Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Anders Hammershoi' _publ_contact_author_address ; Department of Chemistry University of Copenhagen Universitetesparken 5 DK-2100 Copenhagen O Denmark ; _publ_contact_author_email anders@kiku.dk _publ_section_title ; Facile cobalt(III) template synthesis of novel branched polyamine monocarboxylates ; loop_ _publ_author_name 'Anders Hammershoi' 'Rasmus Barford' 'Jette Eriksen' 'Bernard T. Golding' 'Thomas Amos Jacobsen' ; A.Langkilde ; 'Sine Larsen' 'Ole Monsted' 'A. M. Sargeson' 'Henning Osholm Sorensen' data_3 _database_code_depnum_ccdc_archive 'CCDC 255276' _audit_creation_method SHELXL-97 _chemical_name_common p-(Co(tren)((MeO)2CHCH2gly))(O3SCF3)2 _chemical_formula_moiety 'C12 H30 Co N5 O4 2+, 2(O3 S C F3 1-)' _chemical_formula_sum 'C14 H30 Co F6 N5 O10 S2' _chemical_formula_weight 665.48 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.3490(1) _cell_length_b 12.6570(1) _cell_length_c 21.2560(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2515.23(4) _cell_formula_units_Z 4 _cell_measurement_temperature 122.4(5) _cell_measurement_reflns_used 3190 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 27.48 _exptl_crystal_description octahedra _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 122.4(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method \w _diffrn_reflns_number 23691 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5690 _reflns_number_gt 4997 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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 sigma _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)] _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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.089(14) _refine_ls_number_reflns 5690 _refine_ls_number_parameters 416 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.728 _refine_ls_restrained_S_all 1.726 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.16457(4) 0.48623(3) 0.951463(18) 0.01396(10) Uani 1 1 d . . . N3 N 0.2937(3) 0.5152(2) 0.88149(11) 0.0185(6) Uani 1 1 d . . . N4 N 0.3323(3) 0.5050(2) 1.00624(11) 0.0196(6) Uani 1 1 d D . . HN4A H 0.323(4) 0.5558(18) 1.0364(11) 0.024 Uiso 1 1 d D . . HN4B H 0.346(4) 0.4447(15) 1.0281(13) 0.024 Uiso 1 1 d D . . N5 N 0.0175(3) 0.4578(2) 0.88768(12) 0.0186(6) Uani 1 1 d D . . HN5A H -0.066(2) 0.492(2) 0.8920(13) 0.022 Uiso 1 1 d D . . HN5B H -0.002(3) 0.3877(10) 0.8911(14) 0.022 Uiso 1 1 d D . . N2 N 0.1243(3) 0.6365(2) 0.95211(13) 0.0178(6) Uani 1 1 d D . . HN2A H 0.0368(18) 0.652(3) 0.9353(13) 0.021 Uiso 1 1 d D . . HN2B H 0.117(3) 0.668(2) 0.9904(8) 0.021 Uiso 1 1 d D . . C9 C 0.4375(4) 0.4782(3) 0.90234(16) 0.0242(8) Uani 1 1 d D . . H9A H 0.518(2) 0.499(3) 0.8750(12) 0.029 Uiso 1 1 d D . . H9B H 0.434(4) 0.4007(9) 0.8987(15) 0.029 Uiso 1 1 d D . . C10 C 0.4657(4) 0.5188(3) 0.96800(16) 0.0263(8) Uani 1 1 d D . . H10A H 0.494(3) 0.5941(11) 0.9662(16) 0.032 Uiso 1 1 d D . . H10B H 0.545(3) 0.478(2) 0.9876(13) 0.032 Uiso 1 1 d D . . C11 C 0.2377(4) 0.4547(3) 0.82657(14) 0.0252(8) Uani 1 1 d D . . H11A H 0.260(4) 0.3797(11) 0.8341(15) 0.030 Uiso 1 1 d D . . H11B H 0.295(3) 0.469(3) 0.7885(9) 0.030 Uiso 1 1 d D . . C12 C 0.0792(4) 0.4738(3) 0.82342(15) 0.0247(8) Uani 1 1 d D . . H12A H 0.033(3) 0.424(2) 0.7944(12) 0.030 Uiso 1 1 d D . . H12B H 0.057(4) 0.5480(11) 0.8140(15) 0.030 Uiso 1 1 d D . . C8 C 0.2975(4) 0.6329(3) 0.86651(16) 0.0219(8) Uani 1 1 d D . . H8A H 0.221(3) 0.638(2) 0.8350(12) 0.026 Uiso 1 1 d D . . H8B H 0.3966(16) 0.657(2) 0.8582(15) 0.026 Uiso 1 1 d D . . C7 C 0.2446(4) 0.6963(3) 0.92138(17) 0.0285(8) Uani 1 1 d D . . H7A H 0.214(4) 0.7665(14) 0.9058(15) 0.034 Uiso 1 1 d D . . H7B H 0.315(3) 0.701(3) 0.9569(11) 0.034 Uiso 1 1 d D . . O1 O 0.2142(2) 0.34074(15) 0.94969(10) 0.0176(5) Uani 1 1 d . . . O2 O 0.1513(2) 0.18181(16) 0.98660(10) 0.0229(5) Uani 1 1 d . . . C1 C 0.1330(3) 0.2774(2) 0.98291(14) 0.0176(7) Uani 1 1 d . . . C2 C 0.0088(4) 0.3302(3) 1.01587(16) 0.0203(7) Uani 1 1 d D . . H2A H -0.002(3) 0.294(2) 1.0568(8) 0.024 Uiso 1 1 d D . . H2B H -0.081(2) 0.323(3) 0.9919(13) 0.024 Uiso 1 1 d D . . N1 N 0.0381(3) 0.4461(2) 1.02210(12) 0.0195(6) Uani 1 1 d D . . HN1 H 0.063(3) 0.468(2) 1.0622(7) 0.023 Uiso 1 1 d D . . C3 C -0.0947(4) 0.5074(3) 1.03351(16) 0.0284(8) Uani 1 1 d D . . H3A H -0.159(3) 0.495(3) 0.9966(10) 0.034 Uiso 1 1 d D . . H3B H -0.060(4) 0.5820(12) 1.0353(16) 0.034 Uiso 1 1 d D . . C4 C -0.1630(4) 0.4810(3) 1.09668(15) 0.0278(8) Uani 1 1 d . . . H4 H -0.206(4) 0.399(3) 1.0989(15) 0.033 Uiso 1 1 d . . . O3 O -0.2761(3) 0.54929(18) 1.10200(12) 0.0400(7) Uani 1 1 d . . . O4 O -0.0566(3) 0.4966(3) 1.14101(12) 0.0489(8) Uani 1 1 d . . . C5 C -0.3958(4) 0.5112(3) 1.13772(17) 0.0366(9) Uani 1 1 d . . . H5A H -0.4702 0.5656 1.1391 0.055 Uiso 1 1 calc . . . H5B H -0.3647 0.4945 1.1806 0.055 Uiso 1 1 calc . . . H5C H -0.4341 0.4473 1.1178 0.055 Uiso 1 1 calc . . . C6 C -0.0794(5) 0.4494(4) 1.2012(2) 0.0520(12) Uani 1 1 d . . . H6A H 0.0026 0.4643 1.2285 0.078 Uiso 1 1 calc . . . H6B H -0.0900 0.3728 1.1963 0.078 Uiso 1 1 calc . . . H6C H -0.1664 0.4786 1.2202 0.078 Uiso 1 1 calc . . . S1 S 0.25200(9) 0.77417(6) 1.10053(4) 0.01847(18) Uani 1 1 d . . . O11 O 0.3709(2) 0.72123(18) 1.07048(10) 0.0293(6) Uani 1 1 d . . . O12 O 0.1147(2) 0.74670(19) 1.07496(10) 0.0263(6) Uani 1 1 d . . . O13 O 0.2750(3) 0.88495(18) 1.11159(12) 0.0361(7) Uani 1 1 d . . . C13 C 0.2477(5) 0.7151(3) 1.17888(17) 0.0387(10) Uani 1 1 d . . . F11 F 0.3634(3) 0.7402(2) 1.21044(11) 0.0683(8) Uani 1 1 d . . . F12 F 0.2438(3) 0.61020(17) 1.17400(11) 0.0546(7) Uani 1 1 d . . . F13 F 0.1349(3) 0.7471(2) 1.21066(11) 0.0679(8) Uani 1 1 d . . . S2 S 0.83126(10) 0.18833(6) 0.83969(3) 0.01824(18) Uani 1 1 d . . . O21 O 0.9656(3) 0.24062(19) 0.85056(12) 0.0362(7) Uani 1 1 d . . . O22 O 0.7623(3) 0.1498(2) 0.89600(11) 0.0388(7) Uani 1 1 d . . . O23 O 0.8283(3) 0.11595(19) 0.78826(11) 0.0378(6) Uani 1 1 d . . . C23 C 0.7184(4) 0.2955(3) 0.81416(19) 0.0357(10) Uani 1 1 d . . . F21 F 0.7220(2) 0.37636(16) 0.85284(14) 0.0571(8) Uani 1 1 d . . . F22 F 0.7578(4) 0.3301(2) 0.75798(13) 0.0846(10) Uani 1 1 d . . . F23 F 0.5804(3) 0.2681(2) 0.81044(13) 0.0600(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 Co 0.0144(2) 0.0126(2) 0.01496(19) 0.00056(16) 0.00025(18) 0.00010(18) N3 0.0218(15) 0.0131(14) 0.0207(13) 0.0010(11) 0.0039(10) 0.0000(12) N4 0.0214(14) 0.0161(15) 0.0214(14) 0.0023(11) -0.0003(12) -0.0006(15) N5 0.0197(15) 0.0160(16) 0.0201(14) 0.0017(11) -0.0019(12) -0.0004(12) N2 0.0143(14) 0.0182(14) 0.0210(14) 0.0006(12) -0.0003(12) 0.0008(11) C9 0.0160(17) 0.0205(18) 0.0360(19) 0.0079(16) 0.0083(15) 0.0012(15) C10 0.0175(18) 0.0210(19) 0.040(2) 0.0090(16) -0.0024(14) -0.0006(15) C11 0.037(2) 0.0212(18) 0.0177(18) -0.0043(14) 0.0056(15) -0.0043(17) C12 0.033(2) 0.0215(19) 0.0196(17) 0.0006(15) -0.0047(15) -0.0087(16) C8 0.025(2) 0.0175(17) 0.0231(18) 0.0069(14) 0.0007(14) -0.0053(15) C7 0.032(2) 0.0189(18) 0.034(2) 0.0052(16) 0.0062(17) 0.0021(17) O1 0.0210(12) 0.0132(10) 0.0185(11) 0.0006(9) 0.0055(10) -0.0025(9) O2 0.0241(13) 0.0126(12) 0.0320(13) 0.0030(9) 0.0056(11) -0.0009(11) C1 0.0185(18) 0.0173(18) 0.0168(16) -0.0003(13) -0.0015(13) 0.0009(14) C2 0.0212(19) 0.0149(18) 0.0248(18) 0.0025(14) 0.0030(15) -0.0003(15) N1 0.0243(16) 0.0136(14) 0.0206(14) -0.0026(11) 0.0059(12) 0.0013(12) C3 0.0247(19) 0.025(2) 0.036(2) 0.0039(17) 0.0092(15) 0.0038(17) C4 0.0279(19) 0.0281(19) 0.0275(18) -0.0048(15) 0.0161(17) -0.0028(19) O3 0.0474(18) 0.0186(13) 0.0540(17) 0.0051(12) 0.0164(14) 0.0080(13) O4 0.0479(18) 0.065(2) 0.0343(15) -0.0024(16) -0.0002(13) -0.0180(17) C5 0.0204(19) 0.042(2) 0.047(2) 0.001(2) 0.0042(17) 0.0008(19) C6 0.051(3) 0.059(3) 0.046(3) 0.002(2) -0.001(2) 0.020(2) S1 0.0197(4) 0.0166(4) 0.0191(4) -0.0004(3) 0.0001(3) -0.0019(4) O11 0.0246(14) 0.0296(14) 0.0337(14) -0.0006(11) 0.0072(10) 0.0001(11) O12 0.0196(12) 0.0300(14) 0.0292(13) 0.0007(10) -0.0025(10) -0.0006(11) O13 0.0426(17) 0.0163(13) 0.0496(17) -0.0033(11) -0.0065(13) -0.0055(12) C13 0.040(3) 0.051(3) 0.025(2) -0.0034(18) -0.0028(19) 0.010(2) F11 0.0737(19) 0.094(2) 0.0372(15) 0.0096(14) -0.0318(13) -0.0086(18) F12 0.0710(18) 0.0378(14) 0.0550(16) 0.0281(11) 0.0059(13) 0.0006(14) F13 0.077(2) 0.092(2) 0.0348(14) 0.0023(14) 0.0269(13) 0.0184(17) S2 0.0221(4) 0.0161(4) 0.0165(4) -0.0008(3) 0.0007(4) -0.0013(4) O21 0.0230(14) 0.0250(14) 0.0606(18) -0.0113(13) -0.0053(12) -0.0027(12) O22 0.0448(17) 0.0449(16) 0.0267(14) 0.0162(12) 0.0163(12) 0.0134(15) O23 0.0559(17) 0.0314(14) 0.0262(13) -0.0130(10) -0.0054(13) -0.0001(14) C23 0.032(2) 0.026(2) 0.049(2) 0.0083(18) -0.0063(18) -0.0027(17) F21 0.0271(13) 0.0254(12) 0.119(2) -0.0277(14) -0.0102(14) 0.0072(11) F22 0.114(2) 0.0704(19) 0.0690(19) 0.0511(16) 0.0118(18) 0.029(2) F23 0.0306(14) 0.0414(15) 0.108(2) -0.0011(14) -0.0340(14) 0.0022(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O1 1.8994(19) . yes Co N2 1.939(3) . yes Co N3 1.950(2) . yes Co N5 1.964(3) . yes Co N4 1.968(3) . yes Co N1 1.978(3) . yes N3 C11 1.491(4) . yes N3 C9 1.491(4) . yes N3 C8 1.524(4) . yes N4 C10 1.498(4) . yes N5 C12 1.496(4) . yes N2 C7 1.505(4) . yes C9 C10 1.510(5) . yes C11 C12 1.503(5) . yes C8 C7 1.499(5) . yes O1 C1 1.311(4) . yes O2 C1 1.224(4) . yes C1 C2 1.512(5) . yes C2 N1 1.498(4) . yes N1 C3 1.484(4) . yes C3 C4 1.524(4) . yes C4 O3 1.370(4) . yes C4 O4 1.385(4) . yes O3 C5 1.436(4) . yes O4 C6 1.429(5) . yes S1 O12 1.437(2) . yes S1 O13 1.438(2) . yes S1 O11 1.446(2) . yes S1 C13 1.826(4) . yes C13 F11 1.312(5) . yes C13 F13 1.316(5) . yes C13 F12 1.333(4) . yes S2 O23 1.427(2) . yes S2 O21 1.438(2) . yes S2 O22 1.444(2) . yes S2 C23 1.802(4) . yes C23 F21 1.314(4) . yes C23 F22 1.324(5) . yes C23 F23 1.338(4) . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co N2 176.97(10) . . yes O1 Co N3 90.91(10) . . yes N2 Co N3 86.64(11) . . yes O1 Co N5 88.82(10) . . yes N2 Co N5 92.81(11) . . yes N3 Co N5 86.63(11) . . yes O1 Co N4 86.24(10) . . yes N2 Co N4 91.82(11) . . yes N3 Co N4 86.28(11) . . yes N5 Co N4 171.29(11) . . yes O1 Co N1 84.96(10) . . yes N2 Co N1 97.50(11) . . yes N3 Co N1 175.86(11) . . yes N5 Co N1 93.35(11) . . yes N4 Co N1 93.36(11) . . yes C11 N3 C9 112.8(3) . . yes C11 N3 C8 110.3(2) . . yes C9 N3 C8 110.4(3) . . yes C11 N3 Co 106.46(19) . . yes C9 N3 Co 105.82(18) . . yes C8 N3 Co 110.94(19) . . yes C10 N4 Co 110.87(19) . . yes C12 N5 Co 109.6(2) . . yes C7 N2 Co 110.2(2) . . yes N3 C9 C10 108.9(3) . . yes N4 C10 C9 108.5(3) . . yes N3 C11 C12 107.4(3) . . yes N5 C12 C11 108.5(3) . . yes C7 C8 N3 110.7(3) . . yes C8 C7 N2 108.4(3) . . yes C1 O1 Co 116.19(19) . . yes O2 C1 O1 123.9(3) . . yes O2 C1 C2 121.0(3) . . yes O1 C1 C2 115.0(3) . . yes N1 C2 C1 109.5(3) . . yes C3 N1 C2 112.0(3) . . yes C3 N1 Co 119.3(2) . . yes C2 N1 Co 107.1(2) . . yes N1 C3 C4 112.3(3) . . yes O3 C4 O4 114.1(3) . . yes O3 C4 C3 104.9(3) . . yes O4 C4 C3 105.5(3) . . yes C4 O3 C5 115.7(3) . . yes C4 O4 C6 116.3(3) . . yes O12 S1 O13 115.56(16) . . yes O12 S1 O11 114.04(13) . . yes O13 S1 O11 114.14(16) . . yes O12 S1 C13 103.08(18) . . yes O13 S1 C13 104.67(17) . . yes O11 S1 C13 103.30(17) . . yes F11 C13 F13 108.9(3) . . yes F11 C13 F12 107.6(4) . . yes F13 C13 F12 108.9(4) . . yes F11 C13 S1 110.5(3) . . yes F13 C13 S1 111.1(3) . . yes F12 C13 S1 109.7(2) . . yes O23 S2 O21 115.80(17) . . yes O23 S2 O22 114.18(16) . . yes O21 S2 O22 114.32(16) . . yes O23 S2 C23 103.96(17) . . yes O21 S2 C23 102.33(16) . . yes O22 S2 C23 104.04(17) . . yes F21 C23 F22 107.4(3) . . yes F21 C23 F23 105.3(3) . . yes F22 C23 F23 107.5(3) . . yes F21 C23 S2 112.5(3) . . yes F22 C23 S2 111.0(3) . . yes F23 C23 S2 112.8(3) . