Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Hartshorn, Richard' 'Browne, Julian M. W.' 'Fitchett, Christopher M.' 'Wikaira, Jan' _publ_contact_author_name 'Dr Richard Hartshorn' _publ_contact_author_address ; Department of Chemistry University of Canterbury Private bag 4800 Christchurch NEW ZEALAND ; _publ_contact_author_email 'R.HARTSHORN@CHEM.CANTERBURY.AC.NZ' _publ_section_title ; Polydentate ligand construction: intramolecular condensation reactions in the synthesis of imine containing ligands. ; data_compound1 #mffma-[Co(Aimtetraen)]ZnCl4 _database_code_CSD 176555 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H24 Cl4 Co N5 O2 Zn' _chemical_formula_weight 524.45 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' 'Zn' 'Zn' 0.2839 1.4301 '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 8.927(3) _cell_length_b 15.035(5) _cell_length_c 14.714(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.915(4) _cell_angle_gamma 90.00 _cell_volume 1908.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 2.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7629 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23538 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.38 _reflns_number_total 3883 _reflns_number_gt 3644 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0258P)^2^+3.1353P] 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 3883 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.02782(3) 0.107906(19) 0.69835(2) 0.01587(8) Uani 1 1 d . . . Zn1 Zn 0.01111(3) -0.205292(18) 0.867573(19) 0.02231(8) Uani 1 1 d . . . Cl4 Cl -0.23746(7) -0.16640(4) 0.86657(4) 0.02663(13) Uani 1 1 d . . . Cl3 Cl 0.18225(7) -0.10149(4) 0.94132(5) 0.03238(15) Uani 1 1 d . . . Cl2 Cl 0.05374(8) -0.34008(4) 0.93843(5) 0.03484(16) Uani 1 1 d . . . Cl1 Cl 0.03069(8) -0.21102(5) 0.71660(5) 0.03699(16) Uani 1 1 d . . . O1 O 0.12802(18) 0.01858(10) 0.64161(11) 0.0201(3) Uani 1 1 d . . . N1 N 0.2037(2) 0.09542(13) 0.79944(13) 0.0192(4) Uani 1 1 d . . . N2 N -0.0446(2) 0.19314(13) 0.77880(13) 0.0212(4) Uani 1 1 d . . . H2' H -0.0899 0.2411 0.7419 0.025 Uiso 1 1 calc R . . N4 N -0.1458(2) 0.11644(13) 0.58799(13) 0.0195(4) Uani 1 1 d . . . H4' H -0.2166 0.1577 0.5992 0.023 Uiso 1 1 calc R . . N3 N -0.0945(2) 0.01756(14) 0.74246(14) 0.0228(4) Uani 1 1 d . . . H3' H -0.0364 -0.0344 0.7557 0.027 Uiso 1 1 calc R . . O2 O 0.3486(2) -0.06093(12) 0.67254(13) 0.0308(4) Uani 1 1 d . . . N5 N 0.1296(2) 0.19784(13) 0.63730(13) 0.0202(4) Uani 1 1 d . . . H5B' H 0.1557 0.2465 0.6761 0.024 Uiso 1 1 calc R . . H5A' H 0.2192 0.1746 0.6271 0.024 Uiso 1 1 calc R . . C1 C 0.2631(3) -0.00633(15) 0.69389(17) 0.0213(5) Uani 1 1 d . . . C7 C -0.2417(3) -0.00176(18) 0.66778(18) 0.0284(5) Uani 1 1 d . . . H7B H -0.3295 0.0309 0.6817 0.034 Uiso 1 1 calc R . . H7A H -0.2651 -0.0662 0.6666 0.034 Uiso 1 1 calc R . . C8 C -0.2202(3) 0.02720(16) 0.57336(17) 0.0247(5) Uani 1 1 d . . . H8A H -0.1533 -0.0156 0.5509 0.030 Uiso 1 1 calc R . . H8B H -0.3215 0.0305 0.5262 0.030 Uiso 1 1 calc R . . C3 C 0.2116(3) 0.15086(17) 0.88326(16) 0.0263(5) Uani 1 1 d . . . H3A H 0.3173 0.1753 0.9077 0.032 Uiso 1 1 calc R . . H3B H 0.1849 0.1152 0.9335 0.032 Uiso 1 1 calc R . . C10 C 0.0239(3) 0.22592(16) 0.54592(16) 0.0230(5) Uani 1 1 d . . . H10A H 0.0847 0.2415 0.5006 0.028 Uiso 1 1 calc R . . H10B H -0.0369 0.2787 0.5551 0.028 Uiso 1 1 calc R . . C2 C 0.3081(3) 0.04119(16) 0.78904(16) 0.0212(5) Uani 1 1 d . . . C9 C -0.0833(3) 0.14862(16) 0.50912(16) 0.0229(5) Uani 1 1 d . . . H9A H -0.1691 0.1681 0.4557 0.027 Uiso 1 1 calc R . . H9B H -0.0258 0.1004 0.4871 0.027 Uiso 1 1 calc R . . C5 C -0.1653(3) 0.14953(17) 0.81778(18) 0.0279(5) Uani 1 1 d . . . H5A H -0.2689 0.1573 0.7738 0.034 Uiso 1 1 calc R . . H5B H -0.1667 0.1772 0.8786 0.034 Uiso 1 1 calc R . . C6 C -0.1273(3) 0.05135(17) 0.83168(18) 0.0271(5) Uani 1 1 d . . . H6A H -0.0356 0.0427 0.8855 0.032 Uiso 1 1 calc R . . H6B H -0.2159 0.0187 0.8447 0.032 Uiso 1 1 calc R . . C4 C 0.0942(3) 0.22621(17) 0.85164(17) 0.0273(5) Uani 1 1 d . . . H4A H 0.0613 0.2493 0.9065 0.033 Uiso 1 1 calc R . . H4B H 0.1433 0.2755 0.8252 0.033 Uiso 1 1 calc R . . C11 C 0.4592(3) 0.0243(2) 0.85793(19) 0.0321(6) Uani 1 1 d . . . H11A H 0.4667 0.0607 0.9142 0.048 Uiso 1 1 calc R . . H11B H 0.5438 0.0398 0.8297 0.048 Uiso 1 1 calc R . . H11C H 0.4667 -0.0388 0.8754 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01655(15) 0.01624(15) 0.01464(15) -0.00109(11) 0.00368(11) 0.00076(11) Zn1 0.02374(15) 0.02091(14) 0.02479(15) 0.00237(11) 0.01079(11) -0.00064(10) Cl4 0.0238(3) 0.0248(3) 0.0335(3) -0.0029(2) 0.0114(2) -0.0018(2) Cl3 0.0305(3) 0.0261(3) 0.0380(3) 0.0019(3) 0.0043(3) -0.0047(2) Cl2 0.0345(3) 0.0231(3) 0.0509(4) 0.0118(3) 0.0182(3) 0.0024(3) Cl1 0.0416(4) 0.0476(4) 0.0262(3) 0.0011(3) 0.0168(3) 0.0018(3) O1 0.0199(8) 0.0190(8) 0.0207(8) -0.0042(6) 0.0038(6) 0.0021(6) N1 0.0215(9) 0.0201(9) 0.0158(9) 0.0003(7) 0.0042(7) -0.0014(8) N2 0.0259(10) 0.0190(9) 0.0196(9) 0.0002(8) 0.0074(8) 0.0031(8) N4 0.0183(9) 0.0194(9) 0.0201(9) -0.0028(8) 0.0037(7) 0.0024(7) N3 0.0199(9) 0.0232(10) 0.0255(10) 0.0034(8) 0.0062(8) 0.0005(8) O2 0.0265(9) 0.0267(9) 0.0388(10) -0.0059(8) 0.0077(8) 0.0068(7) N5 0.0201(9) 0.0204(10) 0.0196(9) -0.0009(8) 0.0041(8) -0.0006(8) C1 0.0193(11) 0.0192(11) 0.0252(12) 0.0005(9) 0.0056(9) -0.0005(9) C7 0.0212(12) 0.0280(13) 0.0349(14) -0.0001(11) 0.0054(10) -0.0061(10) C8 0.0210(11) 0.0221(12) 0.0288(13) -0.0059(10) 0.0027(10) -0.0024(9) C3 0.0306(13) 0.0321(13) 0.0141(11) -0.0056(10) 0.0020(9) -0.0013(10) C10 0.0273(12) 0.0232(12) 0.0187(11) 0.0037(9) 0.0062(9) 0.0027(10) C2 0.0200(11) 0.0212(11) 0.0215(11) 0.0037(9) 0.0035(9) -0.0019(9) C9 0.0256(12) 0.0267(12) 0.0155(10) 0.0000(9) 0.0035(9) 0.0037(10) C5 0.0290(13) 0.0289(13) 0.0294(13) 0.0032(10) 0.0139(11) 0.0054(10) C6 0.0283(13) 0.0275(13) 0.0288(13) 0.0061(10) 0.0135(10) 0.0025(10) C4 0.0342(14) 0.0249(12) 0.0231(12) -0.0067(10) 0.0078(10) -0.0015(10) C11 0.0222(12) 0.0417(15) 0.0280(13) 0.0032(12) -0.0015(10) 0.0023(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.873(2) . ? Co1 O1 1.9198(16) . ? Co1 N4 1.9389(19) . ? Co1 N3 1.955(2) . ? Co1 N2 1.964(2) . ? Co1 N5 1.970(2) . ? Zn1 Cl3 2.2570(8) . ? Zn1 Cl2 2.2660(9) . ? Zn1 Cl1 2.2744(10) . ? Zn1 Cl4 2.2911(9) . ? O1 C1 1.307(3) . ? N1 C2 1.277(3) . ? N1 C3 1.475(3) . ? N2 C5 1.496(3) . ? N2 C4 1.499(3) . ? N4 C8 1.488(3) . ? N4 C9 1.492(3) . ? N3 C6 1.505(3) . ? N3 C7 1.509(3) . ? O2 C1 1.216(3) . ? N5 C10 1.491(3) . ? C1 C2 1.530(3) . ? C7 C8 1.515(4) . ? C3 C4 1.532(4) . ? C10 C9 1.514(3) . ? C2 C11 1.486(3) . ? C5 C6 1.517(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 O1 83.46(8) . . ? N1 Co1 N4 175.78(8) . . ? O1 Co1 N4 92.49(8) . . ? N1 Co1 N3 95.28(8) . . ? O1 Co1 N3 91.19(8) . . ? N4 Co1 N3 85.98(8) . . ? N1 Co1 N2 85.72(8) . . ? O1 Co1 N2 168.92(8) . . ? N4 Co1 N2 98.37(8) . . ? N3 Co1 N2 87.41(9) . . ? N1 Co1 N5 92.32(8) . . ? O1 Co1 N5 87.75(8) . . ? N4 Co1 N5 86.30(8) . . ? N3 Co1 N5 172.16(8) . . ? N2 Co1 N5 95.10(9) . . ? Cl3 Zn1 Cl2 112.61(3) . . ? Cl3 Zn1 Cl1 106.45(3) . . ? Cl2 Zn1 Cl1 111.69(3) . . ? Cl3 Zn1 Cl4 111.18(3) . . ? Cl2 Zn1 Cl4 106.19(3) . . ? Cl1 Zn1 Cl4 108.73(3) . . ? C1 O1 Co1 114.02(14) . . ? C2 N1 C3 125.5(2) . . ? C2 N1 Co1 117.21(16) . . ? C3 N1 Co1 117.22(15) . . ? C5 N2 C4 114.55(19) . . ? C5 N2 Co1 109.05(15) . . ? C4 N2 Co1 107.92(15) . . ? C8 N4 C9 114.97(18) . . ? C8 N4 Co1 106.99(14) . . ? C9 N4 Co1 107.16(14) . . ? C6 N3 C7 111.80(19) . . ? C6 N3 Co1 107.80(15) . . ? C7 N3 Co1 110.38(15) . . ? C10 N5 Co1 110.29(14) . . ? O2 C1 O1 125.9(2) . . ? O2 C1 C2 121.1(2) . . ? O1 C1 C2 112.94(19) . . ? N3 C7 C8 108.66(19) . . ? N4 C8 C7 106.49(19) . . ? N1 C3 C4 106.38(19) . . ? N5 C10 C9 107.46(19) . . ? N1 C2 C11 126.2(2) . . ? N1 C2 C1 112.3(2) . . ? C11 C2 C1 121.5(2) . . ? N4 C9 C10 107.41(18) . . ? N2 C5 C6 108.7(2) . . ? N3 C6 C5 107.3(2) . . ? N2 C4 C3 110.3(2) . . ? 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 Co1 O1 C1 -1.52(16) . . . . ? N4 Co1 O1 C1 177.27(16) . . . . ? N3 Co1 O1 C1 -96.70(16) . . . . ? N2 Co1 O1 C1 -14.1(5) . . . . ? N5 Co1 O1 C1 91.08(16) . . . . ? O1 Co1 N1 C2 2.08(17) . . . . ? N4 Co1 N1 C2 -14.5(12) . . . . ? N3 Co1 N1 C2 92.68(18) . . . . ? N2 Co1 N1 C2 179.67(18) . . . . ? N5 Co1 N1 C2 -85.38(18) . . . . ? O1 Co1 N1 C3 -179.55(17) . . . . ? N4 Co1 N1 C3 163.8(11) . . . . ? N3 Co1 N1 C3 -88.95(18) . . . . ? N2 Co1 N1 C3 -1.96(17) . . . . ? N5 Co1 N1 C3 92.98(17) . . . . ? N1 Co1 N2 C5 -103.18(16) . . . . ? O1 Co1 N2 C5 -90.6(4) . . . . ? N4 Co1 N2 C5 77.87(16) . . . . ? N3 Co1 N2 C5 -7.68(16) . . . . ? N5 Co1 N2 C5 164.87(15) . . . . ? N1 Co1 N2 C4 21.83(15) . . . . ? O1 Co1 N2 C4 34.4(5) . . . . ? N4 Co1 N2 C4 -157.12(15) . . . . ? N3 Co1 N2 C4 117.33(16) . . . . ? N5 Co1 N2 C4 -70.12(16) . . . . ? N1 Co1 N4 C8 77.4(12) . . . . ? O1 Co1 N4 C8 60.82(15) . . . . ? N3 Co1 N4 C8 -30.20(15) . . . . ? N2 Co1 N4 C8 -116.98(15) . . . . ? N5 Co1 N4 C8 148.40(15) . . . . ? N1 Co1 N4 C9 -46.4(12) . . . . ? O1 Co1 N4 C9 -62.99(15) . . . . ? N3 Co1 N4 C9 -154.01(15) . . . . ? N2 Co1 N4 C9 119.22(15) . . . . ? N5 Co1 N4 C9 24.59(15) . . . . ? N1 Co1 N3 C6 66.68(16) . . . . ? O1 Co1 N3 C6 150.22(15) . . . . ? N4 Co1 N3 C6 -117.36(16) . . . . ? N2 Co1 N3 C6 -18.78(15) . . . . ? N5 Co1 N3 C6 -127.6(6) . . . . ? N1 Co1 N3 C7 -170.95(16) . . . . ? O1 Co1 N3 C7 -87.40(16) . . . . ? N4 Co1 N3 C7 5.01(16) . . . . ? N2 Co1 N3 C7 103.59(17) . . . . ? N5 Co1 N3 C7 -5.3(7) . . . . ? N1 Co1 N5 C10 178.06(15) . . . . ? O1 Co1 N5 C10 94.70(15) . . . . ? N4 Co1 N5 C10 2.06(15) . . . . ? N3 Co1 N5 C10 12.3(7) . . . . ? N2 Co1 N5 C10 -96.03(15) . . . . ? Co1 O1 C1 O2 -179.0(2) . . . . ? Co1 O1 C1 C2 0.8(2) . . . . ? C6 N3 C7 C8 141.0(2) . . . . ? Co1 N3 C7 C8 21.0(2) . . . . ? C9 N4 C8 C7 167.38(19) . . . . ? Co1 N4 C8 C7 48.5(2) . . . . ? N3 C7 C8 N4 -45.0(3) . . . . ? C2 N1 C3 C4 160.4(2) . . . . ? Co1 N1 C3 C4 -17.9(2) . . . . ? Co1 N5 C10 C9 -27.9(2) . . . . ? C3 N1 C2 C11 -1.3(4) . . . . ? Co1 N1 C2 C11 176.9(2) . . . . ? C3 N1 C2 C1 179.7(2) . . . . ? Co1 N1 C2 C1 -2.1(3) . . . . ? O2 C1 C2 N1 -179.3(2) . . . . ? O1 C1 C2 N1 0.8(3) . . . . ? O2 C1 C2 C11 1.6(4) . . . . ? O1 C1 C2 C11 -178.3(2) . . . . ? C8 N4 C9 C10 -164.86(19) . . . . ? Co1 N4 C9 C10 -46.1(2) . . . . ? N5 C10 C9 N4 48.2(2) . . . . ? C4 N2 C5 C6 -88.6(2) . . . . ? Co1 N2 C5 C6 32.5(2) . . . . ? C7 N3 C6 C5 -80.6(2) . . . . ? Co1 N3 C6 C5 40.8(2) . . . . ? N2 C5 C6 N3 -48.2(3) . . . . ? C5 N2 C4 C3 84.6(2) . . . . ? Co1 N2 C4 C3 -37.1(2) . . . . ? N1 C3 C4 N2 35.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.907 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.068 #===END data_compound2 #mmf(f)-[Co(Aimtrenen)]ZnCl4·H2O _database_code_CSD 176556 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H26 Cl4 Co N5 O3 Zn' _chemical_formula_weight 542.47 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' 'Zn' 'Zn' 0.2839 1.4301 '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 7.933(3) _cell_length_b 22.849(10) _cell_length_c 11.323(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.984(7) _cell_angle_gamma 90.00 _cell_volume 2052.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Rod _exptl_crystal_colour Orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 2.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7856 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing, Acta. Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23646 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.40 _reflns_number_total 3626 _reflns_number_gt 2586 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0251P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3626 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0535 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.085 _refine_ls_shift/su_mean 0.001 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 0.77062(5) -0.119990(17) 0.57351(4) 0.01951(12) Uani 1 1 d . . . O1 O 0.7293(3) -0.03760(8) 0.54936(19) 0.0256(5) Uani 1 1 d . . . C1 C 0.6316(4) -0.01586(14) 0.6291(3) 0.0270(8) Uani 1 1 d . . . O2 O 0.5783(3) 0.03477(9) 0.6304(2) 0.0354(6) Uani 1 1 d . . . C2 C 0.5805(4) -0.05874(13) 0.7267(3) 0.0247(8) Uani 1 1 d . . . N1 N 0.6374(3) -0.11013(10) 0.7072(2) 0.0216(6) Uani 1 1 d . . . C3 C 0.6153(4) -0.16388(13) 0.7783(3) 0.0258(8) Uani 1 1 d . . . H3A H 0.5045 -0.1820 0.7603 0.031 Uiso 1 1 calc R . . H3B H 0.6212 -0.1545 0.8636 0.031 Uiso 1 1 calc R . . C4 C 0.7559(4) -0.20515(13) 0.7463(3) 0.0235(8) Uani 1 1 d . . . H4A H 0.8596 -0.1948 0.7915 0.028 Uiso 1 1 calc R . . H4B H 0.7243 -0.2458 0.7669 0.028 Uiso 1 1 calc R . . N2 N 0.7880(3) -0.20104(10) 0.6168(2) 0.0223(6) Uani 1 1 d . . . H2A' H 0.7107 -0.2186 0.5780 0.022 Uiso 1 1 d R . . C5 C 0.9497(4) -0.22404(13) 0.5728(3) 0.0245(8) Uani 1 1 d . . . H5A H 0.9462 -0.2673 0.5693 0.029 Uiso 1 1 calc R . . H5B H 1.0436 -0.2123 0.6265 0.029 Uiso 1 1 calc R . . C6 C 0.9763(4) -0.19892(12) 0.4501(3) 0.0245(8) Uani 1 1 d . . . H6A H 0.9133 -0.2228 0.3913 0.029 Uiso 1 1 calc R . . H6B H 1.0975 -0.2010 0.4312 0.029 Uiso 1 1 calc R . . N3 N 0.9170(3) -0.13530(10) 0.4417(2) 0.0223(6) Uani 1 1 d . . . C7 C 1.0607(4) -0.09306(13) 0.4540(3) 0.0250(8) Uani 1 1 d . . . H7A H 1.0223 -0.0530 0.4341 0.030 Uiso 1 1 calc R . . H7B H 1.1520 -0.1040 0.3996 0.030 Uiso 1 1 calc R . . C8 C 1.1250(4) -0.09528(14) 0.5812(3) 0.0247(8) Uani 1 1 d . . . H8A H 1.1949 -0.1307 0.5939 0.030 Uiso 1 1 calc R . . H8B H 1.1954 -0.0605 0.5988 0.030 Uiso 1 1 calc R . . N4 N 0.9772(3) -0.09654(10) 0.6603(2) 0.0220(6) Uani 1 1 d . . . H4A' H 0.9563 -0.0646 0.6842 0.033 Uiso 1 1 d R . . H4B' H 1.0007 -0.1168 0.7174 0.033 Uiso 1 1 d R . . C9 C 0.8168(4) -0.12492(14) 0.3303(3) 0.0271(8) Uani 1 1 d . . . H9A H 0.8754 -0.1420 0.2620 0.032 Uiso 1 1 calc R . . H9B H 0.8026 -0.0824 0.3164 0.032 Uiso 1 1 calc R . . C10 C 0.6466(4) -0.15380(14) 0.3450(3) 0.0286(8) Uani 1 1 d . . . H10A H 0.5676 -0.1411 0.2814 0.034 Uiso 1 1 calc R . . H10B H 0.6579 -0.1969 0.3412 0.034 Uiso 1 1 calc R . . N5 N 0.5822(3) -0.13567(10) 0.4628(2) 0.0251(7) Uani 1 1 d . . . H5A' H 0.5157 -0.1600 0.4915 0.038 Uiso 1 1 d R . . H5B' H 0.5316 -0.1043 0.4659 0.038 Uiso 1 1 d R . . C11 C 0.4776(4) -0.03901(15) 0.8280(3) 0.0400(10) Uani 1 1 d . . . H11A H 0.4570 -0.0722 0.8806 0.060 Uiso 1 1 calc R . . H11B H 0.3697 -0.0235 0.7985 0.060 Uiso 1 1 calc R . . H11C H 0.5385 -0.0083 0.8716 0.060 Uiso 1 1 calc R . . Zn1 Zn 1.04402(5) -0.158547(15) 1.02189(3) 0.02339(11) Uani 1 1 d . . . Cl1 Cl 0.86082(11) -0.08539(4) 0.99409(8) 0.0388(2) Uani 1 1 d . . . Cl2 Cl 1.23126(11) -0.14160(3) 1.17092(7) 0.0329(2) Uani 1 1 d . . . Cl3 Cl 1.19322(10) -0.17817(3) 0.85553(7) 0.0287(2) Uani 1 1 d . . . Cl4 Cl 0.89498(10) -0.24326(3) 1.06229(8) 0.0285(2) Uani 1 1 d . . . O30 O 0.9228(3) 0.01000(10) 0.7871(2) 0.0516(8) Uani 1 1 d . . . H30A H 0.8827 0.0393 0.7933 0.077 Uiso 1 1 d R . . H30B H 0.9580 0.0076 0.8545 0.077 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0179(3) 0.0150(2) 0.0256(3) 0.00176(19) -0.00286(19) 0.00014(19) O1 0.0258(14) 0.0164(12) 0.0343(14) 0.0027(10) -0.0053(11) -0.0007(10) C1 0.022(2) 0.0204(19) 0.038(2) -0.0051(16) -0.0153(17) -0.0010(16) O2 0.0328(15) 0.0172(12) 0.0556(17) -0.0034(11) -0.0176(12) 0.0073(11) C2 0.0164(19) 0.0228(18) 0.035(2) -0.0031(16) -0.0059(16) 0.0009(15) N1 0.0180(15) 0.0177(14) 0.0291(17) -0.0017(12) -0.0023(13) 0.0002(12) C3 0.025(2) 0.0235(18) 0.029(2) 0.0019(15) 0.0032(16) -0.0041(15) C4 0.025(2) 0.0221(18) 0.0234(19) 0.0032(15) 0.0015(15) 0.0008(15) N2 0.0195(16) 0.0172(14) 0.0301(17) 0.0000(12) -0.0030(13) 0.0018(12) C5 0.0215(19) 0.0187(17) 0.033(2) 0.0002(15) 0.0013(16) 0.0026(14) C6 0.0212(19) 0.0203(18) 0.032(2) -0.0020(15) 0.0006(16) 0.0031(14) N3 0.0231(16) 0.0211(14) 0.0224(16) 0.0014(11) -0.0061(12) -0.0032(12) C7 0.025(2) 0.0245(18) 0.025(2) 0.0004(15) 0.0009(16) -0.0058(15) C8 0.0182(19) 0.0264(18) 0.029(2) 0.0014(15) 0.0002(16) -0.0062(15) N4 0.0244(16) 0.0197(14) 0.0220(16) 0.0028(11) -0.0024(13) 0.0021(12) C9 0.030(2) 0.0271(19) 0.024(2) 0.0041(15) -0.0043(16) -0.0013(16) C10 0.028(2) 0.0262(19) 0.031(2) -0.0025(16) -0.0086(17) 0.0025(16) N5 0.0209(16) 0.0149(14) 0.0395(19) 0.0024(12) -0.0045(13) -0.0008(12) C11 0.031(2) 0.037(2) 0.053(3) -0.0118(19) 0.0060(19) 0.0071(17) Zn1 0.0233(2) 0.0211(2) 0.0256(2) 0.00014(17) -0.00338(17) 0.00096(17) Cl1 0.0401(6) 0.0298(5) 0.0460(6) 0.0030(4) -0.0104(5) 0.0117(4) Cl2 0.0342(5) 0.0290(5) 0.0352(5) -0.0063(4) -0.0124(4) 0.0039(4) Cl3 0.0234(5) 0.0353(5) 0.0275(5) 0.0027(4) 0.0017(4) 0.0020(4) Cl4 0.0226(5) 0.0227(4) 0.0402(5) 0.0024(4) 0.0000(4) -0.0015(4) O30 0.089(2) 0.0300(14) 0.0350(16) -0.0076(11) -0.0136(15) 0.0076(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.874(3) . ? Co1 N2 1.920(2) . ? Co1 O1 1.930(2) . ? Co1 N3 1.938(3) . ? Co1 N5 1.967(2) . ? Co1 N4 1.970(2) . ? O1 C1 1.298(4) . ? C1 O2 1.232(4) . ? C1 C2 1.537(4) . ? C2 N1 1.279(4) . ? C2 C11 1.489(4) . ? N1 C3 1.481(4) . ? C3 C4 1.510(4) . ? C4 N2 1.496(4) . ? N2 C5 1.480(4) . ? C5 C6 1.521(4) . ? C6 N3 1.530(4) . ? N3 C7 1.499(4) . ? N3 C9 1.499(4) . ? C7 C8 1.520(4) . ? C8 N4 1.488(4) . ? C9 C10 1.515(4) . ? C10 N5 1.496(4) . ? Zn1 Cl1 2.2337(11) . ? Zn1 Cl2 2.2623(11) . ? Zn1 Cl3 2.2863(12) . ? Zn1 Cl4 2.3177(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N2 87.07(11) . . ? N1 Co1 O1 84.28(10) . . ? N2 Co1 O1 171.30(10) . . ? N1 Co1 N3 175.48(10) . . ? N2 Co1 N3 88.92(10) . . ? O1 Co1 N3 99.76(10) . . ? N1 Co1 N5 95.93(11) . . ? N2 Co1 N5 92.16(10) . . ? O1 Co1 N5 87.83(9) . . ? N3 Co1 N5 86.29(11) . . ? N1 Co1 N4 92.32(11) . . ? N2 Co1 N4 94.55(10) . . ? O1 Co1 N4 86.74(9) . . ? N3 Co1 N4 85.92(11) . . ? N5 Co1 N4 169.62(11) . . ? C1 O1 Co1 112.1(2) . . ? O2 C1 O1 125.3(3) . . ? O2 C1 C2 119.6(3) . . ? O1 C1 C2 115.1(3) . . ? N1 C2 C11 127.7(3) . . ? N1 C2 C1 111.2(3) . . ? C11 C2 C1 121.1(3) . . ? C2 N1 C3 128.5(3) . . ? C2 N1 Co1 117.1(2) . . ? C3 N1 Co1 114.40(19) . . ? N1 C3 C4 107.0(2) . . ? N2 C4 C3 109.6(2) . . ? C5 N2 C4 118.1(2) . . ? C5 N2 Co1 108.39(18) . . ? C4 N2 Co1 107.36(17) . . ? N2 C5 C6 107.9(2) . . ? C5 C6 N3 111.6(2) . . ? C7 N3 C9 111.6(2) . . ? C7 N3 C6 111.9(2) . . ? C9 N3 C6 111.1(2) . . ? C7 N3 Co1 106.11(18) . . ? C9 N3 Co1 107.68(19) . . ? C6 N3 Co1 108.13(18) . . ? N3 C7 C8 108.0(2) . . ? N4 C8 C7 108.4(3) . . ? C8 N4 Co1 111.26(18) . . ? N3 C9 C10 107.4(3) . . ? N5 C10 C9 107.2(2) . . ? C10 N5 Co1 110.61(18) . . ? Cl1 Zn1 Cl2 113.23(4) . . ? Cl1 Zn1 Cl3 112.05(4) . . ? Cl2 Zn1 Cl3 107.79(5) . . ? Cl1 Zn1 Cl4 108.65(5) . . ? Cl2 Zn1 Cl4 109.05(4) . . ? Cl3 Zn1 Cl4 105.78(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 Co1 O1 C1 -1.8(2) . . . . ? N2 Co1 O1 C1 4.3(7) . . . . ? N3 Co1 O1 C1 -179.75(19) . . . . ? N5 Co1 O1 C1 94.4(2) . . . . ? N4 Co1 O1 C1 -94.5(2) . . . . ? Co1 O1 C1 O2 -175.8(2) . . . . ? Co1 O1 C1 C2 3.4(3) . . . . ? O2 C1 C2 N1 175.5(3) . . . . ? O1 C1 C2 N1 -3.8(4) . . . . ? O2 C1 C2 C11 -4.6(4) . . . . ? O1 C1 C2 C11 176.2(3) . . . . ? C11 C2 N1 C3 0.8(5) . . . . ? C1 C2 N1 C3 -179.3(3) . . . . ? C11 C2 N1 Co1 -177.7(3) . . . . ? C1 C2 N1 Co1 2.2(3) . . . . ? N2 Co1 N1 C2 -179.5(2) . . . . ? O1 Co1 N1 C2 -0.5(2) . . . . ? N3 Co1 N1 C2 153.0(12) . . . . ? N5 Co1 N1 C2 -87.7(2) . . . . ? N4 Co1 N1 C2 86.0(2) . . . . ? N2 Co1 N1 C3 1.8(2) . . . . ? O1 Co1 N1 C3 -179.2(2) . . . . ? N3 Co1 N1 C3 -25.7(14) . . . . ? N5 Co1 N1 C3 93.6(2) . . . . ? N4 Co1 N1 C3 -92.7(2) . . . . ? C2 N1 C3 C4 -158.7(3) . . . . ? Co1 N1 C3 C4 19.8(3) . . . . ? N1 C3 C4 N2 -38.2(3) . . . . ? C3 C4 N2 C5 162.5(2) . . . . ? C3 C4 N2 Co1 39.7(3) . . . . ? N1 Co1 N2 C5 -151.7(2) . . . . ? O1 Co1 N2 C5 -157.8(6) . . . . ? N3 Co1 N2 C5 26.22(19) . . . . ? N5 Co1 N2 C5 112.5(2) . . . . ? N4 Co1 N2 C5 -59.6(2) . . . . ? N1 Co1 N2 C4 -23.11(19) . . . . ? O1 Co1 N2 C4 -29.2(7) . . . . ? N3 Co1 N2 C4 154.80(19) . . . . ? N5 Co1 N2 C4 -118.95(19) . . . . ? N4 Co1 N2 C4 68.98(19) . . . . ? C4 N2 C5 C6 -163.0(2) . . . . ? Co1 N2 C5 C6 -40.8(3) . . . . ? N2 C5 C6 N3 38.0(3) . . . . ? C5 C6 N3 C7 99.2(3) . . . . ? C5 C6 N3 C9 -135.3(3) . . . . ? C5 C6 N3 Co1 -17.3(3) . . . . ? N1 Co1 N3 C7 -97.6(13) . . . . ? N2 Co1 N3 C7 -125.03(19) . . . . ? O1 Co1 N3 C7 55.59(19) . . . . ? N5 Co1 N3 C7 142.74(19) . . . . ? N4 Co1 N3 C7 -30.39(18) . . . . ? N1 Co1 N3 C9 142.8(12) . . . . ? N2 Co1 N3 C9 115.37(18) . . . . ? O1 Co1 N3 C9 -64.01(19) . . . . ? N5 Co1 N3 C9 23.14(18) . . . . ? N4 Co1 N3 C9 -149.99(19) . . . . ? N1 Co1 N3 C6 22.6(14) . . . . ? N2 Co1 N3 C6 -4.80(18) . . . . ? O1 Co1 N3 C6 175.82(17) . . . . ? N5 Co1 N3 C6 -97.03(18) . . . . ? N4 Co1 N3 C6 89.84(18) . . . . ? C9 N3 C7 C8 164.9(3) . . . . ? C6 N3 C7 C8 -69.9(3) . . . . ? Co1 N3 C7 C8 47.8(3) . . . . ? N3 C7 C8 N4 -43.0(3) . . . . ? C7 C8 N4 Co1 18.2(3) . . . . ? N1 Co1 N4 C8 -177.23(19) . . . . ? N2 Co1 N4 C8 95.5(2) . . . . ? O1 Co1 N4 C8 -93.10(19) . . . . ? N3 Co1 N4 C8 6.94(19) . . . . ? N5 Co1 N4 C8 -34.6(6) . . . . ? C7 N3 C9 C10 -161.0(2) . . . . ? C6 N3 C9 C10 73.4(3) . . . . ? Co1 N3 C9 C10 -44.9(3) . . . . ? N3 C9 C10 N5 47.8(3) . . . . ? C9 C10 N5 Co1 -28.9(3) . . . . ? N1 Co1 N5 C10 -172.57(19) . . . . ? N2 Co1 N5 C10 -85.3(2) . . . . ? O1 Co1 N5 C10 103.41(19) . . . . ? N3 Co1 N5 C10 3.47(19) . . . . ? N4 Co1 N5 C10 45.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.365 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.071 #===END data_compound3 #mff-[Co(Aimtrien)Cl]Cl _database_code_CSD 176557 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H19 Cl2 Co N4 O2' _chemical_formula_weight 345.11 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 8.966(4) _cell_length_b 14.474(7) _cell_length_c 10.343(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.319(7) _cell_angle_gamma 90.00 _cell_volume 1328.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.694 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7879 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'blessing, Acta Cyst. (1995)A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16417 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 26.39 _reflns_number_total 2690 _reflns_number_gt 2351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.4692P] 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 2690 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.004 _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 0.16547(3) 0.666426(18) 0.88587(2) 0.01459(10) Uani 1 1 d . C . Cl1 Cl 0.11115(6) 0.63604(4) 1.08745(5) 0.02362(13) Uani 1 1 d . . . Cl2 Cl 0.17534(6) 0.88601(4) 0.61879(6) 0.03338(15) Uani 1 1 d . . . O1 O 0.26585(15) 0.77837(9) 0.94441(13) 0.0184(3) Uani 1 1 d . . . O2 O 0.21248(16) 0.92545(10) 0.98125(15) 0.0248(3) Uani 1 1 d . . . N1 N -0.00301(17) 0.74304(11) 0.85123(15) 0.0160(3) Uani 1 1 d . . . N2 N 0.03264(18) 0.56695(11) 0.81235(16) 0.0183(3) Uani 1 1 d . C . H2' H 0.0546 0.5143 0.8631 0.022 Uiso 1 1 calc R . . N3 N 0.21843(19) 0.68259(12) 0.71137(16) 0.0199(4) Uani 1 1 d . . . H3' H 0.2192 0.7452 0.6914 0.024 Uiso 1 1 calc R A 1 N4 N 0.35417(19) 0.60065(12) 0.92203(17) 0.0219(4) Uani 1 1 d . . . H4'A H 0.3946 0.6075 1.0085 0.026 Uiso 1 1 calc R B 1 H4'B H 0.3394 0.5387 0.9050 0.026 Uiso 1 1 calc R B 1 C1 C 0.1783(2) 0.84905(13) 0.93905(19) 0.0179(4) Uani 1 1 d . . . C2 C 0.0178(2) 0.82842(13) 0.87666(19) 0.0171(4) Uani 1 1 d . . . C9 C -0.0948(2) 0.90363(15) 0.8534(2) 0.0239(4) Uani 1 1 d . . . H9A H -0.1916 0.8781 0.8127 0.036 Uiso 1 1 calc R . . H9B H -0.0602 0.9499 0.7953 0.036 Uiso 1 1 calc R . . H9C H -0.1072 0.9326 0.9368 0.036 Uiso 1 1 calc R . . C3 C -0.1442(2) 0.69920(15) 0.7959(2) 0.0218(4) Uani 1 1 d . . . H3A H -0.1657 0.7110 0.7007 0.026 Uiso 1 1 calc R . . H3B H -0.2287 0.7238 0.8375 0.026 Uiso 1 1 calc R . . C4 C -0.1250(2) 0.59601(15) 0.8224(2) 0.0223(4) Uani 1 1 d . . . H4A H -0.1484 0.5819 0.9109 0.027 Uiso 1 1 calc R . . H4B H -0.1963 0.5611 0.7583 0.027 Uiso 1 1 calc R . . C5 C 0.0603(2) 0.54652(15) 0.6773(2) 0.0237(5) Uani 1 1 d . . . H5A H -0.0323 0.5213 0.6255 0.028 Uiso 1 1 calc R C . H5S H 0.1414 0.5000 0.6789 0.028 Uiso 1 1 calc R . . C6 C 0.1058(2) 0.63501(16) 0.6162(2) 0.0258(5) Uani 1 1 d . C . H6A H 0.1492 0.6211 0.5357 0.031 Uiso 1 1 calc R . . H6B H 0.0165 0.6751 0.5927 0.031 Uiso 1 1 calc R . . C7B C 0.3712(4) 0.6414(4) 0.7017(4) 0.0260(9) Uani 0.776(11) 1 d P C 1 H7B1 H 0.3598 0.5778 0.6663 0.031 Uiso 0.776(11) 1 calc