# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2068 data_stdpg _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Cl2 Co N5 O10' _chemical_formula_weight 694.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.620(8) _cell_length_b 24.487(13) _cell_length_c 10.296(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.54(3) _cell_angle_gamma 90.00 _cell_volume 2665(3) _cell_formula_units_Z 3 _cell_measurement_temperature 150 _cell_measurement_reflns_used - _cell_measurement_theta_min - _cell_measurement_theta_max - _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1062 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 26963 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 23.51 _reflns_number_total 3873 _reflns_number_gt 2772 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3873 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _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 0.20942(4) 0.141177(18) 0.37514(5) 0.01835(16) Uani 1 1 d . . . N1 N 0.0923(3) 0.15630(11) 0.1810(3) 0.0194(7) Uani 1 1 d . . . N2 N 0.3367(3) 0.15840(11) 0.3063(3) 0.0189(7) Uani 1 1 d . . . N3 N 0.0599(3) 0.12853(11) 0.4067(3) 0.0216(7) Uani 1 1 d . . . N4 N 0.3267(3) 0.13133(11) 0.5705(3) 0.0195(7) Uani 1 1 d . . . N5 N 0.2365(3) 0.06058(11) 0.3636(3) 0.0201(7) Uani 1 1 d . . . O1 O 0.2041(2) 0.21604(9) 0.4129(2) 0.0216(6) Uani 1 1 d . . . O2 O 0.1569(3) 0.29649(10) 0.3027(3) 0.0341(7) Uani 1 1 d . . . C1 C 0.1473(3) 0.24705(15) 0.3014(4) 0.0223(8) Uani 1 1 d . . . C2 C 0.0635(3) 0.21679(13) 0.1707(4) 0.0246(9) Uani 1 1 d . . . H2A H 0.0736 0.2317 0.0888 0.030 Uiso 1 1 calc R . . H2B H -0.0239 0.2220 0.1555 0.030 Uiso 1 1 calc R . . C4 C 0.1574(3) 0.14254(15) 0.0868(3) 0.0215(8) Uani 1 1 d . . . H4A H 0.1189 0.1624 -0.0025 0.026 Uiso 1 1 calc R . . H4B H 0.1500 0.1038 0.0657 0.026 Uiso 1 1 calc R . . C5 C 0.2945(3) 0.15816(13) 0.1640(4) 0.0206(8) Uani 1 1 d . . . C6 C 0.3718(3) 0.17311(15) 0.0979(4) 0.0264(9) Uani 1 1 d . . . H6 H 0.3416 0.1716 -0.0010 0.032 Uiso 1 1 calc R . . C7 C 0.4941(3) 0.19031(15) 0.1791(4) 0.0288(9) Uani 1 1 d . . . H7 H 0.5474 0.2000 0.1360 0.035 Uiso 1 1 calc R . . C8 C 0.5353(3) 0.19284(14) 0.3244(4) 0.0242(9) Uani 1 1 d . . . H8 H 0.6160 0.2057 0.3815 0.029 Uiso 1 1 calc R . . C9 C 0.4555(3) 0.17613(14) 0.3846(4) 0.0223(9) Uani 1 1 d . . . H9 H 0.4846 0.1771 0.4834 0.027 Uiso 1 1 calc R . . C10 C -0.0266(3) 0.12474(15) 0.1525(4) 0.0243(9) Uani 1 1 d . . . H10A H -0.0978 0.1415 0.0750 0.029 Uiso 1 1 calc R . . H10B H -0.0180 0.0875 0.1257 0.029 Uiso 1 1 calc R . . C11 C -0.0476(3) 0.12519(13) 0.2864(3) 0.0209(8) Uani 1 1 d . . . C12 C -0.1635(4) 0.12272(14) 0.2910(4) 0.0282(9) Uani 1 1 d . . . H12 H -0.2368 0.1209 0.2069 0.034 Uiso 1 1 calc R . . C13 C -0.1710(4) 0.12297(16) 0.4208(4) 0.0328(10) Uani 1 1 d . . . H13 H -0.2493 0.1210 0.4252 0.039 Uiso 1 1 calc R . . C14 C -0.0627(4) 0.12619(15) 0.5428(4) 0.0309(10) Uani 1 1 d . . . H14 H -0.0658 0.1267 0.6316 0.037 Uiso 1 1 calc R . . C15 C 0.0511(4) 0.12868(14) 0.5324(4) 0.0273(9) Uani 1 1 d . . . H15 H 0.1251 0.1306 0.6159 0.033 Uiso 1 1 calc R . . C16 C 0.3714(3) 0.16989(15) 0.6714(4) 0.0234(8) Uani 1 1 d . . . H16 H 0.3430 0.2057 0.6499 0.028 Uiso 1 1 calc R . . C17 C 0.4589(3) 0.15703(15) 0.8067(4) 0.0242(9) Uani 1 1 d . . . H17 H 0.4906 0.1844 0.8751 0.029 Uiso 1 1 calc R . . C18 C 0.4997(3) 0.10464(15) 0.8415(4) 0.0262(9) Uani 1 1 d . . . H18 H 0.5582 0.0964 0.9335 0.031 Uiso 1 1 calc R . . C19 C 0.4540(3) 0.06334(14) 0.7394(3) 0.0231(8) Uani 1 1 d . . . C20 C 0.4898(4) 0.00700(15) 0.7622(4) 0.0290(9) Uani 1 1 d . . . H20 H 0.5454 -0.0045 0.8527 0.035 Uiso 1 1 calc R . . C21 C 0.4447(4) -0.02973(15) 0.6557(4) 0.0300(10) Uani 1 1 d . . . H21 H 0.4703 -0.0660 0.6738 0.036 Uiso 1 1 calc R . . C22 C 0.3587(3) -0.01410(14) 0.5161(4) 0.0226(8) Uani 1 1 d . . . C23 C 0.3103(3) -0.05028(15) 0.4008(4) 0.0279(9) Uani 1 1 d . . . H23 H 0.3350 -0.0867 0.4112 0.033 Uiso 1 1 calc R . . C24 C 0.2260(4) -0.03055(14) 0.2729(4) 0.0284(9) Uani 1 1 d . . . H24 H 0.1916 -0.0538 0.1947 0.034 Uiso 1 1 calc R . . C25 C 0.1914(3) 0.02416(15) 0.2587(4) 0.0269(9) Uani 1 1 d . . . H25 H 0.1328 0.0361 0.1701 0.032 Uiso 1 1 calc R . . C26 C 0.3198(3) 0.04051(14) 0.4921(3) 0.0201(8) Uani 1 1 d . . . C27 C 0.3685(3) 0.07913(14) 0.6043(3) 0.0184(8) Uani 1 1 d . . . Cl1 Cl 0.78239(9) 0.20250(4) 0.79572(10) 0.0291(2) Uani 1 1 d . . . O11 O 0.8312(6) 0.25122(17) 0.7789(5) 0.140(2) Uani 1 1 d . . . O12 O 0.8738(4) 0.16045(16) 0.8249(3) 0.0813(13) Uani 1 1 d . . . O13 O 0.6791(3) 0.18802(19) 0.6722(3) 0.0934(14) Uani 1 1 d . . . O14 O 0.7460(3) 0.20668(14) 0.9120(3) 0.0569(9) Uani 1 1 d . . . Cl2 Cl -0.19662(9) -0.01743(4) 0.12081(10) 0.0345(3) Uani 1 1 d . . . O21 O -0.1677(4) -0.01811(15) 0.2661(3) 0.0781(12) Uani 1 1 d . . . O22 O -0.2567(3) 0.03315(11) 0.0619(3) 0.0616(10) Uani 1 1 d . . . O23 O -0.0848(3) -0.02245(13) 0.0948(3) 0.0591(9) Uani 1 1 d . . . O24 O -0.2821(3) -0.06081(12) 0.0488(4) 0.0632(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0192(3) 0.0184(3) 0.0146(3) -0.0005(2) 0.0042(2) 0.0006(2) N1 0.0182(16) 0.0213(17) 0.0166(16) -0.0009(12) 0.0051(13) 0.0005(13) N2 0.0209(17) 0.0175(16) 0.0170(16) 0.0009(12) 0.0065(14) 0.0024(13) N3 0.0242(17) 0.0202(17) 0.0208(16) -0.0005(13) 0.0097(14) 0.0008(13) N4 0.0219(16) 0.0214(17) 0.0145(15) 0.0008(13) 0.0070(13) -0.0009(13) N5 0.0214(17) 0.0203(16) 0.0178(16) -0.0017(13) 0.0073(14) -0.0014(13) O1 0.0250(14) 0.0178(13) 0.0161(13) 