Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Hammershoi, Anders' 'Bendahl, Lars' 'Jensen, Dan Kjaergaard' 'Larsen, Sine' 'Riisager, Anders' 'Sargeson, A. M.' 'Sorensen, Henning Osholm' _publ_contact_author_name 'Anders Hammershoi' _publ_contact_author_address ; Department of Chemistry University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denmark ; _publ_contact_author_phone '(+45)35320110' _publ_contact_author_fax '(+45)35320133' _publ_contact_author_email 'anders@kiku.dk' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Metal complex amino acid synthons: syntheses, structures and stereoselective reactions of (iminoacetato)cobalt(III) complexes ; data_9 _database_code_CSD 180573 _audit_creation_method 'SHELXL-97 and manual editing' _chemical_name_systematic ; LAMBDA(+)578-[(en)2Co(O2CCH=NH)]Br2,H2O ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Co N5 O2, 2Br, H2O' _chemical_formula_sum 'C6 H20 Br2 Co N5 O3' _chemical_formula_weight 429.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.1300(2) _cell_length_b 8.3730(3) _cell_length_c 20.9660(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1427.21(7) _cell_formula_units_Z 4 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 172 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 23.9 _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 6.807 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.167 _exptl_absorpt_correction_T_max 0.579 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 122(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\q and \f scans' _diffrn_reflns_number 30189 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 35.01 _reflns_number_total 6211 _reflns_number_gt 5893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DIRAX (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep II (Johnson, 1976)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0184P)^2^+10.0960P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _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 0.032(14) _refine_ls_number_reflns 6211 _refine_ls_number_parameters 208 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 1.280 _refine_ls_restrained_S_all 1.274 _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 Co Co -0.18325(7) -0.03792(7) -0.84650(3) 0.00916(9) Uani 1 1 d . . . N11 N -0.3018(5) -0.1368(4) -0.91686(17) 0.0115(5) Uani 1 1 d D . . H11D H -0.298(9) -0.070(6) -0.951(2) 0.014 Uiso 1 1 d D . . H11E H -0.400(5) -0.164(8) -0.899(3) 0.014 Uiso 1 1 d D . . C11 C -0.2130(6) -0.2860(6) -0.9351(2) 0.0171(8) Uani 1 1 d D . . H11A H -0.239(9) -0.330(9) -0.9799(19) 0.021 Uiso 1 1 d D . . H11B H -0.247(9) -0.378(6) -0.905(3) 0.021 Uiso 1 1 d D . . C12 C -0.0305(6) -0.2472(6) -0.9344(2) 0.0188(9) Uani 1 1 d D . . H12A H 0.038(8) -0.350(6) -0.939(3) 0.023 Uiso 1 1 d D . . H12B H 0.013(9) -0.180(8) -0.972(3) 0.023 Uiso 1 1 d D . . N12 N 0.0049(5) -0.1688(5) -0.87247(19) 0.0144(6) Uani 1 1 d D . . H12D H 0.018(9) -0.237(7) -0.839(2) 0.017 Uiso 1 1 d D . . H12E H 0.097(6) -0.109(7) -0.876(3) 0.017 Uiso 1 1 d D . . N21 N -0.1150(5) 0.1412(5) -0.89999(19) 0.0132(6) Uani 1 1 d D . . H21D H -0.071(8) 0.101(8) -0.936(2) 0.016 Uiso 1 1 d D . . H21E H -0.013(5) 0.153(9) -0.884(3) 0.016 Uiso 1 1 d D . . C21 C -0.2509(6) 0.2576(6) -0.9050(2) 0.0168(8) Uani 1 1 d D . . H21A H -0.324(8) 0.210(8) -0.940(3) 0.020 Uiso 1 1 d D . . H21B H -0.215(9) 0.366(5) -0.922(3) 0.020 Uiso 1 1 d D . . C22 C -0.3361(6) 0.2647(5) -0.8406(2) 0.0180(8) Uani 1 1 d D . . H22A H -0.248(7) 0.309(8) -0.810(3) 0.022 Uiso 1 1 d D . . H22B H -0.434(6) 0.337(8) -0.851(3) 0.022 Uiso 1 1 d D . . N22 N -0.3701(5) 0.0963(5) -0.82271(18) 0.0138(6) Uani 1 1 d D . . H22D H -0.394(9) 0.101(9) -0.7803(15) 0.017 Uiso 1 1 d D . . H22E H -0.465(6) 0.047(8) -0.835(3) 0.017 Uiso 1 1 d D . . O1 O -0.0571(4) 0.0448(4) -0.77639(16) 0.0141(6) Uani 1 1 d . . . C1 C -0.0679(5) -0.0384(6) -0.7242(2) 0.0133(7) Uani 1 1 d . . . O2 O 0.0090(5) -0.0146(5) -0.67568(17) 0.0193(7) Uani 1 1 d . . . C2 C -0.1913(6) -0.1735(5) -0.7292(2) 0.0139(7) Uani 1 1 d D . . H2 H -0.194(10) -0.225(7) -0.6878(15) 0.017 Uiso 1 1 d D . . N1 N -0.2514(5) -0.1932(5) -0.78561(19) 0.0157(7) Uani 1 1 d D . . H1 H -0.324(7) -0.277(6) -0.786(3) 0.019 Uiso 1 1 d D . . O3 O -0.1968(6) 0.0394(5) -1.03218(18) 0.0261(8) Uani 1 1 d . . . Br1 Br -0.39991(6) 0.15597(6) -0.66313(2) 0.01624(9) Uani 1 1 d . . . Br2 Br -0.30367(6) 0.58612(5) -0.57569(2) 0.01576(9) 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 0.0082(2) 0.0100(2) 0.0093(2) 0.00072(17) -0.00102(18) -0.00128(18) N11 0.0124(14) 0.0100(13) 0.0122(13) 0.0004(11) -0.0036(12) 0.0021(12) C11 0.019(2) 0.0139(17) 0.0189(19) -0.0024(14) -0.0029(15) 0.0031(15) C12 0.018(2) 0.019(2) 0.020(2) -0.0023(16) 0.0028(16) 0.0046(16) N12 0.0132(15) 0.0151(16) 0.0149(15) 0.0000(13) -0.0030(12) 0.0025(13) N21 0.0115(15) 0.0119(14) 0.0161(15) 0.0025(12) 0.0003(12) -0.0012(12) C21 0.0191(19) 0.0131(17) 0.0183(19) 0.0041(15) -0.0032(16) 0.0048(15) C22 0.022(2) 0.0124(17) 0.0200(19) -0.0028(15) 0.0018(17) 0.0042(15) N22 0.0117(14) 0.0180(16) 0.0118(14) -0.0046(13) 0.0006(11) -0.0002(13) O1 0.0139(13) 0.0137(13) 0.0148(13) 0.0022(11) -0.0048(11) -0.0036(11) C1 0.0141(17) 0.0128(16) 0.0131(16) -0.0008(14) -0.0036(13) 0.0018(14) O2 0.0167(15) 0.0255(18) 0.0157(15) -0.0054(13) -0.0084(12) 0.0052(13) C2 0.0139(16) 0.0137(16) 0.0143(16) 0.0023(13) -0.0029(15) -0.0004(15) N1 0.0156(16) 0.0181(17) 0.0135(15) 0.0035(13) -0.0021(13) -0.0048(13) O3 0.041(2) 0.0205(16) 0.0169(15) -0.0051(13) 0.0045(17) -0.0009(18) Br1 0.01342(17) 0.02134(19) 0.01395(17) -0.00170(16) -0.00154(15) 0.00405(16) Br2 0.01385(17) 0.01532(17) 0.01810(18) -0.00143(15) -0.00299(16) 0.00139(15) _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 N1 1.904(4) . ? Co O1 1.921(3) . ? Co N11 1.947(4) . ? Co N21 1.954(4) . ? Co N22 1.954(4) . ? Co N12 1.959(4) . ? N11 C11 1.493(6) . ? N11 H11D 0.91(3) . ? N11 H11E 0.91(3) . ? C11 C12 1.519(7) . ? C11 H11A 1.03(3) . ? C11 H11B 1.03(3) . ? C12 N12 1.483(7) . ? C12 H12A 1.03(3) . ? C12 H12B 1.03(3) . ? N12 H12D 0.91(3) . ? N12 H12E 0.90(3) . ? N21 C21 1.477(6) . ? N21 H21D 0.91(3) . ? N21 H21E 0.90(3) . ? C21 C22 1.519(7) . ? C21 H21A 1.03(3) . ? C21 H21B 1.02(3) . ? C22 N22 1.485(7) . ? C22 H22A 1.03(3) . ? C22 H22B 1.03(3) . ? N22 H22D 0.91(3) . ? N22 H22E 0.91(3) . ? O1 C1 1.299(5) . ? C1 O2 1.211(5) . ? C1 C2 1.516(6) . ? C2 N1 1.291(6) . ? C2 H2 0.968(10) . ? N1 H1 0.914(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co O1 83.59(16) . . ? N1 Co N11 