 125.09(2) . . ? Co2 Co1 Co4 70.70(3) . . ? Co2 Co1 Co4 69.97(3) 2_655 . ? Co4 Co1 Co4 109.82(4) 2_655 . ? O5 Co2 O3 93.00(15) . . ? O5 Co2 O2 80.36(15) . . ? O3 Co2 O2 88.36(15) . . ? O5 Co2 O6 94.02(14) . . ? O3 Co2 O6 172.89(15) . . ? O2 Co2 O6 93.89(15) . . ? O5 Co2 O12 104.26(14) . 2_655 ? O3 Co2 O12 90.43(15) . 2_655 ? O2 Co2 O12 175.29(14) . 2_655 ? O6 Co2 O12 86.78(14) . 2_655 ? O5 Co2 Cl2 172.68(11) . . ? O3 Co2 Cl2 93.63(11) . . ? O2 Co2 Cl2 96.73(11) . . ? O6 Co2 Cl2 79.42(10) . . ? O12 Co2 Cl2 78.79(10) 2_655 . ? O5 Co2 Co3 40.08(11) . . ? O3 Co2 Co3 90.29(11) . . ? O2 Co2 Co3 40.29(10) . . ? O6 Co2 Co3 95.79(10) . . ? O12 Co2 Co3 144.31(10) 2_655 . ? Cl2 Co2 Co3 136.74(4) . . ? O5 Co2 Co1 116.32(11) . . ? O3 Co2 Co1 129.57(11) . . ? O2 Co2 Co1 134.04(11) . . ? O6 Co2 Co1 45.41(10) . . ? O12 Co2 Co1 44.84(10) 2_655 . ? Cl2 Co2 Co1 61.09(4) . . ? Co3 Co2 Co1 138.72(3) . . ? O1 Co3 O4 92.74(18) . . ? O1 Co3 N1 95.79(18) . . ? O4 Co3 N1 86.03(19) . . ? O1 Co3 N2 90.01(18) . . ? O4 Co3 N2 95.15(19) . . ? N1 Co3 N2 174.02(19) . . ? O1 Co3 O5 89.31(17) . . ? O4 Co3 O5 177.94(17) . . ? N1 Co3 O5 93.94(18) . . ? N2 Co3 O5 84.66(18) . . ? O1 Co3 O2 175.88(17) . . ? O4 Co3 O2 91.36(17) . . ? N1 Co3 O2 84.17(17) . . ? N2 Co3 O2 89.93(17) . . ? O5 Co3 O2 86.59(15) . . ? O1 Co3 Co2 131.88(13) . . ? O4 Co3 Co2 135.37(13) . . ? N1 Co3 Co2 88.13(14) . . ? N2 Co3 Co2 86.92(14) . . ? O5 Co3 Co2 42.58(11) . . ? O2 Co3 Co2 44.01(11) . . ? O11 Co4 O9 92.79(16) 2_655 . ? O11 Co4 O8 79.88(15) 2_655 . ? O9 Co4 O8 88.38(15) . . ? O11 Co4 O6 106.86(15) 2_655 2_655 ? O9 Co4 O6 90.22(14) . 2_655 ? O8 Co4 O6 173.19(15) . 2_655 ? O11 Co4 O12 94.17(14) 2_655 2_655 ? O9 Co4 O12 172.89(16) . 2_655 ? O8 Co4 O12 94.24(14) . 2_655 ? O6 Co4 O12 86.40(14) 2_655 2_655 ? O11 Co4 Cl2 170.28(11) 2_655 . ? O9 Co4 Cl2 95.25(12) . . ? O8 Co4 Cl2 94.87(11) . . ? O6 Co4 Cl2 78.62(11) 2_655 . ? O12 Co4 Cl2 77.96(10) 2_655 . ? O11 Co4 Co5 39.75(10) 2_655 . ? O9 Co4 Co5 91.26(11) . . ? O8 Co4 Co5 40.14(11) . . ? O6 Co4 Co5 146.60(11) 2_655 . ? O12 Co4 Co5 95.00(10) 2_655 . ? Cl2 Co4 Co5 134.36(4) . . ? O11 Co4 Co1 117.52(11) 2_655 . ? O9 Co4 Co1 130.04(11) . . ? O8 Co4 Co1 132.95(11) . . ? O6 Co4 Co1 45.11(10) 2_655 . ? O12 Co4 Co1 44.55(10) 2_655 . ? Cl2 Co4 Co1 60.47(4) . . ? Co5 Co4 Co1 137.69(3) . . ? O7 Co5 O10 91.88(18) . 