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co N3 C11 63.2(2) . . . . yes N2 Co N3 C11 -118.6(2) . . . . yes N5 Co N3 C11 -25.6(2) . . . . yes N4 Co N3 C11 149.4(2) . . . . yes N1 Co N3 C11 64.3(16) . . . . yes O1 Co N3 C9 -57.1(2) . . . . yes N2 Co N3 C9 121.2(2) . . . . yes N5 Co N3 C9 -145.8(2) . . . . yes N4 Co N3 C9 29.1(2) . . . . yes N1 Co N3 C9 -56.0(16) . . . . yes O1 Co N3 C8 -176.8(2) . . . . yes N2 Co N3 C8 1.4(2) . . . . yes N5 Co N3 C8 94.4(2) . . . . yes N4 Co N3 C8 -90.6(2) . . . . yes N1 Co N3 C8 -175.7(15) . . . . yes O1 Co N4 C10 85.2(2) . . . . yes N2 Co N4 C10 -92.5(2) . . . . yes N3 Co N4 C10 -6.0(2) . . . . yes N5 Co N4 C10 29.6(9) . . . . yes N1 Co N4 C10 169.9(2) . . . . yes O1 Co N5 C12 -91.6(2) . . . . yes N2 Co N5 C12 85.9(2) . . . . yes N3 Co N5 C12 -0.6(2) . . . . yes N4 Co N5 C12 -36.1(9) . . . . yes N1 Co N5 C12 -176.4(2) . . . . yes O1 Co N2 C7 14(2) . . . . yes N3 Co N2 C7 -22.1(2) . . . . yes N5 Co N2 C7 -108.6(2) . . . . yes N4 Co N2 C7 64.0(2) . . . . yes N1 Co N2 C7 157.7(2) . . . . yes C11 N3 C9 C10 -162.9(3) . . . . yes C8 N3 C9 C10 73.2(3) . . . . yes Co N3 C9 C10 -46.9(3) . . . . yes Co N4 C10 C9 -18.7(3) . . . . yes N3 C9 C10 N4 43.1(4) . . . . yes C9 N3 C11 C12 162.1(3) . . . . yes C8 N3 C11 C12 -74.0(3) . . . . yes Co N3 C11 C12 46.4(3) . . . . yes Co N5 C12 C11 26.7(3) . . . . yes N3 C11 C12 N5 -48.1(4) . . . . yes C11 N3 C8 C7 137.4(3) . . . . yes C9 N3 C8 C7 -97.3(3) . . . . yes Co N3 C8 C7 19.7(3) . . . . yes N3 C8 C7 N2 -36.8(4) . . . . yes Co N2 C7 C8 37.9(3) . . . . yes N2 Co O1 C1 156(2) . . . . yes N3 Co O1 C1 -167.9(2) . . . . yes N5 Co O1 C1 -81.3(2) . . . . yes N4 Co O1 C1 105.9(2) . . . . yes N1 Co O1 C1 12.2(2) . . . . yes Co O1 C1 O2 -179.9(3) . . . . yes Co O1 C1 C2 2.0(3) . . . . yes O2 C1 C2 N1 161.1(3) . . . . yes O1 C1 C2 N1 -20.7(4) . . . . yes C1 C2 N1 C3 160.6(3) . . . . yes C1 C2 N1 Co 28.0(3) . . . . yes O1 Co N1 C3 -150.8(2) . . . . yes N2 Co N1 C3 31.0(3) . . . . yes N3 Co N1 C3 -151.9(15) . . . . yes N5 Co N1 C3 -62.3(3) . . . . yes N4 Co N1 C3 123.3(2) . . . . yes O1 Co N1 C2 -22.3(2) . . . . yes N2 Co N1 C2 159.5(2) . . . . yes N3 Co N1 C2 -23.4(17) . . . . yes N5 Co N1 C2 66.2(2) . . . . yes N4 Co N1 C2 -108.3(2) . . . . yes C2 N1 C3 C4 65.5(4) . . . . yes Co N1 C3 C4 -168.3(2) . . . . yes N1 C3 C4 O3 175.4(3) . . . . yes N1 C3 C4 O4 54.6(4) . . . . yes O4 C4 O3 C5 -95.0(4) . . . . yes C3 C4 O3 C5 150.0(3) . . . . yes O3 C4 O4 C6 82.6(4) . . . . yes C3 C4 O4 C6 -162.8(3) . . . . yes O12 S1 C13 F11 -175.4(3) . . . . yes O13 S1 C13 F11 -54.1(3) . . . . yes O11 S1 C13 F11 65.6(3) . . . . yes O12 S1 C13 F13 -54.4(3) . . . . yes O13 S1 C13 F13 66.8(3) . . . . yes O11 S1 C13 F13 -173.4(3) . . . . yes O12 S1 C13 F12 66.1(3) . . . . yes O13 S1 C13 F12 -172.6(3) . . . . yes O11 S1 C13 F12 -52.9(4) . . . . yes O23 S2 C23 F21 -172.2(3) . . . . yes O21 S2 C23 F21 -51.3(3) . . . . yes O22 S2 C23 F21 67.9(3) . . . . yes O23 S2 C23 F22 -51.9(3) . . . . yes O21 S2 C23 F22 69.0(3) . . . . yes O22 S2 C23 F22 -171.7(3) . . . . yes O23 S2 C23 F23 68.8(3) . . . . yes O21 S2 C23 F23 -170.3(3) . . . . yes O22 S2 C23 F23 -51.0(3) . . . . yes _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.296 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.085 data_5 _database_code_depnum_ccdc_archive 'CCDC 255277' _audit_creation_method maXus _chemical_compound_source 'Local laboratory' _exptl_crystal_description Cube _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_F_000 1072 _cell_measurement_temperature 122.4(5) _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _computing_data_collection KappaCCD _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _chemical_formula_weight 528.449 _diffrn_radiation_type ' MoK\a' 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' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_cell_setting Monoclinic _chemical_formula_moiety 'C10 H22 Co N5 O2 2+, Cl4 Zn 2-, H2 O ' _chemical_formula_sum 'C10 H24 Cl4 Co N5 O3 Zn ' _chemical_name_systematic ; i-[Co(tren-enimgly)] ZnCL4 H2O ; _cell_length_a 11.7097(3) _cell_length_b 9.0617(2) _cell_length_c 17.7087(4) _cell_angle_alpha 90.000 _cell_angle_beta 101.501(2) _cell_angle_gamma 90.000 _cell_volume 1841.34(7) _diffrn_reflns_number 55554 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_av_R_equivalents 0.023 _cell_measurement_reflns_used 162 _cell_measurement_theta_min 3.906 _cell_measurement_theta_max 21.767 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.030 0 1 2 0.150 0 -1 2 0.100 0 0 1 0.160 0 -1 -2 0.115 0 0 -1 0.140 -1 0 0 0.090 0 1 -2 0.150 -1 0 2 0.130 1 0 -2 0.110 -3 0 -1 0.080 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.491 _exptl_absorpt_correction_T_max 0.750 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; 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' 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 4226 _reflns_number_gt 4119 _reflns_threshold_expression >2sigma(I) _exptl_absorpt_coefficient_mu 2.804 _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^)+(0.0000P)^2^+21.0811P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_number_reflns 4226 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1444 _refine_ls_goodness_of_fit_ref 1.345 _refine_ls_restrained_S_all 1.345 _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 C1 C 0.5602(5) 0.1503(7) 0.4770(3) 0.0186(11) Uani 1 1 d . A . C2 C 0.6764(6) 0.0702(8) 0.4849(3) 0.0269(14) Uani 1 1 d . . . H2A H 0.7208 0.1135 0.4505 0.032 Uiso 1 1 d R A . H2B H 0.6629 -0.0322 0.4723 0.032 Uiso 1 1 d R . . C3 C 0.8650(6) 0.0652(10) 0.5863(4) 0.0373(19) Uani 1 1 d . . . H3A H 0.8824 -0.0381 0.5931 0.045 Uiso 1 1 d R A . H3B H 0.9039 0.1046 0.5478 0.045 Uiso 1 1 d R . . C4 C 0.9015(5) 0.1434(8) 0.6612(4) 0.0275(14) Uani 1 1 d . A . H4 H 0.9768 0.1322 0.6940 0.033 Uiso 1 1 d R . . C5 C 0.8431(5) 0.3221(7) 0.7505(3) 0.0214(12) Uani 1 1 d . A . H5A H 0.8150 0.2685 0.7899 0.026 Uiso 1 1 d R . . H5B H 0.9242 0.3446 0.7680 0.026 Uiso 1 1 d R . . C6 C 0.7708(5) 0.4602(7) 0.7261(3) 0.0201(12) Uani 1 1 d . A . H6A H 0.8137 0.5239 0.6986 0.024 Uiso 1 1 d R . . H6B H 0.7560 0.5105 0.7709 0.024 Uiso 1 1 d R . . C7 C 0.6119(5) 0.5355(6) 0.6179(3) 0.0166(11) Uani 1 1 d . A . H7A H 0.5355 0.5086 0.5905 0.020 Uiso 1 1 d R . . H7B H 0.6075 0.6262 0.6452 0.020 Uiso 1 1 d R . . C8 C 0.6957(5) 0.5513(7) 0.5636(3) 0.0223(12) Uani 1 1 d . A . H8A H 0.7547 0.6225 0.5835 0.027 Uiso 1 1 d R . . H8B H 0.6537 0.5832 0.5141 0.027 Uiso 1 1 d R . . C9 C 0.5701(5) 0.3702(7) 0.7221(3) 0.0205(12) Uani 1 1 d . A . H9A H 0.6111 0.3480 0.7733 0.025 Uiso 1 1 d R . . H9B H 0.5155 0.4485 0.7239 0.025 Uiso 1 1 d R . . C10 C 0.5067(5) 0.2352(7) 0.6866(4) 0.0231(12) Uani 1 1 d . A . H10A H 0.4536 0.2588 0.6395 0.028 Uiso 1 1 d R . . H10B H 0.4648 0.1899 0.7218 0.028 Uiso 1 1 d R . . N1 N 0.7379(6) 0.0744(9) 0.5665(4) 0.018(2) Uiso 0.75(2) 1 d P A 1 H1 H 0.7096 -0.0045 0.5909 0.022 Uiso 0.75(2) 1 calc PR A 1 N1' N 0.7606(18) 0.122(3) 0.5402(13) 0.020(6) Uiso 0.25(2) 1 d P A 2 H1' H 0.7917 0.1939 0.5127 0.024 Uiso 0.25(2) 1 calc PR A 2 N2 N 0.8291(4) 0.2312(6) 0.6807(3) 0.0214(10) Uani 1 1 d . . . N3 N 0.6572(4) 0.4164(5) 0.6745(3) 0.0154(9) Uani 1 1 d . . . N4 N 0.7513(4) 0.4050(7) 0.5532(3) 0.0238(11) Uani 1 1 d . . . H14A H 0.8336 0.4142 0.5725 0.029 Uiso 1 1 d R A . H14B H 0.7373 0.3794 0.4996 0.029 Uiso 1 1 d R . . N5 N 0.5976(5) 0.1321(6) 0.6705(3) 0.0257(12) Uani 1 1 d . . . H15A H 0.5642 0.0496 0.6399 0.031 Uiso 1 1 d R A . H15B H 0.6475 0.0971 0.7167 0.031 Uiso 1 1 d R . . O1 O 0.5535(3) 0.2480(5) 0.5287(2) 0.0214(9) Uani 1 1 d . . . O2 O 0.4796(4) 0.1224(5) 0.4229(2) 0.0275(10) Uani 1 1 d . . . O3 O 0.9396(9) 0.2708(13) 0.9611(6) 0.060(4) Uani 0.64(2) 1 d P . . Cl1 Cl 0.83056(15) -0.2972(2) 0.91544(11) 0.0368(4) Uani 1 1 d . . . Cl2 Cl 0.68653(12) 0.07454(17) 0.86358(8) 0.0204(3) Uani 1 1 d . . . Cl3 Cl 0.7786(2) -0.1565(2) 0.71723(10) 0.0406(5) Uani 1 1 d . . . Cl4 Cl 0.99376(14) 0.0294(3) 0.86317(14) 0.0521(6) Uani 1 1 d . . . Co1 Co 0.68865(7) 0.25149(9) 0.61134(5) 0.0196(2) Uani 1 1 d . A . Zn1 Zn 0.82375(6) -0.09370(9) 0.84339(4) 0.02295(18) 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 C1 0.022(3) 0.018(3) 0.014(3) 0.002(2) 0.001(2) -0.001(2) C2 0.032(3) 0.030(3) 0.017(3) -0.006(3) 0.000(2) 0.013(3) C3 0.026(3) 0.061(5) 0.025(3) -0.008(3) 0.003(3) 0.027(3) C4 0.019(3) 0.040(4) 0.022(3) 0.003(3) 0.000(2) 0.011(3) C5 0.026(3) 0.017(3) 0.016(3) 0.001(2) -0.007(2) 0.003(2) C6 0.021(3) 0.020(3) 0.015(3) -0.007(2) -0.006(2) 0.001(2) C7 0.017(3) 0.015(3) 0.016(3) 0.001(2) -0.001(2) 0.005(2) C8 0.018(3) 0.030(3) 0.018(3) 0.003(2) 0.003(2) 0.001(2) C9 0.025(3) 0.022(3) 0.014(3) 0.002(2) 0.004(2) 0.000(2) C10 0.022(3) 0.019(3) 0.026(3) 0.007(2) 0.001(2) -0.003(2) N2 0.018(2) 0.019(3) 0.023(2) 0.000(2) -0.0038(19) 0.003(2) N3 0.017(2) 0.014(2) 0.014(2) 0.0008(18) -0.0013(17) 0.0022(18) N4 0.016(2) 0.040(3) 0.014(2) -0.005(2) -0.0006(18) 0.006(2) N5 0.029(3) 0.014(2) 0.027(3) 0.000(2) -0.011(2) 0.002(2) O1 0.018(2) 0.021(2) 0.021(2) -0.0102(17) -0.0050(16) 0.0040(17) O2 0.034(2) 0.020(2) 0.020(2) -0.0064(17) -0.0125(18) 0.0054(19) O3 0.049(6) 0.063(8) 0.061(7) -0.029(6) -0.006(5) 0.018(5) Cl1 0.0309(8) 0.0342(9) 0.0439(10) 0.0192(8) 0.0039(7) -0.0040(7) Cl2 0.0166(6) 0.0296(7) 0.0151(6) -0.0002(5) 0.0031(5) 0.0016(6) Cl3 0.0642(13) 0.0235(8) 0.0303(9) -0.0039(7) 0.0002(8) 0.0148(8) Cl4 0.0123(7) 0.0663(14) 0.0733(14) 0.0419(12) -0.0018(8) -0.0039(8) Co1 0.0166(4) 0.0197(4) 0.0188(4) -0.0084(3) -0.0055(3) 0.0075(3) Zn1 0.0177(3) 0.0257(4) 0.0260(4) 0.0079(3) 0.0058(3) 0.0046(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 C1 O2 1.230(7) . yes C1 O1 1.288(7) . yes C1 C2 1.523(8) . yes C2 N1' 1.33(2) . yes C2 N1 1.481(9) . yes C2 H2A 0.9601 . yes C2 H2B 0.9600 . yes C3 N1' 1.42(2) . yes C3 N1 1.462(9) . yes C3 C4 1.490(9) . yes C3 H3A 0.9600 . yes C3 H3B 0.9599 . yes C4 N2 1.261(8) . yes C4 H4 0.9600 . yes C5 N2 1.467(8) . yes C5 C6 1.524(8) . yes C5 H5A 0.9600 . yes C5 H5B 0.9600 . yes C6 N3 1.510(7) . yes C6 H6A 0.9601 . yes C6 H6B 0.9600 . yes C7 N3 1.496(7) . yes C7 C8 1.511(8) . yes C7 H7A 0.9601 . yes C7 H7B 0.9600 . yes C8 N4 1.505(8) . yes C8 H8A 0.9600 . yes C8 H8B 0.9599 . yes C9 C10 1.502(8) . yes C9 N3 1.505(7) . yes C9 H9A 0.9601 . yes C9 H9B 0.9600 . yes C10 N5 1.485(8) . yes C10 H10A 0.9600 . yes C10 H10B 0.9599 . yes N1 Co1 1.929(7) . yes N1 H1 0.9300 . yes N1' Co1 2.03(2) . yes N1' H1' 0.9300 . yes N2 Co1 1.855(5) . yes N3 Co1 1.945(5) . yes N4 Co1 1.958(6) . yes N4 H14A 0.9600 . yes N4 H14B 0.9599 . yes N5 Co1 1.962(6) . yes N5 H15A 0.9600 . yes N5 H15B 0.9600 . yes O1 Co1 1.930(4) . yes Cl1 Zn1 2.2346(18) . yes Cl2 Zn1 2.2942(16) . yes Cl3 Zn1 2.2635(19) . yes Cl4 Zn1 2.2479(19) . yes 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 O2 C1 O1 123.3(6) . . yes O2 C1 C2 120.4(5) . . yes O1 C1 C2 116.3(5) . . yes N1' C2 N1 29.2(11) . . yes N1' C2 C1 114.7(10) . . yes N1 C2 C1 109.2(5) . . yes N1' C2 H2A 84.7 . . yes N1 C2 H2A 112.9 . . yes C1 C2 H2A 109.5 . . yes N1' C2 H2B 125.1 . . yes N1 C2 H2B 106.0 . . yes C1 C2 H2B 109.7 . . yes H2A C2 H2B 109.5 . . yes N1' C3 N1 29.0(10) . . yes N1' C3 C4 113.6(10) . . yes N1 C3 C4 106.5(5) . . yes N1' C3 H3A 124.0 . . yes N1 C3 H3A 105.4 . . yes C4 C3 H3A 109.6 . . yes N1' C3 H3B 86.2 . . yes N1 C3 H3B 114.4 . . yes C4 C3 H3B 111.3 . . yes H3A C3 H3B 109.5 . . yes N2 C4 C3 117.1(6) . . yes N2 C4 H4 119.2 . . yes C3 C4 H4 123.6 . . yes N2 C5 C6 105.0(4) . . yes N2 C5 H5A 109.3 . . yes C6 C5 H5A 111.7 . . yes N2 C5 H5B 109.2 . . yes C6 C5 H5B 112.0 . . yes H5A C5 H5B 109.5 . . yes N3 C6 C5 109.1(5) . . yes N3 C6 H6A 109.7 . . yes C5 C6 H6A 108.7 . . yes N3 C6 H6B 110.0 . . yes C5 C6 H6B 109.8 . . yes H6A C6 H6B 109.5 . . yes N3 C7 C8 107.8(5) . . yes N3 C7 H7A 109.0 . . yes C8 C7 H7A 111.2 . . yes N3 C7 H7B 109.1 . . yes C8 C7 H7B 110.2 . . yes H7A C7 H7B 109.5 . . yes N4 C8 C7 110.2(5) . . yes N4 C8 H8A 109.9 . . yes C7 C8 H8A 110.0 . . yes N4 C8 H8B 108.0 . . yes C7 C8 H8B 109.3 . . yes H8A C8 H8B 109.5 . . yes C10 C9 N3 