PR C 1 H7B2 H 0.4243 0.6791 0.6427 0.031 Uiso 0.776(11) 1 calc PR C 1 C8B C 0.4583(3) 0.6403(3) 0.8359(3) 0.0249(10) Uani 0.776(11) 1 d P C 1 H8B1 H 0.4892 0.7037 0.8642 0.030 Uiso 0.776(11) 1 calc PR C 1 H8B2 H 0.5497 0.6016 0.8385 0.030 Uiso 0.776(11) 1 calc PR C 1 C8A C 0.4227(13) 0.5901(12) 0.8013(11) 0.028(4) Uani 0.224(11) 1 d P C 2 H8A1 H 0.5338 0.5860 0.8222 0.034 Uiso 0.224(11) 1 calc PR C 2 H8A2 H 0.3848 0.5334 0.7539 0.034 Uiso 0.224(11) 1 calc PR C 2 C7A C 0.3788(17) 0.6726(11) 0.7217(15) 0.025(4) Uiso 0.224(11) 1 d P C 2 H7A2 H 0.4296 0.7280 0.7635 0.030 Uiso 0.224(11) 1 calc PR C 2 H7A1 H 0.4087 0.6655 0.6338 0.030 Uiso 0.224(11) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01342(15) 0.01418(15) 0.01571(15) -0.00037(10) 0.00060(10) 0.00031(10) Cl1 0.0267(3) 0.0264(3) 0.0174(2) 0.00215(19) 0.0020(2) -0.0033(2) Cl2 0.0304(3) 0.0276(3) 0.0424(3) 0.0141(2) 0.0061(2) 0.0018(2) O1 0.0152(7) 0.0169(7) 0.0223(7) -0.0023(6) 0.0007(5) -0.0013(5) O2 0.0235(8) 0.0196(8) 0.0310(8) -0.0068(6) 0.0029(6) -0.0018(6) N1 0.0121(7) 0.0198(8) 0.0163(8) -0.0002(7) 0.0023(6) 0.0004(6) N2 0.0181(8) 0.0161(8) 0.0198(8) 0.0003(7) 0.0003(7) -0.0002(7) N3 0.0201(8) 0.0188(9) 0.0208(8) 0.0011(7) 0.0035(7) 0.0001(7) N4 0.0204(9) 0.0220(9) 0.0225(9) 0.0003(7) 0.0006(7) 0.0044(7) C1 0.0176(10) 0.0182(10) 0.0184(10) 0.0002(8) 0.0044(8) -0.0010(8) C2 0.0175(9) 0.0190(10) 0.0156(9) 0.0010(7) 0.0051(7) 0.0019(8) C9 0.0218(10) 0.0245(11) 0.0251(11) -0.0002(9) 0.0027(8) 0.0065(9) C3 0.0123(9) 0.0242(11) 0.0280(11) -0.0036(9) -0.0004(8) -0.0002(8) C4 0.0145(9) 0.0244(11) 0.0282(11) -0.0024(9) 0.0038(8) -0.0036(8) C5 0.0224(11) 0.0255(11) 0.0230(11) -0.0090(9) 0.0028(8) -0.0024(9) C6 0.0270(11) 0.0340(13) 0.0162(10) -0.0043(9) 0.0029(8) -0.0018(9) C7B 0.0192(16) 0.030(2) 0.0302(19) -0.0039(17) 0.0086(12) -0.0001(15) C8B 0.0153(14) 0.028(2) 0.0312(18) -0.0037(15) 0.0028(12) 0.0006(13) C8A 0.019(5) 0.039(9) 0.027(6) -0.011(5) 0.008(4) 0.001(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 Co1 N1 1.8663(17) . ? Co1 O1 1.9090(15) . ? Co1 N4 1.9301(18) . ? Co1 N3 1.9456(19) . ? Co1 N2 1.9513(17) . ? Co1 Cl1 2.2519(11) . ? O1 C1 1.286(2) . ? O2 C1 1.212(3) . ? N1 C2 1.272(3) . ? N1 C3 1.457(2) . ? N2 C5 1.484(3) . ? N2 C4 1.493(3) . ? N3 C7A 1.433(15) . ? N3 C6 1.475(3) . ? N3 C7B 1.510(4) . ? N4 C8A 1.477(10) . ? N4 C8B 1.495(4) . ? C1 C2 1.519(3) . ? C2 C9 1.480(3) . ? C3 C4 1.524(3) . ? C5 C6 1.510(3) . ? C7B C8B 1.491(6) . ? C8A C7A 1.47(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 N1 Co1 O1 83.56(7) . . ? N1 Co1 N4 173.06(7) . . ? O1 Co1 N4 89.85(7) . . ? N1 Co1 N3 92.86(7) . . ? O1 Co1 N3 91.43(7) . . ? N4 Co1 N3 85.09(7) . . ? N1 Co1 N2 86.11(8) . . ? O1 Co1 N2 169.43(6) . . ? N4 Co1 N2 100.37(8) . . ? N3 Co1 N2 86.81(7) . . ? N1 Co1 Cl1 90.93(5) . . ? O1 Co1 Cl1 91.57(5) . . ? N4 Co1 Cl1 91.44(6) . . ? N3 Co1 Cl1 175.41(5) . . ? N2 Co1 Cl1 90.86(6) . . ? C1 O1 Co1 113.87(13) . . ? C2 N1 C3 126.69(17) . . ? C2 N1 Co1 116.58(14) . . ? C3 N1 Co1 116.72(13) . . ? C5 N2 C4 114.24(16) . . ? C5 N2 Co1 109.78(12) . . ? C4 N2 Co1 107.20(12) . . ? C7A N3 C6 125.8(7) . . ? C7A N3 C7B 19.2(6) . . ? C6 N3 C7B 108.1(2) . . ? C7A N3 Co1 107.2(6) . . ? C6 N3 Co1 109.11(13) . . ? C7B N3 Co1 111.08(17) . . ? C8A N4 C8B 33.3(6) . . ? C8A N4 Co1 110.3(4) . . ? C8B N4 Co1 107.48(15) . . ? O2 C1 O1 126.12(19) . . ? O2 C1 C2 120.46(18) . . ? O1 C1 C2 113.39(17) . . ? N1 C2 C9 127.22(19) . . ? N1 C2 C1 112.35(17) . . ? C9 C2 C1 120.42(18) . . ? N1 C3 C4 106.70(16) . . ? N2 C4 C3 110.30(16) . . ? N2 C5 C6 108.47(16) . . ? N3 C6 C5 108.50(17) . . ? C8B C7B N3 107.5(3) . . ? C7B C8B N4 105.7(3) . . ? C7A C8A N4 106.2(11) . . ? N3 C7A C8A 107.9(11) . . ? 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 Co1 O1 C1 2.54(13) . . . . ? N4 Co1 O1 C1 -179.67(14) . . . . ? N3 Co1 O1 C1 95.25(14) . . . . ? N2 Co1 O1 C1 15.0(4) . . . . ? Cl1 Co1 O1 C1 -88.23(13) . . . . ? O1 Co1 N1 C2 0.83(14) . . . . ? N4 Co1 N1 C2 -17.7(7) . . . . ? N3 Co1 N1 C2 -90.29(15) . . . . ? N2 Co1 N1 C2 -176.90(15) . . . . ? Cl1 Co1 N1 C2 92.30(15) . . . . ? O1 Co1 N1 C3 179.86(14) . . . . ? N4 Co1 N1 C3 161.3(5) . . . . ? N3 Co1 N1 C3 88.74(14) . . . . ? N2 Co1 N1 C3 2.14(14) . . . . ? Cl1 Co1 N1 C3 -88.67(13) . . . . ? N1 Co1 N2 C5 102.39(13) . . . . ? O1 Co1 N2 C5 90.0(4) . . . . ? N4 Co1 N2 C5 -75.11(14) . . . . ? N3 Co1 N2 C5 9.30(13) . . . . ? Cl1 Co1 N2 C5 -166.73(12) . . . . ? N1 Co1 N2 C4 -22.22(13) . . . . ? O1 Co1 N2 C4 -34.6(4) . . . . ? N4 Co1 N2 C4 160.28(13) . . . . ? N3 Co1 N2 C4 -115.31(13) . . . . ? Cl1 Co1 N2 C4 68.66(12) . . . . ? N1 Co1 N3 C7A 151.0(7) . . . . ? O1 Co1 N3 C7A 67.4(7) . . . . ? N4 Co1 N3 C7A -22.3(7) . . . . ? N2 Co1 N3 C7A -123.1(7) . . . . ? Cl1 Co1 N3 C7A -63.4(10) . . . . ? N1 Co1 N3 C6 -69.92(14) . . . . ? O1 Co1 N3 C6 -153.54(14) . . . . ? N4 Co1 N3 C6 116.73(15) . . . . ? N2 Co1 N3 C6 16.03(14) . . . . ? Cl1 Co1 N3 C6 75.7(7) . . . . ? N1 Co1 N3 C7B 171.0(2) . . . . ? O1 Co1 N3 C7B 87.3(2) . . . . ? N4 Co1 N3 C7B -2.4(2) . . . . ? N2 Co1 N3 C7B -103.1(2) . . . . ? Cl1 Co1 N3 C7B -43.5(7) . . . . ? N1 Co1 N4 C8A -79.1(10) . . . . ? O1 Co1 N4 C8A -97.5(8) . . . . ? N3 Co1 N4 C8A -6.0(8) . . . . ? N2 Co1 N4 C8A 79.8(8) . . . . ? Cl1 Co1 N4 C8A 170.9(8) . . . . ? N1 Co1 N4 C8B -43.9(7) . . . . ? O1 Co1 N4 C8B -62.4(2) . . . . ? N3 Co1 N4 C8B 29.1(2) . . . . ? N2 Co1 N4 C8B 114.9(2) . . . . ? Cl1 Co1 N4 C8B -153.9(2) . . . . ? Co1 O1 C1 O2 173.04(17) . . . . ? Co1 O1 C1 C2 -4.8(2) . . . . ? C3 N1 C2 C9 -1.6(3) . . . . ? Co1 N1 C2 C9 177.36(16) . . . . ? C3 N1 C2 C1 177.61(17) . . . . ? Co1 N1 C2 C1 -3.5(2) . . . . ? O2 C1 C2 N1 -172.50(18) . . . . ? O1 C1 C2 N1 5.5(2) . . . . ? O2 C1 C2 C9 6.7(3) . . . . ? O1 C1 C2 C9 -175.25(17) . . . . ? C2 N1 C3 C4 -162.99(19) . . . . ? Co1 N1 C3 C4 18.1(2) . . . . ? C5 N2 C4 C3 -84.2(2) . . . . ? Co1 N2 C4 C3 37.66(19) . . . . ? N1 C3 C4 N2 -35.9(2) . . . . ? C4 N2 C5 C6 88.4(2) . . . . ? Co1 N2 C5 C6 -32.03(19) . . . . ? C7A N3 C6 C5 92.0(7) . . . . ? C7B N3 C6 C5 83.4(2) . . . . ? Co1 N3 C6 C5 -37.51(19) . . . . ? N2 C5 C6 N3 45.5(2) . . . . ? C7A N3 C7B C8B 56.9(19) . . . . ? C6 N3 C7B C8B -144.6(4) . . . . ? Co1 N3 C7B C8B -24.9(4) . . . . ? N3 C7B C8B N4 47.5(5) . . . . ? C8A N4 C8B C7B 50.9(8) . . . . ? Co1 N4 C8B C7B -49.7(4) . . . . ? C8B N4 C8A C7A -58.8(13) . . . . ? Co1 N4 C8A C7A 32.3(14) . . . . ? C6 N3 C7A C8A -83.8(13) . . . . ? C7B N3 C7A C8A -58.4(19) . . . . ? Co1 N3 C7A C8A 46.5(14) . . . . ? N4 C8A C7A N3 -51.5(17) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.895 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.069 #===END data_compound4 #mffm-[Co(Aim2trien)]2ZnCl4 _database_code_CSD 176558 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H40 Cl4 Co2 N8 O8 Zn' _chemical_formula_weight 893.67 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 10.797(3) _cell_length_b 10.797(3) _cell_length_c 30.419(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3546(2) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 1.952 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8077 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22282 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0134 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 26.40 _reflns_number_total 1824 _reflns_number_gt 1575 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0309P)^2^+1.8840P] 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 1824 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.7500 0.051428(10) 0.01708(10) Uani 1 2 d S . . O2 O 0.09580(11) 0.82927(11) 0.00623(4) 0.0245(3) Uani 1 1 d . . . O1 O 0.24335(14) 0.77320(13) -0.04155(5) 0.0426(4) Uani 1 1 d . . . C1 C 0.18491(17) 0.75807(16) -0.00755(6) 0.0269(4) Uani 1 1 d . . . C2 C 0.21199(16) 0.64684(15) 0.02171(6) 0.0231(4) Uani 1 1 d . . . N3 N 0.12755(13) 0.63113(12) 0.05058(4) 0.0197(3) Uani 1 1 d . . . C4 C 0.11743(16) 0.53090(16) 0.08310(5) 0.0244(4) Uani 1 1 d . . . H4A H 0.1660 0.5507 0.1098 0.029 Uiso 1 1 calc R . . H4B H 0.1479 0.4518 0.0707 0.029 Uiso 1 1 calc R . . C5 C -0.02010(17) 0.52236(16) 0.09386(6) 0.0288(4) Uani 1 1 d . . . H5A H -0.0632 0.4750 0.0706 0.035 Uiso 1 1 calc R . . H5B H -0.0314 0.4780 0.1221 0.035 Uiso 1 1 calc R . . N6 N -0.07535(13) 0.65020(13) 0.09723(5) 0.0240(3) Uani 1 1 d . . . H6A H -0.1630 0.6396 0.0910 0.029 Uiso 1 1 d R . . C7 C -0.05970(18) 0.71404(18) 0.14060(6) 0.0323(4) Uani 1 1 d . . . H7A H -0.0585 0.6520 0.1646 0.039 Uiso 1 1 calc R . . H7B H -0.1301 0.7709 0.1458 0.039 Uiso 1 1 calc R . . C8 C 0.32531(17) 0.57057(18) 0.01501(7) 0.0319(4) Uani 1 1 d . . . H8A H 0.3989 0.6211 0.0208 0.048 Uiso 1 1 calc R . . H8B H 0.3277 0.5405 -0.0154 0.048 Uiso 1 1 calc R . . H8C H 0.3240 0.4998 0.0352 0.048 Uiso 1 1 calc R . . Zn1 Zn 0.5000 0.7500 0.1250 0.02208(11) Uani 1 4 d S . . Cl1 Cl 0.37421(4) 0.87164(4) 0.082972(15) 0.02991(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01844(17) 0.01897(17) 0.01384(17) 0.000 0.000 0.00113(12) O2 0.0280(6) 0.0236(6) 0.0220(6) 0.0039(5) 0.0071(5) 0.0035(5) O1 0.0507(9) 0.0417(8) 0.0354(8) 0.0106(7) 0.0244(7) 0.0111(7) C1 0.0302(9) 0.0264(9) 0.0241(9) -0.0008(7) 0.0065(7) -0.0009(7) C2 0.0241(9) 0.0224(9) 0.0228(9) -0.0045(7) 0.0005(7) 0.0007(7) N3 0.0226(7) 0.0187(7) 0.0179(7) -0.0012(5) -0.0010(6) 0.0022(6) C4 0.0317(9) 0.0211(8) 0.0204(9) 0.0023(7) -0.0001(7) 0.0055(7) C5 0.0338(10) 0.0234(9) 0.0292(10) 0.0060(7) 0.0018(8) -0.0019(7) N6 0.0211(7) 0.0281(8) 0.0228(8) 0.0064(6) 0.0017(6) 0.0021(6) C7 0.0425(11) 0.0365(11) 0.0178(9) 0.0069(8) 0.0092(8) 0.0154(9) C8 0.0281(10) 0.0315(10) 0.0361(11) -0.0033(8) 0.0054(8) 0.0061(8) Zn1 0.02020(14) 0.02020(14) 0.0258(2) 0.000 0.000 0.000 Cl1 0.0241(2) 0.0303(2) 0.0354(3) 0.00727(18) -0.00387(18) 0.00089(17) _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 N3 1.8827(14) 6_464 ? Co1 N3 1.8827(14) . ? Co1 O2 1.9216(13) . ? Co1 O2 1.9216(12) 6_464 ? Co1 N6 1.9402(15) 6_464 ? Co1 N6 1.9402(15) . ? O2 C1 1.301(2) . ? O1 C1 1.222(2) . ? C1 C2 1.523(2) . ? C2 N3 1.277(2) . ? C2 C8 1.489(2) . ? N3 C4 1.470(2) . ? C4 C5 1.523(2) . ? C5 N6 1.507(2) . ? N6 C7 1.498(2) . ? C7 C7 1.505(4) 6_464 ? Zn1 Cl1 2.2813(7) 15_565 ? Zn1 Cl1 2.2813(7) 12_766 ? Zn1 Cl1 2.2813(7) . ? Zn1 Cl1 2.2813(7) 6_564 ? 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 N3 Co1 N3 178.43(9) 6_464 . ? N3 Co1 O2 94.61(5) 6_464 . ? N3 Co1 O2 84.26(5) . . ? N3 Co1 O2 84.26(5) 6_464 6_464 ? N3 Co1 O2 94.61(5) . 6_464 ? O2 Co1 O2 88.65(8) . 6_464 ? N3 Co1 N6 86.44(6) 6_464 6_464 ? N3 Co1 N6 94.69(6) . 6_464 ? O2 Co1 N6 92.33(6) . 6_464 ? O2 Co1 N6 170.70(5) 6_464 6_464 ? N3 Co1 N6 94.69(6) 6_464 . ? N3 Co1 N6 86.44(6) . . ? O2 Co1 N6 170.70(5) . . ? O2 Co1 N6 92.33(6) 6_464 . ? N6 Co1 N6 88.20(9) 6_464 . ? C1 O2 Co1 111.44(10) . . ? O1 C1 O2 125.13(17) . . ? O1 C1 C2 120.03(16) . . ? O2 C1 C2 114.81(15) . . ? N3 C2 C8 127.39(16) . . ? N3 C2 C1 111.68(15) . . ? C8 C2 C1 120.93(15) . . ? C2 N3 C4 127.84(14) . . ? C2 N3 Co1 116.17(12) . . ? C4 N3 Co1 115.99(11) . . ? N3 C4 C5 105.16(14) . . ? N6 C5 C4 110.19(14) . . ? C7 N6 C5 115.89(14) . . ? C7 N6 Co1 109.24(12) . . ? C5 N6 Co1 107.09(10) . . ? N6 C7 C7 109.52(11) . 6_464 ? Cl1 Zn1 Cl1 111.83(4) 15_565 12_766 ? Cl1 Zn1 Cl1 108.303(17) 15_565 . ? Cl1 Zn1 Cl1 108.303(17) 12_766 . ? Cl1 Zn1 Cl1 108.303(17) 15_565 6_564 ? Cl1 Zn1 Cl1 108.303(17) 12_766 6_564 ? Cl1 Zn1 Cl1 111.83(4) . 6_564 ? 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 N3 Co1 O2 C1 -168.76(12) 6_464 . . . ? N3 Co1 O2 C1 10.14(12) . . . . ? O2 Co1 O2 C1 -84.63(12) 6_464 . . . ? N6 Co1 O2 C1 104.62(12) 6_464 . . . ? N6 Co1 O2 C1 11.5(4) . . . . ? Co1 O2 C1 O1 164.15(17) . . . . ? Co1 O2 C1 C2 -14.16(18) . . . . ? O1 C1 C2 N3 -166.74(18) . . . . ? O2 C1 C2 N3 11.7(2) . . . . ? O1 C1 C2 C8 13.1(3) . . . . ? O2 C1 C2 C8 -168.50(16) . . . . ? C8 C2 N3 C4 -3.2(3) . . . . ? C1 C2 N3 C4 176.65(15) . . . . ? C8 C2 N3 Co1 177.26(14) . . . . ? C1 C2 N3 Co1 -2.92(18) . . . . ? N3 Co1 N3 C2 40.58(12) 6_464 . . . ? O2 Co1 N3 C2 -3.56(12) . . . . ? O2 Co1 N3 C2 84.62(13) 6_464 . . . ? N6 Co1 N3 C2 -95.43(13) 6_464 . . . ? N6 Co1 N3 C2 176.67(13) . . . . ? N3 Co1 N3 C4 -139.05(11) 6_464 . . . ? O2 Co1 N3 C4 176.82(12) . . . . ? O2 Co1 N3 C4 -95.01(12) 6_464 . . . ? N6 Co1 N3 C4 84.94(12) 6_464 . . . ? N6 Co1 N3 C4 -2.96(12) . . . . ? C2 N3 C4 C5 -155.06(17) . . . . ? Co1 N3 C4 C5 24.52(16) . . . . ? N3 C4 C5 N6 -40.47(18) . . . . ? C4 C5 N6 C7 -83.25(18) . . . . ? C4 C5 N6 Co1 38.92(16) . . . . ? N3 Co1 N6 C7 -74.84(11) 6_464 . . . ? N3 Co1 N6 C7 106.25(11) . . . . ? O2 Co1 N6 C7 104.9(4) . . . . ? O2 Co1 N6 C7 -159.28(11) 6_464 . . . ? N6 Co1 N6 C7 11.44(8) 6_464 . . . ? N3 Co1 N6 C5 158.92(11) 6_464 . . . ? N3 Co1 N6 C5 -19.99(11) . . . . ? O2 Co1 N6 C5 -21.4(4) . . . . ? O2 Co1 N6 C5 74.48(11) 6_464 . . . ? N6 Co1 N6 C5 -114.80(12) 6_464 . . . ? C5 N6 C7 C7 89.2(2) . . . 