Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Hartshorn, Richard' 'Otter, Carl A.' _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_requested_journal 'Dalton Transactions' _publ_section_title ; Polydentate ligand construction: preparation of oxime-imine complexes via intramolecular condensation reactions ; data_c136s _database_code_CSD 188183 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H31 Cl4 Co N6 O3 Zn' _chemical_formula_sum 'C14 H31 Cl4 Co N6 O3 Zn' _chemical_formula_weight 597.55 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 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.598(5) _cell_length_b 11.705(4) _cell_length_c 15.371(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.312(6) _cell_angle_gamma 90.00 _cell_volume 2335.6(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 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 2.223 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _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 23123 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.45 _reflns_number_total 4793 _reflns_number_gt 4012 _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^)+(0.0433P)^2^+1.0221P] 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 4793 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.003 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 O3 O 0.5466(2) 0.97715(18) 0.84422(19) 0.0461(5) Uani 1 1 d . . . Zn1 Zn 0.80407(2) 0.01865(2) 0.159298(19) 0.02382(8) Uani 1 1 d . . . Co1 Co 0.21832(2) 0.96906(2) 0.289076(19) 0.01632(8) Uani 1 1 d . . . Cl3 Cl 0.88241(4) -0.15432(5) 0.16536(4) 0.02812(14) Uani 1 1 d . . . Cl4 Cl 0.90949(4) 0.15238(5) 0.12604(4) 0.02586(13) Uani 1 1 d . . . Cl2 Cl 0.64923(5) 0.01714(6) 0.05215(5) 0.04557(18) Uani 1 1 d . . . Cl1 Cl 0.78401(6) 0.06978(6) 0.29474(5) 0.04617(19) Uani 1 1 d . . . N2 N 0.20627(13) 1.03518(15) 0.17584(12) 0.0196(4) Uani 1 1 d . . . O1 O 0.33817(12) 1.12338(14) 0.41680(11) 0.0282(4) Uani 1 1 d . . . N1 N 0.29745(13) 1.10344(15) 0.33230(12) 0.0198(4) Uani 1 1 d . . . N5 N 0.23349(13) 0.91106(15) 0.40635(12) 0.0181(4) Uani 1 1 d . . . N6 N 0.09694(14) 1.04694(16) 0.30408(13) 0.0218(4) Uani 1 1 d . . . H6A H 0.1131 1.1211 0.3228 0.026 Uiso 1 1 calc R . . H6B H 0.0452 1.0482 0.2496 0.026 Uiso 1 1 calc R . . N3 N 0.13553(14) 0.84248(15) 0.21693(12) 0.0207(4) Uani 1 1 d . . . H3A H 0.1608 0.7731 0.2419 0.025 Uiso 1 1 calc R . . H3B H 0.0680 0.8484 0.2166 0.025 Uiso 1 1 calc R . . C8 C 0.38239(16) 0.83881(17) 0.38622(15) 0.0198(4) Uani 1 1 d . . . C9 C 0.31749(16) 0.85831(18) 0.44650(15) 0.0197(4) Uani 1 1 d . . . C4 C 0.23958(18) 1.2033(2) 0.09304(17) 0.0276(5) Uani 1 1 d . . . H4A H 0.2381 1.1524 0.0413 0.033 Uiso 1 1 calc R . . H4B H 0.2996 1.2549 0.1031 0.033 Uiso 1 1 calc R . . C14 C 0.06240(17) 0.9831(2) 0.37406(16) 0.0258(5) Uani 1 1 d . . . H14A H 0.0231 0.9143 0.3465 0.031 Uiso 1 1 calc R . . H14B H 0.0172 1.0321 0.3982 0.031 Uiso 1 1 calc R . . C6 C 0.13837(19) 0.97596(19) 0.09649(15) 0.0258(5) Uani 1 1 d . . . H6C H 0.1627 0.9870 0.0424 0.031 Uiso 1 1 calc R . . H6D H 0.0670 1.0052 0.0824 0.031 Uiso 1 1 calc R . . C12 C 0.42077(19) 0.9215(2) 0.60051(17) 0.0347(6) Uani 1 1 d . . . H12A H 0.4813 0.9317 0.5792 0.052 Uiso 1 1 calc R . . H12B H 0.4430 0.9005 0.6652 0.052 Uiso 1 1 calc R . . H12C H 0.3816 0.9930 0.5925 0.052 Uiso 1 1 calc R . . C2 C 0.25024(16) 1.13329(19) 0.17683(15) 0.0210(4) Uani 1 1 d . . . C1 C 0.30566(16) 1.17339(18) 0.26731(16) 0.0214(5) Uani 1 1 d . . . C7 C 0.14277(19) 0.8516(2) 0.12243(16) 0.0267(5) Uani 1 1 d . . . H7A H 0.0850 0.8098 0.0797 0.032 Uiso 1 1 calc R . . H7B H 0.2082 0.8175 0.1192 0.032 Uiso 1 1 calc R . . C3 C 0.36522(18) 1.2818(2) 0.28845(17) 0.0293(5) Uani 1 1 d . . . H3C H 0.3733 1.3037 0.3517 0.044 Uiso 1 1 calc R . . H3D H 0.3283 1.3422 0.2475 0.044 Uiso 1 1 calc R . . H3E H 0.4333 1.2708 0.2800 0.044 Uiso 1 1 calc R . . C10 C 0.48026(17) 0.7728(2) 0.41472(17) 0.0282(5) Uani 1 1 d . . . H10A H 0.5069 0.7634 0.3625 0.042 Uiso 1 1 calc R . . H10B H 0.4675 0.6975 0.4371 0.042 Uiso 1 1 calc R . . H10C H 0.5309 0.8141 0.4634 0.042 Uiso 1 1 calc R . . C11 C 0.35268(18) 0.8268(2) 0.54539(15) 0.0253(5) Uani 1 1 d . . . H11A H 0.3919 0.7544 0.5535 0.030 Uiso 1 1 calc R . . H11B H 0.2921 0.8153 0.5676 0.030 Uiso 1 1 calc R . . C13 C 0.15695(17) 0.9491(2) 0.45007(16) 0.0251(5) Uani 1 1 d . . . H13A H 0.1835 1.0149 0.4907 0.030 Uiso 1 1 calc R . . H13B H 0.1404 0.8865 0.4867 0.030 Uiso 1 1 calc R . . O2 O 0.39622(13) 0.86142(16) 0.24464(12) 0.0280(4) Uani 1 1 d . . . N4 N 0.34422(13) 0.88559(15) 0.30707(12) 0.0196(4) Uani 1 1 d . . . C5 C 0.1406(2) 1.2740(2) 0.07016(18) 0.0363(6) Uani 1 1 d . . . H5A H 0.0820 1.2237 0.0671 0.054 Uiso 1 1 calc R . . H5B H 0.1300 1.3117 0.0112 0.054 Uiso 1 1 calc R . . H5C H 0.1463 1.3318 0.1175 0.054 Uiso 1 1 calc R . . H3WA H 0.487(3) 0.976(3) 0.831(2) 0.055(12) Uiso 1 1 d . . . H2OX H 0.404(2) 0.921(3) 0.219(2) 0.036(8) Uiso 1 1 d . . . H3WB H 0.580(3) 0.986(3) 0.908(3) 0.069(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3 0.0525(14) 0.0431(12) 0.0540(15) 0.0109(10) 0.0330(12) 0.0029(10) Zn1 0.02388(14) 0.02179(15) 0.02810(16) -0.00091(11) 0.01129(11) 0.00159(10) Co1 0.01624(15) 0.01574(15) 0.01702(15) -0.00036(11) 0.00499(11) 0.00063(10) Cl3 0.0231(3) 0.0220(3) 0.0372(3) -0.0017(2) 0.0058(2) 0.0032(2) Cl4 0.0295(3) 0.0239(3) 0.0264(3) 0.0010(2) 0.0116(2) -0.0020(2) Cl2 0.0243(3) 0.0467(4) 0.0577(5) 0.0065(3) 0.0001(3) 0.0067(3) Cl1 0.0799(5) 0.0297(3) 0.0462(4) -0.0073(3) 0.0453(4) -0.0073(3) N2 0.0212(9) 0.0198(9) 0.0179(9) 0.0006(7) 0.0059(7) 0.0013(7) O1 0.0286(8) 0.0299(9) 0.0219(9) -0.0052(7) 0.0011(7) -0.0053(7) N1 0.0160(8) 0.0191(9) 0.0230(10) -0.0032(7) 0.0040(7) 0.0004(7) N5 0.0185(9) 0.0173(9) 0.0198(9) -0.0021(7) 0.0079(7) -0.0018(7) N6 0.0198(9) 0.0213(9) 0.0234(10) -0.0012(8) 0.0049(7) 0.0033(7) N3 0.0222(9) 0.0190(9) 0.0207(10) -0.0016(7) 0.0060(7) -0.0015(7) C8 0.0187(10) 0.0158(10) 0.0242(12) -0.0017(9) 0.0053(9) -0.0024(8) C9 0.0221(10) 0.0145(10) 0.0228(11) -0.0018(8) 0.0072(9) -0.0041(8) C4 0.0313(12) 0.0247(12) 0.0298(13) 0.0060(10) 0.0139(10) -0.0011(10) C14 0.0220(11) 0.0317(13) 0.0267(13) -0.0014(10) 0.0117(10) 0.0023(9) C6 0.0330(13) 0.0273(12) 0.0158(11) -0.0026(9) 0.0052(9) -0.0018(10) C12 0.0292(13) 0.0469(16) 0.0247(13) -0.0039(11) 0.0028(10) 0.0002(11) C2 0.0180(10) 0.0219(11) 0.0249(12) 0.0022(9) 0.0093(9) 0.0037(8) C1 0.0189(10) 0.0179(11) 0.0292(12) 0.0011(9) 0.0097(9) 0.0004(8) C7 0.0336(13) 0.0253(12) 0.0211(12) -0.0060(9) 0.0080(10) -0.0025(10) C3 0.0272(12) 0.0218(12) 0.0389(14) -0.0019(10) 0.0097(10) -0.0049(9) C10 0.0206(11) 0.0276(12) 0.0353(13) 0.0014(10) 0.0069(10) 0.0063(9) C11 0.0269(12) 0.0269(12) 0.0219(12) 0.0042(9) 0.0067(9) 0.0020(9) C13 0.0252(11) 0.0305(13) 0.0226(12) -0.0017(9) 0.0118(9) 0.0045(9) O2 0.0332(9) 0.0282(9) 0.0306(9) 0.0027(7) 0.0216(8) 0.0058(7) N4 0.0195(9) 0.0195(9) 0.0230(10) -0.0016(7) 0.0110(7) -0.0003(7) C5 0.0389(14) 0.0292(13) 0.0390(15) 0.0126(11) 0.0089(12) 0.0028(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 O3 H3WA 