94.22(17) . . ? O1 Co N11 175.64(15) . . ? N1 Co N21 172.62(18) . . ? O1 Co N21 90.62(16) . . ? N11 Co N21 91.85(16) . . ? N1 Co N22 89.74(18) . . ? O1 Co N22 90.72(16) . . ? N11 Co N22 93.04(16) . . ? N21 Co N22 85.74(17) . . ? N1 Co N12 91.80(19) . . ? O1 Co N12 89.85(16) . . ? N11 Co N12 86.44(16) . . ? N21 Co N12 92.77(17) . . ? N22 Co N12 178.41(18) . . ? C11 N11 Co 108.1(3) . . ? C11 N11 H11D 107(4) . . ? Co N11 H11D 109(4) . . ? C11 N11 H11E 109(5) . . ? Co N11 H11E 103(4) . . ? H11D N11 H11E 120(6) . . ? N11 C11 C12 106.9(4) . . ? N11 C11 H11A 116(4) . . ? C12 C11 H11A 106(4) . . ? N11 C11 H11B 109(4) . . ? C12 C11 H11B 115(4) . . ? H11A C11 H11B 104(6) . . ? N12 C12 C11 107.0(4) . . ? N12 C12 H12A 110(4) . . ? C11 C12 H12A 110(4) . . ? N12 C12 H12B 111(4) . . ? C11 C12 H12B 117(4) . . ? H12A C12 H12B 102(6) . . ? C12 N12 Co 109.8(3) . . ? C12 N12 H12D 115(5) . . ? Co N12 H12D 103(5) . . ? C12 N12 H12E 109(4) . . ? Co N12 H12E 111(5) . . ? H12D N12 H12E 108(6) . . ? C21 N21 Co 109.6(3) . . ? C21 N21 H21D 119(4) . . ? Co N21 H21D 108(5) . . ? C21 N21 H21E 130(5) . . ? Co N21 H21E 97(5) . . ? H21D N21 H21E 90(6) . . ? N21 C21 C22 107.7(4) . . ? N21 C21 H21A 103(4) . . ? C22 C21 H21A 113(4) . . ? N21 C21 H21B 113(4) . . ? C22 C21 H21B 115(4) . . ? H21A C21 H21B 105(6) . . ? N22 C22 C21 105.8(4) . . ? N22 C22 H22A 109(4) . . ? C21 C22 H22A 104(4) . . ? N22 C22 H22B 118(4) . . ? C21 C22 H22B 101(4) . . ? H22A C22 H22B 117(6) . . ? C22 N22 Co 109.7(3) . . ? C22 N22 H22D 104(5) . . ? Co N22 H22D 116(5) . . ? C22 N22 H22E 121(5) . . ? Co N22 H22E 109(4) . . ? H22D N22 H22E 97(6) . . ? C1 O1 Co 114.5(3) . . ? O2 C1 O1 125.8(5) . . ? O2 C1 C2 121.4(4) . . ? O1 C1 C2 112.8(4) . . ? N1 C2 C1 114.1(4) . . ? N1 C2 H2 139(4) . . ? C1 C2 H2 107(4) . . ? C2 N1 Co 114.7(3) . . ? C2 N1 H1 111(4) . . ? Co N1 H1 134(4) . . ? 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 N1 Co N11 C11 -72.7(3) . . . . ? O1 Co N11 C11 -13(2) . . . . ? N21 Co N11 C11 111.5(3) . . . . ? N22 Co N11 C11 -162.7(3) . . . . ? N12 Co N11 C11 18.8(3) . . . . ? Co N11 C11 C12 -42.4(4) . . . . ? N11 C11 C12 N12 50.2(5) . . . . ? C11 C12 N12 Co -34.7(5) . . . . ? N1 Co N12 C12 103.4(3) . . . . ? O1 Co N12 C12 -173.0(3) . . . . ? N11 Co N12 C12 9.3(3) . . . . ? N21 Co N12 C12 -82.4(3) . . . . ? N22 Co N12 C12 -62(6) . . . . ? N1 Co N21 C21 -64.7(15) . . . . ? O1 Co N21 C21 -103.0(3) . . . . ? N11 Co N21 C21 80.6(3) . . . . ? N22 Co N21 C21 -12.3(3) . . . . ? N12 Co N21 C21 167.1(3) . . . . ? Co N21 C21 C22 37.5(4) . . . . ? N21 C21 C22 N22 -50.1(5) . . . . ? C21 C22 N22 Co 39.8(4) . . . . ? N1 Co N22 C22 158.0(3) . . . . ? O1 Co N22 C22 74.4(3) . . . . ? N11 Co N22 C22 -107.8(3) . . . . ? N21 Co N22 C22 -16.1(3) . . . . ? N12 Co N22 C22 -37(6) . . . . ? N1 Co O1 C1 2.6(3) . . . . ? N11 Co O1 C1 -57(2) . . . . ? N21 Co O1 C1 178.0(3) . . . . ? N22 Co O1 C1 92.2(3) . . . . ? N12 Co O1 C1 -89.2(3) . . . . ? Co O1 C1 O2 174.9(4) . . . . ? Co O1 C1 C2 -5.5(5) . . . . ? O2 C1 C2 N1 -173.6(5) . . . . ? O1 C1 C2 N1 6.7(6) . . . . ? C1 C2 N1 Co -4.7(5) . . . . ? O1 Co N1 C2 1.5(4) . . . . ? N11 Co N1 C2 177.7(4) . . . . ? N21 Co N1 C2 -37.1(16) . . . . ? N22 Co N1 C2 -89.3(4) . . . . ? N12 Co N1 C2 91.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 35.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.124 _refine_diff_density_min -1.299 _refine_diff_density_rms 0.212 #===END data_10 _database_code_CSD 180574 _audit_creation_method 'SHELXL-97 and manual editing' _chemical_name_systematic ; [(en)2Co(O2CCH=NMe)]S2O6,1.5H2O ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H20 Co N5, S2 O6 , 1.5 H2 O' _chemical_formula_sum 'C7 H23 Co N5 O9.50 S2' _chemical_formula_weight 452.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/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 7.3390(2) _cell_length_b 16.3540(3) _cell_length_c 14.3640(3) _cell_angle_alpha 90.0000 _cell_angle_beta 92.7780(16) _cell_angle_gamma 90.0000 _cell_volume 1721.97(7) _cell_formula_units_Z 4 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 179 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 23.8 _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 1.295 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.763 _exptl_absorpt_correction_T_max 0.839 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 122(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\q and \f scans' _diffrn_reflns_number 57596 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 35.00 _reflns_number_total 7557 _reflns_number_gt 6691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DIRAX (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep II (Johnson, 1976)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0390P)^2^+2.1714P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7557 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 Co Co 0.84720(2) 0.891638(11) 0.635345(12) 0.00899(5) Uani 1 1 d . . . O1 O 0.80657(14) 0.95795(6) 0.52731(7) 0.01227(17) Uani 1 1 d . . . C1 C 0.70694(18) 1.02113(8) 0.53930(9) 0.0113(2) Uani 1 1 d . . . O2 O 0.66517(15) 1.07149(7) 0.47780(8) 0.01610(19) Uani 1 1 d . . . C2 C 0.64219(19) 1.02966(9) 0.63616(10) 0.0132(2) Uani 1 1 d . . . H2 H 0.577(3) 1.0725(15) 0.6546(16) 0.016 Uiso 1 1 d . . . N1 N 0.69729(17) 0.97397(8) 0.69338(8) 0.0129(2) Uani 1 1 d . . . C3 C 0.6439(2) 0.97770(11) 0.78986(10) 0.0186(3) Uani 1 1 d . . . H3A H 0.596(4) 0.9275(17) 0.8071(19) 0.028 Uiso 1 1 d . . . H3B H 0.556(4) 1.0178(17) 0.7958(19) 0.028 Uiso 1 1 d . . . H3C H 0.748(4) 0.9927(17) 0.8236(19) 0.028 Uiso 1 1 d . . . N11 N 0.89776(17) 0.82701(8) 0.74778(8) 0.0133(2) Uani 1 1 d . . . H11D H 0.798(3) 0.8192(14) 0.7820(16) 0.016 Uiso 1 1 d . . . H11E H 0.930(3) 0.7776(15) 0.7325(16) 0.016 Uiso 1 1 d . . . C11 C 1.0457(2) 0.86652(10) 0.80706(11) 0.0184(3) Uani 1 1 d . . . H11A H 0.984(4) 0.9082(16) 0.8450(18) 0.022 Uiso 1 1 d . . . H11B H 1.105(4) 0.8293(16) 0.8463(18) 0.022 Uiso 1 1 d . . . C12 C 1.1796(2) 0.90260(9) 0.74205(12) 0.0171(3) Uani 1 1 d . . . H12A H 1.268(3) 0.9369(15) 0.7747(17) 0.021 Uiso 1 1 d . . . H12B H 1.248(3) 0.8625(16) 0.7127(17) 0.021 Uiso 1 1 d . . . N12 N 1.07237(17) 0.94976(8) 0.67019(9) 0.0131(2) Uani 1 1 d . . . H12D H 1.132(3) 0.9566(15) 0.6226(17) 0.016 Uiso 1 1 d . . . H12E H 1.047(3) 0.9955(15) 0.6909(16) 0.016 Uiso 1 1 d . . . N21 N 0.97956(17) 0.81602(8) 0.55849(8) 0.01230(19) Uani 1 1 d . . . H21D H 1.003(3) 0.8412(14) 0.5078(17) 0.015 Uiso 1 1 d . . . H21E H 1.089(3) 0.7991(14) 0.5816(16) 0.015 Uiso 1 1 d . . . C21 C 0.8645(2) 0.74341(9) 