Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof. Claudio N. Verani' _publ_contact_author_address ; Department of Chemistry Wayne State University Detroit, Michigan 48202 ; _publ_contact_author_email cnverani@chem.wayne.edu _publ_section_title ; Structural, SPectroscopic, and Electrochemical Behavior of Trans-Phenolato Cobalt(III) Complexes of Asymmetric NN'O Ligands as Archetypes for Metallomesogens. ; loop_ _publ_author_name _publ_author_address 'Rajendra Shakya' ; Wayne State University Detroit, Michigan 48202, USA ; 'Camille Imbert' ; Wayne State University Detroit, Michigan 48202, USA ; 'Hrant P. Hratchian' ; Wayne State University Detroit, Michigan 48202, USA ; 'Mauricio Lanznaster' ; Wayne State University Detroit, Michigan 48202, USA ; 'Mary Jane Heeg' ; Wayne State University Detroit, Michigan 48202, USA ; ; B.R.McGarvey ; ; University of Windsor Windsor ON N9B 1P4, Canada ; 'Marco Allard' ; Wayne State University Detroit, Michigan 48202, USA ; 'H. Bernhard Schlegel' ; Wayne State University Detroit, Michigan 48202, USA ; 'Claudio N. Verani' ; Wayne State University Detroit, Michigan 48202, USA ; #=== data_coca _database_code_depnum_ccdc_archive 'CCDC 285941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 Cl Co N4 O6' _chemical_formula_weight 584.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.2884(15) _cell_length_b 8.4867(7) _cell_length_c 15.4068(12) _cell_angle_alpha 90.00 _cell_angle_beta 109.344(2) _cell_angle_gamma 90.00 _cell_volume 2503.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 943 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 28.5 _exptl_crystal_description irregular _exptl_crystal_colour dark _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6316 _exptl_absorpt_correction_T_max 0.7291 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4/CCD' _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8898 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.31 _reflns_number_total 2953 _reflns_number_gt 2302 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\\s^2^(Fo^2^)+(0.0364P)^2^+1.9475P] 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 SHELXL _refine_ls_extinction_coef 0.00027(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\\l^3^/sin(2\\q)]^-1/4^ _refine_ls_number_reflns 2953 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.2500 0.0000 0.03424(12) Uani 1 2 d S . . N1 N 0.17899(7) 0.41209(18) -0.01183(10) 0.0386(3) Uani 1 1 d . . . C1 C 0.11036(10) 0.4020(3) -0.05939(14) 0.0455(4) Uani 1 1 d . . . C2 C 0.06415(11) 0.5208(3) -0.05891(16) 0.0561(6) Uani 1 1 d . . . C3 C 0.08832(13) 0.6522(3) -0.00735(18) 0.0646(7) Uani 1 1 d . . . C4 C 0.15827(13) 0.6630(3) 0.04326(17) 0.0567(6) Uani 1 1 d . . . C5 C 0.20242(10) 0.5407(2) 0.03991(13) 0.0422(4) Uani 1 1 d . . . C6 C 0.27844(11) 0.5373(2) 0.09401(16) 0.0462(5) Uani 1 1 d . . . N2 N 0.30137(8) 0.37143(19) 0.11002(11) 0.0395(4) Uani 1 1 d . . . C7 C 0.29536(10) 0.3077(3) 0.19754(14) 0.0446(4) Uani 1 1 d . . . C8 C 0.22098(10) 0.2861(2) 0.19171(13) 0.0415(4) Uani 1 1 d . . . C9 C 0.19221(12) 0.3620(3) 0.25048(15) 0.0513(5) Uani 1 1 d . . . C10 C 0.12399(13) 0.3327(3) 0.24549(17) 0.0602(6) Uani 1 1 d . . . C11 C 0.08480(12) 0.2253(3) 0.18302(17) 0.0576(6) Uani 1 1 d . . . C12 C 0.11158(10) 0.1508(3) 0.12214(16) 0.0492(5) Uani 1 1 d . . . C13 C 0.17992(9) 0.1825(2) 0.12436(13) 0.0396(4) Uani 1 1 d . . . O1 O 0.20575(6) 0.11523(15) 0.06393(9) 0.0417(3) Uani 1 1 d . . . Cl2 Cl 0.5000 0.35298(12) 0.2500 0.0843(3) Uani 1 2 d S . . O2 O 0.45368(8) 0.4495(2) 0.18027(15) 0.0892(6) Uani 1 1 d . . . O3 O 0.54059(12) 0.2570(3) 0.2124(2) 0.1445(12) Uani 1 1 d . . . H1N2 H 0.3414(12) 0.372(3) 0.1156(15) 0.053(6) Uiso 1 1 d . . . H1 H 0.0949(10) 0.315(3) -0.0938(14) 0.044(6) Uiso 1 1 d . . . H2 H 0.0188(12) 0.506(3) -0.0965(15) 0.058(6) Uiso 1 1 d . . . H3 H 0.0593(15) 0.733(3) -0.0063(19) 0.084(9) Uiso 1 1 d . . . H4 H 0.1760(13) 0.743(3) 0.0757(17) 0.063(7) Uiso 1 1 d . . . H6A H 0.2864(11) 0.589(3) 0.1504(15) 0.049(6) Uiso 1 1 d . . . H6B H 0.3024(11) 0.589(3) 0.0609(15) 0.056(6) Uiso 1 1 d . . . H7A H 0.3178(11) 0.378(3) 0.2467(14) 0.050(6) Uiso 1 1 d . . . H7B H 0.3210(10) 0.208(2) 0.2076(14) 0.041(5) Uiso 1 1 d . . . H9 H 0.2198(12) 0.427(3) 0.2945(16) 0.058(7) Uiso 1 1 d . . . H10 H 0.1077(13) 0.385(3) 0.2849(17) 0.070(7) Uiso 1 1 d . . . H11 H 0.0387(14) 0.200(3) 0.1789(17) 0.071(7) Uiso 1 1 d . . . H12 H 0.0866(11) 0.085(3) 0.0793(15) 0.050(6) Uiso 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 0.02750(16) 0.03368(18) 0.0414(2) -0.00286(15) 0.01115(13) -0.00173(13) N1 0.0349(7) 0.0388(8) 0.0444(8) 0.0020(7) 0.0161(6) 0.0011(6) C1 0.0363(9) 0.0504(12) 0.0499(11) 0.0022(10) 0.0145(8) 0.0038(9) C2 0.0422(11) 0.0678(15) 0.0596(13) 0.0118(11) 0.0188(10) 0.0150(10) C3 0.0656(15) 0.0629(16) 0.0692(15) 0.0049(12) 0.0278(12) 0.0278(13) C4 0.0702(15) 0.0439(12) 0.0566(13) -0.0031(10) 0.0219(11) 0.0114(11) C5 0.0482(10) 0.0368(10) 0.0449(10) 0.0020(8) 0.0198(8) 0.0013(8) C6 0.0494(11) 0.0364(10) 0.0531(12) -0.0069(9) 0.0174(9) -0.0075(8) N2 0.0303(7) 0.0396(8) 0.0479(9) -0.0042(7) 0.0120(6) -0.0038(6) C7 0.0390(10) 0.0464(11) 0.0425(10) -0.0022(9) 0.0057(8) -0.0022(9) C8 0.0422(9) 0.0413(10) 0.0408(10) 0.0056(7) 0.0133(8) 0.0019(7) C9 0.0642(13) 0.0456(11) 0.0455(11) 0.0042(9) 0.0198(10) 0.0059(10) C10 0.0705(15) 0.0625(15) 0.0592(14) 0.0109(12) 0.0372(12) 0.0189(12) C11 0.0462(11) 0.0693(16) 0.0650(14) 0.0190(12) 0.0290(11) 0.0116(11) C12 0.0389(10) 0.0541(13) 0.0547(12) 0.0068(10) 0.0157(9) -0.0006(9) C13 0.0368(9) 0.0392(9) 0.0441(10) 0.0068(8) 0.0151(8) 0.0027(8) O1 0.0395(6) 0.0385(7) 0.0497(7) -0.0036(6) 0.0183(6) -0.0058(5) Cl2 0.0337(4) 0.0676(6) 