6_464 ? Co1 N6 C7 C7 -31.9(2) . . . 6_464 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.254 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.049 #===END data_compound5 #m-[Co(Aimen)2]2ZnCl4 _database_code_CSD 176559 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 Cl2 Co N4 O5 Zn0.50' _chemical_formula_weight 436.80 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' 'Zn' 'Zn' 0.2839 1.4301 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.501(3) _cell_length_b 19.753(4) _cell_length_c 14.227(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.397(7) _cell_angle_gamma 90.00 _cell_volume 3270.9(12) _cell_formula_units_Z 8 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 2.119 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7918 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995)A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41392 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.41 _reflns_number_total 6690 _reflns_number_gt 5742 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0520P)^2^+3.9734P] 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 6690 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.001 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 Zn1 Zn 0.30974(3) 0.562601(16) 0.70078(2) 0.02068(9) Uani 1 1 d . . . Co2 Co 0.02469(3) 0.711728(17) 0.41025(3) 0.01435(9) Uani 1 1 d . . . Co1 Co 0.56856(3) 0.750147(18) 0.53372(3) 0.01567(10) Uani 1 1 d . . . Cl4 Cl 0.38087(6) 0.67049(4) 0.70648(5) 0.02401(16) Uani 1 1 d . . . Cl3 Cl 0.43770(6) 0.48285(4) 0.78705(6) 0.02732(16) Uani 1 1 d . . . Cl2 Cl 0.17250(7) 0.57089(4) 0.76728(7) 0.03122(18) Uani 1 1 d . . . Cl1 Cl 0.24955(8) 0.53724(4) 0.53174(6) 0.03484(19) Uani 1 1 d . . . O21 O 0.17592(16) 0.71406(10) 0.40330(14) 0.0197(4) Uani 1 1 d . . . O1 O 0.61642(16) 0.76003(10) 0.67733(14) 0.0190(4) Uani 1 1 d . . . O22 O 0.28204(17) 0.65966(11) 0.33033(16) 0.0273(5) Uani 1 1 d . . . O31 O -0.03836(17) 0.76614(10) 0.29116(14) 0.0201(4) Uani 1 1 d . . . N12 N 0.4108(2) 0.76459(13) 0.52379(17) 0.0210(5) Uani 1 1 d . . . H12A H 0.3664 0.7279 0.4932 0.025 Uiso 1 1 calc R . . H12B H 0.4083 0.7692 0.5873 0.025 Uiso 1 1 calc R . . O2 O 0.68724(18) 0.69732(11) 0.81742(15) 0.0258(5) Uani 1 1 d . . . O12 O 0.85822(17) 0.83442(12) 0.55464(17) 0.0301(5) Uani 1 1 d . . . O11 O 0.72581(17) 0.75532(10) 0.54411(14) 0.0206(4) Uani 1 1 d . . . N21 N 0.01375(19) 0.63011(11) 0.34008(16) 0.0168(5) Uani 1 1 d . . . C13 C 0.4589(2) 0.87884(15) 0.4887(2) 0.0219(6) Uani 1 1 d . . . H13A H 0.4446 0.9111 0.4321 0.026 Uiso 1 1 calc R . . H13B H 0.4622 0.9047 0.5493 0.026 Uiso 1 1 calc R . . N32 N 0.0876(2) 0.67249(12) 0.54492(16) 0.0182(5) Uani 1 1 d . . . H32A H 0.0484 0.6335 0.5475 0.022 Uiso 1 1 calc R . . H32B H 0.1637 0.6617 0.5607 0.022 Uiso 1 1 calc R . . C11 C 0.7598(2) 0.81703(15) 0.5401(2) 0.0202(6) Uani 1 1 d . . . C21 C 0.1946(2) 0.66543(14) 0.3511(2) 0.0198(6) Uani 1 1 d . . . N1 N 0.5786(2) 0.65712(11) 0.56410(17) 0.0185(5) Uani 1 1 d . . . N22 N -0.1322(2) 0.69429(12) 0.39893(17) 0.0192(5) Uani 1 1 d . . . H22A H -0.1334 0.6745 0.4570 0.023 Uiso 1 1 calc R . . H22B H -0.1733 0.7340 0.3883 0.023 Uiso 1 1 calc R . . N31 N 0.0444(2) 0.79510(11) 0.47688(17) 0.0168(5) Uani 1 1 d . . . O32 O -0.09473(18) 0.87354(11) 0.24916(16) 0.0267(5) Uani 1 1 d . . . C12 C 0.6636(2) 0.86973(14) 0.5153(2) 0.0185(5) Uani 1 1 d . . . N2 N 0.5252(2) 0.72193(12) 0.39419(17) 0.0228(5) Uani 1 1 d . . . H2A H 0.4466 0.7230 0.3623 0.027 Uiso 1 1 calc R . . H2B H 0.5573 0.7503 0.3604 0.027 Uiso 1 1 calc R . . C1 C 0.6445(2) 0.70322(14) 0.7249(2) 0.0192(6) Uani 1 1 d . . . C32 C 0.0109(2) 0.84749(14) 0.4217(2) 0.0204(6) Uani 1 1 d . . . C33 C 0.1027(2) 0.79205(14) 0.5872(2) 0.0204(6) Uani 1 1 d . . . H33A H 0.0741 0.8282 0.6201 0.024 Uiso 1 1 calc R . . H33B H 0.1867 0.7977 0.6062 0.024 Uiso 1 1 calc R . . C25 C 0.1058(3) 0.55154(16) 0.2578(2) 0.0298(7) Uani 1 1 d . . . H25A H 0.0345 0.5255 0.2409 0.045 Uiso 1 1 calc R . . H25B H 0.1708 0.5238 0.2996 0.045 Uiso 1 1 calc R . . H25C H 0.1171 0.5646 0.1956 0.045 Uiso 1 1 calc R . . C22 C 0.0983(2) 0.61380(14) 0.3150(2) 0.0192(6) Uani 1 1 d . . . C4 C 0.5689(3) 0.65165(15) 0.3958(2) 0.0254(6) Uani 1 1 d . . . H4A H 0.6527 0.6526 0.4105 0.030 Uiso 1 1 calc R . . H4B H 0.5307 0.6301 0.3291 0.030 Uiso 1 1 calc R . . C14 C 0.3642(4) 0.8278(2) 0.4627(4) 0.0504(10) Uani 1 1 d . . . H14A H 0.3366 0.8172 0.3897 0.060 Uiso 1 1 calc R . . H14B H 0.2990 0.8459 0.4787 0.060 Uiso 1 1 calc R . . C31 C -0.0460(2) 0.82948(14) 0.3106(2) 0.0199(6) Uani 1 1 d . . . C34 C 0.0756(2) 0.72329(14) 0.6186(2) 0.0199(6) Uani 1 1 d . . . H34A H 0.1294 0.7124 0.6876 0.024 Uiso 1 1 calc R . . H34B H -0.0036 0.7226 0.6184 0.024 Uiso 1 1 calc R . . N11 N 0.5680(2) 0.84350(11) 0.50828(17) 0.0181(5) Uani 1 1 d . . . C35 C 0.0231(3) 0.91915(15) 0.4561(3) 0.0330(8) Uani 1 1 d . . . H35A H 0.0610 0.9207 0.5297 0.050 Uiso 1 1 calc R . . H35B H -0.0531 0.9400 0.4364 0.050 Uiso 1 1 calc R . . H35C H 0.0694 0.9440 0.4249 0.050 Uiso 1 1 calc R . . C3 C 0.5445(3) 0.61165(14) 0.4762(2) 0.0233(6) Uani 1 1 d . . . H3A H 0.4619 0.6001 0.4542 0.028 Uiso 1 1 calc R . . H3B H 0.5901 0.5693 0.4922 0.028 Uiso 1 1 calc R . . C24 C -0.1828(2) 0.64741(16) 0.3106(2) 0.0247(6) Uani 1 1 d . . . H24A H -0.2020 0.6728 0.2466 0.030 Uiso 1 1 calc R . . H24B H -0.2539 0.6264 0.3124 0.030 Uiso 1 1 calc R . . C23 C -0.0943(2) 0.59332(15) 0.3177(2) 0.0231(6) Uani 1 1 d . . . H23A H -0.0884 0.5607 0.3721 0.028 Uiso 1 1 calc R . . H23B H -0.1147 0.5684 0.2531 0.028 Uiso 1 1 calc R . . C15 C 0.6875(3) 0.94246(15) 0.5046(2) 0.0277(7) Uani 1 1 d . . . H15A H 0.6173 0.9689 0.4921 0.041 Uiso 1 1 calc R . . H15B H 0.7135 0.9481 0.4479 0.041 Uiso 1 1 calc R . . H15C H 0.7475 0.9584 0.5669 0.041 Uiso 1 1 calc R . . C5 C 0.6443(3) 0.57203(15) 0.7010(2) 0.0282(7) Uani 1 1 d . . . H5A H 0.6244 0.5386 0.6465 0.042 Uiso 1 1 calc R . . H5B H 0.5979 0.5640 0.7425 0.042 Uiso 1 1 calc R . . H5C H 0.7259 0.5679 0.7430 0.042 Uiso 1 1 calc R . . C2 C 0.6209(2) 0.64100(14) 0.6573(2) 0.0195(6) Uani 1 1 d . . . O2W O -0.1172(2) 0.60010(12) 0.55390(17) 0.0374(6) Uani 1 1 d . . . O1W O 0.3270(4) 0.8960(3) 0.6631(3) 0.1090(17) 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 Zn1 0.01956(17) 0.01921(17) 0.02195(18) 0.00046(12) 0.00599(14) 0.00024(12) Co2 0.01390(18) 0.01588(18) 0.01356(18) -0.00118(13) 0.00535(14) 0.00003(13) Co1 0.01652(19) 0.01748(19) 0.01328(18) -0.00037(13) 0.00573(15) -0.00103(14) Cl4 0.0249(4) 0.0227(3) 0.0258(4) 0.0001(3) 0.0110(3) -0.0053(3) Cl3 0.0275(4) 0.0249(4) 0.0276(4) 0.0031(3) 0.0076(3) 0.0069(3) Cl2 0.0277(4) 0.0251(4) 0.0473(5) 0.0029(3) 0.0213(4) -0.0001(3) Cl1 0.0464(5) 0.0273(4) 0.0224(4) -0.0048(3) 0.0025(3) 0.0049(3) O21 0.0159(9) 0.0241(10) 0.0195(10) -0.0042(8) 0.0068(8) -0.0024(8) O1 0.0199(10) 0.0216(10) 0.0141(9) -0.0013(7) 0.0047(8) -0.0014(8) O22 0.0185(10) 0.0389(12) 0.0278(11) -0.0025(9) 0.0123(9) 0.0025(9) O31 0.0226(10) 0.0216(10) 0.0166(9) 0.0007(8) 0.0077(8) 0.0005(8) N12 0.0179(12) 0.0280(13) 0.0164(11) 0.0008(10) 0.0053(9) -0.0045(10) O2 0.0256(11) 0.0342(12) 0.0159(10) 0.0020(8) 0.0053(9) -0.0006(9) O12 0.0165(11) 0.0378(13) 0.0365(12) 0.0067(10) 0.0103(9) -0.0006(9) O11 0.0193(10) 0.0235(10) 0.0203(10) 0.0015(8) 0.0090(8) 0.0029(8) N21 0.0172(11) 0.0191(11) 0.0129(10) -0.0008(9) 0.0043(9) 0.0000(9) C13 0.0167(14) 0.0248(15) 0.0233(14) -0.0009(11) 0.0065(12) 0.0029(11) N32 0.0191(12) 0.0180(11) 0.0172(11) -0.0004(9) 0.0064(9) 0.0011(9) C11 0.0188(14) 0.0271(15) 0.0166(13) 0.0023(11) 0.0088(11) 0.0012(11) C21 0.0177(14) 0.0260(15) 0.0157(13) 0.0011(11) 0.0060(11) 0.0025(11) N1 0.0178(12) 0.0189(11) 0.0195(12) -0.0027(9) 0.0077(9) -0.0016(9) N22 0.0172(11) 0.0230(12) 0.0185(11) -0.0009(9) 0.0075(9) 0.0009(9) N31 0.0179(11) 0.0195(11) 0.0149(11) -0.0019(9) 0.0082(9) -0.0007(9) O32 0.0290(12) 0.0275(11) 0.0255(11) 0.0090(9) 0.0120(9) 0.0053(9) C12 0.0203(14) 0.0203(13) 0.0155(13) 0.0000(10) 0.0070(11) -0.0015(11) N2 0.0271(13) 0.0254(13) 0.0159(11) 0.0004(9) 0.0079(10) 0.0006(10) C1 0.0151(13) 0.0264(15) 0.0178(13) -0.0009(11) 0.0082(11) -0.0027(11) C32 0.0249(15) 0.0189(14) 0.0227(14) 0.0006(11) 0.0152(12) 0.0000(11) C33 0.0209(14) 0.0222(14) 0.0168(13) -0.0025(11) 0.0054(11) -0.0009(11) C25 0.0343(18) 0.0263(16) 0.0329(17) -0.0072(13) 0.0172(14) 0.0014(13) C22 0.0209(14) 0.0196(13) 0.0160(13) 0.0008(10) 0.0054(11) 0.0034(11) C4 0.0299(16) 0.0276(16) 0.0202(14) -0.0052(12) 0.0111(13) 0.0029(13) C14 0.044(2) 0.047(2) 0.065(3) 0.002(2) 0.025(2) 0.0037(18) C31 0.0189(14) 0.0240(14) 0.0194(13) 0.0034(11) 0.0102(11) 0.0001(11) C34 0.0232(14) 0.0215(14) 0.0147(13) -0.0003(11) 0.0066(11) 0.0017(11) N11 0.0203(12) 0.0196(11) 0.0152(11) -0.0003(9) 0.0074(9) 0.0006(9) C35 0.055(2) 0.0179(14) 0.0310(17) 0.0008(12) 0.0213(16) -0.0005(14) C3 0.0257(15) 0.0199(14) 0.0209(14) -0.0061(11) 0.0045(12) -0.0010(12) C24 0.0158(14) 0.0341(17) 0.0231(15) -0.0064(12) 0.0057(12) -0.0033(12) C23 0.0219(15) 0.0223(14) 0.0259(15) -0.0070(12) 0.0095(12) -0.0067(11) C15 0.0256(16) 0.0229(15) 0.0349(17) 0.0022(13) 0.0115(14) -0.0038(12) C5 0.0264(16) 0.0260(16) 0.0301(16) 0.0082(13) 0.0080(13) 0.0017(12) C2 0.0149(13) 0.0228(14) 0.0215(14) 0.0019(11) 0.0073(11) -0.0016(11) O2W 0.0531(16) 0.0356(13) 0.0249(11) -0.0003(10) 0.0159(11) -0.0162(11) O1W 0.099(3) 0.173(5) 0.056(2) -0.012(3) 0.029(2) -0.077(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl2 2.2472(9) . ? Zn1 Cl3 2.2614(8) . ? Zn1 Cl1 2.2980(9) . ? Zn1 Cl4 2.2992(9) . ? Co2 N31 1.871(2) . ? Co2 N21 1.875(2) . ? Co2 O31 1.9165(19) . ? Co2 O21 1.929(2) . ? Co2 N22 1.939(2) . ? Co2 N32 1.947(2) . ? Co1 N11 1.879(2) . ? Co1 N1 1.881(2) . ? Co1 O1 1.9180(19) . ? Co1 O11 1.919(2) . ? Co1 N2 1.939(2) . ? Co1 N12 1.947(2) . ? O21 C21 1.286(3) . ? O1 C1 1.291(3) . ? O22 C21 1.238(3) . ? O31 C31 1.292(4) . ? N12 C14 1.511(5) . ? O2 C1 1.232(3) . ? O12 C11 1.220(4) . ? O11 C11 1.299(4) . ? N21 C22 1.274(4) . ? N21 C23 1.462(4) . ? C13 N11 1.465(4) . ? C13 C14 1.495(5) . ? N32 C34 1.497(3) . ? C11 C12 1.531(4) . ? C21 C22 1.517(4) . ? N1 C2 1.276(4) . ? N1 C3 1.471(3) . ? N22 C24 1.502(4) . ? N31 C32 1.274(4) . ? N31 C33 1.471(3) . ? O32 C31 1.227(3) . ? C12 N11 1.272(4) . ? C12 C15 1.486(4) . ? N2 C4 1.489(4) . ? C1 C2 1.522(4) . ? C32 C35 1.487(4) . ? C32 C31 1.519(4) . ? C33 C34 1.506(4) . ? C25 C22 1.496(4) . ? C4 C3 1.510(4) . ? C24 C23 1.515(4) . ? C5 C2 1.482(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Zn1 Cl3 108.65(3) . . ? Cl2 Zn1 Cl1 116.60(4) . . ? Cl3 Zn1 Cl1 108.23(3) . . ? Cl2 Zn1 Cl4 105.22(3) . . ? Cl3 Zn1 Cl4 116.02(3) . . ? Cl1 Zn1 Cl4 102.34(3) . . ? N31 Co2 N21 175.70(10) . . ? N31 Co2 O31 83.68(9) . . ? N21 Co2 O31 94.87(9) . . ? N31 Co2 O21 93.14(9) . . ? N21 Co2 O21 82.86(9) . . ? O31 Co2 O21 92.06(8) . . ? N31 Co2 N22 98.08(10) . . ? N21 Co2 N22 85.87(10) . . ? O31 Co2 N22 87.07(9) . . ? O21 Co2 N22 168.58(9) . . ? N31 Co2 N32 85.44(10) . . ? N21 Co2 N32 96.12(10) . . ? O31 Co2 N32 168.95(9) . . ? O21 Co2 N32 90.50(9) . . ? N22 Co2 N32 92.52(10) . . ? N11 Co1 N1 176.51(10) . . ? N11 Co1 O1 94.77(9) . . ? N1 Co1 O1 83.45(9) . . ? N11 Co1 O11 83.92(9) . . ? N1 Co1 O11 93.07(9) . . ? O1 Co1 O11 89.99(8) . . ? N11 Co1 N2 96.02(10) . . ? N1 Co1 N2 85.69(10) . . ? O1 Co1 N2 169.07(9) . . ? O11 Co1 N2 89.42(10) . . ? N11 Co1 N12 84.84(10) . . ? N1 Co1 N12 98.10(10) . . ? O1 Co1 N12 88.65(9) . . ? O11 Co1 N12 168.52(10) . . ? N2 Co1 N12 94.05(10) . . ? C21 O21 Co2 113.53(17) . . ? C1 O1 Co1 112.91(17) . . ? C31 O31 Co2 113.10(17) . . ? C14 N12 Co1 109.3(2) . . ? C11 O11 Co1 112.87(17) . . ? C22 N21 C23 127.4(2) . . ? C22 N21 Co2 117.4(2) . . ? C23 N21 Co2 115.19(17) . . ? N11 C13 C14 108.9(3) . . ? C34 N32 Co2 108.32(16) . . ? O12 C11 O11 125.6(3) . . ? O12 C11 C12 120.4(3) . . ? O11 C11 C12 114.0(2) . . ? O22 C21 O21 124.7(3) . . ? O22 C21 C22 121.2(3) . . ? O21 C21 C22 114.1(2) . . ? C2 N1 C3 127.8(2) . . ? C2 N1 Co1 116.8(2) . . ? C3 N1 Co1 115.27(18) . . ? C24 N22 Co2 106.47(17) . . ? C32 N31 C33 127.9(2) . . ? C32 N31 Co2 116.71(19) . . ? C33 N31 Co2 115.27(17) . . ? N11 C12 C15 127.1(3) . . ? N11 C12 C11 112.2(2) . . ? C15 C12 C11 120.7(2) . . ? C4 N2 Co1 106.74(17) . . ? O2 C1 O1 124.8(3) . . ? O2 C1 C2 120.5(3) . . ? O1 C1 C2 114.7(2) . . ? N31 C32 C35 126.8(3) . . ? N31 C32 C31 112.0(2) . . ? C35 C32 C31 121.2(3) . . ? N31 C33 C34 106.0(2) . . ? N21 C22 C25 125.7(3) . . ? N21 C22 C21 111.8(2) . . ? C25 C22 C21 122.5(3) . . ? N2 C4 C3 109.0(2) . . ? C13 C14 N12 108.1(3) . . ? O32 C31 O31 126.2(3) . . ? O32 C31 C32 119.8(3) . . ? O31 C31 C32 114.0(2) . . ? N32 C34 C33 107.9(2) . . ? C12 N11 C13 127.1(2) . . ? C12 N11 Co1 116.6(2) . . ? C13 N11 Co1 116.21(18) . . ? N1 C3 C4 104.4(2) . . ? N22 C24 C23 107.8(2) . . ? N21 C23 C24 104.9(2) . . ? N1 C2 C5 127.5(3) . . ? N1 C2 C1 111.5(2) . . ? C5 C2 C1 120.9(2) . . ? 