# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address P.Braunstein ;Laboratoire de Chimie de Coordination CNRS Universit\'e de Strasbourg Institut Le Bel 4, rue Blaise Pascal CS 90032 67081 STRASBOURG cedex FRANCE ; R.Pattacini ;Laboratoire de Chimie de Coordination CNRS Universit\'e de Strasbourg Institut Le Bel 4, rue Blaise Pascal CS 90032 67081 STRASBOURG cedex FRANCE ; J.Zhang ;Department of Chemistry National University of Singapore 3, Science Drive 3, Singapore 117543, Singapore ; A.T.S.Hor ;Department of Chemistry National University of Singapore 3, Science Drive 3, Singapore 117543, Singapore ; P.Teo ;Department of Chemistry National University of Singapore 3, Science Drive 3, Singapore 117543, Singapore ; A.K.Powell ;Institute of Inorganic Chemistry Karlsruhe Institute of Technology (KIT) Engesserstrasse 15, 76131 Karlsruhe, Germany. ; ; Y.Lan ; ;Institute of Inorganic Chemistry Karlsruhe Institute of Technology (KIT) Engesserstrasse 15, 76131 Karlsruhe, Germany. ; _publ_contact_author_address ;Laboratoire de Chimie de Coordination CNRS Universit\'e de Strasbourg Institut Le Bel 4, rue Blaise Pascal CS 90032 67081 STRASBOURG cedex FRANCE ; _publ_contact_author_email braunstein@unistra.fr _publ_contact_author_fax '+ 33 368 851 322' _publ_contact_author_phone '+ 33 368 851 308' _publ_contact_author_name 'Dr Pierre Braunstein' data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 821779' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H72 Co7 N12 O12, 4(C H2 Cl2), 2(Cl)' _chemical_formula_sum 'C76 H80 Cl10 Co7 N12 O12' _chemical_formula_weight 2120.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.495(7) _cell_length_b 14.180(1) _cell_length_c 14.571(1) _cell_angle_alpha 61.785(3) _cell_angle_beta 73.167(4) _cell_angle_gamma 75.014(4) _cell_volume 2154.7(12) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8142 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.42 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1075 _exptl_absorpt_coefficient_mu 1.689 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12470 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.1875 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9116 _reflns_number_gt 3729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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^)+(0.0350P)^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 9116 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2014 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1341 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.011 _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 0.0000 0.5000 0.0289(3) Uani 1 2 d S . . Co2 Co 0.51218(6) -0.09104(6) 0.74243(6) 0.0333(2) Uani 1 1 d . . . Co3 Co 0.60164(6) 0.13102(6) 0.57302(6) 0.0336(2) Uani 1 1 d . . . Co4 Co 0.44788(6) -0.23680(6) 0.66069(6) 0.0324(2) Uani 1 1 d . . . O1 O 0.4526(3) 0.0492(3) 0.6231(3) 0.0294(10) Uani 1 1 d . . . O2 O 0.6413(3) -0.0039(3) 0.6996(3) 0.0417(11) Uani 1 1 d . . . O3 O 0.6368(2) 0.0850(3) 0.4501(3) 0.0278(10) Uani 1 1 d . . . O4 O 0.5375(3) 0.2726(3) 0.4598(3) 0.0357(10) Uani 1 1 d . . . O5 O 0.5736(2) -0.1450(3) 0.6157(3) 0.0264(10) Uani 1 1 d . . . O6 O 0.4057(3) -0.1945(3) 0.7849(3) 0.0371(11) Uani 1 1 d . . . N1 N 0.4024(4) -0.0087(4) 0.8317(4) 0.0379(13) Uani 1 1 d . . . N2 N 0.6257(4) -0.2002(4) 0.8439(4) 0.0331(13) Uani 1 1 d . . . N3 N 0.7740(4) 0.1542(4) 0.5086(4) 0.0378(13) Uani 1 1 d . . . N4 N 0.5335(4) 0.2333(4) 0.6530(4) 0.0362(13) Uani 1 1 d . . . N5 N 0.5815(3) -0.3598(4) 0.7236(4) 0.0355(13) Uani 1 1 d . . . N6 N 0.3009(4) -0.3087(4) 0.7509(4) 0.0414(14) Uani 1 1 d . . . C1 C 0.3934(5) -0.0332(6) 0.9346(6) 0.056(2) Uani 1 1 d . . . H1 H 0.4413 -0.0921 0.9734 0.067 Uiso 1 1 calc R . . C2 C 0.3171(6) 0.0244(5) 0.9846(6) 0.061(2) Uani 1 1 d . . . H2 H 0.3128 0.0049 1.0560 0.074 Uiso 1 1 calc R . . C3 C 0.2464(5) 0.1126(5) 0.9269(6) 0.0543(19) Uani 1 1 d . . . H3 H 0.1943 0.1538 0.9586 0.065 Uiso 1 1 calc R . . C4 C 0.2542(5) 0.1379(5) 0.8227(5) 0.0408(17) Uani 1 1 d . . . H4 H 0.2063 0.1960 0.7831 0.049 Uiso 1 1 calc R . . C5 C 0.3350(4) 0.0758(5) 0.7752(5) 0.0345(16) Uani 1 1 d . . . C6 C 0.3470(4) 0.0988(4) 0.6614(5) 0.0346(16) Uani 1 1 d . . . H6A H 0.2866 0.0724 0.6549 0.041 Uiso 1 1 calc R . . H6B H 0.3400 0.1764 0.6182 0.041 Uiso 1 1 calc R . . C7 C 0.6091(5) -0.3020(5) 0.9197(5) 0.0405(17) Uani 1 1 d . . . H7 H 0.5427 -0.3264 0.9290 0.049 Uiso 1 1 calc R . . C8 C 0.6853(5) -0.3705(5) 0.9831(4) 0.0414(17) Uani 1 1 d . . . H8 H 0.6718 -0.4397 1.0337 0.050 Uiso 1 1 calc R . . C9 C 0.7833(5) -0.3323(5) 0.9688(5) 0.0493(19) Uani 1 1 d . . . H9 H 0.8358 -0.3754 1.0118 0.059 Uiso 1 1 calc R . . C10 C 0.8030(5) -0.2311(5) 0.8913(5) 0.0407(17) Uani 1 1 d . . . H10 H 0.8696 -0.2061 0.8801 0.049 Uiso 1 1 calc R . . C11 C 0.7221(5) -0.1663(5) 0.8298(5) 0.0354(16) Uani 1 1 d . . . C12 C 0.7362(4) -0.0537(4) 0.7439(5) 0.0375(16) Uani 1 1 d . . . H12A H 0.7507 -0.0110 0.7737 0.045 Uiso 1 1 calc R . . H12B H 0.8009 -0.0575 0.6890 0.045 Uiso 1 1 calc R . . C13 C 0.8362(5) 0.2017(5) 0.5311(6) 0.055(2) Uani 1 1 d . . . H13 H 0.8030 0.2291 0.5812 0.067 Uiso 1 1 calc R . . C14 C 0.9479(6) 0.2115(6) 0.4826(7) 0.080(3) Uani 1 1 d . . . H14 H 0.9885 0.2463 0.4986 0.096 Uiso 1 1 calc R . . C15 C 0.9977(5) 0.1697(6) 0.4112(7) 0.078(3) Uani 1 1 d . . . H15 H 1.0732 0.1749 0.3784 0.093 Uiso 1 1 calc R . . C16 C 0.9362(5) 0.1200(5) 0.3879(6) 0.055(2) Uani 1 1 d . . . H16 H 0.9688 0.0917 0.3384 0.066 Uiso 1 1 calc R . . C17 C 0.8240(4) 0.1124(5) 0.4394(5) 0.0351(16) Uani 1 1 d . . . C18 C 0.7526(4) 0.0559(4) 0.4193(4) 0.0296(15) Uani 1 1 d . . . H18A H 0.7697 0.0732 0.3443 0.036 Uiso 1 1 calc R . . H18B H 0.7719 -0.0217 0.4580 0.036 Uiso 1 1 calc R . . C19 C 0.5369(5) 0.2083(5) 0.7540(6) 0.0485(19) Uani 1 1 d . . . H19 H 0.5841 0.1463 0.7894 0.058 Uiso 1 1 calc R . . C20 C 0.4750(5) 0.2688(6) 0.8073(6) 0.056(2) Uani 1 1 d . . . H20 H 0.4808 0.2488 0.8765 0.067 Uiso 1 1 calc R . . C21 C 0.4049(5) 0.3587(5) 0.7566(5) 0.055(2) Uani 1 1 d . . . H21 H 0.3610 0.4008 0.7911 0.066 Uiso 1 1 calc R . . C23 C 0.4659(5) 0.3223(5) 0.6052(5) 0.0366(16) Uani 1 1 d . . . C24 C 0.4635(5) 0.3480(5) 0.4915(5) 0.0416(17) Uani 1 1 d . . . H24A H 0.3875 0.3484 0.4869 0.050 Uiso 