0.53456(11) 0.0158(2) Uani 1 1 d . . . H21A H 0.910(3) 0.7176(15) 0.4817(17) 0.019 Uiso 1 1 d . . . H21B H 0.874(3) 0.7062(15) 0.5861(17) 0.019 Uiso 1 1 d . . . C22 C 0.6727(2) 0.77509(10) 0.51665(11) 0.0167(2) Uani 1 1 d . . . H22A H 0.583(3) 0.7333(16) 0.5126(17) 0.020 Uiso 1 1 d . . . H22B H 0.664(3) 0.8086(16) 0.4623(17) 0.020 Uiso 1 1 d . . . N22 N 0.63143(16) 0.82758(8) 0.59747(8) 0.01220(19) Uani 1 1 d . . . H22D H 0.541(3) 0.8579(15) 0.5756(16) 0.015 Uiso 1 1 d . . . H22E H 0.597(3) 0.7958(15) 0.6445(16) 0.015 Uiso 1 1 d . . . S1 S 0.52873(5) 0.68467(2) 0.78547(2) 0.01295(6) Uani 1 1 d . . . O11 O 0.52159(17) 0.62891(7) 0.86414(8) 0.0171(2) Uani 1 1 d . . . O12 O 0.66868(16) 0.66469(8) 0.72105(9) 0.0207(2) Uani 1 1 d . . . O13 O 0.52523(17) 0.77097(7) 0.80989(9) 0.0205(2) Uani 1 1 d . . . S2 S 0.28083(5) 0.66381(2) 0.70588(3) 0.01607(7) Uani 1 1 d . . . O14 O 0.29188(17) 0.72064(8) 0.62836(9) 0.0205(2) Uani 1 1 d . . . O15 O 0.13347(17) 0.68105(9) 0.76676(11) 0.0255(3) Uani 1 1 d . . . O16 O 0.2938(2) 0.57815(8) 0.67964(11) 0.0267(3) Uani 1 1 d . . . O1W O 1.1139(7) 0.9338(3) 1.0289(4) 0.0744(19) Uiso 0.599(10) 1 d P A 1 O2W O 0.8157(9) 0.9806(4) 1.0073(5) 0.059(2) Uiso 0.375(9) 1 d P B 2 O3W O 0.5677(7) 0.9902(4) 1.0148(4) 0.073(2) Uiso 0.508(9) 1 d P . 3 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 0.00897(8) 0.00929(8) 0.00875(7) 0.00136(5) 0.00074(5) 0.00095(6) O1 0.0133(4) 0.0120(4) 0.0116(4) 0.0030(3) 0.0023(3) 0.0030(3) C1 0.0094(5) 0.0112(5) 0.0133(5) 0.0014(4) 0.0001(4) 0.0002(4) O2 0.0141(4) 0.0151(5) 0.0190(5) 0.0072(4) -0.0002(4) 0.0024(4) C2 0.0122(5) 0.0126(5) 0.0149(5) -0.0007(4) 0.0017(4) 0.0011(4) N1 0.0117(5) 0.0150(5) 0.0123(5) 0.0001(4) 0.0016(4) 0.0011(4) C3 0.0179(6) 0.0263(7) 0.0121(5) -0.0019(5) 0.0040(5) 0.0048(6) N11 0.0145(5) 0.0136(5) 0.0115(5) 0.0026(4) -0.0008(4) -0.0006(4) C11 0.0218(7) 0.0187(6) 0.0141(6) 0.0016(5) -0.0062(5) -0.0014(5) C12 0.0143(6) 0.0136(6) 0.0228(6) 0.0009(5) -0.0055(5) 0.0001(5) N12 0.0126(5) 0.0103(5) 0.0165(5) 0.0008(4) 0.0003(4) 0.0001(4) N21 0.0120(5) 0.0126(5) 0.0124(4) 0.0011(4) 0.0016(4) 0.0015(4) C21 0.0171(6) 0.0130(6) 0.0174(6) -0.0024(5) 0.0014(5) 0.0005(5) C22 0.0158(6) 0.0193(6) 0.0149(6) -0.0032(5) -0.0016(5) -0.0005(5) N22 0.0106(4) 0.0138(5) 0.0122(5) 0.0019(4) -0.0001(4) -0.0001(4) S1 0.01121(13) 0.01171(14) 0.01604(14) 0.00475(11) 0.00176(10) 0.00030(10) O11 0.0204(5) 0.0151(5) 0.0159(5) 0.0054(4) 0.0017(4) 0.0003(4) O12 0.0141(5) 0.0262(6) 0.0222(5) 0.0071(4) 0.0062(4) 0.0036(4) O13 0.0210(5) 0.0120(5) 0.0285(6) 0.0020(4) 0.0000(4) -0.0028(4) S2 0.01238(14) 0.01181(14) 0.02383(17) 0.00472(12) -0.00109(12) -0.00047(11) O14 0.0185(5) 0.0192(5) 0.0233(5) 0.0084(4) -0.0038(4) 0.0008(4) O15 0.0122(5) 0.0267(6) 0.0380(7) 0.0092(5) 0.0064(5) 0.0018(4) O16 0.0306(7) 0.0130(5) 0.0356(7) 0.0000(5) -0.0061(5) -0.0025(5) _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 1.9047(10) . yes Co N1 1.9511(12) . yes Co N11 1.9506(12) . yes Co N12 1.9506(13) . yes Co N21 1.9481(12) . yes Co N22 1.9538(12) . yes O1 C1 1.2822(17) . no C1 O2 1.2354(17) . no C1 C2 1.498(2) . no C2 N1 1.2792(19) . no C2 H2 0.90(2) . no N1 C3 1.4595(19) . no C3 H3A 0.93(3) . no C3 H3B 0.93(3) . no C3 H3C 0.92(3) . no N11 C11 1.494(2) . no N11 H11D 0.91(2) . no N11 H11E 0.87(2) . no C11 C12 1.508(2) . no C11 H11A 0.99(3) . no C11 H11B 0.92(3) . no C12 N12 1.483(2) . no C12 H12A 0.96(3) . no C12 H12B 0.94(3) . no N12 H12D 0.84(2) . no N12 H12E 0.83(2) . no N21 C21 1.488(2) . no N21 H21D 0.86(2) . no N21 H21E 0.90(2) . no C21 C22 1.510(2) . no C21 H21A 0.95(2) . no C21 H21B 0.96(2) . no C22 N22 1.487(2) . no C22 H22A 0.95(3) . no C22 H22B 0.95(3) . no N22 H22D 0.87(2) . no N22 H22E 0.90(2) . no S1 O12 1.4526(13) . no S1 O11 1.4549(11) . no S1 O13 1.4549(13) . no S1 S2 2.1287(5) . no S2 O15 1.4510(14) . no S2 O16 1.4549(14) . no S2 O14 1.4558(13) . no O3W O3W 1.109(11) 3_677 no 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 N21 87.85(5) . . no O1 Co N11 177.42(5) . . no N21 Co N11 92.59(5) . . no O1 Co N12 91.65(5) . . no N21 Co N12 90.87(5) . . no N11 Co N12 85.80(5) . . no O1 Co N1 83.45(5) . . no N21 Co N1 170.77(5) . . no N11 Co N1 96.24(5) . . no N12 Co N1 92.43(5) . . no O1 Co N22 89.18(5) . . no N21 Co N22 85.50(5) . . no N11 Co N22 93.39(5) . . no N12 Co N22 176.25(5) . . no N1 Co N22 91.30(5) . . no C1 O1 Co 114.66(9) . . no O2 C1 O1 124.37(13) . . no O2 C1 C2 121.53(13) . . no O1 C1 C2 114.10(12) . . no N1 C2 C1 115.19(12) . . no N1 C2 H2 121.6(15) . . no C1 C2 H2 123.1(15) . . no C2 N1 C3 119.29(13) . . no C2 N1 Co 112.59(10) . . no C3 N1 Co 128.12(10) . . no N1 C3 H3A 109.7(17) . . no N1 C3 H3B 109.7(17) . . no H3A C3 H3B 109(2) . . no N1 C3 H3C 104.9(17) . . no H3A C3 H3C 114(2) . . no H3B C3 H3C 109(2) . . no C11 N11 Co 109.97(9) . . no C11 N11 H11D 109.5(15) . . no Co N11 H11D 113.4(15) . . no C11 N11 H11E 110.1(16) . . no Co N11 H11E 109.7(15) . . no H11D N11 H11E 104(2) . . no N11 C11 C12 107.07(12) . . no N11 C11 H11A 105.8(15) . . no C12 C11 H11A 113.4(15) . . no N11 C11 H11B 111.9(16) . . no C12 C11 H11B 109.4(16) . . no H11A C11 H11B 109(2) . . no N12 C12 C11 107.15(12) . . no N12 C12 H12A 111.0(15) . . no C11 C12 H12A 111.8(15) . . no N12 C12 H12B 109.2(15) . . no C11 C12 H12B 112.7(16) . . no H12A C12 H12B 105(2) . . no C12 N12 Co 109.83(9) . . no C12 N12 H12D 110.9(17) . . no Co N12 H12D 109.1(17) . . no C12 N12 H12E 109.9(16) . . no Co N12 H12E 109.2(16) . . no H12D N12 H12E 108(2) . . no C21 N21 Co 110.16(9) . . no C21 N21 H21D 108.6(16) . . no Co N21 H21D 107.6(16) . . no C21 N21 H21E 109.2(15) . . no Co N21 H21E 116.6(15) . . no H21D N21 H21E 104(2) . . no N21 C21 C22 106.22(12) . . no N21 C21 H21A 108.8(15) . . no C22 C21 H21A 112.4(15) . . no N21 C21 H21B 107.9(15) . . no C22 C21 H21B 112.6(15) . . no H21A C21 H21B 109(2) . . no N22 C22 C21 106.77(12) . . no N22 C22 H22A 107.2(15) . . no C21 C22 H22A 113.8(15) . . no N22 C22 H22B 107.4(15) . . no C21 C22 H22B 111.2(15) . . no H22A C22 H22B 110(2) . . no C22 N22 Co 109.51(9) . . no C22 N22 H22D 103.1(15) . . no Co N22 H22D 112.6(16) . . no C22 N22 H22E 109.1(15) . . no Co N22 H22E 110.7(15) . . no H22D N22 H22E 111(2) . . no O12 S1 O11 114.02(7) . . no O12 S1 O13 113.15(8) . . no O11 S1 O13 114.77(7) . . no O12 S1 S2 103.54(6) . . no O11 S1 S2 104.75(5) . . no O13 S1 S2 105.09(6) . . no O15 S2 O16 113.77(9) . . no O15 S2 O14 114.06(8) . . no O16 S2 O14 114.19(9) . . no O15 S2 S1 106.73(6) . . no O16 S2 S1 103.22(6) . . no O14 S2 S1 103.34(5) . . no 