0.0010(10) 0.0027(11) 0.0031(11) O2 0.0451(18) 0.0191(16) 0.0259(15) 0.0000(12) 0.0027(13) -0.0016(13) C1 0.021(2) 0.027(2) 0.019(2) -0.0008(17) 0.0084(17) 0.0044(18) C2 0.028(2) 0.023(2) 0.0173(19) 0.0020(16) 0.0035(17) 0.0041(17) C4 0.022(2) 0.026(2) 0.0144(18) 0.0009(16) 0.0060(16) 0.0010(17) C5 0.021(2) 0.0182(19) 0.019(2) -0.0010(15) 0.0048(17) 0.0029(16) C6 0.029(2) 0.033(2) 0.018(2) 0.0017(17) 0.0103(18) 0.0039(18) C7 0.029(2) 0.032(2) 0.029(2) 0.0055(18) 0.0166(19) 0.0025(18) C8 0.019(2) 0.022(2) 0.028(2) 0.0002(16) 0.0063(17) 0.0002(17) C9 0.020(2) 0.023(2) 0.0187(19) 0.0008(16) 0.0028(17) 0.0019(17) C10 0.018(2) 0.030(2) 0.0213(19) -0.0025(16) 0.0048(17) -0.0031(16) C11 0.024(2) 0.017(2) 0.020(2) -0.0006(15) 0.0072(17) 0.0000(16) C12 0.023(2) 0.027(2) 0.029(2) -0.0041(17) 0.0054(18) -0.0008(17) C13 0.030(2) 0.035(2) 0.040(3) -0.0005(19) 0.021(2) -0.0010(19) C14 0.032(2) 0.038(3) 0.027(2) -0.0012(18) 0.017(2) -0.0020(19) C15 0.032(2) 0.027(2) 0.023(2) -0.0033(16) 0.0115(18) -0.0018(18) C16 0.026(2) 0.024(2) 0.021(2) -0.0026(16) 0.0110(18) -0.0007(17) C17 0.027(2) 0.027(2) 0.017(2) -0.0037(16) 0.0067(17) -0.0060(17) C18 0.025(2) 0.038(2) 0.0127(18) 0.0064(17) 0.0041(17) 0.0023(18) C19 0.021(2) 0.027(2) 0.020(2) 0.0047(17) 0.0076(17) 0.0003(17) C20 0.029(2) 0.032(2) 0.023(2) 0.0088(18) 0.0076(18) 0.0041(18) C21 0.031(2) 0.023(2) 0.034(2) 0.0103(18) 0.012(2) 0.0051(18) C22 0.019(2) 0.022(2) 0.028(2) 0.0018(17) 0.0111(18) -0.0015(17) C23 0.033(2) 0.019(2) 0.037(2) 0.0007(18) 0.021(2) 0.0021(18) C24 0.035(2) 0.022(2) 0.027(2) -0.0080(17) 0.0118(19) -0.0048(18) C25 0.029(2) 0.028(2) 0.021(2) -0.0028(17) 0.0075(18) -0.0017(18) C26 0.0183(19) 0.021(2) 0.0208(19) 0.0022(16) 0.0081(16) -0.0011(16) C27 0.0195(19) 0.019(2) 0.0188(19) 0.0018(16) 0.0099(16) 0.0002(16) Cl1 0.0261(5) 0.0287(6) 0.0270(5) -0.0029(4) 0.0056(4) 0.0021(4) O11 0.262(6) 0.061(3) 0.153(4) -0.024(3) 0.143(5) -0.080(4) O12 0.090(3) 0.114(3) 0.042(2) 0.0068(19) 0.028(2) 0.061(2) O13 0.051(2) 0.169(4) 0.037(2) -0.029(2) -0.0046(18) -0.006(2) O14 0.048(2) 0.091(3) 0.0347(17) -0.0011(16) 0.0201(15) 0.0279(18) Cl2 0.0400(6) 0.0291(6) 0.0327(6) -0.0029(4) 0.0133(5) 0.0013(5) O21 0.116(3) 0.087(3) 0.035(2) 0.0171(17) 0.035(2) 0.030(2) O22 0.065(2) 0.0345(19) 0.052(2) -0.0032(15) -0.0090(17) 0.0128(17) O23 0.0379(19) 0.077(2) 0.067(2) -0.0309(18) 0.0260(17) -0.0172(16) O24 0.060(2) 0.0359(19) 0.108(3) -0.0279(18) 0.049(2) -0.0196(16) _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 1.880(2) . ? Co N4 1.919(3) . ? Co N3 1.921(3) . ? Co N1 1.930(3) . ? Co N2 1.933(3) . ? Co N5 2.010(3) . ? N1 C4 1.495(4) . ? N1 C10 1.502(4) . ? N1 C2 1.513(4) . ? N2 C5 1.338(4) . ? N2 C9 1.349(4) . ? N3 C15 1.339(4) . ? N3 C11 1.347(4) . ? N4 C16 1.339(4) . ? N4 C27 1.361(4) . ? N5 C25 1.328(4) . ? N5 C26 1.366(4) . ? O1 C1 1.304(4) . ? O2 C1 1.215(4) . ? C1 C2 1.490(5) . ? C4 C5 1.504(5) . ? C5 C6 1.383(5) . ? C6 C7 1.381(5) . ? C7 C8 1.370(5) . ? C8 C9 1.374(5) . ? C10 C11 1.497(5) . ? C11 C12 1.369(5) . ? C12 C13 1.375(5) . ? C13 C14 1.362(5) . ? C14 C15 1.372(5) . ? C16 C17 1.378(5) . ? C17 C18 1.363(5) . ? C18 C19 1.395(5) . ? C19 C27 1.387(5) . ? C19 C20 1.432(5) . ? C20 C21 1.345(5) . ? C21 C22 1.421(5) . ? C22 C23 1.398(5) . ? C22 C26 1.400(5) . ? C23 C24 1.362(5) . ? C24 C25 1.389(5) . ? C26 C27 1.416(5) . ? Cl1 O11 1.363(4) . ? Cl1 O13 1.384(3) . ? Cl1 O12 1.419(3) . ? Cl1 O14 1.429(3) . ? Cl2 O21 1.390(3) . ? Cl2 O22 1.428(3) . ? Cl2 O24 1.433(3) . ? Cl2 O23 1.437(3) . ? 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 N4 88.61(11) . . ? O1 Co N3 90.70(11) . . ? N4 Co N3 95.78(13) . . ? O1 Co N1 87.57(11) . . ? N4 Co N1 176.15(12) . . ? N3 Co N1 84.73(13) . . ? O1 Co N2 87.66(11) . . ? N4 Co N2 95.35(13) . . ? N3 Co N2 168.71(12) . . ? N1 Co N2 84.03(13) . . ? O1 Co N5 171.51(10) . . ? N4 Co N5 83.01(11) . . ? N3 Co N5 91.52(11) . . ? N1 Co N5 100.80(11) . . ? N2 Co N5 91.73(11) . . ? C4 N1 C10 115.4(3) . . ? C4 N1 C2 109.4(3) . . ? C10 N1 C2 109.4(3) . . ? C4 N1 Co 107.4(2) . . ? C10 N1 Co 107.4(2) . . ? C2 N1 Co 107.51(19) . . ? C5 N2 C9 118.3(3) . . ? C5 N2 Co 114.4(2) . . ? C9 N2 Co 126.9(2) . . ? C15 N3 C11 118.4(3) . . ? C15 N3 Co 126.9(2) . . ? C11 N3 Co 114.3(2) . . ? C16 N4 C27 118.8(3) . . ? C16 N4 Co 127.0(2) . . ? C27 N4 Co 114.2(2) . . ? C25 N5 C26 115.3(3) . . ? C25 N5 Co 133.5(2) . . ? C26 N5 Co 111.2(2) . . ? C1 O1 Co 115.7(2) . . ? O2 C1 O1 124.0(3) . . ? O2 C1 C2 121.9(3) . . ? O1 C1 C2 114.0(3) . . ? C1 C2 N1 112.4(3) . . ? N1 C4 C5 108.0(3) . . ? N2 C5 C6 121.4(3) . . ? N2 C5 C4 113.9(3) . . ? C6 C5 C4 124.7(3) . . ? C7 C6 C5 119.9(3) . . ? C8 C7 C6 118.7(3) . . ? C7 C8 C9 118.9(3) . . ? N2 C9 C8 122.8(3) . . ? C11 C10 N1 107.8(3) . . ? N3 C11 C12 121.4(3) . . ? N3 C11 C10 113.8(3) . . ? C12 C11 C10 124.8(3) . . ? C11 C12 C13 119.6(3) . . ? C14 C13 C12 119.3(4) . . ? C13 C14 C15 118.8(3) . . ? N3 C15 C14 122.5(3) . . ? N4 C16 C17 120.6(3) . . ? C18 C17 C16 120.7(3) . . ? C17 C18 C19 120.1(3) . . ? C27 C19 C18 116.3(3) . . ? C27 C19 C20 118.1(3) . . ? C18 C19 C20 125.5(3) . . ? C21 C20 C19 121.5(3) . . ? C20 C21 C22 121.1(3) . . ? C23 C22 C26 118.0(3) . . ? C23 C22 C21 123.6(3) . . ? C26 C22 C21 118.4(3) . . ? C24 C23 C22 118.0(3) . . ? C23 C24 C25 120.3(3) . . ? N5 C25 C24 124.3(3) . . ? N5 C26 C22 124.1(3) . . ? N5 C26 C27 115.6(3) . . ? C22 C26 C27 120.2(3) . . ? N4 C27 C19 123.4(3) . . ? N4 C27 C26 116.1(3) . . ? C19 C27 C26 120.6(3) . . ? O11 Cl1 O13 110.8(3) . . ? O11 Cl1 O12 110.4(3) . . ? O13 Cl1 O12 107.2(2) . . ? O11 Cl1 O14 109.1(2) . . ? O13 Cl1 O14 110.0(2) . . ? O12 Cl1 O14 109.31(19) . . ? O21 Cl2 O22 108.9(2) . . ? O21 Cl2 O24 110.7(2) . . ? O22 Cl2 O24 108.2(2) . . ? O21 Cl2 O23 111.5(2) . . ? O22 Cl2 O23 108.4(2) . . ? O24 Cl2 O23 109.06(18) . . ? 