0.77(4) . ? O3 H3WB 0.95(4) . ? Zn1 Cl2 2.2544(9) . ? Zn1 Cl1 2.2594(10) . ? Zn1 Cl3 2.2767(9) . ? Zn1 Cl4 2.2809(8) . ? Co1 N2 1.8669(19) . ? Co1 N5 1.8792(19) . ? Co1 N1 1.9098(18) . ? Co1 N4 1.9184(18) . ? Co1 N6 1.9583(19) . ? Co1 N3 1.9873(18) . ? N2 C2 1.293(3) . ? N2 C6 1.466(3) . ? O1 N1 1.273(2) . ? N1 C1 1.322(3) . ? N5 C9 1.284(3) . ? N5 C13 1.466(3) . ? N6 C14 1.496(3) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? N3 C7 1.489(3) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? C8 N4 1.294(3) . ? C8 C9 1.475(3) . ? C8 C10 1.487(3) . ? C9 C11 1.497(3) . ? C4 C2 1.497(3) . ? C4 C5 1.529(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C14 C13 1.511(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C6 C7 1.506(3) . ? C6 H6C 0.9900 . ? C6 H6D 0.9900 . ? C12 C11 1.528(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C2 C1 1.449(3) . ? C1 C3 1.488(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O2 N4 1.380(2) . ? O2 H2OX 0.83(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H3WA O3 H3WB 114(4) . . ? Cl2 Zn1 Cl1 109.43(4) . . ? Cl2 Zn1 Cl3 110.29(3) . . ? Cl1 Zn1 Cl3 112.40(3) . . ? Cl2 Zn1 Cl4 110.75(3) . . ? Cl1 Zn1 Cl4 106.32(3) . . ? Cl3 Zn1 Cl4 107.57(3) . . ? N2 Co1 N5 176.52(8) . . ? N2 Co1 N1 82.36(8) . . ? N5 Co1 N1 94.25(8) . . ? N2 Co1 N4 99.94(8) . . ? N5 Co1 N4 80.75(7) . . ? N1 Co1 N4 89.03(8) . . ? N2 Co1 N6 94.22(8) . . ? N5 Co1 N6 84.89(8) . . ? N1 Co1 N6 89.03(8) . . ? N4 Co1 N6 165.32(8) . . ? N2 Co1 N3 84.89(8) . . ? N5 Co1 N3 98.52(8) . . ? N1 Co1 N3 167.18(8) . . ? N4 Co1 N3 91.94(8) . . ? N6 Co1 N3 93.17(8) . . ? C2 N2 C6 127.17(19) . . ? C2 N2 Co1 116.44(15) . . ? C6 N2 Co1 116.00(14) . . ? O1 N1 C1 123.28(19) . . ? O1 N1 Co1 122.34(14) . . ? C1 N1 Co1 114.38(15) . . ? C9 N5 C13 125.26(19) . . ? C9 N5 Co1 117.58(15) . . ? C13 N5 Co1 116.10(14) . . ? C14 N6 Co1 107.95(13) . . ? C14 N6 H6A 110.1 . . ? Co1 N6 H6A 110.1 . . ? C14 N6 H6B 110.1 . . ? Co1 N6 H6B 110.1 . . ? H6A N6 H6B 108.4 . . ? C7 N3 Co1 107.46(13) . . ? C7 N3 H3A 110.2 . . ? Co1 N3 H3A 110.2 . . ? C7 N3 H3B 110.2 . . ? Co1 N3 H3B 110.2 . . ? H3A N3 H3B 108.5 . . ? N4 C8 C9 112.19(18) . . ? N4 C8 C10 124.8(2) . . ? C9 C8 C10 123.1(2) . . ? N5 C9 C8 112.68(19) . . ? N5 C9 C11 125.2(2) . . ? C8 C9 C11 121.96(19) . . ? C2 C4 C5 110.3(2) . . ? C2 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? C2 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N6 C14 C13 108.11(18) . . ? N6 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? N6 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? N2 C6 C7 105.73(18) . . ? N2 C6 H6C 110.6 . . ? C7 C6 H6C 110.6 . . ? N2 C6 H6D 110.6 . . ? C7 C6 H6D 110.6 . . ? H6C C6 H6D 108.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C2 C1 113.9(2) . . ? N2 C2 C4 123.4(2) . . ? C1 C2 C4 122.5(2) . . ? N1 C1 C2 112.83(19) . . ? N1 C1 C3 121.7(2) . . ? C2 C1 C3 125.4(2) . . ? N3 C7 C6 108.59(18) . . ? N3 C7 H7A 110.0 . . ? C6 C7 H7A 110.0 . . ? N3 C7 H7B 110.0 . . ? C6 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? C1 C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C12 110.01(19) . . ? C9 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C9 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N5 C13 C14 106.40(18) . . ? N5 C13 H13A 110.4 . . ? C14 C13 H13A 110.4 . . ? N5 C13 H13B 110.4 . . ? C14 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? N4 O2 H2OX 109(2) . . ? C8 N4 O2 114.96(17) . . ? C8 N4 Co1 116.25(14) . . ? O2 N4 Co1 128.61(14) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.266 _refine_diff_density_min -1.042 _refine_diff_density_rms 0.076 #====END data_c204b _database_code_CSD 188184 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H22 Cl4 Co N5 O2 Zn' _chemical_formula_weight 486.41 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.006(4) _cell_length_b 10.967(4) _cell_length_c 16.506(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.348(5) _cell_angle_gamma 90.00 _cell_volume 1809.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.840 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'blessing, Acta. Crys., 1995, A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22618 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.41 _reflns_number_total 3682 _reflns_number_gt 3081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0598P)^2^+6.8403P] 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 3682 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.31079(5) 0.22448(5) 0.04636(3) 0.02499(16) Uani 1 1 d . . . Co1 Co 0.30879(6) 0.24409(5) 0.38773(3) 0.01858(16) Uani 1 1 d . . . Cl3 Cl 0.41896(11) 0.35987(11) -0.03082(7) 0.0306(3) Uani 1 1 d . . . Cl4 Cl 0.16008(13) 0.33798(11) 0.11335(8) 0.0368(3) Uani 1 1 d . . . Cl5 Cl 0.20402(12) 0.08808(11) -0.03633(7) 0.0346(3) Uani 1 1 d . . . Cl6 Cl 0.45902(13) 0.13269(12) 0.13111(8) 0.0414(3) Uani 1 1 d . . . N1 N 0.3953(4) 0.3630(3) 0.3261(2) 0.0224(8) Uani 1 1 d . . . N3 N 0.2439(4) 0.1100(3) 0.4555(2) 0.0242(8) Uani 1 1 d . . . H3A H 0.1527 0.1158 0.4595 0.029 Uiso 1 1 calc R . . H3B H 0.2631 0.0362 0.4322 0.029 Uiso 1 1 calc R . . O2 O 0.4658(3) 0.1519(3) 0.36973(18) 0.0244(7) Uani 1 1 d . . . N2 N 0.3859(4) 0.3105(4) 0.4888(2) 0.0252(8) Uani 1 1 d . . . H2A H 0.4767 0.2972 0.4915 0.030 Uiso 1 1 calc R . . H2B H 0.3712 0.3933 0.4906 0.030 Uiso 1 1 calc R . . O1 O 0.3484(3) 0.4686(3) 0.3117(2) 0.0335(8) Uani 1 1 d . . . N4 N 0.2227(4) 0.1754(4) 0.2896(2) 0.0264(8) Uani 1 1 d . . . H4A H 0.2592 0.2088 0.2444 0.032 Uiso 1 1 calc R . . H4B H 0.2358 0.0924 0.2884 0.032 Uiso 1 1 calc R . . N5 N 0.1467(4) 0.3410(3) 0.3967(2) 0.0228(8) Uani 1 1 d . . . H5A H 0.0994 0.3139 0.4399 0.027 Uiso 1 1 calc R . . H5B H 0.1689 0.4214 0.4056 0.027 Uiso 1 1 calc R . . C2 C 0.5442(4) 0.2076(4) 0.3244(3) 0.0241(9) Uani 1 1 d . . . C4 C 0.6702(5) 0.1451(5) 0.3018(3) 0.0341(11) Uani 1 1 d . . . H4C H 0.7448 0.1742 0.3369 0.051 Uiso 1 1 calc R . . H4D H 0.6881 0.1634 0.2451 0.051 Uiso 1 1 calc R . . H4E H 0.6602 0.0569 0.3085 0.051 Uiso 1 1 calc R . . C7 C 0.0772(5) 0.2028(5) 0.2897(3) 0.0286(10) Uani 1 1 d . . . H7A H 0.0314 0.1446 0.3250 0.034 Uiso 1 1 calc R . . H7B H 0.0369 0.1962 0.2341 0.034 Uiso 1 1 calc R . . C1 C 0.5102(4) 0.3270(4) 0.2979(3) 0.0256(9) Uani 1 1 d . . . C8 C 0.0630(5) 0.3299(4) 0.3207(3) 0.0290(10) Uani 1 1 d . . . H8A H 0.0930 0.3892 0.2800 0.035 Uiso 1 1 calc R . . H8B H -0.0318 0.3470 0.3315 0.035 Uiso 1 1 calc R . . C6 C 0.3101(5) 0.1181(5) 0.5369(3) 0.0334(11) Uani 1 1 d . . . H6A H 0.3994 0.0792 0.5369 0.040 Uiso 1 1 calc R . . H6B H 0.2559 0.0757 0.5771 0.040 Uiso 1 1 calc R . . C5 C 0.3236(5) 0.2508(5) 0.5581(3) 0.0320(11) Uani 1 1 d . . . H5C H 0.2347 0.2868 0.5670 0.038 Uiso 1 1 calc R . . H5D H 0.3804 0.2612 0.6081 0.038 Uiso 1 1 calc R . . C3 C 0.5921(5) 0.4085(5) 0.2471(4) 0.0409(13) Uani 1 1 d . . . H3C H 0.5439 0.4241 0.1952 0.061 Uiso 1 1 calc R . . H3D H 0.6778 0.3691 0.2372 0.061 Uiso 1 1 calc R . . H3E H 0.6083 0.4859 0.2756 0.061 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 Zn1 0.0248(3) 0.0233(3) 0.0270(3) 0.0018(2) 0.0028(2) -0.0001(2) Co1 