109.0(5) . . yes C10 C9 H9A 109.7 . . yes N3 C9 H9A 108.8 . . yes C10 C9 H9B 109.8 . . yes N3 C9 H9B 110.1 . . yes H9A C9 H9B 109.5 . . yes N5 C10 C9 106.2(5) . . yes N5 C10 H10A 109.8 . . yes C9 C10 H10A 111.3 . . yes N5 C10 H10B 109.5 . . yes C9 C10 H10B 110.5 . . yes H10A C10 H10B 109.5 . . yes C3 N1 C2 120.4(7) . . yes C3 N1 Co1 108.8(5) . . yes C2 N1 Co1 107.2(5) . . yes C3 N1 H1 106.6 . . yes C2 N1 H1 106.6 . . yes Co1 N1 H1 106.6 . . yes C2 N1' C3 136.2(17) . . yes C2 N1' Co1 108.8(13) . . yes C3 N1' Co1 105.6(12) . . yes C2 N1' H1' 99.9 . . yes C3 N1' H1' 99.9 . . yes Co1 N1' H1' 99.9 . . yes C4 N2 C5 128.1(5) . . yes C4 N2 Co1 115.9(4) . . yes C5 N2 Co1 116.0(4) . . yes C7 N3 C9 112.7(4) . . yes C7 N3 C6 111.6(4) . . yes C9 N3 C6 110.4(4) . . yes C7 N3 Co1 104.6(3) . . yes C9 N3 Co1 109.6(4) . . yes C6 N3 Co1 107.8(3) . . yes C8 N4 Co1 110.2(4) . . yes C8 N4 H14A 108.0 . . yes Co1 N4 H14A 109.3 . . yes C8 N4 H14B 110.0 . . yes Co1 N4 H14B 109.9 . . yes H14A N4 H14B 109.5 . . yes C10 N5 Co1 104.0(4) . . yes C10 N5 H15A 111.8 . . yes Co1 N5 H15A 109.4 . . yes C10 N5 H15B 112.5 . . yes Co1 N5 H15B 109.5 . . yes H15A N5 H15B 109.5 . . yes C1 O1 Co1 113.1(4) . . yes N2 Co1 N1 83.8(3) . . yes N2 Co1 O1 170.2(2) . . yes N1 Co1 O1 86.6(2) . . yes N2 Co1 N3 86.5(2) . . yes N1 Co1 N3 169.2(3) . . yes O1 Co1 N3 103.15(18) . . yes N2 Co1 N4 92.4(2) . . yes N1 Co1 N4 101.6(3) . . yes O1 Co1 N4 87.1(2) . . yes N3 Co1 N4 83.7(2) . . yes N2 Co1 N5 95.5(2) . . yes N1 Co1 N5 90.0(3) . . yes O1 Co1 N5 86.8(2) . . yes N3 Co1 N5 86.0(2) . . yes N4 Co1 N5 166.6(2) . . yes N2 Co1 N1' 86.0(6) . . yes N1 Co1 N1' 20.9(7) . . yes O1 Co1 N1' 84.2(6) . . yes N3 Co1 N1' 162.4(8) . . yes N4 Co1 N1' 80.7(8) . . yes N5 Co1 N1' 110.5(8) . . yes Cl1 Zn1 Cl4 113.01(7) . . yes Cl1 Zn1 Cl3 109.33(8) . . yes Cl4 Zn1 Cl3 107.69(9) . . yes Cl1 Zn1 Cl2 113.93(7) . . yes Cl4 Zn1 Cl2 105.78(8) . . yes Cl3 Zn1 Cl2 106.73(7) . . yes 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 O2 C1 C2 N1' 172.5(14) . . . . yes O1 C1 C2 N1' -6.5(16) . . . . yes O2 C1 C2 N1 -156.5(6) . . . . yes O1 C1 C2 N1 24.5(8) . . . . yes N1' C3 C4 N2 11.1(16) . . . . yes N1 C3 C4 N2 -18.9(10) . . . . yes N2 C5 C6 N3 41.8(6) . . . . yes N3 C7 C8 N4 31.2(6) . . . . yes N3 C9 C10 N5 47.4(6) . . . . yes N1' C3 N1 C2 43.6(18) . . . . yes C4 C3 N1 C2 152.7(7) . . . . yes N1' C3 N1 Co1 -80.6(19) . . . . yes C4 C3 N1 Co1 28.5(8) . . . . yes N1' C2 N1 C3 -47.3(19) . . . . yes C1 C2 N1 C3 -153.7(7) . . . . yes N1' C2 N1 Co1 77.7(19) . . . . yes C1 C2 N1 Co1 -28.8(7) . . . . yes N1 C2 N1' C3 70(3) . . . . yes C1 C2 N1' C3 155(2) . . . . yes N1 C2 N1' Co1 -69.9(18) . . . . yes C1 C2 N1' Co1 15.4(19) . . . . yes N1 C3 N1' C2 -73(3) . . . . yes C4 C3 N1' C2 -155(2) . . . . yes N1 C3 N1' Co1 67.5(17) . . . . yes C4 C3 N1' Co1 -14.0(17) . . . . yes C3 C4 N2 C5 -179.5(7) . . . . yes C3 C4 N2 Co1 -1.0(9) . . . . yes C6 C5 N2 C4 148.4(7) . . . . yes C6 C5 N2 Co1 -30.1(6) . . . . yes C8 C7 N3 C9 -169.0(5) . . . . yes C8 C7 N3 C6 66.1(6) . . . . yes C8 C7 N3 Co1 -50.1(5) . . . . yes C10 C9 N3 C7 96.7(6) . . . . yes C10 C9 N3 C6 -137.8(5) . . . . yes C10 C9 N3 Co1 -19.3(5) . . . . yes C5 C6 N3 C7 -150.4(5) . . . . yes C5 C6 N3 C9 83.5(6) . . . . yes C5 C6 N3 Co1 -36.2(5) . . . . yes C7 C8 N4 Co1 2.0(6) . . . . yes C9 C10 N5 Co1 -52.3(5) . . . . yes O2 C1 O1 Co1 174.0(5) . . . . yes C2 C1 O1 Co1 -7.0(7) . . . . yes C4 N2 Co1 N1 15.0(6) . . . . yes C5 N2 Co1 N1 -166.4(5) . . . . yes C4 N2 Co1 O1 0.9(16) . . . . yes C5 N2 Co1 O1 179.5(11) . . . . yes C4 N2 Co1 N3 -169.9(5) . . . . yes C5 N2 Co1 N3 8.7(4) . . . . yes C4 N2 Co1 N4 -86.4(5) . . . . yes C5 N2 Co1 N4 92.2(5) . . . . yes C4 N2 Co1 N5 104.4(5) . . . . yes C5 N2 Co1 N5 -77.0(5) . . . . yes C4 N2 Co1 N1' -5.9(9) . . . . yes C5 N2 Co1 N1' 172.7(9) . . . . yes C3 N1 Co1 N2 -24.6(6) . . . . yes C2 N1 Co1 N2 -156.3(6) . . . . yes C3 N1 Co1 O1 153.0(6) . . . . yes C2 N1 Co1 O1 21.3(5) . . . . yes C3 N1 Co1 N3 -51.8(19) . . . . yes C2 N1 Co1 N3 176.5(13) . . . . yes C3 N1 Co1 N4 66.6(6) . . . . yes C2 N1 Co1 N4 -65.1(6) . . . . yes C3 N1 Co1 N5 -120.2(6) . . . . yes C2 N1 Co1 N5 108.1(6) . . . . yes C3 N1 Co1 N1' 70.4(18) . . . . yes C2 N1 Co1 N1' -61.2(17) . . . . yes C1 O1 Co1 N2 5.5(15) . . . . yes C1 O1 Co1 N1 -8.6(5) . . . . yes C1 O1 Co1 N3 176.1(4) . . . . yes C1 O1 Co1 N4 93.2(4) . . . . yes C1 O1 Co1 N5 -98.8(4) . . . . yes C1 O1 Co1 N1' 12.2(9) . . . . yes C7 N3 Co1 N2 134.6(4) . . . . yes C9 N3 Co1 N2 -104.3(4) . . . . yes C6 N3 Co1 N2 15.8(4) . . . . yes C7 N3 Co1 N1 161.7(15) . . . . yes C9 N3 Co1 N1 -77.2(16) . . . . yes C6 N3 Co1 N1 42.9(17) . . . . yes C7 N3 Co1 O1 -43.8(4) . . . . yes C9 N3 Co1 O1 77.3(4) . . . . yes C6 N3 Co1 O1 -162.6(4) . . . . yes C7 N3 Co1 N4 41.8(3) . . . . yes C9 N3 Co1 N4 162.9(4) . . . . yes C6 N3 Co1 N4 -77.0(4) . . . . yes C7 N3 Co1 N5 -129.6(4) . . . . yes C9 N3 Co1 N5 -8.5(4) . . . . yes C6 N3 Co1 N5 111.6(4) . . . . yes C7 N3 Co1 N1' 69(2) . . . . yes C9 N3 Co1 N1' -169(2) . . . . yes C6 N3 Co1 N1' -49(2) . . . . yes C8 N4 Co1 N2 -111.2(4) . . . . yes C8 N4 Co1 N1 164.6(4) . . . . yes C8 N4 Co1 O1 78.6(4) . . . . yes C8 N4 Co1 N3 -25.0(4) . . . . yes C8 N4 Co1 N5 15.3(11) . . . . yes C8 N4 Co1 N1' 163.2(7) . . . . yes C10 N5 Co1 N2 120.2(4) . . . . yes C10 N5 Co1 N1 -156.0(4) . . . . yes C10 N5 Co1 O1 -69.4(4) . . . . yes C10 N5 Co1 N3 34.1(4) . . . . yes C10 N5 Co1 N4 -6.1(11) . . . . yes C10 N5 Co1 N1' -152.0(7) . . . . yes C2 N1' Co1 N2 163.5(16) . . . . yes C3 N1' Co1 N2 11.0(14) . . . . yes C2 N1' Co1 N1 80(2) . . . . yes C3 N1' Co1 N1 -72.0(19) . . . . yes C2 N1' Co1 O1 -15.4(15) . . . . yes C3 N1' Co1 O1 -167.8(15) . . . . yes C2 N1' Co1 N3 -131.3(15) . . . . yes C3 N1' Co1 N3 76(3) . . . . yes C2 N1' Co1 N4 -103.4(16) . . . . yes C3 N1' Co1 N4 104.1(14) . . . . yes C2 N1' Co1 N5 69.1(17) . . . . yes C3 N1' Co1 N5 -83.4(14) . . . . yes _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.872 _refine_diff_density_min -2.158 _refine_diff_density_rms 0.172 _chemical_name_common 'i-(Co(tren-enimgly)) ZnCL4 H2O' data_s-6 _database_code_depnum_ccdc_archive 'CCDC 255278' _audit_creation_method maXus _chemical_compound_source 'Local laboratory' _exptl_crystal_description Cube _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_F_000 2080 _cell_measurement_temperature 122.4(5) _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _computing_data_collection KappaCCD _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _chemical_formula_weight 512.450 _diffrn_radiation_type ' MoK\a' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z '-X,-Y,+Z+ 1/2' '-X+ 1/2,+Y,+Z+ 1/2' '+X+ 1/2,-Y,+Z' _symmetry_space_group_name_H-M 'P c a 21 ' _symmetry_space_group_name_Hall 'P 2c -2ac ' _symmetry_cell_setting Orthorhombic _chemical_formula_moiety 'C10 H24 Co N5 O2 2+, Cl4 Zn 2- ' _chemical_formula_sum 'C10 H24 Cl4 Co N5 O2 Zn ' _chemical_name_common 's-(Co(tren-engly)) ZnCl4' _cell_length_a 19.4050(10) _cell_length_b 8.4970(5) _cell_length_c 23.116(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3811.5(5) _diffrn_reflns_number 169109 _diffrn_reflns_theta_max 35.00 _diffrn_reflns_av_R_equivalents 0.025 _cell_measurement_reflns_used 1245 _cell_measurement_theta_min 0.838 _cell_measurement_theta_max 20.362 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -2 1 0.030 1 0 2 0.144 0 2 -1 0.065 0 0 1 0.083 0 0 -1 0.095 1 0 -2 0.110 -1 0 2 0.120 0 1 1 0.080 0 -1 -1 0.090 -1 0 -2 0.140 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co .3494 .9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 16766 _reflns_number_gt 16089 _reflns_threshold_expression >2sigma(I) _exptl_absorpt_coefficient_mu 2.702 _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^)+(0.0143P)^2^+3.0789P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(9) _refine_ls_number_reflns 16766 _refine_ls_number_parameters 416 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_restrained_S_all 1.289 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.303137(12) 0.06664(3) -0.143073(10) 0.01060(4) Uani 1 1 d . . . O1 O 0.34129(7) 0.16647(15) -0.21063(6) 0.0134(2) Uani 1 1 d . . . O2 O 0.43343(8) 0.15458(18) -0.26824(6) 0.0194(3) Uani 1 1 d . . . N1 N 0.36831(8) -0.09806(18) -0.15916(7) 0.0143(3) Uani 1 1 d . . . H11 H 0.3486 -0.1724 -0.1860 0.017 Uiso 1 1 d R . . N2 N 0.27904(8) -0.04789(18) -0.07460(7) 0.0143(3) Uani 1 1 d . . . H12 H 0.3012 -0.0013 -0.0417 0.017 Uiso 1 1 d R . . N3 N 0.22904(8) 0.21352(18) -0.12288(7) 0.0138(3) Uani 1 1 d . . . N4 N 0.36450(8) 0.20397(18) -0.09713(7) 0.0146(3) Uani 1 1 d . . . H14A H 0.3981 0.2497 -0.1221 0.018 Uiso 1 1 d R . . H14B H 0.3872 0.1407 -0.0682 0.018 Uiso 1 1 d R . . N5 N 0.23460(8) -0.03007(19) -0.19487(7) 0.0157(3) Uani 1 1 d . . . H15A H 0.2251 -0.1353 -0.1813 0.019 Uiso 1 1 d R . . H15B H 0.2535 -0.0355 -0.2331 0.019 Uiso 1 1 d R . . C1 C 0.39980(9) 0.1064(2) -0.22663(8) 0.0141(3) Uani 1 1 d . . . C2 C 0.42728(10) -0.0288(2) -0.19011(8) 0.0161(3) Uani 1 1 d . . . H2A H 0.4490 -0.1040 -0.2148 0.019 Uiso 1 1 d R . . H2B H 0.4606 0.0124 -0.1631 0.019 Uiso 1 1 d R . . C3 C 0.38011(10) -0.1864(2) -0.10430(9) 0.0180(3) Uani 1 1 d . . . H3A H 0.4081 -0.1272 -0.0776 0.022 Uiso 1 1 d R . . H3B H 0.4015 -0.2869 -0.1112 0.022 Uiso 1 1 d R . . C4 C 0.30837(11) -0.2097(2) -0.07910(8) 0.0174(3) Uani 1 1 d . . . H4A H 0.2819 -0.2749 -0.1054 0.021 Uiso 1 1 d R . . H4B H 0.3118 -0.2608 -0.0426 0.021 Uiso 1 1 d R . . C5 C 0.20438(10) -0.0300(2) -0.06463(8) 0.0170(3) Uani 1 1 d . . . H5A H 0.1921 -0.0613 -0.0264 0.020 Uiso 1 1 d R . . H5B H 0.1781 -0.0898 -0.0923 0.020 Uiso 1 1 d R . . C6 C 0.18898(10) 0.1451(2) -0.07227(9) 0.0174(3) Uani 1 1 d . . . H6A H 0.1401 0.1595 -0.0796 0.021 Uiso 1 1 d R . . H6B H 0.2010 0.2018 -0.0379 0.021 Uiso 1 1 d R . . C7 C 0.26234(9) 0.3666(2) -0.10753(9) 0.0157(3) Uani 1 1 d . . . H7A H 0.2302 0.4333 -0.0875 0.019 Uiso 1 1 d R . . H7B H 0.2780 0.4193 -0.1419 0.019 Uiso 1 1 d R . . C8 C 0.32331(10) 0.3308(2) -0.06868(8) 0.0163(3) Uani 1 1 d . . . H8A H 0.3511 0.4228 -0.0633 0.020 Uiso 1 1 d R . . H8B H 0.3073 0.2952 -0.0310 0.020 Uiso 1 1 d R . . C9 C 0.18480(10) 0.2273(2) -0.17552(9) 0.0179(3) Uani 1 1 d . . . H9A H 0.2077 0.2836 -0.2055 0.022 Uiso 1 1 d R . . H9B H 0.1417 0.2805 -0.1664 0.022 Uiso 1 1 d R . . C10 C 0.16891(10) 0.0622(2) -0.19615(9) 0.0196(3) Uani 1 1 d . . . H10A H 0.1356 0.0159 -0.1709 0.024 Uiso 1 1 d R . . H10B H 0.1510 0.0667 -0.2348 0.024 Uiso 1 1 d R . . Co1' Co 0.058423(12) -0.44695(3) 0.152400(10) 0.01120(4) Uani 1 1 d . . . O1' O 0.09439(7) -0.34289(15) 0.22006(6) 0.0138(2) Uani 1 1 d . . . O2' O 0.18626(8) -0.34733(18) 0.27846(6) 0.0210(3) Uani 1 1 d . . . N1' N 0.12649(8) -0.60464(18) 0.16870(7) 0.0143(3) Uani 1 1 d . . . H11C H 0.1078 -0.6797 0.1955 0.017 Uiso 1 1 d R . . N2' N 0.03700(9) -0.56432(19) 0.08405(7) 0.0168(3) Uani 1 1 d . . . H12C H 0.0589 -0.5170 0.0516 0.020 Uiso 1 1 d R . . N3' N -0.01657(8) -0.30490(18) 0.13026(7) 0.0136(3) Uani 1 1 d . . . N4' N -0.01009(8) -0.54485(19) 0.20415(7) 0.0160(3) Uani 1 1 d . . . H14C H 0.0078 -0.5471 0.2429 0.019 Uiso 1 1 d R . . H14D H -0.0185 -0.6511 0.1914 0.019 Uiso 1 1 d R . . N5' N 0.11948(9) -0.30912(19) 0.10683(7) 0.0160(3) Uani 1 1 d . . . H15C H 0.1439 -0.3701 0.0788 0.019 Uiso 1 1 d R . . H15D H 0.1523 -0.2584 0.1323 0.019 Uiso 1 1 d R . . C1' C 0.15393(9) -0.3968(2) 0.23644(7) 0.0144(3) Uani 1 1 d . . . C2' C 0.18418(10) -0.5281(2) 0.19930(8) 0.0162(3) Uani 1 1 d . . . H2C H 0.2160 -0.4833 0.1724 0.019 Uiso 1 1 d R . . H2D H 0.2078 -0.6019 0.2238 0.019 Uiso 1 1 d R . . C3' C 0.14003(10) -0.6930(2) 0.11424(9) 0.0180(3) Uani 1 1 d . . . H3C H 0.1632 -0.7907 0.1205 0.022 Uiso 1 1 d R . . H3D H 0.1666 -0.6310 0.0866 0.022 Uiso 1 1 d R . . C4' C 0.06848(11) -0.7225(2) 0.08877(9) 0.0183(3) Uani 1 1 d . . . H4C H 0.0730 -0.7740 0.0522 0.022 Uiso 1 1 d R . . H4D H 0.0437 -0.7907 0.1151 0.022 