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 O1 Co N1 C4 117.2(2) . . . . ? N4 Co N1 C4 110.3(17) . . . . ? N3 Co N1 C4 -151.9(2) . . . . ? N2 Co N1 C4 29.3(2) . . . . ? N5 Co N1 C4 -61.3(2) . . . . ? O1 Co N1 C10 -118.0(2) . . . . ? N4 Co N1 C10 -125.0(17) . . . . ? N3 Co N1 C10 -27.1(2) . . . . ? N2 Co N1 C10 154.1(2) . . . . ? N5 Co N1 C10 63.4(2) . . . . ? O1 Co N1 C2 -0.4(2) . . . . ? N4 Co N1 C2 -7.4(18) . . . . ? N3 Co N1 C2 90.5(2) . . . . ? N2 Co N1 C2 -88.4(2) . . . . ? N5 Co N1 C2 -179.0(2) . . . . ? O1 Co N2 C5 -103.9(2) . . . . ? N4 Co N2 C5 167.7(2) . . . . ? N3 Co N2 C5 -22.1(7) . . . . ? N1 Co N2 C5 -16.1(2) . . . . ? N5 Co N2 C5 84.6(2) . . . . ? O1 Co N2 C9 68.0(3) . . . . ? N4 Co N2 C9 -20.4(3) . . . . ? N3 Co N2 C9 149.8(5) . . . . ? N1 Co N2 C9 155.8(3) . . . . ? N5 Co N2 C9 -103.5(3) . . . . ? O1 Co N3 C15 -73.1(3) . . . . ? N4 Co N3 C15 15.6(3) . . . . ? N1 Co N3 C15 -160.6(3) . . . . ? N2 Co N3 C15 -154.6(5) . . . . ? N5 Co N3 C15 98.7(3) . . . . ? O1 Co N3 C11 99.3(2) . . . . ? N4 Co N3 C11 -172.1(2) . . . . ? N1 Co N3 C11 11.8(2) . . . . ? N2 Co N3 C11 17.7(7) . . . . ? N5 Co N3 C11 -88.9(2) . . . . ? O1 Co N4 C16 0.0(3) . . . . ? N3 Co N4 C16 -90.6(3) . . . . ? N1 Co N4 C16 6.9(19) . . . . ? N2 Co N4 C16 87.5(3) . . . . ? N5 Co N4 C16 178.6(3) . . . . ? O1 Co N4 C27 -178.5(2) . . . . ? N3 Co N4 C27 91.0(2) . . . . ? N1 Co N4 C27 -171.5(16) . . . . ? N2 Co N4 C27 -90.9(2) . . . . ? N5 Co N4 C27 0.2(2) . . . . ? O1 Co N5 C25 -170.3(6) . . . . ? N4 Co N5 C25 -179.7(3) . . . . ? N3 Co N5 C25 84.6(3) . . . . ? N1 Co N5 C25 -0.3(3) . . . . ? N2 Co N5 C25 -84.6(3) . . . . ? O1 Co N5 C26 9.2(8) . . . . ? N4 Co N5 C26 -0.2(2) . . . . ? N3 Co N5 C26 -95.9(2) . . . . ? N1 Co N5 C26 179.2(2) . . . . ? N2 Co N5 C26 94.9(2) . . . . ? N4 Co O1 C1 169.4(2) . . . . ? N3 Co O1 C1 -94.8(2) . . . . ? N1 Co O1 C1 -10.1(2) . . . . ? N2 Co O1 C1 74.0(2) . . . . ? N5 Co O1 C1 160.1(6) . . . . ? Co O1 C1 O2 -164.6(3) . . . . ? Co O1 C1 C2 17.9(4) . . . . ? O2 C1 C2 N1 164.6(3) . . . . ? O1 C1 C2 N1 -17.9(4) . . . . ? C4 N1 C2 C1 -107.0(3) . . . . ? C10 N1 C2 C1 125.7(3) . . . . ? Co N1 C2 C1 9.4(3) . . . . ? C10 N1 C4 C5 -156.4(3) . . . . ? C2 N1 C4 C5 79.7(3) . . . . ? Co N1 C4 C5 -36.7(3) . . . . ? C9 N2 C5 C6 3.1(5) . . . . ? Co N2 C5 C6 175.8(3) . . . . ? C9 N2 C5 C4 -174.7(3) . . . . ? Co N2 C5 C4 -2.1(4) . . . . ? N1 C4 C5 N2 25.7(4) . . . . ? N1 C4 C5 C6 -152.0(3) . . . . ? N2 C5 C6 C7 -2.0(5) . . . . ? C4 C5 C6 C7 175.6(3) . . . . ? C5 C6 C7 C8 -0.9(5) . . . . ? C6 C7 C8 C9 2.6(5) . . . . ? C5 N2 C9 C8 -1.3(5) . . . . ? Co N2 C9 C8 -173.0(3) . . . . ? C7 C8 C9 N2 -1.5(5) . . . . ? C4 N1 C10 C11 156.4(3) . . . . ? C2 N1 C10 C11 -79.8(3) . . . . ? Co N1 C10 C11 36.6(3) . . . . ? C15 N3 C11 C12 0.8(5) . . . . ? Co N3 C11 C12 -172.2(3) . . . . ? C15 N3 C11 C10 -179.4(3) . . . . ? Co N3 C11 C10 7.6(4) . . . . ? N1 C10 C11 N3 -29.3(4) . . . . ? N1 C10 C11 C12 150.5(3) . . . . ? N3 C11 C12 C13 -0.8(5) . . . . ? C10 C11 C12 C13 179.4(3) . . . . ? C11 C12 C13 C14 0.6(5) . . . . ? C12 C13 C14 C15 -0.5(6) . . . . ? C11 N3 C15 C14 -0.7(5) . . . . ? Co N3 C15 C14 171.4(3) . . . . ? C13 C14 C15 N3 0.6(6) . . . . ? C27 N4 C16 C17 0.6(5) . . . . ? Co N4 C16 C17 -177.8(2) . . . . ? N4 C16 C17 C18 -1.5(5) . . . . ? C16 C17 C18 C19 0.7(5) . . . . ? C17 C18 C19 C27 0.8(5) . . . . ? C17 C18 C19 C20 179.6(3) . . . . ? C27 C19 C20 C21 1.6(5) . . . . ? C18 C19 C20 C21 -177.2(4) . . . . ? C19 C20 C21 C22 -0.6(6) . . . . ? C20 C21 C22 C23 178.9(3) . . . . ? C20 C21 C22 C26 -1.0(5) . . . . ? C26 C22 C23 C24 -1.5(5) . . . . ? C21 C22 C23 C24 178.5(3) . . . . ? C22 C23 C24 C25 0.8(5) . . . . ? C26 N5 C25 C24 -1.5(5) . . . . ? Co N5 C25 C24 178.0(3) . . . . ? C23 C24 C25 N5 0.8(6) . . . . ? C25 N5 C26 C22 0.6(5) . . . . ? Co N5 C26 C22 -179.0(3) . . . . ? C25 N5 C26 C27 179.9(3) . . . . ? Co N5 C26 C27 0.3(4) . . . . ? C23 C22 C26 N5 0.8(5) . . . . ? C21 C22 C26 N5 -179.2(3) . . . . ? C23 C22 C26 C27 -178.4(3) . . . . ? C21 C22 C26 C27 1.6(5) . . . . ? C16 N4 C27 C19 1.1(5) . . . . ? Co N4 C27 C19 179.6(3) . . . . ? C16 N4 C27 C26 -178.6(3) . . . . ? Co N4 C27 C26 0.0(4) . . . . ? C18 C19 C27 N4 -1.8(5) . . . . ? C20 C19 C27 N4 179.3(3) . . . . ? C18 C19 C27 C26 177.9(3) . . . . ? C20 C19 C27 C26 -1.0(5) . . . . ? N5 C26 C27 N4 -0.2(4) . . . . ? C22 C26 C27 N4 179.1(3) . . . . ? N5 C26 C27 C19 -179.9(3) . . . . ? C22 C26 C27 C19 -0.