1 1 calc R . . H24B H 0.4842 0.4194 0.4441 0.050 Uiso 1 1 calc R . . C25 C 0.5770(5) -0.4647(5) 0.7905(5) 0.0469(19) Uani 1 1 d . . . H25 H 0.5082 -0.4904 0.8127 0.056 Uiso 1 1 calc R . . C26 C 0.6684(5) -0.5350(5) 0.8272(5) 0.054(2) Uani 1 1 d . . . H26 H 0.6612 -0.6064 0.8756 0.065 Uiso 1 1 calc R . . C27 C 0.7717(5) -0.4995(5) 0.7920(5) 0.055(2) Uani 1 1 d . . . H27 H 0.8355 -0.5469 0.8152 0.065 Uiso 1 1 calc R . . C28 C 0.7792(5) -0.3934(5) 0.7224(5) 0.0434(18) Uani 1 1 d . . . H28 H 0.8482 -0.3677 0.6982 0.052 Uiso 1 1 calc R . . C29 C 0.6816(4) -0.3235(5) 0.6876(4) 0.0328(15) Uani 1 1 d . . . C30 C 0.6828(4) -0.2070(4) 0.6112(4) 0.0332(16) Uani 1 1 d . . . H30A H 0.7334 -0.1774 0.6269 0.040 Uiso 1 1 calc R . . H30B H 0.7119 -0.2014 0.5397 0.040 Uiso 1 1 calc R . . C31 C 0.2539(5) -0.3684(5) 0.7294(5) 0.050(2) Uani 1 1 d . . . H31 H 0.2900 -0.3822 0.6705 0.060 Uiso 1 1 calc R . . C32 C 0.1547(5) -0.4117(5) 0.7889(7) 0.063(2) Uani 1 1 d . . . H32 H 0.1252 -0.4543 0.7722 0.076 Uiso 1 1 calc R . . C33 C 0.1027(6) -0.3876(6) 0.8741(7) 0.065(3) Uani 1 1 d . . . H33 H 0.0355 -0.4137 0.9160 0.079 Uiso 1 1 calc R . . C34 C 0.1484(5) -0.3257(6) 0.8979(6) 0.060(2) Uani 1 1 d . . . H34 H 0.1129 -0.3103 0.9559 0.071 Uiso 1 1 calc R . . C35 C 0.2480(5) -0.2862(5) 0.8345(6) 0.0443(19) Uani 1 1 d . . . C36 C 0.3025(5) -0.2169(5) 0.8565(5) 0.0473(19) Uani 1 1 d . . . H36A H 0.2525 -0.1498 0.8488 0.057 Uiso 1 1 calc R . . H36B H 0.3153 -0.2546 0.9287 0.057 Uiso 1 1 calc R . . C37 C 0.9185(8) -0.4408(7) 0.3974(7) 0.113(3) Uani 1 1 d . . . H37A H 0.9976 -0.4712 0.3974 0.136 Uiso 1 1 calc R . . H37B H 0.9017 -0.4249 0.3302 0.136 Uiso 1 1 calc R . . C38 C 1.0674(6) -0.1329(6) 0.1311(7) 0.094(3) Uani 1 1 d . . . H38A H 1.0970 -0.0999 0.0552 0.112 Uiso 1 1 calc R . . H38B H 1.0151 -0.1800 0.1444 0.112 Uiso 1 1 calc R . . Cl1 Cl 0.95709(12) 0.65303(14) 0.13690(15) 0.0566(5) Uani 1 1 d . . . Cl2 Cl 0.8289(3) -0.5334(2) 0.5070(3) 0.1807(17) Uani 1 1 d . . . Cl3 Cl 0.88809(18) -0.32407(19) 0.4182(2) 0.0984(8) Uani 1 1 d . . . Cl4 Cl 1.17952(18) -0.21049(19) 0.1981(2) 0.1024(8) Uani 1 1 d . . . Cl5 Cl 0.99568(19) -0.0325(2) 0.1718(3) 0.1281(11) Uani 1 1 d . . . C22 C 0.3996(5) 0.3864(5) 0.6546(6) 0.0500(19) Uani 1 1 d . . . H22 H 0.3520 0.4477 0.6187 0.060 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 0.0279(6) 0.0282(7) 0.0301(8) -0.0107(6) -0.0094(5) -0.0027(5) Co2 0.0329(4) 0.0329(5) 0.0309(6) -0.0109(4) -0.0122(4) 0.0015(4) Co3 0.0325(4) 0.0322(5) 0.0364(6) -0.0134(4) -0.0120(4) -0.0020(4) Co4 0.0281(4) 0.0317(5) 0.0328(6) -0.0098(4) -0.0073(4) -0.0035(3) O1 0.027(2) 0.033(2) 0.025(2) -0.013(2) -0.0082(18) 0.0064(17) O2 0.040(2) 0.036(3) 0.042(3) -0.004(2) -0.022(2) -0.0014(19) O3 0.0201(19) 0.031(2) 0.029(2) -0.0101(19) -0.0052(17) -0.0018(16) O4 0.039(2) 0.031(2) 0.036(3) -0.018(2) -0.009(2) 0.0050(19) O5 0.0176(18) 0.030(2) 0.028(2) -0.0105(19) -0.0078(17) 0.0029(16) O6 0.034(2) 0.045(3) 0.034(3) -0.022(2) 0.002(2) -0.0076(19) N1 0.046(3) 0.039(3) 0.032(4) -0.019(3) -0.012(3) 0.001(2) N2 0.040(3) 0.035(3) 0.019(3) -0.011(3) -0.009(2) 0.006(2) N3 0.041(3) 0.041(3) 0.037(4) -0.019(3) -0.012(3) -0.005(3) N4 0.035(3) 0.036(3) 0.043(4) -0.023(3) -0.014(3) 0.004(2) N5 0.035(3) 0.031(3) 0.040(4) -0.010(3) -0.013(3) -0.006(2) N6 0.033(3) 0.029(3) 0.055(4) -0.009(3) -0.015(3) -0.003(2) C1 0.063(4) 0.052(5) 0.050(5) -0.031(4) -0.012(4) 0.015(4) C2 0.080(5) 0.055(5) 0.046(5) -0.024(4) -0.026(4) 0.014(4) C3 0.059(4) 0.053(5) 0.052(5) -0.035(4) 0.002(4) 0.001(4) C4 0.046(4) 0.037(4) 0.038(5) -0.018(4) -0.009(3) 0.000(3) C5 0.026(3) 0.031(4) 0.046(5) -0.015(3) -0.011(3) 0.001(3) C6 0.035(3) 0.032(4) 0.042(5) -0.018(3) -0.012(3) -0.004(3) C7 0.038(3) 0.057(5) 0.026(4) -0.022(4) -0.007(3) 0.000(3) C8 0.053(4) 0.034(4) 0.020(4) -0.005(3) -0.005(3) 0.005(3) C9 0.054(4) 0.043(5) 0.043(5) -0.016(4) -0.024(4) 0.016(3) C10 0.034(3) 0.050(5) 0.038(4) -0.016(4) -0.020(3) 0.004(3) C11 0.032(3) 0.039(4) 0.036(4) -0.017(3) -0.012(3) 0.001(3) C12 0.034(3) 0.039(4) 0.044(4) -0.021(3) -0.017(3) 0.003(3) C13 0.051(4) 0.058(5) 0.068(6) -0.030(4) -0.016(4) -0.014(4) C14 0.047(5) 0.090(7) 0.134(9) -0.068(6) -0.012(5) -0.025(4) C15 0.029(4) 0.087(6) 0.139(9) -0.071(6) -0.009(5) -0.009(4) C16 0.029(4) 0.056(5) 0.085(6) -0.037(4) -0.008(4) -0.003(3) C17 0.028(3) 0.031(4) 0.046(5) -0.011(3) -0.018(3) -0.003(3) C18 0.025(3) 0.030(4) 0.030(4) -0.012(3) -0.008(3) 0.003(3) C19 0.052(4) 0.043(5) 0.054(5) -0.024(4) -0.020(4) 0.003(3) C20 0.072(5) 0.058(5) 0.051(5) -0.033(4) -0.027(4) 0.007(4) C21 0.076(5) 0.046(5) 0.042(5) -0.026(4) -0.018(4) 0.011(4) C23 0.040(4) 0.032(4) 0.037(4) -0.012(3) -0.010(3) -0.003(3) C24 0.046(4) 0.037(4) 0.039(5) -0.017(4) -0.006(3) -0.002(3) C25 0.042(4) 0.035(4) 0.053(5) -0.010(4) -0.014(3) -0.002(3) C26 0.055(4) 0.030(4) 0.045(5) 0.008(3) -0.011(4) -0.002(3) C27 0.053(4) 0.044(5) 0.055(5) -0.014(4) -0.023(4) 0.012(4) C28 0.037(3) 0.047(5) 0.040(4) -0.019(4) -0.009(3) 0.005(3) C29 0.032(3) 0.033(4) 0.032(4) -0.014(3) -0.010(3) 0.002(3) C30 0.029(3) 0.032(4) 0.032(4) -0.011(3) -0.007(3) 0.003(3) C31 0.038(4) 0.031(4) 0.065(5) -0.009(4) -0.016(4) 0.003(3) C32 0.042(4) 0.038(5) 0.089(7) -0.008(5) -0.012(4) -0.013(3) C33 0.037(4) 0.045(5) 0.081(7) -0.002(5) -0.004(4) -0.011(4) C34 0.043(4) 0.050(5) 0.052(5) -0.004(4) 0.002(4) -0.002(4) C35 0.028(3) 0.035(4) 0.046(5) -0.002(4) -0.003(3) -0.003(3) C36 0.036(3) 0.056(5) 0.028(4) -0.007(4) -0.002(3) 0.002(3) C37 0.165(9) 0.104(8) 0.063(7) -0.037(6) -0.027(7) 0.001(7) C38 0.084(6) 0.081(7) 0.136(9) -0.055(6) -0.043(6) -0.004(5) Cl1 0.0461(9) 0.0615(12) 0.0696(14) -0.0366(11) -0.0139(9) -0.0002(8) Cl2 0.174(3) 0.086(2) 0.265(5) -0.023(3) -0.124(3) -0.005(2) Cl3 0.1000(16) 0.0910(18) 0.125(2) -0.0568(17) -0.0558(16) 0.0122(13) Cl4 0.0972(16) 0.0926(19) 0.120(2) -0.0404(16) -0.0455(16) -0.0020(13) Cl5 0.0923(16) 0.114(2) 0.218(3) -0.108(2) -0.041(2) 0.0050(15) C22 0.063(4) 0.031(4) 0.053(5) -0.018(4) -0.018(4) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.101(4) . ? Co1 O1 2.101(4) 2_656 ? Co1 O3 2.103(3) . ? Co1 O3 2.103(3) 2_656 ? Co1 O5 2.135(3) 2_656 ? Co1 O5 2.135(3) . ? Co2 O6 1.995(4) . ? Co2 O2 2.058(4) . ? Co2 O1 2.061(3) . ? Co2 N2 2.123(4) . ? Co2 N1 2.124(5) . ? Co2 O5 2.190(4) . ? Co3 O2 