# Supplementary 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 _publ_contact_author_name 'Shiping Yang' _publ_contact_author_email SHIPINGY@SHNU.EDU.CN _publ_section_title ; Syntheses, crystal structures, and magnetic properties of three novel cobalt (II) complex containing imidazole derivative Groups ; loop_ _publ_author_name 'Shiping Yang' 'Jia-Min Chen' 'Jing-Jia Sun' # Attachment 'ccdc667565.cif' data_ccdc667565 _database_code_depnum_ccdc_archive 'CCDC 667565' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H51 Cl3 Co2 N12 O4' _chemical_formula_weight 976.13 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 _symmetry_space_group_name_Hall '-C 2yc' 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 25.4578(16) _cell_length_b 13.8919(9) _cell_length_c 27.9785(17) _cell_angle_alpha 90.00 _cell_angle_beta 110.2230(10) _cell_angle_gamma 90.00 _cell_volume 9284.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 10072 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour blue-pueple _exptl_crystal_size_max 0.518 _exptl_crystal_size_mid 0.506 _exptl_crystal_size_min 0.325 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3994.3 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.620 _exptl_absorpt_correction_T_max 0.740 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 23004 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8149 _reflns_number_gt 5676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^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 8149 _refine_ls_number_parameters 589 _refine_ls_number_restraints 123 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1826 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.20877(3) 0.97000(4) 0.96609(2) 0.0372(2) Uani 1 1 d . . . Co2 Co 0.17308(3) 0.99168(4) 0.76176(2) 0.0370(2) Uani 1 1 d . . . Cl1 Cl 0.22242(6) 0.94723(10) 1.04956(5) 0.0607(4) Uani 1 1 d . . . Cl2 Cl 0.15864(6) 0.98225(9) 0.67766(5) 0.0526(3) Uani 1 1 d . . . N1 N 0.28599(16) 0.9806(3) 0.96326(14) 0.0420(9) Uani 1 1 d . . . N2 N 0.37064(18) 0.9669(3) 0.95828(17) 0.0606(12) Uani 1 1 d . . . H2C H 0.3974 0.9416 0.9492 0.073 Uiso 1 1 calc R . . N3 N 0.14508(15) 0.8643(3) 0.77631(13) 0.0396(9) Uani 1 1 d . . . N4 N 0.13791(18) 0.7065(3) 0.78812(16) 0.0571(11) Uani 1 1 d . . . H4A H 0.1500 0.6478 0.7977 0.069 Uiso 1 1 calc R . . N5 N 0.16972(14) 1.0976(2) 0.94884(13) 0.0367(8) Uani 1 1 d . . . N6 N 0.13651(16) 1.2460(3) 0.92838(15) 0.0456(10) Uani 1 1 d . . . H6A H 0.1368 1.3061 0.9184 0.055 Uiso 1 1 calc R . . N7 N 0.25636(15) 1.0137(3) 0.79409(15) 0.0407(9) Uani 1 1 d . . . N8 N 0.34163(17) 1.0762(3) 0.82521(17) 0.0599(12) Uani 1 1 d . . . H8A H 0.3677 1.1176 0.8419 0.072 Uiso 1 1 calc R . . N9 N 0.15879(15) 0.8585(2) 0.93223(13) 0.0385(9) Uani 1 1 d . . . N10 N 0.08432(17) 0.7637(3) 0.90114(16) 0.0553(11) Uani 1 1 d . . . H10A H 0.0507 0.7470 0.8807 0.066 Uiso 1 1 calc R . . N11 N 0.13209(15) 1.1097(2) 0.77154(13) 0.0380(8) Uani 1 1 d . . . N12 N 0.08029(17) 1.2278(3) 0.78597(15) 0.0475(10) Uani 1 1 d . . . H12C H 0.0538 1.2539 0.7951 0.057 Uiso 1 1 calc R . . O1 O 0.52138(18) 0.8416(3) 0.8372(2) 0.0944(14) Uani 1 1 d U . . O2 O 0.60313(17) 0.9123(3) 0.86608(16) 0.0708(10) Uani 1 1 d U . . C1 C 0.3211(2) 1.0548(4) 0.9980(2) 0.0563(13) Uani 1 1 d . . . H1A H 0.3243 1.0414 1.0337 0.068 Uiso 1 1 calc R . . H1B H 0.3046 1.1196 0.9885 0.068 Uiso 1 1 calc R . . C2 C 0.3773(3) 1.0489(5) 0.9922(3) 0.0791(19) Uani 1 1 d . . . H2A H 0.3858 1.1084 0.9767 0.095 Uiso 1 1 calc R . . H2B H 0.4073 1.0374 1.0253 0.095 Uiso 1 1 calc R . . C3 C 0.31804(19) 0.9357(3) 0.94311(17) 0.0410(10) Uani 1 1 d . . . C4 C 0.29975(17) 0.8560(3) 0.90629(16) 0.0353(10) Uani 1 1 d . . . C5 C 0.3357(2) 0.7820(3) 0.90536(18) 0.0449(11) Uani 1 1 d . . . H5 H 0.3731 0.7816 0.9287 0.054 Uiso 1 1 calc R . . C6 C 0.3169(2) 0.7085(3) 0.87011(18) 0.0482(12) Uani 1 1 d . . . H6 H 0.3417 0.6579 0.8694 0.058 Uiso 1 1 calc R . . C7 C 0.2631(2) 0.7077(3) 0.83626(18) 0.0428(11) Uani 1 1 d . . . H7 H 0.2505 0.6556 0.8131 0.051 Uiso 1 1 calc R . . C8 C 0.22701(18) 0.7823(3) 0.83566(15) 0.0348(10) Uani 1 1 d . . . C9 C 0.24538(17) 0.8553(3) 0.87091(15) 0.0360(10) Uani 1 1 d . . . H9 H 0.2205 0.9062 0.8711 0.043 Uiso 1 1 calc R . . C10 C 0.16903(18) 0.7860(3) 0.79936(16) 0.0361(10) Uani 1 1 d . . . C11 C 0.0805(2) 0.7320(4) 0.7574(2) 0.0635(15) Uani 1 1 d . . . H11A H 0.0552 0.7268 0.7773 0.076 Uiso 1 1 calc R . . H11B H 0.0661 0.6908 0.7267 0.076 Uiso 1 1 calc R . . C12 C 0.08671(19) 0.8359(4) 0.74320(19) 0.0521(13) Uani 1 1 d . . . H12A H 0.0821 0.8412 0.7067 0.062 Uiso 1 1 calc R . . H12B H 0.0585 0.8774 0.7501 0.062 Uiso 1 1 calc R . . C13 C 0.1241(2) 1.1088(3) 0.97069(19) 0.0486(12) Uani 1 1 d . . . H13A H 0.1397 1.1106 1.0084 0.058 Uiso 1 1 calc R . . H13B H 0.0970 1.0550 0.9600 0.058 Uiso 1 1 calc R . . C14 C 0.0958(2) 1.2050(4) 0.9492(2) 0.0566(14) Uani 1 1 d . . . H14A H 0.0589 1.1949 0.9223 0.068 Uiso 1 1 calc R . . H14B H 0.0911 1.2462 0.9763 0.068 Uiso 1 1 calc R . . C15 C 0.17308(17) 1.1783(3) 0.92685(16) 0.0359(10) Uani 1 1 d . . . C16 C 0.21428(17) 1.2009(3) 0.90206(16) 0.0355(10) Uani 1 1 d . . . C17 C 0.2359(2) 1.2949(3) 0.90487(19) 0.0498(12) Uani 1 1 d . . . H17 H 0.2239 1.3436 0.9226 0.060 Uiso 1 1 calc R . . C18 C 0.2744(2) 1.3166(4) 0.8819(2) 0.0570(14) Uani 1 1 d . . . H18 H 0.2890 1.3800 0.8842 0.068 Uiso 1 1 calc R . . C19 C 0.2918(2) 1.2464(3) 0.8555(2) 0.0533(13) Uani 1 1 d . . . H19 H 0.3189 1.2614 0.8403 0.064 Uiso 1 1 calc R . . C20 C 0.26971(19) 1.1538(3) 0.85141(17) 0.0398(10) Uani 1 1 d . . . C21 C 0.23188(17) 1.1317(3) 0.87466(15) 0.0342(9) Uani 1 1 d . . . H21 H 0.2174 1.0681 0.8721 0.041 Uiso 1 1 calc R . . C22 C 0.28829(19) 1.0795(3) 0.82295(17) 0.0401(10) Uani 1 1 d . . . C23 C 0.3506(2) 0.9955(4) 0.7966(2) 0.0560(14) Uani 1 1 d . . . H23A H 0.3770 0.9485 0.8190 0.067 Uiso 1 1 calc R . . H23B H 0.3651 1.0167 0.7697 0.067 Uiso 1 1 calc R . . C24 C 0.2922(2) 0.9536(4) 0.7739(2) 0.0515(13) Uani 1 1 d . . . H24A H 0.2789 0.9567 0.7362 0.062 Uiso 1 1 calc R . . H24B H 0.2917 0.8856 0.7843 0.062 Uiso 1 1 calc R . . C25 C 0.1773(2) 0.7599(3) 0.9535(2) 0.0526(13) Uani 1 1 d . . . H25A H 0.1949 0.7621 0.9911 0.063 Uiso 1 1 calc R . . H25B H 0.2044 0.7323 0.9390 0.063 Uiso 1 1 calc R . . C26 C 0.1233(2) 0.7010(4) 0.9376(2) 0.0622(15) Uani 1 1 d . . . H26A H 0.1277 0.6392 0.9218 0.075 Uiso 1 1 calc R . . H26B H 0.1112 0.6879 0.9670 0.075 Uiso 1 1 calc R . . C27 C 0.10724(18) 