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 23.51 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.855 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.065 #===END data_stmetf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H22 Cl2 Co N5 O9' _chemical_formula_weight 666.31 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 Orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.158(5) _cell_length_b 8.978(2) _cell_length_c 34.173(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5571(2) _cell_formula_units_Z 8 _cell_measurement_temperature 159(2) _cell_measurement_reflns_used - _cell_measurement_theta_min - _cell_measurement_theta_max - _exptl_crystal_description block _exptl_crystal_colour psychedelic _exptl_crystal_size_max .1 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .65 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 159(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 42616 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.65 _reflns_number_total 11940 _reflns_number_gt 7354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.326(17) _refine_ls_number_reflns 11940 _refine_ls_number_parameters 773 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _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 0.11436(3) 0.25045(6) 0.456341(19) 0.03412(14) Uani 1 1 d . . . N1 N 0.0401(2) 0.2613(4) 0.49825(12) 0.0402(10) Uani 1 1 d . . . C1 C -0.0295(3) 0.2130(5) 0.49748(16) 0.0464(13) Uani 1 1 d . . . H1A H -0.0476 0.1646 0.4747 0.056 Uiso 1 1 calc R . . N1' N 0.2875(2) 0.2479(4) 0.21377(11) 0.0368(9) Uani 1 1 d . . . C1' C 0.2175(3) 0.2933(6) 0.21544(18) 0.0486(13) Uani 1 1 d . . . H1'A H 0.2000 0.3359 0.2391 0.058 Uiso 1 1 calc R . . C2 C -0.0760(4) 0.2324(7) 0.5296(2) 0.0610(18) Uani 1 1 d . . . H2A H -0.1258 0.2007 0.5278 0.073 Uiso 1 1 calc R . . Co2 Co 0.36343(3) 0.25472(6) 0.254251(18) 0.03298(14) Uani 1 1 d . . . C2' C 0.1694(3) 0.2813(7) 0.1844(2) 0.0569(16) Uani 1 1 d . . . H2'A H 0.1208 0.3200 0.1861 0.068 Uiso 1 1 calc R . . C3 C -0.0510(4) 0.2967(7) 0.5639(2) 0.0598(18) Uani 1 1 d . . . H3A H -0.0827 0.3061 0.5859 0.072 Uiso 1 1 calc R . . C3' C 0.1934(4) 0.2121(7) 0.1510(2) 0.0578(17) Uani 1 1 d . . . H3'A H 0.1598 0.1976 0.1301 0.069 Uiso 1 1 calc R . . C4 C 0.0219(3) 0.3478(5) 0.56558(16) 0.0485(14) Uani 1 1 d . . . C4' C 0.2650(3) 0.1628(5) 0.14700(15) 0.0471(13) Uani 1 1 d . . . C5 C 0.0542(4) 0.4187(6) 0.59807(18) 0.0616(16) Uani 1 1 d . . . H5A H 0.0247 0.4373 0.6205 0.074 Uiso 1 1 calc R . . C5' C 0.2955(4) 0.0875(6) 0.11260(16) 0.0615(17) Uani 1 1 d . . . H5'A H 0.2652 0.0715 0.0903 0.074 Uiso 1 1 calc R . . C6 C 0.1259(5) 0.4615(8) 0.5986(2) 0.072(2) Uani 1 1 d . . . H6A H 0.1456 0.5060 0.6215 0.086 Uiso 1 1 calc R . . C6' C 0.3674(4) 0.0399(7) 0.1123(2) 0.0540(17) Uani 1 1 d . . . H6'A H 0.3858 -0.0126 0.0902 0.065 Uiso 1 1 calc R . . C7 C 0.1733(3) 0.4402(6) 0.56438(15) 0.0479(14) Uani 1 1 d . . . C7' C 0.4148(3) 0.0688(5) 0.14489(14) 0.0433(13) Uani 1 1 d . . . C8 C 0.2473(5) 0.4764(6) 0.5628(2) 0.054(2) Uani 1 1 d . . . H8A H 0.2703 0.5237 0.5845 0.064 Uiso 1 1 calc R . . C8' C 0.4909(5) 0.0318(7) 0.1453(2) 0.0502(17) Uani 1 1 d . . . H8'A H 0.5130 -0.0128 0.1230 0.060 Uiso 1 1 calc R . . C9 C 0.2869(3) 0.4438(6) 0.53008(16) 0.0481(13) Uani 1 1 d . . . H9A H 0.3380 0.4658 0.5289 0.058 Uiso 1 1 calc R . . C9' C 0.5324(3) 0.0605(5) 0.17791(15) 0.0453(13) Uani 1 1 d . . . H9'A H 0.5831 0.0348 0.1787 0.054 Uiso 1 1 calc R . . N10 N 0.1812(2) 0.3415(4) 0.49809(11) 0.0332(9) Uani 1 1 d . . . C10 C 0.2507(3) 0.3762(4) 0.49738(14) 0.0379(11) Uani 1 1 d . . . H10A H 0.2784 0.3559 0.4744 0.046 Uiso 1 1 calc R . . N10' N 0.4271(2) 0.1655(4) 0.21107(11) 0.0339(9) Uani 1 1 d . . . C10' C 0.4981(3) 0.1290(5) 0.21030(15) 0.0386(11) Uani 1 1 d . . . H10B H 0.5272 0.1503 0.2327 0.046 Uiso 1 1 calc R . . C11 C 0.1418(3) 0.3706(5) 0.53179(14) 0.0350(11) Uani 1 1 d . . . C11' C 0.3860(3) 0.1379(5) 0.17798(14) 0.0383(12) Uani 1 1 d . . . C12 C 0.0663(3) 0.3250(5) 0.53148(14) 0.0405(12) Uani 1 1 d . . . C12' C 0.3106(3) 0.1827(5) 0.17887(14) 0.0373(11) Uani 1 1 d . . . N13 N 0.1536(2) 0.2101(4) 0.40595(12) 0.0378(10) Uani 1 1 d . . . C13 C 0.0789(3) 0.1651(6) 0.40827(17) 0.0434(13) Uani 1 1 d . . . H13A H 0.059(2) 0.046(6) 0.4081(14) 0.047(13) Uiso 1 1 d . . . H13B H 0.051(3) 0.214(6) 0.3967(16) 0.038(17) Uiso 1 1 d . . . N13' N 0.4055(2) 0.2911(4) 0.30445(12) 0.0354(9) Uani 1 1 d . . . C13' C 0.3306(3) 0.3361(6) 0.30323(16) 0.0422(13) Uani 1 1 d . . . H13C H 0.321(2) 0.440(6) 0.3059(12) 0.028(11) Uiso 1 1 d . . . H13D H 0.304(3) 0.291(6) 0.3174(14) 0.029(14) Uiso 1 1 d . . . C14 C 0.2112(3) 0.0937(5) 0.40683(15) 0.0458(13) Uani 1 1 d . . . H14A H 0.2605 0.1406 0.4073 0.055 Uiso 1 1 calc R . . H14B H 0.2078 0.0310 0.3831 0.055 Uiso 1 1 calc R . . C14' C 0.4623(3) 0.4080(5) 0.30402(15) 0.0443(12) Uani 1 1 d . . . H14C H 0.5119 0.3630 0.3020 0.053 Uiso 1 1 calc R . . H14D H 0.4600 0.4676 0.3284 0.053 Uiso 1 1 calc R . . N15 N 0.1521(2) 0.0555(4) 0.46922(13) 0.0399(10) Uani 1 1 d . . . C15 C 0.2010(5) 0.0003(5) 0.4423(3) 0.042(2) Uani 1 1 d . . . N15' N 0.4012(2) 0.4515(5) 0.24145(13) 0.0395(10) Uani 1 1 d . . . C15' C 0.4470(5) 0.5049(5) 0.2690(3) 0.043(2) Uani 1 1 d . . . C16 C 0.2348(3) -0.1363(5) 0.44750(19) 0.0573(16) Uani 1 1 d . . . H16A H 0.2655 -0.1763 0.4276 0.069 Uiso 1 1 calc R . . C16' C 0.4845(3) 0.6400(5) 0.26333(19) 0.0552(15) Uani 1 1 d . . . H16B H 0.5190 0.6754 0.2821 0.066 Uiso 1 1 calc R . . C17' C 0.4697(4) 0.7201(5) 0.2294(2) 0.0650(18) Uani 1 1 d . . . H17A H 0.4938 0.8125 0.2250 0.078 Uiso 1 1 calc R . . C17 C 0.2239(3) -0.2133(5) 0.48154(19) 0.0570(16) Uani 1 1 d . . . H17B H 0.2497 -0.3035 0.4863 0.068 Uiso 1 1 calc R . . C18 C 0.1745(4) -0.1581(6) 0.50915(19) 0.0588(16) Uani 1 1 d . . . H18A H 0.1654 -0.2118 0.5326 0.071 Uiso 1 1 calc R . . C18' C 0.4205(3) 0.6668(5) 0.2024(2) 0.0604(17) Uani 1 1 d . . . H18B H 0.4094 0.7220 0.1795 0.072 Uiso 1 1 calc R . . C19 C 0.1392(5) -0.0258(6) 0.5023(2) 0.0504(19) Uani 1 1 d . . . H19A H 0.1048 0.0103 0.5209 0.061 Uiso 1 1 calc R . . C19' C 0.3875(4) 0.5305(7) 0.2094(2) 0.0486(17) Uani 1 1 d . . . H19B H 0.3538 0.4922 0.1907 0.058 Uiso 1 1 calc R . . N20 N 0.0949(2) 0.4465(4) 