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 N21 Co O1 C1 176.52(10) . . . . no N11 Co O1 C1 -83.7(11) . . . . no N12 Co O1 C1 -92.67(10) . . . . no N1 Co O1 C1 -0.42(10) . . . . no N22 Co O1 C1 90.99(10) . . . . no Co O1 C1 O2 180.00(11) . . . . no Co O1 C1 C2 -0.20(15) . . . . no O2 C1 C2 N1 -179.09(14) . . . . no O1 C1 C2 N1 1.10(19) . . . . no C1 C2 N1 C3 179.00(13) . . . . no C1 C2 N1 Co -1.40(16) . . . . no O1 Co N1 C2 1.04(11) . . . . no N21 Co N1 C2 -18.4(4) . . . . no N11 Co N1 C2 178.47(11) . . . . no N12 Co N1 C2 92.43(11) . . . . no N22 Co N1 C2 -87.98(11) . . . . no O1 Co N1 C3 -179.40(14) . . . . no N21 Co N1 C3 161.1(3) . . . . no N11 Co N1 C3 -1.97(14) . . . . no N12 Co N1 C3 -88.01(13) . . . . no N22 Co N1 C3 91.58(13) . . . . no O1 Co N11 C11 3.5(12) . . . . no N21 Co N11 C11 103.15(11) . . . . no N12 Co N11 C11 12.46(11) . . . . no N1 Co N11 C11 -79.52(11) . . . . no N22 Co N11 C11 -171.21(11) . . . . no Co N11 C11 C12 -36.60(15) . . . . no N11 C11 C12 N12 48.56(16) . . . . no C11 C12 N12 Co -38.75(14) . . . . no O1 Co N12 C12 -165.40(10) . . . . no N21 Co N12 C12 -77.53(10) . . . . no N11 Co N12 C12 15.00(10) . . . . no N1 Co N12 C12 111.09(10) . . . . no N22 Co N12 C12 -62.7(8) . . . . no O1 Co N21 C21 -103.22(10) . . . . no N11 Co N21 C21 79.32(10) . . . . no N12 Co N21 C21 165.16(10) . . . . no N1 Co N21 C21 -83.9(3) . . . . no N22 Co N21 C21 -13.87(10) . . . . no Co N21 C21 C22 38.67(13) . . . . no N21 C21 C22 N22 -50.30(15) . . . . no C21 C22 N22 Co 39.54(14) . . . . no O1 Co N22 C22 73.17(10) . . . . no N21 Co N22 C22 -14.73(10) . . . . no N11 Co N22 C22 -107.06(10) . . . . no N12 Co N22 C22 -29.6(8) . . . . no N1 Co N22 C22 156.60(10) . . . . no O12 S1 S2 O15 178.86(8) . . . . no O11 S1 S2 O15 59.11(8) . . . . no O13 S1 S2 O15 -62.21(8) . . . . no O12 S1 S2 O16 58.67(9) . . . . no O11 S1 S2 O16 -61.09(9) . . . . no O13 S1 S2 O16 177.59(9) . . . . no O12 S1 S2 O14 -60.56(8) . . . . no O11 S1 S2 O14 179.69(8) . . . . no O13 S1 S2 O14 58.37(8) . . . . no _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 35.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.564 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.126 #===END data_22 _database_code_CSD 180575 _audit_creation_method 'SHELXL-97 and manual editing' _chemical_name_systematic ; (LAMBDA-S,DELTA-R)-[(en)2Co{O2CCH(CH(CO2Et)2)NH2}](ClO)2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H30 Co N5 O6, 2 Cl O4' _chemical_formula_sum 'C13 H30 Cl2 Co N5 O14' _chemical_formula_weight 610.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 23.9830(2) _cell_length_b 8.8240(6) _cell_length_c 22.0290(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4661.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 207 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 1.045 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.661 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 122(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_reflns_number 83343 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 35.00 _reflns_number_total 17496 _reflns_number_gt 15541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DIRAX (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep II (Johnson, 1976)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0483P)^2^+6.0994P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _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 0.669(9) _refine_ls_number_reflns 17496 _refine_ls_number_parameters 812 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.010 _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 Co Co -0.144551(11) -0.02990(3) 0.415462(14) 0.00720(5) Uani 1 1 d . . . N11 N -0.10638(8) -0.2255(2) 0.41800(11) 0.0109(3) Uani 1 1 d D . . H11D H -0.1022(13) -0.256(4) 0.4546(9) 0.013 Uiso 1 1 d D . . H11E H -0.0731(9) -0.218(4) 0.4034(16) 0.013 Uiso 1 1 d D . . C11 C -0.13919(10) -0.3397(3) 0.38309(12) 0.0133(4) Uani 1 1 d . . . H11A H -0.1706(14) -0.376(4) 0.4083(18) 0.016 Uiso 1 1 d . . . H11B H -0.1175(15) -0.419(4) 0.3709(18) 0.016 Uiso 1 1 d . . . C12 C -0.16276(9) -0.2609(3) 0.32772(12) 0.0124(4) Uani 1 1 d . . . H12A H -0.1355(15) -0.235(4) 0.2997(17) 0.015 Uiso 1 1 d . . . H12B H -0.1925(15) -0.327(4) 0.3079(17) 0.015 Uiso 1 1 d . . . N12 N -0.18774(8) -0.1165(2) 0.34867(9) 0.0102(3) Uani 1 1 d D . . H12D H -0.1879(14) -0.052(3) 0.3194(13) 0.012 Uiso 1 1 d D . . H12E H -0.2207(9) -0.138(4) 0.3626(16) 0.012 Uiso 1 1 d D . . N21 N -0.20009(8) -0.0943(2) 0.47518(10) 0.0110(3) Uani 1 1 d D . . H21D H -0.1962(14) -0.182(2) 0.4914(16) 0.013 Uiso 1 1 d D . . H21E H -0.2341(8) -0.098(4) 0.4626(17) 0.013 Uiso 1 1 d D . . C21 C -0.19575(9) 0.0098(3) 0.52819(12) 0.0138(4) Uani 1 1 d . . . H21A H -0.2148(15) -0.041(4) 0.5615(18) 0.017 Uiso 1 1 d . . . H21B H -0.2115(14) 0.106(4) 0.5163(18) 0.017 Uiso 1 1 d . . . C22 C -0.13413(10) 0.0199(3) 0.54314(12) 0.0132(4) Uani 1 1 d . . . H22A H -0.1266(15) 0.087(5) 0.5725(17) 0.016 Uiso 1 1 d . . . H22B H -0.1198(14) -0.079(4) 0.5548(18) 0.016 Uiso 1 1 d . . . N22 N -0.10513(8) 0.0584(2) 0.48534(10) 0.0108(3) Uani 1 1 d D . . H22D H -0.1043(14) 0.156(2) 0.4843(17) 0.013 Uiso 1 1 d D . . H22E H -0.0712(8) 0.027(4) 0.4883(17) 0.013 Uiso 1 1 d D . . O1 O -0.18516(6) 0.15233(19) 0.40264(8) 0.0100(3) Uani 1 1 d . . . C1 C -0.16323(8) 0.2467(3) 0.36495(11) 0.0090(4) Uani 1 1 d . . . O2 O -0.18799(6) 0.3571(2) 0.34358(9) 0.0123(3) Uani 1 1 d . . . C2 C -0.10226(8) 0.2182(2) 0.34754(10) 0.0081(4) Uani 1 1 d . . . H2 H -0.0808(13) 0.276(4) 0.3736(16) 0.010 Uiso 1 1 d . . . N1 N -0.08851(8) 0.0568(2) 0.36051(10) 0.0096(3) Uani 1 1 d D . . H1D H -0.0909(14) 0.006(4) 0.3274(11) 0.011 Uiso 1 1 d D . . H1E H -0.0542(8) 0.054(4) 0.3726(16) 0.011 Uiso 1 1 d D . . C3 C -0.09085(9) 0.2644(3) 0.28154(11) 0.0107(4) Uani 1 1 d . . . H3 H -0.0969(14) 0.359(4) 0.2766(17) 0.013 Uiso 1 1 d . . . C4 C -0.13060(9) 0.1854(3) 0.23839(11) 0.0141(4) Uani 1 1 d . . . O3 O -0.14780(8) 0.0584(3) 0.24687(10) 0.0214(4) Uani 1 1 d . . . O4 O -0.14280(8) 0.2686(2) 0.19033(10) 0.0199(4) Uani 1 1 d . . . C5 C -0.17343(14) 0.1892(4) 0.14202(15) 0.0278(6) Uani 1 1 d . . . H5A H -0.2088(19) 0.176(5) 0.161(2) 0.033 Uiso 1 1 d . . . H5B H -0.1475(18) 0.097(6) 0.127(2) 0.033 Uiso 1 1 d . . . C6 C -0.18231(14) 0.3001(5) 0.09173(15) 0.0293(7) Uani 1 1 d . . . H6A H -0.201(2) 0.249(6) 0.058(2) 0.044 Uiso 1 1 d . . . H6B H -0.146(2) 0.339(6) 0.078(2) 0.044 Uiso 1 1 d . . . H6C H -0.2073(19) 0.392(6) 0.104(2) 0.044 Uiso 1 1 d . . . C7 C -0.03077(9) 0.2249(3) 0.26419(12) 0.0134(4) Uani 1 1 d . . . O5 