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 N31 Co2 O21 C21 -173.59(19) . . . . ? N21 Co2 O21 C21 4.85(19) . . . . ? O31 Co2 O21 C21 -89.81(19) . . . . ? N22 Co2 O21 C21 -4.4(6) . . . . ? N32 Co2 O21 C21 100.95(19) . . . . ? N11 Co1 O1 C1 -169.58(19) . . . . ? N1 Co1 O1 C1 7.41(19) . . . . ? O11 Co1 O1 C1 -85.68(18) . . . . ? N2 Co1 O1 C1 1.2(6) . . . . ? N12 Co1 O1 C1 105.72(19) . . . . ? N31 Co2 O31 C31 -4.82(19) . . . . ? N21 Co2 O31 C31 179.25(19) . . . . ? O21 Co2 O31 C31 -97.74(19) . . . . ? N22 Co2 O31 C31 93.65(19) . . . . ? N32 Co2 O31 C31 5.5(6) . . . . ? N11 Co1 N12 C14 23.0(2) . . . . ? N1 Co1 N12 C14 -158.9(2) . . . . ? O1 Co1 N12 C14 117.9(2) . . . . ? O11 Co1 N12 C14 34.6(6) . . . . ? N2 Co1 N12 C14 -72.7(2) . . . . ? N11 Co1 O11 C11 6.55(18) . . . . ? N1 Co1 O11 C11 -171.69(18) . . . . ? O1 Co1 O11 C11 -88.25(18) . . . . ? N2 Co1 O11 C11 102.66(19) . . . . ? N12 Co1 O11 C11 -5.1(5) . . . . ? N31 Co2 N21 C22 18.0(14) . . . . ? O31 Co2 N21 C22 88.1(2) . . . . ? O21 Co2 N21 C22 -3.4(2) . . . . ? N22 Co2 N21 C22 174.8(2) . . . . ? N32 Co2 N21 C22 -93.1(2) . . . . ? N31 Co2 N21 C23 -160.2(13) . . . . ? O31 Co2 N21 C23 -90.04(19) . . . . ? O21 Co2 N21 C23 178.5(2) . . . . ? N22 Co2 N21 C23 -3.34(19) . . . . ? N32 Co2 N21 C23 88.8(2) . . . . ? N31 Co2 N32 C34 19.62(18) . . . . ? N21 Co2 N32 C34 -164.40(18) . . . . ? O31 Co2 N32 C34 9.4(6) . . . . ? O21 Co2 N32 C34 112.73(18) . . . . ? N22 Co2 N32 C34 -78.29(18) . . . . ? Co1 O11 C11 O12 172.5(2) . . . . ? Co1 O11 C11 C12 -7.0(3) . . . . ? Co2 O21 C21 O22 174.4(2) . . . . ? Co2 O21 C21 C22 -5.3(3) . . . . ? N11 Co1 N1 C2 52.4(17) . . . . ? O1 Co1 N1 C2 -7.1(2) . . . . ? O11 Co1 N1 C2 82.6(2) . . . . ? N2 Co1 N1 C2 171.7(2) . . . . ? N12 Co1 N1 C2 -94.8(2) . . . . ? N11 Co1 N1 C3 -123.1(16) . . . . ? O1 Co1 N1 C3 177.4(2) . . . . ? O11 Co1 N1 C3 -93.0(2) . . . . ? N2 Co1 N1 C3 -3.8(2) . . . . ? N12 Co1 N1 C3 89.7(2) . . . . ? N31 Co2 N22 C24 155.50(18) . . . . ? N21 Co2 N22 C24 -22.79(18) . . . . ? O31 Co2 N22 C24 72.31(18) . . . . ? O21 Co2 N22 C24 -13.6(6) . . . . ? N32 Co2 N22 C24 -118.75(18) . . . . ? N21 Co2 N31 C32 70.8(14) . . . . ? O31 Co2 N31 C32 0.3(2) . . . . ? O21 Co2 N31 C32 92.0(2) . . . . ? N22 Co2 N31 C32 -85.8(2) . . . . ? N32 Co2 N31 C32 -177.7(2) . . . . ? N21 Co2 N31 C33 -106.0(13) . . . . ? O31 Co2 N31 C33 -176.5(2) . . . . ? O21 Co2 N31 C33 -84.82(19) . . . . ? N22 Co2 N31 C33 97.34(19) . . . . ? N32 Co2 N31 C33 5.43(19) . . . . ? O12 C11 C12 N11 -176.1(3) . . . . ? O11 C11 C12 N11 3.4(3) . . . . ? O12 C11 C12 C15 2.4(4) . . . . ? O11 C11 C12 C15 -178.0(2) . . . . ? N11 Co1 N2 C4 155.04(19) . . . . ? N1 Co1 N2 C4 -21.90(19) . . . . ? O1 Co1 N2 C4 -15.7(6) . . . . ? O11 Co1 N2 C4 71.22(19) . . . . ? N12 Co1 N2 C4 -119.73(19) . . . . ? Co1 O1 C1 O2 173.4(2) . . . . ? Co1 O1 C1 C2 -6.6(3) . . . . ? C33 N31 C32 C35 0.0(5) . . . . ? Co2 N31 C32 C35 -176.4(2) . . . . ? C33 N31 C32 C31 179.9(2) . . . . ? Co2 N31 C32 C31 3.5(3) . . . . ? C32 N31 C33 C34 155.0(3) . . . . ? Co2 N31 C33 C34 -28.6(3) . . . . ? C23 N21 C22 C25 -1.3(5) . . . . ? Co2 N21 C22 C25 -179.2(2) . . . . ? C23 N21 C22 C21 179.3(2) . . . . ? Co2 N21 C22 C21 1.4(3) . . . . ? O22 C21 C22 N21 -177.0(3) . . . . ? O21 C21 C22 N21 2.7(3) . . . . ? O22 C21 C22 C25 3.5(4) . . . . ? O21 C21 C22 C25 -176.7(3) . . . . ? Co1 N2 C4 C3 43.2(3) . . . . ? N11 C13 C14 N12 34.6(4) . . . . ? Co1 N12 C14 C13 -37.5(3) . . . . ? Co2 O31 C31 O32 -171.2(2) . . . . ? Co2 O31 C31 C32 7.7(3) . . . . ? N31 C32 C31 O32 171.5(3) . . . . ? C35 C32 C31 O32 -8.6(4) . . . . ? N31 C32 C31 O31 -7.5(3) . . . . ? C35 C32 C31 O31 172.4(3) . . . . ? Co2 N32 C34 C33 -39.9(3) . . . . ? N31 C33 C34 N32 43.3(3) . . . . ? C15 C12 N11 C13 -0.5(5) . . . . ? C11 C12 N11 C13 178.0(2) . . . . ? C15 C12 N11 Co1 -176.3(2) . . . . ? C11 C12 N11 Co1 2.1(3) . . . . ? C14 C13 N11 C12 166.9(3) . . . . ? C14 C13 N11 Co1 -17.3(3) . . . . ? N1 Co1 N11 C12 25.6(17) . . . . ? O1 Co1 N11 C12 84.7(2) . . . . ? O11 Co1 N11 C12 -4.7(2) . . . . ? N2 Co1 N11 C12 -93.5(2) . . . . ? N12 Co1 N11 C12 172.9(2) . . . . ? N1 Co1 N11 C13 -150.7(16) . . . . ? O1 Co1 N11 C13 -91.56(19) . . . . ? O11 Co1 N11 C13 179.0(2) . . . . ? N2 Co1 N11 C13 90.2(2) . . . . ? N12 Co1 N11 C13 -3.36(19) . . . . ? C2 N1 C3 C4 -147.3(3) . . . . ? Co1 N1 C3 C4 27.7(3) . . . . ? N2 C4 C3 N1 -45.2(3) . . . . ? Co2 N22 C24 C23 43.8(3) . . . . ? C22 N21 C23 C24 -149.8(3) . . . . ? Co2 N21 C23 C24 28.1(3) . . . . ? N22 C24 C23 N21 -45.8(3) . . . . ? C3 N1 C2 C5 -1.4(5) . . . . ? Co1 N1 C2 C5 -176.3(2) . . . . ? C3 N1 C2 C1 -180.0(2) . . . . ? Co1 N1 C2 C1 5.2(3) . . . . ? O2 C1 C2 N1 -178.9(3) . . . . ? O1 C1 C2 N1 1.1(3) . . . . ? O2 C1 C2 C5 2.5(4) . . . . ? O1 C1 C2 C5 -177.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.759 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.090 #===END #mffma-[Co(Eimtetraen)]ZnCl4 data_jmbi _database_code_CSD 176560 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H26 Cl4 Co N5 O6 Zn' _chemical_formula_weight 614.49 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 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' _cell_length_a 14.131(5) _cell_length_b 9.479(3) _cell_length_c 17.514(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2345.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 2.224 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7754 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing Acta Cryst. (1995)A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26513 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 26.39 _reflns_number_total 4746 _reflns_number_gt 4547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0439P)^2^+1.6735P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.029(12) _refine_ls_number_reflns 4746 _refine_ls_number_parameters 301 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.09112(2) 0.71826(4) 0.14693(3) 0.02235(9) Uani 1 1 d . . . O1 O -0.22541(14) 0.7358(2) 0.13027(12) 0.0248(4) Uani 1 1 d . . . N1 N -0.10137(18) 0.5771(3) 0.07209(17) 0.0290(6) Uani 1 1 d . . . N3 N -0.1132(2) 0.5859(3) 0.23188(17) 0.0320(6) Uani 1 1 d . . . H3 H -0.1656 0.5302 0.2208 0.038 Uiso 1 1 calc R . . N4 N -0.09257(18) 0.8622(3) 0.22509(16) 0.0284(6) Uani 1 1 d . . . H4 H -0.0324 0.8689 0.2462 0.034 Uiso 1 1 calc R . . N5 N -0.0685(2) 0.8723(3) 0.07551(16) 0.0287(5) Uani 1 1 d . . . H5A H -0.0153 0.8535 0.0470 0.034 Uiso 1 1 calc R . . H5B H -0.1190 0.8804 0.0427 0.034 Uiso 1 1 calc R . . N2 N 0.04250(17) 0.6674(3) 0.1521(2) 0.0316(5) Uani 1 1 d . . . H2 H 0.0780 0.7500 0.1539 0.038 Uiso 1 1 calc R . . C1 C -0.2600(2) 0.6417(3) 0.08572(17) 0.0270(6) Uani 1 1 d . . . C8 C -0.1592(2) 0.8134(4) 0.28495(19) 0.0344(7) Uani 1 1 d . . . H8A H -0.2251 0.8158 0.2658 0.041 Uiso 1 1 calc R . . H8B H -0.1548 0.8743 0.3307 0.041 Uiso 1 1 calc R . . C3 C -0.0145(3) 0.4994(4) 0.0519(3) 0.0420(9) Uani 1 1 d . . . H3A H -0.0104 0.4860 -0.0041 0.050 Uiso 1 1 calc R . . H3B H -0.0139 0.4056 0.0768 0.050 Uiso 1 1 calc R . . C10 C -0.0555(2) 1.0074(3) 0.1181(2) 0.0313(7) Uani 1 1 d . . . H10A H -0.0749 1.0884 0.0860 0.038 Uiso 1 1 calc R . . H10B H 0.0117 1.0197 0.1326 0.038 Uiso 1 1 calc R . . C9 C -0.1165(3) 0.9991(3) 0.1883(2) 0.0328(7) Uani 1 1 d . . . H9A H -0.1027 1.0786 0.2232 0.039 Uiso 1 1 calc R . . H9B H -0.1844 1.0020 0.1743 0.039 Uiso 1 1 calc R . . C2 C -0.1856(2) 0.5452(3) 0.0500(2) 0.0318(7) Uani 1 1 d . . . C5 C 0.0593(3) 0.5878(4) 0.2234(3) 0.0423(9) Uani 1 1 d . . . H5A' H 0.0681 0.6539 0.2666 0.051 Uiso 1 1 calc R . . H5B' H 0.1172 0.5297 0.2184 0.051 Uiso 1 1 calc R . . C7 C -0.1308(3) 0.6653(4) 0.3040(2) 0.0383(8) Uani 1 1 d . . . H7A H -0.0728 0.6661 0.3356 0.046 Uiso 1 1 calc R . . H7B H -0.1817 0.6187 0.3335 0.046 Uiso 1 1 calc R . . C4 C 0.0679(3) 0.5890(4) 0.0803(3) 0.0418(9) Uani 1 1 d . . . H4A H 0.1231 0.5274 0.0903 0.050 Uiso 1 1 calc R . . H4B H 0.0860 0.6574 0.0402 0.050 Uiso 1 1 calc R . . C6 C -0.0264(3) 0.4934(4) 0.2379(3) 0.0444(10) Uani 1 1 d . . . H6A H -0.0291 0.4168 0.1995 0.053 Uiso 1 1 calc R . . H6B H -0.0225 0.4504 0.2893 0.053 Uiso 1 1 calc R . . Zn1 Zn -0.10611(3) -0.00652(4) -0.11657(3) 0.03514(10) Uani 1 1 d . . . Cl4 Cl -0.13706(6) 0.04579(9) -0.23991(5) 0.03475(17) Uani 1 1 d . . . Cl3 Cl -0.2424(6) -0.0302(11) -0.0459(4) 0.0424(12) Uani 0.72(7) 1 d P . . Cl2 Cl -0.0201(9) 0.174(2) -0.0658(7) 0.0488(18) Uani 0.72(7) 1 d P . . Cl1 Cl -0.0443(6) -0.2333(6) -0.10420(18) 0.0438(11) Uani 0.62(2) 1 d P . . O2 O -0.34404(15) 0.6246(2) 0.07067(14) 0.0340(5) Uani 1 1 d . . . O3 O -0.1920(2) 0.3237(3) 0.1476(2) 0.0578(7) Uani 1 1 d . . . C11 C -0.2135(3) 0.4274(4) -0.0023(3) 0.0505(10) Uani 1 1 d . . . H11A H -0.1563 0.3725 -0.0160 0.061 Uiso 1 1 calc R . . H11B H -0.2396 0.4679 -0.0500 0.061 Uiso 1 1 calc R . . C12 C -0.2853(3) 0.3298(4) 0.0320(3) 0.0607(13) Uani 1 1 d . . . H12A H -0.3484 0.3748 0.0290 0.073 Uiso 1 1 calc R . . H12B H -0.2876 0.2422 0.0013 0.073 Uiso 1 1 calc R . . C13 C -0.2659(3) 0.2916(4) 0.1132(4) 0.0629(15) Uani 1 1 d . . . O4 O -0.3353(2) 0.2209(4) 0.1458(3) 0.0819(12) Uani 1 1 d . . . H4" H -0.3183 0.1945 0.1895 0.098 Uiso 1 1 calc R . . Cl1A Cl -0.0040(13) -0.1942(13) -0.1162(5) 0.054(3) Uani 0.38(2) 1 d P . . Cl3A Cl -0.233(2) -0.054(5) -0.0471(14) 0.059(5) Uani 0.28(7) 1 d P . . Cl2A Cl -0.010(3) 0.141(4) -0.064(2) 0.052(5) Uani 0.28(7) 1 d P . . O1W O -0.1935(5) -0.3410(4) -0.2119(3) 0.134(3) Uani 1 1 d . . . O2W O -0.3266(6) -0.2903(16) -0.1289(6) 0.286(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01886(17) 0.02163(17) 0.02657(19) 0.00362(16) -0.00073(17) 0.00057(13) O1 0.0225(10) 0.0256(9) 0.0262(11) 0.0002(8) -0.0001(8) 0.0010(8) N1 0.0227(13) 0.0249(13) 0.0393(15) -0.0006(12) -0.0008(11) 0.0032(10) N3 0.0258(14) 0.0329(15) 0.0373(15) 0.0123(12) -0.0110(11) -0.0070(11) N4 0.0215(13) 0.0351(15) 0.0287(13) -0.0010(11) -0.0040(10) -0.0032(10) N5 0.0290(13) 0.0282(13) 0.0289(13) 0.0024(11) 0.0037(11) 0.0012(11) N2 0.0212(11) 0.0240(11) 0.0497(16) -0.0005(13) 0.0008(13) -0.0021(9) C1 0.0254(15) 0.0283(15) 0.0273(16) 0.0041(12) -0.0034(12) 0.0013(12) C8 0.0244(15) 0.0503(19) 0.0286(16) -0.0044(14) 0.0005(12) -0.0067(14) C3 0.0283(17) 0.0340(19) 0.064(3) -0.0091(17) 0.0011(17) 0.0079(15) C10 0.0348(17) 0.0216(14) 0.0374(17) 0.0057(12) 0.0020(14) -0.0011(13) C9 0.0327(17) 0.0269(15) 0.0387(19) -0.0047(13) -0.0003(14) 0.0018(14) C2 0.0291(16) 0.0301(15) 0.0361(17) -0.0023(13) -0.0029(13) 0.0010(13) C5 0.0223(17) 0.039(2) 0.065(2) 0.0132(18) -0.0097(17) 0.0024(15) C7 0.0330(17) 0.053(2) 0.0286(17) 0.0119(16) -0.0057(14) -0.0140(16) C4 0.0308(18) 0.0314(18) 0.063(2) -0.0040(17) 0.0080(17) 0.0014(14) C6 0.036(2) 0.0352(19) 0.062(3) 0.0190(17) -0.0158(17) -0.0012(16) Zn1 0.03642(19) 0.0414(2) 0.02761(18) 0.00250(16) 0.00236(17) 0.00942(16) Cl4 0.0310(4) 0.0450(4) 0.0283(4) 0.0052(3) 0.0017(3) -0.0011(3) Cl3 0.0329(13) 