0.43484(12) 0.0336(9) Uani 1 1 d . . . C20 C 0.0556(3) 0.5568(5) 0.45164(16) 0.0367(11) Uani 1 1 d . . . H20A H 0.0332 0.5392 0.4763 0.044 Uiso 1 1 calc R . . N20' N 0.3436(2) 0.0572(4) 0.27557(12) 0.0359(9) Uani 1 1 d . . . C20' C 0.3049(3) -0.0517(5) 0.25829(17) 0.0391(11) Uani 1 1 d . . . H20B H 0.2840 -0.0354 0.2331 0.047 Uiso 1 1 calc R . . C21 C 0.0467(3) 0.6953(5) 0.43413(15) 0.0406(12) Uani 1 1 d . . . H21A H 0.0199 0.7725 0.4468 0.049 Uiso 1 1 calc R . . C21' C 0.2948(3) -0.1882(5) 0.27678(16) 0.0453(13) Uani 1 1 d . . . H21B H 0.2678 -0.2648 0.2640 0.054 Uiso 1 1 calc R . . C22 C 0.0784(3) 0.7174(5) 0.39736(16) 0.0442(13) Uani 1 1 d . . . H22A H 0.0731 0.8109 0.3846 0.053 Uiso 1 1 calc R . . C22' C 0.3233(3) -0.2128(6) 0.31292(19) 0.0548(16) Uani 1 1 d . . . H22B H 0.3148 -0.3044 0.3261 0.066 Uiso 1 1 calc R . . C23 C 0.1175(3) 0.6049(5) 0.37932(17) 0.0442(13) Uani 1 1 d . . . H23A H 0.1383 0.6193 0.3541 0.053 Uiso 1 1 calc R . . C23' C 0.3653(3) -0.1017(6) 0.33034(17) 0.0479(13) Uani 1 1 d . . . H23B H 0.3870 -0.1170 0.3553 0.057 Uiso 1 1 calc R . . C24 C 0.1255(3) 0.4715(6) 0.3986(2) 0.0335(14) Uani 1 1 d . . . C24' C 0.3752(4) 0.0333(7) 0.3105(2) 0.0396(14) Uani 1 1 d . . . C25 C 0.1703(3) 0.3464(5) 0.38260(15) 0.0416(12) Uani 1 1 d . . . H25A H 0.2234 0.3705 0.3845 0.050 Uiso 1 1 calc R . . H25B H 0.1580 0.3296 0.3547 0.050 Uiso 1 1 calc R . . C25' C 0.4236(3) 0.1565(5) 0.32594(15) 0.0459(13) Uani 1 1 d . . . H25C H 0.4147 0.1713 0.3543 0.055 Uiso 1 1 calc R . . H25D H 0.4762 0.1308 0.3221 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.05087(12) 0.2039(2) 0.04564(6) 0.0792(6) Uani 1 1 d . . . O11 O 0.1153(4) 0.1354(7) 0.0408(4) 0.237(6) Uani 1 1 d . . . O12 O 0.0671(5) 0.2814(9) 0.0832(2) 0.157(3) Uani 1 1 d . . . O13 O -0.0069(3) 0.1115(8) 0.05462(19) 0.142(3) Uani 1 1 d . . . O14 O 0.0365(3) 0.3273(7) 0.02295(18) 0.115(2) Uani 1 1 d . . . Cl2 Cl 0.69698(12) 0.2890(2) 0.16359(6) 0.0788(6) Uani 1 1 d . . . O21 O 0.6793(4) 0.2257(9) 0.12609(19) 0.145(3) Uani 1 1 d . . . O22 O 0.6322(4) 0.3606(6) 0.1759(3) 0.177(4) Uani 1 1 d . . . O23 O 0.7520(4) 0.3925(7) 0.1590(2) 0.154(3) Uani 1 1 d . . . O24 O 0.2119(4) -0.1687(6) 0.18631(17) 0.120(2) Uani 1 1 d . . . Cl3 Cl 0.36996(9) 0.53171(17) 0.40789(5) 0.0413(4) Uani 1 1 d . . . O31 O 0.3012(2) 0.5931(4) 0.39401(12) 0.0584(10) Uani 1 1 d . . . O32 O 0.4296(2) 0.5959(5) 0.38682(11) 0.0632(11) Uani 1 1 d . . . O33 O 0.3782(3) 0.5587(5) 0.44867(11) 0.0648(12) Uani 1 1 d . . . O34 O 0.3684(3) 0.3725(4) 0.40095(13) 0.0668(12) Uani 1 1 d . . . Cl4 Cl 0.62002(9) -0.03056(17) 0.30051(5) 0.0392(3) Uani 1 1 d . . . O41 O 0.5572(2) -0.0989(4) 0.31817(14) 0.0722(12) Uani 1 1 d . . . O42 O 0.6199(3) 0.1196(5) 0.31135(18) 0.107(2) Uani 1 1 d . . . O43 O 0.6858(2) -0.1020(5) 0.31378(12) 0.0772(13) Uani 1 1 d . . . O44 O 0.6178(3) -0.0429(7) 0.25899(14) 0.0974(18) Uani 1 1 d . . . OW1 O 0.3848(3) 0.1009(6) 0.4439(2) 0.122(2) Uani 1 1 d . . . OW2 O 0.6338(3) 0.3933(6) 0.2647(2) 0.120(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0391(3) 0.0277(3) 0.0355(3) -0.0011(2) -0.0004(3) 0.0036(3) N1 0.040(3) 0.035(2) 0.046(3) 0.0048(18) 0.001(2) 0.0059(17) C1 0.040(3) 0.045(3) 0.053(3) 0.010(2) -0.002(3) 0.005(2) N1' 0.038(2) 0.0304(17) 0.042(2) 0.0056(17) 0.0004(19) -0.0031(17) C1' 0.037(3) 0.046(3) 0.063(4) 0.003(2) 0.002(3) -0.003(2) C2 0.040(4) 0.049(3) 0.094(5) 0.012(3) 0.010(4) -0.002(3) Co2 0.0348(3) 0.0291(3) 0.0351(3) -0.0010(3) 0.0006(3) -0.0018(3) C2' 0.035(3) 0.062(3) 0.074(5) 0.025(3) -0.014(3) 0.001(3) C3 0.070(5) 0.049(3) 0.060(4) 0.011(3) 0.032(4) 0.020(3) C3' 0.056(4) 0.062(3) 0.055(4) 0.012(3) -0.017(3) -0.011(3) C4 0.052(4) 0.045(3) 0.048(3) 0.012(2) 0.015(3) 0.012(2) C4' 0.050(4) 0.052(3) 0.040(3) 0.011(2) -0.011(3) -0.011(2) C5 0.073(5) 0.069(4) 0.043(4) 0.002(3) 0.017(3) 0.012(3) C5' 0.093(5) 0.060(3) 0.031(3) 0.003(2) -0.012(3) -0.028(3) C6 0.107(7) 0.065(3) 0.045(5) 0.003(4) 0.001(4) 0.013(5) C6' 0.068(5) 0.063(3) 0.032(4) -0.007(3) -0.003(3) -0.018(4) C7 0.064(4) 0.045(3) 0.035(3) -0.004(2) -0.003(3) 0.007(3) C7' 0.057(4) 0.037(3) 0.037(3) 0.006(2) 0.007(3) -0.005(2) C8 0.076(5) 0.036(2) 0.049(4) -0.003(3) -0.018(4) -0.004(3) C8' 0.065(5) 0.050(3) 0.036(4) -0.001(3) 0.015(3) -0.005(3) C9 0.058(4) 0.040(3) 0.046(3) 0.007(2) -0.018(3) -0.002(3) C9' 0.046(3) 0.040(3) 0.050(3) 0.003(2) 0.004(3) -0.001(2) N10 0.033(2) 0.0302(18) 0.037(2) 0.0023(15) -0.0018(19) 0.0031(15) C10 0.044(3) 0.029(2) 0.041(3) 0.0027(19) -0.001(2) 0.007(2) N10' 0.035(2) 0.0279(18) 0.038(2) -0.0022(15) 0.0022(19) -0.0081(16) C10' 0.037(3) 0.034(2) 0.045(3) 0.000(2) 0.003(2) -0.0028(19) C11 0.041(3) 0.031(2) 0.033(3) 0.0056(18) 0.005(2) 0.007(2) C11' 0.050(3) 0.029(2) 0.036(3) 0.0039(19) 0.003(3) -0.010(2) C12 0.056(4) 0.033(2) 0.033(3) 0.0032(19) 0.003(3) 0.012(2) C12' 0.043(3) 0.030(2) 0.039(3) 0.0110(19) -0.002(2) -0.007(2) N13 0.043(3) 0.0326(18) 0.038(2) -0.0051(17) 0.002(2) 0.0045(17) C13 0.045(4) 0.035(3) 0.049(4) -0.002(2) -0.004(3) 0.002(2) N13' 0.032(2) 0.0411(19) 0.033(2) -0.0085(17) 0.0001(19) 0.0000(17) C13' 0.048(4) 0.037(3) 0.042(3) -0.005(2) 0.014(3) -0.006(2) C14 0.051(3) 0.041(2) 0.046(3) -0.004(2) -0.006(3) 0.014(2) C14' 0.040(3) 0.047(2) 0.046(3) -0.016(2) 0.000(3) -0.006(2) N15 0.041(3) 0.034(2) 0.045(3) 0.0010(19) -0.007(2) 0.0054(19) C15 0.040(5) 0.038(4) 0.049(5) -0.0086(19) -0.016(4) 0.0060(19) N15' 0.041(3) 0.029(2) 0.048(3) -0.0043(19) 0.006(2) 0.0001(18) C15' 0.042(5) 0.030(4) 0.057(6) -0.012(2) 