0.1257(8) 0.000 -0.0084(4) 0.000 O2 0.0460(9) 0.0816(13) 0.1113(15) 0.0061(11) -0.0127(9) 0.0011(9) O3 0.0650(13) 0.134(2) 0.201(3) -0.065(2) -0.0014(16) 0.0309(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.9158(12) 7 ? Co1 O1 1.9158(12) . ? Co1 N1 1.9563(15) 7 ? Co1 N1 1.9563(15) . ? Co1 N2 1.9624(15) . ? Co1 N2 1.9624(15) 7 ? N1 C5 1.342(2) . ? N1 C1 1.344(2) . ? C1 C2 1.379(3) . ? C2 C3 1.362(4) . ? C3 C4 1.377(4) . ? C4 C5 1.383(3) . ? C5 C6 1.491(3) . ? C6 N2 1.477(3) . ? N2 C7 1.495(3) . ? C7 C8 1.493(3) . ? C8 C9 1.387(3) . ? C8 C13 1.404(3) . ? C9 C10 1.383(3) . ? C10 C11 1.372(4) . ? C11 C12 1.383(3) . ? C12 C13 1.402(3) . ? C13 O1 1.338(2) . ? Cl2 O3 1.412(3) . ? Cl2 O3 1.412(3) 2_655 ? Cl2 O2 1.4281(18) 2_655 ? Cl2 O2 1.4281(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 180.00(9) 7 . ? O1 Co1 N1 90.66(6) 7 7 ? O1 Co1 N1 89.34(6) . 7 ? O1 Co1 N1 89.34(6) 7 . ? O1 Co1 N1 90.66(6) . . ? N1 Co1 N1 180.00(11) 7 . ? O1 Co1 N2 85.72(6) 7 . ? O1 Co1 N2 94.28(6) . . ? N1 Co1 N2 97.16(7) 7 . ? N1 Co1 N2 82.84(7) . . ? O1 Co1 N2 94.28(6) 7 7 ? O1 Co1 N2 85.72(6) . 7 ? N1 Co1 N2 82.84(7) 7 7 ? N1 Co1 N2 97.16(7) . 7 ? N2 Co1 N2 180.00(13) . 7 ? C5 N1 C1 118.35(17) . . ? C5 N1 Co1 114.29(12) . . ? C1 N1 Co1 127.14(14) . . ? N1 C1 C2 122.3(2) . . ? C3 C2 C1 119.2(2) . . ? C2 C3 C4 119.3(2) . . ? C3 C4 C5 119.2(2) . . ? N1 C5 C4 121.73(19) . . ? N1 C5 C6 114.42(16) . . ? C4 C5 C6 123.83(19) . . ? N2 C6 C5 108.80(15) . . ? C6 N2 C7 112.33(17) . . ? C6 N2 Co1 107.96(12) . . ? C7 N2 Co1 114.24(12) . . ? C8 C7 N2 111.90(15) . . ? C9 C8 C13 119.87(19) . . ? C9 C8 C7 122.62(19) . . ? C13 C8 C7 117.50(17) . . ? C10 C9 C8 120.7(2) . . ? C11 C10 C9 119.7(2) . . ? C10 C11 C12 120.9(2) . . ? C11 C12 C13 120.2(2) . . ? O1 C13 C12 120.88(18) . . ? O1 C13 C8 120.54(16) . . ? C12 C13 C8 118.57(19) . . ? C13 O1 Co1 117.47(11) . . ? O3 Cl2 O3 109.5(3) . 2_655 ? O3 Cl2 O2 108.15(13) . 2_655 ? O3 Cl2 O2 110.50(17) 2_655 2_655 ? O3 Cl2 O2 110.50(17) . . ? O3 Cl2 O2 108.15(13) 2_655 . ? O2 Cl2 O2 109.99(17) 2_655 . ? 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 Co1 N1 C5 -70.15(13) 7 . . . ? O1 Co1 N1 C5 109.85(13) . . . . ? N1 Co1 N1 C5 160(13) 7 . . . ? N2 Co1 N1 C5 15.62(13) . . . . ? N2 Co1 N1 C5 -164.38(13) 7 . . . ? O1 Co1 N1 C1 115.41(16) 7 . . . ? O1 Co1 N1 C1 -64.59(16) . . . . ? N1 Co1 N1 C1 -14(13) 7 . . . ? N2 Co1 N1 C1 -158.83(17) . . . . ? N2 Co1 N1 C1 21.17(17) 7 . . . ? C5 N1 C1 C2 2.1(3) . . . . ? Co1 N1 C1 C2 176.33(15) . . . . ? N1 C1 C2 C3 -1.2(3) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C1 N1 C5 C4 -1.7(3) . . . . ? Co1 N1 C5 C4 -176.67(16) . . . . ? C1 N1 C5 C6 176.82(18) . . . . ? Co1 N1 C5 C6 1.8(2) . . . . ? C3 C4 C5 N1 0.4(3) . . . . ? C3 C4 C5 C6 -178.0(2) . . . . ? N1 C5 C6 N2 -25.4(2) . . . . ? C4 C5 C6 N2 153.1(2) . . . . ? C5 C6 N2 C7 -90.69(19) . . . . ? C5 C6 N2 Co1 36.2(2) . . . . ? O1 Co1 N2 C6 61.25(13) 7 . . . ? O1 Co1 N2 C6 -118.75(13) . . . . ? N1 Co1 N2 C6 151.38(13) 7 . . . ? N1 Co1 N2 C6 -28.62(13) . . . . ? N2 Co1 N2 C6 -69(68) 7 . . . ? O1 Co1 N2 C7 -173.03(14) 7 . . . ? O1 Co1 N2 C7 6.97(14) . . . . ? N1 Co1 N2 C7 -82.90(14) 7 . . . ? N1 Co1 N2 C7 97.10(14) . . . . ? N2 Co1 N2 C7 57(68) 7 . . . ? C6 N2 C7 C8 70.2(2) . . . . ? Co1 N2 C7 C8 -53.2(2) . . . . ? N2 C7 C8 C9 -120.6(2) . . . . ? N2 C7 C8 C13 60.4(2) . . . . ? C13 C8 C9 C10 2.1(3) . . . . ? C7 C8 C9 C10 -176.9(2) . . . . ? C8 C9 C10 C11 1.3(3) . . . . ? C9 C10 C11 C12 -2.8(3) . . . . ? C10 C11 C12 C13 0.9(3) . . . . ? C11 C12 C13 O1 -177.77(18) . . . . ? C11 C12 C13 C8 2.5(3) . . . . ? C9 C8 C13 O1 176.28(17) . . . . ? C7 C8 C13 O1 -4.7(3) . . . . ? C9 C8 C13 C12 -3.9(3) . . . . ? C7 C8 C13 C12 175.11(18) . . . . ? C12 C13 O1 Co1 130.40(16) . . . . ? C8 C13 O1 Co1 -49.8(2) . . . . ? O1 Co1 O1 C13 -50(100) 7 . . . ? N1 Co1 O1 C13 140.70(12) 7 . . . ? N1 Co1 O1 C13 -39.30(12) . . . . ? N2 Co1 O1 C13 43.56(13) . . . . ? N2 Co1 O1 C13 -136.44(13) 7 . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.247 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.043 #=== data_omec _database_code_depnum_ccdc_archive 'CCDC 285942' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 Cl Co N4 O9' _chemical_formula_weight 662.96 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8170(8) _cell_length_b 14.8833(9) _cell_length_c 17.2517(12) _cell_angle_alpha 90.00 _cell_angle_beta 108.448(3) _cell_angle_gamma 90.00 _cell_volume 2878.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8817 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26.9 _exptl_crystal_description rod _exptl_crystal_colour dark _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8957 _exptl_absorpt_correction_T_max 0.9851 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 kappa' _diffrn_measurement_method 'Bruker APEX2' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79107 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.33 _reflns_number_total 7147 _reflns_number_gt 4779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\\s^2^(Fo^2^)+(0.0388P)^2^+1.8481P] 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 7147 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.5000 0.5000 0.01039(10) Uani 1 2 d S . . N1 N -0.12680(15) 0.41175(12) 0.45949(11) 0.0122(4) Uani 1 1 d . . . N2 N -0.00364(17) 0.50741(13) 0.38586(11) 0.0127(4) Uani 1 1 d . . . O1 O -0.11745(13) 0.59235(10) 0.48933(9) 0.0134(3) Uani 1 1 d . . . C1 C -0.19736(19) 0.37675(15) 0.49964(14) 0.0150(5) Uani 1 1 d . . . C2 C -0.2844(2) 0.31384(17) 0.46481(16) 0.0200(5) Uani 1 1 d . . . C3 C -0.3028(2) 0.28711(17) 0.38521(15) 0.0203(5) Uani 1 1 d . . . C4 C -0.2316(2) 0.32390(16) 0.34308(15) 0.0186(5) Uani 1 1 d . . . C5 