0.0203(3) 0.0135(3) 0.0222(3) -0.0003(2) 0.0045(2) -0.0009(2) Cl3 0.0285(6) 0.0280(6) 0.0360(6) 0.0005(5) 0.0100(5) -0.0043(4) Cl4 0.0406(7) 0.0316(6) 0.0394(7) 0.0075(5) 0.0188(5) 0.0062(5) Cl5 0.0380(6) 0.0259(6) 0.0392(7) 0.0007(5) -0.0074(5) -0.0051(5) Cl6 0.0422(7) 0.0332(7) 0.0472(7) 0.0043(5) -0.0169(6) 0.0014(5) N1 0.0255(19) 0.0181(18) 0.0237(18) 0.0010(14) 0.0022(15) -0.0018(14) N3 0.0225(18) 0.0203(18) 0.030(2) 0.0002(15) 0.0043(15) 0.0000(14) O2 0.0270(16) 0.0187(15) 0.0279(16) 0.0008(12) 0.0066(13) 0.0027(12) N2 0.0225(18) 0.027(2) 0.0264(19) -0.0013(16) 0.0009(15) -0.0005(15) O1 0.0384(19) 0.0207(17) 0.042(2) 0.0083(14) 0.0048(15) 0.0030(14) N4 0.0281(19) 0.026(2) 0.0255(19) -0.0046(15) 0.0058(15) -0.0030(16) N5 0.0231(18) 0.0204(18) 0.0251(19) -0.0005(15) 0.0028(15) 0.0007(14) C2 0.024(2) 0.027(2) 0.021(2) -0.0015(18) -0.0007(17) 0.0005(18) C4 0.028(2) 0.043(3) 0.032(3) 0.003(2) 0.005(2) 0.011(2) C7 0.027(2) 0.035(3) 0.024(2) -0.0004(19) 0.0009(18) -0.007(2) C1 0.026(2) 0.025(2) 0.027(2) 0.0013(18) 0.0039(18) -0.0020(18) C8 0.027(2) 0.030(2) 0.030(2) 0.0020(19) -0.0038(19) 0.0026(19) C6 0.037(3) 0.034(3) 0.029(2) 0.010(2) -0.002(2) -0.002(2) C5 0.034(3) 0.041(3) 0.022(2) 0.000(2) 0.0000(19) 0.000(2) C3 0.037(3) 0.035(3) 0.052(3) 0.013(2) 0.017(2) 0.001(2) _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 Cl6 2.2361(14) . ? Zn1 Cl3 2.2609(13) . ? Zn1 Cl5 2.2633(14) . ? Zn1 Cl4 2.2765(14) . ? Co1 N1 1.886(4) . ? Co1 O2 1.902(3) . ? Co1 N2 1.949(4) . ? Co1 N5 1.950(4) . ? Co1 N4 1.954(4) . ? Co1 N3 1.973(4) . ? N1 O1 1.269(5) . ? N1 C1 1.318(6) . ? N3 C6 1.476(6) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? O2 C2 1.264(5) . ? N2 C5 1.479(6) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N4 C7 1.486(6) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? N5 C8 1.484(6) . ? N5 H5A 0.9200 . ? N5 H5B 0.9200 . ? C2 C1 1.417(6) . ? C2 C4 1.495(6) . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C4 H4E 0.9800 . ? C7 C8 1.494(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C1 C3 1.493(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C6 C5 1.502(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5 H5C 0.9900 . ? C5 H5D 0.9900 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl6 Zn1 Cl3 109.12(6) . . ? Cl6 Zn1 Cl5 111.36(6) . . ? Cl3 Zn1 Cl5 108.63(6) . . ? Cl6 Zn1 Cl4 112.20(6) . . ? Cl3 Zn1 Cl4 104.86(5) . . ? Cl5 Zn1 Cl4 110.40(6) . . ? N1 Co1 O2 83.27(15) . . ? N1 Co1 N2 91.66(16) . . ? O2 Co1 N2 91.83(15) . . ? N1 Co1 N5 93.78(16) . . ? O2 Co1 N5 175.33(14) . . ? N2 Co1 N5 91.88(16) . . ? N1 Co1 N4 90.91(16) . . ? O2 Co1 N4 90.25(15) . . ? N2 Co1 N4 176.86(16) . . ? N5 Co1 N4 86.17(16) . . ? N1 Co1 N3 171.84(16) . . ? O2 Co1 N3 89.17(14) . . ? N2 Co1 N3 85.49(16) . . ? N5 Co1 N3 93.96(16) . . ? N4 Co1 N3 92.19(16) . . ? O1 N1 C1 122.0(4) . . ? O1 N1 Co1 123.8(3) . . ? C1 N1 Co1 114.2(3) . . ? C6 N3 Co1 109.0(3) . . ? C6 N3 H3A 109.9 . . ? Co1 N3 H3A 109.9 . . ? C6 N3 H3B 109.9 . . ? Co1 N3 H3B 109.9 . . ? H3A N3 H3B 108.3 . . ? C2 O2 Co1 111.9(3) . . ? C5 N2 Co1 109.4(3) . . ? C5 N2 H2A 109.8 . . ? Co1 N2 H2A 109.8 . . ? C5 N2 H2B 109.8 . . ? Co1 N2 H2B 109.8 . . ? H2A N2 H2B 108.2 . . ? C7 N4 Co1 108.7(3) . . ? C7 N4 H4A 110.0 . . ? Co1 N4 H4A 110.0 . . ? C7 N4 H4B 110.0 . . ? Co1 N4 H4B 110.0 . . ? H4A N4 H4B 108.3 . . ? C8 N5 Co1 109.5(3) . . ? C8 N5 H5A 109.8 . . ? Co1 N5 H5A 109.8 . . ? C8 N5 H5B 109.8 . . ? Co1 N5 H5B 109.8 . . ? H5A N5 H5B 108.2 . . ? O2 C2 C1 118.8(4) . . ? O2 C2 C4 118.4(4) . . ? C1 C2 C4 122.7(4) . . ? C2 C4 H4C 109.5 . . ? C2 C4 H4D 109.5 . . ? H4C C4 H4D 109.5 . . ? C2 C4 H4E 109.5 . . ? H4C C4 H4E 109.5 . . ? H4D C4 H4E 109.5 . . ? N4 C7 C8 107.2(4) . . ? N4 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? N4 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? N1 C1 C2 111.7(4) . . ? N1 C1 C3 121.7(4) . . ? C2 C1 C3 126.6(4) . . ? N5 C8 C7 108.0(4) . . ? N5 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? N5 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? N3 C6 C5 107.6(4) . . ? N3 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? N3 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? N2 C5 C6 106.6(4) . . ? N2 C5 H5C 110.4 . . ? C6 C5 H5C 110.4 . . ? N2 C5 H5D 110.4 . . ? C6 C5 H5D 110.4 . . ? H5C C5 H5D 108.6 . . ? C1 C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.355 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.120 #====END data_carbol _database_code_CSD 188185 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31 Cl4 Co N6 O4' _chemical_formula_weight 524.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.137(5) _cell_length_b 11.532(4) _cell_length_c 14.020(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.683(4) _cell_angle_gamma 90.00 _cell_volume 2270.2(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 block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28940 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 26.42 _reflns_number_total 4609 _reflns_number_gt 3501 _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^)+(0.0303P)^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 4609 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _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 0.282462(17) 0.46843(2) 0.122234(15) 0.01649(7) Uani 1 1 d . . . Cl1 Cl 0.38189(3) 0.40986(4) 0.24933(3) 0.02153(11) Uani 1 1 d . . . Cl3 Cl 0.34684(4) 0.57575(4) 0.47515(3) 0.02854(12) Uani 1 1 d . . . Cl4 Cl 0.39159(3) 0.45627(5) 0.83561(3) 0.03347(13) Uani 1 1 d . . . Cl2 Cl 0.04369(4) 0.74343(4) 0.09931(4) 0.03351(13) Uani 1 1 d . . . N1 N 0.17470(11) 0.45562(13) 0.19572(10) 0.0201(3) Uani 1 1 d . . . N5 N 0.27869(10) 0.31737(12) 0.05994(9) 0.0159(3) Uani 1 1 d . . . O1 O 0.11516(9) 0.36313(12) 0.20479(9) 0.0288(3) Uani 1 1 d . . . H1OX H 0.1227 0.3136 0.1624 0.043 Uiso 1 1 calc R . . O2 O 0.16625(10) 0.61483(11) -0.01872(9) 0.0296(3) Uani 1 1 d . . . H2OX H 0.1391 0.6428 0.0262 0.044 Uiso 1 1 d R . . N3 N 0.39166(11) 0.51941(13) 0.06080(10) 0.0208(3) Uani 1 1 d . . . H3A H 0.4471 0.4948 0.0958 0.025 Uiso 1 1 calc R . . H3B H 0.3889 0.4884 0.0001 0.025 Uiso 1 1 calc R . . N2 N 0.28548(11) 0.61875(12) 0.17485(10) 0.0212(4) Uani 1 1 d . . . N4 N 0.20141(11) 0.50621(13) 0.00739(10) 0.0194(3) Uani 1 1 d . . . C7 C 0.23705(12) 0.31662(15) -0.02694(12) 0.0188(4) Uani 1 1 d . . . N6 N 0.45984(11) 0.08056(13) 0.12782(10) 0.0229(4) Uani 1 1 d . . . H6A H 0.4490 0.0748 0.1904 0.034 Uiso 1 1 calc R . . H6B H 0.5235 0.0751 0.1237 0.034 Uiso 1 1 calc R . . H6C H 0.4289 0.0223 0.0933 0.034 Uiso 1 1 calc R . . C6 C 0.19191(12) 0.42885(16) -0.05895(12) 0.0188(4) Uani 1 1 d . . . C1 C 0.16055(13) 0.54404(16) 0.24915(12) 0.0228(4) Uani 1 1 d . . . C5 C 0.39010(14) 0.64887(16) 0.05536(13) 0.0273(5) Uani 1 1 d . . . H5A H 0.3436 0.6746 0.0012 0.033 Uiso 1 1 calc R . . H5B H 0.4538 0.6784 0.0448 0.033 Uiso 1 1 calc R . . C2 C 0.22683(14) 0.64129(16) 0.23591(12) 0.0240(4) Uani 1 1 d . . . O3 O 0.16385(11) 0.97311(13) 0.08730(11) 0.0504(4) Uani 1 1 d . . . H3WA H 0.2064 0.9528 0.0602 0.076 Uiso 1 1 d R . . H3WB H 0.1285 0.9111 0.0900 0.076 Uiso 1 1 d R . . C8 C 0.14015(14) 0.44703(16) -0.15674(12) 0.0263(5) Uani 1 1 d . . . H8A H 0.0976 0.5140 -0.1557 0.039 Uiso 1 1 calc R . . H8B H 0.1027 0.3777 -0.1762 0.039 Uiso 1 1 calc R . . H8C H 0.1862 0.4613 -0.2025 0.039 Uiso 1 1 calc R . . C3 C 0.22403(16) 0.75191(17) 0.29086(13) 0.0359(5) Uani 1 1 d . . . H3C H 0.2749 0.8034 0.2746 0.054 Uiso 1 1 calc R . . H3D H 0.2331 0.7352 0.3599 0.054 Uiso 1 1 calc R . . H3E H 0.1622 0.7897 0.2742 0.054 Uiso 1 1 calc R . . O4 O 0.09020(10) 0.19417(12) 0.08719(9) 0.0362(4) Uani 1 1 d . . . H4WA H 0.1135 0.1300 0.0924 0.054 Uiso 1 1 d R . . H4WB H 0.0542 0.2042 0.0405 0.054 Uiso 1 1 d R . . C9 C 0.22894(14) 0.21678(17) -0.09470(12) 0.0261(5) Uani 1 1 d . . . H9A H 0.2635 0.1501 -0.0645 0.039 Uiso 1 1 calc R . . H9B H 0.2563 0.2380 -0.1534 0.039 Uiso 1 1 calc R . . H9C H 0.1617 0.1964 -0.1109 0.039 Uiso 1 1 calc R . . C11 C 0.42400(13) 0.19478(16) 0.08842(13) 0.0221(4) Uani 1 1 d . . . H11A H 0.4305 0.1988 0.0190 0.027 Uiso 1 1 calc R . . H11B H 0.4622 0.2583 0.1211 0.027 Uiso 1 1 calc R . . C4 C 0.36210(14) 0.69513(16) 0.14916(13) 0.0279(5) Uani 1 1 d . . . H4A H 0.4171 0.6932 0.1997 0.033 Uiso 1 1 calc R . . H4B H 0.3392 0.7761 0.1413 0.033 Uiso 1 1 calc R . . C10 C 0.31929(12) 0.20909(15) 0.10406(12) 0.0188(4) Uani 1 1 d . . . H10A H 0.2824 0.1420 0.0757 0.023 Uiso 1 1 calc R . . H10B H 0.3138 0.2102 0.1738 0.023 Uiso 1 1 calc R . . C20 C 0.08729(14) 0.55097(18) 0.31720(13) 0.0329(5) Uani 1 1 d . . . H20A H 0.0486 0.4803 0.3122 0.049 Uiso 1 1 calc R . . H20B H 0.0463 0.6184 0.3013 0.049 Uiso 1 1 calc R . . H20C H 0.1188 0.5588 0.3829 0.049 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 0.02090(14) 0.01580(13) 0.01309(12) 0.00013(10) 0.00336(10) -0.00009(11) Cl1 0.0248(3) 0.0233(2) 0.0159(2) 0.00059(18) 0.00016(18) -0.0013(2) Cl3 0.0343(3) 0.0233(3) 0.0285(3) 0.0001(2) 0.0055(2) 0.0003(2) Cl4 0.0239(3) 0.0577(4) 0.0197(2) -0.0083(2) 0.0062(2) -0.0069(3) Cl2 0.0301(3) 0.0332(3) 0.0378(3) 0.0027(2) 0.0069(2) 0.0052(2) N1 0.0219(9) 0.0228(9) 0.0154(7) 0.0027(6) 0.0018(6) 0.0004(7) N5 0.0153(8) 0.0162(8) 0.0165(7) 0.0009(6) 0.0027(6) -0.0008(6) O1 0.0301(8) 0.0332(9) 0.0246(7) -0.0021(6) 0.0095(6) -0.0098(7) O2 0.0436(9) 0.0224(8) 0.0236(7) 0.0053(6) 0.0074(6) 0.0123(7) N3 0.0237(9) 0.0227(9) 0.0162(7) 0.0003(7) 0.0037(6) -0.0015(7) N2 0.0299(9) 0.0159(8) 0.0175(8) 0.0003(6) 0.0012(7) 0.0012(7) N4 0.0228(9) 0.0175(8) 0.0184(8) 0.0043(6) 0.0044(6) 0.0027(7) C7 0.0185(10) 0.0220(10) 0.0169(9) -0.0001(8) 0.0063(8) -0.0021(8) N6 0.0241(9) 0.0248(9) 0.0200(8) 0.0005(7) 0.0027(7) 0.0042(7) C6 0.0162(10) 0.0233(11) 0.0176(9) 0.0023(8) 0.0045(7) -0.0011(8) C1 0.0245(11) 0.0283(11) 0.0149(9) 0.0005(8) 0.0000(8) 0.0086(9) C5 0.0348(13) 0.0205(11) 0.0275(10) 0.0049(8) 0.0076(9) -0.0061(9) C2 0.0322(12) 0.0218(11) 0.0169(9) 0.0002(8) -0.0015(8) 0.0085(9) O3 0.0491(10) 0.0343(9) 0.0715(11) -0.0049(8) 0.0227(9) -0.0065(8) C8 0.0290(11) 0.0303(12) 0.0186(9) 0.0026(8) -0.0017(8) -0.0013(9) C3 0.0497(15) 0.0285(12) 0.0284(11) -0.0078(9) -0.0003(10) 0.0131(11) O4 0.0354(9) 0.0336(9) 0.0389(8) -0.0031(7) 0.0009(7) -0.0041(7) C9 0.0301(12) 0.0267(11) 0.0210(10) -0.0049(8) 0.0009(8) 0.0003(9) C11 0.0238(11) 0.0197(10) 0.0233(10) 0.0028(8) 0.0045(8) 0.0020(9) C4 0.0379(13) 0.0181(10) 0.0273(10) -0.0007(8) 0.0024(9) -0.0065(9) C10 0.0216(10) 0.0159(10) 0.0192(9) 0.0016(7) 0.0036(8) 0.0008(8) C20 0.0318(12) 0.0458(14) 0.0220(10) -0.0037(9) 0.0073(9) 0.0107(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.8825(16) . ? Co1 N4 1.9146(15) . ? Co1 N1 1.9416(15) . ? Co1 N3 1.9443(15) . ? Co1 N5 1.9466(15) . ? Co1 Cl1 2.2415(7) . ? N1 C1 1.295(2) . ? N1 O1 1.3737(19) . ? N5 C7 1.290(2) . ? N5 C10 1.479(2) . ? O1 H1OX 0.8400 . ? O2 N4 1.3813(18) . ? O2 H2OX 0.8399 . ? N3 C5 1.495(2) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N2 C2 1.286(2) . ? N2 C4 1.473(2) . ? N4 C6 1.284(2) . ? C7 C9 1.489(2) . ? C7 C6 1.489(2) . ? N6 C11 1.494(2) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N6 H6C 0.9100 . ? C6 C8 1.492(2) . ? C1 C2 1.487(3) . ? C1 C20 1.490(2) . ? C5 C4 1.514(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C2 C3 1.493(2) . ? O3 H3WA 0.7833 . ? O3 H3WB 0.8752 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? O4 H4WA 0.8101 . ? O4 H4WB 0.7900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C10 1.530(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N4 95.97(6) . . ? N2 Co1 N1 81.11(7) . . ? N4 Co1 N1 91.94(7) . . ? N2 Co1 N3 84.96(7) . . ? N4 Co1 N3 89.25(7) . . ? N1 Co1 N3 166.07(6) . . ? N2 Co1 N5 176.44(6) . . ? N4 Co1 N5 81.02(6) . . ? N1 Co1 N5 100.82(6) . . ? N3 Co1 N5 93.07(6) . . ? N2 Co1 Cl1 88.99(5) . . ? N4 Co1 Cl1 174.66(5) . . ? N1 Co1 Cl1 90.77(5) . . ? N3 Co1 Cl1 89.22(5) . . ? N5 Co1 Cl1 93.95(5) . . ? C1 N1 O1 114.86(15) . . ? C1 N1 Co1 115.51(13) . . ? O1 N1 Co1 129.44(11) . . ? C7 N5 C10 120.09(15) . . ? C7 N5 Co1 114.54(12) . . ? C10 N5 Co1 125.36(11) . . ? N1 O1 H1OX 109.5 . . ? N4 O2 H2OX 109.4 . . ? C5 N3 Co1 108.47(11) . . ? C5 N3 H3A 110.0 . . ? Co1 N3 H3A 110.0 . . ? C5 N3 H3B 110.0 . . ? Co1 N3 H3B 110.0 . . ? H3A N3 H3B 108.4 . . ? C2 N2 C4 126.26(16) . . ? C2 N2 Co1 117.40(13) . . ? C4 N2 Co1 116.02(12) . . ? C6 N4 O2 115.71(14) . . ? C6 N4 Co1 116.93(13) . . ? O2 N4 Co1 126.22(11) . . ? N5 C7 C9 126.92(16) . . ? N5 C7 C6 114.29(15) . . ? C9 C7 C6 118.79(15) . . ? C11 N6 H6A 109.5 . . ? C11 N6 H6B 109.5 . . ? H6A N6 H6B 109.5 . . ? C11 N6 H6C 109.5 . . ? H6A N6 H6C 109.5 . . ? H6B N6 H6C 109.5 . . ? N4 C6 C7 112.36(15) . . ? N4 C6 C8 124.52(17) . . ? C7 C6 C8 123.11(16) . . ? N1 C1 C2 112.33(16) . . ? N1 C1 C20 125.35(18) . . ? C2 C1 C20 122.32(17) . . ? N3 C5 C4 108.15(14) . . ? N3 C5 H5A 110.1 . . ? C4 C5 H5A 110.1 . . ? N3 C5 H5B 110.1 . . ? C4 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N2 C2 C1 113.28(16) . . ? N2 C2 C3 125.04(18) . . ? C1 C2 C3 121.68(17) . . ? H3WA O3 H3WB 104.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C3 H3C 109.5 . . ? C2 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C2 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? H4WA O4 H4WB 115.1 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C11 C10 109.53(14) . . ? N6 C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? N6 C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? N2 C4 C5 106.01(15) . . ? N2 C4 H4A 110.5 . . ? C5 C4 H4A 110.5 . . ? N2 C4 H4B 110.5 . . ? C5 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? N5 C10 C11 111.46(14) . . ? N5 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N5 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C1 C20 H20A 109.5 . . ? C1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.426 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.049 #====END data_carloznm _database_code_CSD 188186 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 Cl5 Co N6 O3 Zn' _chemical_formula_sum 'C12 H28 Cl5 Co N6 O3 Zn' _chemical_formula_weight 605.95 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.229(2) _cell_length_b 20.348(6) _cell_length_c 14.258(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.293(4) _cell_angle_gamma 90.00 _cell_volume 2356.