2.002(3) . ? Co3 O4 2.049(3) . ? Co3 O3 2.080(4) . ? Co3 N3 2.128(5) . ? Co3 N4 2.138(5) . ? Co3 O1 2.207(3) . ? Co4 O4 1.995(4) 2_656 ? Co4 O6 2.055(4) . ? Co4 O5 2.061(3) . ? Co4 N6 2.108(5) . ? Co4 N5 2.130(4) . ? Co4 O3 2.210(3) 2_656 ? O1 C6 1.418(6) . ? O2 C12 1.379(5) . ? O3 C18 1.398(5) . ? O3 Co4 2.210(3) 2_656 ? O4 C24 1.386(6) . ? O4 Co4 1.995(4) 2_656 ? O5 C30 1.422(5) . ? O6 C36 1.404(6) . ? N1 C5 1.331(6) . ? N1 C1 1.345(7) . ? N2 C11 1.337(6) . ? N2 C7 1.365(7) . ? N3 C17 1.329(7) . ? N3 C13 1.339(7) . ? N4 C23 1.323(6) . ? N4 C19 1.352(7) . ? N5 C29 1.343(6) . ? N5 C25 1.344(7) . ? N6 C31 1.332(7) . ? N6 C35 1.348(8) . ? C1 C2 1.366(8) . ? C1 H1 0.9300 . ? C2 C3 1.385(8) . ? C2 H2 0.9300 . ? C3 C4 1.363(8) . ? C3 H3 0.9300 . ? C4 C5 1.410(8) . ? C4 H4 0.9300 . ? C5 C6 1.498(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.373(7) . ? C7 H7 0.9300 . ? C8 C9 1.386(8) . ? C8 H8 0.9300 . ? C9 C10 1.373(8) . ? C9 H9 0.9300 . ? C10 C11 1.391(7) . ? C10 H10 0.9300 . ? C11 C12 1.507(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.379(8) . ? C13 H13 0.9300 . ? C14 C15 1.355(10) . ? C14 H14 0.9300 . ? C15 C16 1.364(9) . ? C15 H15 0.9300 . ? C16 C17 1.390(7) . ? C16 H16 0.9300 . ? C17 C18 1.507(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.369(8) . ? C19 H19 0.9300 . ? C20 C21 1.359(8) . ? C20 H20 0.9300 . ? C21 C22 1.363(8) . ? C21 H21 0.9300 . ? C23 C22 1.384(8) . ? C23 C24 1.526(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.359(7) . ? C25 H25 0.9300 . ? C26 C27 1.374(8) . ? C26 H26 0.9300 . ? C27 C28 1.371(8) . ? C27 H27 0.9300 . ? C28 C29 1.409(7) . ? C28 H28 0.9300 . ? C29 C30 1.494(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.390(8) . ? C31 H31 0.9300 . ? C32 C33 1.378(10) . ? C32 H32 0.9300 . ? C33 C34 1.371(9) . ? C33 H33 0.9300 . ? C34 C35 1.386(8) . ? C34 H34 0.9300 . ? C35 C36 1.517(9) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 Cl3 1.749(9) . ? C37 Cl2 1.808(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 Cl5 1.735(8) . ? C38 Cl4 1.763(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C22 H22 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 O1 Co1 O1 180.00(8) . 2_656 ? O1 Co1 O3 84.22(14) . . ? O1 Co1 O3 95.78(14) 2_656 . ? O1 Co1 O3 95.78(14) . 2_656 ? O1 Co1 O3 84.22(14) 2_656 2_656 ? O3 Co1 O3 180.00(18) . 2_656 ? O1 Co1 O5 96.76(13) . 2_656 ? O1 Co1 O5 83.24(13) 2_656 2_656 ? O3 Co1 O5 84.30(12) . 2_656 ? O3 Co1 O5 95.70(12) 2_656 2_656 ? O1 Co1 O5 83.24(13) . . ? O1 Co1 O5 96.76(13) 2_656 . ? O3 Co1 O5 95.70(12) . . ? O3 Co1 O5 84.30(12) 2_656 . ? O5 Co1 O5 180.0(3) 2_656 . ? O6 Co2 O2 171.23(14) . . ? O6 Co2 O1 105.27(14) . . ? O2 Co2 O1 81.11(13) . . ? O6 Co2 N2 96.79(17) . . ? O2 Co2 N2 76.57(16) . . ? O1 Co2 N2 157.64(17) . . ? O6 Co2 N1 93.69(17) . . ? O2 Co2 N1 93.43(17) . . ? O1 Co2 N1 79.13(16) . . ? N2 Co2 N1 103.33(18) . . ? O6 Co2 O5 78.98(14) . . ? O2 Co2 O5 96.12(14) . . ? O1 Co2 O5 82.84(13) . . ? N2 Co2 O5 98.14(15) . . ? N1 Co2 O5 158.01(14) . . ? O2 Co3 O4 170.78(15) . . ? O2 Co3 O3 105.44(15) . . ? O4 Co3 O3 80.91(14) . . ? O2 Co3 N3 92.22(16) . . ? O4 Co3 N3 95.63(16) . . ? O3 Co3 N3 78.79(17) . . ? O2 Co3 N4 96.94(18) . . ? O4 Co3 N4 76.29(17) . . ? O3 Co3 N4 157.09(16) . . ? N3 Co3 N4 105.53(19) . . ? O2 Co3 O1 78.84(13) . . ? O4 Co3 O1 95.69(13) . . ? O3 Co3 O1 82.14(13) . . ? N3 Co3 O1 155.95(17) . . ? N4 Co3 O1 97.74(15) . . ? O4 Co4 O6 170.87(13) 2_656 . ? O4 Co4 O5 105.85(15) 2_656 . ? O6 Co4 O5 80.71(14) . . ? O4 Co4 N6 95.4(2) 2_656 . ? O6 Co4 N6 77.7(2) . . ? O5 Co4 N6 158.3(2) . . ? O4 Co4 N5 93.94(16) 2_656 . ? O6 Co4 N5 93.52(16) . . ? O5 Co4 N5 79.40(15) . . ? N6 Co4 N5 103.81(17) . . ? O4 Co4 O3 78.99(14) 2_656 2_656 ? O6 Co4 O3 95.74(14) . 2_656 ? O5 Co4 O3 83.41(12) . 2_656 ? N6 Co4 O3 96.70(14) . 2_656 ? N5 Co4 O3 158.88(16) . 2_656 ? C6 O1 Co2 111.9(3) . . ? C6 O1 Co1 130.3(3) . . ? Co2 O1 Co1 99.35(15) . . ? C6 O1 Co3 117.9(3) . . ? Co2 O1 Co3 96.39(12) . . ? Co1 O1 Co3 94.84(13) . . ? C12 O2 Co3 135.8(3) . . ? C12 O2 Co2 119.4(3) . . ? Co3 O2 Co2 103.23(14) . . ? C18 O3 Co3 112.2(3) . . ? C18 O3 Co1 131.0(3) . . ? Co3 O3 Co1 98.67(14) . . ? C18 O3 Co4 118.2(3) . 2_656 ? Co3 O3 Co4 95.81(14) . 2_656 ? Co1 O3 Co4 94.27(11) . 2_656 ? C24 O4 Co4 132.2(3) . 2_656 ? C24 O4 Co3 118.6(4) . . ? Co4 O4 Co3 103.90(17) 2_656 . ? C30 O5 Co4 111.8(3) . . ? C30 O5 Co1 132.0(3) . . ? Co4 O5 Co1 97.77(12) . . ? C30 O5 Co2 117.7(3) . . ? Co4 O5 Co2 96.57(13) . . ? Co1 O5 Co2 94.38(13) . . ? C36 O6 Co2 134.9(4) . . ? C36 O6 Co4 119.2(4) . . ? Co2 O6 Co4 103.20(16) . . ? C5 N1 C1 119.1(5) . . ? C5 N1 Co2 112.8(4) . . ? C1 N1 Co2 128.1(4) . . ? C11 N2 C7 118.0(4) . . ? C11 N2 Co2 116.6(4) . . ? C7 N2 Co2 125.3(4) . . ? C17 N3 C13 117.9(5) . . ? C17 N3 Co3 113.5(4) . . ? C13 N3 Co3 128.6(5) . . ? C23 N4 C19 116.3(5) . . ? C23 N4 Co3 116.1(4) . . ? C19 N4 Co3 126.6(4) . . ? C29 N5 C25 118.8(4) . . ? C29 N5 Co4 112.6(4) . . ? C25 N5 Co4 128.6(4) . . ? C31 N6 C35 118.3(6) . . ? C31 N6 Co4 126.1(5) . . ? C35 N6 Co4 115.5(4) . . ? N1 C1 C2 122.9(6) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 118.6(7) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 119.0(6) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.8(6) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 120.5(6) . . ? N1 C5 C6 117.1(5) . . ? C4 C5 C6 122.4(5) . . ? O1 C6 C5 111.7(4) . . ? O1 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? O1 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 123.4(6) . . ? N2 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C7 C8 C9 117.4(6) . . ? C7 C8 H8 121.3 . . ? C9 C8 H8 121.3 . . ? C10 C9 C8 120.2(5) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.3(6) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N2 C11 C10 121.6(6) . . ? N2 C11 C12 115.5(5) . . ? C10 C11 C12 122.8(5) . . ? O2 C12 C11 111.5(5) . . ? O2 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? O2 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? N3 C13 C14 122.3(7) . . ? N3 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 119.2(7) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 119.4(7) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 118.7(7) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? N3 C17 C16 122.3(6) . . ? N3 