O 0.00918(8) 0.2541(3) 0.29506(10) 0.0227(4) Uani 1 1 d . . . O6 O -0.02976(8) 0.1520(3) 0.21198(10) 0.0223(4) Uani 1 1 d . . . C8 C 0.02303(12) 0.0860(4) 0.19165(17) 0.0274(7) Uani 1 1 d . . . H8A H 0.0406(18) 0.031(5) 0.227(2) 0.033 Uiso 1 1 d . . . H8B H 0.0416(18) 0.171(5) 0.172(2) 0.033 Uiso 1 1 d . . . C9 C 0.00833(15) -0.0303(4) 0.14450(16) 0.0275(6) Uani 1 1 d . . . H9A H 0.045(2) -0.078(6) 0.133(2) 0.041 Uiso 1 1 d . . . H9B H -0.007(2) 0.018(6) 0.108(2) 0.041 Uiso 1 1 d . . . H9C H -0.020(2) -0.109(6) 0.161(2) 0.041 Uiso 1 1 d . . . Co_1 Co 0.156340(11) 0.52455(3) 0.335822(14) 0.00709(5) Uani 1 1 d . . . N11_1 N 0.11812(8) 0.7195(2) 0.33407(10) 0.0104(3) Uani 1 1 d D . . H11D_1 H 0.0865(9) 0.711(4) 0.3518(15) 0.012 Uiso 1 1 d D . . H11E_1 H 0.1128(14) 0.753(4) 0.2980(10) 0.012 Uiso 1 1 d D . . C11_1 C 0.15166(10) 0.8335(3) 0.36774(13) 0.0138(4) Uani 1 1 d . . . H11A_1 H 0.1298(15) 0.924(5) 0.3766(18) 0.017 Uiso 1 1 d . . . H11B_1 H 0.1795(14) 0.863(4) 0.3423(18) 0.017 Uiso 1 1 d . . . C12_1 C 0.17511(10) 0.7567(3) 0.42328(12) 0.0132(4) Uani 1 1 d . . . H12A_1 H 0.2044(14) 0.820(4) 0.4407(17) 0.016 Uiso 1 1 d . . . H12B_1 H 0.1488(14) 0.739(4) 0.4549(18) 0.016 Uiso 1 1 d . . . N12_1 N 0.19990(8) 0.6114(2) 0.40250(10) 0.0105(3) Uani 1 1 d D . . H12D_1 H 0.2014(14) 0.549(3) 0.4321(12) 0.013 Uiso 1 1 d D . . H12E_1 H 0.2338(8) 0.617(4) 0.3904(16) 0.013 Uiso 1 1 d D . . N21_1 N 0.21071(8) 0.5911(2) 0.27500(10) 0.0114(3) Uani 1 1 d D . . H21D_1 H 0.2438(9) 0.590(4) 0.2897(16) 0.014 Uiso 1 1 d D . . H21E_1 H 0.2043(14) 0.683(2) 0.2642(17) 0.014 Uiso 1 1 d D . . C21_1 C 0.20483(10) 0.4921(3) 0.22062(12) 0.0141(4) Uani 1 1 d . . . H21A_1 H 0.2201(14) 0.400(5) 0.2296(18) 0.017 Uiso 1 1 d . . . H21B_1 H 0.2249(14) 0.518(4) 0.1856(18) 0.017 Uiso 1 1 d . . . C22_1 C 0.14335(10) 0.4805(3) 0.20811(12) 0.0134(4) Uani 1 1 d . . . H22A_1 H 0.1293(15) 0.567(4) 0.1956(18) 0.016 Uiso 1 1 d . . . H22B_1 H 0.1328(14) 0.405(4) 0.1743(18) 0.016 Uiso 1 1 d . . . N22_1 N 0.11633(8) 0.4353(2) 0.26636(10) 0.0101(3) Uani 1 1 d D . . H22D_1 H 0.1178(14) 0.340(2) 0.2735(17) 0.012 Uiso 1 1 d D . . H22E_1 H 0.0820(8) 0.461(4) 0.2639(18) 0.012 Uiso 1 1 d D . . O1_1 O 0.19725(6) 0.34243(19) 0.34773(8) 0.0101(3) Uani 1 1 d . . . C1_1 C 0.17469(8) 0.2457(3) 0.38389(11) 0.0094(4) Uani 1 1 d . . . O2_1 O 0.19935(7) 0.13416(19) 0.40461(9) 0.0113(3) Uani 1 1 d . . . C2_1 C 0.11352(8) 0.2734(3) 0.40049(11) 0.0086(4) Uani 1 1 d . . . H2_1 H 0.0920(13) 0.219(4) 0.3728(16) 0.010 Uiso 1 1 d . . . N1_1 N 0.10110(8) 0.4372(2) 0.39137(10) 0.0093(3) Uani 1 1 d D . . H1D_1 H 0.1023(14) 0.481(4) 0.4261(10) 0.011 Uiso 1 1 d D . . H1E_1 H 0.0691(9) 0.451(4) 0.3757(16) 0.011 Uiso 1 1 d D . . C3_1 C 0.10091(9) 0.2173(3) 0.46509(11) 0.0107(4) Uani 1 1 d . . . H3_1 H 0.1028(13) 0.103(4) 0.4629(17) 0.013 Uiso 1 1 d . . . C4_1 C 0.04195(9) 0.2633(3) 0.48357(12) 0.0120(4) Uani 1 1 d . . . O3_1 O 0.00132(7) 0.2372(3) 0.45246(10) 0.0206(4) Uani 1 1 d . . . O4_1 O 0.04171(7) 0.3374(2) 0.53560(9) 0.0175(4) Uani 1 1 d . . . C5_1 C -0.01148(11) 0.4039(4) 0.55509(14) 0.0207(5) Uani 1 1 d . . . H5A_1 H -0.0358(17) 0.320(5) 0.5681(18) 0.025 Uiso 1 1 d . . . H5B_1 H -0.0292(16) 0.453(5) 0.519(2) 0.025 Uiso 1 1 d . . . C6_1 C 0.00120(15) 0.5068(5) 0.60744(15) 0.0280(7) Uani 1 1 d . . . H6A_1 H -0.033(2) 0.554(6) 0.621(2) 0.042 Uiso 1 1 d . . . H6B_1 H 0.0275(19) 0.589(6) 0.592(2) 0.042 Uiso 1 1 d . . . H6C_1 H 0.019(2) 0.456(6) 0.640(2) 0.042 Uiso 1 1 d . . . C7_1 C 0.14350(9) 0.2805(3) 0.50951(11) 0.0119(4) Uani 1 1 d . . . O5_1 O 0.16372(8) 0.4056(3) 0.50372(10) 0.0188(4) Uani 1 1 d . . . O6_1 O 0.15551(8) 0.1833(2) 0.55354(9) 0.0173(4) Uani 1 1 d . . . C8_1 C 0.19056(11) 0.2408(4) 0.60296(13) 0.0207(5) Uani 1 1 d . . . H8A_1 H 0.2169(16) 0.324(5) 0.586(2) 0.025 Uiso 1 1 d . . . H8B_1 H 0.2106(16) 0.154(5) 0.6183(19) 0.025 Uiso 1 1 d . . . C9_1 C 0.15426(14) 0.3038(5) 0.65241(15) 0.0284(6) Uani 1 1 d . . . H9A_1 H 0.1753(19) 0.336(5) 0.686(2) 0.043 Uiso 1 1 d . . . H9B_1 H 0.131(2) 0.233(5) 0.670(2) 0.043 Uiso 1 1 d . . . H9C_1 H 0.134(2) 0.383(6) 0.638(2) 0.043 Uiso 1 1 d . . . Cl1_1 Cl -0.01532(2) -0.32224(6) 0.27749(3) 0.01181(9) Uani 1 1 d . . . O11_1 O -0.06125(8) -0.3938(2) 0.24697(10) 0.0189(4) Uani 1 1 d . . . O12_1 O -0.02910(8) -0.1669(2) 0.29127(12) 0.0237(4) Uani 1 1 d . . . O13_1 O 0.03360(7) -0.3265(3) 0.23967(9) 0.0181(4) Uani 1 1 d . . . O14_1 O -0.00360(9) -0.4006(3) 0.33403(11) 0.0255(4) Uani 1 1 d . . . Cl2_1 Cl 0.33540(2) 0.52707(7) 0.52559(3) 0.01450(10) Uani 1 1 d . . . O21_1 O 0.37229(9) 0.5998(3) 0.48298(11) 0.0230(4) Uani 1 1 d . . . O22_1 O 0.35659(13) 0.3775(3) 0.53791(14) 0.0372(6) Uani 1 1 d . . . O23_1 O 0.33307(12) 0.6125(3) 0.58076(11) 0.0322(5) Uani 1 1 d . . . O24_1 O 0.28127(10) 0.5129(5) 0.49903(14) 0.0558(10) Uani 1 1 d . . . Cl3_1 Cl -0.32339(2) -0.02522(8) 0.22436(3) 0.01575(11) Uani 1 1 d . . . O31_1 O -0.36017(8) -0.0951(2) 0.26775(10) 0.0204(4) Uani 1 1 d . . . O32_1 O -0.34247(14) 0.1265(3) 0.21291(14) 0.0420(7) Uani 1 1 d . . . O33_1 O -0.32384(15) -0.1089(3) 0.16891(12) 0.0422(7) Uani 1 1 d . . . O34_1 O -0.26904(11) -0.0203(6) 0.24920(16) 0.0802(16) Uani 1 1 d . . . Cl4_1 Cl 0.02826(2) 0.81053(7) 0.48088(3) 0.01307(10) Uani 1 1 d . . . O41_1 O -0.02292(7) 0.8101(3) 0.51550(10) 0.0196(4) Uani 1 1 d . . . O42_1 O 0.07187(8) 0.8832(3) 0.51490(10) 0.0218(4) Uani 1 1 d . . . O43_1 O 0.04381(9) 0.6572(2) 0.46697(12) 0.0264(5) Uani 1 1 d . . . O44_1 O 0.01892(10) 0.8922(3) 0.42442(11) 0.0282(5) 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 0.00585(10) 0.00712(12) 0.00862(13) 0.00032(11) -0.00002(9) -0.00039(9) N11 0.0110(7) 0.0096(8) 0.0120(9) -0.0010(7) -0.0020(7) -0.0004(6) C11 0.0170(10) 0.0083(10) 0.0145(11) -0.0033(8) -0.0012(8) -0.0015(7) C12 0.0138(9) 0.0116(9) 0.0119(11) -0.0043(8) 0.0007(7) 0.0001(7) N12 0.0088(7) 0.0119(8) 0.0098(9) 0.0000(7) 0.0003(6) -0.0012(6) N21 0.0100(7) 0.0121(9) 0.0110(9) 0.0017(7) -0.0009(6) -0.0020(6) C21 0.0105(8) 0.0186(11) 0.0124(10) 0.0015(9) 0.0022(7) -0.0004(7) C22 0.0131(9) 0.0166(11) 0.0100(10) -0.0013(9) -0.0004(7) -0.0011(8) N22 0.0095(7) 0.0102(8) 0.0127(9) -0.0007(7) -0.0004(6) 0.0007(6) O1 0.0077(6) 0.0097(7) 0.0126(8) 0.0004(6) 0.0004(5) 0.0004(5) C1 0.0072(7) 0.0110(9) 0.0087(10) -0.0014(7) -0.0022(6) -0.0006(6) O2 0.0099(6) 0.0101(7) 0.0169(9) -0.0004(6) -0.0016(6) 0.0024(5) C2 0.0067(7) 0.0069(8) 0.0108(10) -0.0004(7) 0.0003(6) -0.0001(6) N1 0.0084(7) 0.0086(8) 0.0118(9) -0.0001(7) 0.0018(6) 0.0016(6) C3 0.0086(8) 0.0114(9) 0.0122(10) 0.0010(8) 0.0005(7) -0.0006(7) C4 