0.8518(3) 0.90324(16) 0.0374(10) Uani 1 1 d . . . C28 C 0.07406(17) 0.9324(3) 0.87303(15) 0.0357(10) Uani 1 1 d . . . C29 C 0.09793(19) 0.9931(3) 0.84706(16) 0.0367(10) Uani 1 1 d . . . H29 H 0.1350 0.9809 0.8479 0.044 Uiso 1 1 calc R . . C30 C 0.06882(17) 1.0714(3) 0.81976(15) 0.0337(9) Uani 1 1 d . . . C31 C 0.01623(19) 1.0905(3) 0.82003(16) 0.0427(11) Uani 1 1 d . . . H31 H -0.0033 1.1458 0.8029 0.051 Uiso 1 1 calc R . . C32 C -0.0090(2) 1.0296(4) 0.84520(19) 0.0494(12) Uani 1 1 d . . . H32 H -0.0459 1.0428 0.8444 0.059 Uiso 1 1 calc R . . C33 C 0.01937(19) 0.9502(4) 0.87139(18) 0.0452(11) Uani 1 1 d . . . H33 H 0.0019 0.9081 0.8881 0.054 Uiso 1 1 calc R . . C34 C 0.09527(17) 1.1353(3) 0.79203(15) 0.0341(10) Uani 1 1 d . . . C35 C 0.1146(2) 1.2792(3) 0.7618(2) 0.0540(13) Uani 1 1 d . . . H35A H 0.1420 1.3223 0.7861 0.065 Uiso 1 1 calc R . . H35B H 0.0912 1.3172 0.7321 0.065 Uiso 1 1 calc R . . C36 C 0.1435(2) 1.1965(3) 0.74553(19) 0.0495(12) Uani 1 1 d . . . H36A H 0.1283 1.1882 0.7081 0.059 Uiso 1 1 calc R . . H36B H 0.1843 1.2084 0.7561 0.059 Uiso 1 1 calc R . . C37 C 0.5525(3) 0.9147(4) 0.8459(2) 0.0647(13) Uani 1 1 d U . . C38 C 0.5243(3) 1.0107(5) 0.8270(4) 0.104(2) Uani 1 1 d U . . H38A H 0.5523 1.0621 0.8364 0.156 Uiso 1 1 calc R . . H38B H 0.4958 1.0231 0.8426 0.156 Uiso 1 1 calc R . . H38C H 0.5064 1.0086 0.7899 0.156 Uiso 1 1 calc R . . Cl3 Cl 0.45514(10) 1.19815(19) 0.88319(13) 0.0969(9) Uani 0.800(5) 1 d PU A 1 Cl3' Cl 0.4647(4) 1.1988(8) 0.9214(5) 0.0928(14) Uani 0.200(5) 1 d PU A -2 O1W O 0.17221(18) 0.5340(3) 0.84264(17) 0.0610(13) Uani 0.80 1 d PU . . O2W O 0.4278(6) 1.3830(14) 0.9333(5) 0.054(5) Uani 0.20 1 d PU . . O3 O 0.5229(9) 1.2696(16) 1.0085(8) 0.110(6) Uani 0.25 1 d PDU . . C39 C 0.5345(13) 1.3707(16) 1.0086(10) 0.109(11) Uani 0.25 1 d PDU . . C40 C 0.4606(6) 0.8692(9) 0.9128(5) 0.133(5) Uani 0.392(10) 1 d PDU B 1 O4 O 0.4492(5) 0.7944(8) 0.8749(4) 0.092(5) Uani 0.392(10) 1 d PDU B 1 C40' C 0.4606(6) 0.8692(9) 0.9128(5) 0.133(5) Uani 0.239(6) 1 d PDU B -2 O4' O 0.4675(6) 0.9629(9) 0.9351(5) 0.093(5) Uani 0.358(10) 1 d PDU B -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 0.0418(4) 0.0295(4) 0.0386(4) -0.0006(2) 0.0118(3) -0.0016(2) Co2 0.0433(4) 0.0269(3) 0.0441(4) -0.0002(3) 0.0193(3) -0.0016(2) Cl1 0.0821(10) 0.0558(8) 0.0408(7) 0.0044(6) 0.0169(7) -0.0027(7) Cl2 0.0694(9) 0.0475(7) 0.0486(7) 0.0012(5) 0.0301(6) 0.0052(6) N1 0.041(2) 0.036(2) 0.046(2) -0.0089(17) 0.0107(19) -0.0031(17) N2 0.039(2) 0.062(3) 0.076(3) -0.020(2) 0.014(2) -0.011(2) N3 0.043(2) 0.030(2) 0.043(2) 0.0017(16) 0.0124(18) -0.0015(16) N4 0.065(3) 0.029(2) 0.062(3) 0.0062(19) 0.003(2) -0.0121(19) N5 0.040(2) 0.030(2) 0.045(2) 0.0016(16) 0.0210(17) -0.0001(15) N6 0.054(2) 0.029(2) 0.063(3) 0.0056(18) 0.031(2) 0.0039(17) N7 0.039(2) 0.031(2) 0.055(2) -0.0054(17) 0.0203(19) -0.0023(16) N8 0.044(3) 0.057(3) 0.087(3) -0.020(2) 0.033(2) -0.012(2) N9 0.039(2) 0.0279(19) 0.043(2) 0.0030(16) 0.0065(17) 0.0009(16) N10 0.048(2) 0.039(2) 0.062(3) 0.013(2) -0.002(2) -0.0093(19) N11 0.047(2) 0.0272(19) 0.041(2) 0.0049(16) 0.0174(18) 0.0005(16) N12 0.059(3) 0.028(2) 0.063(3) 0.0057(18) 0.032(2) 0.0054(18) O1 0.080(3) 0.055(2) 0.140(4) -0.010(3) 0.027(3) -0.010(2) O2 0.062(2) 0.054(2) 0.095(3) 0.019(2) 0.026(2) 0.0069(18) C1 0.050(3) 0.048(3) 0.057(3) -0.019(3) 0.001(2) -0.008(2) C2 0.060(4) 0.078(4) 0.097(5) -0.035(4) 0.025(4) -0.027(3) C3 0.036(3) 0.039(3) 0.045(3) 0.005(2) 0.010(2) -0.002(2) C4 0.035(2) 0.032(2) 0.039(2) 0.0009(19) 0.014(2) -0.0005(18) C5 0.040(3) 0.045(3) 0.049(3) 0.003(2) 0.014(2) 0.007(2) C6 0.055(3) 0.041(3) 0.052(3) 0.003(2) 0.023(3) 0.013(2) C7 0.055(3) 0.031(2) 0.045(3) -0.003(2) 0.020(2) 0.002(2) C8 0.042(3) 0.028(2) 0.036(2) -0.0004(18) 0.015(2) -0.0024(18) C9 0.037(2) 0.030(2) 0.044(2) -0.0002(19) 0.017(2) 0.0028(18) C10 0.041(3) 0.030(2) 0.038(2) -0.0028(19) 0.014(2) -0.0039(19) C11 0.056(3) 0.048(3) 0.068(3) 0.009(3) -0.002(3) -0.015(3) C12 0.040(3) 0.046(3) 0.058(3) 0.005(2) 0.002(2) -0.008(2) C13 0.056(3) 0.040(3) 0.058(3) -0.003(2) 0.030(3) 0.000(2) C14 0.053(3) 0.046(3) 0.081(4) 0.003(3) 0.037(3) 0.003(2) C15 0.038(2) 0.027(2) 0.042(2) -0.0062(19) 0.013(2) -0.0039(18) C16 0.040(2) 0.029(2) 0.041(2) 0.0003(18) 0.017(2) -0.0030(18) C17 0.071(3) 0.026(2) 0.061(3) -0.010(2) 0.034(3) -0.007(2) C18 0.073(4) 0.034(3) 0.079(4) -0.011(3) 0.045(3) -0.020(2) C19 0.067(3) 0.037(3) 0.070(3) -0.013(2) 0.041(3) -0.018(2) C20 0.045(3) 0.033(2) 0.045(3) -0.004(2) 0.019(2) -0.0025(19) C21 0.041(2) 0.024(2) 0.038(2) -0.0041(18) 0.014(2) -0.0050(18) C22 0.045(3) 0.031(2) 0.048(3) 0.001(2) 0.020(2) -0.001(2) C23 0.049(3) 0.051(3) 0.076(4) -0.010(3) 0.032(3) 0.002(2) C24 0.053(3) 0.044(3) 0.068(3) -0.012(2) 0.033(3) -0.001(2) C25 0.060(3) 0.030(3) 0.060(3) 0.007(2) 0.010(3) -0.002(2) C26 0.061(3) 0.038(3) 0.074(4) 0.016(3) 0.006(3) -0.007(2) C27 0.041(3) 0.032(2) 0.040(2) 0.0013(19) 0.015(2) -0.0038(19) C28 0.033(2) 0.038(2) 0.032(2) 0.0001(19) 0.0059(19) -0.0036(19) C29 0.038(2) 0.033(2) 0.038(2) -0.0017(19) 0.013(2) -0.0019(19) C30 0.036(2) 0.029(2) 0.032(2) -0.0032(18) 0.0065(19) -0.0010(18) C31 0.039(3) 0.043(3) 0.040(2) 0.005(2) 0.006(2) 0.005(2) C32 0.033(3) 0.058(3) 0.056(3) 0.007(2) 0.014(2) 0.003(2) C33 0.036(3) 0.050(3) 0.048(3) 0.005(2) 0.014(2) -0.009(2) C34 0.038(2) 0.027(2) 0.034(2) 0.0015(18) 0.009(2) 0.0042(18) C35 0.066(3) 0.032(3) 0.066(3) 0.009(2) 0.026(3) 0.000(2) C36 0.064(3) 0.034(3) 0.061(3) 0.007(2) 0.034(3) 0.001(2) C37 0.066(3) 0.041(3) 0.090(3) -0.003(3) 0.031(3) 0.003(2) C38 0.089(4) 0.057(3) 0.145(6) 0.011(4) 0.012(4) 0.019(3) Cl3 0.0623(13) 0.0951(16) 0.116(2) -0.0064(17) 0.0087(15) -0.0250(11) Cl3' 0.058(2) 0.092(2) 0.115(3) -0.001(3) 0.013(3) -0.027(2) O1W 0.058(3) 0.041(3) 0.067(3) 0.031(2) 0.001(2) -0.008(2) O2W 0.040(9) 0.105(14) 0.032(8) -0.007(9) 0.030(7) -0.010(9) O3 0.110(6) 0.111(6) 0.110(6) 0.0001(10) 0.038(2) 0.0002(10) C39 0.15(3) 0.12(3) 0.081(17) 0.063(17) 0.076(18) 0.08(2) C40 0.132(5) 0.133(5) 0.133(5) 0.0005(7) 0.0460(18) -0.0002(7) O4 0.091(5) 0.093(5) 0.092(5) 0.0004(10) 0.0322(19) -0.0005(10) C40' 0.132(5) 0.133(5) 0.133(5) 0.0005(7) 0.0460(18) -0.0002(7) O4' 0.092(5) 0.094(5) 0.094(5) 0.0003(10) 0.033(2) 0.0006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.000(4) . ? Co1 N5 2.007(3) . ? Co1 N9 2.020(4) . ? Co1 Cl1 2.2613(13) . ? Co2 N3 2.002(4) . ? Co2 N11 2.012(4) . ? Co2 N7 2.020(4) . ? Co2 Cl2 2.2562(13) . ? N1 C3 1.300(6) . ? N1 C1 