0.057(2) 0.038(2) 0.0211(15) 0.0100(13) 0.0137(13) Cl2 0.0480(16) 0.061(4) 0.037(2) -0.007(3) 0.0064(14) -0.014(3) Cl1 0.047(2) 0.0438(14) 0.0404(10) -0.0006(9) -0.0006(11) 0.0169(15) O2 0.0251(11) 0.0399(13) 0.0369(12) -0.0050(10) -0.0047(9) 0.0034(10) O3 0.0578(17) 0.0380(13) 0.078(2) -0.0004(16) 0.0128(19) -0.0047(12) C11 0.040(2) 0.046(2) 0.066(3) -0.027(2) -0.0078(19) 0.0072(17) C12 0.046(2) 0.039(2) 0.097(4) -0.022(2) -0.013(2) -0.0004(18) C13 0.044(2) 0.0267(18) 0.118(4) -0.029(2) 0.028(3) -0.0097(17) O4 0.067(2) 0.0513(18) 0.128(4) -0.021(2) 0.029(2) -0.0269(17) Cl1A 0.073(7) 0.049(3) 0.042(2) -0.011(2) -0.013(3) 0.031(4) Cl3A 0.038(6) 0.070(11) 0.067(7) 0.039(6) -0.005(4) -0.002(7) Cl2A 0.061(10) 0.052(9) 0.044(5) 0.010(6) 0.001(5) -0.022(7) O1W 0.210(6) 0.048(2) 0.144(5) -0.014(3) -0.095(5) 0.025(3) O2W 0.120(5) 0.493(18) 0.244(10) -0.244(12) 0.063(6) -0.122(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 N1 1.878(3) . ? Co1 O1 1.927(2) . ? Co1 N4 1.933(3) . ? Co1 N5 1.949(3) . ? Co1 N2 1.951(3) . ? Co1 N3 1.971(3) . ? O1 C1 1.282(4) . ? N1 C2 1.288(4) . ? N1 C3 1.475(4) . ? N3 C7 1.491(5) . ? N3 C6 1.512(5) . ? N4 C8 1.484(4) . ? N4 C9 1.488(4) . ? N5 C10 1.493(4) . ? N2 C5 1.477(5) . ? N2 C4 1.505(5) . ? C1 O2 1.227(4) . ? C1 C2 1.528(5) . ? C8 C7 1.497(6) . ? C3 C4 1.524(5) . ? C10 C9 1.503(5) . ? C2 C11 1.497(5) . ? C5 C6 1.528(5) . ? Zn1 Cl2A 2.15(3) . ? Zn1 Cl3A 2.22(3) . ? Zn1 Cl4 2.2591(12) . ? Zn1 Cl2 2.276(15) . ? Zn1 Cl1A 2.291(5) . ? Zn1 Cl3 2.301(7) . ? Zn1 Cl1 2.330(3) . ? Cl1 Cl1A 0.712(14) . ? O3 C13 1.244(6) . ? C11 C12 1.500(7) . ? C12 C13 1.492(8) . ? C13 O4 1.318(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 O1 83.09(10) . . ? N1 Co1 N4 174.92(11) . . ? O1 Co1 N4 92.06(10) . . ? N1 Co1 N5 95.65(13) . . ? O1 Co1 N5 89.98(10) . . ? N4 Co1 N5 85.83(11) . . ? N1 Co1 N2 86.06(12) . . ? O1 Co1 N2 168.94(10) . . ? N4 Co1 N2 98.72(12) . . ? N5 Co1 N2 93.25(12) . . ? N1 Co1 N3 93.52(12) . . ? O1 Co1 N3 90.74(10) . . ? N4 Co1 N3 85.01(13) . . ? N5 Co1 N3 170.83(12) . . ? N2 Co1 N3 87.76(12) . . ? C1 O1 Co1 114.08(19) . . ? C2 N1 C3 125.4(3) . . ? C2 N1 Co1 116.7(2) . . ? C3 N1 Co1 117.3(2) . . ? C7 N3 C6 111.7(3) . . ? C7 N3 Co1 110.2(2) . . ? C6 N3 Co1 107.0(2) . . ? C8 N4 C9 115.7(3) . . ? C8 N4 Co1 106.7(2) . . ? C9 N4 Co1 108.1(2) . . ? C10 N5 Co1 110.0(2) . . ? C5 N2 C4 114.6(3) . . ? C5 N2 Co1 108.7(2) . . ? C4 N2 Co1 108.3(2) . . ? O2 C1 O1 126.3(3) . . ? O2 C1 C2 120.0(3) . . ? O1 C1 C2 113.8(3) . . ? N4 C8 C7 106.2(3) . . ? N1 C3 C4 106.2(3) . . ? N5 C10 C9 107.1(3) . . ? N4 C9 C10 105.6(3) . . ? N1 C2 C11 127.1(3) . . ? N1 C2 C1 111.8(3) . . ? C11 C2 C1 121.1(3) . . ? N2 C5 C6 108.2(3) . . ? N3 C7 C8 109.2(3) . . ? N2 C4 C3 111.4(3) . . ? N3 C6 C5 107.0(3) . . ? Cl2A Zn1 Cl3A 114.2(18) . . ? Cl2A Zn1 Cl4 112.6(8) . . ? Cl3A Zn1 Cl4 114.4(7) . . ? Cl2A Zn1 Cl2 8.2(12) . . ? Cl3A Zn1 Cl2 111.8(10) . . ? Cl4 Zn1 Cl2 108.2(4) . . ? Cl2A Zn1 Cl1A 96.2(14) . . ? Cl3A Zn1 Cl1A 110.5(15) . . ? Cl4 Zn1 Cl1A 107.2(2) . . ? Cl2 Zn1 Cl1A 104.2(6) . . ? Cl2A Zn1 Cl3 111.2(13) . . ? Cl3A Zn1 Cl3 6.3(14) . . ? Cl4 Zn1 Cl3 112.0(2) . . ? Cl2 Zn1 Cl3 108.1(4) . . ? Cl1A Zn1 Cl3 116.7(6) . . ? Cl2A Zn1 Cl1 109.0(12) . . ? Cl3A Zn1 Cl1 93.7(14) . . ? Cl4 Zn1 Cl1 111.34(7) . . ? Cl2 Zn1 Cl1 117.1(5) . . ? Cl1A Zn1 Cl1 17.7(4) . . ? Cl3 Zn1 Cl1 100.0(3) . . ? Cl1A Cl1 Zn1 78.0(5) . . ? C2 C11 C12 113.1(4) . . ? C13 C12 C11 114.0(4) . . ? O3 C13 O4 122.6(6) . . ? O3 C13 C12 123.8(4) . . ? O4 C13 C12 113.6(5) . . ? Cl1 Cl1A Zn1 84.3(8) . . ? 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 Co1 O1 C1 6.5(2) . . . . ? N4 Co1 O1 C1 -172.0(2) . . . . ? N5 Co1 O1 C1 102.2(2) . . . . ? N2 Co1 O1 C1 -4.8(7) . . . . ? N3 Co1 O1 C1 -86.9(2) . . . . ? O1 Co1 N1 C2 -6.6(3) . . . . ? N4 Co1 N1 C2 10.8(16) . . . . ? N5 Co1 N1 C2 -95.9(3) . . . . ? N2 Co1 N1 C2 171.3(3) . . . . ? N3 Co1 N1 C2 83.8(3) . . . . ? O1 Co1 N1 C3 -178.2(3) . . . . ? N4 Co1 N1 C3 -160.8(13) . . . . ? N5 Co1 N1 C3 92.5(3) . . . . ? N2 Co1 N1 C3 -0.4(3) . . . . ? N3 Co1 N1 C3 -87.9(3) . . . . ? N1 Co1 N3 C7 -168.0(2) . . . . ? O1 Co1 N3 C7 -84.9(2) . . . . ? N4 Co1 N3 C7 7.1(2) . . . . ? N5 Co1 N3 C7 9.6(9) . . . . ? N2 Co1 N3 C7 106.1(2) . . . . ? N1 Co1 N3 C6 70.4(2) . . . . ? O1 Co1 N3 C6 153.5(2) . . . . ? N4 Co1 N3 C6 -114.5(2) . . . . ? N5 Co1 N3 C6 -112.0(8) . . . . ? N2 Co1 N3 C6 -15.5(2) . . . . ? N1 Co1 N4 C8 41.1(15) . . . . ? O1 Co1 N4 C8 58.4(2) . . . . ? N5 Co1 N4 C8 148.2(2) . . . . ? N2 Co1 N4 C8 -119.1(2) . . . . ? N3 Co1 N4 C8 -32.2(2) . . . . ? N1 Co1 N4 C9 -84.0(14) . . . . ? O1 Co1 N4 C9 -66.7(2) . . . . ? N5 Co1 N4 C9 23.1(2) . . . . ? N2 Co1 N4 C9 115.8(2) . . . . ? N3 Co1 N4 C9 -157.2(2) . . . . ? N1 Co1 N5 C10 -179.4(2) . . . . ? O1 Co1 N5 C10 97.5(2) . . . . ? N4 Co1 N5 C10 5.5(2) . . . . ? N2 Co1 N5 C10 -93.1(2) . . . . ? N3 Co1 N5 C10 3.0(9) . . . . ? N1 Co1 N2 C5 -106.0(2) . . . . ? O1 Co1 N2 C5 -94.7(6) . . . . ? N4 Co1 N2 C5 72.3(2) . . . . ? N5 Co1 N2 C5 158.6(2) . . . . ? N3 Co1 N2 C5 -12.3(2) . . . . ? N1 Co1 N2 C4 19.1(2) . . . . ? O1 Co1 N2 C4 30.4(7) . . . . ? N4 Co1 N2 C4 -162.7(2) . . . . ? N5 Co1 N2 C4 -76.4(2) . . . . ? N3 Co1 N2 C4 112.8(2) . . . . ? Co1 O1 C1 O2 174.6(3) . . . . ? Co1 O1 C1 C2 -5.4(3) . . . . ? C9 N4 C8 C7 170.6(3) . . . . ? Co1 N4 C8 C7 50.3(3) . . . . ? C2 N1 C3 C4 171.2(3) . . . . ? Co1 N1 C3 C4 -18.0(4) . . . . ? Co1 N5 C10 C9 -32.5(3) . . . . ? C8 N4 C9 C10 -165.8(3) . . . . ? Co1 N4 C9 C10 -46.3(3) . . . . ? N5 C10 C9 N4 50.8(3) . . . . ? C3 N1 C2 C11 -2.3(6) . . . . ? Co1 N1 C2 C11 -173.2(3) . . . . ? C3 N1 C2 C1 176.1(3) . . . . ? Co1 N1 C2 C1 5.3(4) . . . . ? O2 C1 C2 N1 -179.7(3) . . . . ? O1 C1 C2 N1 0.2(4) . . . . ? O2 C1 C2 C11 -1.2(5) . . . . ? O1 C1 C2 C11 178.8(3) . . . . ? C4 N2 C5 C6 -83.9(4) . . . . ? Co1 N2 C5 C6 37.3(4) . . . . ? C6 N3 C7 C8 138.3(3) . . . . ? Co1 N3 C7 C8 19.5(3) . . . . ? N4 C8 C7 N3 -45.2(3) . . . . ? C5 N2 C4 C3 87.4(4) . . . . ? Co1 N2 C4 C3 -34.1(3) . . . . ? N1 C3 C4 N2 33.2(4) . . . . ? C7 N3 C6 C5 -81.6(4) . . . . ? Co1 N3 C6 C5 39.1(4) . . . . ? N2 C5 C6 N3 -50.6(4) . . . . ? Cl2A Zn1 Cl1 Cl1A -45.3(12) . . . . ? Cl3A Zn1 Cl1 Cl1A -162.5(8) . . . . ? Cl4 Zn1 Cl1 Cl1A 79.5(5) . . . . ? Cl2 Zn1 Cl1 Cl1A -45.7(6) . . . . ? Cl3 Zn1 Cl1 Cl1A -162.0(5) . . . . ? N1 C2 C11 C12 124.3(4) . . . . ? C1 C2 C11 C12 -54.0(5) . . . . ? C2 C11 C12 C13 -43.3(5) . . . . ? C11 C12 C13 O3 -7.7(6) . . . . ? C11 C12 C13 O4 171.8(4) . . . . ? Cl2A Zn1 Cl1A Cl1 137.4(10) . . . . ? Cl3A Zn1 Cl1A Cl1 18.7(9) . . . . ? Cl4 Zn1 Cl1A Cl1 -106.5(5) . . . . ? Cl2 Zn1 Cl1A Cl1 138.9(6) . . . . ? Cl3 Zn1 Cl1A Cl1 19.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.827 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.062 #===END data_compound7 #maffm-[Co(pimtetraen)](ZnCl4)Cl _database_code_CSD 176561 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H26 Cl5 Co N6 Zn' _chemical_formula_weight 579.96 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' '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.627(2) _cell_length_b 9.318(2) _cell_length_c 14.226(4) _cell_angle_alpha 82.903(3) _cell_angle_beta 75.790(3) _cell_angle_gamma 84.019(4) _cell_volume 1096.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'orange - brown' _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 2.472 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8277 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13500 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.44 _reflns_number_total 4374 _reflns_number_gt 4227 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0384P)^2^+0.8585P] 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 4374 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.46186(3) 0.73730(2) -0.253300(17) 0.01335(7) Uani 1 1 d . . . Zn1 Zn -0.86015(3) 1.20972(2) -0.331054(15) 0.01920(7) Uani 1 1 d . . . Cl2 Cl -0.60005(5) 1.17369(5) -0.42078(3) 0.02213(11) Uani 1 1 d . . . Cl4 Cl -0.92054(5) 0.99468(5) -0.24040(4) 0.02241(11) Uani 1 1 d . . . Cl3 Cl -0.86765(6) 1.38583(5) -0.23401(4) 0.02700(12) Uani 1 1 d . . . Cl5 Cl -0.36433(7) 0.71835(6) 0.03518(4) 0.03162(13) Uani 1 1 d . . . Cl1 Cl -1.02411(7) 1.26820(7) -0.43401(4) 0.03636(14) Uani 1 1 d . . . N4 N -0.26108(18) 0.77173(17) -0.35711(11) 0.0168(3) Uani 1 1 d . . . H4 H -0.2652 0.7286 -0.4119 0.020 Uiso 1 1 calc R . . N1 N -0.59830(19) 0.80700(17) -0.34504(12) 0.0176(3) Uani 1 1 d . . . H1A H -0.6817 0.8688 -0.3159 0.021 Uiso 1 1 calc R . . H1B H -0.5391 0.8575 -0.3994 0.021 Uiso 1 1 calc R . . N3 N -0.31979(19) 0.63975(18) -0.17384(12) 0.0197(3) Uani 1 1 d . . . H3 H -0.3600 0.6625 -0.1101 0.024 Uiso 1 1 calc R . . N5 N -0.43822(18) 0.92644(17) -0.22632(11) 0.0169(3) Uani 1 1 d . . . N6 N -0.64602(19) 0.74890(17) -0.13854(11) 0.0167(3) Uani 1 1 d . . . C10 C -0.6588(2) 0.8781(2) -0.10033(14) 0.0191(4) Uani 1 1 d . . . N2 N -0.4962(2) 0.54465(17) -0.28055(12) 0.0204(3) Uani 1 1 d . . . H2 H -0.5855 0.5140 -0.2338 0.025 Uiso 1 1 calc R . . C1 C -0.6633(2) 0.6812(2) -0.37444(15) 0.0243(4) Uani 1 1 d . . . H1B' H -0.6866 0.7059 -0.4396 0.029 Uiso 1 1 calc R . . H1C H -0.7640 0.6559 -0.3270 0.029 Uiso 1 1 calc R . . C8 C -0.3092(2) 1.0086(2) -0.29087(14) 0.0204(4) Uani 1 1 d . . . H8A H -0.2190 1.0092 -0.2593 0.024 Uiso 1 1 calc R . . H8B H -0.3495 1.1101 -0.3061 0.024 Uiso 1 1 calc R . . C4 C -0.3191(3) 0.4785(2) -0.17436(17) 0.0288(5) Uani 1 1 d . . . H4A H -0.3991 0.4393 -0.1169 0.035 Uiso 1 1 calc R . . H4B H -0.2121 0.4321 -0.1701 0.035 Uiso 1 1 calc R . . C14 C -0.7554(2) 0.6542(2) -0.09505(14) 0.0222(4) Uani 1 1 d . . . H14A H -0.7478 0.5627 -0.1195 0.027 Uiso 1 1 calc R . . C9 C -0.5385(2) 0.9763(2) -0.15382(15) 0.0219(4) Uani 1 1 d . . . H9A H -0.5352 1.0706 -0.1359 0.026 Uiso 1 1 calc R . . C3 C -0.3583(3) 0.4432(2) -0.26627(17) 0.0292(5) Uani 1 1 d . . . H3A H -0.2653 0.4566 -0.3225 0.035 Uiso 1 1 calc R . . H3B H -0.3867 0.3415 -0.2592 0.035 Uiso 1 1 calc R . . C5 C -0.1585(2) 0.6962(2) -0.21069(14) 0.0224(4) Uani 1 1 d . . . H5A H -0.0776 0.6302 -0.1849 0.027 Uiso 1 1 calc R . . H5B H -0.1591 0.7931 -0.1889 0.027 Uiso 1 1 calc R . . C11 C -0.7778(2) 0.9146(2) -0.02031(15) 0.0236(4) Uani 1 1 d . . . H11A H -0.7818 1.0052 0.0047 0.028 Uiso 1 1 calc R . . C7 C -0.2549(2) 0.9324(2) -0.38309(14) 0.0194(4) Uani 1 1 d . . . H7A H -0.3257 0.9668 -0.4278 0.023 Uiso 1 1 calc R . . H7B H -0.1440 0.9551 -0.4167 0.023 Uiso 1 1 calc R . . C2 C -0.5382(3) 0.5558(2) -0.37676(15) 0.0241(4) Uani 1 1 d . . . H2A H -0.5815 0.4653 -0.3855 0.029 Uiso 1 1 calc R . . H2B H -0.4429 0.5746 -0.4306 0.029 Uiso 1 1 calc R . . C12 C -0.8915(3) 0.8159(2) 0.02284(15) 0.0258(4) Uani 1 1 d . . . H12A H -0.9755 0.8380 0.0774 0.031 Uiso 1 1 calc R . . C6 C -0.1170(2) 0.7062(2) -0.32106(15) 0.0220(4) Uani 1 1 d . . . H6A H -0.0258 0.7673 -0.3479 0.026 Uiso 1 1 calc R . . H6B H -0.0853 0.6084 -0.3430 0.026 Uiso 1 1 calc R . . C13 C -0.8792(3) 0.6854(2) -0.01563(16) 0.0280(4) Uani 1 1 d . . . H13A H -0.9557 0.6166 0.0123 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01157(12) 0.01357(13) 0.01408(13) -0.00365(9) -0.00030(9) -0.00117(9) Zn1 0.01720(12) 0.02104(13) 0.01745(12) -0.00372(9) -0.00007(9) -0.00026(9) Cl2 0.0176(2) 0.0243(2) 0.0206(2) -0.00287(17) 0.00266(17) -0.00071(17) Cl4 0.0163(2) 0.0223(2) 0.0269(2) -0.00116(18) -0.00145(18) -0.00347(17) Cl3 0.0295(3) 0.0237(2) 0.0246(2) -0.00804(19) 0.00348(19) -0.0051(2) Cl5 0.0396(3) 0.0280(3) 0.0271(3) -0.0108(2) -0.0028(2) -0.0049(2) Cl1 0.0278(3) 0.0564(4) 0.0233(3) -0.0068(2) -0.0074(2) 0.0107(2) N4 0.0145(7) 0.0184(8) 0.0166(7) -0.0025(6) -0.0016(6) -0.0014(6) N1 0.0144(7) 0.0196(8) 0.0181(8) -0.0021(6) -0.0015(6) -0.0031(6) N3 0.0171(8) 0.0225(8) 0.0168(8) 0.0002(6) -0.0003(6) -0.0007(6) N5 0.0147(7) 0.0177(8) 0.0186(8) -0.0035(6) -0.0028(6) -0.0031(6) N6 0.0161(7) 0.0182(8) 0.0150(7) -0.0027(6) -0.0024(6) 0.0001(6) C10 0.0190(9) 0.0206(9) 0.0179(9) -0.0052(7) -0.0037(7) 0.0004(7) N2 0.0200(8) 0.0182(8) 0.0210(8) -0.0054(6) 0.0018(6) -0.0036(6) C1 0.0215(10) 0.0316(11) 0.0228(10) -0.0037(8) -0.0064(8) -0.0112(8) C8 0.0172(9) 0.0180(9) 0.0254(10) -0.0032(7) -0.0016(7) -0.0057(7) C4 0.0280(11) 0.0197(10) 0.0349(12) 0.0052(8) -0.0049(9) 