0.0102(8) 0.0209(11) 0.0113(10) 0.0022(9) -0.0006(7) -0.0012(8) O3 0.0220(9) 0.0268(11) 0.0154(9) 0.0045(8) -0.0014(7) -0.0120(8) O4 0.0220(9) 0.0228(10) 0.0148(9) 0.0059(8) -0.0056(7) -0.0030(7) C5 0.0309(14) 0.0338(16) 0.0188(13) 0.0036(12) -0.0091(11) -0.0080(12) C6 0.0293(14) 0.0416(19) 0.0171(13) 0.0067(13) -0.0035(11) 0.0025(13) C7 0.0101(8) 0.0156(10) 0.0147(11) 0.0047(9) 0.0030(7) -0.0021(7) O5 0.0111(7) 0.0338(12) 0.0233(11) -0.0047(9) 0.0000(7) -0.0035(7) O6 0.0130(8) 0.0332(12) 0.0206(10) -0.0086(9) 0.0018(7) 0.0022(7) C8 0.0151(11) 0.0339(17) 0.0333(18) -0.0062(14) 0.0106(10) 0.0036(11) C9 0.0333(15) 0.0303(16) 0.0190(14) -0.0028(13) 0.0075(11) 0.0062(12) Co_1 0.00573(10) 0.00723(12) 0.00832(13) 0.00004(12) -0.00017(9) -0.00048(9) N11_1 0.0123(7) 0.0082(8) 0.0106(9) -0.0007(7) -0.0014(7) 0.0008(5) C11_1 0.0161(10) 0.0094(10) 0.0158(12) -0.0024(9) -0.0034(8) -0.0018(7) C12_1 0.0158(9) 0.0132(10) 0.0106(11) -0.0020(8) -0.0024(8) -0.0008(7) N12_1 0.0102(7) 0.0109(8) 0.0103(9) 0.0009(7) -0.0006(6) -0.0005(6) N21_1 0.0099(7) 0.0120(9) 0.0121(9) -0.0006(8) -0.0008(6) -0.0010(6) C21_1 0.0122(9) 0.0179(11) 0.0121(11) -0.0034(9) 0.0022(7) 0.0006(7) C22_1 0.0152(9) 0.0153(11) 0.0096(10) 0.0006(9) -0.0011(8) 0.0002(8) N22_1 0.0086(7) 0.0090(8) 0.0128(9) 0.0011(7) -0.0010(6) 0.0009(6) O1_1 0.0079(6) 0.0095(7) 0.0130(8) 0.0004(6) 0.0003(5) 0.0018(5) C1_1 0.0071(7) 0.0095(9) 0.0116(10) -0.0020(7) -0.0013(6) 0.0004(6) O2_1 0.0107(6) 0.0089(7) 0.0142(8) 0.0017(6) -0.0016(5) 0.0023(5) C2_1 0.0076(7) 0.0082(8) 0.0099(9) 0.0002(7) -0.0003(6) -0.0002(6) N1_1 0.0084(7) 0.0077(8) 0.0116(9) 0.0006(7) 0.0006(6) 0.0021(6) C3_1 0.0094(8) 0.0110(9) 0.0115(10) 0.0016(8) -0.0005(7) -0.0015(6) C4_1 0.0097(8) 0.0140(10) 0.0123(10) 0.0016(8) 0.0028(7) -0.0042(7) O3_1 0.0100(7) 0.0302(11) 0.0215(10) -0.0027(9) -0.0006(6) -0.0025(7) O4_1 0.0123(7) 0.0240(10) 0.0162(9) -0.0024(8) 0.0006(6) 0.0035(6) C5_1 0.0140(10) 0.0266(14) 0.0213(13) 0.0017(11) 0.0055(9) 0.0050(9) C6_1 0.0315(15) 0.0359(18) 0.0168(13) 0.0016(12) 0.0049(11) 0.0137(13) C7_1 0.0100(8) 0.0150(10) 0.0107(10) 0.0011(8) 0.0017(7) -0.0001(7) O5_1 0.0190(8) 0.0236(10) 0.0139(9) 0.0003(8) -0.0034(7) -0.0098(7) O6_1 0.0207(8) 0.0193(9) 0.0117(8) 0.0037(7) -0.0041(6) 0.0019(7) C8_1 0.0176(10) 0.0309(15) 0.0136(11) -0.0008(10) -0.0045(8) 0.0015(10) C9_1 0.0276(14) 0.0393(18) 0.0183(14) -0.0070(13) 0.0009(11) -0.0045(13) Cl1_1 0.01038(19) 0.0127(2) 0.0124(2) -0.00234(19) -0.00062(16) 0.00202(16) O11_1 0.0141(7) 0.0217(9) 0.0208(10) -0.0043(8) -0.0054(6) -0.0043(6) O12_1 0.0209(9) 0.0138(9) 0.0363(13) -0.0089(9) 0.0063(8) 0.0024(7) O13_1 0.0114(7) 0.0281(11) 0.0149(9) -0.0032(8) 0.0031(6) 0.0043(7) O14_1 0.0240(9) 0.0337(12) 0.0188(10) 0.0098(10) -0.0039(8) 0.0004(8) Cl2_1 0.0150(2) 0.0159(2) 0.0126(3) -0.0018(2) -0.00202(18) 0.00018(19) O21_1 0.0274(10) 0.0208(10) 0.0210(10) 0.0039(9) 0.0009(8) -0.0075(8) O22_1 0.0699(19) 0.0133(11) 0.0284(14) 0.0049(10) 0.0104(12) 0.0077(11) O23_1 0.0602(16) 0.0220(12) 0.0145(11) -0.0077(9) -0.0027(10) 0.0081(11) O24_1 0.0117(9) 0.125(3) 0.0303(15) -0.0070(17) -0.0051(9) -0.0089(13) Cl3_1 0.0148(2) 0.0211(3) 0.0114(3) 0.0014(2) -0.00126(18) -0.00096(19) O31_1 0.0245(9) 0.0195(9) 0.0172(10) 0.0055(8) 0.0003(7) -0.0063(7) O32_1 0.087(2) 0.0117(11) 0.0271(14) 0.0027(10) 0.0113(14) 0.0007(11) O33_1 0.083(2) 0.0258(13) 0.0176(13) -0.0044(10) 0.0095(12) 0.0101(13) O34_1 0.0149(11) 0.181(5) 0.0445(19) 0.040(2) -0.0101(11) -0.0211(18) Cl4_1 0.0134(2) 0.0120(2) 0.0138(2) -0.00224(19) 0.00015(18) 0.00142(17) O41_1 0.0114(7) 0.0264(10) 0.0209(10) -0.0040(8) 0.0025(6) 0.0051(7) O42_1 0.0160(8) 0.0253(10) 0.0241(11) -0.0054(8) -0.0047(7) -0.0065(7) O43_1 0.0264(10) 0.0132(9) 0.0398(14) -0.0077(9) 0.0094(9) 0.0037(7) O44_1 0.0332(11) 0.0329(12) 0.0185(11) 0.0102(9) -0.0037(9) -0.0026(9) _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 1.9011(17) . yes Co N11 1.954(2) . yes Co N12 1.955(2) . yes Co N21 1.956(2) . yes Co N1 1.964(2) . yes Co N22 1.967(2) . yes N11 C11 1.492(3) . no N11 H11D 0.855(17) . no N11 H11E 0.862(17) . no C11 C12 1.514(4) . no C11 H11A 0.99(4) . no C11 H11B 0.91(4) . no C12 N12 1.482(3) . no C12 H12A 0.93(4) . no C12 H12B 1.02(4) . no N12 H12D 0.859(17) . no N12 H12E 0.871(17) . no N21 C21 1.489(4) . no N21 H21D 0.862(17) . no N21 H21E 0.863(17) . no C21 C22 1.517(3) . no C21 H21A 0.98(4) . no C21 H21B 0.97(4) . no C22 N22 1.490(3) . no C22 H22A 0.90(4) . no C22 H22B 0.97(4) . no N22 H22D 0.864(17) . no N22 H22E 0.861(17) . no O1 C1 1.288(3) . yes C1 O2 1.234(3) . yes C1 C2 1.532(3) . yes C2 N1 1.489(3) . yes C2 C3 1.534(3) . no C2 H2 0.92(3) . no N1 H1D 0.858(17) . no N1 H1E 0.866(17) . no C3 C4 1.516(3) . no C3 C7 1.531(3) . no C3 H3 0.85(4) . no C4 O3 1.209(3) . no C4 O4 1.321(3) . no O4 C5 1.471(4) . no C5 C6 1.493(5) . no C5 H5A 0.95(5) . no C5 H5B 1.08(5) . no C6 H6A 0.98(5) . no C6 H6B 0.98(5) . no C6 H6C 1.05(5) . no C7 O5 1.203(3) . no C7 O6 1.318(3) . no O6 C8 1.464(3) . no C8 C9 1.502(5) . no C8 H8A 1.00(5) . no C8 H8B 0.97(5) . no C9 H9A 1.00(5) . no C9 H9B 0.98(5) . no C9 H9C 1.04(5) . no Co_1 O1_1 1.9010(17) . yes Co_1 N11_1 1.9495(19) . yes Co_1 N12_1 1.958(2) . yes Co_1 N21_1 1.960(2) . yes Co_1 N1_1 1.961(2) . yes Co_1 N22_1 1.971(2) . yes N11_1 C11_1 1.486(3) . no N11_1 H11D_1 0.855(16) . no N11_1 H11E_1 0.858(17) . no C11_1 C12_1 1.507(4) . no C11_1 H11A_1 0.98(4) . no C11_1 H11B_1 0.91(4) . no C12_1 N12_1 1.486(3) . no C12_1 H12A_1 0.98(4) . no C12_1 H12B_1 0.95(4) . no N12_1 H12D_1 0.852(17) . no N12_1 H12E_1 0.857(17) . no N21_1 C21_1 1.489(3) . no N21_1 H21D_1 0.857(17) . no N21_1 H21E_1 0.859(17) . no C21_1 C22_1 1.504(3) . no C21_1 H21A_1 0.91(4) . no C21_1 H21B_1 0.94(4) . no C22_1 N22_1 1.492(3) . no C22_1 H22A_1 0.88(4) . no C22_1 H22B_1 1.03(4) . no N22_1 H22D_1 0.854(17) . no N22_1 H22E_1 0.854(17) . no O1_1 C1_1 1.287(3) . yes C1_1 O2_1 1.236(3) . yes C1_1 C2_1 1.532(3) . yes C2_1 N1_1 1.489(3) . yes C2_1 C3_1 1.537(3) . no C2_1 H2_1 0.93(4) . no N1_1 H1D_1 0.856(17) . no N1_1 H1E_1 0.851(17) . no C3_1 C7_1 1.520(3) . no C3_1 C4_1 1.526(3) . no C3_1 H3_1 1.01(4) . no C4_1 O3_1 1.213(3) . no C4_1 O4_1 1.320(3) . no O4_1 C5_1 1.468(3) . no C5_1 C6_1 1.499(5) . no C5_1 H5A_1 0.99(4) . no C5_1 H5B_1 1.01(4) . no C6_1 H6A_1 0.97(5) . no C6_1 H6B_1 1.02(5) . no C6_1 H6C_1 0.95(5) . no C7_1 O5_1 1.213(3) . no C7_1 O6_1 1.327(3) . no O6_1 C8_1 1.466(3) . no C8_1 C9_1 1.501(4) . no C8_1 H8A_1 1.03(4) . no C8_1 H8B_1 0.97(4) . no C9_1 H9A_1 0.93(5) . no C9_1 H9B_1 0.93(5) . no C9_1 H9C_1 0.91(5) . no