1.486(6) . ? N2 C3 1.329(6) . ? N2 C2 1.454(7) . ? N2 H2C 0.8800 . ? N3 C10 1.303(5) . ? N3 C12 1.507(6) . ? N4 C10 1.333(6) . ? N4 C11 1.461(7) . ? N4 H4A 0.8800 . ? N5 C15 1.297(5) . ? N5 C13 1.497(6) . ? N6 C15 1.334(5) . ? N6 C14 1.469(6) . ? N6 H6A 0.8800 . ? N7 C22 1.301(6) . ? N7 C24 1.485(6) . ? N8 C22 1.338(6) . ? N8 C23 1.440(6) . ? N8 H8A 0.8800 . ? N9 C27 1.285(5) . ? N9 C25 1.504(6) . ? N10 C27 1.348(6) . ? N10 C26 1.445(6) . ? N10 H10A 0.8800 . ? N11 C34 1.306(5) . ? N11 C36 1.488(5) . ? N12 C34 1.334(5) . ? N12 C35 1.463(6) . ? N12 H12C 0.8800 . ? O1 C37 1.259(7) . ? O2 C37 1.216(6) . ? C1 C2 1.498(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.474(6) . ? C4 C5 1.383(6) . ? C4 C9 1.396(6) . ? C5 C6 1.384(7) . ? C5 H5 0.9500 . ? C6 C7 1.370(7) . ? C6 H6 0.9500 . ? C7 C8 1.382(6) . ? C7 H7 0.9500 . ? C8 C9 1.379(6) . ? C8 C10 1.475(6) . ? C9 H9 0.9500 . ? C11 C12 1.519(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.538(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.477(6) . ? C16 C21 1.396(6) . ? C16 C17 1.410(6) . ? C17 C18 1.378(6) . ? C17 H17 0.9500 . ? C18 C19 1.386(7) . ? C18 H18 0.9500 . ? C19 C20 1.393(6) . ? C19 H19 0.9500 . ? C20 C21 1.371(6) . ? C20 C22 1.478(6) . ? C21 H21 0.9500 . ? C23 C24 1.519(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.529(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.479(6) . ? C28 C29 1.383(6) . ? C28 C33 1.399(6) . ? C29 C30 1.388(6) . ? C29 H29 0.9500 . ? C30 C31 1.367(6) . ? C30 C34 1.484(6) . ? C31 C32 1.391(6) . ? C31 H31 0.9500 . ? C32 C33 1.382(7) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C35 C36 1.516(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.520(8) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O3 C39 1.435(10) . ? C40 O4 1.441(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N5 109.73(15) . . ? N1 Co1 N9 120.41(15) . . ? N5 Co1 N9 112.62(15) . . ? N1 Co1 Cl1 104.41(12) . . ? N5 Co1 Cl1 104.97(10) . . ? N9 Co1 Cl1 102.94(11) . . ? N3 Co2 N11 117.04(15) . . ? N3 Co2 N7 115.81(14) . . ? N11 Co2 N7 109.21(15) . . ? N3 Co2 Cl2 102.70(11) . . ? N11 Co2 Cl2 106.50(10) . . ? N7 Co2 Cl2 104.07(11) . . ? C3 N1 C1 106.9(4) . . ? C3 N1 Co1 139.0(3) . . ? C1 N1 Co1 113.7(3) . . ? C3 N2 C2 109.9(4) . . ? C3 N2 H2C 125.0 . . ? C2 N2 H2C 125.0 . . ? C10 N3 C12 106.2(4) . . ? C10 N3 Co2 134.4(3) . . ? C12 N3 Co2 116.8(3) . . ? C10 N4 C11 109.3(4) . . ? C10 N4 H4A 125.4 . . ? C11 N4 H4A 125.4 . . ? C15 N5 C13 106.9(3) . . ? C15 N5 Co1 140.3(3) . . ? C13 N5 Co1 112.6(3) . . ? C15 N6 C14 109.5(4) . . ? C15 N6 H6A 125.2 . . ? C14 N6 H6A 125.2 . . ? C22 N7 C24 107.3(4) . . ? C22 N7 Co2 135.9(3) . . ? C24 N7 Co2 115.6(3) . . ? C22 N8 C23 110.8(4) . . ? C22 N8 H8A 124.6 . . ? C23 N8 H8A 124.6 . . ? C27 N9 C25 107.2(4) . . ? C27 N9 Co1 133.7(3) . . ? C25 N9 Co1 116.9(3) . . ? C27 N10 C26 109.6(4) . . ? C27 N10 H10A 125.2 . . ? C26 N10 H10A 125.2 . . ? C34 N11 C36 106.5(3) . . ? C34 N11 Co2 140.1(3) . . ? C36 N11 Co2 113.3(3) . . ? C34 N12 C35 109.8(4) . . ? C34 N12 H12C 125.1 . . ? C35 N12 H12C 125.1 . . ? N1 C1 C2 105.7(4) . . ? N1 C1 H1A 110.6 . . ? C2 C1 H1A 110.6 . . ? N1 C1 H1B 110.6 . . ? C2 C1 H1B 110.6 . . ? H1A C1 H1B 108.7 . . ? N2 C2 C1 102.3(4) . . ? N2 C2 H2A 111.3 . . ? C1 C2 H2A 111.3 . . ? N2 C2 H2B 111.3 . . ? C1 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? N1 C3 N2 114.8(4) . . ? N1 C3 C4 124.7(4) . . ? N2 C3 C4 120.5(4) . . ? C5 C4 C9 118.8(4) . . ? C5 C4 C3 121.4(4) . . ? C9 C4 C3 119.8(4) . . ? C4 C5 C6 119.5(4) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 121.1(4) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 120.2(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 118.9(4) . . ? C9 C8 C10 118.6(4) . . ? C7 C8 C10 122.5(4) . . ? C8 C9 C4 121.4(4) . . ? C8 C9 H9 119.3 . . ? C4 C9 H9 119.3 . . ? N3 C10 N4 115.9(4) . . ? N3 C10 C8 123.7(4) . . ? N4 C10 C8 120.3(4) . . ? N4 C11 C12 102.2(4) . . ? N4 C11 H11A 111.3 . . ? C12 C11 H11A 111.3 . . ? N4 C11 H11B 111.3 . . ? C12 C11 H11B 111.3 . . ? H11A C11 H11B 109.2 . . ? N3 C12 C11 105.0(4) . . ? N3 C12 H12A 110.8 . . ? C11 C12 H12A 110.8 . . ? N3 C12 H12B 110.8 . . ? C11 C12 H12B 110.8 . . ? H12A C12 H12B 108.8 . . ? N5 C13 C14 104.8(4) . . ? N5 C13 H13A 110.8 . . ? C14 C13 H13A 110.8 . . ? N5 C13 H13B 110.8 . . ? C14 C13 H13B 110.8 . . ? H13A C13 H13B 108.9 . . ? N6 C14 C13 101.2(4) . . ? N6 C14 H14A 111.5 . . ? C13 C14 H14A 111.5 . . ? N6 C14 H14B 111.5 . . ? C13 C14 H14B 111.5 . . ? H14A C14 H14B 109.4 . . ? N5 C15 N6 115.7(4) . . ? N5 C15 C16 125.5(4) . . ? N6 C15 C16 118.8(4) . . ? C21 C16 C17 118.4(4) . . ? C21 C16 C15 121.8(4) . . ? C17 C16 C15 119.8(4) . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C20 119.9(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 119.9(4) . . ? C21 C20 C22 120.5(4) . . ? C19 C20 C22 119.6(4) . . ? C20 C21 C16 121.2(4) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? N7 C22 N8 114.3(4) . . ? N7 C22 C20 125.2(4) . . ? N8 C22 C20 120.5(4) . . ? N8 C23 C24 102.1(4) . . ? N8 C23 H23A 111.3 . . ? C24 C23 H23A 111.3 . . ? N8 C23 H23B 111.3 . . ? C24 C23 H23B 111.3 . . ? H23A C23 H23B 109.2 . . ? N7 C24 C23 105.4(4) . . ? N7 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? N7 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? N9 C25 C26 104.2(4) . . ? N9 C25 H25A 110.9 . . ? C26 C25 H25A 110.9 . . ? N9 C25 H25B 110.9 . . ? C26 C25 H25B 110.9 . . ? H25A C25 H25B 108.9 . . ? N10 C26 C25 102.2(4) . . ? N10 C26 H26A 111.3 . . ? C25 C26 H26A 111.3 . . ? N10 C26 H26B 111.3 . . ? C25 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? N9 C27 N10 115.1(4) . . ? N9 C27 C28 124.3(4) . . ? N10 C27 C28 120.6(4) . . ? C29 C28 C33 119.2(4) . . ? C29 C28 C27 119.6(4) . . ? C33 C28 C27 121.2(4) . . ? C28 C29 C30 121.3(4) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C31 C30 C29 119.1(4) . . ? C31 C30 C34 120.6(4) . . ? C29 C30 C34 120.3(4) . . ? C30 C31 C32 120.6(4) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 120.4(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C28 119.3(4) . . ? C32 C33 H33 120.3 . . ? C28 C33 H33 120.3 . . ? N11 C34 N12 115.1(4) . . ? N11 C34 C30 126.2(4) . . ? N12 C34 C30 118.7(4) . . ? N12 C35 C36 101.4(4) . . ? N12 C35 H35A 111.5 . . ? C36 C35 H35A 111.5 . . ? N12 C35 H35B 111.5 . . ? C36 C35 H35B 111.5 . . ? H35A C35 H35B 109.3 . . ? N11 C36 C35 105.7(3) . . ? N11 C36 H36A 110.6 . . ? C35 C36 H36A 110.6 . . ? N11 C36 H36B 110.6 . . ? C35 C36 H36B 110.6 . . ? H36A C36 H36B 108.7 . . ? O2 C37 O1 124.2(5) . . ? O2 C37 C38 119.0(6) . . ? O1 C37 C38 116.7(6) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.099 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.114 # Attachment 'ccdc667566.cif' data_ccdc667566 _database_code_depnum_ccdc_archive 'CCDC 667566' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H42 Cl2 Co2 N12, 2(C H4 O), 2(Cl), O' _chemical_formula_sum 'C38 H50 Cl4 Co2 N12 O3' _chemical_formula_weight 982.