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 2.314 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30869 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.46 _reflns_number_total 4801 _reflns_number_gt 3496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0981P)^2^+5.5426P] 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 4801 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1963 _refine_ls_wR_factor_gt 0.1714 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.49741(8) 0.11164(3) 0.71417(5) 0.0345(2) Uani 1 1 d . . . N1 N 0.6561(5) 0.0575(2) 0.6650(3) 0.0378(9) Uani 1 1 d . . . N2 N 0.5887(5) 0.0683(2) 0.8269(3) 0.0370(9) Uani 1 1 d . . . N3 N 0.3627(6) 0.1586(2) 0.7943(3) 0.0415(10) Uani 1 1 d . . . H3A H 0.3514 0.2019 0.7761 0.050 Uiso 1 1 calc R . . H3B H 0.2595 0.1401 0.7880 0.050 Uiso 1 1 calc R . . N4 N 0.6356(5) 0.1890(2) 0.7183(3) 0.0382(9) Uani 1 1 d . . . N5 N 0.4043(5) 0.1516(2) 0.5985(3) 0.0376(9) Uani 1 1 d . . . N6 N 0.3271(6) 0.0443(2) 0.6818(3) 0.0443(10) Uani 1 1 d . . . H6A H 0.3733 0.0064 0.6625 0.053 Uiso 1 1 calc R . . H6B H 0.2794 0.0346 0.7342 0.053 Uiso 1 1 calc R . . O1 O 0.6815(6) 0.0538(2) 0.5719(3) 0.0524(10) Uani 1 1 d . . . H1OX H 0.7056 0.0912 0.5533 0.079 Uiso 1 1 calc R . . O2 O 0.7572(5) 0.2066(2) 0.7917(3) 0.0497(10) Uani 1 1 d . . . H2OX H 0.8265 0.1761 0.8022 0.075 Uiso 1 1 calc R . . O3 O 0.8070(7) 0.1687(3) 0.5340(4) 0.0752(15) Uani 1 1 d . . . H3WA H 0.9051 0.1920 0.5713 0.113 Uiso 1 1 d R . . H3WB H 0.8381 0.1740 0.4812 0.113 Uiso 1 1 d R . . C1 C 0.7402(6) 0.0169(3) 0.7245(4) 0.0388(11) Uani 1 1 d . . . C2 C 0.6971(6) 0.0227(3) 0.8226(4) 0.0399(11) Uani 1 1 d . . . C3 C 0.8617(7) -0.0302(3) 0.7005(4) 0.0484(13) Uani 1 1 d . . . H3C H 0.8837 -0.0213 0.6362 0.073 Uiso 1 1 calc R . . H3D H 0.8186 -0.0750 0.7033 0.073 Uiso 1 1 calc R . . H3E H 0.9640 -0.0260 0.7459 0.073 Uiso 1 1 calc R . . C4 C 0.7697(9) -0.0201(3) 0.9012(4) 0.0578(16) Uani 1 1 d . . . H4A H 0.7668 0.0022 0.9618 0.087 Uiso 1 1 calc R . . H4B H 0.8841 -0.0300 0.8951 0.087 Uiso 1 1 calc R . . H4C H 0.7067 -0.0611 0.8990 0.087 Uiso 1 1 calc R . . C5 C 0.5139(8) 0.0853(3) 0.9120(4) 0.0470(13) Uani 1 1 d . . . H5A H 0.5979 0.0837 0.9701 0.056 Uiso 1 1 calc R . . H5B H 0.4245 0.0541 0.9194 0.056 Uiso 1 1 calc R . . C6 C 0.4468(8) 0.1538(3) 0.8955(4) 0.0479(13) Uani 1 1 d . . . H6C H 0.3674 0.1632 0.9391 0.058 Uiso 1 1 calc R . . H6D H 0.5374 0.1863 0.9077 0.058 Uiso 1 1 calc R . . C7 C 0.5925(7) 0.2324(3) 0.6522(4) 0.0418(12) Uani 1 1 d . . . C8 C 0.4590(7) 0.2079(3) 0.5788(4) 0.0423(12) Uani 1 1 d . . . C9 C 0.6663(8) 0.2986(3) 0.6493(5) 0.0576(16) Uani 1 1 d . . . H9A H 0.7635 0.3020 0.6988 0.086 Uiso 1 1 calc R . . H9B H 0.5855 0.3320 0.6602 0.086 Uiso 1 1 calc R . . H9C H 0.6988 0.3058 0.5869 0.086 Uiso 1 1 calc R . . C10 C 0.4022(10) 0.2469(3) 0.4897(5) 0.0621(17) Uani 1 1 d . . . H10A H 0.3034 0.2264 0.4539 0.093 Uiso 1 1 calc R . . H10B H 0.4896 0.2477 0.4505 0.093 Uiso 1 1 calc R . . H10C H 0.3765 0.2920 0.5068 0.093 Uiso 1 1 calc R . . C11 C 0.2772(7) 0.1122(3) 0.5390(4) 0.0514(14) Uani 1 1 d . . . H11A H 0.3273 0.0851 0.4935 0.062 Uiso 1 1 calc R . . H11B H 0.1932 0.1412 0.5026 0.062 Uiso 1 1 calc R . . C12 C 0.2012(8) 0.0695(4) 0.6045(5) 0.0589(16) Uani 1 1 d . . . H12A H 0.1178 0.0949 0.6321 0.071 Uiso 1 1 calc R . . H12B H 0.1448 0.0321 0.5685 0.071 Uiso 1 1 calc R . . Zn Zn 0.19283(8) 0.35214(3) 0.73806(5) 0.0450(2) Uani 1 1 d . . . Cl1 Cl 0.0219(2) 0.39070(8) 0.83573(13) 0.0592(4) Uani 1 1 d . . . Cl2 Cl 0.42968(17) 0.32019(7) 0.83527(10) 0.0495(4) Uani 1 1 d . . . Cl3 Cl 0.1015(2) 0.26402(8) 0.64574(13) 0.0623(4) Uani 1 1 d . . . Cl4 Cl 0.2508(2) 0.43688(8) 0.64485(11) 0.0598(4) Uani 1 1 d . . . Cl5 Cl 0.01991(19) 0.10788(8) 0.83578(15) 0.0661(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0330(4) 0.0338(4) 0.0355(4) 0.0012(3) 0.0019(3) 0.0001(3) N1 0.043(2) 0.032(2) 0.038(2) -0.0010(17) 0.0041(18) -0.0020(18) N2 0.037(2) 0.032(2) 0.041(2) 0.0019(17) 0.0039(18) -0.0011(17) N3 0.038(2) 0.043(2) 0.042(2) 0.0018(19) 0.0032(19) 0.0065(19) N4 0.033(2) 0.038(2) 0.044(2) -0.0027(18) 0.0066(18) -0.0010(17) N5 0.034(2) 0.038(2) 0.040(2) -0.0013(18) 0.0044(17) 0.0015(17) N6 0.044(2) 0.040(2) 0.047(3) 0.0020(19) 0.001(2) -0.0034(19) O1 0.068(3) 0.054(2) 0.038(2) 0.0000(17) 0.0162(19) 0.003(2) O2 0.043(2) 0.047(2) 0.054(2) -0.0094(18) -0.0057(18) -0.0018(17) O3 0.083(4) 0.087(4) 0.061(3) -0.011(3) 0.029(3) -0.033(3) C1 0.035(3) 0.037(3) 0.043(3) -0.001(2) 0.000(2) -0.002(2) C2 0.039(3) 0.035(3) 0.044(3) -0.001(2) 0.001(2) 0.001(2) C3 0.047(3) 0.043(3) 0.053(3) -0.005(3) 0.003(3) 0.004(2) C4 0.063(4) 0.060(4) 0.050(3) 0.014(3) 0.007(3) 0.014(3) C5 0.057(3) 0.050(3) 0.034(3) 0.003(2) 0.007(2) 0.005(3) C6 0.048(3) 0.059(4) 0.038(3) -0.007(2) 0.008(2) 0.003(3) C7 0.038(3) 0.043(3) 0.046(3) -0.001(2) 0.014(2) 0.002(2) C8 0.041(3) 0.046(3) 0.039(3) 0.003(2) 0.005(2) 0.006(2) C9 0.058(4) 0.042(3) 0.074(4) 0.005(3) 0.012(3) -0.007(3) C10 0.073(4) 0.060(4) 0.052(4) 0.017(3) 0.008(3) 0.010(3) C11 0.046(3) 0.060(4) 0.043(3) -0.001(3) -0.009(2) -0.006(3) C12 0.057(4) 0.065(4) 0.051(3) 0.000(3) -0.003(3) -0.008(3) Zn 0.0435(4) 0.0409(4) 0.0498(4) -0.0020(3) 0.0052(3) 0.0029(3) Cl1 0.0585(9) 0.0511(9) 0.0726(11) -0.0019(7) 0.0248(8) 0.0100(7) Cl2 0.0438(7) 0.0509(8) 0.0526(8) 0.0005(6) 0.0040(6) 0.0043(6) Cl3 0.0546(9) 0.0544(9) 0.0753(11) -0.0180(8) 0.0021(8) -0.0026(7) Cl4 0.0696(10) 0.0572(9) 0.0483(8) 0.0083(7) -0.0034(7) -0.0095(7) Cl5 0.0398(8) 0.0581(10) 0.0989(14) 0.0011(9) 0.0069(8) -0.0032(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N2 1.881(4) . ? Co N5 1.886(4) . ? Co N1 1.925(4) . ? Co N4 1.937(4) . ? Co N6 1.962(5) . ? Co N3 1.963(5) . ? N1 C1 1.301(7) . ? N1 O1 1.380(6) . ? N2 C2 1.295(7) . ? N2 C5 1.487(7) . ? N3 C6 1.500(7) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N4 C7 1.298(7) . ? N4 O2 1.373(6) . ? N5 C8 1.280(7) . ? N5 C11 1.472(7) . ? N6 C12 1.477(8) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? O1 H1OX 0.8400 . ? O2 H2OX 0.8400 . ? O3 H3WA 1.0101 . ? O3 H3WB 0.8399 . ? C1 C3 1.464(8) . ? C1 C2 1.502(8) . ? C2 C4 1.468(8) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.505(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6C 0.9900 . ? C6 H6D 0.9900 . ? C7 C8 1.477(8) . ? C7 C9 1.482(8) . ? C8 C10 1.507(8) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.486(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? Zn Cl1 2.2729(17) . ? Zn Cl4 2.2743(18) . ? Zn Cl3 2.2787(17) . ? Zn Cl2 2.2955(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co N5 177.51(18) . . ? N2 Co N1 80.91(18) . . ? N5 Co N1 97.58(18) . . ? N2 Co N4 101.78(19) . . ? N5 Co N4 80.22(19) . . ? N1 Co N4 92.67(18) . . ? N2 Co N6 92.55(19) . . ? N5 Co N6 85.49(19) . . ? N1 Co N6 90.9(2) . . ? N4 Co N6 165.61(19) . . ? N2 Co N3 85.19(19) . . ? N5 Co N3 96.38(18) . . ? N1 Co N3 165.97(18) . . ? N4 Co N3 88.34(19) . . ? N6 Co N3 91.6(2) . . ? C1 N1 O1 116.4(4) . . ? C1 