Uiso 1 1 d R . . C5' C -0.03727(11) -0.5516(2) 0.07235(9) 0.0200(3) Uani 1 1 d . . . H5C H -0.0640 -0.6126 0.0993 0.024 Uiso 1 1 d R . . H5D H -0.0479 -0.5846 0.0336 0.024 Uiso 1 1 d R . . C6' C -0.05485(10) -0.3770(2) 0.07954(9) 0.0175(3) Uani 1 1 d . . . H6C H -0.0420 -0.3212 0.0449 0.021 Uiso 1 1 d R . . H6D H -0.1033 -0.3650 0.0860 0.021 Uiso 1 1 d R . . C7' C -0.06187(10) -0.2911(2) 0.18190(9) 0.0181(3) Uani 1 1 d . . . H7C H -0.1042 -0.2403 0.1715 0.022 Uiso 1 1 d R . . H7D H -0.0392 -0.2317 0.2116 0.022 Uiso 1 1 d R . . C8' C -0.07664(10) -0.4562(2) 0.20330(9) 0.0188(3) Uani 1 1 d . . . H8C H -0.0954 -0.4504 0.2419 0.023 Uiso 1 1 d R . . H8D H -0.1090 -0.5062 0.1783 0.023 Uiso 1 1 d R . . C9' C 0.01532(9) -0.1510(2) 0.11420(9) 0.0161(3) Uani 1 1 d . . . H9C H 0.0295 -0.0940 0.1482 0.019 Uiso 1 1 d R . . H9D H -0.0167 -0.0880 0.0927 0.019 Uiso 1 1 d R . . C10' C 0.07741(10) -0.1862(2) 0.07690(8) 0.0167(3) Uani 1 1 d . . . H10C H 0.0625 -0.2242 0.0393 0.020 Uiso 1 1 d R . . H10D H 0.1040 -0.0918 0.0712 0.020 Uiso 1 1 d R . . Zn1 Zn 0.561956(11) 0.35035(3) -0.108000(9) 0.01561(4) Uani 1 1 d . . . Cl1 Cl 0.46980(3) 0.46436(6) -0.15192(2) 0.02454(10) Uani 1 1 d . . . Cl2 Cl 0.52939(2) 0.11398(5) -0.06975(2) 0.01841(8) Uani 1 1 d . . . Cl3 Cl 0.64743(2) 0.34353(5) -0.173079(19) 0.01808(8) Uani 1 1 d . . . Cl4 Cl 0.60741(4) 0.49475(9) -0.03364(2) 0.04005(17) Uani 1 1 d . . . Zn1' Zn 0.311255(12) -0.12954(3) 0.115603(9) 0.01554(4) Uani 1 1 d . . . Cl1' Cl 0.40326(2) -0.13524(5) 0.17438(2) 0.01925(8) Uani 1 1 d . . . Cl2' Cl 0.28701(2) -0.36456(5) 0.07290(2) 0.01861(8) Uani 1 1 d . . . Cl3' Cl 0.21757(3) -0.04951(6) 0.16745(2) 0.02155(9) Uani 1 1 d . . . Cl4' Cl 0.33498(4) 0.05865(7) 0.04753(2) 0.03881(16) 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 0.01191(9) 0.00903(8) 0.01086(8) 0.00088(7) 0.00197(7) 0.00057(7) O1 0.0135(5) 0.0127(5) 0.0139(5) 0.0025(4) 0.0015(4) 0.0002(4) O2 0.0175(6) 0.0220(7) 0.0186(6) 0.0043(5) 0.0052(5) -0.0016(5) N1 0.0178(7) 0.0123(6) 0.0130(6) 0.0015(5) 0.0026(5) 0.0025(5) N2 0.0172(7) 0.0128(6) 0.0129(6) 0.0002(5) 0.0017(5) -0.0008(5) N3 0.0130(6) 0.0129(6) 0.0156(6) 0.0014(5) 0.0023(5) 0.0013(5) N4 0.0143(6) 0.0128(6) 0.0167(7) -0.0005(5) -0.0008(5) 0.0008(5) N5 0.0153(7) 0.0146(6) 0.0173(7) -0.0016(5) 0.0015(5) -0.0031(5) C1 0.0136(7) 0.0147(7) 0.0140(7) 0.0000(6) 0.0006(5) -0.0012(6) C2 0.0149(7) 0.0164(7) 0.0170(7) 0.0014(6) 0.0040(6) 0.0022(6) C3 0.0238(8) 0.0136(7) 0.0166(7) 0.0034(6) 0.0013(7) 0.0048(6) C4 0.0281(9) 0.0095(6) 0.0147(7) 0.0029(5) 0.0022(6) 0.0012(6) C5 0.0159(7) 0.0176(7) 0.0175(8) 0.0021(6) 0.0061(6) -0.0030(6) C6 0.0165(8) 0.0151(7) 0.0206(8) -0.0008(6) 0.0071(6) -0.0005(6) C7 0.0152(7) 0.0108(6) 0.0212(8) 0.0002(6) 0.0018(6) 0.0009(5) C8 0.0182(8) 0.0132(7) 0.0176(7) -0.0031(6) 0.0017(6) 0.0008(6) C9 0.0156(8) 0.0178(7) 0.0205(8) 0.0033(6) -0.0023(6) 0.0016(6) C10 0.0156(8) 0.0218(9) 0.0214(8) -0.0003(7) -0.0030(6) -0.0013(7) Co1' 0.01301(9) 0.00985(9) 0.01076(8) -0.00004(7) -0.00215(7) 0.00188(7) O1' 0.0144(5) 0.0146(5) 0.0125(5) -0.0009(4) -0.0020(4) 0.0002(4) O2' 0.0212(7) 0.0235(7) 0.0182(6) -0.0024(5) -0.0068(5) -0.0014(6) N1' 0.0164(6) 0.0129(6) 0.0136(6) 0.0005(5) -0.0015(5) 0.0031(5) N2' 0.0196(7) 0.0145(6) 0.0163(6) -0.0015(5) -0.0022(5) 0.0015(6) N3' 0.0128(6) 0.0115(6) 0.0166(6) 0.0013(5) -0.0008(5) 0.0008(5) N4' 0.0158(7) 0.0143(6) 0.0180(7) 0.0025(5) -0.0008(5) -0.0007(5) N5' 0.0168(6) 0.0168(6) 0.0143(6) 0.0023(5) 0.0020(5) 0.0040(5) C1' 0.0154(7) 0.0151(7) 0.0125(6) 0.0023(5) -0.0006(5) -0.0013(6) C2' 0.0159(8) 0.0168(7) 0.0160(7) 0.0009(6) -0.0034(6) 0.0037(6) C3' 0.0217(8) 0.0159(7) 0.0163(7) -0.0026(6) 0.0012(7) 0.0048(6) C4' 0.0246(9) 0.0122(7) 0.0180(8) -0.0029(6) 0.0008(7) 0.0025(6) C5' 0.0196(8) 0.0204(8) 0.0200(8) -0.0031(7) -0.0042(6) 0.0006(7) C6' 0.0157(8) 0.0182(8) 0.0187(8) 0.0025(6) -0.0065(6) -0.0002(6) C7' 0.0163(8) 0.0165(7) 0.0215(8) 0.0000(6) 0.0034(6) 0.0014(6) C8' 0.0156(8) 0.0171(8) 0.0235(8) 0.0028(7) 0.0034(6) 0.0008(6) C9' 0.0155(7) 0.0102(6) 0.0225(8) 0.0018(6) -0.0012(6) 0.0019(5) C10' 0.0186(8) 0.0140(7) 0.0174(7) 0.0052(6) -0.0002(6) 0.0002(6) Zn1 0.01563(9) 0.01507(9) 0.01613(9) -0.00162(7) 0.00272(7) -0.00054(7) Cl1 0.0196(2) 0.0213(2) 0.0328(3) 0.00710(18) 0.00543(18) 0.00715(16) Cl2 0.01641(18) 0.01735(17) 0.02148(19) 0.00291(15) -0.00370(15) -0.00230(15) Cl3 0.01887(19) 0.01848(18) 0.01691(17) 0.00111(15) 0.00464(14) 0.00483(15) Cl4 0.0568(4) 0.0450(3) 0.0184(2) -0.0137(2) 0.0165(2) -0.0354(3) Zn1' 0.01689(9) 0.01474(9) 0.01498(9) 0.00211(7) -0.00201(7) -0.00186(7) Cl1' 0.01802(19) 0.01825(18) 0.02147(19) 0.00094(15) -0.00507(15) 0.00073(15) Cl2' 0.01648(18) 0.01737(18) 0.02198(19) -0.00302(15) 0.00227(15) -0.00209(14) Cl3' 0.0204(2) 0.0220(2) 0.0222(2) -0.00400(17) -0.00295(16) 0.00528(17) Cl4' 0.0664(4) 0.0312(3) 0.0188(2) 0.0112(2) -0.0171(3) -0.0290(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 N2 1.9159(15) . yes Co1 N1 1.9225(15) . yes Co1 O1 1.9252(13) . yes Co1 N3 1.9604(15) . yes Co1 N5 1.9692(16) . yes Co1 N4 1.9767(16) . yes O1 C1 1.299(2) . yes O2 C1 1.232(2) . yes N1 C2 1.472(2) . yes N1 C3 1.491(2) . yes N1 H11 0.9648 . yes N2 C5 1.475(2) . yes N2 C4 1.492(2) . yes N2 H12 0.9594 . yes N3 C9 1.494(2) . yes N3 C7 1.495(2) . yes N3 C6 1.520(2) . yes N4 C8 1.494(2) . yes N4 H14A 0.9544 . yes N4 H14B 0.9644 . yes N5 C10 1.497(3) . yes N5 H15A 0.9652 . yes N5 H15B 0.9584 . yes C1 C2 1.522(3) . yes C2 H2A 0.9551 . yes C2 H2B 0.9638 . yes C3 C4 1.522(3) . yes C3 H3A 0.9637 . yes C3 H3B 0.9627 . yes C4 H4A 0.9703 . yes C4 H4B 0.9504 . yes C5 C6 1.528(3) . yes C5 H5A 0.9543 . yes C5 H5B 0.9631 . yes C6 H6A 0.9710 . yes C6 H6B 0.9589 . yes C7 C8 1.516(3) . yes C7 H7A 0.9611 . yes C7 H7B 0.9617 . yes C8 H8A 0.9583 . yes C8 H8B 0.9727 . yes C9 C10 1.513(3) . yes C9 H9A 0.9518 . yes C9 H9B 0.9743 . yes C10 H10A 0.9551 . yes C10 H10B 0.9597 . yes Co1' N2' 1.9142(16) . yes Co1' N1' 1.9188(15) . yes Co1' O1' 1.9274(13) . yes Co1' N3' 1.9588(15) . yes Co1' N5' 1.9710(17) . yes Co1' N4' 1.9725(16) . yes O1' C1' 1.299(2) . yes O2' C1' 1.230(2) . yes N1' C2' 1.475(3) . yes N1' C3' 1.489(2) . yes N1' H11C 0.9599 . yes N2' C5' 1.470(3) . yes N2' C4' 1.481(2) . yes N2' H12C 0.9515 . yes N3' C7' 1.487(2) . yes N3' C9' 1.494(2) . yes N3' C6' 1.517(2) . yes N4' C8' 1.495(3) . yes N4' H14C 0.9610 . yes N4' H14D 0.9633 . yes N5' C10' 1.496(2) . yes N5' H15C 0.9557 . yes N5' H15D 0.9685 . yes C1' C2' 1.525(3) . yes C2' H2C 0.9568 . yes C2' H2D 0.9616 . yes C3' C4' 1.529(3) . yes C3' H3C 0.9550 . yes C3' H3D 0.9753 . yes C4' H4C 0.9559 . yes C4' H4D 0.9680 . yes C5' C6' 1.532(3) . yes C5' H5C 0.9617 . yes C5' H5D 0.9603 . yes C6' H6C 0.9638 . yes C6' H6D 0.9577 . yes C7' C8' 1.515(3) . yes C7' H7C 0.9588 . yes C7' H7D 0.9597 . yes C8' H8C 0.9651 . yes C8' H8D 0.9543 . yes C9' C10' 1.511(3) . yes C9' H9C 0.9640 . yes C9' H9D 0.9601 . yes C10' H10C 0.9706 . yes C10' H10D 0.9625 . yes Zn1 Cl3 2.2399(5) . yes Zn1 Cl1 2.2731(6) . yes Zn1 Cl2 2.2836(6) . yes Zn1 Cl4 2.2888(6) . yes Zn1' Cl1' 2.2440(5) . yes Zn1' Cl2' 2.2768(5) . yes Zn1' Cl3' 2.2812(5) . yes Zn1' Cl4' 2.2902(6) . yes 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 N1 87.17(6) . . yes N2 Co1 O1 171.03(6) . . yes N1 Co1 O1 84.89(6) . . yes N2 Co1 N3 87.00(6) . . yes N1 Co1 N3 172.74(7) . . yes O1 Co1 N3 101.22(6) . . yes N2 Co1 N5 97.21(7) . . yes N1 Co1 N5 91.31(7) . . yes O1 Co1 N5 87.15(6) . . yes N3 Co1 N5 85.13(7) . . yes N2 Co1 N4 90.17(7) . . yes N1 Co1 N4 97.90(7) . . yes O1 Co1 N4 86.80(6) . . yes N3 Co1 N4 86.45(6) . . yes N5 Co1 N4 168.48(7) . . yes C1 O1 Co1 113.21(11) . . yes C2 N1 C3 119.67(15) . . yes C2 N1 Co1 108.32(11) . . yes C3 N1 Co1 107.64(11) . . yes C2 N1 H11 104.9 . . yes C3 N1 H11 106.2 . . yes Co1 N1 H11 109.9 . . yes C5 N2 C4 118.73(15) . . yes C5 N2 Co1 108.46(12) . . yes C4 N2 Co1 108.51(11) . . yes C5 N2 H12 105.9 . . yes C4 N2 H12 105.3 . . yes Co1 N2 H12 109.7 . . yes C9 N3 C7 111.94(14) . . yes C9 N3 C6 111.29(14) . . yes C7 N3 C6 111.77(14) . . yes C9 N3 Co1 106.10(11) . . yes C7 N3 Co1 107.06(11) . . yes C6 N3 Co1 108.36(11) . . yes C8 N4 Co1 109.87(11) . . yes C8 N4 H14A 109.8 . . yes Co1 N4 H14A 109.1 . . yes C8 N4 H14B 110.0 . . yes Co1 N4 H14B 108.6 . . yes H14A N4 H14B 109.6 . . yes C10 N5 Co1 111.63(12) . . yes C10 N5 H15A 109.2 . . yes Co1 N5 H15A 108.5 . . yes C10 N5 H15B 109.4 . . yes Co1 N5 H15B 108.9 . . yes H15A N5 H15B 109.2 . . yes O2 C1 O1 123.71(17) . . yes O2 C1 C2 119.87(17) . . yes O1 C1 C2 116.41(15) . . yes N1 C2 C1 107.39(15) . . yes N1 C2 H2A 111.5 . . yes C1 C2 H2A 109.1 . . yes N1 C2 H2B 110.6 . . yes C1 C2 H2B 108.6 . . yes H2A C2 H2B 109.6 . . yes N1 C3 C4 104.51(15) . . yes N1 C3 H3A 111.6 . . yes C4 C3 H3A 109.8 . . yes N1 C3 H3B 111.9 . . yes C4 C3 H3B 110.0 . . yes H3A C3 H3B 108.9 . . yes N2 C4 C3 104.82(14) . . yes N2 C4 H4A 111.6 . . yes C3 C4 H4A 108.6 . . yes N2 C4 H4B 112.7 . . yes C3 C4 H4B 109.5 . . yes H4A C4 H4B 109.4 . . yes N2 C5 C6 105.92(14) . . yes N2 C5 H5A 111.3 . . yes C6 C5 H5A 109.2 . . yes N2 C5 H5B 111.2 . . yes C6 C5 H5B 109.5 . . yes H5A C5 H5B 109.7 . . yes N3 C6 C5 111.17(14) . . yes N3 C6 H6A 108.5 . . yes C5 C6 H6A 109.5 . . yes N3 C6 H6B 108.8 . . yes C5 C6 H6B 110.2 . . yes H6A C6 H6B 108.6 . . yes N3 C7 C8 107.63(14) . . yes N3 C7 H7A 110.3 . . yes C8 C7 H7A 109.9 . . yes N3 C7 H7B 110.2 . . yes C8 C7 H7B 109.6 . . yes H7A C7 H7B 109.2 . . yes N4 C8 C7 107.56(15) . . yes N4 C8 H8A 110.1 . . yes C7 C8 H8A 110.6 . . yes N4 C8 H8B 109.9 . . yes C7 C8 H8B 110.1 . . yes H8A C8 H8B 108.6 . . yes N3 C9 C10 107.54(15) . . yes N3 C9 H9A 111.3 . . yes C10 C9 H9A 109.4 . . yes N3 C9 H9B 110.7 . . yes C10 C9 H9B 108.9 . . yes H9A C9 H9B 109.0 . . yes N5 C10 C9 107.80(15) . . yes N5 C10 H10A 110.4 . . yes C9 C10 H10A 109.1 . . yes N5 C10 H10B 110.4 . . yes C9 C10 H10B 109.3 . . yes H10A C10 H10B 109.9 . . yes N2' Co1' N1' 87.00(7) . . yes N2' Co1' O1' 170.92(7) . . yes N1' Co1' O1' 84.94(6) . . yes N2' Co1' N3' 86.79(7) . . yes N1' Co1' N3' 173.23(7) . . yes O1' Co1' N3' 101.44(6) . . yes N2' Co1' N5' 89.94(7) . . yes N1' Co1' N5' 96.09(7) . . yes O1' Co1' N5' 86.75(6) . . yes N3' Co1' N5' 86.61(7) . . yes N2' Co1' N4' 97.73(7) . . yes N1' Co1' N4' 92.89(7) . . yes O1' Co1' N4' 86.87(6) . . yes N3' Co1' N4' 85.27(7) . . yes N5' Co1' N4' 168.48(7) . . yes C1' O1' Co1' 113.36(11) . . yes C2' N1' C3' 119.58(15) . . yes C2' N1' Co1' 107.99(11) . . yes C3' N1' Co1' 107.91(11) . . yes C2' N1' H11C 105.7 . . yes C3' N1' H11C 106.1 . . yes Co1' N1' H11C 109.3 . . yes C5' N2' C4' 118.99(16) . . yes C5' N2' Co1' 109.05(12) . . yes C4' N2' Co1' 108.82(12) . . yes C5' N2' H12C 105.2 . . yes C4' N2' H12C 104.9 . . yes Co1' N2' H12C 109.5 . . yes C7' N3' C9' 112.06(14) . . yes C7' N3' C6' 111.27(15) . . yes C9' N3' C6' 111.36(14) . . yes C7' N3' Co1' 106.14(11) . . yes C9' N3' Co1' 107.25(11) . . yes C6' N3' Co1' 108.48(11) . . yes C8' N4' Co1' 111.20(12) . . yes C8' N4' H14C 109.6 . . yes Co1' N4' H14C 109.2 . . yes C8' N4' H14D 108.8 . . yes Co1' N4' H14D 108.9 . . yes H14C N4' H14D 109.1 . . yes C10' N5' Co1' 109.52(12) . . yes C10' N5' H15C 109.6 . . yes Co1' N5' H15C 109.8 . . yes C10' N5' H15D 109.2 . . yes Co1' N5' H15D 109.5 . . yes H15C N5' H15D 109.1 . . yes O2' C1' O1' 124.25(18) . . yes O2' C1' C2' 119.88(17) . . yes O1' C1' C2' 115.87(15) . . yes N1' C2' C1' 107.47(15) . . yes N1' C2' H2C 110.7 . . yes C1' C2' H2C 108.9 . . yes N1' C2' H2D 110.9 . . yes C1' C2' H2D 109.2 . . yes H2C C2' H2D 109.6 . . yes N1' C3' C4' 104.36(15) . . yes N1' C3' H3C 113.2 . . yes C4' C3' H3C 110.0 . . yes N1' C3' H3D 112.0 . . yes C4' C3' H3D 108.5 . . yes H3C C3' H3D 108.6 . . yes N2' C4' C3' 104.71(15) . . yes N2' C4' H4C 112.8 . . yes C3' C4' H4C 109.4 . . yes N2' C4' H4D 112.6 . . yes C3' C4' H4D 107.9 . . yes H4C C4' H4D 109.1 . . yes N2' C5' C6' 105.64(16) . . yes N2' C5' H5C 111.7 . . yes C6' C5' H5C 109.4 . . yes N2' C5' H5D 111.2 . . yes C6' C5' H5D 109.6 . . yes H5C C5' H5D 109.3 . . yes N3' C6' C5' 111.45(15) . . yes N3' C6' H6C 108.5 . . yes C5' C6' H6C 109.2 . . yes N3' C6' H6D 108.5 . . yes C5' C6' H6D 109.8 . . yes H6C C6' H6D 109.4 . . yes N3' C7' C8' 107.52(15) . . yes N3' C7' H7C 110.0 . . yes C8' C7' H7C 109.7 . . yes N3' C7' H7D 110.2 . . yes C8' C7' H7D 109.9 . . yes H7C C7' H7D 109.6 . . yes N4' C8' C7' 107.92(15) . . yes N4' C8' H8C 109.9 . . yes C7' C8' H8C 109.1 . . yes N4' C8' H8D 110.6 . . yes C7' C8' H8D 109.8 . . yes H8C C8' H8D 109.5 . . yes N3' C9' C10' 107.41(14) . . yes N3' C9' H9C 110.8 . . yes C10' C9' H9C 109.7 . . yes N3' C9' H9D 110.4 . . yes C10' C9' H9D 109.3 . . yes H9C C9' H9D 109.1 . . yes N5' C10' C9' 108.01(15) . . yes N5' C10' H10C 110.1 . . yes C9' C10' H10C 109.8 . . yes N5' C10' H10D 110.6 . . yes C9' C10' H10D 109.9 . . yes H10C C10' H10D 108.4 . . yes Cl3 Zn1 Cl1 107.07(2) . . yes Cl3 Zn1 Cl2 116.24(2) . . yes Cl1 Zn1 Cl2 109.27(2) . . yes Cl3 Zn1 Cl4 103.47(2) . . yes Cl1 Zn1 Cl4 114.22(3) . . yes Cl2 Zn1 Cl4 106.70(2) . . yes Cl1' Zn1' Cl2' 114.08(2) . . yes Cl1' Zn1' Cl3' 108.81(2) . . yes Cl2' Zn1' Cl3' 108.942(19) . . yes Cl1' Zn1' Cl4' 105.73(2) . . yes Cl2' Zn1' Cl4' 110.86(2) . . yes Cl3' Zn1' Cl4' 108.24(3) . . yes 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 O1 C1 12.1(5) . . . . yes N1 Co1 O1 C1 -15.73(13) . . . . yes N3 Co1 O1 C1 168.24(12) . . . . yes N5 Co1 O1 C1 -107.30(13) . . . . yes N4 Co1 O1 C1 82.50(13) . . . . yes N2 Co1 N1 C2 -148.65(13) . . . . yes O1 Co1 N1 C2 27.18(12) . . . . yes N3 Co1 N1 C2 174.7(5) . . . . yes N5 Co1 N1 C2 114.20(12) . . . . yes N4 Co1 N1 C2 -58.86(13) . . . . yes N2 Co1 N1 C3 -17.92(13) . . . . yes O1 Co1 N1 C3 157.90(13) . . . . yes N3 Co1 N1 C3 -54.5(6) . . . . yes N5 Co1 N1 C3 -115.07(13) . . . . yes N4 Co1 N1 C3 71.86(13) . . . . yes N1 Co1 N2 C5 -144.06(12) . . . . yes O1 Co1 N2 C5 -171.8(4) . . . . yes N3 Co1 N2 C5 31.61(12) . . . . yes N5 Co1 N2 C5 -53.09(12) . . . . yes N4 Co1 N2 C5 118.05(12) . . . . yes N1 Co1 N2 C4 -13.81(12) . . . . yes O1 Co1 N2 C4 -41.5(5) . . . . yes N3 Co1 N2 C4 161.86(13) . . . . yes N5 Co1 N2 C4 77.16(13) . . . . yes N4 Co1 N2 C4 -111.71(12) . . . . yes N2 Co1 N3 C9 -127.72(12) . . . . yes N1 Co1 N3 C9 -91.1(5) . . . . yes O1 Co1 N3 C9 55.90(12) . . . . yes N5 Co1 N3 C9 -30.21(12) . . . . yes N4 Co1 N3 C9 141.92(12) . . . . yes N2 Co1 N3 C7 112.59(12) . . . . yes N1 Co1 N3 C7 149.2(5) . . . . yes O1 Co1 N3 C7 -63.79(12) . . . . yes N5 Co1 N3 C7 -149.91(12) . . . . yes N4 Co1 N3 C7 22.23(12) . . . . yes N2 Co1 N3 C6 -8.12(12) . . . . yes N1 Co1 N3 C6 28.5(6) . . . . yes O1 Co1 N3 C6 175.50(11) . . . . yes N5 Co1 N3 C6 89.39(12) . . . . yes N4 Co1 N3 C6 -98.48(12) . . . . yes N2 Co1 N4 C8 -82.12(12) . . . . yes N1 Co1 N4 C8 -169.28(12) . . . . yes O1 Co1 N4 C8 106.33(12) . . . . yes N3 Co1 N4 C8 4.86(12) . . . . yes N5 Co1 N4 C8 47.9(4) . . . . yes N2 Co1 N5 C10 91.76(13) . . . . yes N1 Co1 N5 C10 179.07(13) . . . . yes O1 Co1 N5 C10 -96.11(13) . . . . yes N3 Co1 N5 C10 5.42(13) . . . . yes N4 Co1 N5 C10 -37.7(4) . . . . yes Co1 O1 C1 O2 -178.82(15) . . . . yes Co1 O1 C1 C2 0.0(2) . . . . yes C3 N1 C2 C1 -155.98(15) . . . . yes Co1 N1 C2 C1 -32.20(17) . . . . yes O2 C1 C2 N1 -159.43(17) . . . . yes O1 C1 C2 N1 21.7(2) . . . . yes C2 N1 C3 C4 168.71(15) . . . . yes Co1 N1 C3 C4 44.60(16) . . . . yes C5 N2 C4 C3 165.83(16) . . . . yes Co1 N2 C4 C3 41.48(16) . . . . yes N1 C3 C4 N2 -55.70(18) . . . . yes C4 N2 C5 C6 -170.76(15) . . . . yes Co1 N2 C5 C6 -46.39(17) . . . . yes C9 N3 C6 C5 100.04(18) . . . . yes C7 N3 C6 C5 -133.99(16) . . . . yes Co1 N3 C6 C5 -16.24(18) . . . . yes N2 C5 C6 N3 40.5(2) . . . . yes C9 N3 C7 C8 -160.53(15) . . . . yes C6 N3 C7 C8 73.86(18) . . . . yes Co1 N3 C7 C8 -44.66(16) . . . . yes Co1 N4 C8 C7 -30.55(17) . . . . yes N3 C7 C8 N4 49.34(19) . . . . yes C7 N3 C9 C10 165.60(15) . . . . yes C6 N3 C9 C10 -68.52(19) . . . . yes Co1 N3 C9 C10 49.15(17) . . . . yes Co1 N5 C10 C9 20.55(19) . . . . yes N3 C9 C10 N5 -45.3(2) . . . . yes N2' Co1' O1' C1' -12.0(5) . . . . yes N1' Co1' O1' C1' 15.62(12) . . . . yes N3' Co1' O1' C1' -166.67(12) . . . . yes N5' Co1' O1' C1' -80.79(13) . . . . yes N4' Co1' O1' C1' 108.81(13) . . . . yes N2' Co1' N1' C2' 148.10(13) . . . . yes O1' Co1' N1' C2' -27.70(12) . . . . yes N3' Co1' N1' C2' 171.7(5) . . . . yes N5' Co1' N1' C2' 58.48(13) . . . . yes N4' Co1' N1' C2' -114.30(12) . . . . yes N2' Co1' N1' C3' 17.53(13) . . . . yes O1' Co1' N1' C3' -158.27(12) . . . . yes N3' Co1' N1' C3' 41.1(6) . . . . yes N5' Co1' N1' C3' -72.09(13) . . . . yes N4' Co1' N1' C3' 115.13(12) . . . . yes N1' Co1' N2' C5' 145.63(13) . . . . yes O1' Co1' N2' C5' 173.1(4) . . . . yes N3' Co1' N2' C5' -31.66(13) . . . . yes N5' Co1' N2' C5' -118.27(13) . . . . yes N4' Co1' N2' C5' 53.12(14) . . . . yes N1' Co1' N2' C4' 14.39(13) . . . . yes O1' Co1' N2' C4' 41.9(5) . . . . yes N3' Co1' N2' C4' -162.91(13) . . . . yes N5' Co1' N2' C4' 110.49(13) . . . . yes N4' Co1' N2' C4' -78.13(14) . . . . yes N2' Co1' N3' C7' 128.03(12) . . . . yes N1' Co1' N3' C7' 104.4(6) . . . . yes O1' Co1' N3' C7' -55.85(12) . . . . yes N5' Co1' N3' C7' -141.84(12) . . . . yes N4' Co1' N3' C7' 29.99(12) . . . . yes N2' Co1' N3' C9' -112.02(12) . . . . yes N1' Co1' N3' C9' -135.6(5) . . . . yes O1' Co1' N3' C9' 64.10(12) . . . . yes N5' Co1' N3' C9' -21.89(12) . . . . yes N4' Co1' N3' C9' 149.94(12) . . . . yes N2' Co1' N3' C6' 8.36(12) . . . . yes N1' Co1' N3' C6' -15.2(6) . . . . yes O1' Co1' N3' C6' -175.51(11) . . . . yes N5' Co1' N3' C6' 98.49(12) . . . . yes N4' Co1' N3' C6' -89.68(12) . . . . yes N2' Co1' N4' C8' -90.96(13) . . . . yes N1' Co1' N4' C8' -178.33(13) . . . . yes O1' Co1' N4' C8' 96.91(13) . . . . yes N3' Co1' N4' C8' -4.85(13) . . . . yes N5' Co1' N4' C8' 40.4(4) . . . . yes N2' Co1' N5' C10' 81.70(13) . . . . yes N1' Co1' N5' C10' 168.68(12) . . . . yes O1' Co1' N5' C10' -106.77(12) . . . . yes N3' Co1' N5' C10' -5.10(12) . . . . yes N4' Co1' N5' C10' -50.3(4) . . . . yes Co1' O1' C1' O2' 179.86(15) . . . . yes Co1' O1' C1' C2' 0.87(19) . . . . yes C3' N1' C2' C1' 157.12(15) . . . . yes Co1' N1' C2' C1' 33.34(16) . . . . yes O2' C1' C2' N1' 157.95(17) . . . . yes O1' C1' C2' N1' -23.0(2) . . . . yes C2' N1' C3' C4' -167.90(15) . . . . yes Co1' N1' C3' C4' -44.07(16) . . . . yes C5' N2' C4' C3' -167.46(17) . . . . yes Co1' N2' C4' C3' -41.80(17) . . . . yes N1' C3' C4' N2' 55.48(18) . . . . yes C4' N2' C5' C6' 171.41(16) . . . . yes Co1' N2' C5' C6' 45.87(18) . . . . yes C7' N3' C6' C5' -100.79(18) . . . . yes C9' N3' C6' C5' 133.41(16) . . . . yes Co1' N3' C6' C5' 15.62(18) . . . . yes N2' C5' C6' N3' -39.6(2) . . . . yes C9' N3' C7' C8' -165.91(15) . . . . yes C6' N3' C7' C8' 68.68(19) . . . . yes Co1' N3' C7' C8' -49.15(17) . . . . yes Co1' N4' C8' C7' -21.15(19) . . . . yes N3' C7' C8' N4' 45.8(2) . . . . yes C7' N3' C9' C10' 160.27(15) . . . . yes C6' N3' C9' C10' -74.37(18) . . . . yes Co1' N3' C9' C10' 44.17(17) . . . . yes Co1' N5' C10' C9' 30.79(17) . . . . yes N3' C9' C10' N5' -49.21(19) . . . . yes _diffrn_measured_fraction_theta_max .999 _diffrn_reflns_theta_full 35.00 _diffrn_measured_fraction_theta_full .999 _refine_diff_density_max .820 _refine_diff_density_min -.666 _refine_diff_density_rms .083 data_p-6 _database_code_depnum_ccdc_archive 'CCDC 255279' _audit_creation_method maXus _chemical_compound_source 'Local laboratory' _exptl_crystal_description Cube _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.25 _exptl_crystal_F_000 1040 _cell_measurement_temperature 122.4(5) _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _computing_data_collection KappaCCD _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.00805 _diffrn_orient_matrix_UB_12 -0.09164 _diffrn_orient_matrix_UB_13 0.07029 _diffrn_orient_matrix_UB_21 0.08415 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 -0.00964 _diffrn_orient_matrix_UB_31 0.00500 _diffrn_orient_matrix_UB_32 0.03394 _diffrn_orient_matrix_UB_33 0.04368 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _chemical_formula_weight 512.450 _diffrn_radiation_type ' MoK\a' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z '-X,-Y,+Z+ 1/2' '-X+ 1/2,+Y+ 1/2,+Z+ 1/2' '+X+ 1/2,-Y+ 1/2,+Z' _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_space_group_name_Hall 'P 2c -2n ' _symmetry_cell_setting Orthorhombic _chemical_formula_moiety 'C10 H24 Co N5 O2 2+, Cl4 Zn 2-' _chemical_formula_sum 'C10 H24 Cl4 Co N5 O2 Zn ' _chemical_name_common 'p-(Co(tren-engly)) ZnCl4' _cell_length_a 18.0055(7) _cell_length_b 11.8078(7) _cell_length_c 8.6392(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1836.74(16) _diffrn_reflns_number 55837 _diffrn_reflns_theta_max 40.00 _diffrn_reflns_av_R_equivalents 0.034 _cell_measurement_reflns_used 3599 _cell_measurement_theta_min 0.626 _cell_measurement_theta_max 20.362 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 -1 0.180 -1 0 2 0.170 0 1 1 0.120 1 -1 0 0.160 -1 1 0 0.190 -1 -1 0 0.190 1 1 0 0.190 0 -1 1 0.090 0 -1 -1 0.200 0 0 -1 0.140 1 0 2 0.170 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.421 _exptl_absorpt_correction_T_max 0.561 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co .3494 .9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 10073 _reflns_number_gt 9859 _reflns_threshold_expression >2sigma(I) _exptl_absorpt_coefficient_mu 2.804 _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^)+(0.0308P)^2^+0.8862P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.014(5) _refine_ls_number_reflns 10073 _refine_ls_number_parameters 208 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.109761(8) 0.222835(12) 0.196317(19) 0.00826(2) Uani 1 1 d . . . O1 O 0.07459(5) 0.12658(8) 0.35690(11) 0.01127(12) Uani 1 1 d . . . O2 O 0.06696(6) 0.11870(9) 0.61418(12) 0.01727(16) Uani 1 1 d . . . N1 N 0.18988(6) 0.25917(9) 0.34486(13) 0.01330(16) Uani 1 1 d . . . H11 H 0.2031 0.3377 0.3390 0.016 Uiso 1 1 d R . . N2 N 0.17189(6) 0.09876(9) 0.12422(14) 0.01448(16) Uani 1 1 d . . . H12 H 0.1964 0.1180 0.0290 0.017 Uiso 1 1 d R . . N3 N 0.03566(5) 0.17002(9) 0.04971(12) 0.01068(14) Uani 1 1 d . . . N4 N 0.02942(6) 0.32638(9) 0.26227(13) 0.01264(15) Uani 1 1 d . . . H14A H 0.0375 0.3492 0.3675 0.015 Uiso 1 1 d R . . H14B H 0.0292 0.3920 0.1967 0.015 Uiso 1 1 d R . . N5 N 0.14369(6) 0.32675(9) 0.03473(13) 0.01277(15) Uani 1 1 d . . . H15A H 0.1324 0.4032 0.0644 0.015 Uiso 1 1 d R . . H15B H 0.1964 0.3189 0.0217 0.015 Uiso 1 1 d R . . C1 C 0.09665(6) 0.15312(9) 0.49599(14) 0.01132(15) Uani 1 1 d . . . C2 C 0.16271(7) 0.23273(11) 0.50280(15) 0.01439(18) Uani 1 1 d . . . H2A H 0.1485 0.3020 0.5529 0.017 Uiso 1 1 d R . . H2B H 0.2021 0.1975 0.5602 0.017 Uiso 1 1 d R . . C3 C 0.25580(7) 0.18992(13) 0.2994(2) 0.0195(2) Uani 1 1 d . . . H3A H 0.2884 0.1806 0.3864 0.023 Uiso 1 1 d R . . H3B H 0.2821 0.2264 0.2166 0.023 Uiso 1 1 d R . . C4 C 0.22841(8) 0.07482(13) 0.24537(19) 0.0190(2) Uani 1 1 d . . . H4A H 0.2694 0.0324 0.2044 0.023 Uiso 1 1 d R . . H4B H 0.2073 0.0347 0.3314 0.023 Uiso 1 1 d R . . C5 C 0.11891(9) 0.00585(11) 0.08660(17) 0.0172(2) Uani 1 1 d . . . H5A H 0.1448 -0.0545 0.0351 0.021 Uiso 1 1 d R . . H5B H 0.0971 -0.0225 0.1805 0.021 Uiso 1 1 d R . . C6 C 0.06053(8) 0.05827(11) -0.01773(15) 0.01532(18) Uani 1 1 d . . . H6A H 0.0187 0.0083 -0.0258 0.018 Uiso 1 1 d R . . H6B H 0.0813 0.0707 -0.1186 0.018 Uiso 1 1 d R . . C7 C -0.03516(6) 0.16025(11) 0.13819(15) 0.01425(18) Uani 1 1 d . . . H7A H -0.0764 0.1585 0.0678 0.017 Uiso 1 1 d R . . H7B H -0.0345 0.0918 0.1982 0.017 Uiso 1 1 d R . . C8 C -0.04284(7) 0.26283(11) 0.24735(17) 0.01528(18) Uani 1 1 d . . . H8A H -0.0579 0.2360 0.3476 0.018 Uiso 1 1 d R . . H8B H -0.0803 0.3122 0.2065 0.018 Uiso 1 1 d R . . C9 C 0.02839(7) 0.25729(11) -0.07528(14) 0.01339(17) Uani 1 1 d . . . H9A