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9775(12) _cell_length_b 14.3746(17) _cell_length_c 14.7491(17) _cell_angle_alpha 78.341(2) _cell_angle_beta 88.920(2) _cell_angle_gamma 74.691(2) _cell_volume 2197.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8060 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour blue-pueple _exptl_crystal_size_max 0.477 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.177 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 0.830 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 11570 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.1056 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8185 _reflns_number_gt 5008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0915P)^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 8060 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1964 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.01385(7) 0.86127(5) 0.28644(5) 0.0344(2) Uani 1 1 d . . . Co2 Co 0.50993(7) 0.71796(6) 0.27506(5) 0.0372(2) Uani 1 1 d . . . Cl1 Cl -0.22670(14) 0.92148(12) 0.28008(11) 0.0506(4) Uani 1 1 d . . . Cl2 Cl 0.71909(15) 0.65264(13) 0.26273(12) 0.0580(5) Uani 1 1 d . . . Cl3 Cl 0.29682(17) 0.72227(14) 0.73910(11) 0.0674(5) Uani 1 1 d . . . Cl4 Cl 0.1959(2) 0.35456(19) 0.2331(2) 0.1227(10) Uani 1 1 d . . . O1 O 0.4570(8) 0.2024(5) 0.2350(6) 0.150(3) Uani 1 1 d . . . O2 O 0.2323(7) 0.2501(5) 0.0508(5) 0.109(2) Uani 1 1 d . . . H2D H 0.1925 0.2858 0.0861 0.163 Uiso 1 1 calc R . . O3 O 0.2192(6) 0.6078(4) 0.9205(4) 0.0821(17) Uani 1 1 d . . . H3 H 0.1875 0.6681 0.8995 0.123 Uiso 1 1 calc R . . N1 N 0.0487(4) 0.9760(3) 0.2189(3) 0.0361(11) Uani 1 1 d . . . N2 N 0.0995(5) 1.0981(3) 0.1195(3) 0.0483(13) Uani 1 1 d . . . H2 H 0.1305 1.1261 0.0690 0.058 Uiso 1 1 calc R . . N3 N 0.4312(4) 0.6440(3) 0.2004(3) 0.0376(11) Uani 1 1 d . . . N4 N 0.3663(5) 0.5908(3) 0.0825(3) 0.0483(13) Uani 1 1 d . . . H4 H 0.3276 0.5954 0.0295 0.058 Uiso 1 1 calc R . . N5 N 0.4644(4) 0.8653(3) 0.2265(3) 0.0348(11) Uani 1 1 d . . . N6 N 0.4265(5) 1.0270(4) 0.2041(4) 0.0563(15) Uani 1 1 d . . . H6 H 0.3975 1.0860 0.2169 0.068 Uiso 1 1 calc R . . N7 N 0.0317(4) 0.8250(3) 0.4233(3) 0.0369(11) Uani 1 1 d . . . N8 N 0.0920(5) 0.8046(4) 0.5708(3) 0.0500(13) Uani 1 1 d . . . H8A H 0.1315 0.8144 0.6179 0.060 Uiso 1 1 calc R . . N9 N 0.4863(4) 0.6981(3) 0.4123(3) 0.0379(11) Uani 1 1 d . . . N10 N 0.4526(5) 0.6591(4) 0.5637(3) 0.0603(16) Uani 1 1 d . . . H10 H 0.4245 0.6282 0.6140 0.072 Uiso 1 1 calc R . . N11 N 0.0307(4) 0.7414(3) 0.2308(3) 0.0368(11) Uani 1 1 d . . . N12 N 0.0680(5) 0.5875(4) 0.2092(4) 0.0571(15) Uani 1 1 d . . . H12 H 0.0973 0.5229 0.2226 0.068 Uiso 1 1 calc R . . C1 C -0.0036(6) 1.0702(4) 0.2565(4) 0.0458(15) Uani 1 1 d . . . H1A H -0.0967 1.0850 0.2601 0.055 Uiso 1 1 calc R . . H1B H 0.0333 1.0631 0.3191 0.055 Uiso 1 1 calc R . . C2 C 0.0337(7) 1.1507(4) 0.1888(5) 0.0590(19) Uani 1 1 d . . . H2A H -0.0415 1.2034 0.1610 0.071 Uiso 1 1 calc R . . H2B H 0.0903 1.1798 0.2188 0.071 Uiso 1 1 calc R . . C3 C 0.1067(5) 1.0006(4) 0.1430(4) 0.0354(13) Uani 1 1 d . . . C4 C 0.1721(5) 0.9315(4) 0.0860(4) 0.0314(12) Uani 1 1 d . . . C5 C 0.2363(5) 0.8357(4) 0.1273(4) 0.0327(12) Uani 1 1 d . . . H5 H 0.2370 0.8151 0.1927 0.039 Uiso 1 1 calc R . . C6 C 0.2983(5) 0.7709(4) 0.0751(4) 0.0341(13) Uani 1 1 d . . . C7 C 0.2971(5) 0.7998(4) -0.0218(4) 0.0400(14) Uani 1 1 d . . . H7 H 0.3385 0.7542 -0.0583 0.048 Uiso 1 1 calc R . . C8 C 0.2357(5) 0.8945(4) -0.0632(4) 0.0389(14) Uani 1 1 d . . . H8 H 0.2344 0.9150 -0.1286 0.047 Uiso 1 1 calc R . . C9 C 0.1760(5) 0.9597(4) -0.0099(4) 0.0406(14) Uani 1 1 d . . . H9 H 0.1363 1.0258 -0.0391 0.049 Uiso 1 1 calc R . . C10 C 0.3672(5) 0.6672(4) 0.1207(4) 0.0345(13) Uani 1 1 d . . . C11 C 0.4387(6) 0.4976(4) 0.1409(4) 0.0567(18) Uani 1 1 d . . . H11A H 0.5131 0.4650 0.1090 0.068 Uiso 1 1 calc R . . H11B H 0.3855 0.4516 0.1602 0.068 Uiso 1 1 calc R . . C12 C 0.4778(6) 0.5345(4) 0.2229(4) 0.0524(17) Uani 1 1 d . . . H12A H 0.4398 0.5074 0.2802 0.063 Uiso 1 1 calc R . . H12B H 0.5709 0.5140 0.2323 0.063 Uiso 1 1 calc R . . C13 C 0.4914(7) 1.0067(5) 0.1207(5) 0.0632(19) Uani 1 1 d . . . H13A H 0.5704 1.0281 0.1152 0.076 Uiso 1 1 calc R . . H13B H 0.4367 1.0392 0.0645 0.076 Uiso 1 1 calc R . . C14 C 0.5182(6) 0.8974(5) 0.1364(4) 0.0470(15) Uani 1 1 d . . . H14A H 0.4784 0.8780 0.0861 0.056 Uiso 1 1 calc R . . H14B H 0.6104 0.8669 0.1382 0.056 Uiso 1 1 calc R . . C15 C 0.4176(5) 0.9431(4) 0.2585(4) 0.0379(13) Uani 1 1 d . . . C16 C 0.3518(5) 0.9478(4) 0.3481(4) 0.0362(13) Uani 1 1 d . . . C17 C 0.3753(6) 1.0080(4) 0.4058(4) 0.0457(15) Uani 1 1 d . . . H17 H 0.4325 1.0472 0.3879 0.055 Uiso 1 1 calc R . . C18 C 0.3160(6) 1.0104(5) 0.4881(4) 0.0536(17) Uani 1 1 d . . . H18 H 0.3342 1.0496 0.5280 0.064 Uiso 1 1 calc R . . C19 C 0.2291(6) 0.9557(5) 0.5133(4) 0.0474(16) Uani 1 1 d . . . H19 H 0.1885 0.9579 0.5706 0.057 Uiso 1 1 calc R . . C20 C 0.2011(5) 0.8981(4) 0.4562(4) 0.0359(13) Uani 1 1 d . . . C21 C 0.2646(5) 0.8945(4) 0.3742(4) 0.0340(12) Uani 1 1 d . . . H21 H 0.2477 0.8541 0.3350 0.041 Uiso 1 1 calc R . . C22 C 0.1067(5) 0.8420(4) 0.4812(4) 0.0368(13) Uani 1 1 d . . . C23 C 0.0022(7) 0.7460(6) 0.5787(4) 0.064(2) Uani 1 1 d . . . H23A H -0.0659 0.7674 0.6210 0.077 Uiso 1 1 calc R . . H23B H 0.0440 0.6751 0.6007 0.077 Uiso 1 1 calc R . . C24 C -0.0479(6) 0.7675(5) 0.4795(4) 0.0490(16) Uani 1 1 d . . . H24A H -0.0415 0.7054 0.4582 0.059 Uiso 1 1 calc R . . H24B H -0.1376 0.8061 0.4742 0.059 Uiso 1 1 calc R . . C25 C 0.5760(6) 0.7357(5) 0.4612(4) 0.0510(16) Uani 1 1 d . . . H25A H 0.5660 0.8067 0.4359 0.061 Uiso 1 1 calc R . . H25B H 0.6645 0.6992 0.4543 0.061 Uiso 1 1 calc R . . C26 C 0.5416(7) 0.7192(6) 0.5617(5) 0.072(2) Uani 1 1 d . . . H26A H 0.6169 0.6837 0.6027 0.086 Uiso 1 1 calc R . . H26B H 0.5013 0.7823 0.5805 0.086 Uiso 1 1 calc R . . C27 C 0.4204(5) 0.6584(4) 0.4757(4) 0.0410(14) Uani 1 1 d . . . C28 C 0.3198(5) 