0.003(4) -0.0025(18) C16 0.053(4) 0.042(3) 0.078(5) -0.016(3) -0.003(3) 0.010(2) C16' 0.047(3) 0.037(2) 0.081(5) -0.013(3) 0.011(3) -0.011(2) C17' 0.075(5) 0.031(3) 0.089(5) -0.003(3) 0.029(4) -0.010(3) C17 0.068(4) 0.028(2) 0.075(4) 0.001(3) -0.014(4) 0.009(2) C18 0.075(5) 0.043(3) 0.058(4) 0.010(3) -0.009(3) 0.000(3) C18' 0.076(5) 0.035(3) 0.071(4) 0.009(3) 0.009(4) -0.010(3) C19 0.069(5) 0.036(2) 0.047(4) -0.004(3) -0.004(3) 0.003(3) C19' 0.053(4) 0.041(2) 0.052(5) 0.008(3) 0.008(3) -0.003(3) N20 0.041(3) 0.025(2) 0.035(3) -0.0008(18) -0.003(2) -0.0022(18) C20 0.036(3) 0.035(3) 0.038(3) 0.000(2) -0.003(3) 0.001(2) N20' 0.037(3) 0.038(2) 0.033(3) 0.0015(19) 0.006(2) -0.0039(19) C20' 0.037(3) 0.035(3) 0.045(3) -0.006(2) 0.012(3) -0.004(2) C21 0.040(3) 0.031(2) 0.051(3) -0.001(2) -0.004(3) 0.002(2) C21' 0.045(3) 0.034(2) 0.057(4) -0.004(2) 0.010(3) -0.004(2) C22 0.053(4) 0.029(2) 0.051(3) 0.009(2) -0.008(3) 0.002(2) C22' 0.056(4) 0.038(3) 0.071(4) 0.005(3) 0.017(3) 0.008(3) C23 0.048(4) 0.037(3) 0.048(4) 0.005(3) -0.011(3) -0.002(2) C23' 0.057(4) 0.048(3) 0.038(3) 0.009(2) 0.006(3) 0.016(3) C24 0.027(3) 0.037(2) 0.037(4) -0.007(3) -0.003(3) 0.001(3) C24' 0.043(4) 0.041(2) 0.034(4) 0.008(3) 0.005(3) 0.012(3) C25 0.046(3) 0.040(3) 0.039(3) 0.001(2) -0.005(3) 0.003(2) C25' 0.053(4) 0.048(3) 0.036(3) -0.001(2) -0.006(3) 0.005(2) Cl1 0.0784(15) 0.0765(11) 0.0828(14) 0.0391(11) -0.0212(11) -0.0246(10) O11 0.082(5) 0.090(4) 0.539(19) 0.081(8) -0.077(7) -0.002(4) O12 0.183(8) 0.152(6) 0.137(6) 0.004(5) -0.056(6) -0.005(5) O13 0.105(5) 0.179(6) 0.142(6) 0.060(5) -0.018(4) -0.090(4) O14 0.111(4) 0.110(4) 0.124(5) 0.065(4) -0.027(4) 0.008(3) Cl2 0.0725(14) 0.0816(11) 0.0822(14) 0.0366(11) -0.0195(11) -0.0262(10) O21 0.125(5) 0.214(8) 0.095(5) 0.036(5) -0.062(4) -0.029(5) O22 0.124(5) 0.078(4) 0.331(11) 0.014(5) 0.096(6) 0.001(4) O23 0.119(5) 0.131(5) 0.210(7) 0.026(5) -0.016(5) -0.064(4) O24 0.155(6) 0.113(4) 0.093(4) -0.052(3) -0.011(4) -0.031(4) Cl3 0.0450(9) 0.0401(5) 0.0389(8) -0.0026(7) 0.0016(7) 0.0007(8) O31 0.046(2) 0.0485(19) 0.080(3) -0.0030(18) -0.012(2) 0.0078(17) O32 0.048(2) 0.090(3) 0.052(2) 0.012(2) 0.0128(19) -0.010(2) O33 0.082(3) 0.082(3) 0.030(2) -0.009(2) -0.003(2) -0.022(2) O34 0.087(4) 0.0372(19) 0.076(3) -0.0061(18) -0.022(3) 0.009(2) Cl4 0.0393(9) 0.0391(5) 0.0392(8) -0.0002(7) 0.0012(6) 0.0019(7) O41 0.053(3) 0.065(2) 0.099(3) -0.012(2) 0.020(2) -0.012(2) O42 0.105(4) 0.051(2) 0.166(5) -0.046(3) 0.074(4) -0.024(3) O43 0.049(3) 0.116(3) 0.067(3) 0.047(3) 0.001(2) 0.017(2) O44 0.099(4) 0.161(5) 0.033(3) 0.001(3) -0.016(3) 0.032(4) OW1 0.095(4) 0.077(3) 0.195(6) 0.021(4) -0.025(4) -0.018(3) OW2 0.078(3) 0.086(3) 0.195(6) 0.009(4) 0.028(4) 0.021(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 N13 1.898(4) . ? Co1 C13 1.924(6) . ? Co1 N15 1.931(4) . ? Co1 N20 1.940(4) . ? Co1 N1 1.970(4) . ? Co1 N10 2.044(4) . ? N1 C1 1.335(7) . ? N1 C12 1.358(6) . ? C1 C2 1.395(8) . ? N1' C1' 1.338(6) . ? N1' C12' 1.393(6) . ? N1' Co2 1.953(4) . ? C1' C2' 1.377(8) . ? C2 C3 1.385(10) . ? Co2 N13' 1.906(4) . ? Co2 C13' 1.921(5) . ? Co2 N15' 1.945(4) . ? Co2 N20' 1.951(4) . ? Co2 N10' 2.038(4) . ? C2' C3' 1.370(9) . ? C3 C4 1.403(8) . ? C3' C4' 1.381(8) . ? C4 C5 1.408(8) . ? C4 C12 1.431(7) . ? C4' C12' 1.380(7) . ? C4' C5' 1.464(8) . ? C5 C6 1.358(10) . ? C5' C6' 1.374(9) . ? C6 C7 1.464(9) . ? C6' C7' 1.433(8) . ? C7 C8 1.383(10) . ? C7 C11 1.400(7) . ? C7' C11' 1.392(7) . ? C7' C8' 1.421(9) . ? C8 C9 1.362(10) . ? C8' C9' 1.370(9) . ? C9 C10 1.431(7) . ? C9' C10' 1.411(7) . ? N10 C10 1.300(6) . ? N10 C11 1.381(6) . ? N10' C10' 1.330(6) . ? N10' C11' 1.376(6) . ? C11 C12 1.430(7) . ? C11' C12' 1.428(7) . ? N13 C13 1.417(7) . ? N13 C14 1.480(6) . ? N13 C25 1.492(6) . ? N13' C13' 1.420(7) . ? N13' C25' 1.452(6) . ? N13' C14' 1.472(6) . ? C14 C15 1.484(9) . ? C14' C15' 1.506(9) . ? N15 C19 1.365(8) . ? N15 C15 1.372(9) . ? C15 C16 1.383(7) . ? N15' C19' 1.328(8) . ? N15' C15' 1.344(9) . ? C15' C16' 1.404(7) . ? C16 C17 1.368(8) . ? C16' C17' 1.390(8) . ? C17' C18' 1.370(9) . ? C17 C18 1.392(8) . ? C18 C19 1.371(8) . ? C18' C19' 1.384(8) . ? N20 C20 1.349(6) . ? N20 C24 1.378(8) . ? C20 C21 1.389(7) . ? N20' C24' 1.340(8) . ? N20' C20' 1.342(7) . ? C20' C21' 1.391(7) . ? C21 C22 1.397(7) . ? C21' C22' 1.357(8) . ? C22 C23 1.379(7) . ? C22' C23' 1.390(8) . ? C23 C24 1.374(7) . ? C23' C24' 1.400(8) . ? C24 C25 1.489(7) . ? C24' C25' 1.509(8) . ? Cl1 O11 1.332(8) . ? Cl1 O13 1.371(5) . ? Cl1 O14 1.378(5) . ? Cl1 O12 1.488(8) . ? Cl2 O24 1.357(5) 3 ? Cl2 O23 1.373(6) . ? Cl2 O22 1.405(6) . ? Cl2 O21 1.439(7) . ? O24 Cl2 1.357(5) 3_455 ? Cl3 O32 1.422(4) . ? Cl3 O33 1.422(4) . ? Cl3 O31 1.444(4) . ? Cl3 O34 1.449(3) . ? Cl4 O42 1.398(4) . ? Cl4 O44 1.424(5) . ? Cl4 O41 1.430(4) . ? Cl4 O43 1.430(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 N13 Co1 C13 43.5(2) . . ? N13 Co1 N15 84.31(18) . . ? C13 Co1 N15 87.3(2) . . ? N13 Co1 N20 84.12(17) . . ? C13 Co1 N20 88.7(2) . . ? N15 Co1 N20 166.82(19) . . ? N13 Co1 N1 157.79(18) . . ? C13 Co1 N1 114.3(2) . . ? N15 Co1 N1 97.03(17) . . ? N20 Co1 N1 96.06(17) . . ? N13 Co1 N10 119.13(17) . . ? C13 Co1 N10 162.6(2) . . ? N15 Co1 N10 89.59(16) . . ? N20 Co1 N10 90.54(15) . . ? N1 Co1 N10 83.07(17) . . ? C1 N1 C12 119.0(5) . . ? C1 N1 Co1 128.1(4) . . ? C12 N1 Co1 112.9(3) . . ? N1 C1 C2 121.1(6) . . ? C1' N1' C12' 116.8(4) . . ? C1' N1' Co2 129.1(4) . . ? C12' N1' Co2 114.0(3) . . ? N1' C1' C2' 123.1(6) . . ? C3 