H 0.0059 0.2236 -0.1649 0.016 Uiso 1 1 d R . . H9B H -0.0021 0.3184 -0.0390 0.016 Uiso 1 1 d R . . C10 C 0.10556(7) 0.29967(11) -0.11398(15) 0.01441(18) Uani 1 1 d . . . H10A H 0.1026 0.3667 -0.1766 0.017 Uiso 1 1 d R . . H10B H 0.1331 0.2425 -0.1683 0.017 Uiso 1 1 d R . . Zn1 Zn 0.162019(8) 0.600287(13) 0.30131(2) 0.01387(3) Uani 1 1 d . . . Cl1 Cl 0.266944(17) 0.49853(3) 0.24777(5) 0.01924(5) Uani 1 1 d . . . Cl2 Cl 0.107322(18) 0.51316(3) 0.50767(4) 0.01707(5) Uani 1 1 d . . . Cl3 Cl 0.08398(2) 0.58916(3) 0.09623(5) 0.01992(6) Uani 1 1 d . . . Cl4 Cl 0.19588(2) 0.77818(3) 0.36476(5) 0.02042(6) 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 0.00916(5) 0.00904(5) 0.00659(5) 0.00098(4) 0.00026(4) -0.00069(4) O1 0.0143(3) 0.0119(3) 0.0076(3) 0.0008(2) 0.0003(2) -0.0026(2) O2 0.0232(4) 0.0202(4) 0.0085(3) 0.0015(3) 0.0022(3) -0.0055(3) N1 0.0134(4) 0.0145(4) 0.0120(4) 0.0044(3) -0.0022(3) -0.0038(3) N2 0.0154(4) 0.0157(4) 0.0123(4) 0.0015(3) 0.0032(3) 0.0032(3) N3 0.0122(3) 0.0122(3) 0.0077(3) -0.0006(3) 0.0010(3) -0.0013(3) N4 0.0156(4) 0.0118(3) 0.0105(4) -0.0011(3) 0.0001(3) 0.0009(3) N5 0.0144(3) 0.0139(4) 0.0099(4) 0.0017(3) 0.0008(3) -0.0019(3) C1 0.0144(4) 0.0107(4) 0.0089(4) 0.0012(3) -0.0001(3) -0.0006(3) C2 0.0178(4) 0.0152(4) 0.0101(4) 0.0024(4) -0.0038(3) -0.0046(3) C3 0.0110(4) 0.0275(6) 0.0200(5) 0.0069(5) -0.0009(4) -0.0003(4) C4 0.0161(4) 0.0221(5) 0.0187(5) 0.0053(5) 0.0020(4) 0.0082(4) C5 0.0266(6) 0.0117(4) 0.0132(5) -0.0008(4) 0.0030(4) 0.0023(4) C6 0.0212(5) 0.0136(4) 0.0111(4) -0.0035(3) 0.0023(4) -0.0025(4) C7 0.0114(4) 0.0200(5) 0.0113(4) -0.0011(4) 0.0007(3) -0.0041(3) C8 0.0125(4) 0.0193(5) 0.0141(5) -0.0004(4) 0.0030(3) 0.0016(3) C9 0.0151(4) 0.0165(4) 0.0086(4) 0.0013(3) -0.0016(3) -0.0003(3) C10 0.0183(4) 0.0166(4) 0.0083(4) 0.0022(4) 0.0011(3) -0.0020(4) Zn1 0.01353(5) 0.01352(5) 0.01456(6) 0.00007(5) -0.00260(5) -0.00295(4) Cl1 0.01367(10) 0.01655(11) 0.02750(15) 0.00339(11) 0.00228(10) -0.00183(9) Cl2 0.01999(12) 0.01493(11) 0.01629(13) 0.00101(10) 0.00065(9) -0.00203(9) Cl3 0.02347(13) 0.01766(11) 0.01863(14) 0.00126(10) -0.00919(11) -0.00177(10) Cl4 0.01955(12) 0.01488(11) 0.02683(16) -0.00333(11) -0.00300(11) -0.00500(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 O1 1.9019(9) . yes Co1 N3 1.9425(10) . yes Co1 N2 1.9457(11) . yes Co1 N5 1.9564(11) . yes Co1 N1 1.9779(11) . yes Co1 N4 1.9779(10) . yes O1 C1 1.3038(15) . yes O2 C1 1.2222(15) . yes N1 C2 1.4827(17) . yes N1 C3 1.4939(18) . yes N1 H11 0.9589 . yes N2 C4 1.4870(19) . yes N2 C5 1.4896(19) . yes N2 H12 0.9609 . yes N3 C7 1.4911(15) . yes N3 C9 1.4983(16) . yes N3 C6 1.5103(16) . yes N4 C8 1.5075(16) . yes N4 H14A 0.9591 . yes N4 H14B 0.9604 . yes N5 C10 1.4914(17) . yes N5 H15A 0.9606 . yes N5 H15B 0.9595 . yes C1 C2 1.5172(16) . yes C2 H2A 0.9600 . yes C2 H2B 0.9600 . yes C3 C4 1.519(2) . yes C3 H3A 0.9600 . yes C3 H3B 0.9600 . yes C4 H4A 0.9601 . yes C4 H4B 0.9599 . yes C5 C6 1.517(2) . yes C5 H5A 0.9609 . yes C5 H5B 0.9610 . yes C6 H6A 0.9601 . yes C6 H6B 0.9595 . yes C7 C8 1.5414(19) . yes C7 H7A 0.9606 . yes C7 H7B 0.9604 . yes C8 H8A 0.9605 . yes C8 H8B 0.9588 . yes C9 C10 1.5144(18) . yes C9 H9A 0.9603 . yes C9 H9B 0.9592 . yes C10 H10A 0.9597 . yes C10 H10B 0.9604 . yes Zn1 Cl4 2.2548(3) . yes Zn1 Cl3 2.2651(4) . yes Zn1 Cl2 2.2818(4) . yes Zn1 Cl1 2.2863(4) . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N3 93.15(4) . . yes O1 Co1 N2 88.57(4) . . yes N3 Co1 N2 86.82(5) . . yes O1 Co1 N5 177.74(4) . . yes N3 Co1 N5 87.17(4) . . yes N2 Co1 N5 93.69(5) . . yes O1 Co1 N1 84.22(4) . . yes N3 Co1 N1 173.55(5) . . yes N2 Co1 N1 87.23(5) . . yes N5 Co1 N1 95.69(4) . . yes O1 Co1 N4 85.16(4) . . yes N3 Co1 N4 83.33(4) . . yes N2 Co1 N4 168.00(5) . . yes N5 Co1 N4 92.65(5) . . yes N1 Co1 N4 102.27(5) . . yes C1 O1 Co1 115.28(7) . . yes C2 N1 C3 112.88(11) . . yes C2 N1 Co1 108.10(7) . . yes C3 N1 Co1 106.87(9) . . yes C2 N1 H11 109.5 . . yes C3 N1 H11 108.6 . . yes Co1 N1 H11 110.9 . . yes C4 N2 C5 116.87(11) . . yes C4 N2 Co1 108.14(9) . . yes C5 N2 Co1 104.85(8) . . yes C4 N2 H12 109.4 . . yes C5 N2 H12 106.4 . . yes Co1 N2 H12 111.1 . . yes C7 N3 C9 110.36(10) . . yes C7 N3 C6 112.56(10) . . yes C9 N3 C6 110.41(10) . . yes C7 N3 Co1 106.14(7) . . yes C9 N3 Co1 108.01(7) . . yes C6 N3 Co1 109.17(8) . . yes C8 N4 Co1 107.40(7) . . yes C8 N4 H14A 110.6 . . yes Co1 N4 H14A 109.6 . . yes C8 N4 H14B 110.4 . . yes Co1 N4 H14B 109.4 . . yes H14A N4 H14B 109.4 . . yes C10 N5 Co1 109.66(8) . . yes C10 N5 H15A 109.5 . . yes Co1 N5 H15A 109.4 . . yes C10 N5 H15B 109.5 . . yes Co1 N5 H15B 109.4 . . yes H15A N5 H15B 109.4 . . yes O2 C1 O1 123.83(11) . . yes O2 C1 C2 121.10(11) . . yes O1 C1 C2 115.06(10) . . yes N1 C2 C1 110.69(10) . . yes N1 C2 H2A 108.9 . . yes C1 C2 H2A 109.6 . . yes N1 C2 H2B 108.8 . . yes C1 C2 H2B 109.3 . . yes H2A C2 H2B 109.5 . . yes N1 C3 C4 108.21(10) . . yes N1 C3 H3A 110.0 . . yes C4 C3 H3A 109.7 . . yes N1 C3 H3B 110.0 . . yes C4 C3 H3B 109.4 . . yes H3A C3 H3B 109.5 . . yes N2 C4 C3 105.57(11) . . yes N2 C4 H4A 111.5 . . yes C3 C4 H4A 109.3 . . yes N2 C4 H4B 111.5 . . yes C3 C4 H4B 109.4 . . yes H4A C4 H4B 109.5 . . yes N2 C5 C6 105.84(10) . . yes N2 C5 H5A 109.6 . . yes C6 C5 H5A 111.4 . . yes N2 C5 H5B 109.5 . . yes C6 C5 H5B 111.2 . . yes H5A C5 H5B 109.3 . . yes N3 C6 C5 109.44(10) . . yes N3 C6 H6A 109.4 . . yes C5 C6 H6A 109.7 . . yes N3 C6 H6B 109.4 . . yes C5 C6 H6B 109.4 . . yes H6A C6 H6B 109.5 . . yes N3 C7 C8 109.24(10) . . yes N3 C7 H7A 109.8 . . yes C8 C7 H7A 109.6 . . yes N3 C7 H7B 109.4 . . yes C8 C7 H7B 109.4 . . yes H7A C7 H7B 109.4 . . yes N4 C8 C7 111.47(9) . . yes N4 C8 H8A 109.3 . . yes C7 C8 H8A 108.5 . . yes N4 C8 H8B 109.6 . . yes C7 C8 H8B 108.4 . . yes H8A C8 H8B 109.6 . . yes N3 C9 C10 107.83(10) . . yes N3 C9 H9A 109.4 . . yes C10 C9 H9A 110.3 . . yes N3 C9 H9B 109.4 . . yes C10 C9 H9B 110.5 . . yes H9A C9 H9B 109.5 . . yes N5 C10 C9 107.64(10) . . yes N5 C10 H10A 109.5 . . yes C9 C10 H10A 110.2 . . yes N5 C10 H10B 109.5 . . yes C9 C10 H10B 110.4 . . yes H10A C10 H10B 109.5 . . yes Cl4 Zn1 Cl3 114.325(15) . . yes Cl4 Zn1 Cl2 110.292(16) . . yes Cl3 Zn1 Cl2 108.493(15) . . yes Cl4 Zn1 Cl1 108.380(14) . . yes Cl3 Zn1 Cl1 108.899(16) . . yes Cl2 Zn1 Cl1 106.128(14) . . yes 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 O1 C1 -163.12(9) . . . . yes N2 Co1 O1 C1 110.15(9) . . . . yes N5 Co1 O1 C1 -65.0(11) . . . . yes N1 Co1 O1 C1 22.79(9) . . . . yes N4 Co1 O1 C1 -80.09(9) . . . . yes O1 Co1 N1 C2 -22.20(8) . . . . yes N3 Co1 N1 C2 -88.4(4) . . . . yes N2 Co1 N1 C2 -111.03(9) . . . . yes N5 Co1 N1 C2 155.53(8) . . . . yes N4 Co1 N1 C2 61.56(9) . . . . yes O1 Co1 N1 C3 99.58(8) . . . . yes N3 Co1 N1 C3 33.4(4) . . . . yes N2 Co1 N1 C3 10.74(8) . . . . yes N5 Co1 N1 C3 -82.69(9) . . . . yes N4 Co1 N1 C3 -176.66(8) . . . . yes O1 Co1 N2 C4 -65.68(9) . . . . yes N3 Co1 N2 C4 -158.92(9) . . . . yes N5 Co1 N2 C4 114.13(9) . . . . yes N1 Co1 N2 C4 18.60(9) . . . . yes N4 Co1 N2 C4 -124.1(2) . . . . yes O1 Co1 N2 C5 59.68(9) . . . . yes N3 Co1 N2 C5 -33.55(8) . . . . yes N5 Co1 N2 C5 -120.51(9) . . . . yes N1 Co1 N2 C5 143.96(9) . . . . yes N4 Co1 N2 C5 1.2(3) . . . . yes O1 Co1 N3 C7 41.33(8) . . . . yes N2 Co1 N3 C7 129.72(8) . . . . yes N5 Co1 N3 C7 -136.42(8) . . . . yes N1 Co1 N3 C7 107.1(4) . . . . yes N4 Co1 N3 C7 -43.42(8) . . . . yes O1 Co1 N3 C9 159.69(8) . . . . yes N2 Co1 N3 C9 -111.93(8) . . . . yes N5 Co1 N3 C9 -18.07(8) . . . . yes N1 Co1 N3 C9 -134.6(4) . . . . yes N4 Co1 N3 C9 74.93(8) . . . . yes O1 Co1 N3 C6 -80.23(8) . . . . yes N2 Co1 N3 C6 8.16(8) . . . . yes N5 Co1 N3 C6 102.01(8) . . . . yes N1 Co1 N3 C6 -14.5(4) . . . . yes N4 Co1 N3 C6 -164.98(8) . . . . yes O1 Co1 N4 C8 -58.47(8) . . . . yes N3 Co1 N4 C8 35.29(8) . . . . yes N2 Co1 N4 C8 0.3(3) . . . . yes N5 Co1 N4 C8 122.12(8) . . . . yes N1 Co1 N4 C8 -141.47(8) . . . . yes O1 Co1 N5 C10 -106.8(11) . . . . yes N3 Co1 N5 C10 -8.55(8) . . . . yes N2 Co1 N5 C10 78.07(9) . . . . yes N1 Co1 N5 C10 165.65(8) . . . . yes N4 Co1 N5 C10 -91.74(9) . . . . yes Co1 O1 C1 O2 162.41(10) . . . . yes Co1 O1 C1 C2 -16.84(13) . . . . yes C3 N1 C2 C1 -99.08(12) . . . . yes Co1 N1 C2 C1 18.91(12) . . . . yes O2 C1 C2 N1 178.28(12) . . . . yes O1 C1 C2 N1 -2.45(15) . . . . yes C2 N1 C3 C4 81.18(14) . . . . yes Co1 N1 C3 C4 -37.53(13) . . . . yes C5 N2 C4 C3 -160.97(11) . . . . yes Co1 N2 C4 C3 -43.06(12) . . . . yes N1 C3 C4 N2 53.31(14) . . . . yes C4 N2 C5 C6 170.67(11) . . . . yes Co1 N2 C5 C6 50.98(11) . . . . yes C7 N3 C6 C5 -98.51(12) . . . . yes C9 N3 C6 C5 137.67(11) . . . . yes Co1 N3 C6 C5 19.08(12) . . . . yes N2 C5 C6 N3 -46.14(13) . . . . yes C9 N3 C7 C8 -75.47(12) . . . . yes C6 N3 C7 C8 160.68(10) . . . . yes Co1 N3 C7 C8 41.31(11) . . . . yes Co1 N4 C8 C7 -19.50(12) . . . . yes N3 C7 C8 N4 -13.77(14) . . . . yes C7 N3 C9 C10 156.26(10) . . . . yes C6 N3 C9 C10 -78.67(12) . . . . yes Co1 N3 C9 C10 40.63(11) . . . . yes Co1 N5 C10 C9 32.93(12) . . . . yes N3 C9 C10 N5 -48.06(13) . . . . yes _diffrn_measured_fraction_theta_max .997 _diffrn_reflns_theta_full 39.99 _diffrn_measured_fraction_theta_full .997 _refine_diff_density_max .963 _refine_diff_density_min -.846 _refine_diff_density_rms .094 data_t-6 _database_code_depnum_ccdc_archive 'CCDC 255280' _audit_creation_method maXus _chemical_compound_source 'Local laboratory' _exptl_crystal_description Cube _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_F_000 432 _cell_measurement_temperature 122.4(5) _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _computing_data_collection KappaCCD _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _chemical_formula_weight 412.204 _diffrn_radiation_type ' MoK\a' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' _symmetry_cell_setting Triclinic _chemical_formula_moiety 'C10 H24 Co N5 O2 2+, 2(Cl 1-), 2(H2 O) ' _chemical_formula_sum 'C10 H28 Cl2 Co N5 O4 ' _chemical_name_common 't-(Co(tren-engly)) Cl2 2(H2O)' _cell_length_a 8.8197(7) _cell_length_b 8.8710(11) _cell_length_c 11.3494(12) _cell_angle_alpha 80.102(7) _cell_angle_beta 89.441(10) _cell_angle_gamma 69.214(8) _cell_volume 816.55(15) _diffrn_reflns_number 52142 _diffrn_reflns_theta_max 34.99 _diffrn_reflns_av_R_equivalents 0.040 _cell_measurement_reflns_used 337 _cell_measurement_theta_min 0.838 _cell_measurement_theta_max 20.362 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 1 0.110 0 -1 -1 0.090 1 0 0 0.090 -1 -1 1 0.140 -1 0 -1 0.130 1 1 0 0.150 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.788 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; 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' 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' 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' _reflns_number_total 7165 _reflns_number_gt 6928 _reflns_threshold_expression >2sigma(I) _exptl_absorpt_coefficient_mu 1.403 _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^+0.7233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7165 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _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 C1 C -0.15292(14) 0.25719(15) 0.63444(11) 0.01333(18) Uani 1 1 d . . . C2 C -0.09702(15) 0.11074(15) 0.73481(12) 0.01505(19) Uani 1 1 d . . . H2A H -0.1178 0.0230 0.7115 0.018 Uiso 1 1 d R . . H2B H -0.1445 0.1395 0.8055 0.018 Uiso 1 1 d R . . C3 C 0.17115(16) -0.07472(14) 0.69109(11) 0.01501(19) Uani 1 1 d . . . H3A H 0.2723 -0.1449 0.7339 0.018 Uiso 1 1 d R . . H3B H 0.1068 -0.1384 0.6796 0.018 Uiso 1 1 d R . . C4 C 0.20496(16) 0.00785(15) 0.57151(11) 0.01497(19) Uani 1 1 d . . . H4A H 0.1110 0.0621 0.5221 0.018 Uiso 1 1 d R . . H4B H 0.2830 -0.0711 0.5314 0.018 Uiso 1 1 d R . . C5 C 0.44831(14) 0.05243(16) 0.64495(11) 0.0161(2) Uani 1 1 d . . . H5A H 0.4978 -0.0557 0.6265 0.019 Uiso 1 1 d R . . H5B H 0.5150 0.1182 0.6097 0.019 Uiso 1 1 d R . . C6 C 0.45556(15) 