0.6133(4) 0.4585(4) 0.0402(14) Uani 1 1 d . . . C29 C 0.2884(6) 0.5398(5) 0.5229(4) 0.0541(17) Uani 1 1 d . . . H29 H 0.3327 0.5171 0.5813 0.065 Uiso 1 1 calc R . . C30 C 0.1949(7) 0.4994(5) 0.5041(5) 0.063(2) Uani 1 1 d . . . H30 H 0.1748 0.4492 0.5496 0.076 Uiso 1 1 calc R . . C31 C 0.1284(6) 0.5307(5) 0.4189(5) 0.0553(18) Uani 1 1 d . . . H31 H 0.0665 0.4998 0.4050 0.066 Uiso 1 1 calc R . . C32 C 0.1540(5) 0.6084(4) 0.3540(4) 0.0419(14) Uani 1 1 d . . . C33 C 0.2493(5) 0.6487(4) 0.3737(4) 0.0380(13) Uani 1 1 d . . . H33 H 0.2675 0.7009 0.3296 0.046 Uiso 1 1 calc R . . C34 C 0.0812(5) 0.6475(4) 0.2625(4) 0.0397(14) Uani 1 1 d . . . C35 C -0.0305(6) 0.7478(4) 0.1397(4) 0.0428(14) Uani 1 1 d . . . H35A H 0.0045 0.7894 0.0898 0.051 Uiso 1 1 calc R . . H35B H -0.1228 0.7769 0.1406 0.051 Uiso 1 1 calc R . . C36 C -0.0030(6) 0.6448(5) 0.1241(5) 0.0579(18) Uani 1 1 d . . . H36A H -0.0819 0.6256 0.1167 0.069 Uiso 1 1 calc R . . H36B H 0.0483 0.6369 0.0688 0.069 Uiso 1 1 calc R . . C37 C 0.3243(9) 0.2903(7) 0.0091(6) 0.103(3) Uani 1 1 d . . . H37A H 0.3164 0.3543 0.0256 0.155 Uiso 1 1 calc R . . H37B H 0.3147 0.2991 -0.0582 0.155 Uiso 1 1 calc R . . H37C H 0.4076 0.2461 0.0303 0.155 Uiso 1 1 calc R . . C38 C 0.1384(9) 0.5541(7) 0.8983(6) 0.097(3) Uani 1 1 d . . . H38A H 0.1055 0.5228 0.9552 0.146 Uiso 1 1 calc R . . H38B H 0.1852 0.5034 0.8658 0.146 Uiso 1 1 calc R . . H38C H 0.0679 0.5987 0.8583 0.146 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 0.0377(5) 0.0335(4) 0.0322(4) -0.0087(3) -0.0005(3) -0.0082(3) Co2 0.0389(5) 0.0411(5) 0.0291(4) -0.0067(3) -0.0003(3) -0.0067(4) Cl1 0.0385(9) 0.0572(10) 0.0532(9) -0.0103(8) -0.0053(7) -0.0083(7) Cl2 0.0425(9) 0.0667(11) 0.0573(10) -0.0085(8) 0.0081(7) -0.0049(8) Cl3 0.0685(12) 0.0816(13) 0.0405(9) -0.0098(9) 0.0024(8) -0.0019(10) Cl4 0.0904(19) 0.0858(18) 0.198(3) -0.0386(19) 0.0194(18) -0.0272(14) O1 0.192(8) 0.104(6) 0.177(8) -0.063(5) -0.015(6) -0.053(5) O2 0.123(6) 0.121(6) 0.097(5) 0.003(4) -0.003(4) -0.075(5) O3 0.112(4) 0.095(4) 0.053(3) -0.001(3) -0.022(3) -0.060(4) N1 0.036(3) 0.032(3) 0.038(3) -0.011(2) 0.002(2) -0.003(2) N2 0.061(4) 0.032(3) 0.050(3) 0.000(2) 0.006(3) -0.017(2) N3 0.042(3) 0.034(3) 0.032(3) -0.005(2) -0.008(2) -0.003(2) N4 0.060(3) 0.041(3) 0.042(3) -0.016(2) -0.012(2) -0.003(3) N5 0.030(3) 0.043(3) 0.030(2) -0.008(2) 0.0021(19) -0.007(2) N6 0.075(4) 0.042(3) 0.051(3) 0.000(3) 0.006(3) -0.022(3) N7 0.039(3) 0.037(3) 0.035(3) -0.009(2) 0.001(2) -0.010(2) N8 0.057(3) 0.066(4) 0.027(3) -0.012(2) 0.004(2) -0.014(3) N9 0.041(3) 0.044(3) 0.029(3) -0.010(2) -0.006(2) -0.008(2) N10 0.065(4) 0.081(4) 0.026(3) -0.003(3) -0.002(2) -0.008(3) N11 0.040(3) 0.032(3) 0.039(3) -0.009(2) -0.002(2) -0.008(2) N12 0.059(4) 0.037(3) 0.080(4) -0.026(3) -0.006(3) -0.010(3) C1 0.053(4) 0.034(3) 0.052(4) -0.019(3) 0.006(3) -0.005(3) C2 0.076(5) 0.035(3) 0.072(5) -0.024(3) 0.027(4) -0.017(3) C3 0.030(3) 0.034(3) 0.038(3) -0.002(3) -0.005(2) -0.005(2) C4 0.028(3) 0.034(3) 0.033(3) -0.005(2) -0.002(2) -0.011(2) C5 0.032(3) 0.036(3) 0.028(3) -0.008(2) -0.001(2) -0.005(2) C6 0.031(3) 0.040(3) 0.030(3) -0.004(2) -0.002(2) -0.009(2) C7 0.044(4) 0.051(4) 0.029(3) -0.012(3) 0.000(2) -0.016(3) C8 0.041(3) 0.041(3) 0.031(3) -0.003(3) -0.003(2) -0.007(3) C9 0.038(3) 0.039(3) 0.038(3) 0.003(3) -0.002(3) -0.008(3) C10 0.031(3) 0.040(3) 0.034(3) -0.014(3) 0.008(2) -0.008(3) C11 0.068(5) 0.033(3) 0.063(4) -0.008(3) -0.013(3) -0.002(3) C12 0.065(4) 0.036(3) 0.048(4) -0.006(3) -0.012(3) -0.001(3) C13 0.073(5) 0.067(5) 0.055(4) -0.006(4) 0.021(4) -0.033(4) C14 0.044(4) 0.061(4) 0.040(3) -0.008(3) 0.007(3) -0.023(3) C15 0.037(3) 0.042(3) 0.036(3) -0.003(3) -0.008(2) -0.015(3) C16 0.036(3) 0.037(3) 0.032(3) -0.006(2) -0.005(2) -0.005(3) C17 0.046(4) 0.046(4) 0.050(4) -0.016(3) -0.004(3) -0.015(3) C18 0.052(4) 0.066(4) 0.053(4) -0.037(3) -0.003(3) -0.015(3) C19 0.044(4) 0.062(4) 0.036(3) -0.021(3) 0.001(3) -0.005(3) C20 0.035(3) 0.038(3) 0.029(3) -0.009(2) -0.005(2) 0.001(3) C21 0.036(3) 0.036(3) 0.030(3) -0.007(2) -0.004(2) -0.009(3) C22 0.034(3) 0.040(3) 0.032(3) -0.013(3) 0.001(2) 0.002(3) C23 0.072(5) 0.075(5) 0.047(4) -0.003(4) 0.009(3) -0.030(4) C24 0.047(4) 0.053(4) 0.047(4) -0.006(3) 0.011(3) -0.017(3) C25 0.053(4) 0.056(4) 0.043(4) -0.009(3) -0.011(3) -0.011(3) C26 0.070(5) 0.099(6) 0.053(5) -0.035(4) -0.007(4) -0.017(5) C27 0.041(4) 0.046(4) 0.029(3) -0.007(3) -0.002(3) 0.001(3) C28 0.041(3) 0.043(3) 0.029(3) -0.001(3) 0.007(2) -0.002(3) C29 0.051(4) 0.054(4) 0.045(4) 0.004(3) 0.002(3) -0.004(3) C30 0.055(5) 0.049(4) 0.067(5) 0.017(4) 0.011(4) -0.004(3) C31 0.047(4) 0.043(4) 0.070(5) 0.004(3) 0.011(3) -0.014(3) C32 0.041(4) 0.031(3) 0.047(4) -0.002(3) 0.007(3) -0.004(3) C33 0.039(3) 0.039(3) 0.035(3) -0.005(3) 0.006(2) -0.010(3) C34 0.028(3) 0.040(3) 0.053(4) -0.016(3) 0.009(3) -0.008(3) C35 0.046(4) 0.044(4) 0.040(3) -0.014(3) -0.004(3) -0.011(3) C36 0.059(4) 0.058(4) 0.062(4) -0.030(4) -0.006(3) -0.011(3) C37 0.105(8) 0.110(8) 0.074(6) -0.012(6) 0.012(5) 0.001(6) C38 0.114(8) 0.107(7) 0.101(7) -0.041(6) 0.006(5) -0.067(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 N11 1.998(4) . ? Co1 N7 2.018(4) . ? Co1 N1 2.023(5) . ? Co1 Cl1 2.2639(17) . ? Co2 N9 2.007(4) . ? Co2 N3 2.021(4) . ? Co2 N5 2.022(5) . ? Co2 Cl2 2.2586(18) . ? O2 C37 1.367(10) . ? O2 H2D 0.8400 . ? O3 C38 1.402(8) . ? O3 H3 0.8400 . ? N1 C3 1.309(7) . ? N1 C1 1.534(7) . ? N2 C3 1.356(7) . ? N2 C2 1.460(8) . ? N2 H2 0.8800 . ? N3 C10 1.317(6) . ? N3 C12 1.489(7) . ? N4 C10 1.335(7) . ? N4 C11 1.471(7) . ? N4 H4 0.8800 . ? N5 C15 1.280(7) . ? N5 C14 1.481(7) . ? N6 C15 1.332(7) . ? N6 C13 1.452(8) . ? N6 H6 0.8800 . ? N7 C22 1.299(7) . ? N7 C24 1.487(7) . ? N8 C22 1.346(7) . ? N8 C23 1.445(8) . ? N8 H8A 0.8800 . ? N9 C27 1.304(7) . ? N9 C25 1.500(7) . ? N10 C27 1.353(7) . ? N10 C26 1.461(9) . ? N10 H10 0.8800 . ? N11 C34 1.307(7) . ? N11 C35 1.489(7) . ? N12 C34 1.315(7) . ? N12 C36 1.464(8) . ? N12 H12 0.8800 . ? C1 C2 1.507(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.466(8) . ? C4 C5 1.389(7) . ? C4 C9 1.393(7) . ? C5 C6 1.364(7) . ? C5 H5 0.9500 . ? C6 C7 1.405(7) . ? C6 C10 1.504(7) . ? C7 C8 1.369(7) . ? C7 H7 0.9500 . ? C8 C9 1.370(8) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C11 C12 1.526(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.491(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.499(8) . ? C16 C21 1.381(7) . ? C16 C17 1.402(7) . ? C17 C18 1.368(8) . ? C17 H17 0.9500 . ? C18 C19 1.389(9) . ? C18 H18 0.9500 . ? C19 C20 1.384(8) . ? C19 H19 0.9500 . ? C20 C21 1.388(7) . ? C20 C22 1.472(8) . ? C21 H21 0.9500 . ? C23 C24 1.517(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.510(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.470(8) . ? C28 C29 1.383(8) . ? C28 C33 1.413(7) . ? C29 C30 1.363(9) . ? C29 H29 0.9500 . ? C30 C31 1.396(9) . ? C30 H30 0.9500 . ? C31 C32 1.402(8) . ? C31 H31 0.9500 . ? C32 C33 1.383(8) . ? C32 C34 1.507(8) . ? C33 H33 0.9500 . ? C35 C36 1.495(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? 