C17 C18 116.4(5) . . ? C16 C17 C18 121.3(6) . . ? O3 C18 C17 112.7(5) . . ? O3 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? O3 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? N4 C19 C20 123.9(6) . . ? N4 C19 H19 118.1 . . ? C20 C19 H19 118.1 . . ? C21 C20 C19 118.4(7) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C20 C21 C22 119.3(7) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? N4 C23 C22 123.0(6) . . ? N4 C23 C24 115.0(6) . . ? C22 C23 C24 122.0(5) . . ? O4 C24 C23 111.2(5) . . ? O4 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? O4 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? N5 C25 C26 122.9(6) . . ? N5 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C25 C26 C27 119.3(6) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C28 C27 C26 119.0(6) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 119.4(6) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? N5 C29 C28 120.5(5) . . ? N5 C29 C30 116.8(4) . . ? C28 C29 C30 122.7(5) . . ? O5 C30 C29 112.3(4) . . ? O5 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? O5 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? N6 C31 C32 124.5(7) . . ? N6 C31 H31 117.7 . . ? C32 C31 H31 117.7 . . ? C33 C32 C31 115.9(7) . . ? C33 C32 H32 122.0 . . ? C31 C32 H32 122.0 . . ? C34 C33 C32 121.1(7) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 119.2(8) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? N6 C35 C34 121.0(7) . . ? N6 C35 C36 117.2(5) . . ? C34 C35 C36 121.7(7) . . ? O6 C36 C35 109.7(5) . . ? O6 C36 H36A 109.7 . . ? C35 C36 H36A 109.7 . . ? O6 C36 H36B 109.7 . . ? C35 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? Cl3 C37 Cl2 105.2(5) . . ? Cl3 C37 H37A 110.7 . . ? Cl2 C37 H37A 110.7 . . ? Cl3 C37 H37B 110.7 . . ? Cl2 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? Cl5 C38 Cl4 111.8(5) . . ? Cl5 C38 H38A 109.3 . . ? Cl4 C38 H38A 109.3 . . ? Cl5 C38 H38B 109.3 . . ? Cl4 C38 H38B 109.3 . . ? H38A C38 H38B 107.9 . . ? C21 C22 C23 119.1(6) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.305 _refine_diff_density_min -1.211 _refine_diff_density_rms 0.120 data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 821780' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C72 H72 Co6 N12 Na O12, 2(C H2 Cl2), Cl' _chemical_formula_sum 'C74 H76 Cl5 Co6 N12 Na O12' _chemical_melting_point ? _exptl_crystal_description Block _exptl_crystal_colour Orange _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1879.29 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' 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' Na Na 0.0362 0.0249 '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' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2761(7) _cell_length_b 13.5914(9) _cell_length_c 14.2153(9) _cell_angle_alpha 93.097(1) _cell_angle_beta 95.183(1) _cell_angle_gamma 90.982(1) _cell_volume 1973.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8863 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.48 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 958 _exptl_absorpt_coefficient_mu 1.474 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4717 _exptl_absorpt_correction_T_max 0.8203 _exptl_absorpt_process_details ; R.H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38 ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 21040 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9021 _reflns_number_gt 7698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. dichloromethane molecule was found disordered in two positions with equal occupancy factors ; _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^)+(0.0793P)^2^+2.9667P] 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 9021 _refine_ls_number_parameters 524 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.39363(4) 0.63998(3) 0.34130(3) 0.01633(11) Uani 1 1 d . . . Co2 Co 0.48015(4) 0.42558(3) 0.28213(3) 0.01646(11) Uani 1 1 d . . . Co3 Co 0.55138(4) 0.27919(3) 0.44540(3) 0.01710(11) Uani 1 1 d . . . Cl1 Cl 0.96439(16) 0.97399(11) 0.09057(13) 0.0296(3) Uani 0.50 1 d P . . Na1 Na 0.5000 0.5000 0.5000 0.0130(3) Uani 1 2 d S . . O1 O 0.4701(2) 0.76202(15) 0.42287(15) 0.0213(4) Uani 1 1 d . . . O2 O 0.33630(19) 0.60778(15) 0.47158(15) 0.0177(4) Uani 1 1 d . . . O3 O 0.3358(2) 0.52737(15) 0.24780(15) 0.0205(4) Uani 1 1 d . . . O4 O 0.56081(19) 0.54572(15) 0.35790(14) 0.0174(4) Uani 1 1 d . . . O5 O 0.6037(2) 0.31677(16) 0.31486(16) 0.0239(5) Uani 1 1 d . . . O6 O 0.4021(2) 0.37150(15) 0.40789(15) 0.0181(4) Uani 1 1 d . . . N1 N 0.4881(2) 0.72477(18) 0.24261(18) 0.0188(5) Uani 1 1 d . . . N2 N 0.2001(2) 0.70035(18) 0.33545(18) 0.0198(5) Uani 1 1 d . . . N3 N 0.3389(3) 0.34282(19) 0.18789(18) 0.0206(5) Uani 1 1 d . . . N4 N 0.6126(3) 0.48066(18) 0.18566(18) 0.0195(5) Uani 1 1 d . . . N5 N 0.7069(3) 0.18170(18) 0.42139(19) 0.0213(5) Uani 1 1 d . . . N6 N 0.4030(3) 0.17494(19) 0.38235(18) 0.0223(5) Uani 1 1 d . . . C1 C 0.4914(3) 0.6994(2) 0.1502(2) 0.0236(6) Uani 1 1 d . . . H1 H 0.4378 0.6475 0.1235 0.028 Uiso 1 1 calc R . . C2 C 0.5707(4) 0.7471(3) 0.0934(2) 0.0298(7) Uani 1 1 d . . . H2 H 0.5712 0.7276 0.0297 0.036 Uiso 1 1 calc R . . C3 C 0.6501(4) 0.8249(3) 0.1335(3) 0.0315(7) Uani 1 1 d . . . H3 H 0.7054 0.8580 0.0970 0.038 Uiso 1 1 calc R . . C4 C 0.6460(3) 0.8526(2) 0.2276(2) 0.0267(7) Uani 1 1 d . . . H4 H 0.6969 0.9055 0.2552 0.032 Uiso 1 1 calc R . . C5 C 0.5643(3) 0.8001(2) 0.2813(2) 0.0194(6) Uani 1 1 d . . . C6 C 0.5620(3) 0.8207(2) 0.3868(2) 0.0218(6) Uani 1 1 d . . . H6A H 0.6476 0.8088 0.4182 0.026 Uiso 1 1 calc R . . H6B H 0.5423 0.8894 0.3995 0.026 Uiso 1 1 calc R . . C7 C 0.1444(3) 0.7603(2) 0.2723(2) 0.0236(6) Uani 1 1 d . . . H7 H 0.1903 0.7761 0.2215 0.028 Uiso 1 1 calc R . . C8 C 0.0218(3) 0.8000(2) 0.2790(3) 0.0271(7) Uani 1 1 d . . . H8 H -0.0145 0.8407 0.2336 0.033 Uiso 1 1 calc R . . C9 C -0.0447(3) 0.7765(2) 0.3561(3) 0.0301(7) Uani 1 1 d . . . H9 H -0.1261 0.8028 0.3641 0.036 Uiso 1 1 calc R . . C10 C 0.0110(3) 0.7139(2) 0.4205(2) 0.0261(7) Uani 1 1 d . . . H10 H -0.0330 0.6969 0.4719 0.031 Uiso 1 1 calc R . . C11 C 0.1338(3) 0.6765(2) 0.4079(2) 0.0204(6) Uani 1 1 d . . . C12 C 0.2019(3) 0.6062(2) 0.4753(2) 0.0208(6) Uani 1 1 d . . . H12A H 0.1823 0.6242 0.5394 0.025 Uiso 1 1 calc R . . H12B H 0.1680 0.5398 0.4592 0.025 Uiso 1 1 calc R . . C13 C 0.3533(3) 0.2494(2) 0.1534(2) 0.0246(6) Uani 1 1 d . . . H13 H 0.4344 0.2204 0.1633 0.030 Uiso 1 1 calc R . . C14 C 0.2513(4) 0.1954(2) 0.1036(2) 0.0299(7) Uani 1 1 d . . . H14 H 0.2644 0.1319 0.0791 0.036 Uiso 1 1 calc R . . C15 C 0.1304(4) 0.2373(3) 0.0910(3) 0.0349(8) Uani 1 1 d . . . H15 H 0.0601 0.2021 0.0588 0.042 Uiso 1 1 calc R . . C16 C 0.1151(3) 0.3330(3) 0.1271(2) 0.0297(7) Uani 1 1 d . . . H16 H 0.0343 0.3627 0.1193 0.036 Uiso 1 1 calc R . . C17 C 0.2221(3) 0.3840(2) 0.1752(2) 0.0213(6) Uani 1 1 d . . . C18 C 0.2126(3) 0.4885(2) 0.2179(2) 0.0217(6) Uani 1 1 d . . . H18A H 0.1702 0.5296 0.1711 0.026 Uiso 1 1 calc R . . H18B H 0.1599 0.4880 0.2711 0.026 Uiso 1 1 calc R . . C19 C 0.6211(3) 0.4570(2) 0.0942(2) 0.0269(7) Uani 1 1 d . . . H19 H 0.5569 0.4154 0.0623 0.032 Uiso 1 1 calc R . . C20 C 0.7211(4) 0.4913(3) 0.0443(3) 0.0347(8) Uani 1 1 d . . . H20 H 0.7224 0.4753 -0.0200 0.042 Uiso 1 1 calc R . . C21 C 0.8188(4) 0.5499(3) 0.0933(3) 0.0369(9) Uani 1 1 d . . . H21 H 0.8887 0.5726 0.0626 0.044 Uiso 1 1 calc R . . C22 C 0.8115(3) 0.5744(3) 0.1883(2) 0.0290(7) Uani 1 1 d . . . H22 H 0.8766 0.6135 0.2223 0.035 Uiso 1 1 calc R . . C23 C 0.7051(3) 0.5397(2) 0.2324(2) 0.0195(6) Uani 1 1 d . . . C24 C 0.6862(3) 0.5674(2) 0.3352(2) 0.0190(6) Uani 1 1 d . . . H24A H 0.7484 0.5322 0.3756 0.023 Uiso 1 1 calc R . . H24B H 0.7044 0.6374 0.3476 0.023 Uiso 1 1 calc R . . C25 C 0.7431(3) 0.1089(2) 0.4772(2) 0.0242(6) Uani 1 1 d . . . H25 H 0.7100 0.1067 0.5358 0.029 Uiso 1 1 calc R . . C26 C 0.8282(3) 0.0364(2) 0.4507(3) 0.0271(7) Uani 1 1 d . . . H26 H 0.8519 -0.0136 0.4906 0.033 Uiso 1 1 calc R . . C27 C 0.8768(3) 0.0408(2) 0.3633(3) 0.0295(7) Uani 1 1 d . . . H27 H 0.9338 -0.0068 0.3434 0.035 Uiso 1 1 calc R . . C28 C 0.8405(3) 0.1157(2) 0.3062(2) 0.0261(7) Uani 1 1 d . . . H28 H 0.8725 0.1192 0.2473 0.031 Uiso 1 1 calc R . . C29 C 0.7549(3) 0.1869(2) 0.3376(2) 0.0215(6) Uani 1 1 d . . . C30 C 0.7104(3) 0.2733(2) 0.2803(2) 0.0241(6) Uani 1 1 d . . . H30A H 0.7813 0.3216 0.2821 0.029 Uiso 1 1 calc R . . H30B H 0.6884 0.2505 0.2148 0.029 Uiso 1 1 calc R . . C31 C 0.4149(4) 0.0818(2) 0.3494(2) 0.0281(7) Uani 1 1 d . . . H31 H 0.4965 0.0533 0.3569 0.034 Uiso 1 1 calc R . . C32 C 0.3114(4) 0.0257(3) 0.3046(3) 0.0329(8) Uani 1 1 d . . . H32 H 0.3233 -0.0389 0.2825 0.040 Uiso 1 1 calc R . . C33 C 0.1903(4) 0.0678(3) 0.2934(3) 0.0323(8) Uani 1 1 d . . . H33 H 0.1190 0.0324 0.2629 0.039 Uiso 1 1 calc R . . C34 C 0.1766(3) 0.1642(3) 0.3285(2) 0.0277(7) Uani 1 1 d . . . H34 H 0.0955 0.1937 0.3231 0.033 Uiso 1 1 calc R . . C35 C 0.2859(3) 0.2160(2) 0.3719(2) 0.0211(6) Uani 1 1 d . . . C36 C 0.2822(3) 0.3236(2) 0.4088(2) 0.0203(6) Uani 1 1 d . . . H36A H 0.2168 0.3575 0.3699 0.024 Uiso 1 1 calc R . . H36B H 0.2568 0.3261 0.4729 0.024 Uiso 1 1 calc R . . C1S C 0.2734(8) 0.8768(5) 1.0375(6) 0.088(3) Uani 0.857(3) 1 d PD A 1 H1S1 H 0.3288 0.8726 1.0960 0.106 Uiso 0.857(3) 1 calc PR A 1 H1S2 H 0.1987 0.9163 1.0505 0.106 Uiso 0.857(3) 1 calc PR A 1 Cl1A Cl 0.3588(3) 0.9311(2) 0.9558(3) 0.1327(13) Uani 0.857(3) 1 d PD A 1 Cl1B Cl 0.22164(13) 0.76159(11) 0.99511(10) 0.0540(4) Uani 0.857(3) 1 d PD A 1 Cl2A Cl 0.4108(5) 0.9207(4) 0.9072(4) 0.0183(14) Uani 0.143(3) 1 d PD A 2 Cl2B Cl 0.3300(8) 0.9303(5) 1.0974(5) 0.042(2) Uani 0.143(3) 1 d PD A 2 C2S C 0.299(4) 0.873(3) 0.9839(16) 0.088(3) Uani 0.143(3) 1 d PD A 2 H2S1 H 0.2098 0.8853 0.9592 0.106 Uiso 0.143(3) 1 calc PR A 2 H2S2 H 0.3086 0.8024 0.9869 0.106 Uiso 0.143(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01471(19) 0.01449(19) 0.0199(2) 0.00233(14) 0.00137(15) -0.00068(14) Co2 0.0159(2) 0.01416(19) 0.0193(2) 0.00121(14) 0.00124(15) -0.00092(14) Co3 0.0171(2) 0.01391(19) 0.0205(2) 0.00185(15) 0.00219(15) 0.00106(14) Cl1 0.0255(8) 0.0184(7) 0.0421(9) 0.0019(6) -0.0123(7) 0.0006(6) Na1 0.0132(7) 0.0105(7) 0.0154(7) 0.0022(5) 0.0012(6) 0.0007(5) O1 0.0233(11) 0.0184(10) 0.0223(10) 0.0017(8) 0.0041(8) -0.0061(8) O2 0.0142(9) 0.0167(10) 0.0224(10) 0.0043(8) 0.0016(8) -0.0001(8) O3 0.0158(10) 0.0178(10) 0.0269(11) -0.0003(8) -0.0022(8) -0.0011(8) O4 0.0140(9) 0.0172(10) 0.0211(10) 0.0016(8) 0.0022(8) -0.0006(8) O5 0.0245(11) 0.0223(11) 0.0267(11) 0.0068(9) 0.0075(9) 0.0086(9) O6 0.0152(10) 0.0171(10) 0.0219(10) 0.0020(8) 0.0016(8) -0.0014(8) N1 0.0171(12) 0.0166(11) 0.0227(12) 0.0043(9) 0.0006(9) 0.0008(9) N2 0.0170(12) 0.0167(12) 0.0252(13) 0.0017(10) -0.0014(10) 0.0000(9) N3 0.0233(13) 0.0187(12) 0.0197(12) 0.0017(10) 0.0024(10) -0.0048(10) N4 0.0215(12) 0.0157(11) 0.0215(12) 0.0033(9) 0.0016(10) 0.0009(9) N5 0.0203(12) 0.0169(12) 0.0265(13) -0.0003(10) 0.0018(10) 0.0013(10) N6 0.0260(13) 0.0184(12) 0.0220(12) 0.0018(10) 0.0001(10) -0.0022(10) C1 0.0244(15) 0.0213(15) 0.0247(15) 0.0037(12) -0.0013(12) -0.0015(12) C2 0.0377(19) 0.0307(17) 0.0214(15) 0.0060(13) 0.0038(14) -0.0029(14) C3 0.0325(18) 0.0300(17) 0.0333(18) 0.0088(14) 0.0076(14) -0.0067(14) C4 0.0282(17) 0.0224(15) 0.0296(16) 0.0055(13) 0.0021(13) -0.0076(13) C5 0.0181(14) 0.0167(13) 0.0233(14) 0.0051(11) 0.0000(11) 0.0011(11) C6 0.0234(15) 0.0147(13) 0.0273(16) 0.0017(11) 0.0022(12) -0.0039(11) C7 0.0208(15) 0.0197(14) 0.0296(16) 0.0018(12) -0.0013(12) -0.0011(11) C8 0.0235(16) 0.0184(15) 0.0381(18) 0.0034(13) -0.0061(13) 0.0026(12) C9 0.0166(15) 0.0231(16) 0.050(2) -0.0009(14) 0.0015(14) 0.0028(12) C10 0.0175(14) 0.0251(15) 0.0358(17) -0.0008(13) 0.0058(13) -0.0022(12) C11 0.0156(14) 0.0159(13) 0.0291(15) 0.0000(11) 0.0001(11) -0.0022(11) C12 0.0163(14) 0.0196(14) 0.0271(15) 0.0042(12) 0.0032(11) -0.0023(11) C13 0.0290(16) 0.0219(15) 0.0233(15) 0.0016(12) 0.0047(12) -0.0035(12) C14 0.041(2) 0.0224(15) 0.0258(16) -0.0030(13) 0.0043(14) -0.0077(14) C15 0.039(2) 0.0319(18) 0.0311(18) -0.0039(14) -0.0052(15) -0.0134(15) C16 0.0255(17) 0.0315(17) 0.0307(17) 0.0010(14) -0.0034(13) -0.0069(14) C17 0.0229(15) 0.0211(14) 0.0195(14) 0.0034(11) 0.0003(11) -0.0051(12) C18 0.0174(14) 0.0213(15) 0.0257(15) 0.0015(12) -0.0010(11) -0.0029(11) C19 0.0312(17) 0.0250(16) 0.0242(15) -0.0011(12) 0.0028(13) -0.0021(13) C20 0.046(2) 0.0336(18) 0.0256(17) -0.0009(14) 0.0129(15) -0.0049(16) C21 0.038(2) 0.039(2) 0.0361(19) 0.0018(16) 0.0196(16) -0.0086(16) C22 0.0254(16) 0.0296(17) 0.0325(17) 