Cl1_1 O11_1 1.4370(19) . no Cl1_1 O13_1 1.4394(19) . no Cl1_1 O12_1 1.443(2) . no Cl1_1 O14_1 1.452(2) . no Cl2_1 O24_1 1.430(2) . no Cl2_1 O23_1 1.431(2) . no Cl2_1 O22_1 1.440(3) . no Cl2_1 O21_1 1.441(2) . no Cl3_1 O34_1 1.414(3) . no Cl3_1 O33_1 1.427(3) . no Cl3_1 O32_1 1.437(3) . no Cl3_1 O31_1 1.439(2) . no Cl4_1 O43_1 1.437(2) . no Cl4_1 O42_1 1.438(2) . no Cl4_1 O41_1 1.4453(19) . no Cl4_1 O44_1 1.455(2) . no 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 N11 172.37(9) . . no O1 Co N12 86.98(8) . . no N11 Co N12 85.67(9) . . no O1 Co N21 89.81(8) . . no N11 Co N21 92.48(9) . . no N12 Co N21 91.83(8) . . no O1 Co N1 85.95(8) . . no N11 Co N1 92.36(8) . . no N12 Co N1 92.92(9) . . no N21 Co N1 173.46(9) . . no O1 Co N22 91.57(8) . . no N11 Co N22 95.87(9) . . no N12 Co N22 176.69(8) . . no N21 Co N22 85.18(9) . . no N1 Co N22 89.95(9) . . no C11 N11 Co 109.56(15) . . no C11 N11 H11D 110(2) . . no Co N11 H11D 111(2) . . no C11 N11 H11E 110(2) . . no Co N11 H11E 111(2) . . no H11D N11 H11E 105(3) . . no N11 C11 C12 107.6(2) . . no N11 C11 H11A 109(2) . . no C12 C11 H11A 109(2) . . no N11 C11 H11B 112(2) . . no C12 C11 H11B 109(3) . . no H11A C11 H11B 111(3) . . no N12 C12 C11 107.2(2) . . no N12 C12 H12A 106(2) . . no C11 C12 H12A 113(2) . . no N12 C12 H12B 110(2) . . no C11 C12 H12B 110(2) . . no H12A C12 H12B 110(3) . . no C12 N12 Co 110.88(14) . . no C12 N12 H12D 110(2) . . no Co N12 H12D 108(2) . . no C12 N12 H12E 107(2) . . no Co N12 H12E 108(2) . . no H12D N12 H12E 114(3) . . no C21 N21 Co 107.50(15) . . no C21 N21 H21D 103(3) . . no Co N21 H21D 118(2) . . no C21 N21 H21E 110(3) . . no Co N21 H21E 116(3) . . no H21D N21 H21E 102(3) . . no N21 C21 C22 105.93(19) . . no N21 C21 H21A 106(2) . . no C22 C21 H21A 109(2) . . no N21 C21 H21B 108(2) . . no C22 C21 H21B 113(2) . . no H21A C21 H21B 115(3) . . no N22 C22 C21 106.4(2) . . no N22 C22 H22A 112(2) . . no C21 C22 H22A 113(2) . . no N22 C22 H22B 105(2) . . no C21 C22 H22B 111(2) . . no H22A C22 H22B 109(3) . . no C22 N22 Co 110.72(15) . . no C22 N22 H22D 105(2) . . no Co N22 H22D 113(2) . . no C22 N22 H22E 108(3) . . no Co N22 H22E 113(2) . . no H22D N22 H22E 107(3) . . no C1 O1 Co 115.67(14) . . no O2 C1 O1 124.03(19) . . no O2 C1 C2 119.5(2) . . no O1 C1 C2 116.43(19) . . no N1 C2 C1 108.66(17) . . no N1 C2 C3 113.34(18) . . no C1 C2 C3 111.33(17) . . no N1 C2 H2 106(2) . . no C1 C2 H2 107(2) . . no C3 C2 H2 110(2) . . no C2 N1 Co 109.83(13) . . no C2 N1 H1D 109(2) . . no Co N1 H1D 106(2) . . no C2 N1 H1E 107(2) . . no Co N1 H1E 117(2) . . no H1D N1 H1E 108(3) . . no C4 C3 C7 109.3(2) . . no C4 C3 C2 111.09(18) . . no C7 C3 C2 110.12(19) . . no C4 C3 H3 105(2) . . no C7 C3 H3 111(2) . . no C2 C3 H3 110(2) . . no O3 C4 O4 124.3(2) . . no O3 C4 C3 123.0(2) . . no O4 C4 C3 112.7(2) . . no C4 O4 C5 115.2(2) . . no O4 C5 C6 107.2(3) . . no O4 C5 H5A 101(3) . . no C6 C5 H5A 106(3) . . no O4 C5 H5B 107(2) . . no C6 C5 H5B 110(2) . . no H5A C5 H5B 124(4) . . no C5 C6 H6A 109(3) . . no C5 C6 H6B 110(3) . . no H6A C6 H6B 110(4) . . no C5 C6 H6C 114(3) . . no H6A C6 H6C 107(4) . . no H6B C6 H6C 108(4) . . no O5 C7 O6 125.7(2) . . no O5 C7 C3 124.1(2) . . no O6 C7 C3 110.3(2) . . no C7 O6 C8 118.5(2) . . no O6 C8 C9 106.3(3) . . no O6 C8 H8A 109(3) . . no C9 C8 H8A 107(3) . . no O6 C8 H8B 103(3) . . no C9 C8 H8B 109(3) . . no H8A C8 H8B 121(4) . . no C8 C9 H9A 105(3) . . no C8 C9 H9B 111(3) . . no H9A C9 H9B 108(4) . . no C8 C9 H9C 111(3) . . no H9A C9 H9C 112(4) . . no H9B C9 H9C 110(4) . . no O1_1 Co_1 N11_1 172.43(9) . . no O1_1 Co_1 N12_1 87.24(8) . . no N11_1 Co_1 N12_1 85.44(9) . . no O1_1 Co_1 N21_1 90.23(8) . . no N11_1 Co_1 N21_1 92.01(9) . . no N12_1 Co_1 N21_1 92.33(8) . . no O1_1 Co_1 N1_1 86.01(8) . . no N11_1 Co_1 N1_1 92.37(8) . . no N12_1 Co_1 N1_1 92.64(9) . . no N21_1 Co_1 N1_1 173.62(9) . . no O1_1 Co_1 N22_1 91.17(8) . . no N11_1 Co_1 N22_1 96.23(9) . . no N12_1 Co_1 N22_1 176.89(8) . . no N21_1 Co_1 N22_1 85.00(9) . . no N1_1 Co_1 N22_1 89.91(9) . . no C11_1 N11_1 Co_1 109.44(15) . . no C11_1 N11_1 H11D_1 108(2) . . no Co_1 N11_1 H11D_1 110(2) . . no C11_1 N11_1 H11E_1 108(2) . . no Co_1 N11_1 H11E_1 113(2) . . no H11D_1 N11_1 H11E_1 109(3) . . no N11_1 C11_1 C12_1 107.6(2) . . no N11_1 C11_1 H11A_1 111(2) . . no C12_1 C11_1 H11A_1 114(2) . . no N11_1 C11_1 H11B_1 106(2) . . no C12_1 C11_1 H11B_1 111(2) . . no H11A_1 C11_1 H11B_1 107(3) . . no N12_1 C12_1 C11_1 106.7(2) . . no N12_1 C12_1 H12A_1 109(2) . . no C11_1 C12_1 H12A_1 109(2) . . no N12_1 C12_1 H12B_1 110(2) . . no C11_1 C12_1 H12B_1 115(2) . . no H12A_1 C12_1 H12B_1 106(3) . . no C12_1 N12_1 Co_1 110.80(14) . . no C12_1 N12_1 H12D_1 110(2) . . no Co_1 N12_1 H12D_1 110(2) . . no C12_1 N12_1 H12E_1 115(2) . . no Co_1 N12_1 H12E_1 107(2) . . no H12D_1 N12_1 H12E_1 104(3) . . no C21_1 N21_1 Co_1 108.14(15) . . no C21_1 N21_1 H21D_1 113(2) . . no Co_1 N21_1 H21D_1 111(2) . . no C21_1 N21_1 H21E_1 108(3) . . no Co_1 N21_1 H21E_1 111(2) . . no H21D_1 N21_1 H21E_1 106(3) . . no N21_1 C21_1 C22_1 106.26(19) . . no N21_1 C21_1 H21A_1 108(3) . . no C22_1 C21_1 H21A_1 112(2) . . no N21_1 C21_1 H21B_1 118(2) . . no C22_1 C21_1 H21B_1 112(2) . . no H21A_1 C21_1 H21B_1 101(3) . . no N22_1 C22_1 C21_1 106.7(2) . . no N22_1 C22_1 H22A_1 110(3) . . no C21_1 C22_1 H22A_1 112(2) . . no N22_1 C22_1 H22B_1 110(2) . . no C21_1 C22_1 H22B_1 115(2) . . no H22A_1 C22_1 H22B_1 104(3) . . no C22_1 N22_1 Co_1 110.45(15) . . no C22_1 N22_1 H22D_1 114(3) . . no Co_1 N22_1 H22D_1 103(2) . . no C22_1 N22_1 H22E_1 107(3) . . no Co_1 N22_1 H22E_1 114(3) . . no H22D_1 N22_1 H22E_1 108(3) . . no C1_1 O1_1 Co_1 115.42(14) . . no O2_1 C1_1 O1_1 123.76(19) . . no O2_1 C1_1 C2_1 119.9(2) . . no O1_1 C1_1 C2_1 116.38(19) . . no N1_1 C2_1 C1_1 108.33(18) . . no N1_1 C2_1 C3_1 113.47(19) . . no C1_1 C2_1 C3_1 110.97(18) . . no N1_1 C2_1 H2_1 108(2) . . no C1_1 C2_1 H2_1 107(2) . . no C3_1 C2_1 H2_1 109(2) . . no C2_1 N1_1 Co_1 109.29(14) . . no C2_1 N1_1 H1D_1 108(2) . . no Co_1 N1_1 H1D_1 111(2) . . no C2_1 N1_1 H1E_1 112(2) . . no Co_1 N1_1 H1E_1 107(2) . . no H1D_1 N1_1 H1E_1 109(3) . . no C7_1 C3_1 C4_1 110.7(2) . . no C7_1 C3_1 C2_1 110.21(18) . . no C4_1 C3_1 C2_1 110.10(19) . . no C7_1 C3_1 H3_1 111.4(19) . . no C4_1 C3_1 H3_1 108.7(18) . . no C2_1 C3_1 H3_1 106(2) . . no O3_1 C4_1 O4_1 125.5(2) . . no O3_1 C4_1 C3_1 122.9(2) . . no O4_1 C4_1 C3_1 111.6(2) . . no C4_1 O4_1 C5_1 117.1(2) . . no O4_1 C5_1 C6_1 106.9(2) . . no O4_1 C5_1 H5A_1 107(2) . . no C6_1 C5_1 H5A_1 111(2) . . no O4_1 C5_1 H5B_1 108(2) . . no