C -0.1438(2) 0.38522(14) 0.38177(13) 0.0139(5) Uani 1 1 d . . . C6 C -0.0608(2) 0.42530(16) 0.34160(14) 0.0147(5) Uani 1 1 d . . . C7 C -0.0603(2) 0.59113(16) 0.34340(15) 0.0159(5) Uani 1 1 d . . . C8 C -0.1871(2) 0.59793(15) 0.34307(14) 0.0147(5) Uani 1 1 d . . . C9 C -0.2820(2) 0.60333(15) 0.27023(15) 0.0186(5) Uani 1 1 d . . . C10 C -0.3973(2) 0.61009(16) 0.27218(15) 0.0217(5) Uani 1 1 d . . . C11 C -0.4201(2) 0.61141(16) 0.34597(16) 0.0203(5) Uani 1 1 d . . . C12 C -0.3270(2) 0.60540(15) 0.41898(14) 0.0162(5) Uani 1 1 d . . . C13 C -0.20781(19) 0.59814(14) 0.41851(14) 0.0135(5) Uani 1 1 d . . . O2 O -0.34168(14) 0.60751(12) 0.49517(10) 0.0221(4) Uani 1 1 d . . . C14 C -0.4582(3) 0.6312(2) 0.4979(2) 0.0315(7) Uani 1 1 d . . . Co2 Co 0.0000 0.0000 0.5000 0.00899(9) Uani 1 2 d S . . N3 N 0.08443(15) 0.06450(12) 0.43695(10) 0.0110(4) Uani 1 1 d . . . N4 N 0.00331(16) 0.11573(12) 0.55381(11) 0.0116(4) Uani 1 1 d . . . O3 O 0.14948(12) -0.03984(10) 0.57353(9) 0.0122(3) Uani 1 1 d . . . C15 C 0.14840(19) 0.02959(16) 0.39173(14) 0.0145(5) Uani 1 1 d . . . C16 C 0.2121(2) 0.08282(17) 0.35468(15) 0.0182(5) Uani 1 1 d . . . C17 C 0.2148(2) 0.17495(17) 0.36655(15) 0.0190(5) Uani 1 1 d . . . C18 C 0.1513(2) 0.21147(17) 0.41379(14) 0.0163(5) Uani 1 1 d . . . C19 C 0.08553(19) 0.15487(15) 0.44681(13) 0.0133(5) Uani 1 1 d . . . C20 C 0.0096(2) 0.18745(15) 0.49554(15) 0.0138(4) Uani 1 1 d . . . C21 C 0.10006(19) 0.12391(16) 0.63409(14) 0.0131(5) Uani 1 1 d . . . C22 C 0.22101(18) 0.10496(15) 0.62597(13) 0.0124(4) Uani 1 1 d . . . C23 C 0.31260(19) 0.16873(16) 0.64614(13) 0.0137(5) Uani 1 1 d . . . C24 C 0.4252(2) 0.14612(16) 0.64415(14) 0.0158(5) Uani 1 1 d . . . C25 C 0.4463(2) 0.05977(16) 0.62055(14) 0.0157(5) Uani 1 1 d . . . C26 C 0.35450(19) -0.00251(15) 0.59569(13) 0.0142(4) Uani 1 1 d . . . C27 C 0.23846(19) 0.01959(14) 0.59761(13) 0.0123(5) Uani 1 1 d . . . O4 O 0.36509(14) -0.08732(10) 0.56719(10) 0.0200(4) Uani 1 1 d . . . C28 C 0.4833(2) -0.11470(19) 0.5727(2) 0.0252(6) Uani 1 1 d . . . Cl3 Cl -0.20043(5) 0.21420(4) 0.69414(4) 0.02470(14) Uani 1 1 d . . . O5 O -0.14951(17) 0.20421(13) 0.62885(12) 0.0323(5) Uani 1 1 d . . . O6 O -0.10983(19) 0.24154(18) 0.76683(14) 0.0601(8) Uani 1 1 d . . . O7 O -0.29428(18) 0.27879(15) 0.67118(13) 0.0438(6) Uani 1 1 d . . . O8 O -0.2480(2) 0.12835(15) 0.70855(14) 0.0494(6) Uani 1 1 d . . . O9 O 0.21436(19) 0.46600(16) 0.35245(15) 0.0367(5) Uani 1 1 d . . . H1N2 H 0.067(2) 0.5070(16) 0.3871(15) 0.014(6) Uiso 1 1 d . . . H1 H -0.189(2) 0.3978(16) 0.5541(16) 0.017(6) Uiso 1 1 d . . . H2 H -0.328(2) 0.2905(18) 0.4977(16) 0.023(7) Uiso 1 1 d . . . H3 H -0.360(2) 0.2434(17) 0.3587(16) 0.023(7) Uiso 1 1 d . . . H4 H -0.241(2) 0.3087(17) 0.2891(16) 0.020(7) Uiso 1 1 d . . . H6A H 0.002(2) 0.3830(16) 0.3451(14) 0.014(6) Uiso 1 1 d . . . H6B H -0.100(2) 0.4390(16) 0.2858(15) 0.015(6) Uiso 1 1 d . . . H7A H -0.055(2) 0.5919(16) 0.2897(16) 0.019(7) Uiso 1 1 d . . . H7B H -0.012(2) 0.6397(16) 0.3748(14) 0.013(6) Uiso 1 1 d . . . H9 H -0.264(2) 0.6020(17) 0.2226(16) 0.018(7) Uiso 1 1 d . . . H10 H -0.460(2) 0.6129(17) 0.2226(16) 0.024(7) Uiso 1 1 d . . . H11 H -0.497(2) 0.6165(17) 0.3476(15) 0.020(7) Uiso 1 1 d . . . H14A H -0.513(3) 0.582(2) 0.4715(18) 0.034(8) Uiso 1 1 d . . . H14B H -0.481(3) 0.689(2) 0.4693(18) 0.037(8) Uiso 1 1 d . . . H14C H -0.453(3) 0.6327(19) 0.5547(19) 0.034(8) Uiso 1 1 d . . . H1N4 H -0.061(2) 0.1220(16) 0.5633(15) 0.016(7) Uiso 1 1 d . . . H15 H 0.149(2) -0.0348(19) 0.3861(16) 0.028(7) Uiso 1 1 d . . . H16 H 0.249(2) 0.0603(16) 0.3219(15) 0.013(6) Uiso 1 1 d . . . H17 H 0.260(2) 0.2158(18) 0.3429(16) 0.027(7) Uiso 1 1 d . . . H18 H 0.151(2) 0.2713(18) 0.4256(16) 0.021(7) Uiso 1 1 d . . . H20A H 0.040(2) 0.2423(16) 0.5234(14) 0.009(6) Uiso 1 1 d . . . H20B H -0.071(2) 0.1979(16) 0.4590(15) 0.015(6) Uiso 1 1 d . . . H21A H 0.0838(19) 0.0794(15) 0.6730(14) 0.008(6) Uiso 1 1 d . . . H21B H 0.099(2) 0.1832(17) 0.6568(14) 0.014(6) Uiso 1 1 d . . . H23 H 0.295(2) 0.2247(17) 0.6636(15) 0.015(6) Uiso 1 1 d . . . H24 H 0.486(2) 0.1898(18) 0.6592(16) 0.025(7) Uiso 1 1 d . . . H25 H 0.522(2) 0.0434(17) 0.6192(15) 0.023(7) Uiso 1 1 d . . . H28A H 0.523(2) -0.0749(18) 0.5422(16) 0.026(7) Uiso 1 1 d . . . H28B H 0.474(2) -0.173(2) 0.5496(17) 0.036(8) Uiso 1 1 d . . . H28C H 0.536(3) -0.1124(18) 0.6313(18) 0.031(8) Uiso 1 1 d . . . H109 H 0.224(3) 0.438(3) 0.315(2) 0.057(12) Uiso 1 1 d . . . H110 H 0.251(3) 0.437(3) 0.400(3) 0.071(13) Uiso 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 0.00845(19) 0.0114(2) 0.0108(2) -0.00160(17) 0.00235(15) 0.00064(17) N1 0.0100(9) 0.0120(9) 0.0134(9) -0.0005(7) 0.0020(7) 0.0022(7) N2 0.0105(9) 0.0130(10) 0.0144(9) -0.0023(8) 0.0035(7) 0.0008(8) O1 0.0112(7) 0.0148(8) 0.0124(8) -0.0017(6) 0.0015(6) 0.0029(6) C1 0.0126(11) 0.0166(12) 0.0166(12) -0.0021(9) 0.0056(9) 0.0004(9) C2 0.0113(11) 0.0232(13) 0.0255(13) 0.0032(10) 0.0058(10) -0.0012(9) C3 0.0149(11) 0.0177(12) 0.0234(13) 0.0004(10) -0.0009(10) -0.0041(10) C4 0.0207(12) 0.0158(12) 0.0145(12) -0.0016(9) -0.0011(10) -0.0022(9) C5 0.0150(11) 0.0108(11) 0.0141(11) 0.0005(8) 0.0019(9) 0.0028(9) C6 0.0169(11) 0.0165(12) 0.0101(11) -0.0017(9) 0.0037(9) 0.0008(9) C7 0.0202(12) 0.0131(12) 0.0138(12) -0.0001(9) 0.0046(10) 0.0003(9) C8 0.0154(11) 0.0097(11) 0.0177(12) -0.0009(9) 0.0033(9) 0.0007(8) C9 0.0242(13) 0.0124(12) 0.0172(12) -0.0020(9) 0.0037(10) 0.0038(9) C10 0.0189(12) 0.0181(13) 0.0192(13) -0.0038(10) -0.0066(10) 0.0013(10) C11 0.0105(11) 0.0165(12) 0.0302(14) -0.0030(10) 0.0011(10) -0.0005(9) C12 0.0141(11) 0.0132(12) 0.0205(12) -0.0013(9) 0.0044(9) 0.0000(9) C13 0.0124(10) 0.0101(11) 0.0160(11) 0.0004(9) 0.0017(9) 0.0012(8) O2 0.0130(8) 