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 N11 Co1 N7 110.53(18) . . ? N11 Co1 N1 115.42(18) . . ? N7 Co1 N1 113.22(18) . . ? N11 Co1 Cl1 108.79(14) . . ? N7 Co1 Cl1 103.92(14) . . ? N1 Co1 Cl1 103.99(13) . . ? N9 Co2 N3 118.89(19) . . ? N9 Co2 N5 106.34(18) . . ? N3 Co2 N5 114.10(17) . . ? N9 Co2 Cl2 103.89(14) . . ? N3 Co2 Cl2 102.82(14) . . ? N5 Co2 Cl2 110.10(13) . . ? C37 O2 H2D 109.5 . . ? C38 O3 H3 109.5 . . ? C3 N1 C1 106.8(4) . . ? C3 N1 Co1 139.2(4) . . ? C1 N1 Co1 113.0(3) . . ? C3 N2 C2 111.2(5) . . ? C3 N2 H2 124.4 . . ? C2 N2 H2 124.4 . . ? C10 N3 C12 106.5(4) . . ? C10 N3 Co2 134.9(4) . . ? C12 N3 Co2 116.5(3) . . ? C10 N4 C11 111.0(5) . . ? C10 N4 H4 124.5 . . ? C11 N4 H4 124.5 . . ? C15 N5 C14 106.6(5) . . ? C15 N5 Co2 137.1(4) . . ? C14 N5 Co2 115.1(4) . . ? C15 N6 C13 109.9(5) . . ? C15 N6 H6 125.1 . . ? C13 N6 H6 125.1 . . ? C22 N7 C24 106.7(5) . . ? C22 N7 Co1 139.0(4) . . ? C24 N7 Co1 114.2(3) . . ? C22 N8 C23 110.5(5) . . ? C22 N8 H8A 124.8 . . ? C23 N8 H8A 124.8 . . ? C27 N9 C25 106.9(5) . . ? C27 N9 Co2 140.5(4) . . ? C25 N9 Co2 112.5(4) . . ? C27 N10 C26 109.2(5) . . ? C27 N10 H10 125.4 . . ? C26 N10 H10 125.4 . . ? C34 N11 C35 105.4(4) . . ? C34 N11 Co1 134.9(4) . . ? C35 N11 Co1 117.7(3) . . ? C34 N12 C36 109.4(5) . . ? C34 N12 H12 125.3 . . ? C36 N12 H12 125.3 . . ? C2 C1 N1 105.5(5) . . ? C2 C1 H1A 110.6 . . ? N1 C1 H1A 110.6 . . ? C2 C1 H1B 110.6 . . ? N1 C1 H1B 110.6 . . ? H1A C1 H1B 108.8 . . ? N2 C2 C1 102.5(5) . . ? N2 C2 H2A 111.3 . . ? C1 C2 H2A 111.3 . . ? N2 C2 H2B 111.3 . . ? C1 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? N1 C3 N2 113.9(5) . . ? N1 C3 C4 124.5(5) . . ? N2 C3 C4 121.6(5) . . ? C5 C4 C9 117.8(5) . . ? C5 C4 C3 120.2(5) . . ? C9 C4 C3 121.9(5) . . ? C6 C5 C4 120.8(5) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 120.3(5) . . ? C5 C6 C10 120.3(5) . . ? C7 C6 C10 119.4(5) . . ? C8 C7 C6 119.4(5) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 119.8(5) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C4 121.8(5) . . ? C8 C9 H9 119.1 . . ? C4 C9 H9 119.1 . . ? N3 C10 N4 114.8(5) . . ? N3 C10 C6 123.8(5) . . ? N4 C10 C6 121.4(5) . . ? N4 C11 C12 100.8(5) . . ? N4 C11 H11A 111.6 . . ? C12 C11 H11A 111.6 . . ? N4 C11 H11B 111.6 . . ? C12 C11 H11B 111.6 . . ? H11A C11 H11B 109.4 . . ? N3 C12 C11 106.8(4) . . ? N3 C12 H12A 110.4 . . ? C11 C12 H12A 110.4 . . ? N3 C12 H12B 110.4 . . ? C11 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? N6 C13 C14 101.7(5) . . ? N6 C13 H13A 111.4 . . ? C14 C13 H13A 111.4 . . ? N6 C13 H13B 111.4 . . ? C14 C13 H13B 111.4 . . ? H13A C13 H13B 109.3 . . ? N5 C14 C13 106.6(5) . . ? N5 C14 H14A 110.4 . . ? C13 C14 H14A 110.4 . . ? N5 C14 H14B 110.4 . . ? C13 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? N5 C15 N6 115.3(5) . . ? N5 C15 C16 126.2(5) . . ? N6 C15 C16 118.5(5) . . ? C21 C16 C17 118.8(5) . . ? C21 C16 C15 120.5(5) . . ? C17 C16 C15 120.7(5) . . ? C18 C17 C16 120.1(6) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.2(6) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.9(6) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 118.2(5) . . ? C19 C20 C22 121.3(5) . . ? C21 C20 C22 120.6(5) . . ? C16 C21 C20 121.8(5) . . ? C16 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? N7 C22 N8 114.6(5) . . ? N7 C22 C20 125.5(5) . . ? N8 C22 C20 119.9(5) . . ? N8 C23 C24 101.4(5) . . ? N8 C23 H23A 111.5 . . ? C24 C23 H23A 111.5 . . ? N8 C23 H23B 111.5 . . ? C24 C23 H23B 111.5 . . ? H23A C23 H23B 109.3 . . ? N7 C24 C23 106.2(5) . . ? N7 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? N7 C24 H24B 110.5 . . ? C23 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? N9 C25 C26 105.5(5) . . ? N9 C25 H25A 110.6 . . ? C26 C25 H25A 110.6 . . ? N9 C25 H25B 110.6 . . ? C26 C25 H25B 110.6 . . ? H25A C25 H25B 108.8 . . ? N10 C26 C25 102.5(5) . . ? N10 C26 H26A 111.3 . . ? C25 C26 H26A 111.3 . . ? N10 C26 H26B 111.3 . . ? C25 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? N9 C27 N10 114.7(6) . . ? N9 C27 C28 125.4(5) . . ? N10 C27 C28 119.8(5) . . ? C29 C28 C33 118.5(6) . . ? C29 C28 C27 122.9(5) . . ? C33 C28 C27 118.6(5) . . ? C30 C29 C28 121.1(6) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 120.9(6) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C32 119.2(6) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C33 C32 C31 119.4(6) . . ? C33 C32 C34 119.4(5) . . ? C31 C32 C34 121.2(6) . . ? C32 C33 C28 120.8(5) . . ? C32 C33 H33 119.6 . . ? C28 C33 H33 119.6 . . ? N11 C34 N12 116.4(5) . . ? N11 C34 C32 122.8(5) . . ? N12 C34 C32 120.8(5) . . ? N11 C35 C36 106.6(5) . . ? N11 C35 H35A 110.4 . . ? C36 C35 H35A 110.4 . . ? N11 C35 H35B 110.4 . . ? C36 C35 H35B 110.4 . . ? H35A C35 H35B 108.6 . . ? N12 C36 C35 102.2(5) . . ? N12 C36 H36A 111.3 . . ? C35 C36 H36A 111.3 . . ? N12 C36 H36B 111.3 . . ? C35 C36 H36B 111.3 . . ? H36A C36 H36B 109.2 . . ? O2 C37 H37A 109.5 . . ? O2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O3 C38 H38A 109.5 . . ? O3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 Co1 N1 C3 5.2(6) . . . . ? N7 Co1 N1 C3 134.0(5) . . . . ? Cl1 Co1 N1 C3 -113.9(5) . . . . ? N11 Co1 N1 C1 171.9(3) . . . . ? N7 Co1 N1 C1 -59.3(4) . . . . ? Cl1 Co1 N1 C1 52.9(4) . . . . ? N9 Co2 N3 C10 135.9(5) . . . . ? N5 Co2 N3 C10 9.1(6) . . . . ? Cl2 Co2 N3 C10 -110.1(5) . . . . ? N9 Co2 N3 C12 -63.1(5) . . . . ? N5 Co2 N3 C12 170.1(4) . . . . ? Cl2 Co2 N3 C12 50.9(4) . . . . ? N9 Co2 N5 C15 -6.8(6) . . . . ? N3 Co2 N5 C15 126.2(5) . . . . ? Cl2 Co2 N5 C15 -118.8(5) . . . . ? N9 Co2 N5 C14 158.3(4) . . . . ? N3 Co2 N5 C14 -68.6(4) . . . . ? Cl2 Co2 N5 C14 46.4(4) . . . . ? N11 Co1 N7 C22 116.8(6) . . . . ? N1 Co1 N7 C22 -14.4(6) . . . . ? Cl1 Co1 N7 C22 -126.6(6) . . . . ? N11 Co1 N7 C24 -69.1(4) . . . . ? N1 Co1 N7 C24 159.6(4) . . . . ? Cl1 Co1 N7 C24 47.4(4) . . . . ? N3 