0.0006(14) 0.0073(14) -0.0065(13) C23 0.0192(14) 0.0161(13) 0.0234(14) 0.0025(11) 0.0017(11) 0.0008(11) C24 0.0160(13) 0.0182(13) 0.0232(14) 0.0025(11) 0.0033(11) -0.0005(11) C25 0.0246(15) 0.0202(14) 0.0274(16) 0.0020(12) -0.0005(12) 0.0005(12) C26 0.0227(16) 0.0177(14) 0.0403(19) 0.0042(13) -0.0032(14) 0.0015(12) C27 0.0193(15) 0.0194(15) 0.049(2) -0.0044(14) 0.0048(14) 0.0037(12) C28 0.0204(15) 0.0242(15) 0.0336(17) -0.0042(13) 0.0045(13) 0.0018(12) C29 0.0176(14) 0.0184(14) 0.0276(15) -0.0023(12) 0.0002(12) -0.0019(11) C30 0.0222(15) 0.0265(16) 0.0243(15) 0.0025(12) 0.0039(12) 0.0050(12) C31 0.0327(18) 0.0189(15) 0.0319(17) 0.0030(13) -0.0011(14) -0.0032(13) C32 0.046(2) 0.0206(16) 0.0311(18) -0.0003(13) -0.0003(15) -0.0098(15) C33 0.0338(19) 0.0314(18) 0.0303(17) -0.0018(14) 0.0010(14) -0.0175(15) C34 0.0225(16) 0.0300(17) 0.0303(17) 0.0020(13) 0.0028(13) -0.0071(13) C35 0.0241(15) 0.0216(14) 0.0179(13) 0.0042(11) 0.0032(11) -0.0062(12) C36 0.0162(14) 0.0221(14) 0.0229(14) 0.0029(11) 0.0027(11) -0.0028(11) C1S 0.073(5) 0.065(4) 0.119(8) -0.030(5) -0.020(5) 0.033(4) Cl1A 0.130(3) 0.0749(15) 0.191(4) 0.0479(19) -0.020(2) 0.0047(16) Cl1B 0.0438(7) 0.0668(9) 0.0482(7) -0.0065(6) -0.0106(5) 0.0201(6) Cl2A 0.011(2) 0.021(2) 0.023(3) -0.0114(19) 0.0093(17) 0.0020(17) Cl2B 0.059(5) 0.034(4) 0.033(3) -0.001(3) -0.004(3) 0.013(3) C2S 0.073(5) 0.065(4) 0.119(8) -0.030(5) -0.020(5) 0.033(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.017(2) . ? Co1 O2 2.060(2) . ? Co1 O1 2.073(2) . ? Co1 N1 2.150(2) . ? Co1 N2 2.161(3) . ? Co1 O4 2.164(2) . ? Co1 Na1 3.1612(4) . ? Co2 O5 2.012(2) . ? Co2 O4 2.029(2) . ? Co2 O3 2.089(2) . ? Co2 N3 2.144(3) . ? Co2 N4 2.169(3) . ? Co2 O6 2.182(2) . ? Co2 Na1 3.1932(4) . ? Co3 O1 2.013(2) 2_666 ? Co3 O6 2.050(2) . ? Co3 O5 2.066(2) . ? Co3 N5 2.132(3) . ? Co3 O2 2.141(2) 2_666 ? Co3 N6 2.163(3) . ? Co3 Na1 3.1248(4) . ? Na1 O2 2.273(2) 2_666 ? Na1 O2 2.273(2) . ? Na1 O4 2.282(2) 2_666 ? Na1 O4 2.282(2) . ? Na1 O6 2.287(2) 2_666 ? Na1 O6 2.287(2) . ? Na1 Co3 3.1248(4) 2_666 ? Na1 Co1 3.1612(4) 2_666 ? Na1 Co2 3.1933(4) 2_666 ? O1 C6 1.377(4) . ? O1 Co3 2.013(2) 2_666 ? O2 C12 1.387(3) . ? O2 Co3 2.141(2) 2_666 ? O3 C18 1.384(4) . ? O4 C24 1.387(3) . ? O5 C30 1.371(4) . ? O6 C36 1.385(3) . ? N1 C5 1.341(4) . ? N1 C1 1.344(4) . ? N2 C11 1.337(4) . ? N2 C7 1.341(4) . ? N3 C17 1.334(4) . ? N3 C13 1.352(4) . ? N4 C19 1.333(4) . ? N4 C23 1.339(4) . ? N5 C29 1.335(4) . ? N5 C25 1.338(4) . ? N6 C35 1.335(4) . ? N6 C31 1.338(4) . ? C1 C2 1.376(5) . ? C2 C3 1.390(5) . ? C3 C4 1.375(5) . ? C4 C5 1.396(4) . ? C5 C6 1.514(4) . ? C7 C8 1.388(4) . ? C8 C9 1.392(5) . ? C9 C10 1.376(5) . ? C10 C11 1.391(4) . ? C11 C12 1.523(4) . ? C13 C14 1.386(5) . ? C14 C15 1.376(5) . ? C15 C16 1.388(5) . ? C16 C17 1.394(4) . ? C17 C18 1.523(4) . ? C19 C20 1.389(5) . ? C20 C21 1.383(5) . ? C21 C22 1.382(5) . ? C22 C23 1.396(4) . ? C23 C24 1.520(4) . ? C25 C26 1.387(4) . ? C26 C27 1.384(5) . ? C27 C28 1.371(5) . ? C28 C29 1.401(4) . ? C29 C30 1.519(4) . ? C31 C32 1.383(5) . ? C32 C33 1.379(6) . ? C33 C34 1.390(5) . ? C34 C35 1.392(4) . ? C35 C36 1.529(4) . ? C1S Cl1B 1.706(7) . ? C1S Cl1A 1.708(9) . ? Cl2A C2S 1.79(2) . ? Cl2B C2S 1.753(19) . ? 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 O3 Co1 O2 108.39(9) . . ? O3 Co1 O1 171.76(9) . . ? O2 Co1 O1 79.58(8) . . ? O3 Co1 N1 95.71(9) . . ? O2 Co1 N1 155.85(9) . . ? O1 Co1 N1 76.29(9) . . ? O3 Co1 N2 92.61(9) . . ? O2 Co1 N2 78.39(9) . . ? O1 Co1 N2 91.06(9) . . ? N1 Co1 N2 102.69(10) . . ? O3 Co1 O4 79.38(8) . . ? O2 Co1 O4 92.00(8) . . ? O1 Co1 O4 98.59(8) . . ? N1 Co1 O4 90.83(9) . . ? N2 Co1 O4 164.98(9) . . ? O3 Co1 Na1 93.82(6) . . ? O2 Co1 Na1 45.85(6) . . ? O1 Co1 Na1 90.38(6) . . ? N1 Co1 Na1 132.95(7) . . ? N2 Co1 Na1 122.78(7) . . ? O4 Co1 Na1 46.21(5) . . ? O5 Co2 O4 104.03(9) . . ? O5 Co2 O3 173.90(9) . . ? O4 Co2 O3 80.92(8) . . ? O5 Co2 N3 99.06(10) . . ? O4 Co2 N3 156.91(9) . . ? O3 Co2 N3 76.00(9) . . ? O5 Co2 N4 90.37(9) . . ? O4 Co2 N4 78.57(9) . . ? O3 Co2 N4 94.16(9) . . ? N3 Co2 N4 102.16(10) . . ? O5 Co2 O6 78.35(8) . . ? O4 Co2 O6 91.00(8) . . ? O3 Co2 O6 98.17(8) . . ? N3 Co2 O6 93.00(9) . . ? N4 Co2 O6 162.41(9) . . ? O5 Co2 Na1 89.59(7) . . ? O4 Co2 Na1 45.35(6) . . ? O3 Co2 Na1 91.50(6) . . ? N3 Co2 Na1 135.24(7) . . ? N4 Co2 Na1 121.74(7) . . ? O6 Co2 Na1 45.74(5) . . ? O1 Co3 O6 107.86(9) 2_666 . ? O1 Co3 O5 171.12(9) 2_666 . ? O6 Co3 O5 80.25(8) . . ? O1 Co3 N5 95.26(10) 2_666 . ? O6 Co3 N5 155.76(9) . . ? O5 Co3 N5 77.22(9) . . ? O1 Co3 O2 79.04(8) 2_666 2_666 ? O6 Co3 O2 93.57(8) . 2_666 ? O5 Co3 O2 97.16(9) . 2_666 ? N5 Co3 O2 97.96(9) . 2_666 ? O1 Co3 N6 92.78(9) 2_666 . ? O6 Co3 N6 78.85(9) . . ? O5 Co3 N6 92.35(10) . . ? N5 Co3 N6 93.19(10) . . ? O2 Co3 N6 166.70(9) 2_666 . ? O1 Co3 Na1 92.55(6) 2_666 . ? O6 Co3 Na1 47.01(6) . . ? O5 Co3 Na1 90.54(6) . . ? N5 Co3 Na1 141.25(7) . . ? O2 Co3 Na1 46.66(5) 2_666 . ? N6 Co3 Na1 124.30(7) . . ? O2 Na1 O2 180.0 2_666 . ? O2 Na1 O4 83.73(7) 2_666 2_666 ? O2 Na1 O4 96.27(7) . 2_666 ? O2 Na1 O4 96.27(7) 2_666 . ? O2 Na1 O4 83.73(7) . . ? O4 Na1 O4 179.998(1) 2_666 . ? O2 Na1 O6 95.88(7) 2_666 2_666 ? O2 Na1 O6 84.13(7) . 2_666 ? O4 Na1 O6 82.25(7) 2_666 2_666 ? O4 Na1 O6 97.75(7) . 2_666 ? O2 Na1 O6 84.13(7) 2_666 . ? O2 Na1 O6 95.87(7) . . ? O4 Na1 O6 97.75(7) 2_666 . ? O4 Na1 O6 82.25(7) . . ? O6 Na1 O6 179.998(1) 2_666 . ? O2 Na1 Co3 136.76(5) 2_666 2_666 ? O2 Na1 Co3 43.24(5) . 2_666 ? O4 Na1 Co3 90.82(5) 2_666 2_666 ? O4 Na1 Co3 89.18(5) . 2_666 ? O6 Na1 Co3 40.97(5) 2_666 2_666 ? O6 Na1 Co3 139.03(5) . 2_666 ? O2 Na1 Co3 43.24(5) 2_666 . ? O2 Na1 Co3 136.76(5) . . ? O4 Na1 Co3 89.18(5) 2_666 . ? O4 Na1 Co3 90.82(5) . . ? O6 Na1 Co3 139.03(5) 2_666 . ? O6 Na1 Co3 40.97(5) . . ? Co3 Na1 Co3 179.999(2) 2_666 . ? O2 Na1 Co1 40.58(5) 2_666 2_666 ? O2 Na1 Co1 139.42(5) . 2_666 ? O4 Na1 Co1 43.20(5) 2_666 2_666 ? O4 Na1 Co1 136.80(5) . 2_666 ? O6 Na1 Co1 87.48(5) 2_666 2_666 ? O6 Na1 Co1 92.52(5) . 2_666 ? Co3 Na1 Co1 119.500(11) 2_666 2_666 ? Co3 Na1 Co1 60.501(11) . 