2_655 ? O7 Co5 N4 88.09(19) . 2_655 ? O10 Co5 N4 95.77(19) 2_655 2_655 ? O7 Co5 N3 96.39(19) . . ? O10 Co5 N3 86.65(18) 2_655 . ? N4 Co5 N3 174.8(2) 2_655 . ? O7 Co5 O11 90.96(17) . 2_655 ? O10 Co5 O11 177.16(19) 2_655 2_655 ? N4 Co5 O11 84.35(18) 2_655 2_655 ? N3 Co5 O11 93.01(17) . 2_655 ? O7 Co5 O8 177.08(17) . . ? O10 Co5 O8 90.99(17) 2_655 . ? N4 Co5 O8 91.03(18) 2_655 . ? N3 Co5 O8 84.36(18) . . ? O11 Co5 O8 86.18(16) 2_655 . ? O7 Co5 Co4 133.49(13) . . ? O10 Co5 Co4 134.62(14) 2_655 . ? N4 Co5 Co4 86.25(14) 2_655 . ? N3 Co5 Co4 88.81(14) . . ? O11 Co5 Co4 42.55(11) 2_655 . ? O8 Co5 Co4 43.64(11) . . ? Co2 Cl2 Co2 129.48(8) . 2_655 ? Co2 Cl2 Co4 79.89(4) . . ? Co2 Cl2 Co4 79.02(3) 2_655 . ? Co2 Cl2 Co4 79.02(3) . 2_655 ? Co2 Cl2 Co4 79.89(4) 2_655 2_655 ? Co4 Cl2 Co4 129.23(8) . 2_655 ? C7 N1 C8 119.7(5) . . ? C7 N1 Co3 125.0(4) . . ? C8 N1 Co3 115.2(3) . . ? C1 O1 Co3 124.5(4) . . ? C10 O2 Co3 109.0(3) . . ? C10 O2 Co2 118.4(3) . . ? Co3 O2 Co2 95.70(15) . . ? C9 O3 Co2 133.5(3) . . ? O1 C1 C6 125.4(5) . . ? O1 C1 C2 118.2(5) . . ? C6 C1 C2 116.3(5) . . ? C3 C2 C1 121.7(6) . . ? C2 C3 C4 121.2(6) . . ? C5 C4 C3 118.8(6) . . ? C4 C5 C6 121.4(6) . . ? C1 C6 C5 120.2(5) . . ? C1 C6 C7 122.6(5) . . ? C5 C6 C7 117.3(6) . . ? N1 C7 C6 125.7(6) . . ? N1 C8 C9 110.1(4) . . ? N1 C8 C10 105.4(4) . . ? C9 C8 C10 111.3(5) . . ? N1 C8 C11 112.7(4) . . ? C9 C8 C11 107.8(5) . . ? C10 C8 C11 109.5(5) . . ? O3 C9 C8 111.6(4) . . ? O2 C10 C8 110.0(4) . . ? C18 N2 C19 120.6(5) . . ? C18 N2 Co3 124.5(4) . . ? C19 N2 Co3 114.8(3) . . ? C12 O4 Co3 124.2(3) . . ? C20 O5 Co3 107.6(3) . . ? C20 O5 Co2 116.8(3) . . ? Co3 O5 Co2 97.34(16) . . ? C21 O6 Co4 112.2(3) . 