0.0295(10) 0.0263(9) 0.0032(8) 0.0097(7) 0.0060(7) C14 0.0195(13) 0.0384(18) 0.0415(18) 0.0084(15) 0.0166(13) 0.0094(13) Co2 0.00673(18) 0.0099(2) 0.0103(2) 0.00002(17) 0.00267(15) 0.00070(16) N3 0.0075(8) 0.0131(9) 0.0114(9) 0.0005(7) 0.0014(7) -0.0001(7) N4 0.0084(9) 0.0118(10) 0.0153(9) 0.0001(7) 0.0047(8) 0.0011(7) O3 0.0079(7) 0.0120(8) 0.0146(8) 0.0009(6) 0.0008(6) 0.0004(6) C15 0.0120(11) 0.0161(12) 0.0138(11) -0.0012(9) 0.0020(9) 0.0012(9) C16 0.0124(11) 0.0266(14) 0.0182(12) -0.0020(10) 0.0083(10) 0.0001(10) C17 0.0128(11) 0.0253(14) 0.0186(12) 0.0043(10) 0.0045(9) -0.0034(10) C18 0.0169(11) 0.0151(12) 0.0161(12) 0.0021(10) 0.0040(9) -0.0028(9) C19 0.0097(10) 0.0176(12) 0.0101(10) -0.0008(9) -0.0007(8) -0.0002(8) C20 0.0139(11) 0.0093(10) 0.0177(11) 0.0004(9) 0.0045(9) 0.0003(9) C21 0.0109(10) 0.0154(12) 0.0121(11) -0.0021(9) 0.0022(9) 0.0008(8) C22 0.0080(10) 0.0170(12) 0.0107(10) 0.0026(8) 0.0011(8) 0.0011(8) C23 0.0139(11) 0.0142(12) 0.0122(11) 0.0010(9) 0.0028(9) 0.0001(9) C24 0.0119(11) 0.0185(12) 0.0152(11) 0.0023(9) 0.0018(9) -0.0045(9) C25 0.0095(10) 0.0188(12) 0.0190(12) 0.0036(9) 0.0047(9) 0.0006(9) C26 0.0135(10) 0.0132(10) 0.0157(10) 0.0012(9) 0.0044(8) 0.0022(9) C27 0.0108(10) 0.0139(12) 0.0108(10) 0.0028(8) 0.0013(8) 0.0001(8) O4 0.0124(8) 0.0145(8) 0.0337(10) -0.0037(7) 0.0082(7) 0.0019(6) C28 0.0168(12) 0.0181(14) 0.0458(18) -0.0018(12) 0.0172(12) 0.0035(10) Cl3 0.0182(3) 0.0339(3) 0.0243(3) -0.0089(3) 0.0098(2) 0.0033(3) O5 0.0401(12) 0.0310(11) 0.0365(11) -0.0031(9) 0.0274(9) 0.0072(9) O6 0.0257(11) 0.101(2) 0.0458(14) -0.0424(14) 0.0009(10) 0.0034(12) O7 0.0355(12) 0.0527(14) 0.0470(13) -0.0016(11) 0.0184(10) 0.0232(10) O8 0.0597(15) 0.0463(14) 0.0543(15) 0.0070(11) 0.0354(12) -0.0045(11) O9 0.0320(12) 0.0505(14) 0.0317(12) 0.0039(11) 0.0158(10) 0.0141(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 O1 1.9204(15) 3_566 ? Co1 O1 1.9204(15) . ? Co1 N1 1.9484(18) . ? Co1 N1 1.9484(18) 3_566 ? Co1 N2 1.9590(18) 3_566 ? Co1 N2 1.9590(18) . ? N1 C1 1.346(3) . ? N1 C5 1.350(3) . ? N2 C6 1.485(3) . ? N2 C7 1.492(3) . ? O1 C13 1.347(2) . ? C1 C2 1.380(3) . ? C2 C3 1.379(4) . ? C3 C4 1.386(4) . ? C4 C5 1.384(3) . ? C5 C6 1.493(3) . ? C7 C8 1.500(3) . ? C8 C9 1.397(3) . ? C8 C13 1.399(3) . ? C9 C10 1.377(4) . ? C10 C11 1.382(4) . ? C11 C12 1.389(3) . ? C12 O2 1.380(3) . ? C12 C13 1.415(3) . ? O2 C14 1.436(3) . ? Co2 O3 1.9138(14) . ? Co2 O3 1.9138(14) 3_556 ? Co2 N3 1.9460(18) 3_556 ? Co2 N3 1.9460(18) . ? Co2 N4 1.9511(18) 3_556 ? Co2 N4 1.9511(18) . ? N3 C15 1.350(3) . ? N3 C19 1.355(3) . ? N4 C20 1.484(3) . ? N4 C21 1.496(3) . ? O3 C27 1.336(3) . ? C15 C16 1.381(3) . ? C16 C17 1.385(4) . ? C17 C18 1.382(3) . ? C18 C19 1.385(3) . ? C19 C20 1.491(3) . ? C21 C22 1.506(3) . ? C22 C23 1.398(3) . ? C22 C27 1.400(3) . ? C23 C24 1.383(3) . ? C24 C25 1.394(3) . ? C25 C26 1.388(3) . ? C26 O4 1.375(3) . ? C26 C27 1.421(3) . ? O4 C28 1.429(3) . ? Cl3 O7 1.426(2) . ? Cl3 O6 1.426(2) . ? Cl3 O5 1.4430(18) . ? Cl3 O8 1.449(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 180.0 3_566 . ? O1 Co1 N1 90.13(7) 3_566 . ? O1 Co1 N1 89.87(7) . . ? O1 Co1 N1 89.87(7) 3_566 3_566 ? O1 Co1 N1 90.13(7) . 3_566 ? N1 Co1 N1 180.00(8) . 3_566 ? O1 Co1 N2 94.48(7) 3_566 3_566 ? O1 Co1 N2 85.52(7) . 3_566 ? N1 Co1 N2 95.30(8) . 3_566 ? N1 Co1 N2 84.70(8) 3_566 3_566 ? O1 Co1 N2 85.52(7) 3_566 . ? O1 Co1 N2 94.48(7) . . ? N1 Co1 N2 84.70(8) . . ? N1 Co1 N2 95.30(8) 3_566 . ? N2 Co1 N2 180.0 3_566 . ? C1 N1 C5 118.42(19) . . ? C1 N1 Co1 127.41(15) . . ? C5 N1 Co1 114.16(15) . . ? C6 N2 C7 111.98(17) . . ? C6 N2 Co1 109.40(14) . . ? C7 N2 Co1 113.83(14) . . ? C13 O1 Co1 118.30(13) . . ? N1 C1 C2 122.4(2) . . ? C3 C2 C1 119.3(2) . . ? C2 C3 C4 118.5(2) . . ? C5 C4 C3 119.6(2) . . ? N1 C5 C4 121.7(2) . . ? N1 C5 C6 115.51(19) . . ? C4 C5 C6 122.8(2) . . ? N2 C6 C5 110.41(18) . . ? N2 C7 C8 110.52(19) . . ? C9 C8 C13 120.6(2) . . ? C9 C8 C7 121.6(2) . . ? C13 C8 C7 117.7(2) . . ? C10 C9 C8 120.1(2) . . ? C9 C10 C11 120.4(2) . . ? C10 C11 C12 120.3(2) . . ? O2 C12 C11 124.1(2) . . ? O2 C12 C13 115.65(19) . . ? C11 C12 C13 120.3(2) . . ? O1 C13 C8 121.5(2) . . ? O1 C13 C12 120.3(2) . . ? C8 C13 C12 118.3(2) . . ? C12 O2 C14 116.6(2) . . ? O3 Co2 O3 180.0 . 3_556 ? O3 Co2 N3 90.32(7) . 3_556 ? O3 Co2 N3 89.68(7) 3_556 3_556 ? O3 Co2 N3 89.68(7) . . ? O3 Co2 N3 90.32(7) 3_556 . ? N3 Co2 N3 180.0 3_556 . ? O3 Co2 N4 85.25(7) . 3_556 ? O3 Co2 N4 94.75(7) 3_556 3_556 ? N3 Co2 N4 83.90(8) 3_556 3_556 ? N3 Co2 N4 96.10(8) . 3_556 ? O3 Co2 N4 94.75(7) . . ? O3 Co2 N4 85.25(7) 3_556 . ? N3 Co2 N4 96.10(8) 3_556 . ? N3 Co2 N4 83.90(8) . . ? N4 Co2 N4 180.0 3_556 . ? C15 N3 C19 118.00(19) . . ? C15 N3 Co2 127.80(16) . . ? C19 N3 Co2 113.94(15) . . ? C20 N4 C21 112.39(18) . . ? C20 N4 Co2 108.08(14) . . ? C21 N4 Co2 114.00(14) . . ? C27 O3 Co2 118.14(13) . . ? N3 C15 C16 122.2(2) . . ? C15 C16 C17 119.3(2) . . ? C18 C17 C16 119.0(2) . . ? C17 C18 C19 118.9(2) . . ? N3 C19 C18 122.4(2) . . ? N3 C19 C20 114.20(19) . . ? C18 C19 C20 123.4(2) . . ? N4 C20 C19 108.42(18) . . ? N4 C21 C22 111.62(18) . . ? C23 C22 C27 121.0(2) . . ? C23 C22 C21 122.2(2) . . ? C27 C22 C21 116.84(19) . . ? C24 C23 C22 120.2(2) . . ? C23 C24 C25 119.6(2) . . ? C26 C25 C24 120.7(2) . . ? O4 C26 C25 125.0(2) . . ? O4 C26 C27 114.75(19) . . ? C25 C26 C27 120.3(2) . . ? O3 C27 C22 121.40(19) . . ? O3 C27 C26 120.67(19) . . ? C22 C27 C26 117.9(2) . . ? C26 O4 C28 115.83(18) . . ? O7 Cl3 O6 110.70(14) . . ? O7 Cl3 O5 109.42(12) . . ? O6 Cl3 O5 109.47(13) . . ? O7 Cl3 O8 109.43(14) . . ? O6 Cl3 O8 108.95(16) . . ? O5 Cl3 O8 108.85(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.469 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.075 #=== data_akya _database_code_depnum_ccdc_archive 'CCDC 286103' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Cl5 Co N4 O6' _chemical_formula_weight 722.66 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1872(6) _cell_length_b 22.7813(13) _cell_length_c 22.1940(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.922(2) _cell_angle_gamma 90.00 _cell_volume 5587.