N1 Co 116.6(4) . . ? O1 N1 Co 126.8(3) . . ? C2 N2 C5 125.8(5) . . ? C2 N2 Co 118.5(4) . . ? C5 N2 Co 115.3(3) . . ? C6 N3 Co 108.2(3) . . ? C6 N3 H3A 110.1 . . ? Co N3 H3A 110.1 . . ? C6 N3 H3B 110.1 . . ? Co N3 H3B 110.1 . . ? H3A N3 H3B 108.4 . . ? C7 N4 O2 117.1(4) . . ? C7 N4 Co 116.2(4) . . ? O2 N4 Co 125.9(3) . . ? C8 N5 C11 127.0(5) . . ? C8 N5 Co 118.1(4) . . ? C11 N5 Co 114.9(4) . . ? C12 N6 Co 108.7(4) . . ? C12 N6 H6A 109.9 . . ? Co N6 H6A 109.9 . . ? C12 N6 H6B 109.9 . . ? Co N6 H6B 109.9 . . ? H6A N6 H6B 108.3 . . ? N1 O1 H1OX 109.5 . . ? N4 O2 H2OX 109.5 . . ? H3WA O3 H3WB 94.5 . . ? N1 C1 C3 125.1(5) . . ? N1 C1 C2 112.0(5) . . ? C3 C1 C2 122.8(5) . . ? N2 C2 C4 125.9(5) . . ? N2 C2 C1 111.7(4) . . ? C4 C2 C1 122.3(5) . . ? C1 C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 106.2(4) . . ? N2 C5 H5A 110.5 . . ? C6 C5 H5A 110.5 . . ? N2 C5 H5B 110.5 . . ? C6 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? N3 C6 C5 108.1(4) . . ? N3 C6 H6C 110.1 . . ? C5 C6 H6C 110.1 . . ? N3 C6 H6D 110.1 . . ? C5 C6 H6D 110.1 . . ? H6C C6 H6D 108.4 . . ? N4 C7 C8 111.7(5) . . ? N4 C7 C9 125.1(5) . . ? C8 C7 C9 123.2(5) . . ? N5 C8 C7 113.2(5) . . ? N5 C8 C10 125.8(5) . . ? C7 C8 C10 121.0(5) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 106.7(5) . . ? N5 C11 H11A 110.4 . . ? C12 C11 H11A 110.4 . . ? N5 C11 H11B 110.4 . . ? C12 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? N6 C12 C11 110.9(5) . . ? N6 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.0 . . ? Cl1 Zn Cl4 107.78(7) . . ? Cl1 Zn Cl3 116.53(7) . . ? Cl4 Zn Cl3 109.86(7) . . ? Cl1 Zn Cl2 106.08(7) . . ? Cl4 Zn Cl2 109.25(7) . . ? Cl3 Zn Cl2 107.13(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.565 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.134 #====END data_dmeox _database_code_CSD 188187 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H40 Cl5 Co N6 O5 Zn' _chemical_formula_weight 698.09 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.144(3) _cell_length_b 10.782(3) _cell_length_c 14.234(4) _cell_angle_alpha 106.538(4) _cell_angle_beta 93.305(5) _cell_angle_gamma 96.088(4) _cell_volume 1477.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 1.861 _exptl_absorpt_correction_type 'MULTISCAN' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'BLESSING, ACTA. CRYST. 1995, A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19196 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.39 _reflns_number_total 5939 _reflns_number_gt 4449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0459P)^2^+0.1722P] 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 5939 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.005 _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 Zn1 Zn 0.28240(4) 0.30740(3) 0.14946(2) 0.02321(10) Uani 1 1 d . . . Co1 Co 0.74837(4) 0.75786(4) 0.26177(3) 0.01741(11) Uani 1 1 d . . . Cl3 Cl 0.10995(8) 0.23821(7) 0.02890(5) 0.02627(18) Uani 1 1 d . . . Cl1 Cl 0.44040(8) 0.42467(8) 0.08934(6) 0.0345(2) Uani 1 1 d . . . Cl4 Cl 0.37147(9) 0.13488(8) 0.17696(7) 0.0392(2) Uani 1 1 d . . . Cl2 Cl 0.21963(11) 0.43116(9) 0.29267(6) 0.0451(3) Uani 1 1 d . . . N2 N 0.7968(2) 0.6224(2) 0.31226(17) 0.0196(5) Uani 1 1 d . . . N6 N 0.5594(2) 0.7058(2) 0.26717(17) 0.0220(5) Uani 1 1 d . . . H6A H 0.5331 0.6263 0.2211 0.026 Uiso 1 1 calc R . . H6B H 0.5459 0.6964 0.3283 0.026 Uiso 1 1 calc R . . N3 N 0.7512(2) 0.6283(2) 0.13322(16) 0.0194(5) Uani 1 1 d . . . H3A H 0.6652 0.5948 0.1073 0.023 Uiso 1 1 calc R . . H3B H 0.7901 0.6683 0.0908 0.023 Uiso 1 1 calc R . . N1 N 0.7741(2) 0.8525(2) 0.40251(17) 0.0211(5) Uani 1 1 d . . . O2 O 1.0430(2) 0.8562(2) 0.29494(16) 0.0287(5) Uani 1 1 d . . . H2OX H 1.0382 0.8078 0.3319 0.043 Uiso 1 1 calc R . . O1 O 0.7697(3) 0.9822(2) 0.45086(15) 0.0338(6) Uani 1 1 d . . . H1OX H 0.7848 1.0270 0.4121 0.051 Uiso 1 1 calc R . . C10 C 0.7719(3) 0.9506(3) 0.1703(2) 0.0222(7) Uani 1 1 d . . . N5 N 0.6861(2) 0.8768(2) 0.19899(17) 0.0206(5) Uani 1 1 d . . . C1 C 0.8003(3) 0.7830(3) 0.4606(2) 0.0217(7) Uani 1 1 d . . . N4 N 0.9177(2) 0.8571(2) 0.25244(17) 0.0207(5) Uani 1 1 d . . . C14 C 0.4746(3) 0.8067(3) 0.2473(2) 0.0255(7) Uani 1 1 d . . . C2 C 0.8110(3) 0.6454(3) 0.4063(2) 0.0213(6) Uani 1 1 d . . . C8 C 0.9758(3) 0.5604(3) 0.1434(2) 0.0276(7) Uani 1 1 d . . . H8A H 0.9916 0.5921 0.0865 0.041 Uiso 1 1 calc R . . H8B H 1.0253 0.4863 0.1405 0.041 Uiso 1 1 calc R . . H8C H 1.0059 0.6306 0.2041 0.041 Uiso 1 1 calc R . . C6 C 0.8281(3) 0.5175(3) 0.1421(2) 0.0222(7) Uani 1 1 d . . . C13 C 0.5424(3) 0.8575(3) 0.1707(2) 0.0258(7) Uani 1 1 d . . . H13A H 0.5213 0.7938 0.1046 0.031 Uiso 1 1 calc R . . H13B H 0.5115 0.9410 0.1690 0.031 Uiso 1 1 calc R . . C11 C 1.0265(3) 1.0271(3) 0.1871(2) 0.0312(8) Uani 1 1 d . . . H11A H 1.1092 1.0014 0.2104 0.047 Uiso 1 1 calc R . . H11B H 1.0207 1.1184 0.2227 0.047 Uiso 1 1 calc R . . H11C H 1.0258 1.0173 0.1165 0.047 Uiso 1 1 calc R . . C9 C 0.9112(3) 0.9430(3) 0.2049(2) 0.0238(7) Uani 1 1 d . . . C12 C 0.7412(3) 1.0382(3) 0.1091(2) 0.0323(8) Uani 1 1 d . . . H12A H 0.7331 0.9885 0.0393 0.049 Uiso 1 1 calc R . . H12B H 0.8131 1.1108 0.1220 0.049 Uiso 1 1 calc R . . H12C H 0.6572 1.0725 0.1261 0.049 Uiso 1 1 calc R . . C7 C 0.7831(3) 0.3952(3) 0.0551(2) 0.0283(7) Uani 1 1 d . . . H7A H 0.7995 0.4147 -0.0067 0.043 Uiso 1 1 calc R . . H7B H 0.6878 0.3681 0.0553 0.043 Uiso 1 1 calc R . . H7C H 0.8333 0.3246 0.0612 0.043 Uiso 1 1 calc R . . C3 C 0.8225(4) 0.8345(3) 0.5701(2) 0.0318(8) Uani 1 1 d . . . H3C H 0.7950 0.9219 0.5917 0.048 Uiso 1 1 calc R . . H3D H 0.9171 0.8391 0.5909 0.048 Uiso 1 1 calc R . . H3E H 0.7698 0.7763 0.5997 0.048 Uiso 1 1 calc R . . C5 C 0.7947(3) 0.4931(3) 0.2394(2) 0.0246(7) Uani 1 1 d . . . H5A H 0.7057 0.4420 0.2314 0.030 Uiso 1 1 calc R . . H5B H 0.8613 0.4439 0.2613 0.030 Uiso 1 1 calc R . . C16 C 0.4710(4) 0.9160(3) 0.3427(2) 0.0382(9) Uani 1 1 d . . . H16A H 0.5597 0.9662 0.3621 0.057 Uiso 1 1 calc R . . H16B H 0.4443 0.8783 0.3947 0.057 Uiso 1 1 calc R . . H16C H 0.4069 0.9737 0.3322 0.057 Uiso 1 1 calc R . . C15 C 0.3345(3) 0.7403(3) 0.2081(3) 0.0376(8) Uani 1 1 d . . . H15A H 0.2814 0.8033 0.1916 0.056 Uiso 1 1 calc R . . H15B H 0.2933 0.7074 0.2584 0.056 Uiso 1 1 calc R . . H15C H 0.3383 0.6674 0.1490 0.056 Uiso 1 1 calc R . . C4 C 0.8382(4) 0.5499(3) 0.4609(2) 0.0334(8) Uani 1 1 d . . . H4A H 0.7626 0.5365 0.4984 0.050 Uiso 1 1 calc R . . H4B H 0.9188 0.5840 0.5062 0.050 Uiso 1 1 calc R . . H4C H 0.8509 0.4667 0.4140 0.050 Uiso 1 1 calc R . . Cl5 Cl 0.18476(9) 0.80146(7) 0.63352(6) 0.0347(2) Uani 1 1 d . . . O3 O 0.1003(2) 0.7011(2) 0.40085(16) 0.0363(6) Uani 1 1 d . . . H3WA H 0.1372 0.7274 0.4612 0.054 Uiso 1 1 d R . . H3WB H 0.1425 0.6366 0.3810 0.054 Uiso 1 1 d R . . O4 O 0.4740(3) 0.3794(2) 0.56341(18) 0.0526(7) Uani 1 1 d . . . H4WA H 0.4869 0.3516 0.5025 0.079 Uiso 1 1 d R . . H4WB H 0.4800 0.4700 0.5834 0.079 Uiso 1 1 d R . . O5 O 0.5460(3) 0.3254(3) 0.37240(19) 0.0573(8) Uani 1 1 d . . . H5WA H 0.6249 0.2847 0.3646 0.086 Uiso 1 1 d R . . H5WB H 0.4935 0.2772 0.3231 0.086 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 