0.04147(15) 0.78028(11) 0.0163(2) Uani 1 1 d . . . H6A H 0.5686 0.0245 0.8091 0.020 Uiso 1 1 d R . . H6B H 0.4275 -0.0471 0.8186 0.020 Uiso 1 1 d R . . C7 C 0.29606(17) 0.18434(16) 0.93576(11) 0.0176(2) Uani 1 1 d . . . H7A H 0.2832 0.0844 0.9597 0.021 Uiso 1 1 d R . . H7B H 0.3937 0.1835 0.9856 0.021 Uiso 1 1 d R . . C8 C 0.14343(17) 0.32946(16) 0.94719(11) 0.0172(2) Uani 1 1 d . . . H8A H 0.1849 0.4263 0.9443 0.021 Uiso 1 1 d R . . H8B H 0.1074 0.3086 1.0211 0.021 Uiso 1 1 d R . . C9 C 0.41306(15) 0.33058(16) 0.77520(13) 0.0171(2) Uani 1 1 d . . . H9A H 0.4745 0.3450 0.8457 0.021 Uiso 1 1 d R . . H9B H 0.5054 0.2985 0.7184 0.021 Uiso 1 1 d R . . C10 C 0.28418(15) 0.49264(15) 0.71947(12) 0.01542(19) Uani 1 1 d . . . H10A H 0.3498 0.5620 0.6722 0.019 Uiso 1 1 d R . . H10B H 0.2410 0.5474 0.7803 0.019 Uiso 1 1 d R . . N1 N 0.08146(13) 0.05548(12) 0.76084(9) 0.01229(16) Uani 1 1 d . . . H11 H 0.1111 0.0124 0.8448 0.015 Uiso 1 1 d R . . N2 N 0.27544(12) 0.12969(12) 0.59499(9) 0.01172(15) Uani 1 1 d . . . H12 H 0.2815 0.2023 0.5214 0.014 Uiso 1 1 d R . . N3 N 0.34011(12) 0.19920(12) 0.80801(9) 0.01269(16) Uani 1 1 d . . . N4 N 0.02710(13) 0.35519(12) 0.84360(9) 0.01271(16) Uani 1 1 d . . . H14A H -0.0119 0.4708 0.8168 0.015 Uiso 1 1 d R . . H14B H -0.0388 0.3061 0.8710 0.015 Uiso 1 1 d R . . N5 N 0.17346(12) 0.45589(12) 0.64091(9) 0.01224(15) Uani 1 1 d . . . H15A H 0.2336 0.4451 0.5646 0.015 Uiso 1 1 d R . . H15B H 0.0874 0.5454 0.6305 0.015 Uiso 1 1 d R . . O1 O -0.05192(10) 0.33209(11) 0.60900(8) 0.01193(14) Uani 1 1 d . . . O2 O -0.28913(12) 0.30211(14) 0.58390(11) 0.02141(19) Uani 1 1 d . . . O3 O 0.40648(17) 0.35207(16) 0.42362(14) 0.0320(3) Uani 1 1 d . . . O4 O 0.4402(4) 0.3982(4) 1.1094(4) 0.0700(9) Uani 0.708(5) 1 d P . . O5 O 0.3950(11) 0.4325(11) 0.2073(9) 0.0700(9) Uani 0.292(5) 1 d P . . Cl1 Cl 0.14884(4) 0.26541(4) 0.28778(3) 0.01779(6) Uani 1 1 d . . . Cl2 Cl 0.22543(5) -0.22835(5) 0.99155(3) 0.02906(9) Uani 1 1 d . . . Co1 Co 0.140602(17) 0.255109(17) 0.710069(12) 0.00768(4) 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 C1 0.0124(4) 0.0140(4) 0.0155(4) -0.0062(4) 0.0016(3) -0.0055(3) C2 0.0153(4) 0.0131(4) 0.0193(5) -0.0039(4) 0.0048(4) -0.0078(4) C3 0.0186(5) 0.0093(4) 0.0172(5) -0.0039(3) 0.0030(4) -0.0044(4) C4 0.0182(5) 0.0145(4) 0.0134(4) -0.0065(4) 0.0023(4) -0.0056(4) C5 0.0112(4) 0.0162(5) 0.0174(5) -0.0044(4) 0.0015(4) 0.0000(4) C6 0.0136(4) 0.0128(4) 0.0171(5) -0.0021(4) -0.0037(4) 0.0016(4) C7 0.0215(5) 0.0172(5) 0.0094(4) -0.0008(4) -0.0042(4) -0.0019(4) C8 0.0222(5) 0.0175(5) 0.0104(4) -0.0049(4) -0.0001(4) -0.0041(4) C9 0.0124(4) 0.0156(5) 0.0237(5) -0.0036(4) -0.0035(4) -0.0054(4) C10 0.0138(4) 0.0127(4) 0.0211(5) -0.0036(4) -0.0001(4) -0.0061(4) N1 0.0156(4) 0.0094(4) 0.0115(4) -0.0013(3) 0.0021(3) -0.0043(3) N2 0.0123(4) 0.0112(4) 0.0102(4) -0.0020(3) 0.0019(3) -0.0025(3) N3 0.0122(4) 0.0114(4) 0.0119(4) -0.0015(3) -0.0025(3) -0.0014(3) N4 0.0151(4) 0.0106(4) 0.0110(4) -0.0023(3) 0.0019(3) -0.0027(3) N5 0.0117(4) 0.0111(4) 0.0134(4) 0.0009(3) 0.0000(3) -0.0048(3) O1 0.0110(3) 0.0131(3) 0.0113(3) -0.0005(3) -0.0016(2) -0.0046(3) O2 0.0139(4) 0.0250(5) 0.0273(5) -0.0070(4) -0.0036(3) -0.0082(4) O3 0.0264(6) 0.0234(5) 0.0450(7) -0.0014(5) 0.0023(5) -0.0098(4) O4 0.0617(18) 0.0589(18) 0.093(3) -0.0152(17) 0.0220(17) -0.0255(15) O5 0.0617(18) 0.0589(18) 0.093(3) -0.0152(17) 0.0220(17) -0.0255(15) Cl1 0.01582(12) 0.01059(11) 0.02556(14) -0.00283(9) -0.00107(10) -0.00318(9) Cl2 0.02931(17) 0.03021(18) 0.01778(14) 0.00647(12) 0.00598(12) -0.00381(14) Co1 0.00834(7) 0.00724(7) 0.00670(6) -0.00043(4) 0.00021(4) -0.00226(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 C1 O2 1.2354(15) . yes C1 O1 1.2913(14) . yes C1 C2 1.5087(18) . yes C2 N1 1.4889(16) . yes C2 H2A 0.9391 . yes C2 H2B 0.9340 . yes C3 N1 1.4967(16) . yes C3 C4 1.5075(18) . yes C3 H3A 0.9647 . yes C3 H3B 0.9550 . yes C4 N2 1.4848(16) . yes C4 H4A 0.9309 . yes C4 H4B 0.9654 . yes C5 N2 1.5025(16) . yes C5 C6 1.5227(18) . yes C5 H5A 0.9613 . yes C5 H5B 1.0028 . yes C6 N3 1.4925(16) . yes C6 H6A 1.0030 . yes C6 H6B 0.9419 . yes C7 N3 1.4934(17) . yes C7 C8 1.5199(19) . yes C7 H7A 0.9275 . yes C7 H7B 1.0316 . yes C8 N4 1.5007(17) . yes C8 H8A 1.0419 . yes C8 H8B 0.9063 . yes C9 N3 1.5130(17) . yes C9 C10 1.5168(18) . yes C9 H9A 1.0206 . yes C9 H9B 1.0239 . yes C10 N5 1.4825(16) . yes C10 H10A 1.0651 . yes C10 H10B 0.9151 . yes N1 Co1 2.0098(10) . yes N1 H11 0.9648 . yes N2 Co1 1.9719(10) . yes N2 H12 0.9763 . yes N3 Co1 1.9511(10) . yes N4 Co1 1.9721(10) . yes N4 H14A 0.9525 . yes N4 H14B 0.8684 . yes N5 Co1 1.9375(10) . yes N5 H15A 1.0120 . yes N5 H15B 0.8734 . yes O1 Co1 1.9003(9) . yes O4 O5 1.227(10) 1_556 yes O5 O4 1.227(10) 1_554 yes 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 O2 C1 O1 123.65(12) . . yes O2 C1 C2 120.63(11) . . yes O1 C1 C2 115.68(10) . . yes N1 C2 C1 110.72(9) . . yes N1 C2 H2A 107.1 . . yes C1 C2 H2A 109.4 . . yes N1 C2 H2B 105.7 . . yes C1 C2 H2B 110.1 . . yes H2A C2 H2B 113.8 . . yes N1 C3 C4 108.20(9) . . yes N1 C3 H3A 109.6 . . yes C4 C3 H3A 109.6 . . yes N1 C3 H3B 109.9 . . yes C4 C3 H3B 109.9 . . yes H3A C3 H3B 109.6 . . yes N2 C4 C3 107.29(9) . . yes N2 C4 H4A 108.7 . . yes C3 C4 H4A 112.1 . . yes N2 C4 H4B 108.6 . . yes C3 C4 H4B 110.5 . . yes H4A C4 H4B 109.4 . . yes N2 C5 C6 110.46(10) . . yes N2 C5 H5A 110.7 . . yes C6 C5 H5A 109.2 . . yes N2 C5 H5B 111.2 . . yes C6 C5 H5B 108.0 . . yes H5A C5 H5B 107.3 . . yes N3 C6 C5 107.89(9) . . yes N3 C6 H6A 109.6 . . yes C5 C6 H6A 109.6 . . yes N3 C6 H6B 110.5 . . yes C5 C6 H6B 110.5 . . yes H6A C6 H6B 108.7 . . yes N3 C7 C8 108.63(10) . . yes N3 C7 H7A 109.1 . . yes C8 C7 H7A 112.7 . . yes N3 C7 H7B 106.7 . . yes C8 C7 H7B 111.7 . . yes H7A C7 H7B 107.9 . . yes N4 C8 C7 107.97(10) . . yes N4 C8 H8A 112.7 . . yes C7 C8 H8A 103.8 . . yes N4 C8 H8B 115.9 . . yes C7 C8 H8B 107.4 . . yes H8A C8 H8B 108.3 . . yes N3 C9 C10 110.91(10) . . yes N3 C9 H9A 113.2 . . yes C10 C9 H9A 110.5 . . yes N3 C9 H9B 112.2 . . yes C10 C9 H9B 109.7 . . yes H9A C9 H9B 99.9 . . yes N5 C10 C9 107.33(10) . . yes N5 C10 H10A 113.6 . . yes C9 C10 H10A 104.9 . . yes N5 C10 H10B 118.3 . . yes C9 C10 H10B 107.5 . . yes H10A C10 H10B 104.3 . . yes C2 N1 C3 110.84(9) . . yes C2 N1 Co1 105.75(7) . . yes C3 N1 Co1 109.99(7) . . yes C2 N1 H11 112.0 . . yes C3 N1 H11 108.2 . . yes Co1 N1 H11 110.0 . . yes C4 N2 C5 113.04(10) . . yes C4 N2 Co1 107.88(7) . . yes C5 N2 Co1 109.24(7) . . yes C4 N2 H12 111.8 . . yes C5 N2 H12 103.7 . . yes Co1 N2 H12 111.1 . . yes C6 N3 C7 112.36(10) . . yes C6 N3 C9 109.02(10) . . yes C7 N3 C9 111.41(10) . . yes C6 N3 Co1 106.93(7) . . yes C7 N3 Co1 106.99(8) . . yes C9 N3 Co1 110.00(7) . . yes C8 N4 Co1 111.40(8) . . yes C8 N4 H14A 103.4 . . yes Co1 N4 H14A 106.7 . . yes C8 N4 H14B 105.5 . . yes Co1 N4 H14B 109.1 . . yes H14A N4 H14B 120.6 . . yes C10 N5 Co1 111.20(7) . . yes C10 N5 H15A 102.5 . . yes Co1 N5 H15A 111.9 . . yes C10 N5 H15B 103.1 . . yes Co1 N5 H15B 116.4 . . yes H15A N5 H15B 110.6 . . yes C1 O1 Co1 116.17(8) . . yes O1 Co1 N5 87.07(4) . . yes O1 Co1 N3 173.81(4) . . yes N5 Co1 N3 86.78(4) . . yes O1 Co1 N2 93.79(4) . . yes N5 Co1 N2 93.56(4) . . yes N3 Co1 N2 87.35(4) . . yes O1 Co1 N4 93.38(4) . . yes N5 Co1 N4 91.25(4) . . yes N3 Co1 N4 85.99(4) . . yes N2 Co1 N4 171.55(4) . . yes O1 Co1 N1 84.45(4) . . yes N5 Co1 N1 171.25(4) . . yes N3 Co1 N1 101.72(4) . . yes N2 Co1 N1 84.84(4) . . yes N4 Co1 N1 91.43(4) . . yes 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 O2 C1 C2 N1 166.00(11) . . . . yes O1 C1 C2 N1 -15.92(14) . . . . yes N1 C3 C4 N2 48.79(13) . . . . yes N2 C5 C6 N3 -42.65(14) . . . . yes N3 C7 C8 N4 43.43(14) . . . . yes N3 C9 C10 N5 -39.07(14) . . . . yes C1 C2 N1 C3 -92.71(11) . . . . yes C1 C2 N1 Co1 26.46(11) . . . . yes C4 C3 N1 C2 88.53(12) . . . . yes C4 C3 N1 Co1 -28.06(12) . . . . yes C3 C4 N2 C5 74.14(12) . . . . yes C3 C4 N2 Co1 -46.76(11) . . . . yes C6 C5 N2 C4 -99.69(12) . . . . yes C6 C5 N2 Co1 20.44(12) . . . . yes C5 C6 N3 C7 161.29(11) . . . . yes C5 C6 N3 C9 -74.70(12) . . . . yes C5 C6 N3 Co1 44.19(11) . . . . yes C8 C7 N3 C6 -162.78(11) . . . . yes C8 C7 N3 C9 74.54(13) . . . . yes C8 C7 N3 Co1 -45.72(12) . . . . yes C10 C9 N3 C6 140.89(11) . . . . yes C10 C9 N3 C7 -94.54(12) . . . . yes C10 C9 N3 Co1 23.93(13) . . . . yes C7 C8 N4 Co1 -21.07(12) . . . . yes C9 C10 N5 Co1 36.85(12) . . . . yes O2 C1 O1 Co1 173.35(10) . . . . yes C2 C1 O1 Co1 -4.66(13) . . . . yes C1 O1 Co1 N5 -165.42(9) . . . . yes C1 O1 Co1 N3 -158.3(3) . . . . yes C1 O1 Co1 N2 101.20(9) . . . . yes C1 O1 Co1 N4 -74.34(9) . . . . yes C1 O1 Co1 N1 16.77(8) . . . . yes C10 N5 Co1 O1 159.40(8) . . . . yes C10 N5 Co1 N3 -19.83(8) . . . . yes C10 N5 Co1 N2 -106.97(8) . . . . yes C10 N5 Co1 N4 66.08(8) . . . . yes C10 N5 Co1 N1 173.9(2) . . . . yes C6 N3 Co1 O1 -127.9(4) . . . . yes C7 N3 Co1 O1 111.5(4) . . . . yes C9 N3 Co1 O1 -9.6(4) . . . . yes C7 N3 Co1 O1 111.5(4) . . . . yes C9 N3 Co1 O1 -9.6(4) . . . . yes C6 N3 Co1 N5 -120.79(8) . . . . yes C7 N3 Co1 N5 118.62(8) . . . . yes C9 N3 Co1 N5 -2.54(8) . . . . yes C6 N3 Co1 N2 -27.08(8) . . . . yes C7 N3 Co1 N2 -147.66(8) . . . . yes C9 N3 Co1 N2 91.18(8) . . . . yes C6 N3 Co1 N4 147.72(8) . . . . yes C7 N3 Co1 N4 27.14(8) . . . . yes C9 N3 Co1 N4 -94.03(8) . . . . yes C6 N3 Co1 N1 57.09(8) . . . . yes C7 N3 Co1 N1 -63.49(8) . . . . yes C9 N3 Co1 N1 175.34(8) . . . . yes C4 N2 Co1 O1 -59.14(8) . . . . yes C5 N2 Co1 O1 177.61(8) . . . . yes C4 N2 Co1 N5 -146.44(8) . . . . yes C5 N2 Co1 N5 90.32(8) . . . . yes C4 N2 Co1 N3 126.95(8) . . . . yes C5 N2 Co1 N3 3.71(8) . . . . yes C4 N2 Co1 N4 88.9(3) . . . . yes C5 N2 Co1 N4 -34.3(3) . . . . yes C4 N2 Co1 N1 24.93(8) . . . . yes C5 N2 Co1 N1 -98.31(8) . . . . yes C8 N4 Co1 O1 -177.09(8) . . . . yes C8 N4 Co1 N5 -89.95(8) . . . . yes C8 N4 Co1 N3 -3.26(8) . . . . yes C8 N4 Co1 N2 34.8(3) . . . . yes C8 N4 Co1 N1 98.38(8) . . . . yes C2 N1 Co1 O1 -23.45(7) . . . . yes C3 N1 Co1 O1 96.28(8) . . . . yes C2 N1 Co1 N5 -38.0(3) . . . . yes C3 N1 Co1 N5 81.7(3) . . . . yes C2 N1 Co1 N3 156.01(7) . . . . yes C3 N1 Co1 N3 -84.26(8) . . . . yes C2 N1 Co1 N2 -117.78(8) . . . . yes C3 N1 Co1 N2 1.95(8) . . . . yes C2 N1 Co1 N4 69.81(8) . . . . yes C3 N1 Co1 N4 -170.46(8) . . . . yes _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 35.