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9272 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 28.2 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8206 _exptl_absorpt_correction_T_max 0.8472 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 kappa' _diffrn_measurement_method 'Bruker APEX2' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 117026 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.77 _reflns_number_total 14459 _reflns_number_gt 10669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\\s^2^(Fo^2^)+(0.0382P)^2^+1.8173P] 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 14459 _refine_ls_number_parameters 936 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.0000 0.0000 0.01144(8) Uani 1 2 d S . . N1 N 0.64565(15) -0.04668(7) -0.00447(7) 0.0142(3) Uani 1 1 d . . . C1 C 0.6735(2) -0.10021(9) 0.01930(10) 0.0191(4) Uani 1 1 d . . . C2 C 0.7848(2) -0.12621(10) 0.01883(11) 0.0245(5) Uani 1 1 d . . . C3 C 0.8723(2) -0.09603(10) -0.00577(11) 0.0256(5) Uani 1 1 d . . . C4 C 0.8448(2) -0.04088(10) -0.03078(10) 0.0216(5) Uani 1 1 d . . . C5 C 0.73066(18) -0.01783(9) -0.02975(9) 0.0160(4) Uani 1 1 d . . . C6 C 0.68935(19) 0.03900(9) -0.05968(10) 0.0166(4) Uani 1 1 d . . . N2 N 0.59214(15) 0.06446(7) -0.02877(8) 0.0140(3) Uani 1 1 d . . . C7 C 0.63944(19) 0.10774(9) 0.01992(9) 0.0165(4) Uani 1 1 d . . . C8 C 0.72176(18) 0.07729(8) 0.07047(9) 0.0151(4) Uani 1 1 d . . . C9 C 0.84052(18) 0.09531(9) 0.08869(9) 0.0151(4) Uani 1 1 d . . . C10 C 0.90990(17) 0.06762(9) 0.13707(9) 0.0160(4) Uani 1 1 d . . . C11 C 0.86595(19) 0.02016(9) 0.16605(9) 0.0168(4) Uani 1 1 d . . . C12 C 0.74867(18) 0.00158(9) 0.14653(9) 0.0161(4) Uani 1 1 d . . . C13 C 0.67111(17) 0.03025(8) 0.09985(9) 0.0134(4) Uani 1 1 d . . . O1 O 0.55750(12) 0.01363(6) 0.08388(6) 0.0152(3) Uani 1 1 d . . . Cl1 Cl 1.05603(4) 0.09247(2) 0.16347(2) 0.02093(11) Uani 1 1 d . . . Cl2 Cl 0.69453(5) -0.05942(2) 0.18111(2) 0.02161(11) Uani 1 1 d . . . Co2 Co 1.0000 -0.5000 0.0000 0.01356(8) Uani 1 2 d S . . N3 N 1.15595(15) -0.47167(7) -0.01746(7) 0.0164(3) Uani 1 1 d . . . C14 C 1.2006(2) -0.41695(10) -0.00925(10) 0.0222(5) Uani 1 1 d . . . C15 C 1.3144(2) -0.40195(11) -0.02095(11) 0.0263(5) Uani 1 1 d . . . C16 C 1.3863(2) -0.44504(11) -0.04105(10) 0.0264(5) Uani 1 1 d . . . C17 C 1.3420(2) -0.50160(10) -0.04839(10) 0.0229(5) Uani 1 1 d . . . C18 C 1.22650(19) -0.51404(9) -0.03644(9) 0.0178(4) Uani 1 1 d . . . C19 C 1.1695(2) -0.57313(9) -0.04385(10) 0.0188(4) Uani 1 1 d . . . N4 N 1.07623(16) -0.57742(8) -0.00227(8) 0.0155(3) Uani 1 1 d . . . C20 C 1.1254(2) -0.60215(9) 0.05880(9) 0.0175(4) Uani 1 1 d . . . C21 C 1.20739(19) -0.56001(9) 0.09749(9) 0.0169(4) Uani 1 1 d . . . C22 C 1.32351(19) -0.57563(9) 0.12308(9) 0.0180(4) Uani 1 1 d . . . C23 C 1.39411(19) -0.53685(9) 0.16144(9) 0.0196(4) Uani 1 1 d . . . C24 C 1.3501(2) -0.48206(9) 0.17480(10) 0.0189(4) Uani 1 1 d . . . C25 C 1.23430(19) -0.46660(9) 0.14801(9) 0.0179(4) Uani 1 1 d . . . C26 C 1.15973(18) -0.50420(9) 0.10867(9) 0.0162(4) Uani 1 1 d . . . O2 O 1.05042(13) -0.48794(6) 0.08424(6) 0.0170(3) Uani 1 1 d . . . Cl3 Cl 1.54030(5) -0.55668(2) 0.19311(2) 0.02447(12) Uani 1 1 d . . . Cl4 Cl 1.17512(5) -0.39834(2) 0.16217(3) 0.02492(12) Uani 1 1 d . . . Co3 Co 0.63420(2) -0.250622(11) 0.251448(12) 0.01391(6) Uani 1 1 d . . . N5 N 0.49101(15) -0.25877(7) 0.29155(8) 0.0158(3) Uani 1 1 d . . . C27 C 0.4784(2) -0.24262(9) 0.34869(10) 0.0190(4) Uani 1 1 d . . . C28 C 0.3703(2) -0.24776(9) 0.37090(11) 0.0232(5) Uani 1 1 d . . . C29 C 0.2700(2) -0.26834(10) 0.33271(11) 0.0243(5) Uani 1 1 d . . . C30 C 0.2812(2) -0.28526(9) 0.27391(11) 0.0213(5) Uani 1 1 d . . . C31 C 0.39306(18) -0.28072(8) 0.25482(9) 0.0171(4) Uani 1 1 d . . . C32 C 0.41857(19) -0.30280(9) 0.19463(10) 0.0183(4) Uani 1 1 d . . . N6 N 0.52170(15) -0.26894(7) 0.17677(8) 0.0153(3) Uani 1 1 d . . . C33 C 0.4801(2) -0.21643(9) 0.13846(9) 0.0165(4) Uani 1 1 d . . . C34 C 0.42445(19) -0.17105(9) 0.17412(9) 0.0172(4) Uani 1 1 d . . . C35 C 0.30707(19) -0.15041(9) 0.15646(10) 0.0187(4) Uani 1 1 d . . . C36 C 0.2647(2) -0.10506(9) 0.18949(10) 0.0207(5) Uani 1 1 d . . . C37 C 0.3360(2) -0.08012(9) 0.23924(10) 0.0211(5) Uani 1 1 d . . . C38 C 0.4512(2) -0.10189(9) 0.25688(9) 0.0194(4) Uani 1 1 d . . . C39 C 0.49856(18) -0.14827(9) 0.22578(9) 0.0173(4) Uani 1 1 d . . . O3 O 0.60910(13) -0.16818(6) 0.24387(6) 0.0179(3) Uani 1 1 d . . . Cl5 Cl 0.11881(5) -0.07754(2) 0.16616(3) 0.02738(13) Uani 1 1 d . . . Cl6 Cl 0.54521(5) -0.07160(2) 0.31906(2) 0.02554(12) Uani 1 1 d . . . N7 N 0.77672(15) -0.24201(7) 0.21170(8) 0.0162(3) Uani 1 1 d . . . C40 C 0.7934(2) -0.26335(9) 0.15692(10) 0.0206(4) Uani 1 1 d . . . C41 C 0.9004(2) -0.25599(10) 0.13431(10) 0.0237(5) Uani 1 1 d . . . C42 C 0.9939(2) -0.22565(11) 0.16863(11) 0.0284(5) Uani 1 1 d . . . C43 C 0.9790(2) -0.20438(11) 0.22524(11) 0.0258(5) Uani 1 1 d . . . C44 C 0.86916(19) -0.21334(9) 0.24564(9) 0.0191(4) Uani 1 1 d . . . C45 C 0.8424(2) -0.19208(10) 0.30606(10) 0.0200(4) Uani 1 1 d . . . N8 N 0.74746(16) -0.23058(8) 0.32528(8) 0.0172(4) Uani 1 1 d . . . C46 C 0.7986(2) -0.28211(9) 0.36237(9) 0.0178(4) Uani 1 1 d . . . C47 C 0.85010(18) -0.32768(9) 0.32519(9) 0.0169(4) Uani 1 1 d . . . C48 C 0.96787(19) -0.34856(9) 0.34103(10) 0.0196(4) Uani 