0.0006(8) C14 0.0237(10) 0.0218(9) 0.0195(9) -0.0037(7) -0.0004(8) -0.0040(8) C9 0.0228(10) 0.0199(9) 0.0236(10) -0.0077(7) -0.0036(8) -0.0025(8) C3 0.0303(11) 0.0169(9) 0.0369(12) -0.0056(8) -0.0017(9) 0.0026(8) C5 0.0144(9) 0.0284(10) 0.0234(10) -0.0002(8) -0.0046(7) -0.0004(8) C11 0.0245(10) 0.0243(10) 0.0203(9) -0.0054(8) -0.0029(8) 0.0033(8) C7 0.0169(9) 0.0187(9) 0.0209(9) 0.0003(7) -0.0010(7) -0.0050(7) C2 0.0284(10) 0.0243(10) 0.0203(9) -0.0085(8) -0.0008(8) -0.0098(8) C12 0.0241(10) 0.0320(11) 0.0161(9) -0.0030(8) 0.0034(8) 0.0030(8) C6 0.0132(8) 0.0261(10) 0.0238(10) -0.0004(8) -0.0014(7) 0.0017(7) C13 0.0260(10) 0.0306(11) 0.0232(10) -0.0012(8) 0.0036(8) -0.0076(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 Co1 N5 1.8909(16) . ? Co1 N2 1.9493(17) . ? Co1 N3 1.9494(17) . ? Co1 N1 1.9737(16) . ? Co1 N6 1.9838(16) . ? Co1 N4 2.0067(16) . ? Zn1 Cl3 2.2576(7) . ? Zn1 Cl1 2.2587(7) . ? Zn1 Cl4 2.2801(7) . ? Zn1 Cl2 2.3064(7) . ? N4 C7 1.501(2) . ? N4 C6 1.502(2) . ? N1 C1 1.496(2) . ? N3 C5 1.488(2) . ? N3 C4 1.503(3) . ? N5 C9 1.274(3) . ? N5 C8 1.473(2) . ? N6 C14 1.343(3) . ? N6 C10 1.364(2) . ? C10 C11 1.384(3) . ? C10 C9 1.460(3) . ? N2 C3 1.479(3) . ? N2 C2 1.488(3) . ? C1 C2 1.504(3) . ? C8 C7 1.518(3) . ? C4 C3 1.509(3) . ? C14 C13 1.388(3) . ? C5 C6 1.515(3) . ? C11 C12 1.391(3) . ? C12 C13 1.378(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Co1 N2 177.50(7) . . ? N5 Co1 N3 95.25(7) . . ? N2 Co1 N3 86.63(7) . . ? N5 Co1 N1 93.51(7) . . ? N2 Co1 N1 84.72(7) . . ? N3 Co1 N1 170.57(7) . . ? N5 Co1 N6 82.40(7) . . ? N2 Co1 N6 95.90(7) . . ? N3 Co1 N6 92.28(7) . . ? N1 Co1 N6 92.35(7) . . ? N5 Co1 N4 83.04(7) . . ? N2 Co1 N4 98.76(7) . . ? N3 Co1 N4 85.81(7) . . ? N1 Co1 N4 91.79(7) . . ? N6 Co1 N4 165.07(7) . . ? Cl3 Zn1 Cl1 112.38(3) . . ? Cl3 Zn1 Cl4 110.79(3) . . ? Cl1 Zn1 Cl4 110.33(3) . . ? Cl3 Zn1 Cl2 107.99(2) . . ? Cl1 Zn1 Cl2 109.03(3) . . ? Cl4 Zn1 Cl2 106.08(2) . . ? C7 N4 C6 111.59(14) . . ? C7 N4 Co1 107.92(11) . . ? C6 N4 Co1 109.98(12) . . ? C1 N1 Co1 109.94(12) . . ? C5 N3 C4 113.78(16) . . ? C5 N3 Co1 108.72(12) . . ? C4 N3 Co1 109.19(13) . . ? C9 N5 C8 123.92(16) . . ? C9 N5 Co1 117.31(13) . . ? C8 N5 Co1 118.75(12) . . ? C14 N6 C10 117.30(16) . . ? C14 N6 Co1 131.34(13) . . ? C10 N6 Co1 111.36(12) . . ? N6 C10 C11 123.16(18) . . ? N6 C10 C9 113.70(17) . . ? C11 C10 C9 123.10(18) . . ? C3 N2 C2 117.43(16) . . ? C3 N2 Co1 109.13(13) . . ? C2 N2 Co1 109.08(12) . . ? N1 C1 C2 107.41(15) . . ? N5 C8 C7 106.37(15) . . ? N3 C4 C3 110.54(17) . . ? N6 C14 C13 122.23(19) . . ? N5 C9 C10 115.21(17) . . ? N2 C3 C4 106.10(17) . . ? N3 C5 C6 108.44(16) . . ? C10 C11 C12 118.70(19) . . ? N4 C7 C8 109.33(15) . . ? N2 C2 C1 104.86(16) . . ? C13 C12 C11 118.31(19) . . ? N4 C6 C5 108.91(15) . . ? C12 C13 C14 120.28(19) . . ? 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 N5 Co1 N4 C7 -25.40(12) . . . . ? N2 Co1 N4 C7 152.85(12) . . . . ? N3 Co1 N4 C7 -121.21(12) . . . . ? N1 Co1 N4 C7 67.92(12) . . . . ? N6 Co1 N4 C7 -38.1(3) . . . . ? N5 Co1 N4 C6 96.55(13) . . . . ? N2 Co1 N4 C6 -85.20(13) . . . . ? N3 Co1 N4 C6 0.73(13) . . . . ? N1 Co1 N4 C6 -170.14(13) . . . . ? N6 Co1 N4 C6 83.8(3) . . . . ? N5 Co1 N1 C1 -172.37(12) . . . . ? N2 Co1 N1 C1 5.86(12) . . . . ? N3 Co1 N1 C1 29.5(5) . . . . ? N6 Co1 N1 C1 -89.85(13) . . . . ? N4 Co1 N1 C1 104.50(12) . . . . ? N5 Co1 N3 C5 -58.81(13) . . . . ? N2 Co1 N3 C5 122.84(13) . . . . ? N1 Co1 N3 C5 99.3(4) . . . . ? N6 Co1 N3 C5 -141.38(13) . . . . ? N4 Co1 N3 C5 23.80(13) . . . . ? N5 Co1 N3 C4 176.53(13) . . . . ? N2 Co1 N3 C4 -1.82(13) . . . . ? N1 Co1 N3 C4 -25.4(5) . . . . ? N6 Co1 N3 C4 93.96(13) . . . . ? N4 Co1 N3 C4 -100.87(13) . . . . ? N2 Co1 N5 C9 47.4(16) . . . . ? N3 Co1 N5 C9 -91.35(16) . . . . ? N1 Co1 N5 C9 92.16(16) . . . . ? N6 Co1 N5 C9 0.26(15) . . . . ? N4 Co1 N5 C9 -176.46(16) . . . . ? N2 Co1 N5 C8 -131.1(15) . . . . ? N3 Co1 N5 C8 90.19(14) . . . . ? N1 Co1 N5 C8 -86.30(14) . . . . ? N6 Co1 N5 C8 -178.20(14) . . . . ? N4 Co1 N5 C8 5.08(13) . . . . ? N5 Co1 N6 C14 178.57(18) . . . . ? N2 Co1 N6 C14 0.41(18) . . . . ? N3 Co1 N6 C14 -86.44(18) . . . . ? N1 Co1 N6 C14 85.34(18) . . . . ? N4 Co1 N6 C14 -168.7(2) . . . . ? N5 Co1 N6 C10 -1.01(13) . . . . ? N2 Co1 N6 C10 -179.17(13) . . . . ? N3 Co1 N6 C10 93.98(13) . . . . ? N1 Co1 N6 C10 -94.24(13) . . . . ? N4 Co1 N6 C10 11.7(3) . . . . ? C14 N6 C10 C11 -0.1(3) . . . . ? Co1 N6 C10 C11 179.49(15) . . . . ? C14 N6 C10 C9 -178.12(17) . . . . ? Co1 N6 C10 C9 1.5(2) . . . . ? N5 Co1 N2 C3 -162.3(15) . . . . ? N3 Co1 N2 C3 -23.45(14) . . . . ? N1 Co1 N2 C3 152.79(14) . . . . ? N6 Co1 N2 C3 -115.39(13) . . . . ? N4 Co1 N2 C3 61.78(14) . . . . ? N5 Co1 N2 C2 68.2(16) . . . . ? N3 Co1 N2 C2 -152.93(13) . . . . ? N1 Co1 N2 C2 23.30(13) . . . . ? N6 Co1 N2 C2 115.12(13) . . . . ? N4 Co1 N2 C2 -67.70(13) . . . . ? Co1 N1 C1 C2 -33.36(18) . . . . ? C9 N5 C8 C7 -162.12(18) . . . . ? Co1 N5 C8 C7 16.23(19) . . . . ? C5 N3 C4 C3 -95.2(2) . . . . ? Co1 N3 C4 C3 26.5(2) . . . . ? C10 N6 C14 C13 1.3(3) . . . . ? Co1 N6 C14 C13 -178.29(16) . . . . ? C8 N5 C9 C10 178.90(17) . . . . ? Co1 N5 C9 C10 0.5(2) . . . . ? N6 C10 C9 N5 -1.4(3) . . . . ? C11 C10 C9 N5 -179.37(19) . . . . ? C2 N2 C3 C4 167.19(16) . . . . ? Co1 N2 C3 C4 42.44(19) . . . . ? N3 C4 C3 N2 -44.9(2) . . . . ? C4 N3 C5 C6 78.5(2) . . . . ? Co1 N3 C5 C6 -43.46(18) . . . . ? N6 C10 C11 C12 -0.8(3) . . . . ? C9 C10 C11 C12 176.95(19) . . . . ? C6 N4 C7 C8 -80.10(18) . . . . ? Co1 N4 C7 C8 40.84(17) . . . . ? N5 C8 C7 N4 -36.4(2) . . . . ? C3 N2 C2 C1 -171.55(16) . . . . ? Co1 N2 C2 C1 -46.78(17) . . . . ? N1 C1 C2 N2 51.38(19) . . . . ? C10 C11 C12 C13 0.7(3) . . . . ? C7 N4 C6 C5 95.08(18) . . . . ? Co1 N4 C6 C5 -24.65(18) . . . . ? N3 C5 C6 N4 44.3(2) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? N6 C14 C13 C12 -1.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.626 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.085 #===END data_compound8 #f(m)m-[Co(pimtren)Cl](ClO4)2 _database_code_CSD 176562 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 Cl3 Co N5 O9' _chemical_formula_weight 545.63 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.235(3) _cell_length_b 9.612(3) _cell_length_c 14.315(5) _cell_angle_alpha 93.980(5) _cell_angle_beta 94.152(5) _cell_angle_gamma 112.341(5) _cell_volume 1039.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8286 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13220 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 26.50 _reflns_number_total 4200 _reflns_number_gt 3826 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0447P)^2^+1.1265P] 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 4200 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.40727(4) 0.21354(3) 0.29504(2) 0.01911(10) Uani 1 1 d . . . Cl1 Cl 0.63543(7) 0.15482(7) 0.34806(4) 0.02689(14) Uani 1 1 d . . . Cl2 Cl 0.76350(8) 0.36512(7) 0.64142(4) 0.02952(14) Uani 1 1 d . . . N3 N 0.2098(2) 0.2531(2) 0.25321(13) 0.0234(4) Uani 1 1 d . . . N2 N 0.4940(3) 0.2756(2) 0.17544(13) 0.0258(4) Uani 1 1 d . . . N4 N 0.2886(2) 0.1751(2) 0.40971(13) 0.0204(4) Uani 1 1 d . . . N5 N 0.5483(2) 0.4223(2) 0.34831(13) 0.0231(4) Uani 1 1 d . . . H5A' H 0.4744 0.4682 0.3669 0.028 Uiso 1 1 calc R . . H5B' H 0.6200 0.4220 0.4006 0.028 Uiso 1 1 calc R . . N1 N 0.2969(3) 0.0067(2) 0.23144(14) 0.0281(4) Uani 1 1 d . . . H1B' H 0.3400 -0.0554 0.2618 0.034 Uiso 1 1 calc R . . H1A' H 0.1768 -0.0293 0.2342 0.034 Uiso 1 1 calc R . . O11 O 0.6766(3) 0.4209(2) 0.57025(14) 0.0371(4) Uani 1 1 d . . . O14 O 0.7303(3) 0.2085(2) 0.61553(13) 0.0357(4) Uani 1 1 d . . . C3 C 0.3732(3) 0.3392(3) 0.12328(18) 0.0326(6) Uani 1 1 d . . . H3A H 0.4238 0.4509 0.1357 0.039 Uiso 1 1 calc R . . H3B H 0.3668 0.3127 0.0547 0.039 Uiso 1 1 calc R . . C6 C 0.1419(3) 0.2095(2) 0.40427(16) 0.0218(4) Uani 1 1 d . . . C8 C 0.1073(3) 0.1758(3) 0.56581(16) 0.0256(5) Uani 1 1 d . . . H8A H 0.0464 0.1766 0.6196 0.031 Uiso 1 1 calc R . . C4 C 0.1897(3) 0.2780(3) 0.15357(17) 0.0309(5) Uani 1 1 d . . . H4A H 0.1330 0.3513 0.1460 0.037 Uiso 1 1 calc R . . H4B H 0.1159 0.1818 0.1152 0.037 Uiso 1 1 calc R . . C5 C 0.0980(3) 0.2462(3) 0.31091(17) 0.0244(5) Uani 1 1 d . . . H5A H -0.0062 0.2634 0.2947 0.029 Uiso 1 1 calc R . . C7 C 0.0486(3) 0.2109(2) 0.48028(17) 0.0250(5) Uani 1 1 d . . . H7A H -0.0530 0.2352 0.4745 0.030 Uiso 1 1 calc R . . C12 C 0.6593(3) 0.5102(3) 0.27747(17) 0.0286(5) Uani 1 1 d . . . H12A H 0.7789 0.5739 0.3082 0.034 Uiso 1 1 calc R . . H12B H 0.6057 0.5772 0.2510 0.034 Uiso 1 1 calc R . . C10 C 0.3427(3) 0.1396(2) 0.49210(16) 0.0228(4) Uani 1 1 d . . . H10A H 0.4433 0.1137 0.4963 0.027 Uiso 1 1 calc R . . C11 C 0.6718(3) 0.4002(3) 0.19893(17) 0.0288(5) Uani 1 1 d . . . H11A H 0.7100 0.4533 0.1427 0.035 Uiso 1 1 calc R . . H11B H 0.7595 0.3583 0.2198 0.035 Uiso 1 1 calc R . . C9 C 0.2543(3) 0.1398(3) 0.57169(16) 0.0252(5) Uani 1 1 d . . . H9A H 0.2953 0.1152 0.6296 0.030 Uiso 1 1 calc R . . O13 O 0.9484(3) 0.4520(3) 0.6496(3) 0.0777(9) Uani 1 1 d . . . C2 C 0.5018(4) 0.1390(3) 0.12193(18) 0.0366(6) Uani 1 1 d . . . H2A H 0.6058 0.1206 0.1478 0.044 Uiso 1 1 calc R . . H2B H 0.5132 0.1556 0.0548 0.044 Uiso 1 1 calc R . . O12 O 0.6949(4) 0.3824(3) 0.72834(16) 0.0663(7) Uani 1 1 d . . . C1 C 0.3345(4) 0.0039(3) 0.13064(18) 0.0386(6) Uani 1 1 d . . . H1A H 0.2349 0.0086 0.0897 0.046 Uiso 1 1 calc R . . H1B H 0.3494 -0.0908 0.1108 0.046 Uiso 1 1 calc R . . Cl3 Cl 0.79423(9) -0.13509(8) 1.13867(4) 0.03826(16) Uani 1 1 d . . . O1A O 0.6071(9) -0.1846(13) 1.1722(17) 0.058(4) Uani 0.44(4) 1 d P . . O1B O 0.6298(17) -0.238(2) 1.1259(14) 0.094(7) Uani 0.56(4) 1 d P . . O4A O 0.9185(16) -0.195(2) 1.1974(11) 0.065(7) Uani 0.189(10) 1 d P . . O4B O 0.9008(4) -0.0799(4) 1.22614(17) 0.0508(13) Uani 0.811(10) 1 d P . . O2A O 0.9001(10) -0.1223(16) 1.0599(5) 0.103(6) Uani 0.371(11) 1 d P . . O2B O 0.8216(10) -0.2562(7) 1.0989(4) 0.102(3) Uani 0.629(11) 1 d P . . O3A O 0.806(3) -0.014(2) 1.189(2) 0.172(19) Uani 0.220(11) 1 d P . . O3B O 0.8051(5) -0.0156(5) 1.0841(3) 0.088(2) Uani 0.780(11) 1 d P . . O21A O 0.0676(6) 0.5660(6) 1.0293(3) 0.0831(19) Uani 0.615(6) 1 d P . . H20 H 0.1078 0.6767 0.9894 0.125 Uiso 1 1 d R . . O21B O 0.2579(8) 0.5947(6) 1.0402(4) 0.0459(17) Uani 0.385(6) 1 d P . . 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 0.01933(16) 0.02032(16) 0.01866(16) 0.00225(11) 0.00002(11) 0.00909(12) Cl1 0.0247(3) 0.0315(3) 0.0302(3) 0.0035(2) 0.0015(2) 0.0176(2) Cl2 0.0256(3) 0.0270(3) 0.0373(3) -0.0014(2) -0.0011(2) 0.0133(2) N3 0.0224(9) 0.0222(9) 0.0242(9) 0.0059(7) -0.0024(7) 0.0075(8) N2 0.0279(10) 0.0270(10) 0.0220(9) 0.0022(8) 0.0028(8) 0.0100(8) N4 0.0203(9) 0.0188(9) 0.0223(9) 0.0021(7) -0.0001(7) 0.0082(7) N5 0.0209(9) 0.0246(10) 0.0246(9) -0.0001(8) 0.0001(7) 0.0104(8) N1 0.0311(11) 0.0245(10) 0.0268(10) 0.0024(8) -0.0007(8) 0.0093(8) O11 0.0450(11) 0.0306(9) 0.0416(10) 0.0059(8) 0.0007(9) 0.0214(9) O14 0.0422(11) 0.0252(9) 0.0425(10) 0.0044(8) 0.0013(8) 0.0165(8) C3 0.0328(13) 0.0366(14) 0.0259(12) 0.0123(10) -0.0012(10) 0.0100(11) C6 0.0175(10) 0.0184(10) 0.0282(11) 0.0032(8) 0.0001(8) 0.0057(8) C8 0.0265(11) 0.0201(11) 0.0265(11) 0.0006(9) 0.0061(9) 0.0048(9) C4 0.0282(12) 0.0374(14) 0.0254(12) 0.0108(10) -0.0045(10) 0.0108(11) C5 0.0192(10) 0.0229(11) 0.0313(12) 0.0054(9) -0.0030(9) 0.0088(9) C7 0.0193(11) 0.0215(11) 0.0337(12) 0.0021(9) 0.0036(9) 0.0072(9) C12 0.0239(11) 0.0253(12) 0.0338(13) 0.0031(10) 0.0049(10) 0.0062(9) C10 0.0233(11) 0.0221(11) 0.0235(11) 0.0028(9) -0.0004(9) 0.0099(9) C11 0.0241(12) 0.0312(13) 0.0305(12) 0.0051(10) 0.0073(10) 0.0089(10) C9 0.0296(12) 0.0224(11) 0.0218(11) 0.0029(9) 0.0002(9) 0.0083(9) O13 0.0248(11) 0.0405(13) 0.159(3) -0.0057(15) -0.0135(14) 0.0101(10) C2 0.0473(16) 0.0354(14) 0.0259(12) -0.0024(10) 0.0106(11) 0.0143(12) O12 0.105(2) 0.0845(19) 0.0347(12) 0.0047(12) 0.0146(13) 0.0633(17) C1 0.0516(17) 0.0315(14) 0.0263(13) -0.0042(10) 0.0025(12) 0.0105(12) Cl3 0.0411(4) 0.0380(4) 0.0285(3) 0.0033(3) -0.0068(3) 0.0093(3) O1A 0.029(3) 0.072(5) 0.063(9) 0.023(5) -0.001(3) 0.009(3) O1B 0.050(4) 0.114(9) 0.064(7) 0.047(8) -0.018(5) -0.030(5) O4A 0.037(7) 0.094(15) 0.071(10) 0.056(10) 0.005(6) 0.025(7) O4B 0.0397(16) 0.074(3) 0.0256(13) 0.0043(13) -0.0046(11) 0.0096(15) O2A 0.045(4) 0.179(13) 0.024(3) -0.016(5) 0.010(3) -0.021(5) O2B 0.165(7) 0.098(5) 0.069(4) -0.031(3) -0.023(4) 0.095(5) O3A 0.084(13) 0.113(16) 0.28(4) -0.14(2) 0.030(17) 0.019(11) O3B 0.074(3) 0.090(3) 0.085(4) 0.063(3) -0.005(2) 0.009(2) O21A 0.077(3) 0.120(5) 0.088(4) 0.066(3) 0.030(3) 0.065(3) O21B 0.054(4) 0.050(3) 0.041(3) 0.011(2) 0.003(2) 0.029(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.8734(19) . ? Co1 N2 1.947(2) . ? Co1 N4 1.9563(19) . ? Co1 N5 1.961(2) . ? Co1 N1 1.966(2) . ? Co1 Cl1 2.2547(9) . ? Cl2 O13 1.422(2) . ? Cl2 O12 1.428(2) . ? Cl2 O14 1.4399(19) . ? Cl2 O11 1.4491(19) . ? N3 C5 1.267(3) . ? N3 C4 1.470(3) . ? N2 C11 1.494(3) . ? N2 C2 1.499(3) . ? N2 C3 1.529(3) . ? N4 C10 1.342(3) . ? N4 C6 1.367(3) . ? N5 C12 1.498(3) . ? N1 C1 1.498(3) . ? C3 C4 1.507(4) . ? C6 C7 1.379(3) . ? C6 C5 1.461(3) . ? C8 C9 1.379(3) . ? C8 C7 1.394(3) . ? C12 C11 1.525(3) . ? C10 C9 1.396(3) . ? C2 C1 1.513(4) . ? Cl3 O3A 1.297(13) . ? Cl3 O1B 1.328(6) . ? Cl3 O2B 1.363(4) . ? Cl3 O3B 1.412(3) . ? Cl3 O4B 1.419(3) . ? Cl3 O2A 1.458(7) . ? Cl3 O1A 1.553(11) . ? Cl3 O4A 1.575(12) . ? O1A O1B 0.881(14) . ? O1A O3A 1.81(2) . ? O1B O2B 1.72(3) . ? O4A O4B 1.22(2) . ? O4A O2B 1.527(17) . ? O4B O3A 1.29(3) . ? O2A O2B 1.380(12) . ? O2A O3B 1.544(15) . ? O3A O3B 1.50(3) . ? O21A O21B 1.478(7) . ? O21A O21A 1.481(11) 2_567 ? 