2_655 ? C21 O6 Co2 125.1(3) . . ? Co4 O6 Co2 110.34(16) 2_655 . ? C21 O6 Co1 121.9(3) . . ? Co4 O6 Co1 90.88(14) 2_655 . ? Co2 O6 Co1 90.00(14) . . ? O4 C12 C13 118.6(5) . . ? O4 C12 C17 124.4(5) . . ? C13 C12 C17 117.0(5) . . ? C14 C13 C12 121.6(6) . . ? C13 C14 C15 121.3(6) . . ? C16 C15 C14 118.6(6) . . ? C15 C16 C17 121.6(6) . . ? C16 C17 C12 119.9(5) . . ? C16 C17 C18 117.8(5) . . ? C12 C17 C18 122.3(5) . . ? N2 C18 C17 126.1(6) . . ? N2 C19 C22 111.5(5) . . ? N2 C19 C20 104.8(4) . . ? C22 C19 C20 110.2(5) . . ? N2 C19 C21 111.0(4) . . ? C22 C19 C21 107.9(5) . . ? C20 C19 C21 111.5(5) . . ? O5 C20 C19 111.0(4) . . ? O6 C21 C19 116.5(4) . . ? C29 N3 C30 120.5(5) . . ? C29 N3 Co5 124.0(4) . . ? C30 N3 Co5 115.2(4) . . ? C23 O7 Co5 125.9(4) . . ? C31 O8 Co5 108.8(3) . . ? C31 O8 Co4 118.8(3) . . ? Co5 O8 Co4 96.23(16) . . ? C32 O9 Co4 133.5(3) . . ? O7 C23 C24 118.4(6) . . ? O7 C23 C28 124.4(6) . . ? C24 C23 C28 117.1(6) . . ? C25 C24 C23 121.8(7) . . ? C24 C25 C26 121.1(7) . . ? C27 C26 C25 119.1(7) . . ? C26 C27 C28 121.8(7) . . ? C27 C28 C23 119.1(6) . . ? C27 C28 C29 118.0(6) . . ? C23 C28 C29 122.9(6) . . ? N3 C29 C28 126.4(6) . . ? N3 C30 C33 112.3(5) . . ? N3 C30 C32 110.7(5) . . ? C33 C30 C32 107.8(5) . . ? N3 C30 C31 105.0(4) . . ? C33 C30 C31 110.0(5) . . ? C32 C30 C31 111.0(5) . . ? O8 C31 C30 110.0(4) . . ? O9 C32 C30 112.4(4) . . ? C40 N4 C41 119.9(5) . . ? C40 N4 Co5 124.8(4) . 2_655 ? C41 N4 Co5 115.3(3) . 2_655 ? C34 O10 Co5 124.8(4) . 2_655 ? C42 O11 Co5 108.2(3) . 2_655 ? C42 O11 Co4 116.5(3) . 2_655 ? Co5 O11 Co4 97.71(16) 2_655 2_655 ? C43 O12 Co4 125.0(3) . 2_655 ? C43 O12 Co1 119.9(3) . . ? Co4 O12 Co1 91.08(14) 2_655 . ? C43 O12 Co2 112.9(3) . 2_655 ? Co4 O12 Co2 110.88(16) 2_655 2_655 ? Co1 O12 Co2 90.28(14) . 2_655 ? O10 C34 C35 118.1(6) . . ? O10 C34 C39 125.1(5) . . ? C35 C34 C39 116.8(6) . . ? C36 C35 C34 121.2(6) . . ? C35 C36 C37 121.8(6) . . ? C38 C37 C36 118.5(6) . . ? C37 C38 C39 121.7(7) . . ? C38 C39 C34 120.0(6) . . ? C38 C39 C40 117.5(6) . . ? C34 C39 C40 122.5(5) . . ? N4 C40 C39 125.8(6) . . ? N4 C41 C43 111.2(4) . . ? N4 C41 C44 111.6(4) . . ? C43 C41 C44 107.8(5) . . ? N4 C41 C42 104.0(4) . . ? C43 C41 C42 112.4(4) . . ? C44 C41 C42 109.8(5) . . ? O11 C42 C41 110.6(4) . . ? O12 C43 C41 115.7(4) . . ? O13 C45 C46 108.7(8) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.769 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.109