1 1 d . . . C49 C 1.00781(18) -0.39425(9) 0.30841(10) 0.0196(4) Uani 1 1 d . . . C50 C 0.93313(19) -0.42012(9) 0.25988(10) 0.0205(4) Uani 1 1 d . . . C51 C 0.81715(19) -0.39839(9) 0.24398(9) 0.0179(4) Uani 1 1 d . . . C52 C 0.77167(18) -0.35193(9) 0.27544(9) 0.0160(4) Uani 1 1 d . . . O4 O 0.65970(12) -0.33272(6) 0.25937(6) 0.0166(3) Uani 1 1 d . . . Cl7 Cl 1.15445(5) -0.42093(2) 0.32878(3) 0.02685(12) Uani 1 1 d . . . Cl8 Cl 0.72107(5) -0.42981(2) 0.18354(2) 0.02381(12) Uani 1 1 d . . . Cl9 Cl 1.12888(5) -0.25914(2) 0.01837(2) 0.02016(11) Uani 1 1 d . . . O5 O 1.02377(14) -0.29645(7) 0.00942(7) 0.0285(4) Uani 1 1 d . . . O6 O 1.20194(16) -0.27439(8) 0.07503(8) 0.0384(4) Uani 1 1 d . . . O7 O 1.09225(17) -0.19906(7) 0.02008(9) 0.0431(5) Uani 1 1 d . . . O8 O 1.19670(17) -0.26862(9) -0.03066(8) 0.0437(5) Uani 1 1 d . . . Cl10 Cl 0.90812(5) 0.21612(2) 0.50362(2) 0.02078(11) Uani 1 1 d . . . O9 O 0.95640(15) 0.27450(7) 0.50183(7) 0.0303(4) Uani 1 1 d . . . O10 O 0.77892(15) 0.21861(8) 0.50091(8) 0.0339(4) Uani 1 1 d . . . O11 O 0.96247(16) 0.18725(8) 0.55849(7) 0.0343(4) Uani 1 1 d . . . O12 O 0.93563(15) 0.18339(7) 0.45106(7) 0.0310(4) Uani 1 1 d . . . H1 H 0.6148(19) -0.1192(9) 0.0359(10) 0.015(6) Uiso 1 1 d . . . H2 H 0.798(2) -0.1637(11) 0.0338(11) 0.032(7) Uiso 1 1 d . . . H3 H 0.949(2) -0.1097(11) -0.0046(11) 0.029(7) Uiso 1 1 d . . . H4 H 0.895(2) -0.0224(11) -0.0488(11) 0.031(7) Uiso 1 1 d . . . H6A H 0.7533(18) 0.0649(9) -0.0564(9) 0.006(5) Uiso 1 1 d . . . H6B H 0.652(2) 0.0322(10) -0.1026(11) 0.023(6) Uiso 1 1 d . . . H1N2 H 0.545(2) 0.0827(9) -0.0544(10) 0.013(6) Uiso 1 1 d . . . H7A H 0.5671(19) 0.1244(9) 0.0341(9) 0.012(5) Uiso 1 1 d . . . H7B H 0.6813(19) 0.1393(10) 0.0033(10) 0.019(6) Uiso 1 1 d . . . H9 H 0.870(2) 0.1244(10) 0.0707(10) 0.023(6) Uiso 1 1 d . . . H11 H 0.912(2) 0.0011(9) 0.1977(10) 0.015(6) Uiso 1 1 d . . . H14 H 1.152(2) -0.3892(11) 0.0061(10) 0.026(6) Uiso 1 1 d . . . H15 H 1.337(2) -0.3642(11) -0.0163(11) 0.026(6) Uiso 1 1 d . . . H16 H 1.468(2) -0.4341(11) -0.0489(11) 0.029(7) Uiso 1 1 d . . . H17 H 1.388(2) -0.5318(10) -0.0627(10) 0.019(6) Uiso 1 1 d . . . H19A H 1.2286(19) -0.6040(9) -0.0356(9) 0.012(5) Uiso 1 1 d . . . H19B H 1.124(2) -0.5769(10) -0.0859(11) 0.021(6) Uiso 1 1 d . . . H1N4 H 1.024(2) -0.6006(9) -0.0184(10) 0.011(6) Uiso 1 1 d . . . H20A H 1.1651(18) -0.6382(9) 0.0531(9) 0.010(5) Uiso 1 1 d . . . H20B H 1.0538(19) -0.6097(9) 0.0762(9) 0.012(5) Uiso 1 1 d . . . H22 H 1.3503(19) -0.6109(10) 0.1152(10) 0.016(6) Uiso 1 1 d . . . H24 H 1.397(2) -0.4560(10) 0.1994(10) 0.021(6) Uiso 1 1 d . . . H27 H 0.547(2) -0.2268(9) 0.3722(10) 0.014(5) Uiso 1 1 d . . . H28 H 0.364(2) -0.2364(10) 0.4100(11) 0.028(7) Uiso 1 1 d . . . H29 H 0.199(2) -0.2724(11) 0.3465(12) 0.037(7) Uiso 1 1 d . . . H30 H 0.217(2) -0.2989(11) 0.2452(12) 0.039(7) Uiso 1 1 d . . . H32A H 0.352(2) -0.2999(10) 0.1621(11) 0.025(6) Uiso 1 1 d . . . H32B H 0.444(2) -0.3434(11) 0.1983(10) 0.025(6) Uiso 1 1 d . . . H1N6 H 0.557(2) -0.2936(10) 0.1527(11) 0.025(6) Uiso 1 1 d . . . H33A H 0.428(2) -0.2267(10) 0.1035(10) 0.017(6) Uiso 1 1 d . . . H33B H 0.547(2) -0.1996(9) 0.1247(9) 0.015(5) Uiso 1 1 d . . . H35 H 0.258(2) -0.1664(9) 0.1225(10) 0.017(6) Uiso 1 1 d . . . H37 H 0.305(2) -0.0437(12) 0.2627(12) 0.041(7) Uiso 1 1 d . . . H40 H 0.729(2) -0.2841(10) 0.1348(11) 0.023(6) Uiso 1 1 d . . . H41 H 0.901(2) -0.2729(10) 0.1000(11) 0.024(6) Uiso 1 1 d . . . H43 H 1.065(2) -0.2194(11) 0.1537(11) 0.031(7) Uiso 1 1 d . . . H42 H 1.041(2) -0.1835(10) 0.2509(10) 0.024(6) Uiso 1 1 d . . . H45A H 0.810(2) -0.1530(11) 0.3027(11) 0.031(7) Uiso 1 1 d . . . H45B H 0.915(2) -0.1921(10) 0.3383(11) 0.025(6) Uiso 1 1 d . . . H1N8 H 0.710(2) -0.2092(9) 0.3493(10) 0.015(6) Uiso 1 1 d . . . H46A H 0.7318(19) -0.2994(9) 0.3787(9) 0.011(5) Uiso 1 1 d . . . H46B H 0.860(2) -0.2699(11) 0.3956(12) 0.033(7) Uiso 1 1 d . . . H48 H 1.0156(19) -0.3346(9) 0.3735(10) 0.011(5) Uiso 1 1 d . . . H50 H 0.964(2) -0.4537(12) 0.2374(12) 0.044(8) Uiso 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 0.00938(18) 0.01215(18) 0.01263(18) 0.00136(14) 0.00116(14) -0.00027(14) N1 0.0128(8) 0.0145(8) 0.0150(8) 0.0003(6) 0.0006(6) 0.0002(6) C1 0.0177(11) 0.0177(10) 0.0225(11) 0.0027(8) 0.0048(9) 0.0007(8) C2 0.0231(12) 0.0198(11) 0.0310(13) 0.0044(9) 0.0049(10) 0.0072(9) C3 0.0159(12) 0.0296(13) 0.0320(13) -0.0007(10) 0.0057(10) 0.0077(9) C4 0.0155(11) 0.0267(12) 0.0234(12) -0.0018(9) 0.0055(9) 0.0002(9) C5 0.0156(10) 0.0181(10) 0.0139(10) -0.0018(7) 0.0010(8) -0.0007(8) C6 0.0139(10) 0.0191(10) 0.0182(11) 0.0019(8) 0.0066(8) -0.0019(8) N2 0.0120(9) 0.0148(8) 0.0141(8) 0.0039(7) -0.0017(7) 0.0007(7) C7 0.0160(11) 0.0137(10) 0.0197(10) 0.0003(8) 0.0021(8) -0.0014(8) C8 0.0150(10) 0.0152(9) 0.0149(10) -0.0023(7) 0.0019(8) -0.0010(8) C9 0.0147(10) 0.0123(9) 0.0193(10) -0.0001(8) 0.0056(8) -0.0033(8) C10 0.0099(10) 0.0179(10) 0.0202(10) -0.0052(8) 0.0022(8) -0.0025(8) C11 0.0138(10) 0.0190(10) 0.0173(10) -0.0003(8) 0.0013(8) 0.0009(8) C12 0.0158(10) 0.0170(10) 0.0160(10) 0.0018(8) 0.0037(8) -0.0021(8) C13 0.0133(10) 0.0132(9) 0.0140(9) -0.0031(7) 0.0028(8) 0.0003(7) O1 0.0119(7) 0.0195(7) 0.0140(7) 0.0004(5) 0.0017(5) -0.0031(5) Cl1 0.0123(2) 0.0238(3) 0.0259(3) -0.0034(2) 0.0005(2) -0.00389(19) Cl2 0.0198(3) 0.0239(3) 0.0201(3) 0.0081(2) -0.0001(2) -0.0060(2) Co2 0.01369(19) 0.01407(18) 0.01311(18) -0.00009(14) 0.00267(14) -0.00034(15) N3 0.0159(9) 0.0188(9) 0.0144(8) 0.0001(7) 0.0018(7) -0.0020(7) C14 0.0206(12) 0.0197(11) 0.0264(12) 0.0015(9) 0.0039(9) -0.0009(9) C15 0.0214(12) 0.0251(12) 0.0327(13) 0.0021(10) 0.0045(10) -0.0068(10) C16 0.0191(12) 0.0380(14) 0.0228(12) 0.0016(10) 0.0053(9) -0.0049(10) C17 0.0176(11) 