Co2 N9 C27 -11.1(7) . . . . ? N5 Co2 N9 C27 119.3(6) . . . . ? Cl2 Co2 N9 C27 -124.5(6) . . . . ? N3 Co2 N9 C25 165.0(4) . . . . ? N5 Co2 N9 C25 -64.6(4) . . . . ? Cl2 Co2 N9 C25 51.6(4) . . . . ? N7 Co1 N11 C34 0.0(6) . . . . ? N1 Co1 N11 C34 130.1(5) . . . . ? Cl1 Co1 N11 C34 -113.5(5) . . . . ? N7 Co1 N11 C35 161.4(4) . . . . ? N1 Co1 N11 C35 -68.5(4) . . . . ? Cl1 Co1 N11 C35 47.9(4) . . . . ? C3 N1 C1 C2 0.5(6) . . . . ? Co1 N1 C1 C2 -170.5(4) . . . . ? C3 N2 C2 C1 -2.5(7) . . . . ? N1 C1 C2 N2 1.2(7) . . . . ? C1 N1 C3 N2 -2.2(6) . . . . ? Co1 N1 C3 N2 165.0(4) . . . . ? C1 N1 C3 C4 179.0(5) . . . . ? Co1 N1 C3 C4 -13.8(9) . . . . ? C2 N2 C3 N1 3.1(7) . . . . ? C2 N2 C3 C4 -178.0(5) . . . . ? N1 C3 C4 C5 -35.3(8) . . . . ? N2 C3 C4 C5 145.9(5) . . . . ? N1 C3 C4 C9 146.8(5) . . . . ? N2 C3 C4 C9 -31.9(8) . . . . ? C9 C4 C5 C6 -1.6(8) . . . . ? C3 C4 C5 C6 -179.5(5) . . . . ? C4 C5 C6 C7 -0.7(8) . . . . ? C4 C5 C6 C10 -179.9(5) . . . . ? C5 C6 C7 C8 1.6(8) . . . . ? C10 C6 C7 C8 -179.2(5) . . . . ? C6 C7 C8 C9 -0.2(8) . . . . ? C7 C8 C9 C4 -2.2(9) . . . . ? C5 C4 C9 C8 3.1(8) . . . . ? C3 C4 C9 C8 -179.0(5) . . . . ? C12 N3 C10 N4 -2.5(7) . . . . ? Co2 N3 C10 N4 159.8(4) . . . . ? C12 N3 C10 C6 176.8(5) . . . . ? Co2 N3 C10 C6 -20.9(8) . . . . ? C11 N4 C10 N3 0.1(7) . . . . ? C11 N4 C10 C6 -179.2(5) . . . . ? C5 C6 C10 N3 -37.9(8) . . . . ? C7 C6 C10 N3 142.9(5) . . . . ? C5 C6 C10 N4 141.3(6) . . . . ? C7 C6 C10 N4 -37.8(8) . . . . ? C10 N4 C11 C12 2.2(7) . . . . ? C10 N3 C12 C11 3.7(7) . . . . ? Co2 N3 C12 C11 -162.4(4) . . . . ? N4 C11 C12 N3 -3.4(7) . . . . ? C15 N6 C13 C14 -0.1(7) . . . . ? C15 N5 C14 C13 -1.6(6) . . . . ? Co2 N5 C14 C13 -171.1(4) . . . . ? N6 C13 C14 N5 0.9(7) . . . . ? C14 N5 C15 N6 1.6(7) . . . . ? Co2 N5 C15 N6 167.6(4) . . . . ? C14 N5 C15 C16 179.6(5) . . . . ? Co2 N5 C15 C16 -14.4(9) . . . . ? C13 N6 C15 N5 -1.0(7) . . . . ? C13 N6 C15 C16 -179.1(5) . . . . ? N5 C15 C16 C21 -43.6(8) . . . . ? N6 C15 C16 C21 134.3(6) . . . . ? N5 C15 C16 C17 137.9(6) . . . . ? N6 C15 C16 C17 -44.2(7) . . . . ? C21 C16 C17 C18 2.4(8) . . . . ? C15 C16 C17 C18 -179.0(5) . . . . ? C16 C17 C18 C19 -2.1(9) . . . . ? C17 C18 C19 C20 0.0(9) . . . . ? C18 C19 C20 C21 1.7(8) . . . . ? C18 C19 C20 C22 -178.3(5) . . . . ? C17 C16 C21 C20 -0.7(8) . . . . ? C15 C16 C21 C20 -179.2(5) . . . . ? C19 C20 C21 C16 -1.3(8) . . . . ? C22 C20 C21 C16 178.7(5) . . . . ? C24 N7 C22 N8 0.1(7) . . . . ? Co1 N7 C22 N8 174.5(4) . . . . ? C24 N7 C22 C20 -179.1(5) . . . . ? Co1 N7 C22 C20 -4.7(10) . . . . ? C23 N8 C22 N7 5.4(7) . . . . ? C23 N8 C22 C20 -175.4(5) . . . . ? C19 C20 C22 N7 146.0(6) . . . . ? C21 C20 C22 N7 -34.1(8) . . . . ? C19 C20 C22 N8 -33.1(8) . . . . ? C21 C20 C22 N8 146.8(5) . . . . ? C22 N8 C23 C24 -8.0(7) . . . . ? C22 N7 C24 C23 -5.2(7) . . . . ? Co1 N7 C24 C23 178.9(4) . . . . ? N8 C23 C24 N7 7.7(7) . . . . ? C27 N9 C25 C26 -5.0(7) . . . . ? Co2 N9 C25 C26 177.6(4) . . . . ? C27 N10 C26 C25 -11.0(7) . . . . ? N9 C25 C26 N10 9.4(7) . . . . ? C25 N9 C27 N10 -2.2(7) . . . . ? Co2 N9 C27 N10 174.1(4) . . . . ? C25 N9 C27 C28 179.2(5) . . . . ? Co2 N9 C27 C28 -4.6(10) . . . . ? C26 N10 C27 N9 8.9(8) . . . . ? C26 N10 C27 C28 -172.4(6) . . . . ? N9 C27 C28 C29 152.9(6) . . . . ? N10 C27 C28 C29 -25.7(9) . . . . ? N9 C27 C28 C33 -29.3(9) . . . . ? N10 C27 C28 C33 152.2(5) . . . . ? C33 C28 C29 C30 2.5(10) . . . . ? C27 C28 C29 C30 -179.6(6) . . . . ? C28 C29 C30 C31 0.3(11) . . . . ? C29 C30 C31 C32 -3.4(10) . . . . ? C30 C31 C32 C33 3.5(9) . . . . ? C30 C31 C32 C34 -177.6(6) . . . . ? C31 C32 C33 C28 -0.6(9) . . . . ? C34 C32 C33 C28 -179.6(5) . . . . ? C29 C28 C33 C32 -2.4(9) . . . . ? C27 C28 C33 C32 179.7(5) . . . . ? C35 N11 C34 N12 1.0(7) . . . . ? Co1 N11 C34 N12 164.0(4) . . . . ? C35 N11 C34 C32 179.5(5) . . . . ? Co1 N11 C34 C32 -17.5(9) . . . . ? C36 N12 C34 N11 0.2(7) . . . . ? C36 N12 C34 C32 -178.3(5) . . . . ? C33 C32 C34 N11 -50.2(8) . . . . ? C31 C32 C34 N11 130.9(6) . . . . ? C33 C32 C34 N12 128.3(6) . . . . ? C31 C32 C34 N12 -50.7(8) . . . . ? C34 N11 C35 C36 -1.8(6) . . . . ? Co1 N11 C35 C36 -168.3(4) . . . . ? C34 N12 C36 C35 -1.3(7) . . . . ? N11 C35 C36 N12 1.9(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2D Cl4 0.84 2.56 3.304(8) 147.8 . O3 H3 Cl3 0.84 2.70 3.077(6) 109.1 . N2 H2 O2 0.88 2.31 2.943(8) 128.6 1_565 N4 H4 O3 0.88 1.97 2.842(6) 172.0 1_554 N6 H6 O1 0.88 2.02 2.754(9) 140.8 1_565 N8 H8A Cl3 0.88 2.48 3.199(5) 139.7 . N10 H10 Cl3 0.88 2.67 3.226(5) 122.6 . N12 H12 Cl4 0.88 2.35 3.220(6) 169.5 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.753 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.103 # Attachment 'ccdc667567.cif' data_ccdc667567 _database_code_depnum_ccdc_archive 'CCDC 667567' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H54 Co3 F6 K N12 O12 P' _chemical_formula_sum 'C42 H54 Co3 F6 K N12 O12 P' _chemical_formula_weight 1279.83 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' _cell_length_a 14.575(3) _cell_length_b 14.575(3) _cell_length_c 13.889(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2555.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1882 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.99 _exptl_crystal_description block _exptl_crystal_colour blue-purple _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1309.3 _exptl_absorpt_coefficient_mu 1.169 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 12712 _diffrn_reflns_av_R_equivalents 0.1521 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1515 _reflns_number_gt 982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.04(7) _refine_ls_number_reflns 1515 _refine_ls_number_parameters 133 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1205 _refine_ls_R_factor_gt 0.1205 _refine_ls_wR_factor_ref 0.1748 _refine_ls_wR_factor_gt 0.1583 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.33880(9) 0.16940(5) 0.7500 0.0587(5) Uani 1 2 d S . . P1 P 0.3333 0.6667 0.7500 0.0758(14) Uani 1 6 d SD . . K1 K 0.6667 0.3333 0.7500 0.1100(17) Uani 1 6 d S . . O1 O 0.4598(7) 0.2754(7) 0.8286(8) 0.145(3) Uani 1 1 d . . . O2 O 0.3411(7) 0.2531(7) 0.9174(7) 0.141(4) Uani 1 1 d . . . N1 N 0.2653(4) 0.2370(4) 0.6806(4) 0.0469(13) Uani 1 1 d . . . N2 N 0.1721(4) 0.2927(4) 0.5974(4) 0.0626(16) Uani 1 1 d . . . H2C H 0.1145 0.2885 0.5726 0.075 Uiso 1 1 calc R . . F2 F 0.3333 0.6667 0.6418(5) 0.202(7) Uani 1 3 d SD . . C1 C 0.3313(6) 0.3559(5) 0.6779(6) 0.068(2) Uani 1 1 d . . . H1A H 0.4048 0.3792 0.6575 0.082 Uiso 1 1 calc R . . H1B H 0.3327 0.3871 0.7416 0.082 Uiso 1 1 calc R . . C2 C 0.2740(7) 0.3861(6) 0.6034(7) 0.080(2) Uani 1 1 d . . . H2A H 0.2682 0.4477 0.6252 0.095 Uiso 1 1 calc R . . H2B H 0.3109 0.4029 0.5405 0.095 Uiso 1 1 calc R . . C3 C 0.1799(5) 0.2124(5) 0.6363(4) 0.0408(14) Uani 1 1 d . . . C4 C 0.0873(4) 0.1033(5) 0.6307(5) 0.0369(15) Uani 1 1 d . . . C5 C -0.0163(5) 0.0856(5) 0.6299(4) 0.0416(16) Uani 1 1 d . . . H5A H -0.0274 0.1445 0.6287 0.050 Uiso 1 1 calc R . . C6 C 0.4303(14) 0.2964(10) 0.8989(10) 0.109(4) Uani 1 1 d . . . C7 C 0.5180(8) 0.3756(10) 0.9673(11) 0.163(6) Uani 1 1 d . . . H7A H 0.5265 0.3369 1.0210 0.244 Uiso 1 1 calc R . . H7B H 0.4981 0.4261 0.9924 0.244 Uiso 1 1 calc R . . H7C H 0.5850 0.4140 0.9320 0.244 Uiso 1 1 calc R . . F1 F 0.3704(18) 0.5857(13) 0.7530(13) 0.22(2) Uani 0.33 1 d PD A 1 F3 F 0.4465(11) 0.7561(10) 0.7581(12) 0.196(16) Uani 0.33 1 d PD . 