2_666 ? O2 Na1 Co1 139.42(5) 2_666 . ? O2 Na1 Co1 40.57(5) . . ? O4 Na1 Co1 136.80(5) 2_666 . ? O4 Na1 Co1 43.20(5) . . ? O6 Na1 Co1 92.52(5) 2_666 . ? O6 Na1 Co1 87.48(5) . . ? Co3 Na1 Co1 60.500(11) 2_666 . ? Co3 Na1 Co1 119.499(11) . . ? Co1 Na1 Co1 179.999(1) 2_666 . ? O2 Na1 Co2 88.69(5) 2_666 . ? O2 Na1 Co2 91.31(5) . . ? O4 Na1 Co2 140.77(5) 2_666 . ? O4 Na1 Co2 39.23(5) . . ? O6 Na1 Co2 136.91(5) 2_666 . ? O6 Na1 Co2 43.09(5) . . ? Co3 Na1 Co2 119.535(10) 2_666 . ? Co3 Na1 Co2 60.464(10) . . ? Co1 Na1 Co2 120.486(10) 2_666 . ? Co1 Na1 Co2 59.515(10) . . ? O2 Na1 Co2 91.31(5) 2_666 2_666 ? O2 Na1 Co2 88.69(5) . 2_666 ? O4 Na1 Co2 39.23(5) 2_666 2_666 ? O4 Na1 Co2 140.77(5) . 2_666 ? O6 Na1 Co2 43.09(5) 2_666 2_666 ? O6 Na1 Co2 136.91(5) . 2_666 ? Co3 Na1 Co2 60.465(10) 2_666 2_666 ? Co3 Na1 Co2 119.535(10) . 2_666 ? Co1 Na1 Co2 59.514(11) 2_666 2_666 ? Co1 Na1 Co2 120.486(10) . 2_666 ? Co2 Na1 Co2 180.0 . 2_666 ? C6 O1 Co3 132.40(19) . 2_666 ? C6 O1 Co1 118.62(18) . . ? Co3 O1 Co1 101.61(9) 2_666 . ? C12 O2 Co1 113.68(18) . . ? C12 O2 Co3 117.90(18) . 2_666 ? Co1 O2 Co3 97.84(8) . 2_666 ? C12 O2 Na1 135.76(18) . . ? Co1 O2 Na1 93.58(8) . . ? Co3 O2 Na1 90.10(8) 2_666 . ? C18 O3 Co1 131.19(19) . . ? C18 O3 Co2 116.18(18) . . ? Co1 O3 Co2 100.35(9) . . ? C24 O4 Co2 112.37(17) . . ? C24 O4 Co1 126.30(18) . . ? Co2 O4 Co1 97.52(8) . . ? C24 O4 Na1 127.33(18) . . ? Co2 O4 Na1 95.42(8) . . ? Co1 O4 Na1 90.60(7) . . ? C30 O5 Co2 138.4(2) . . ? C30 O5 Co3 118.64(19) . . ? Co2 O5 Co3 102.58(9) . . ? C36 O6 Co3 110.58(17) . . ? C36 O6 Co2 124.89(18) . . ? Co3 O6 Co2 97.45(8) . . ? C36 O6 Na1 132.08(18) . . ? Co3 O6 Na1 92.02(8) . . ? Co2 O6 Na1 91.17(7) . . ? C5 N1 C1 118.9(3) . . ? C5 N1 Co1 115.3(2) . . ? C1 N1 Co1 125.1(2) . . ? C11 N2 C7 118.5(3) . . ? C11 N2 Co1 113.2(2) . . ? C7 N2 Co1 128.3(2) . . ? C17 N3 C13 119.0(3) . . ? C17 N3 Co2 114.9(2) . . ? C13 N3 Co2 125.3(2) . . ? C19 N4 C23 118.8(3) . . ? C19 N4 Co2 130.2(2) . . ? C23 N4 Co2 110.60(19) . . ? C29 N5 C25 119.7(3) . . ? C29 N5 Co3 115.2(2) . . ? C25 N5 Co3 124.3(2) . . ? C35 N6 C31 118.7(3) . . ? C35 N6 Co3 111.6(2) . . ? C31 N6 Co3 129.6(2) . . ? N1 C1 C2 122.7(3) . . ? C1 C2 C3 118.4(3) . . ? C4 C3 C2 119.4(3) . . ? C3 C4 C5 119.1(3) . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 122.4(3) . . ? O1 C6 C5 111.3(2) . . ? N2 C7 C8 123.4(3) . . ? C7 C8 C9 117.5(3) . . ? C10 C9 C8 119.5(3) . . ? C9 C10 C11 119.3(3) . . ? N2 C11 C10 121.9(3) . . ? N2 C11 C12 115.5(3) . . ? C10 C11 C12 122.7(3) . . ? O2 C12 C11 112.2(2) . . ? N3 C13 C14 122.2(3) . . ? C15 C14 C13 118.9(3) . . ? C14 C15 C16 119.0(3) . . ? C15 C16 C17 119.3(3) . . ? N3 C17 C16 121.6(3) . . ? N3 C17 C18 116.0(3) . . ? C16 C17 C18 122.4(3) . . ? O3 C18 C17 110.5(2) . . ? N4 C19 C20 123.2(3) . . ? C21 C20 C19 117.9(3) . . ? C22 C21 C20 119.4(3) . . ? C21 C22 C23 119.1(3) . . ? N4 C23 C22 121.5(3) . . ? N4 C23 C24 116.1(3) . . ? C22 C23 C24 122.4(3) . . ? O4 C24 C23 112.6(2) . . ? N5 C25 C26 122.4(3) . . ? C27 C26 C25 118.0(3) . . ? C28 C27 C26 119.7(3) . . ? C27 C28 C29 119.3(3) . . ? N5 C29 C28 120.8(3) . . ? N5 C29 C30 115.9(3) . . ? C28 C29 C30 123.3(3) . . ? O5 C30 C29 111.3(3) . . ? N6 C31 C32 123.1(3) . . ? C33 C32 C31 118.5(3) . . ? C32 C33 C34 118.8(3) . . ? C33 C34 C35 119.2(3) . . ? N6 C35 C34 121.7(3) . . ? N6 C35 C36 115.1(3) . . ? C34 C35 C36 123.2(3) . . ? O6 C36 C35 112.0(2) . . ? Cl1B C1S Cl1A 109.6(5) . . ? Cl2B C2S Cl2A 109.6(13) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.287 _refine_diff_density_min -1.539 _refine_diff_density_rms 0.131 data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 821781' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 Cl2 Co4 N6 O6, C H2 Cl2' _chemical_formula_sum 'C37 H38 Cl4 Co4 N6 O6' _chemical_formula_weight 1040.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5440(8) _cell_length_b 10.7320(9) _cell_length_c 11.2030(8) _cell_angle_alpha 89.128(4) _cell_angle_beta 65.639(4) _cell_angle_gamma 76.750(4) _cell_volume 1013.41(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13468 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6414 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.99 _reflns_number_total 4390 _reflns_number_gt 3234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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 dichloromethane molecule was found disordered by symmetry over two positions around the symmetry centre. This molecule was refined with constrained anisotropic parameters. ; _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^)+(0.0455P)^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 4390 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.90629(5) 0.39168(4) 0.72952(4) 0.02064(12) Uani 1 1 d . . . Co2 Co 0.88706(5) 0.63977(4) 0.57608(4) 0.02139(13) Uani 1 1 d . . . O1 O 0.8735(2) 0.44964(19) 0.54673(18) 0.0208(4) Uani 1 1 d . . . O2 O 0.8791(2) 0.57739(19) 0.75109(18) 0.0225(5) Uani 1 1 d . . . O3 O 1.0945(2) 0.2782(2) 0.59224(19) 0.0253(5) Uani 1 1 d . . . Cl1 Cl 0.93831(10) 0.32350(8) 0.91783(7) 0.0305(2) Uani 1 1 d . . . Cl2 Cl 0.4990(5) 1.0440(3) 1.0670(4) 0.0602(8) Uani 0.50 1 d P A -1 Cl3 Cl 0.4393(4) 1.0575(2) 0.8333(3) 0.0789(8) Uani 0.50 1 d P A -1 N1 N 0.6798(3) 0.3729(2) 0.7724(2) 0.0220(5) Uani 1 1 d . . . N2 N 0.9143(3) 0.8024(2) 0.6698(2) 0.0262(6) Uani 1 1 d . . . N3 N 1.3564(3) 0.2762(2) 0.3818(2) 0.0264(6) Uani 1 1 d . . . C1 C 0.7432(3) 0.4122(3) 0.5446(3) 0.0256(7) Uani 1 1 d . . . H1A H 0.7806 0.3311 0.4912 0.031 Uiso 1 1 calc R . . H1B H 0.6916 0.4759 0.5037 0.031 Uiso 1 1 calc R . . C2 C 0.6235(3) 0.3975(3) 0.6798(3) 0.0229(7) Uani 1 1 d . . . C3 C 0.4659(4) 0.4081(3) 0.7098(3) 0.0301(7) Uani 1 1 d . . . H3 H 0.4298 0.4233 0.6442 0.036 Uiso 1 1 calc R . . C4 C 0.3609(4) 0.3965(3) 0.8360(3) 0.0374(8) Uani 1 1 d . . . H4 H 0.2539 0.4054 0.8573 0.045 Uiso 1 1 calc R . . C5 C 0.4206(4) 0.3711(4) 0.9305(3) 0.0375(9) Uani 1 1 d . . . H5 H 0.3538 0.3620 1.0166 0.045 Uiso 1 1 calc R . . C6 C 0.5772(4) 0.3598(3) 0.8957(3) 0.0292(7) Uani 1 1 d . . . H6 H 0.6159 0.3422 0.9595 0.035 Uiso 1 1 calc R . . C7 C 0.9570(4) 0.6377(3) 0.8065(3) 0.0250(7) Uani 1 1 d . . . H7A H 1.0694 0.5960 0.7684 0.030 Uiso 1 1 calc R . . H7B H 0.9148 0.6304 0.9006 0.030 Uiso 1 1 calc R . . C8 C 0.9335(3) 0.7773(3) 0.7805(3) 0.0240(7) Uani 1 1 d . . . C9 C 0.9327(4) 0.8738(3) 0.8620(3) 0.0285(7) Uani 1 1 d . . . H9 H 0.9440 0.8546 0.9393 0.034 Uiso 1 1 calc R . . C10 C 0.9149(4) 0.9991(3) 0.8274(3) 0.0365(8) Uani 1 1 d . . . H10 