0.0329(13) 0.0184(11) -0.0035(9) 0.0033(9) 0.0006(10) C18 0.0173(11) 0.0240(11) 0.0121(10) 0.0004(8) 0.0023(8) 0.0014(8) C19 0.0191(11) 0.0210(11) 0.0173(11) -0.0014(8) 0.0055(9) 0.0025(9) N4 0.0136(9) 0.0171(9) 0.0156(9) -0.0005(7) 0.0016(7) -0.0015(7) C20 0.0199(11) 0.0160(10) 0.0166(10) 0.0004(8) 0.0026(8) 0.0004(8) C21 0.0198(11) 0.0182(10) 0.0132(10) 0.0013(8) 0.0040(8) -0.0007(8) C22 0.0218(11) 0.0156(10) 0.0170(10) 0.0011(8) 0.0042(8) 0.0024(8) C23 0.0180(11) 0.0236(11) 0.0166(10) 0.0040(8) 0.0012(8) 0.0019(9) C24 0.0211(11) 0.0186(10) 0.0164(10) -0.0009(8) 0.0010(8) -0.0033(9) C25 0.0238(11) 0.0139(10) 0.0167(10) -0.0003(8) 0.0056(8) 0.0008(8) C26 0.0184(11) 0.0188(10) 0.0116(9) 0.0036(8) 0.0033(8) -0.0014(8) O2 0.0170(7) 0.0198(7) 0.0139(7) -0.0013(5) 0.0017(6) 0.0026(6) Cl3 0.0194(3) 0.0280(3) 0.0242(3) -0.0020(2) -0.0025(2) 0.0040(2) Cl4 0.0270(3) 0.0171(3) 0.0295(3) -0.0064(2) 0.0007(2) 0.0015(2) Co3 0.01263(14) 0.01379(13) 0.01540(14) -0.00039(10) 0.00250(10) -0.00078(10) N5 0.0149(9) 0.0142(8) 0.0183(9) 0.0015(6) 0.0029(7) 0.0004(7) C27 0.0192(11) 0.0162(10) 0.0213(11) -0.0001(8) 0.0025(9) -0.0022(8) C28 0.0257(13) 0.0207(11) 0.0253(12) -0.0031(9) 0.0102(10) 0.0017(9) C29 0.0180(12) 0.0232(11) 0.0341(13) 0.0014(9) 0.0111(10) 0.0007(9) C30 0.0146(11) 0.0196(11) 0.0292(12) 0.0010(9) 0.0022(9) -0.0017(8) C31 0.0171(11) 0.0128(10) 0.0209(11) 0.0010(8) 0.0016(8) 0.0005(8) C32 0.0150(11) 0.0194(11) 0.0194(11) 0.0000(8) -0.0008(9) -0.0028(8) N6 0.0157(9) 0.0141(8) 0.0162(9) 0.0003(7) 0.0030(7) 0.0021(7) C33 0.0160(11) 0.0187(10) 0.0148(10) 0.0019(8) 0.0026(8) 0.0022(8) C34 0.0209(11) 0.0142(10) 0.0180(10) 0.0024(8) 0.0078(8) -0.0002(8) C35 0.0221(11) 0.0167(10) 0.0180(11) 0.0030(8) 0.0051(9) -0.0010(9) C36 0.0217(11) 0.0202(11) 0.0215(11) 0.0077(8) 0.0074(9) 0.0047(9) C37 0.0304(13) 0.0154(10) 0.0202(11) 0.0041(8) 0.0118(9) 0.0062(9) C38 0.0250(12) 0.0171(10) 0.0173(10) -0.0004(8) 0.0067(9) -0.0018(9) C39 0.0212(11) 0.0135(10) 0.0185(10) 0.0041(8) 0.0075(8) -0.0014(8) O3 0.0181(8) 0.0141(7) 0.0218(8) 0.0009(6) 0.0039(6) -0.0007(6) Cl5 0.0231(3) 0.0283(3) 0.0324(3) 0.0063(2) 0.0096(2) 0.0103(2) Cl6 0.0339(3) 0.0228(3) 0.0206(3) -0.0056(2) 0.0066(2) -0.0019(2) N7 0.0158(9) 0.0172(9) 0.0160(8) 0.0011(7) 0.0033(7) 0.0001(7) C40 0.0215(12) 0.0195(11) 0.0207(11) 0.0002(8) 0.0032(9) -0.0005(9) C41 0.0249(12) 0.0293(12) 0.0187(11) -0.0001(9) 0.0089(9) 0.0015(10) C42 0.0201(12) 0.0375(14) 0.0296(13) 0.0031(10) 0.0097(10) -0.0046(10) C43 0.0191(12) 0.0316(13) 0.0265(12) -0.0002(10) 0.0024(9) -0.0061(10) C44 0.0173(11) 0.0193(10) 0.0205(11) 0.0032(8) 0.0023(8) -0.0013(8) C45 0.0174(11) 0.0218(11) 0.0207(11) -0.0003(9) 0.0025(9) -0.0072(9) N8 0.0165(9) 0.0174(9) 0.0178(9) -0.0017(7) 0.0032(7) -0.0014(7) C46 0.0171(11) 0.0207(11) 0.0158(10) 0.0007(8) 0.0032(9) -0.0010(8) C47 0.0159(10) 0.0173(10) 0.0177(10) 0.0045(8) 0.0035(8) -0.0008(8) C48 0.0169(11) 0.0235(11) 0.0174(11) 0.0048(8) -0.0001(8) -0.0048(9) C49 0.0107(10) 0.0215(11) 0.0266(11) 0.0078(9) 0.0029(8) 0.0016(8) C50 0.0197(11) 0.0185(10) 0.0248(11) 0.0036(9) 0.0085(9) 0.0018(9) C51 0.0190(11) 0.0184(10) 0.0163(10) -0.0007(8) 0.0024(8) -0.0023(8) C52 0.0142(10) 0.0172(10) 0.0171(10) 0.0032(8) 0.0042(8) -0.0011(8) O4 0.0132(7) 0.0145(7) 0.0217(8) 0.0002(6) 0.0016(6) 0.0000(5) Cl7 0.0146(3) 0.0313(3) 0.0346(3) 0.0097(2) 0.0035(2) 0.0049(2) Cl8 0.0230(3) 0.0250(3) 0.0229(3) -0.0074(2) 0.0021(2) -0.0016(2) Cl9 0.0192(3) 0.0206(3) 0.0199(2) 0.00386(19) 0.0006(2) -0.0019(2) O5 0.0223(9) 0.0284(9) 0.0356(10) -0.0055(7) 0.0066(7) -0.0094(7) O6 0.0361(10) 0.0455(11) 0.0289(10) 0.0101(8) -0.0103(8) -0.0016(9) O7 0.0451(12) 0.0174(9) 0.0653(13) 0.0101(8) 0.0039(10) 0.0032(8) O8 0.0361(11) 0.0655(13) 0.0330(10) 0.0083(9) 0.0169(8) -0.0009(9) Cl10 0.0198(3) 0.0194(2) 0.0226(3) 0.00237(19) 0.0014(2) -0.0012(2) O9 0.0358(10) 0.0209(8) 0.0342(10) 0.0016(7) 0.0058(8) -0.0066(7) O10 0.0204(9) 0.0391(10) 0.0430(11) 0.0017(8) 0.0069(8) -0.0012(8) O11 0.0406(11) 0.0374(10) 0.0231(9) 0.0105(7) 0.0001(8) -0.0003(8) O12 0.0379(10) 0.0292(9) 0.0261(9) -0.0031(7) 0.0057(7) 0.0055(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.8986(13) 3_655 ? Co1 O1 1.8986(13) . ? Co1 N2 1.9573(16) 3_655 ? Co1 N2 1.9573(16) . ? Co1 N1 1.9611(16) . ? Co1 N1 1.9611(16) 3_655 ? N1 C1 1.346(3) . ? N1 C5 1.348(2) . ? C1 C2 1.380(3) . ? C2 C3 1.376(3) . ? C3 C4 1.389(3) . ? C4 C5 1.384(3) . ? C5 C6 1.495(3) . ? C6 N2 1.490(3) . ? N2 C7 1.497(3) . ? C7 C8 1.506(3) . ? C8 C9 1.389(3) . ? C8 C13 1.417(3) . ? C9 C10 1.377(3) . ? C10 C11 1.387(3) . ? C10 Cl1 1.743(2) . ? C11 C12 1.383(3) . ? C12 C13 1.405(3) . ? C12 Cl2 1.741(2) . ? C13 O1 1.321(2) . ? Co2 O2 1.8874(13) . ? Co2 O2 1.8874(13) 3_745 ? Co2 N3 1.9545(16) . ? Co2 N3 1.9545(16) 3_745 ? Co2 N4 1.9631(17) . ? Co2 N4 1.9631(17) 3_745 ? N3 C14 1.345(3) . ? N3 C18 1.355(3) . ? C14 C15 1.381(3) . ? C15 C16 1.386(3) . ? C16 C17 1.381(3) . ? C17 C18 1.388(3) . ? C18 C19 1.488(3) . ? C19 N4 1.499(3) . ? N4 C20 1.492(3) . ? C20 C21 1.502(3) . ? C21 C22 1.381(3) . ? C21 C26 1.416(3) . ? C22 C23 1.386(3) . ? C23 C24 1.390(3) . ? C23 Cl3 1.737(2) . ? C24 C25 1.385(3) . ? C25 C26 1.402(3) . ? C25 Cl4 1.738(2) . ? C26 O2 1.312(2) . ? Co3 O4 1.8960(14) . ? Co3 O3 1.9025(14) . ? Co3 N7 1.9481(17) . ? Co3 N5 1.9584(17) . ? Co3 N8 1.9634(18) . ? Co3 N6 1.9642(17) . ? N5 C27 1.348(3) . ? N5 C31 1.356(3) . ? C27 C28 1.380(3) . ? C28 C29 1.379(3) . ? C29 C30 1.385(3) . ? C30 C31 1.386(3) . ? C31 C32 1.496(3) . ? C32 N6 1.492(3) . ? N6 C33 1.499(3) . ? C33 C34 1.495(3) . ? C34 C35 1.393(3) . ? C34 C39 1.406(3) . ? C35 C36 1.392(3) . ? C36 C37 1.380(3) . ? C36 Cl5 1.750(2) . ? C37 C38 1.379(3) . ? C38 C39 1.410(3) . ? C38 Cl6 1.743(2) . ? C39 O3 1.320(2) . ? N7 C44 1.350(3) . ? N7 C40 1.349(3) . ? C40 C41 1.379(3) . ? C41 C42 1.380(3) . ? C42 C43 1.381(3) . ? C43 C44 1.389(3) . ? C44 C45 1.499(3) . ? C45 N8 1.490(3) . ? N8 C46 1.496(3) . ? C46 C47 1.496(3) . ? C47 C48 1.394(3) . ? C47 C52 1.412(3) . ? C48 C49 1.381(3) . ? C49 C50 1.388(3) . ? C49 Cl7 1.742(2) . ? C50 C51 1.382(3) . ? C51 C52 1.406(3) . ? C51 Cl8 1.738(2) . ? C52 O4 1.323(2) . ? Cl9 O7 1.4310(17) . ? Cl9 O6 1.4322(17) . ? Cl9 O8 1.4360(18) . ? Cl9 O5 1.4395(16) . ? Cl10 O11 1.4336(16) . ? Cl10 O9 1.4383(16) . ? Cl10 O10 1.4384(17) . ? Cl10 O12 1.4571(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 180.00(8) 3_655 . ? O1 Co1 N2 94.68(6) 3_655 3_655 ? O1 Co1 N2 85.32(6) . 