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 N3 Co1 N2 85.97(9) . . ? N3 Co1 N4 82.63(8) . . ? N2 Co1 N4 167.85(8) . . ? N3 Co1 N5 94.76(8) . . ? N2 Co1 N5 86.63(8) . . ? N4 Co1 N5 90.14(8) . . ? N3 Co1 N1 90.57(9) . . ? N2 Co1 N1 86.93(9) . . ? N4 Co1 N1 97.34(8) . . ? N5 Co1 N1 171.33(8) . . ? N3 Co1 Cl1 177.04(6) . . ? N2 Co1 Cl1 96.18(6) . . ? N4 Co1 Cl1 95.37(6) . . ? N5 Co1 Cl1 87.41(6) . . ? N1 Co1 Cl1 87.51(7) . . ? O13 Cl2 O12 110.14(19) . . ? O13 Cl2 O14 109.43(13) . . ? O12 Cl2 O14 110.48(14) . . ? O13 Cl2 O11 108.99(16) . . ? O12 Cl2 O11 107.58(13) . . ? O14 Cl2 O11 110.19(11) . . ? C5 N3 C4 125.0(2) . . ? C5 N3 Co1 117.66(16) . . ? C4 N3 Co1 117.16(15) . . ? C11 N2 C2 112.6(2) . . ? C11 N2 C3 108.17(19) . . ? C2 N2 C3 112.9(2) . . ? C11 N2 Co1 106.37(14) . . ? C2 N2 Co1 106.70(15) . . ? C3 N2 Co1 109.86(15) . . ? C10 N4 C6 118.61(19) . . ? C10 N4 Co1 129.29(15) . . ? C6 N4 Co1 111.54(14) . . ? C12 N5 Co1 110.82(14) . . ? C1 N1 Co1 110.56(15) . . ? C4 C3 N2 111.61(19) . . ? N4 C6 C7 122.7(2) . . ? N4 C6 C5 112.93(19) . . ? C7 C6 C5 124.4(2) . . ? C9 C8 C7 119.5(2) . . ? N3 C4 C3 106.40(19) . . ? N3 C5 C6 114.7(2) . . ? C6 C7 C8 118.2(2) . . ? N5 C12 C11 109.16(19) . . ? N4 C10 C9 121.4(2) . . ? N2 C11 C12 108.35(19) . . ? C8 C9 C10 119.6(2) . . ? N2 C2 C1 108.8(2) . . ? N1 C1 C2 108.3(2) . . ? O3A Cl3 O1B 111.8(17) . . ? O3A Cl3 O2B 165.3(13) . . ? O1B Cl3 O2B 79.7(16) . . ? O3A Cl3 O3B 67.2(17) . . ? O1B Cl3 O3B 108.6(6) . . ? O2B Cl3 O3B 119.0(4) . . ? O3A Cl3 O4B 56.4(16) . . ? O1B Cl3 O4B 126.2(7) . . ? O2B Cl3 O4B 109.7(3) . . ? O3B Cl3 O4B 111.1(3) . . ? O3A Cl3 O2A 119.5(15) . . ? O1B Cl3 O2A 117.0(13) . . ? O2B Cl3 O2A 58.5(6) . . ? O3B Cl3 O2A 65.1(7) . . ? O4B Cl3 O2A 112.0(3) . . ? O3A Cl3 O1A 78.4(11) . . ? O1B Cl3 O1A 34.5(8) . . ? O2B Cl3 O1A 111.0(7) . . ? O3B Cl3 O1A 103.8(4) . . ? O4B Cl3 O1A 100.5(9) . . ? O2A Cl3 O1A 147.5(9) . . ? O3A Cl3 O4A 104.1(19) . . ? O1B Cl3 O4A 110.7(9) . . ? O2B Cl3 O4A 62.2(8) . . ? O3B Cl3 O4A 140.0(5) . . ? O4B Cl3 O4A 47.7(8) . . ? O2A Cl3 O4A 90.1(8) . . ? O1A Cl3 O4A 112.8(7) . . ? O1B O1A Cl3 58.6(7) . . ? O1B O1A O3A 102.0(11) . . ? Cl3 O1A O3A 44.5(5) . . ? O1A O1B Cl3 86.9(13) . . ? O1A O1B O2B 132.2(9) . . ? Cl3 O1B O2B 51.1(8) . . ? O4B O4A O2B 111.3(9) . . ? O4B O4A Cl3 59.4(6) . . ? O2B O4A Cl3 52.1(4) . . ? O4A O4B O3A 129.9(11) . . ? O4A O4B Cl3 72.8(6) . . ? O3A O4B Cl3 57.0(8) . . ? O2B O2A Cl3 57.3(3) . . ? O2B O2A O3B 109.6(5) . . ? Cl3 O2A O3B 56.0(4) . . ? Cl3 O2B O2A 64.2(5) . . ? Cl3 O2B O4A 65.8(8) . . ? O2A O2B O4A 95.1(7) . . ? Cl3 O2B O1B 49.3(8) . . ? O2A O2B O1B 99.3(7) . . ? O4A O2B O1B 94.5(9) . . ? O4B O3A Cl3 66.6(11) . . ? O4B O3A O3B 113.3(11) . . ? Cl3 O3A O3B 60.0(10) . . ? O4B O3A O1A 93.6(16) . . ? Cl3 O3A O1A 57.1(9) . . ? O3B O3A O1A 89.1(13) . . ? Cl3 O3B O3A 52.7(9) . . ? Cl3 O3B O2A 58.9(4) . . ? O3A O3B O2A 102.8(10) . . ? O21B O21A O21A 123.7(6) . 2_567 ? 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 N2 Co1 N3 C5 -173.04(19) . . . . ? N4 Co1 N3 C5 2.76(18) . . . . ? N5 Co1 N3 C5 -86.77(18) . . . . ? N1 Co1 N3 C5 100.08(18) . . . . ? Cl1 Co1 N3 C5 50.3(13) . . . . ? N2 Co1 N3 C4 11.71(17) . . . . ? N4 Co1 N3 C4 -172.49(18) . . . . ? N5 Co1 N3 C4 97.98(17) . . . . ? N1 Co1 N3 C4 -75.17(17) . . . . ? Cl1 Co1 N3 C4 -125.0(12) . . . . ? N3 Co1 N2 C11 124.32(16) . . . . ? N4 Co1 N2 C11 104.1(4) . . . . ? N5 Co1 N2 C11 29.31(15) . . . . ? N1 Co1 N2 C11 -144.89(16) . . . . ? Cl1 Co1 N2 C11 -57.72(15) . . . . ? N3 Co1 N2 C2 -115.29(17) . . . . ? N4 Co1 N2 C2 -135.5(4) . . . . ? N5 Co1 N2 C2 149.70(17) . . . . ? N1 Co1 N2 C2 -24.50(17) . . . . ? Cl1 Co1 N2 C2 62.67(16) . . . . ? N3 Co1 N2 C3 7.47(16) . . . . ? N4 Co1 N2 C3 -12.8(5) . . . . ? N5 Co1 N2 C3 -87.54(16) . . . . ? N1 Co1 N2 C3 98.26(16) . . . . ? Cl1 Co1 N2 C3 -174.57(14) . . . . ? N3 Co1 N4 C10 -177.0(2) . . . . ? N2 Co1 N4 C10 -156.6(3) . . . . ? N5 Co1 N4 C10 -82.2(2) . . . . ? N1 Co1 N4 C10 93.4(2) . . . . ? Cl1 Co1 N4 C10 5.20(19) . . . . ? N3 Co1 N4 C6 -5.83(15) . . . . ? N2 Co1 N4 C6 14.5(5) . . . . ? N5 Co1 N4 C6 88.94(16) . . . . ? N1 Co1 N4 C6 -95.46(16) . . . . ? Cl1 Co1 N4 C6 176.36(14) . . . . ? N3 Co1 N5 C12 -92.29(16) . . . . ? N2 Co1 N5 C12 -6.62(15) . . . . ? N4 Co1 N5 C12 -174.90(15) . . . . ? N1 Co1 N5 C12 35.5(6) . . . . ? Cl1 Co1 N5 C12 89.73(15) . . . . ? N3 Co1 N1 C1 86.05(18) . . . . ? N2 Co1 N1 C1 0.12(18) . . . . ? N4 Co1 N1 C1 168.70(17) . . . . ? N5 Co1 N1 C1 -41.9(6) . . . . ? Cl1 Co1 N1 C1 -96.21(17) . . . . ? C11 N2 C3 C4 -140.3(2) . . . . ? C2 N2 C3 C4 94.5(3) . . . . ? Co1 N2 C3 C4 -24.5(2) . . . . ? C10 N4 C6 C7 0.8(3) . . . . ? Co1 N4 C6 C7 -171.39(17) . . . . ? C10 N4 C6 C5 179.89(19) . . . . ? Co1 N4 C6 C5 7.7(2) . . . . ? C5 N3 C4 C3 157.9(2) . . . . ? Co1 N3 C4 C3 -27.3(3) . . . . ? N2 C3 C4 N3 32.1(3) . . . . ? C4 N3 C5 C6 175.7(2) . . . . ? Co1 N3 C5 C6 0.9(3) . . . . ? N4 C6 C5 N3 -5.8(3) . . . . ? C7 C6 C5 N3 173.2(2) . . . . ? N4 C6 C7 C8 0.0(3) . . . . ? C5 C6 C7 C8 -179.0(2) . . . . ? C9 C8 C7 C6 -0.5(3) . . . . ? Co1 N5 C12 C11 -17.5(2) . . . . ? C6 N4 C10 C9 -1.1(3) . . . . ? Co1 N4 C10 C9 169.51(16) . . . . ? C2 N2 C11 C12 -162.3(2) . . . . ? C3 N2 C11 C12 72.2(2) . . . . ? Co1 N2 C11 C12 -45.8(2) . . . . ? N5 C12 C11 N2 41.4(3) . . . . ? C7 C8 C9 C10 0.2(3) . . . . ? N4 C10 C9 C8 0.6(3) . . . . ? C11 N2 C2 C1 160.5(2) . . . . ? C3 N2 C2 C1 -76.6(3) . . . . ? Co1 N2 C2 C1 44.2(2) . . . . ? Co1 N1 C1 C2 24.3(3) . . . . ? N2 C2 C1 N1 -44.8(3) . . . . ? O3A Cl3 O1A O1B 166(2) . . . . ? O2B Cl3 O1A O1B -26.1(17) . . . . ? O3B Cl3 O1A O1B 102.9(13) . . . . ? O4B Cl3 O1A O1B -142.1(15) . . . . ? O2A Cl3 O1A O1B 37.8(19) . . . . ? O4A Cl3 O1A O1B -93.7(19) . . . . ? O1B Cl3 O1A O3A -166(2) . . . . ? O2B Cl3 O1A O3A 168.2(18) . . . . ? O3B Cl3 O1A O3A -62.8(18) . . . . ? O4B Cl3 O1A O3A 52.2(18) . . . . ? O2A Cl3 O1A O3A -128(2) . . . . ? O4A Cl3 O1A O3A 101(2) . . . . ? O3A O1A O1B Cl3 10.2(17) . . . . ? Cl3 O1A O1B O2B 26.0(12) . . . . ? O3A O1A O1B O2B 36(3) . . . . ? O3A Cl3 O1B O1A -15(2) . . . . ? O2B Cl3 O1B O1A 155.3(15) . . . . ? O3B Cl3 O1B O1A -87.4(11) . . . . ? O4B Cl3 O1B O1A 48(2) . . . . ? O2A Cl3 O1B O1A -158.3(12) . . . . ? O4A Cl3 O1B O1A 100(2) . . . . ? O3A Cl3 O1B O2B -170(2) . . . . ? O3B Cl3 O1B O2B 117.3(6) . . . . ? O4B Cl3 O1B O2B -106.9(11) . . . . ? O2A Cl3 O1B O2B 46.4(8) . . . . ? O1A Cl3 O1B O2B -155.3(15) . . . . ? O4A Cl3 O1B O2B -54.8(10) . . . . ? O3A Cl3 O4A O4B -0.3(13) . . . . ? O1B Cl3 O4A O4B -120.6(15) . . . . ? O2B Cl3 O4A O4B 174.0(8) . . . . ? O3B Cl3 O4A O4B 71.0(12) . . . . ? O2A Cl3 O4A O4B 120.3(6) . . . . ? O1A Cl3 O4A O4B -83.4(10) . . . . ? O3A Cl3 O4A O2B -174.3(13) . . . . ? O1B Cl3 O4A O2B 65.4(16) . . . . ? O3B Cl3 O4A O2B -103.0(11) . . . . ? O4B Cl3 O4A O2B -174.0(8) . . . . ? O2A Cl3 O4A O2B -53.7(5) . . . . ? O1A Cl3 O4A O2B 102.6(10) . . . . ? O2B O4A O4B O3A 6(2) . . . . ? Cl3 O4A O4B O3A 0.4(17) . . . . ? O2B O4A O4B Cl3 5.1(7) . . . . ? O3A Cl3 O4B O4A 179.6(15) . . . . ? O1B Cl3 O4B O4A 85.8(18) . . . . ? O2B Cl3 O4B O4A -5.7(7) . . . . ? O3B Cl3 O4B O4A -139.3(7) . . . . ? O2A Cl3 O4B O4A -68.7(9) . . . . ? O1A Cl3 O4B O4A 111.3(7) . . . . ? O1B Cl3 O4B O3A -94(2) . . . . ? O2B Cl3 O4B O3A 174.7(15) . . . . ? O3B Cl3 O4B O3A 41.1(14) . . . . ? O2A Cl3 O4B O3A 111.7(16) . . . . ? O1A Cl3 O4B O3A -68.3(15) . . . . ? O4A Cl3 O4B O3A -179.6(16) . . . . ? O3A Cl3 O2A O2B 163.1(17) . . . . ? O1B Cl3 O2A O2B -56.7(12) . . . . ? O3B Cl3 O2A O2B -155.8(5) . . . . ? O4B Cl3 O2A O2B 100.3(4) . . . . ? O1A Cl3 O2A O2B -79.7(14) . . . . ? O4A Cl3 O2A O2B 56.7(8) . . . . ? O3A Cl3 O2A O3B -41.1(17) . . . . ? O1B Cl3 O2A O3B 99.1(11) . . . . ? O2B Cl3 O2A O3B 155.8(5) . . . . ? O4B Cl3 O2A O3B -103.9(4) . . . . ? O1A Cl3 O2A O3B 76.2(13) . . . . ? O4A Cl3 O2A O3B -147.5(8) . . . . ? O3A Cl3 O2B O2A -87(6) . . . . ? O1B Cl3 O2B O2A 130.8(6) . . . . ? O3B Cl3 O2B O2A 25.1(6) . . . . ? O4B Cl3 O2B O2A -104.3(4) . . . . ? O1A Cl3 O2B O2A 145.5(9) . . . . ? O4A Cl3 O2B O2A -109.0(7) . . . . ? O3A Cl3 O2B O4A 22(6) . . . . ? O1B Cl3 O2B O4A -120.1(7) . . . . ? O3B Cl3 O2B O4A 134.2(6) . . . . ? O4B Cl3 O2B O4A 4.8(6) . . . . ? O2A Cl3 O2B O4A 109.0(7) . . . . ? O1A Cl3 O2B O4A -105.4(9) . . . . ? O3A Cl3 O2B O1B 143(6) . . . . ? O3B Cl3 O2B O1B -105.7(5) . . . . ? O4B Cl3 O2B O1B 124.9(4) . . . . ? O2A Cl3 O2B O1B -130.8(6) . . . . ? O1A Cl3 O2B O1B 14.7(6) . . . . ? O4A Cl3 O2B O1B 120.1(7) . . . . ? O3B O2A O2B Cl3 -21.1(4) . . . . ? Cl3 O2A O2B O4A -59.9(7) . . . . ? O3B O2A O2B O4A -81.1(9) . . . . ? Cl3 O2A O2B O1B 35.5(7) . . . . ? O3B O2A O2B O1B 14.4(8) . . . . ? O4B O4A O2B Cl3 -5.6(7) . . . . ? O4B O4A O2B O2A 53.1(11) . . . . ? Cl3 O4A O2B O2A 58.7(6) . . . . ? O4B O4A O2B O1B -46.7(10) . . . . ? Cl3 O4A O2B O1B -41.1(6) . . . . ? O1A O1B O2B Cl3 -34(2) . . . . ? O1A O1B O2B O2A -78(2) . . . . ? Cl3 O1B O2B O2A -43.7(5) . . . . ? O1A O1B O2B O4A 18(2) . . . . ? Cl3 O1B O2B O4A 52.3(7) . . . . ? O4A O4B O3A Cl3 -0.5(19) . . . . ? O4A O4B O3A O3B -39(2) . . . . ? Cl3 O4B O3A O3B -38.8(7) . . . . ? O4A O4B O3A O1A 51(2) . . . . ? Cl3 O4B O3A O1A 51.7(9) . . . . ? O1B Cl3 O3A O4B 119.8(6) . . . . ? O2B Cl3 O3A O4B -20(7) . . . . ? O3B Cl3 O3A O4B -138.3(10) . . . . ? O2A Cl3 O3A O4B -98.0(16) . . . . ? O1A Cl3 O3A O4B 111.1(13) . . . . ? O4A Cl3 O3A O4B 0.3(12) . . . . ? O1B Cl3 O3A O3B -101.8(8) . . . . ? O2B Cl3 O3A O3B 118(6) . . . . ? O4B Cl3 O3A O3B 138.3(10) . . . . ? O2A Cl3 O3A O3B 40.3(13) . . . . ? O1A Cl3 O3A O3B -110.5(9) . . . . ? O4A Cl3 O3A O3B 138.6(7) . . . . ? O1B Cl3 O3A O1A 8.7(13) . . . . ? O2B Cl3 O3A O1A -131(6) . . . . ? O3B Cl3 O3A O1A 110.5(9) . . . . ? O4B Cl3 O3A O1A -111.1(13) . . . . ? O2A Cl3 O3A O1A 150.8(9) . . . . ? O4A Cl3 O3A O1A -110.8(8) . . . . ? O1B O1A O3A O4B -72(2) . . . . ? Cl3 O1A O3A O4B -59.1(7) . . . . ? O1B O1A O3A Cl3 -12(2) . . . . ? O1B O1A O3A O3B 42(2) . . . . ? Cl3 O1A O3A O3B 54.2(7) . . . . ? O1B Cl3 O3B O3A 106.5(18) . . . . ? O2B Cl3 O3B O3A -165.2(10) . . . . ? O4B Cl3 O3B O3A -36.4(10) . . . . ? O2A Cl3 O3B O3A -141.6(10) . . . . ? O1A Cl3 O3B O3A 70.8(13) . . . . ? O4A Cl3 O3B O3A -85.0(17) . . . . ? O3A Cl3 O3B O2A 141.6(10) . . . . ? O1B Cl3 O3B O2A -111.9(16) . . . . ? O2B Cl3 O3B O2A -23.5(5) . . . . ? O4B Cl3 O3B O2A 105.3(4) . . . . ? O1A Cl3 O3B O2A -147.5(9) . . . . ? O4A Cl3 O3B O2A 56.7(13) . . . . ? O4B O3A O3B Cl3 41.6(11) . . . . ? O1A O3A O3B Cl3 -51.8(7) . . . . ? O4B O3A O3B O2A 8.6(15) . . . . ? Cl3 O3A O3B O2A -33.0(8) . . . . ? O1A O3A O3B O2A -84.8(9) . . . . ? O2B O2A O3B Cl3 21.5(4) . . . . ? O2B O2A O3B O3A 51.9(9) . . . . ? Cl3 O2A O3B O3A 30.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.748 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.067