H 0.9156 1.0649 0.8801 0.044 Uiso 1 1 calc R . . C11 C 0.8962(4) 1.0241(3) 0.7132(3) 0.0374(8) Uani 1 1 d . . . H11 H 0.8847 1.1071 0.6872 0.045 Uiso 1 1 calc R . . C12 C 0.8948(4) 0.9251(3) 0.6384(3) 0.0347(8) Uani 1 1 d . . . H12 H 0.8796 0.9433 0.5625 0.042 Uiso 1 1 calc R . . C13 C 1.2321(4) 0.2112(3) 0.6020(3) 0.0316(8) Uani 1 1 d . . . H13A H 1.2280 0.1223 0.6153 0.038 Uiso 1 1 calc R . . H13B H 1.2380 0.2480 0.6778 0.038 Uiso 1 1 calc R . . C14 C 1.3796(4) 0.2157(3) 0.4795(3) 0.0259(7) Uani 1 1 d . . . C15 C 1.5313(4) 0.1608(3) 0.4696(3) 0.0331(8) Uani 1 1 d . . . H15 H 1.5454 0.1187 0.5384 0.040 Uiso 1 1 calc R . . C16 C 1.6601(4) 0.1699(3) 0.3563(3) 0.0363(8) Uani 1 1 d . . . H16 H 1.7624 0.1335 0.3480 0.044 Uiso 1 1 calc R . . C17 C 1.6369(4) 0.2330(3) 0.2555(3) 0.0361(8) Uani 1 1 d . . . H17 H 1.7224 0.2405 0.1783 0.043 Uiso 1 1 calc R . . C18 C 1.4833(4) 0.2845(3) 0.2727(3) 0.0309(8) Uani 1 1 d . . . H18 H 1.4667 0.3273 0.2051 0.037 Uiso 1 1 calc R . . C19 C 0.478(3) 0.984(3) 0.939(2) 0.233(14) Uani 0.50 1 d P A -1 H19A H 0.5762 0.9198 0.8911 0.279 Uiso 0.50 1 calc PR A -1 H19B H 0.3967 0.9368 0.9776 0.279 Uiso 0.50 1 calc PR A -1 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 0.0189(2) 0.0222(2) 0.0198(2) 0.00300(17) -0.00617(18) -0.00700(18) Co2 0.0206(2) 0.0221(2) 0.0186(2) 0.00255(17) -0.00549(18) -0.00506(18) O1 0.0166(11) 0.0245(11) 0.0209(10) 0.0048(9) -0.0059(9) -0.0079(9) O2 0.0281(12) 0.0214(11) 0.0200(10) 0.0040(9) -0.0103(10) -0.0099(10) O3 0.0196(11) 0.0283(12) 0.0196(11) 0.0058(9) -0.0032(9) 0.0000(10) Cl1 0.0356(5) 0.0337(5) 0.0256(4) 0.0070(3) -0.0156(4) -0.0097(4) Cl2 0.0525(19) 0.0670(16) 0.0548(19) -0.0149(13) -0.0157(15) -0.0146(14) Cl3 0.104(2) 0.0582(16) 0.0747(17) 0.0011(13) -0.0393(17) -0.0171(15) N1 0.0203(13) 0.0205(14) 0.0241(13) 0.0011(11) -0.0075(11) -0.0067(11) N2 0.0273(15) 0.0243(15) 0.0233(13) 0.0018(12) -0.0065(12) -0.0074(12) N3 0.0231(14) 0.0262(15) 0.0262(14) 0.0036(12) -0.0063(12) -0.0068(12) C1 0.0234(17) 0.0309(18) 0.0256(16) 0.0017(14) -0.0124(14) -0.0083(14) C2 0.0218(16) 0.0199(16) 0.0255(16) -0.0005(13) -0.0080(14) -0.0060(13) C3 0.0209(17) 0.041(2) 0.0282(17) -0.0002(15) -0.0095(15) -0.0076(15) C4 0.0212(18) 0.054(2) 0.0337(19) 0.0017(18) -0.0061(16) -0.0132(17) C5 0.030(2) 0.056(2) 0.0231(17) 0.0044(17) -0.0034(16) -0.0188(18) C6 0.0282(18) 0.038(2) 0.0213(16) 0.0075(15) -0.0084(15) -0.0128(16) C7 0.0248(17) 0.0281(18) 0.0255(16) 0.0007(14) -0.0122(15) -0.0096(15) C8 0.0190(16) 0.0242(17) 0.0248(16) 0.0011(13) -0.0043(14) -0.0074(14) C9 0.0253(17) 0.0333(19) 0.0261(16) 0.0005(15) -0.0094(15) -0.0084(15) C10 0.033(2) 0.032(2) 0.042(2) -0.0042(17) -0.0106(17) -0.0105(17) C11 0.042(2) 0.0195(18) 0.047(2) 0.0058(16) -0.0149(18) -0.0096(16) C12 0.039(2) 0.030(2) 0.0332(18) 0.0066(16) -0.0115(17) -0.0122(17) C13 0.0250(18) 0.037(2) 0.0284(17) 0.0077(15) -0.0102(15) -0.0022(16) C14 0.0247(17) 0.0216(17) 0.0304(17) 0.0028(14) -0.0108(15) -0.0055(14) C15 0.0268(18) 0.037(2) 0.0327(18) 0.0041(16) -0.0111(16) -0.0058(16) C16 0.0234(18) 0.036(2) 0.047(2) 0.0008(17) -0.0132(17) -0.0046(16) C17 0.0235(18) 0.041(2) 0.0321(19) 0.0021(17) -0.0006(16) -0.0082(16) C18 0.0297(19) 0.0302(19) 0.0256(17) 0.0032(15) -0.0043(15) -0.0081(16) C19 0.053(13) 0.43(4) 0.14(2) -0.12(2) -0.005(12) 0.025(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.955(2) . ? Co1 O3 1.962(2) . ? Co1 N1 2.070(2) . ? Co1 O1 2.2537(17) . ? Co1 Cl1 2.3370(8) . ? Co2 O3 2.0272(18) 2_766 ? Co2 O2 2.0392(18) . ? Co2 O1 2.113(2) . ? Co2 O1 2.116(2) 2_766 ? Co2 N3 2.140(2) 2_766 ? Co2 N2 2.170(3) . ? O1 C1 1.401(3) . ? O1 Co2 2.116(2) 2_766 ? O2 C7 1.404(3) . ? O3 C13 1.392(3) . ? O3 Co2 2.0272(18) 2_766 ? Cl2 C19 1.682(19) . ? Cl3 C19 1.54(3) . ? N1 C2 1.349(3) . ? N1 C6 1.352(4) . ? N2 C8 1.340(4) . ? N2 C12 1.349(4) . ? N3 C14 1.334(3) . ? N3 C18 1.339(4) . ? N3 Co2 2.140(2) 2_766 ? C1 C2 1.507(4) . ? C2 C3 1.376(4) . ? C3 C4 1.379(4) . ? C4 C5 1.392(4) . ? C5 C6 1.356(4) . ? C7 C8 1.505(4) . ? C8 C9 1.389(4) . ? C9 C10 1.386(4) . ? C10 C11 1.377(4) . ? C11 C12 1.369(5) . ? C13 C14 1.517(4) . ? C14 C15 1.391(4) . ? C15 C16 1.377(4) . ? C16 C17 1.378(4) . ? C17 C18 1.376(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 O2 Co1 O3 122.82(8) . . ? O2 Co1 N1 103.63(9) . . ? O3 Co1 N1 121.66(9) . . ? O2 Co1 O1 79.88(7) . . ? O3 Co1 O1 78.55(7) . . ? N1 Co1 O1 77.01(8) . . ? O2 Co1 Cl1 102.37(6) . . ? O3 Co1 Cl1 100.60(6) . . ? N1 Co1 Cl1 101.74(7) . . ? O1 Co1 Cl1 177.67(5) . . ? O3 Co2 O2 172.20(8) 2_766 . ? O3 Co2 O1 105.96(8) 2_766 . ? O2 Co2 O1 81.53(7) . . ? O3 Co2 O1 80.53(7) 2_766 2_766 ? O2 Co2 O1 99.15(7) . 2_766 ? O1 Co2 O1 78.58(8) . 2_766 ? O3 Co2 N3 78.23(8) 2_766 2_766 ? O2 Co2 N3 103.69(9) . 2_766 ? O1 Co2 N3 94.63(8) . 2_766 ? O1 Co2 N3 154.95(8) 2_766 2_766 ? O3 Co2 N2 95.70(9) 2_766 . ? O2 Co2 N2 76.67(8) . . ? O1 Co2 N2 157.87(8) . . ? O1 Co2 N2 101.02(9) 2_766 . ? N3 Co2 N2 94.18(10) 2_766 . ? C1 O1 Co2 126.34(18) . . ? C1 O1 Co2 124.28(18) . 2_766 ? Co2 O1 Co2 101.42(8) . 2_766 ? C1 O1 Co1 110.50(15) . . ? Co2 O1 Co1 92.59(7) . . ? Co2 O1 Co1 91.98(7) 2_766 . ? C7 O2 Co1 125.08(17) . . ? C7 O2 Co2 114.70(16) . . ? Co1 O2 Co2 104.47(9) . . ? C13 O3 Co1 127.62(18) . . ? C13 O3 Co2 118.90(18) . 2_766 ? Co1 O3 Co2 104.00(9) . 2_766 ? C2 N1 C6 118.3(2) . . ? C2 N1 Co1 118.41(19) . . ? C6 N1 Co1 122.22(19) . . ? C8 N2 C12 118.2(3) . . ? C8 N2 Co2 113.87(19) . . ? C12 N2 Co2 127.4(2) . . ? C14 N3 C18 118.6(3) . . ? C14 N3 Co2 114.57(19) . 2_766 ? C18 N3 Co2 126.8(2) . 2_766 ? O1 C1 C2 113.0(2) . . ? N1 C2 C3 120.9(3) . . ? N1 C2 C1 115.8(2) . . ? C3 C2 C1 123.2(3) . . ? C2 C3 C4 120.7(3) . . ? C3 C4 C5 117.7(3) . . ? C6 C5 C4 119.3(3) . . ? N1 C6 C5 123.0(3) . . ? O2 C7 C8 109.6(2) . . ? N2 C8 C9 121.6(3) . . ? N2 C8 C7 114.5(3) . . ? C9 C8 C7 123.8(3) . . ? C10 C9 C8 119.5(3) . . ? C11 C10 C9 118.6(3) . . ? C12 C11 C10 119.2(3) . . ? N2 C12 C11 122.9(3) . . ? O3 C13 C14 111.7(2) . . ? N3 C14 C15 121.6(3) . . ? N3 C14 C13 116.5(3) . . ? C15 C14 C13 121.9(3) . . ? C16 C15 C14 119.0(3) . . ? C15 C16 C17 119.7(3) . . ? C18 C17 C16 117.8(3) . . ? N3 C18 C17 123.4(3) . . ? Cl3 C19 Cl2 128(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.680 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.094