Zn1 0.0254(2) 0.0229(2) 0.02280(19) 0.00815(15) 0.00404(15) 0.00439(15) Co1 0.0206(2) 0.0157(2) 0.0169(2) 0.00547(16) 0.00368(16) 0.00345(16) Cl3 0.0265(4) 0.0287(4) 0.0246(4) 0.0096(3) 0.0031(3) 0.0025(3) Cl1 0.0299(5) 0.0375(5) 0.0338(4) 0.0099(4) 0.0063(4) -0.0062(4) Cl4 0.0395(5) 0.0299(5) 0.0511(5) 0.0145(4) -0.0024(4) 0.0130(4) Cl2 0.0772(7) 0.0399(5) 0.0238(4) 0.0100(4) 0.0156(4) 0.0255(5) N2 0.0230(14) 0.0162(12) 0.0195(13) 0.0053(10) 0.0009(10) 0.0028(10) N6 0.0248(14) 0.0204(13) 0.0211(13) 0.0060(10) 0.0051(11) 0.0021(11) N3 0.0192(13) 0.0192(13) 0.0210(12) 0.0071(10) 0.0034(10) 0.0030(10) N1 0.0256(15) 0.0163(12) 0.0202(12) 0.0032(10) 0.0032(11) 0.0032(11) O2 0.0227(12) 0.0297(13) 0.0358(13) 0.0150(10) -0.0022(10) 0.0003(10) O1 0.0612(17) 0.0146(11) 0.0247(12) 0.0027(9) 0.0052(11) 0.0079(11) C10 0.0339(19) 0.0163(15) 0.0175(14) 0.0054(12) 0.0042(13) 0.0052(13) N5 0.0248(14) 0.0188(13) 0.0182(12) 0.0043(10) 0.0025(10) 0.0055(11) C1 0.0222(17) 0.0212(16) 0.0219(15) 0.0067(13) 0.0036(13) 0.0029(13) N4 0.0223(14) 0.0185(13) 0.0207(12) 0.0045(10) 0.0025(11) 0.0033(10) C14 0.0212(17) 0.0279(17) 0.0291(17) 0.0088(14) 0.0034(13) 0.0095(14) C2 0.0248(17) 0.0207(15) 0.0202(15) 0.0085(12) 0.0017(12) 0.0035(13) C8 0.0277(18) 0.0273(17) 0.0259(16) 0.0028(14) 0.0020(14) 0.0099(14) C6 0.0252(17) 0.0192(15) 0.0229(15) 0.0053(13) 0.0038(13) 0.0085(13) C13 0.0232(18) 0.0271(17) 0.0294(17) 0.0101(14) 0.0015(14) 0.0086(14) C11 0.039(2) 0.0270(18) 0.0290(17) 0.0129(15) 0.0056(15) -0.0060(15) C9 0.0331(19) 0.0194(16) 0.0180(15) 0.0036(12) 0.0065(13) 0.0021(13) C12 0.043(2) 0.0256(18) 0.0358(19) 0.0190(15) 0.0048(16) 0.0066(15) C7 0.0324(19) 0.0264(17) 0.0234(16) 0.0013(14) 0.0037(14) 0.0072(14) C3 0.050(2) 0.0268(18) 0.0189(16) 0.0072(13) 0.0039(15) 0.0056(16) C5 0.0374(19) 0.0158(15) 0.0219(15) 0.0058(12) 0.0050(14) 0.0074(13) C16 0.038(2) 0.039(2) 0.038(2) 0.0067(17) 0.0103(17) 0.0161(17) C15 0.0244(19) 0.044(2) 0.045(2) 0.0134(17) 0.0059(16) 0.0073(16) C4 0.052(2) 0.0265(18) 0.0256(17) 0.0112(14) 0.0053(16) 0.0129(16) Cl5 0.0498(6) 0.0206(4) 0.0332(4) 0.0066(3) 0.0051(4) 0.0052(4) O3 0.0411(15) 0.0377(14) 0.0307(12) 0.0090(11) -0.0011(11) 0.0138(11) O4 0.079(2) 0.0423(16) 0.0375(14) 0.0163(12) 0.0184(14) -0.0069(14) O5 0.0443(17) 0.074(2) 0.0428(16) -0.0012(14) -0.0001(13) 0.0135(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl2 2.2632(10) . ? Zn1 Cl4 2.2715(10) . ? Zn1 Cl3 2.2825(10) . ? Zn1 Cl1 2.2899(10) . ? Co1 N2 1.897(2) . ? Co1 N5 1.898(2) . ? Co1 N6 1.952(3) . ? Co1 N4 1.957(2) . ? Co1 N1 1.960(2) . ? Co1 N3 1.964(2) . ? N2 C2 1.286(4) . ? N2 C5 1.479(4) . ? N6 C14 1.532(4) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? N3 C6 1.525(4) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N1 C1 1.298(4) . ? N1 O1 1.378(3) . ? O2 N4 1.378(3) . ? O2 H2OX 0.8400 . ? O1 H1OX 0.8400 . ? C10 N5 1.280(4) . ? C10 C9 1.488(4) . ? C10 C12 1.498(4) . ? N5 C13 1.466(4) . ? C1 C2 1.483(4) . ? C1 C3 1.493(4) . ? N4 C9 1.298(4) . ? C14 C13 1.520(4) . ? C14 C15 1.520(4) . ? C14 C16 1.529(4) . ? C2 C4 1.494(4) . ? C8 C6 1.518(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C6 C5 1.531(4) . ? C6 C7 1.536(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C11 C9 1.481(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O3 H3WA 0.8718 . ? O3 H3WB 0.8445 . ? O4 H4WA 0.8554 . ? O4 H4WB 0.9306 . ? O5 H5WA 0.9491 . ? O5 H5WB 0.8585 . ? 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 Cl4 109.00(4) . . ? Cl2 Zn1 Cl3 112.24(4) . . ? Cl4 Zn1 Cl3 110.73(4) . . ? Cl2 Zn1 Cl1 110.89(4) . . ? Cl4 Zn1 Cl1 108.25(4) . . ? Cl3 Zn1 Cl1 105.64(4) . . ? N2 Co1 N5 172.83(10) . . ? N2 Co1 N6 91.69(10) . . ? N5 Co1 N6 84.13(10) . . ? N2 Co1 N4 104.76(10) . . ? N5 Co1 N4 79.96(10) . . ? N6 Co1 N4 162.91(10) . . ? N2 Co1 N1 80.37(10) . . ? N5 Co1 N1 105.58(10) . . ? N6 Co1 N1 92.68(10) . . ? N4 Co1 N1 85.65(10) . . ? N2 Co1 N3 83.97(10) . . ? N5 Co1 N3 90.37(10) . . ? N6 Co1 N3 92.35(10) . . ? N4 Co1 N3 93.96(10) . . ? N1 Co1 N3 163.68(10) . . ? C2 N2 C5 125.3(2) . . ? C2 N2 Co1 117.9(2) . . ? C5 N2 Co1 116.09(18) . . ? C14 N6 Co1 111.36(18) . . ? C14 N6 H6A 109.4 . . ? Co1 N6 H6A 109.4 . . ? C14 N6 H6B 109.4 . . ? Co1 N6 H6B 109.4 . . ? H6A N6 H6B 108.0 . . ? C6 N3 Co1 111.31(17) . . ? C6 N3 H3A 109.4 . . ? Co1 N3 H3A 109.4 . . ? C6 N3 H3B 109.4 . . ? Co1 N3 H3B 109.4 . . ? H3A N3 H3B 108.0 . . ? C1 N1 O1 113.9(2) . . ? C1 N1 Co1 115.54(19) . . ? O1 N1 Co1 130.57(18) . . ? N4 O2 H2OX 109.5 . . ? N1 O1 H1OX 109.5 . . ? N5 C10 C9 112.9(3) . . ? N5 C10 C12 125.6(3) . . ? C9 C10 C12 121.5(3) . . ? C10 N5 C13 125.0(3) . . ? C10 N5 Co1 118.3(2) . . ? C13 N5 Co1 115.60(19) . . ? N1 C1 C2 112.7(2) . . ? N1 C1 C3 124.6(3) . . ? C2 C1 C3 122.7(3) . . ? C9 N4 O2 114.3(2) . . ? C9 N4 Co1 116.0(2) . . ? O2 N4 Co1 129.51(18) . . ? C13 C14 C15 111.0(3) . . ? C13 C14 C16 111.3(3) . . ? C15 C14 C16 110.2(3) . . ? C13 C14 N6 105.5(2) . . ? C15 C14 N6 109.2(3) . . ? C16 C14 N6 109.5(2) . . ? N2 C2 C1 113.2(3) . . ? N2 C2 C4 126.5(3) . . ? C1 C2 C4 120.3(2) . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C8 C6 N3 108.8(2) . . ? C8 C6 C5 111.3(3) . . ? N3 C6 C5 105.5(2) . . ? C8 C6 C7 110.3(2) . . ? N3 C6 C7 110.0(2) . . ? C5 C6 C7 110.8(2) . . ? N5 C13 C14 107.1(2) . . ? N5 C13 H13A 110.3 . . ? C14 C13 H13A 110.3 . . ? N5 C13 H13B 110.3 . . ? C14 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C9 C11 125.4(3) . . ? N4 C9 C10 112.2(3) . . ? C11 C9 C10 122.4(3) . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? N2 C5 C6 107.0(2) . . ? N2 C5 H5A 110.3 . . ? C6 C5 H5A 110.3 . . ? N2 C5 H5B 110.3 . . ? C6 C5 H5B 110.3 . . ? H5A C5 H5B 108.6 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? H3WA O3 H3WB 96.8 . . ? H4WA O4 H4WB 110.4 . . ? H5WA O5 H5WB 102.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.428 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.082 #====END data_monoxu _database_code_CSD 188188 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H21 Cl5 Co N5 O Zn' _chemical_formula_sum 'C8 H21 Cl5 Co N5 O Zn' _chemical_formula_weight 504.85 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 Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 16.375(3) _cell_length_b 8.3790(17) _cell_length_c 13.418(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1841.0(7) _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 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 2.932 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'blessing, Acta. Cryst., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12820 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.33 _reflns_number_total 3718 _reflns_number_gt 3681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0221P)^2^+0.8127P] 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 0.00 _refine_ls_number_reflns 3718 _refine_ls_number_parameters 193 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0176 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0441 _refine_ls_wR_factor_gt 0.0440 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.021 _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 Zn Zn 0.751178(17) 0.08902(3) 0.09616(2) 0.02050(6) Uani 1 1 d . . . Cl2 Cl 0.71084(3) -0.15740(6) 0.14882(4) 0.02506(11) Uani 1 1 d . . . Cl3 Cl 0.65346(4) 0.27696(7) 0.11507(4) 0.03137(14) Uani 1 1 d . . . Cl4 Cl 0.86066(3) 0.16966(7) 0.18742(4) 0.02626(12) Uani 1 1 d . . . Cl5 Cl 0.78713(4) 0.06927(7) -0.06544(4) 0.02834(12) Uani 1 1 d . . . Co Co 0.386962(15) 0.40652(3) 0.364959(19) 0.01456(6) Uani 1 1 d . . . N3 N 0.39876(13) 0.3936(2) 0.51021(15) 0.0214(4) Uani 1 1 d . . . H3A H 0.4006 0.4924 0.5365 0.026 Uiso 1 1 calc R . . H3B H 0.3558 0.3417 0.5367 0.026 Uiso 1 1 calc R . . N2 N 0.45570(10) 0.22732(19) 0.36288(13) 0.0190(3) Uani 1 1 d . . . N1 N 0.39613(11) 0.3777(2) 0.22393(14) 0.0170(4) Uani 1 1 d . . . N5 N 0.30938(10) 0.5847(2) 0.36947(15) 0.0192(3) Uani 1 1 d . . . H5A H 0.3106 0.6303 0.4302 0.023 Uiso 1 1 calc R . . H5B H 0.3237 0.6589 0.3242 0.023 Uiso 1 1 calc R . . N4 N 0.28957(10) 0.2708(2) 0.36770(14) 0.0197(3) Uani 1 1 d . . . H4A H 0.2809 0.2291 0.3068 0.024 Uiso 1 1 calc R . . H4B H 0.2971 0.1899 0.4108 0.024 Uiso 1 1 calc R . . O1 O 0.35940(10) 0.46571(18) 0.14952(12) 0.0233(3) Uani 1 1 d . . . H1OX H 0.3555 0.5590 0.1673 0.035 Uiso 1 1 calc R . . Cl1 Cl 0.49160(3) 0.57848(6) 0.35809(4) 0.02396(11) Uani 1 1 d . . . C4 C 0.47550(15) 0.3066(3) 0.53298(17) 0.0274(5) Uani 1 1 d . . . H4C H 0.4746 0.2682 0.6012 0.033 Uiso 1 1 calc R . . H4D H 0.5221 0.3770 0.5251 0.033 Uiso 1 1 calc R . . C3 C 0.48190(15) 0.1667(3) 0.46097(18) 0.0256(5) Uani 1 1 d . . . H3C H 0.5377 0.1281 0.4578 0.031 Uiso 1 1 calc R . . H3D H 0.4469 0.0798 0.4823 0.031 Uiso 1 1 calc R . . C1 C 0.43657(13) 0.2542(2) 0.19358(16) 0.0191(4) Uani 1 1 d . . . C8 C 0.22540(12) 0.5266(3) 0.34790(18) 0.0255(5) Uani 1 1 d . . . H8A H 0.2173 0.5154 0.2766 0.031 Uiso 1 1 calc R . . H8B H 0.1851 0.6009 0.3736 0.031 Uiso 1 1 calc R . . C7 C 0.21728(14) 0.3670(3) 0.39872(18) 0.0257(5) Uani 1 1 d . . . H7A H 0.2165 0.3803 0.4705 0.031 Uiso 1 1 calc R . . H7B H 0.1671 0.3147 0.3784 0.031 Uiso 1 1 calc R . . C2 C 0.47428(13) 0.1663(3) 0.27876(16) 0.0195(4) Uani 1 1 d . . . C6 C 0.52939(15) 0.0256(3) 0.26610(19) 0.0263(5) Uani 1 1 d . . . H6A H 0.5822 0.0500 0.2931 0.039 Uiso 1 1 calc R . . H6B H 0.5346 0.0010 0.1965 0.039 Uiso 1 1 calc R . . H6C H 0.5068 -0.0646 0.3005 0.039 Uiso 1 1 calc R . . C5 C 0.44412(14) 0.2060(3) 0.08736(17) 0.0251(5) Uani 1 1 d . . . H5C H 0.4010 0.1331 0.0708 0.038 Uiso 1 1 calc R . . H5D H 0.4959 0.1551 0.0770 0.038 Uiso 1 1 calc R . . H5E H 0.4403 0.2988 0.0457 0.038 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 Zn 0.02278(12) 0.01461(11) 0.02410(13) -0.00122(10) -0.00320(11) -0.00026(10) Cl2 0.0303(3) 0.0167(2) 0.0281(3) 0.0015(2) -0.0034(2) -0.0030(2) Cl3 0.0318(3) 0.0264(3) 0.0359(3) 0.0056(2) 0.0004(2) 0.0109(2) Cl4 0.0229(3) 0.0226(3) 0.0333(3) -0.0105(2) -0.0040(2) 0.0003(2) Cl5 0.0393(3) 0.0217(3) 0.0240(3) -0.0016(2) 0.0018(2) -0.0022(2) Co 0.01651(12) 0.01182(12) 0.01534(14) 0.00123(11) -0.00025(11) 0.00006(9) N3 0.0278(11) 0.0177(9) 0.0188(9) 0.0015(7) -0.0005(7) 0.0006(8) N2 0.0196(8) 0.0146(8) 0.0227(9) 0.0040(8) -0.0013(8) 0.0002(6) N1 0.0175(9) 0.0159(8) 0.0176(9) 0.0034(7) -0.0011(6) -0.0020(7) N5 0.0228(8) 0.0161(8) 0.0186(9) -0.0007(7) 0.0019(7) 0.0010(7) N4 0.0207(8) 0.0160(8) 0.0225(9) 0.0030(8) -0.0016(8) -0.0015(7) O1 0.0319(9) 0.0179(8) 0.0201(8) 0.0043(7) -0.0046(7) 0.0022(7) Cl1 0.0226(2) 0.0219(2) 0.0274(3) 0.0018(2) -0.0022(2) -0.00696(18) C4 0.0288(12) 0.0321(12) 0.0214(11) 0.0066(9) -0.0064(9) 0.0030(10) C3 0.0275(12) 0.0239(11) 0.0254(11) 0.0089(9) -0.0025(9) 0.0056(10) C1 0.0177(10) 0.0179(10) 0.0217(10) -0.0018(8) 0.0023(8) -0.0041(8) C8 0.0202(10) 0.0243(11) 0.0320(12) 0.0017(10) -0.0028(10) 0.0041(8) C7 0.0186(11) 0.0273(12) 0.0312(13) 0.0008(9) 0.0039(9) -0.0006(9) C2 0.0162(10) 0.0167(10) 0.0257(11) 0.0006(8) 0.0008(8) -0.0024(8) C6 0.0245(12) 0.0200(11) 0.0343(12) -0.0034(10) 0.0005(9) 0.0054(9) C5 0.0269(11) 0.0249(11) 0.0235(11) -0.0050(9) 0.0025(10) 0.0014(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 Zn Cl5 2.2529(8) . ? Zn Cl3 2.2594(7) . ? Zn Cl4 2.2738(7) . ? Zn Cl2 2.2801(7) . ? Co N2 1.8767(17) . ? Co N1 1.9136(19) . ? Co N4 1.9589(17) . ? Co N5 1.9613(17) . ? Co N3 1.961(2) . ? Co Cl1 2.2407(6) . ? N3 C4 1.485(3) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N2 C2 1.276(3) . ? N2 C3 1.475(3) . ? N1 C1 1.294(3) . ? N1 O1 1.379(2) . ? N5 C8 1.487(3) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N4 C7 1.491(3) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? O1 H1OX 0.8200 . ? C4 C3 1.523(3) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C1 C5 1.487(3) . ? C1 C2 1.493(3) . ? C8 C7 1.507(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C2 C6 1.495(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C5 H5C 0.9600 . ? C5 H5D 0.9600 . ? C5 H5E 0.9600 . ? 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 Cl5 Zn Cl3 110.14(2) . . ? Cl5 Zn Cl4 109.52(3) . . ? Cl3 Zn Cl4 106.91(3) . . ? Cl5 Zn Cl2 107.91(2) . . ? Cl3 Zn Cl2 113.03(3) . . ? Cl4 Zn Cl2 109.31(2) . . ? N2 Co N1 80.63(8) . . ? N2 Co N4 91.38(7) . . ? N1 Co N4 90.52(8) . . ? N2 Co N5 176.35(7) . . ? N1 Co N5 100.22(8) . . ? N4 Co N5 85.07(7) . . ? N2 Co N3 84.93(8) . . ? N1 Co N3 165.44(7) . . ? N4 Co N3 91.69(8) . . ? N5 Co N3 94.30(8) . . ? N2 Co Cl1 93.17(5) . . ? N1 Co Cl1 88.89(6) . . ? N4 Co Cl1 175.25(5) . . ? N5 Co Cl1 90.40(5) . . ? N3 Co Cl1 90.06(6) . . ? C4 N3 Co 108.35(14) . . ? C4 N3 H3A 110.0 . . ? Co N3 H3A 110.0 . . ? C4 N3 H3B 110.0 . . ? Co N3 H3B 110.0 . . ? H3A N3 H3B 108.4 . . ? C2 N2 C3 125.61(17) . . ? C2 N2 Co 118.47(15) . . ? C3 N2 Co 115.91(14) . . ? C1 N1 O1 115.01(18) . . ? C1 N1 Co 116.89(15) . . ? O1 N1 Co 127.88(14) . . ? C8 N5 Co 110.09(13) . . ? C8 N5 H5A 109.6 . . ? Co N5 H5A 109.6 . . ? C8 N5 H5B 109.6 . . ? Co N5 H5B 109.6 . . ? H5A N5 H5B 108.2 . . ? C7 N4 Co 109.73(13) . . ? C7 N4 H4A 109.7 . . ? Co N4 H4A 109.7 . . ? C7 N4 H4B 109.7 . . ? Co N4 H4B 109.7 . . ? H4A N4 H4B 108.2 . . ? N1 O1 H1OX 109.5 . . ? N3 C4 C3 107.81(18) . . ? N3 C4 H4C 110.1 . . ? C3 C4 H4C 110.1 . . ? N3 C4 H4D 110.1 . . ? C3 C4 H4D 110.1 . . ? H4C C4 H4D 108.5 . . ? N2 C3 C4 106.32(18) . . ? N2 C3 H3C 110.5 . . ? C4 C3 H3C 110.5 . . ? N2 C3 H3D 110.5 . . ? C4 C3 H3D 110.5 . . ? H3C C3 H3D 108.7 . . ? N1 C1 C5 124.2(2) . . ? N1 C1 C2 111.41(19) . . ? C5 C1 C2 124.44(19) . . ? N5 C8 C7 106.50(17) . . ? N5 C8 H8A 110.4 . . ? C7 C8 H8A 110.4 . . ? N5 C8 H8B 110.4 . . ? C7 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? N4 C7 C8 106.46(17) . . ? N4 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? N4 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? N2 C2 C1 112.40(18) . . ? N2 C2 C6 124.09(19) . . ? C1 C2 C6 123.49(19) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C5 H5C 109.5 . . ? C1 C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? C1 C5 H5E 109.5 . . ? H5C C5 H5E 109.5 . . ? H5D C5 H5E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.191 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.045