C2 C1 121.4(6) . . ? N13' Co2 C13' 43.5(2) . . ? N13' Co2 N15' 84.57(18) . . ? C13' Co2 N15' 87.7(2) . . ? N13' Co2 N20' 83.88(18) . . ? C13' Co2 N20' 87.9(2) . . ? N15' Co2 N20' 167.10(19) . . ? N13' Co2 N1' 157.73(17) . . ? C13' Co2 N1' 114.2(2) . . ? N15' Co2 N1' 96.78(16) . . ? N20' Co2 N1' 96.08(17) . . ? N13' Co2 N10' 119.46(17) . . ? C13' Co2 N10' 163.0(2) . . ? N15' Co2 N10' 89.69(16) . . ? N20' Co2 N10' 90.99(15) . . ? N1' Co2 N10' 82.80(16) . . ? C3' C2' C1' 118.3(6) . . ? C2 C3 C4 118.6(6) . . ? C2' C3' C4' 121.9(6) . . ? C3 C4 C5 124.9(6) . . ? C3 C4 C12 116.9(5) . . ? C5 C4 C12 118.2(5) . . ? C12' C4' C3' 116.4(5) . . ? C12' C4' C5' 117.9(5) . . ? C3' C4' C5' 125.7(6) . . ? C6 C5 C4 122.5(6) . . ? C6' C5' C4' 120.6(6) . . ? C5 C6 C7 121.1(7) . . ? C5' C6' C7' 120.6(6) . . ? C8 C7 C11 118.2(5) . . ? C8 C7 C6 124.8(6) . . ? C11 C7 C6 116.9(6) . . ? C11' C7' C8' 117.5(5) . . ? C11' C7' C6' 119.1(5) . . ? C8' C7' C6' 123.4(6) . . ? C9 C8 C7 119.6(6) . . ? C9' C8' C7' 119.9(6) . . ? C8 C9 C10 119.4(6) . . ? C8' C9' C10' 118.5(6) . . ? C10 N10 C11 118.3(4) . . ? C10 N10 Co1 131.2(3) . . ? C11 N10 Co1 110.5(3) . . ? N10 C10 C9 122.2(5) . . ? C10' N10' C11' 117.6(4) . . ? C10' N10' Co2 131.3(3) . . ? C11' N10' Co2 111.0(3) . . ? N10' C10' C9' 123.4(5) . . ? N10 C11 C7 122.4(4) . . ? N10 C11 C12 115.9(4) . . ? C7 C11 C12 121.7(5) . . ? N10' C11' C7' 123.0(5) . . ? N10' C11' C12' 116.8(4) . . ? C7' C11' C12' 120.2(5) . . ? N1 C12 C11 117.6(4) . . ? N1 C12 C4 122.9(5) . . ? C11 C12 C4 119.5(5) . . ? C4' C12' N1' 123.4(5) . . ? C4' C12' C11' 121.5(5) . . ? N1' C12' C11' 115.2(4) . . ? C13 N13 C14 118.3(4) . . ? C13 N13 C25 117.3(4) . . ? C14 N13 C25 116.5(4) . . ? C13 N13 Co1 69.2(3) . . ? C14 N13 Co1 112.4(3) . . ? C25 N13 Co1 113.9(3) . . ? N13 C13 Co1 67.3(3) . . ? C13' N13' C25' 118.0(4) . . ? C13' N13' C14' 117.9(4) . . ? C25' N13' C14' 116.1(4) . . ? C13' N13' Co2 68.8(3) . . ? C25' N13' Co2 113.8(3) . . ? C14' N13' Co2 113.2(3) . . ? N13' C13' Co2 67.7(3) . . ? N13 C14 C15 109.1(5) . . ? N13' C14' C15' 106.9(4) . . ? C19 N15 C15 118.3(5) . . ? C19 N15 Co1 127.8(4) . . ? C15 N15 Co1 113.8(4) . . ? N15 C15 C16 121.4(7) . . ? N15 C15 C14 115.1(4) . . ? C16 C15 C14 123.4(7) . . ? C19' N15' C15' 120.2(5) . . ? C19' N15' Co2 127.2(4) . . ? C15' N15' Co2 112.6(4) . . ? N15' C15' C16' 120.8(7) . . ? N15' C15' C14' 117.7(4) . . ? C16' C15' C14' 121.2(7) . . ? C17 C16 C15 119.6(6) . . ? C17' C16' C15' 117.9(6) . . ? C18' C17' C16' 120.4(5) . . ? C16 C17 C18 119.4(5) . . ? C19 C18 C17 119.5(6) . . ? C17' C18' C19' 118.4(6) . . ? N15 C19 C18 121.7(7) . . ? N15' C19' C18' 122.2(7) . . ? C20 N20 C24 118.5(5) . . ? C20 N20 Co1 127.0(4) . . ? C24 N20 Co1 114.5(3) . . ? N20 C20 C21 122.4(5) . . ? C24' N20' C20' 119.9(5) . . ? C24' N20' Co2 113.5(4) . . ? C20' N20' Co2 126.5(4) . . ? N20' C20' C21' 120.7(6) . . ? C20 C21 C22 117.8(5) . . ? C22' C21' C20' 120.5(5) . . ? C23 C22 C21 120.7(5) . . ? C21' C22' C23' 118.8(5) . . ? C24 C23 C22 118.7(6) . . ? C22' C23' C24' 118.9(6) . . ? C23 C24 N20 122.0(5) . . ? C23 C24 C25 122.7(6) . . ? N20 C24 C25 115.3(5) . . ? N20' C24' C23' 121.0(6) . . ? N20' C24' C25' 116.3(5) . . ? C23' C24' C25' 122.6(6) . . ? C24 C25 N13 108.1(4) . . ? N13' C25' C24' 107.5(4) . . ? O11 Cl1 O13 114.9(5) . . ? O11 Cl1 O14 117.9(5) . . ? O13 Cl1 O14 117.9(4) . . ? O11 Cl1 O12 98.5(6) . . ? O13 Cl1 O12 104.0(5) . . ? O14 Cl1 O12 98.4(5) . . ? O24 Cl2 O23 117.3(5) 3 . ? O24 Cl2 O22 111.1(5) 3 . ? O23 Cl2 O22 109.5(5) . . ? O24 Cl2 O21 103.9(4) 3 . ? O23 Cl2 O21 109.1(5) . . ? O22 Cl2 O21 105.1(5) . . ? O32 Cl3 O33 110.3(3) . . ? O32 Cl3 O31 109.7(3) . . ? O33 Cl3 O31 110.4(3) . . ? O32 Cl3 O34 109.4(3) . . ? O33 Cl3 O34 109.3(3) . . ? O31 Cl3 O34 107.8(2) . . ? O42 Cl4 O44 109.8(4) . . ? O42 Cl4 O41 107.5(3) . . ? O44 Cl4 O41 111.4(4) . . ? O42 Cl4 O43 110.5(4) . . ? O44 Cl4 O43 107.8(3) . . ? O41 Cl4 O43 109.9(3) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.751 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.061 #===END data_stdrf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H42 Cl4 Co2 N10 O18' _chemical_formula_weight 1306.58 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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.652(10) _cell_length_b 11.320(5) _cell_length_c 12.352(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.142(6) _cell_angle_gamma 90.00 _cell_volume 2763(2) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description thin_block _exptl_crystal_colour ? _exptl_crystal_size_max .04 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.875 _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 168(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 6574 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.1397 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.00 _reflns_number_total 2287 _reflns_number_gt 1194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2287 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _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 0.09184(5) 0.0000 0.17519(9) 0.0232(3) Uani 1 2 d S . . O1 O 0.0021(2) 0.0000 0.0595(4) 0.0296(12) Uani 1 2 d S . . N1 N 0.0704(2) 0.1190(4) 0.2657(4) 0.0282(11) Uani 1 1 d . . . N2 N 0.1830(3) 0.0000 0.3119(5) 0.0270(15) Uani 1 2 d S . . HN2 H 0.2156 0.0000 0.2810 0.032 Uiso 1 2 calc SR . . N3 N 0.12125(19) 0.1151(4) 0.0895(3) 0.0263(11) Uani 1 1 d . . . C1 C 0.0079(3) 0.1646(5) 0.2389(5) 0.0449(16) Uani 1 1 