3_655 ? O1 Co1 N2 85.32(6) 3_655 . ? O1 Co1 N2 94.68(6) . . ? N2 Co1 N2 180.00(12) 3_655 . ? O1 Co1 N1 91.12(6) 3_655 . ? O1 Co1 N1 88.88(6) . . ? N2 Co1 N1 95.35(7) 3_655 . ? N2 Co1 N1 84.65(7) . . ? O1 Co1 N1 88.88(6) 3_655 3_655 ? O1 Co1 N1 91.12(6) . 3_655 ? N2 Co1 N1 84.65(7) 3_655 3_655 ? N2 Co1 N1 95.35(7) . 3_655 ? N1 Co1 N1 180.00(13) . 3_655 ? C1 N1 C5 118.01(17) . . ? C1 N1 Co1 127.96(14) . . ? C5 N1 Co1 113.70(13) . . ? N1 C1 C2 122.7(2) . . ? C3 C2 C1 119.1(2) . . ? C2 C3 C4 118.9(2) . . ? C5 C4 C3 119.0(2) . . ? N1 C5 C4 122.28(19) . . ? N1 C5 C6 114.69(17) . . ? C4 C5 C6 122.93(19) . . ? N2 C6 C5 109.26(16) . . ? C6 N2 C7 112.77(16) . . ? C6 N2 Co1 108.47(12) . . ? C7 N2 Co1 113.80(12) . . ? N2 C7 C8 109.95(16) . . ? C9 C8 C13 121.47(18) . . ? C9 C8 C7 121.82(18) . . ? C13 C8 C7 116.68(17) . . ? C10 C9 C8 119.31(18) . . ? C9 C10 C11 121.44(18) . . ? C9 C10 Cl1 119.95(15) . . ? C11 C10 Cl1 118.60(16) . . ? C12 C11 C10 118.74(19) . . ? C11 C12 C13 122.43(18) . . ? C11 C12 Cl2 118.96(16) . . ? C13 C12 Cl2 118.61(15) . . ? O1 C13 C12 121.54(17) . . ? O1 C13 C8 122.00(17) . . ? C12 C13 C8 116.45(17) . . ? C13 O1 Co1 118.40(12) . . ? O2 Co2 O2 180.0 . 3_745 ? O2 Co2 N3 90.55(6) . . ? O2 Co2 N3 89.45(6) 3_745 . ? O2 Co2 N3 89.45(6) . 3_745 ? O2 Co2 N3 90.55(6) 3_745 3_745 ? N3 Co2 N3 180.00(13) . 3_745 ? O2 Co2 N4 95.27(6) . . ? O2 Co2 N4 84.73(6) 3_745 . ? N3 Co2 N4 83.50(7) . . ? N3 Co2 N4 96.50(7) 3_745 . ? O2 Co2 N4 84.73(6) . 3_745 ? O2 Co2 N4 95.27(6) 3_745 3_745 ? N3 Co2 N4 96.50(7) . 3_745 ? N3 Co2 N4 83.50(7) 3_745 3_745 ? N4 Co2 N4 180.0 . 3_745 ? C14 N3 C18 118.72(18) . . ? C14 N3 Co2 127.11(15) . . ? C18 N3 Co2 114.05(13) . . ? N3 C14 C15 122.5(2) . . ? C14 C15 C16 118.9(2) . . ? C17 C16 C15 118.9(2) . . ? C16 C17 C18 119.7(2) . . ? N3 C18 C17 121.2(2) . . ? N3 C18 C19 114.73(18) . . ? C17 C18 C19 124.03(19) . . ? C18 C19 N4 108.57(16) . . ? C20 N4 C19 112.96(17) . . ? C20 N4 Co2 114.61(13) . . ? C19 N4 Co2 107.68(12) . . ? N4 C20 C21 112.61(17) . . ? C22 C21 C26 121.01(19) . . ? C22 C21 C20 121.50(18) . . ? C26 C21 C20 117.46(18) . . ? C21 C22 C23 119.9(2) . . ? C22 C23 C24 121.1(2) . . ? C22 C23 Cl3 119.60(17) . . ? C24 C23 Cl3 119.30(17) . . ? C25 C24 C23 118.4(2) . . ? C24 C25 C26 122.59(19) . . ? C24 C25 Cl4 120.49(16) . . ? C26 C25 Cl4 116.91(16) . . ? O2 C26 C25 120.76(18) . . ? O2 C26 C21 122.24(18) . . ? C25 C26 C21 117.00(19) . . ? C26 O2 Co2 118.98(12) . . ? O4 Co3 O3 179.72(7) . . ? O4 Co3 N7 91.12(6) . . ? O3 Co3 N7 88.88(6) . . ? O4 Co3 N5 89.21(6) . . ? O3 Co3 N5 90.79(6) . . ? N7 Co3 N5 179.64(7) . . ? O4 Co3 N8 94.80(7) . . ? O3 Co3 N8 84.93(7) . . ? N7 Co3 N8 83.51(7) . . ? N5 Co3 N8 96.33(7) . . ? O4 Co3 N6 86.34(6) . . ? O3 Co3 N6 93.94(7) . . ? N7 Co3 N6 95.83(7) . . ? N5 Co3 N6 84.32(7) . . ? N8 Co3 N6 178.70(7) . . ? C27 N5 C31 118.27(18) . . ? C27 N5 Co3 127.84(15) . . ? C31 N5 Co3 113.79(13) . . ? N5 C27 C28 122.5(2) . . ? C29 C28 C27 118.9(2) . . ? C28 C29 C30 119.3(2) . . ? C29 C30 C31 119.0(2) . . ? N5 C31 C30 121.84(19) . . ? N5 C31 C32 114.38(17) . . ? C30 C31 C32 123.67(19) . . ? N6 C32 C31 109.02(17) . . ? C32 N6 C33 112.24(16) . . ? C32 N6 Co3 107.85(12) . . ? C33 N6 Co3 114.26(13) . . ? C34 C33 N6 111.69(16) . . ? C35 C34 C39 121.06(19) . . ? C35 C34 C33 122.45(19) . . ? C39 C34 C33 116.46(18) . . ? C36 C35 C34 119.1(2) . . ? C37 C36 C35 121.7(2) . . ? C37 C36 Cl5 119.07(16) . . ? C35 C36 Cl5 119.22(17) . . ? C38 C37 C36 118.52(19) . . ? C37 C38 C39 122.4(2) . . ? C37 C38 Cl6 120.32(16) . . ? C39 C38 Cl6 117.27(16) . . ? O3 C39 C34 121.83(18) . . ? O3 C39 C38 120.95(19) . . ? C34 C39 C38 117.20(19) . . ? C39 O3 Co3 118.99(12) . . ? C44 N7 C40 118.46(18) . . ? C44 N7 Co3 113.96(13) . . ? C40 N7 Co3 127.51(15) . . ? N7 C40 C41 122.2(2) . . ? C40 C41 C42 119.1(2) . . ? C43 C42 C41 119.3(2) . . ? C42 C43 C44 118.9(2) . . ? N7 C44 C43 122.0(2) . . ? N7 C44 C45 114.42(18) . . ? C43 C44 C45 123.6(2) . . ? N8 C45 C44 108.44(17) . . ? C45 N8 C46 113.00(17) . . ? C45 N8 Co3 107.11(13) . . ? C46 N8 Co3 114.78(13) . . ? C47 C46 N8 112.85(17) . . ? C48 C47 C52 120.81(19) . . ? C48 C47 C46 121.84(19) . . ? C52 C47 C46 117.20(18) . . ? C49 C48 C47 119.7(2) . . ? C48 C49 C50 121.47(19) . . ? C48 C49 Cl7 119.68(17) . . ? C50 C49 Cl7 118.85(17) . . ? C51 C50 C49 118.3(2) . . ? C50 C51 C52 122.71(19) . . ? C50 C51 Cl8 119.55(16) . . ? C52 C51 Cl8 117.73(16) . . ? O4 C52 C51 121.04(18) . . ? O4 C52 C47 121.95(18) . . ? C51 C52 C47 117.00(18) . . ? C52 O4 Co3 118.29(12) . . ? O7 Cl9 O6 109.60(11) . . ? O7 Cl9 O8 110.56(12) . . ? O6 Cl9 O8 109.40(11) . . ? O7 Cl9 O5 109.71(10) . . ? O6 Cl9 O5 108.70(10) . . ? O8 Cl9 O5 108.84(11) . . ? O11 Cl10 O9 109.64(10) . . ? O11 Cl10 O10 110.16(11) . . ? O9 Cl10 O10 109.97(10) . . ? O11 Cl10 O12 109.33(10) . . ? O9 Cl10 O12 108.91(10) . . ? O10 Cl10 O12 108.81(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.567 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.077 #===end