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 Co 0.0414(7) 0.0605(7) 0.0679(9) 0.0059(7) 0.000 0.0207(4) P1 0.082(2) 0.082(2) 0.062(3) 0.000 0.000 0.0412(11) K1 0.106(2) 0.106(2) 0.118(4) 0.000 0.000 0.0531(12) O1 0.110(6) 0.098(6) 0.197(10) 0.010(6) -0.019(6) 0.030(5) O2 0.118(6) 0.098(6) 0.174(9) -0.013(6) -0.069(7) 0.030(6) N1 0.036(3) 0.039(3) 0.058(3) -0.008(3) -0.003(3) 0.013(2) N2 0.063(4) 0.040(3) 0.079(4) 0.011(3) -0.001(3) 0.021(3) F2 0.271(11) 0.271(11) 0.063(7) 0.000 0.000 0.136(6) C1 0.044(4) 0.044(4) 0.094(5) 0.009(4) 0.003(4) 0.006(4) C2 0.075(6) 0.047(4) 0.094(6) 0.007(4) 0.003(5) 0.013(4) C3 0.056(4) 0.043(4) 0.029(3) 0.005(3) 0.011(3) 0.029(4) C4 0.042(4) 0.038(4) 0.022(3) 0.004(3) 0.005(3) 0.014(3) C5 0.052(4) 0.044(4) 0.029(3) -0.001(3) -0.002(3) 0.025(3) C6 0.156(12) 0.087(9) 0.104(9) 0.007(8) 0.020(10) 0.076(9) C7 0.106(9) 0.098(9) 0.245(17) -0.021(10) -0.087(10) 0.021(7) F1 0.23(4) 0.19(3) 0.34(3) -0.18(3) -0.25(3) 0.18(3) F3 0.20(2) 0.039(9) 0.26(3) 0.018(15) -0.18(2) -0.005(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O1 1.991(9) . ? Co O1 1.991(9) 12_556 ? Co N1 2.026(5) 12_556 ? Co N1 2.026(5) . ? P1 F2 1.502(7) 10_666 ? P1 F2 1.502(7) . ? P1 F3 1.510(9) 3_665 ? P1 F3 1.510(9) 11_556 ? P1 F3 1.510(10) 10_666 ? P1 F3 1.510(10) . ? P1 F3 1.510(9) 5_565 ? P1 F3 1.510(9) 12_566 ? P1 F1 1.523(9) 12_566 ? P1 F1 1.523(9) 5_565 ? P1 F1 1.523(9) 3_665 ? P1 F1 1.523(9) 11_556 ? K1 O1 2.906(9) 3_655 ? K1 O1 2.906(9) 11_656 ? K1 O1 2.906(10) 12_556 ? K1 O1 2.906(10) 5_665 ? K1 O1 2.906(10) . ? K1 O1 2.906(10) 10_666 ? O1 C6 1.168(13) . ? O2 C6 1.154(15) . ? N1 C3 1.269(8) . ? N1 C1 1.504(9) . ? N2 C3 1.344(9) . ? N2 C2 1.430(9) . ? N2 H2C 0.8800 . ? C1 C2 1.527(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.486(9) . ? C4 C5 1.386(8) 5 ? C4 C5 1.399(8) . ? C5 C4 1.386(8) 3 ? C5 H5A 0.9500 . ? C6 C7 1.548(18) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? F1 F1 0.65(4) 10_666 ? F3 F3 0.98(4) 12_566 ? 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 Co O1 79.8(6) . 12_556 ? O1 Co N1 109.9(3) . 12_556 ? O1 Co N1 111.3(3) 12_556 12_556 ? O1 Co N1 111.3(3) . . ? O1 Co N1 109.9(3) 12_556 . ? N1 Co N1 125.5(3) 12_556 . ? F2 P1 F2 180.000(6) 10_666 . ? F2 P1 F3 85.7(7) 10_666 3_665 ? F2 P1 F3 94.3(7) . 3_665 ? F2 P1 F3 94.3(7) 10_666 11_556 ? F2 P1 F3 85.7(7) . 11_556 ? F2 P1 F3 94.3(7) 10_666 10_666 ? F2 P1 F3 85.7(7) . 10_666 ? F3 P1 F3 83.3(15) 3_665 10_666 ? F3 P1 F3 119.45(18) 11_556 10_666 ? F2 P1 F3 85.7(7) 10_666 . ? F2 P1 F3 94.3(7) . . ? F3 P1 F3 119.45(18) 3_665 . ? F3 P1 F3 83.3(15) 11_556 . ? F3 P1 F3 157.1(15) 10_666 . ? F2 P1 F3 85.7(7) 10_666 5_565 ? F2 P1 F3 94.3(7) . 5_565 ? F3 P1 F3 119.45(19) 3_665 5_565 ? F3 P1 F3 157.1(15) 11_556 5_565 ? F3 P1 F3 119.45(17) . 5_565 ? F2 P1 F3 94.3(7) 10_666 12_566 ? F2 P1 F3 85.7(7) . 12_566 ? F3 P1 F3 157.1(15) 3_665 12_566 ? F3 P1 F3 119.45(19) 11_556 12_566 ? F3 P1 F3 119.45(17) 10_666 12_566 ? F3 P1 F3 83.3(14) 5_565 12_566 ? F2 P1 F1 91.6(7) 10_666 12_566 ? F2 P1 F1 88.4(7) . 12_566 ? F3 P1 F1 66.6(14) 3_665 12_566 ? F3 P1 F1 148.8(8) 10_666 12_566 ? F3 P1 F1 53.9(14) . 12_566 ? F3 P1 F1 173.1(15) 5_565 12_566 ? F3 P1 F1 90.5(7) 12_566 12_566 ? F2 P1 F1 88.4(7) 10_666 5_565 ? F2 P1 F1 91.6(7) . 5_565 ? F3 P1 F1 66.6(14) 11_556 5_565 ? F3 P1 F1 53.9(14) 10_666 5_565 ? F3 P1 F1 148.8(8) . 5_565 ? F3 P1 F1 90.5(7) 5_565 5_565 ? F3 P1 F1 173.1(14) 12_566 5_565 ? F1 P1 F1 95.8(17) 12_566 5_565 ? F2 P1 F1 88.4(7) 10_666 3_665 ? F2 P1 F1 91.6(7) . 3_665 ? F3 P1 F1 90.5(7) 3_665 3_665 ? F3 P1 F1 53.9(14) 11_556 3_665 ? F3 P1 F1 173.1(14) 10_666 3_665 ? F3 P1 F1 148.8(8) 5_565 3_665 ? F3 P1 F1 66.6(14) 12_566 3_665 ? F1 P1 F1 119.92(7) 5_565 3_665 ? F2 P1 F1 91.6(7) 10_666 11_556 ? F2 P1 F1 88.4(7) . 11_556 ? F3 P1 F1 53.9(14) 3_665 11_556 ? F3 P1 F1 90.5(7) 11_556 11_556 ? F3 P1 F1 173.1(14) . 11_556 ? F3 P1 F1 66.6(14) 5_565 11_556 ? F3 P1 F1 148.8(8) 12_566 11_556 ? F1 P1 F1 119.92(7) 12_566 11_556 ? F1 P1 F1 144.3(17) 3_665 11_556 ? O1 K1 O1 52.1(4) 3_655 11_656 ? O1 K1 O1 99.4(3) 3_655 12_556 ? O1 K1 O1 106.8(2) 11_656 12_556 ? O1 K1 O1 106.8(2) 3_655 5_665 ? O1 K1 O1 99.4(3) 11_656 5_665 ? O1 K1 O1 150.8(3) 12_556 5_665 ? O1 K1 O1 106.8(2) 3_655 . ? O1 K1 O1 150.8(3) 11_656 . ? O1 K1 O1 52.1(4) 12_556 . ? O1 K1 O1 106.8(2) 5_665 . ? O1 K1 O1 150.8(3) 3_655 10_666 ? O1 K1 O1 106.8(2) 11_656 10_666 ? O1 K1 O1 106.8(2) 12_556 10_666 ? O1 K1 O1 52.1(4) 5_665 10_666 ? O1 K1 O1 99.4(3) . 10_666 ? C6 O1 Co 111.2(11) . . ? C6 O1 K1 134.6(11) . . ? Co O1 K1 114.1(5) . . ? C3 N1 C1 106.6(6) . . ? C3 N1 Co 140.9(5) . . ? C1 N1 Co 112.5(4) . . ? C3 N2 C2 107.8(6) . . ? C3 N2 H2C 126.1 . . ? C2 N2 H2C 126.1 . . ? N1 C1 C2 102.8(6) . . ? N1 C1 H1A 111.2 . . ? C2 C1 H1A 111.2 . . ? N1 C1 H1B 111.2 . . ? C2 C1 H1B 111.2 . . ? H1A C1 H1B 109.1 . . ? N2 C2 C1 102.8(6) . . ? N2 C2 H2A 111.2 . . ? C1 C2 H2A 111.2 . . ? N2 C2 H2B 111.2 . . ? C1 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? N1 C3 N2 116.5(6) . . ? N1 C3 C4 124.4(6) . . ? N2 C3 C4 118.9(6) . . ? C5 C4 C5 118.4(7) 5 . ? C5 C4 C3 120.4(6) 5 . ? C5 C4 C3 121.1(6) . . ? C4 C5 C4 121.6(7) 3 . ? C4 C5 H5A 119.2 3 . ? C4 C5 H5A 119.2 . . ? O2 C6 O1 120.3(17) . . ? O2 C6 C7 123.8(12) . . ? O1 C6 C7 115.7(16) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? F1 F1 P1 77.8(9) 10_666 . ? F3 F3 P1 71.0(8) 12_566 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.362 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.070