d . . . H1 H -0.0291 0.1372 0.1701 0.054 Uiso 1 1 calc R . . C2 C -0.0035(3) 0.2493(6) 0.3084(6) 0.061(2) Uani 1 1 d . . . H2 H -0.0477 0.2795 0.2886 0.073 Uiso 1 1 calc R . . C3 C 0.0505(3) 0.2895(5) 0.4075(6) 0.0566(19) Uani 1 1 d . . . H3 H 0.0439 0.3499 0.4552 0.068 Uiso 1 1 calc R . . C4 C 0.1131(3) 0.2430(5) 0.4370(5) 0.0397(15) Uani 1 1 d . . . H4 H 0.1501 0.2682 0.5067 0.048 Uiso 1 1 calc R . . C5 C 0.1222(3) 0.1580(4) 0.3638(5) 0.0290(13) Uani 1 1 d . . . C6 C 0.1905(2) 0.1111(4) 0.3799(5) 0.0347(14) Uani 1 1 d . . . H6'' H 0.2143 0.1707 0.3524 0.042 Uiso 1 1 calc R . . H6' H 0.2181 0.0960 0.4652 0.042 Uiso 1 1 calc R . . C7 C 0.1174(2) 0.2325(4) 0.0868(5) 0.0324(14) Uani 1 1 d . . . H7 H 0.0993 0.2711 0.1355 0.039 Uiso 1 1 calc R . . C8 C 0.1390(3) 0.3008(5) 0.0156(5) 0.0413(16) Uani 1 1 d . . . H8 H 0.1352 0.3844 0.0163 0.050 Uiso 1 1 calc R . . C9 C 0.1656(3) 0.2487(5) -0.0557(5) 0.0388(15) Uani 1 1 d . . . H9 H 0.1807 0.2956 -0.1039 0.047 Uiso 1 1 calc R . . C10 C 0.1703(2) 0.1259(5) -0.0565(5) 0.0310(14) Uani 1 1 d . . . C11 C 0.1476(2) 0.0625(4) 0.0171(4) 0.0237(12) Uani 1 1 d . . . C12 C 0.1943(2) 0.0590(5) -0.1315(5) 0.0418(16) Uani 1 1 d . . . H12 H 0.2104 0.0999 -0.1819 0.050 Uiso 1 1 calc R . . Cl1 Cl 0.15331(11) 0.5000 -0.27878(18) 0.0354(5) Uani 1 2 d S . . O4 O 0.1445(3) 0.5000 -0.1703(5) 0.0654(19) Uani 1 2 d S . . O3 O 0.1906(2) 0.6030(3) -0.2837(3) 0.0547(12) Uani 1 1 d . . . O2 O 0.0889(3) 0.5000 -0.3754(6) 0.071(2) Uani 1 2 d S . . Cl2 Cl 0.17955(10) 0.5000 -0.69253(18) 0.0402(6) Uani 1 2 d S . . O8 O 0.1655(3) 0.5000 -0.5885(5) 0.0515(16) Uani 1 2 d S . . O7 O 0.2182(2) 0.3955(3) -0.6915(3) 0.0565(12) Uani 1 1 d . . . O6 O 0.1176(3) 0.5000 -0.7970(5) 0.071(2) Uani 1 2 d S . . 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 0.0242(6) 0.0227(6) 0.0197(6) 0.000 0.0060(5) 0.000 O1 0.031(3) 0.048(3) 0.011(3) 0.000 0.010(3) 0.000 N1 0.023(3) 0.037(3) 0.021(3) -0.002(2) 0.005(2) 0.003(2) N2 0.025(4) 0.028(3) 0.029(4) 0.000 0.012(3) 0.000 N3 0.022(3) 0.031(3) 0.016(3) -0.002(2) -0.001(2) -0.0014(19) C1 0.028(4) 0.055(4) 0.043(4) -0.013(3) 0.007(3) 0.001(3) C2 0.044(4) 0.069(4) 0.063(5) -0.033(4) 0.015(4) 0.012(3) C3 0.049(5) 0.069(5) 0.057(5) -0.037(4) 0.026(4) -0.007(4) C4 0.039(4) 0.048(4) 0.032(4) -0.011(3) 0.014(3) -0.006(3) C5 0.033(3) 0.024(3) 0.023(3) 0.003(3) 0.005(3) -0.002(2) C6 0.031(3) 0.035(3) 0.027(3) -0.005(3) 0.000(3) -0.002(3) C7 0.039(4) 0.019(3) 0.032(4) -0.003(3) 0.007(3) -0.002(2) C8 0.053(4) 0.025(3) 0.038(4) 0.005(3) 0.010(3) -0.005(3) C9 0.032(4) 0.041(4) 0.033(4) 0.010(3) 0.003(3) -0.009(3) C10 0.014(3) 0.044(4) 0.029(3) 0.004(3) 0.003(3) -0.005(3) C11 0.017(3) 0.031(3) 0.016(3) 0.001(2) 0.000(2) -0.002(2) C12 0.028(3) 0.067(4) 0.032(3) 0.005(3) 0.014(3) -0.004(3) Cl1 0.0496(14) 0.0282(11) 0.0313(13) 0.000 0.0194(11) 0.000 O4 0.127(6) 0.045(4) 0.054(4) 0.000 0.068(4) 0.000 O3 0.080(3) 0.039(2) 0.056(3) -0.003(2) 0.039(3) -0.018(2) O2 0.049(4) 0.078(5) 0.069(5) 0.000 0.008(4) 0.000 Cl2 0.0474(14) 0.0345(12) 0.0317(14) 0.000 0.0091(12) 0.000 O8 0.067(4) 0.048(3) 0.053(4) 0.000 0.038(4) 0.000 O7 0.084(3) 0.040(2) 0.050(3) -0.002(2) 0.032(3) 0.016(2) O6 0.060(4) 0.067(4) 0.042(4) 0.000 -0.023(3) 0.000 _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 1.883(5) . ? Co N1 1.925(4) 6 ? Co N1 1.925(4) . ? Co N3 1.943(4) 6 ? Co N3 1.943(4) . ? Co N2 2.004(6) . ? O1 O1 1.436(8) 5 ? N1 C5 1.345(6) . ? N1 C1 1.357(6) . ? N2 C6 1.484(5) . ? N2 C6 1.484(5) 6 ? N3 C7 1.332(6) . ? N3 C11 1.377(6) . ? C1 C2 1.375(7) . ? C2 C3 1.380(8) . ? C3 C4 1.357(7) . ? C4 C5 1.388(7) . ? C5 C6 1.506(7) . ? C7 C8 1.387(7) . ? C8 C9 1.367(7) . ? C9 C10 1.394(7) . ? C10 C11 1.397(7) . ? C10 C12 1.448(7) . ? C11 C11 1.414(9) 6 ? C12 C12 1.335(11) 6 ? Cl1 O2 1.417(6) . ? Cl1 O4 1.429(5) . ? Cl1 O3 1.433(4) . ? Cl1 O3 1.433(4) 6_565 ? Cl2 O6 1.431(6) . ? Cl2 O8 1.436(5) . ? Cl2 O7 1.445(4) 6_565 ? Cl2 O7 1.445(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 O1 Co N1 91.23(16) . 6 ? O1 Co N1 91.23(16) . . ? N1 Co N1 88.9(2) 6 . ? O1 Co N3 93.04(15) . 6 ? N1 Co N3 93.31(17) 6 6 ? N1 Co N3 175.17(18) . 6 ? O1 Co N3 93.04(15) . . ? N1 Co N3 175.17(18) 6 . ? N1 Co N3 93.31(17) . . ? N3 Co N3 84.2(3) 6 . ? O1 Co N2 173.6(2) . . ? N1 Co N2 84.20(18) 6 . ? N1 Co N2 84.20(18) . . ? N3 Co N2 91.72(17) 6 . ? N3 Co N2 91.72(17) . . ? O1 O1 Co 113.0(4) 5 . ? C5 N1 C1 118.4(5) . . ? C5 N1 Co 116.3(3) . . ? C1 N1 Co 125.3(4) . . ? C6 N2 C6 115.8(6) . 6 ? C6 N2 Co 108.6(3) . . ? C6 N2 Co 108.6(3) 6 . ? C7 N3 C11 117.0(4) . . ? C7 N3 Co 130.7(4) . . ? C11 N3 Co 112.3(3) . . ? N1 C1 C2 121.9(5) . . ? C1 C2 C3 118.7(6) . . ? C4 C3 C2 120.0(6) . . ? C3 C4 C5 119.2(5) . . ? N1 C5 C4 121.7(5) . . ? N1 C5 C6 114.5(4) . . ? C4 C5 C6 123.5(5) . . ? N2 C6 C5 110.5(4) . . ? N3 C7 C8 122.6(5) . . ? C9 C8 C7 120.5(5) . . ? C8 C9 C10 119.1(5) . . ? C9 C10 C11 117.5(5) . . ? C9 C10 C12 125.0(5) . . ? C11 C10 C12 117.5(5) . . ? N3 C11 C10 123.3(4) . . ? N3 C11 C11 115.6(3) . 6 ? C10 C11 C11 121.0(3) . 6 ? C12 C12 C10 121.6(3) 6 . ? O2 Cl1 O4 109.1(4) . . ? O2 Cl1 O3 109.9(2) . . ? O4 Cl1 O3 109.5(2) . . ? O2 Cl1 O3 109.9(2) . 6_565 ? O4 Cl1 O3 109.5(2) . 6_565 ? O3 Cl1 O3 108.9(3) . 6_565 ? O6 Cl2 O8 110.1(4) . . ? O6 Cl2 O7 109.4(2) . 6_565 ? O8 Cl2 O7 109.0(2) . 6_565 ? O6 Cl2 O7 109.4(2) . . ? O8 Cl2 O7 109.0(2) . . ? O7 Cl2 O7 109.8(3) 6_565 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.588 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.081