C6_1 C5_1 H5B_1 116(2) . . no H5A_1 C5_1 H5B_1 108(3) . . no C5_1 C6_1 H6A_1 109(3) . . no C5_1 C6_1 H6B_1 108(3) . . no H6A_1 C6_1 H6B_1 109(4) . . no C5_1 C6_1 H6C_1 113(3) . . no H6A_1 C6_1 H6C_1 110(4) . . no H6B_1 C6_1 H6C_1 108(4) . . no O5_1 C7_1 O6_1 125.4(2) . . no O5_1 C7_1 C3_1 122.4(2) . . no O6_1 C7_1 C3_1 112.3(2) . . no C7_1 O6_1 C8_1 116.3(2) . . no O6_1 C8_1 C9_1 109.5(2) . . no O6_1 C8_1 H8A_1 109(2) . . no C9_1 C8_1 H8A_1 111(2) . . no O6_1 C8_1 H8B_1 106(2) . . no C9_1 C8_1 H8B_1 109(2) . . no H8A_1 C8_1 H8B_1 112(3) . . no C8_1 C9_1 H9A_1 112(3) . . no C8_1 C9_1 H9B_1 114(3) . . no H9A_1 C9_1 H9B_1 102(4) . . no C8_1 C9_1 H9C_1 110(3) . . no H9A_1 C9_1 H9C_1 108(4) . . no H9B_1 C9_1 H9C_1 110(4) . . no O11_1 Cl1_1 O13_1 110.02(12) . . no O11_1 Cl1_1 O12_1 109.92(13) . . no O13_1 Cl1_1 O12_1 109.49(13) . . no O11_1 Cl1_1 O14_1 109.91(13) . . no O13_1 Cl1_1 O14_1 109.03(12) . . no O12_1 Cl1_1 O14_1 108.46(15) . . no O24_1 Cl2_1 O23_1 111.00(19) . . no O24_1 Cl2_1 O22_1 108.5(2) . . no O23_1 Cl2_1 O22_1 109.66(17) . . no O24_1 Cl2_1 O21_1 109.27(17) . . no O23_1 Cl2_1 O21_1 110.03(16) . . no O22_1 Cl2_1 O21_1 108.34(15) . . no O34_1 Cl3_1 O33_1 110.7(2) . . no O34_1 Cl3_1 O32_1 109.4(3) . . no O33_1 Cl3_1 O32_1 109.21(18) . . no O34_1 Cl3_1 O31_1 108.73(17) . . no O33_1 Cl3_1 O31_1 110.00(16) . . no O32_1 Cl3_1 O31_1 108.68(16) . . no O43_1 Cl4_1 O42_1 110.02(14) . . no O43_1 Cl4_1 O41_1 109.29(13) . . no O42_1 Cl4_1 O41_1 110.12(13) . . no O43_1 Cl4_1 O44_1 108.91(16) . . no O42_1 Cl4_1 O44_1 109.70(14) . . no O41_1 Cl4_1 O44_1 108.77(13) . . no 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 N11 C11 -31.0(7) . . . . no N12 Co N11 C11 -15.35(17) . . . . no N21 Co N11 C11 76.29(17) . . . . no N1 Co N11 C11 -108.10(17) . . . . no N22 Co N11 C11 161.71(17) . . . . no Co N11 C11 C12 38.3(2) . . . . no N11 C11 C12 N12 -47.3(2) . . . . no C11 C12 N12 Co 35.1(2) . . . . no O1 Co N12 C12 166.44(16) . . . . no N11 Co N12 C12 -11.50(16) . . . . no N21 Co N12 C12 -103.85(16) . . . . no N1 Co N12 C12 80.65(16) . . . . no N22 Co N12 C12 -129.5(15) . . . . no O1 Co N21 C21 -67.29(15) . . . . no N11 Co N21 C21 119.99(16) . . . . no N12 Co N21 C21 -154.27(15) . . . . no N1 Co N21 C21 -17.8(8) . . . . no N22 Co N21 C21 24.30(15) . . . . no Co N21 C21 C22 -47.7(2) . . . . no N21 C21 C22 N22 51.5(3) . . . . no C21 C22 N22 Co -31.9(2) . . . . no O1 Co N22 C22 94.37(16) . . . . no N11 Co N22 C22 -87.31(16) . . . . no N12 Co N22 C22 30.4(16) . . . . no N21 Co N22 C22 4.69(16) . . . . no N1 Co N22 C22 -179.68(16) . . . . no N11 Co O1 C1 -74.7(6) . . . . no N12 Co O1 C1 -90.41(17) . . . . no N21 Co O1 C1 177.75(17) . . . . no N1 Co O1 C1 2.73(17) . . . . no N22 Co O1 C1 92.57(17) . . . . no Co O1 C1 O2 167.19(19) . . . . no Co O1 C1 C2 -14.0(3) . . . . no O2 C1 C2 N1 -160.4(2) . . . . no O1 C1 C2 N1 20.7(3) . . . . no O2 C1 C2 C3 -34.9(3) . . . . no O1 C1 C2 C3 146.2(2) . . . . no C1 C2 N1 Co -17.1(2) . . . . no C3 C2 N1 Co -141.41(15) . . . . no O1 Co N1 C2 9.03(15) . . . . no N11 Co N1 C2 -178.43(15) . . . . no N12 Co N1 C2 95.79(15) . . . . no N21 Co N1 C2 -40.7(8) . . . . no N22 Co N1 C2 -82.55(16) . . . . no N1 C2 C3 C4 67.9(2) . . . . no C1 C2 C3 C4 -55.0(2) . . . . no N1 C2 C3 C7 -53.4(2) . . . . no C1 C2 C3 C7 -176.24(19) . . . . no C7 C3 C4 O3 87.8(3) . . . . no C2 C3 C4 O3 -34.0(3) . . . . no C7 C3 C4 O4 -90.5(3) . . . . no C2 C3 C4 O4 147.8(2) . . . . no O3 C4 O4 C5 -8.0(4) . . . . no C3 C4 O4 C5 170.2(2) . . . . no C4 O4 C5 C6 -179.0(3) . . . . no C4 C3 C7 O5 -169.4(3) . . . . no C2 C3 C7 O5 -47.1(3) . . . . no C4 C3 C7 O6 9.0(3) . . . . no C2 C3 C7 O6 131.3(2) . . . . no O5 C7 O6 C8 6.7(4) . . . . no C3 C7 O6 C8 -171.7(3) . . . . no C7 O6 C8 C9 161.2(3) . . . . no O1_1 Co_1 N11_1 C11_1 31.5(7) . . . . no N12_1 Co_1 N11_1 C11_1 16.52(17) . . . . no N21_1 Co_1 N11_1 C11_1 -75.66(17) . . . . no N1_1 Co_1 N11_1 C11_1 108.98(17) . . . . no N22_1 Co_1 N11_1 C11_1 -160.85(17) . . . . no Co_1 N11_1 C11_1 C12_1 -40.0(2) . . . . no N11_1 C11_1 C12_1 N12_1 48.2(2) . . . . no C11_1 C12_1 N12_1 Co_1 -34.9(2) . . . . no O1_1 Co_1 N12_1 C12_1 -167.27(16) . . . . no N11_1 Co_1 N12_1 C12_1 10.77(16) . . . . no N21_1 Co_1 N12_1 C12_1 102.61(17) . . . . no N1_1 Co_1 N12_1 C12_1 -81.40(16) . . . . no N22_1 Co_1 N12_1 C12_1 133.4(16) . . . . no O1_1 Co_1 N21_1 C21_1 69.21(16) . . . . no N11_1 Co_1 N21_1 C21_1 -118.02(16) . . . . no N12_1 Co_1 N21_1 C21_1 156.45(16) . . . . no N1_1 Co_1 N21_1 C21_1 15.3(9) . . . . no N22_1 Co_1 N21_1 C21_1 -21.95(16) . . . . no Co_1 N21_1 C21_1 C22_1 45.9(2) . . . . no N21_1 C21_1 C22_1 N22_1 -51.4(3) . . . . no C21_1 C22_1 N22_1 Co_1 33.7(2) . . . . no O1_1 Co_1 N22_1 C22_1 -96.95(16) . . . . no N11_1 Co_1 N22_1 C22_1 84.66(16) . . . . no N12_1 Co_1 N22_1 C22_1 -37.7(17) . . . . no N21_1 Co_1 N22_1 C22_1 -6.82(16) . . . . no N1_1 Co_1 N22_1 C22_1 177.04(16) . . . . no N11_1 Co_1 O1_1 C1_1 77.6(6) . . . . no N12_1 Co_1 O1_1 C1_1 92.56(17) . . . . no N21_1 Co_1 O1_1 C1_1 -175.12(17) . . . . no N1_1 Co_1 O1_1 C1_1 -0.29(17) . . . . no N22_1 Co_1 O1_1 C1_1 -90.12(17) . . . . no Co_1 O1_1 C1_1 O2_1 -167.39(19) . . . . no Co_1 O1_1 C1_1 C2_1 13.3(3) . . . . no O2_1 C1_1 C2_1 N1_1 157.7(2) . . . . no O1_1 C1_1 C2_1 N1_1 -23.0(3) . . . . no O2_1 C1_1 C2_1 C3_1 32.5(3) . . . . no O1_1 C1_1 C2_1 C3_1 -148.2(2) . . . . no C1_1 C2_1 N1_1 Co_1 20.9(2) . . . . no C3_1 C2_1 N1_1 Co_1 144.60(15) . . . . no O1_1 Co_1 N1_1 C2_1 -12.52(15) . . . . no N11_1 Co_1 N1_1 C2_1 174.90(15) . . . . no N12_1 Co_1 N1_1 C2_1 -99.56(15) . . . . no N21_1 Co_1 N1_1 C2_1 41.6(8) . . . . no N22_1 Co_1 N1_1 C2_1 78.67(15) . . . . no N1_1 C2_1 C3_1 C7_1 -71.5(2) . . . . no C1_1 C2_1 C3_1 C7_1 50.7(2) . . . . no N1_1 C2_1 C3_1 C4_1 50.8(2) . . . . no C1_1 C2_1 C3_1 C4_1 173.09(19) . . . . no C7_1 C3_1 C4_1 O3_1 173.7(2) . . . . no C2_1 C3_1 C4_1 O3_1 51.6(3) . . . . no C7_1 C3_1 C4_1 O4_1 -4.4(3) . . . . no C2_1 C3_1 C4_1 O4_1 -126.5(2) . . . . no O3_1 C4_1 O4_1 C5_1 -5.0(4) . . . . no C3_1 C4_1 O4_1 C5_1 173.0(2) . . . . no C4_1 O4_1 C5_1 C6_1 -168.7(3) . . . . no C4_1 C3_1 C7_1 O5_1 -87.7(3) . . . . no C2_1 C3_1 C7_1 O5_1 34.4(3) . . . . no C4_1 C3_1 C7_1 O6_1 92.9(2) . . . . no C2_1 C3_1 C7_1 O6_1 -145.0(2) . . . . no O5_1 C7_1 O6_1 C8_1 8.3(4) . . . . no C3_1 C7_1 O6_1 C8_1 -172.3(2) . . . . no C7_1 O6_1 C8_1 C9_1 91.1(3) . . . . no _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 35.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.587 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.104 #===END