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.899 _refine_diff_density_min -1.104 _refine_diff_density_rms 0.119 data_s-7 _database_code_depnum_ccdc_archive 'CCDC 255281' _audit_creation_method maXus _chemical_compound_source 'Local laboratory' _exptl_crystal_description Cube _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_F_000 1112 _cell_measurement_temperature 122.4(5) _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _computing_data_collection KappaCCD _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.03370 _diffrn_orient_matrix_UB_12 -0.05284 _diffrn_orient_matrix_UB_13 0.06077 _diffrn_orient_matrix_UB_21 -0.06693 _diffrn_orient_matrix_UB_22 0.04678 _diffrn_orient_matrix_UB_23 0.07784 _diffrn_orient_matrix_UB_31 -0.03132 _diffrn_orient_matrix_UB_32 -0.03876 _diffrn_orient_matrix_UB_33 -0.00366 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _chemical_formula_weight 544.492 _diffrn_radiation_type ' MoK\a' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' 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' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_cell_setting Monoclinic _chemical_formula_moiety 'C11 H26 Co N5 O2 2+, Cl4 Zn 2-, H2 O ' _chemical_formula_sum 'C11 H28 Cl4 Co N5 O3 Zn ' _chemical_name_common 's-(Co(tren-tngly)) ZnCl4 H2O' _cell_length_a 11.6250(5) _cell_length_b 8.8530(4) _cell_length_c 20.297(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.1720(16) _cell_angle_gamma 90.00 _cell_volume 2056.1(2) _diffrn_reflns_number 68656 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_av_R_equivalents 0.034 _cell_measurement_reflns_used 1659 _cell_measurement_theta_min 0.784 _cell_measurement_theta_max 20.362 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 1 0.110 0 1 -2 0.150 0 -1 -1 0.130 0 1 2 0.140 1 0 -2 0.070 -1 0 2 0.070 0 0 -1 0.110 0 0 1 0.070 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co .3494 .9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 4717 _reflns_number_gt 4613 _reflns_threshold_expression >2sigma(I) _exptl_absorpt_coefficient_mu 2.514 _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^)+(0.0679P)^2^+6.3214P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_number_reflns 4717 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 0.20327(3) 0.25684(4) 0.096768(18) 0.01501(11) Uani 1 1 d . . . O1 O 0.06708(17) 0.2541(2) 0.02903(10) 0.0160(4) Uani 1 1 d . . . O2 O -0.01772(18) 0.1331(2) -0.06228(10) 0.0202(4) Uani 1 1 d . . . N1 N 0.2726(2) 0.1222(3) 0.03721(13) 0.0204(5) Uani 1 1 d . . . H21 H 0.3233 0.1849 0.0163 0.024 Uiso 1 1 d R . . N2 N 0.3432(2) 0.2644(3) 0.16647(13) 0.0213(5) Uani 1 1 d . . . H22 H 0.3861 0.3472 0.1522 0.026 Uiso 1 1 d R . . N3 N 0.1304(2) 0.3996(3) 0.15037(12) 0.0170(4) Uani 1 1 d . . . N4 N 0.2509(2) 0.4366(3) 0.05002(13) 0.0185(5) Uani 1 1 d . . . H24A H 0.3346 0.4386 0.0554 0.022 Uiso 1 1 d R . . H24B H 0.2179 0.4309 0.0033 0.022 Uiso 1 1 d R . . N5 N 0.1302(2) 0.0992(3) 0.14253(12) 0.0216(5) Uani 1 1 d . . . H25A H 0.0870 0.0322 0.1100 0.026 Uiso 1 1 d R . . H25B H 0.1895 0.0434 0.1714 0.026 Uiso 1 1 d R . . C1 C 0.0671(2) 0.1556(3) -0.01780(13) 0.0157(5) Uani 1 1 d . . . C2 C 0.1772(2) 0.0634(3) -0.01479(14) 0.0172(5) Uani 1 1 d . . . H2A H 0.2007 0.0668 -0.0578 0.021 Uiso 1 1 d R . . H2B H 0.1603 -0.0391 -0.0043 0.021 Uiso 1 1 d R . . C3 C 0.3502(3) -0.0007(4) 0.06839(16) 0.0249(6) Uani 1 1 d . . . H3A H 0.3062 -0.0672 0.0919 0.030 Uiso 1 1 d R . . H3B H 0.3801 -0.0563 0.0345 0.030 Uiso 1 1 d R . . C4 C 0.4515(3) 0.0582(4) 0.11750(17) 0.0285(7) Uani 1 1 d . . . H4A H 0.4899 0.1306 0.0936 0.034 Uiso 1 1 d R . . H4B H 0.5026 -0.0261 0.1302 0.034 Uiso 1 1 d R . . C5 C 0.4215(3) 0.1311(4) 0.17919(15) 0.0232(6) Uani 1 1 d . . . H5A H 0.4943 0.1588 0.2068 0.028 Uiso 1 1 d R . . H5B H 0.3840 0.0546 0.2014 0.028 Uiso 1 1 d R . . C6 C 0.3066(3) 0.3143(4) 0.22901(14) 0.0242(6) Uani 1 1 d . . . H6A H 0.2753 0.2292 0.2493 0.029 Uiso 1 1 d R . . H6B H 0.3721 0.3546 0.2594 0.029 Uiso 1 1 d R . . C7 C 0.2129(3) 0.4335(4) 0.21407(16) 0.0249(6) Uani 1 1 d . . . H7A H 0.2507 0.5287 0.2102 0.030 Uiso 1 1 d R . . H7B H 0.1711 0.4374 0.2508 0.030 Uiso 1 1 d R . . C8 C 0.1034(3) 0.5398(3) 0.10909(16) 0.0209(6) Uani 1 1 d . . . H8A H 0.0381 0.5211 0.0739 0.025 Uiso 1 1 d R . . H8B H 0.0849 0.6212 0.1366 0.025 Uiso 1 1 d R . . C9 C 0.2091(3) 0.5781(3) 0.07888(17) 0.0235(6) Uani 1 1 d . . . H9A H 0.2700 0.6171 0.1128 0.028 Uiso 1 1 d R . . H9B H 0.1896 0.6517 0.0440 0.028 Uiso 1 1 d R . . C10 C 0.0198(3) 0.3259(4) 0.16203(15) 0.0239(6) Uani 1 1 d . . . H10A H -0.0110 0.3796 0.1961 0.029 Uiso 1 1 d R . . H10B H -0.0367 0.3263 0.1213 0.029 Uiso 1 1 d R . . C11 C 0.0491(3) 0.1646(4) 0.18442(16) 0.0273(6) Uani 1 1 d . . . H11A H -0.0218 0.1067 0.1782 0.033 Uiso 1 1 d R . . H11B H 0.0849 0.1625 0.2308 0.033 Uiso 1 1 d R . . Zn1 Zn 0.70150(3) 0.44777(4) 0.150159(15) 0.01589(10) Uani 1 1 d . . . Cl1 Cl 0.51554(6) 0.54265(8) 0.14642(3) 0.02157(16) Uani 1 1 d . . . Cl2 Cl 0.80976(6) 0.64817(8) 0.12986(3) 0.02190(15) Uani 1 1 d . . . Cl3 Cl 0.75835(7) 0.33795(8) 0.25112(3) 0.02331(16) Uani 1 1 d . . . Cl4 Cl 0.70627(7) 0.27543(9) 0.06928(4) 0.02760(17) Uani 1 1 d . . . O3 O 0.5539(2) 0.6960(3) 0.00926(13) 0.0328(5) Uani 1 1 d . . . H3'A H 0.566(4) 0.668(6) 0.049(3) 0.039 Uiso 1 1 d . . . H3'B H 0.484(5) 0.690(5) -0.014(2) 0.039 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01232(18) 0.01400(19) 0.01705(19) -0.00295(13) -0.00198(13) 0.00111(12) O1 0.0145(9) 0.0162(9) 0.0163(9) -0.0006(7) -0.0003(7) 0.0000(7) O2 0.0226(10) 0.0162(9) 0.0190(9) 0.0027(7) -0.0037(8) -0.0043(8) N1 0.0182(11) 0.0191(11) 0.0226(12) -0.0013(9) 0.0002(9) 0.0017(9) N2 0.0178(11) 0.0236(12) 0.0206(12) -0.0015(9) -0.0016(9) -0.0003(9) N3 0.0193(11) 0.0142(10) 0.0173(10) -0.0005(9) 0.0026(8) 0.0008(9) N4 0.0147(10) 0.0185(11) 0.0229(12) 0.0009(9) 0.0051(9) -0.0035(8) N5 0.0254(12) 0.0170(11) 0.0193(11) 0.0030(9) -0.0048(9) -0.0031(9) C1 0.0178(12) 0.0123(11) 0.0166(12) 0.0042(9) 0.0021(9) -0.0048(9) C2 0.0180(12) 0.0153(12) 0.0183(12) -0.0015(10) 0.0029(10) -0.0003(10) C3 0.0284(15) 0.0217(14) 0.0236(14) -0.0003(12) 0.0021(12) 0.0105(12) C4 0.0219(14) 0.0329(17) 0.0292(16) -0.0006(13) 0.0006(12) 0.0106(12) C5 0.0192(13) 0.0278(15) 0.0201(13) 0.0003(11) -0.0034(10) 0.0059(11) C6 0.0256(14) 0.0309(16) 0.0146(12) -0.0024(11) -0.0006(10) 0.0011(12) C7 0.0257(15) 0.0253(15) 0.0218(14) -0.0086(11) -0.0012(11) 0.0015(12) C8 0.0206(13) 0.0157(13) 0.0276(14) 0.0013(11) 0.0081(11) 0.0012(10) C9 0.0217(14) 0.0176(13) 0.0326(15) 0.0024(12) 0.0082(12) 0.0002(11) C10 0.0217(13) 0.0292(15) 0.0222(13) -0.0005(12) 0.0074(11) -0.0031(12) C11 0.0340(16) 0.0251(15) 0.0229(14) 0.0029(12) 0.0050(12) -0.0086(13) Zn1 0.01562(17) 0.01763(17) 0.01488(17) -0.00200(11) 0.00396(12) -0.00207(11) Cl1 0.0138(3) 0.0285(4) 0.0230(3) -0.0018(3) 0.0047(2) -0.0019(2) Cl2 0.0198(3) 0.0228(3) 0.0241(3) 0.0040(3) 0.0065(2) -0.0047(2) Cl3 0.0341(4) 0.0163(3) 0.0189(3) 0.0017(2) 0.0028(3) -0.0002(3) Cl4 0.0241(4) 0.0316(4) 0.0268(4) -0.0140(3) 0.0037(3) 0.0015(3) O3 0.0212(11) 0.0463(15) 0.0304(12) 0.0141(11) 0.0028(9) -0.0005(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.9049(19) . yes Co1 N5 1.952(3) . yes Co1 N3 1.955(2) . yes Co1 N2 1.959(2) . yes Co1 N1 1.969(3) . yes Co1 N4 1.981(2) . yes O1 C1 1.290(3) . yes O2 C1 1.230(3) . yes N1 C3 1.482(4) . yes N1 C2 1.484(4) . yes N1 H21 0.9612 . yes N2 C6 1.476(4) . yes N2 C5 1.485(4) . yes N2 H22 0.9599 . yes N3 C7 1.498(4) . yes N3 C10 1.499(4) . yes N3 C8 1.499(4) . yes N4 C9 1.500(4) . yes N4 H24A 0.9600 . yes N4 H24B 0.9603 . yes N5 C11 1.494(4) . yes N5 H25A 0.9607 . yes N5 H25B 0.9591 . yes C1 C2 1.510(4) . yes C2 H2A 0.9594 . yes C2 H2B 0.9605 . yes C3 C4 1.496(4) . yes C3 H3A 0.9606 . yes C3 H3B 0.9591 . yes C4 C5 1.503(4) . yes C4 H4A 0.9602 . yes C4 H4B 0.9603 . yes C5 H5A 0.9606 . yes C5 H5B 0.9598 . yes C6 C7 1.508(4) . yes C6 H6A 0.9606 . yes C6 H6B 0.9601 . yes C7 H7A 0.9602 . yes C7 H7B 0.9592 . yes C8 C9 1.506(4) . yes C8 H8A 0.9605 . yes C8 H8B 0.9589 . yes C9 H9A 0.9601 . yes C9 H9B 0.9597 . yes C10 C11 1.518(5) . yes C10 H10A 0.9596 . yes C10 H10B 0.9603 . yes C11 H11A 0.9598 . yes C11 H11B 0.9602 . yes Zn1 Cl4 2.2490(8) . yes Zn1 Cl2 2.2549(7) . yes Zn1 Cl3 2.2589(8) . yes Zn1 Cl1 2.3080(7) . yes O3 H3'A 0.84(5) . yes O3 H3'B 0.87(5) . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N5 87.63(9) . . yes O1 Co1 N3 91.34(9) . . yes N5 Co1 N3 86.00(11) . . yes O1 Co1 N2 178.76(10) . . yes N5 Co1 N2 93.22(11) . . yes N3 Co1 N2 87.82(10) . . yes O1 Co1 N1 85.85(9) . . yes N5 Co1 N1 96.84(11) . . yes N3 Co1 N1 175.91(10) . . yes N2 Co1 N1 94.94(11) . . yes O1 Co1 N4 86.07(9) . . yes N5 Co1 N4 169.79(11) . . yes N3 Co1 N4 86.13(10) . . yes N2 Co1 N4 92.96(11) . . yes N1 Co1 N4 90.72(10) . . yes C1 O1 Co1 115.58(17) . . yes C3 N1 C2 111.6(2) . . yes C3 N1 Co1 117.81(19) . . yes C2 N1 Co1 108.25(17) . . yes C3 N1 H21 103.8 . . yes C2 N1 H21 109.2 . . yes Co1 N1 H21 105.7 . . yes C6 N2 C5 110.4(2) . . yes C6 N2 Co1 107.61(18) . . yes C5 N2 Co1 120.23(19) . . yes C6 N2 H22 106.0 . . yes C5 N2 H22 108.9 . . yes Co1 N2 H22 102.5 . . yes C7 N3 C10 112.8(2) . . yes C7 N3 C8 110.8(2) . . yes C10 N3 C8 110.4(2) . . yes C7 N3 Co1 109.62(18) . . yes C10 N3 Co1 105.92(18) . . yes C8 N3 Co1 107.03(17) . . yes C9 N4 Co1 110.29(18) . . yes C9 N4 H24A 109.4 . . yes Co1 N4 H24A 108.9 . . yes C9 N4 H24B 109.2 . . yes Co1 N4 H24B 109.5 . . yes H24A N4 H24B 109.4 . . yes C11 N5 Co1 111.39(19) . . yes C11 N5 H25A 108.9 . . yes Co1 N5 H25A 109.4 . . yes C11 N5 H25B 108.1 . . yes Co1 N5 H25B 109.5 . . yes H25A N5 H25B 109.5 . . yes O2 C1 O1 123.0(3) . . yes O2 C1 C2 120.4(3) . . yes O1 C1 C2 116.5(2) . . yes N1 C2 C1 111.2(2) . . yes N1 C2 H2A 109.8 . . yes C1 C2 H2A 108.8 . . yes N1 C2 H2B 109.3 . . yes C1 C2 H2B 108.3 . . yes H2A C2 H2B 109.5 . . yes N1 C3 C4 112.1(3) . . yes N1 C3 H3A 109.0 . . yes C4 C3 H3A 107.9 . . yes N1 C3 H3B 109.9 . . yes C4 C3 H3B 108.3 . . yes H3A C3 H3B 109.5 . . yes C3 C4 C5 115.6(3) . . yes C3 C4 H4A 106.1 . . yes C5 C4 H4A 109.4 . . yes C3 C4 H4B 106.6 . . yes C5 C4 H4B 109.5 . . yes H4A C4 H4B 109.5 . . yes N2 C5 C4 114.9(2) . . yes N2 C5 H5A 110.4 . . yes C4 C5 H5A 106.5 . . yes N2 C5 H5B 109.1 . . yes C4 C5 H5B 106.3 . . yes H5A C5 H5B 109.4 . . yes N2 C6 C7 110.1(2) . . yes N2 C6 H6A 108.8 . . yes C7 C6 H6A 108.7 . . yes N2 C6 H6B 110.3 . . yes C7 C6 H6B 109.4 . . yes H6A C6 H6B 109.5 . . yes N3 C7 C6 111.3(2) . . yes N3 C7 H7A 109.7 . . yes C6 C7 H7A 107.8 . . yes N3 C7 H7B 110.1 . . yes C6 C7 H7B 108.4 . . yes H7A C7 H7B 109.5 . . yes N3 C8 C9 108.0(2) . . yes N3 C8 H8A 109.5 . . yes C9 C8 H8A 109.3 . . yes N3 C8 H8B 110.1 . . yes C9 C8 H8B 110.5 . . yes H8A C8 H8B 109.5 . . yes N4 C9 C8 108.3(2) . . yes N4 C9 H9A 109.4 . . yes C8 C9 H9A 109.9 . . yes N4 C9 H9B 109.2 . . yes C8 C9 H9B 110.5 . . yes H9A C9 H9B 109.4 . . yes N3 C10 C11 107.6(3) . . yes N3 C10 H10A 109.8 . . yes C11 C10 H10A 110.0 . . yes N3 C10 H10B 109.8 . . yes C11 C10 H10B 110.1 . . yes H10A C10 H10B 109.5 . . yes N5 C11 C10 109.0(2) . . yes N5 C11 H11A 109.4 . . yes C10 C11 H11A 108.7 . . yes N5 C11 H11B 110.0 . . yes C10 C11 H11B 110.3 . . yes H11A C11 H11B 109.4 . . yes Cl4 Zn1 Cl2 108.29(3) . . yes Cl4 Zn1 Cl3 109.22(3) . . yes Cl2 Zn1 Cl3 114.90(3) . . yes Cl4 Zn1 Cl1 111.51(3) . . yes Cl2 Zn1 Cl1 104.92(3) . . yes Cl3 Zn1 Cl1 107.98(3) . . yes H3'A O3 H3'B 120(5) . . yes 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 O1 C1 -86.29(19) . . . . yes N3 Co1 O1 C1 -172.23(19) . . . . yes N2 Co1 O1 C1 140(4) . . . . yes N1 Co1 O1 C1 10.74(19) . . . . yes N4 Co1 O1 C1 101.75(19) . . . . yes O1 Co1 N1 C3 -142.3(2) . . . . yes N5 Co1 N1 C3 -55.2(2) . . . . yes N3 Co1 N1 C3 171.1(13) . . . . yes N2 Co1 N1 C3 38.6(2) . . . . yes N4 Co1 N1 C3 131.7(2) . . . . yes O1 Co1 N1 C2 -14.58(18) . . . . yes N5 Co1 N1 C2 72.53(19) . . . . yes N3 Co1 N1 C2 -61.2(15) . . . . yes N2 Co1 N1 C2 166.38(18) . . . . yes N4 Co1 N1 C2 -100.59(19) . . . . yes O1 Co1 N2 C6 70(5) . . . . yes N5 Co1 N2 C6 -63.3(2) . . . . yes N3 Co1 N2 C6 22.6(2) . . . . yes N1 Co1 N2 C6 -160.4(2) . . . . yes N4 Co1 N2 C6 108.6(2) . . . . yes O1 Co1 N2 C5 -163(4) . . . . yes N5 Co1 N2 C5 64.2(2) . . . . yes N3 Co1 N2 C5 150.1(2) . . . . yes N1 Co1 N2 C5 -32.9(2) . . . . yes N4 Co1 N2 C5 -123.9(2) . . . . yes O1 Co1 N3 C7 178.85(19) . . . . yes N5 Co1 N3 C7 91.3(2) . . . . yes N2 Co1 N3 C7 -2.1(2) . . . . yes N1 Co1 N3 C7 -134.7(14) . . . . yes N4 Co1 N3 C7 -95.2(2) . . . . yes O1 Co1 N3 C10 56.89(18) . . . . yes N5 Co1 N3 C10 -30.64(18) . . . . yes N2 Co1 N3 C10 -124.02(19) . . . . yes N1 Co1 N3 C10 103.3(14) . . . . yes N4 Co1 N3 C10 142.86(19) . . . . yes O1 Co1 N3 C8 -60.87(18) . . . . yes N5 Co1 N3 C8 -148.40(19) . . . . yes N2 Co1 N3 C8 118.22(19) . . . . yes N1 Co1 N3 C8 -14.4(15) . . . . yes N4 Co1 N3 C8 25.10(18) . . . . yes O1 Co1 N4 C9 91.89(19) . . . . yes N5 Co1 N3 C8 -148.40(19) . . . . yes N2 Co1 N3 C8 118.22(19) . . . . yes N1 Co1 N3 C8 -14.4(15) . . . . yes N5 Co1 N3 C8 -148.40(19) . . . . yes N2 Co1 N3 C8 118.22(19) . . . . yes N1 Co1 N3 C8 -14.4(15) . . . . yes N4 Co1 N3 C8 25.10(18) . . . . yes O1 Co1 N4 C9 91.89(19) . . . . yes O1 Co1 N4 C9 91.89(19) . . . . yes O1 Co1 N4 C9 91.89(19) . . . . yes N5 Co1 N4 C9 39.9(7) . . . . yes N3 Co1 N4 C9 0.28(19) . . . . yes N2 Co1 N4 C9 -87.3(2) . . . . yes N1 Co1 N4 C9 177.7(2) . . . . yes O1 Co1 N5 C11 -84.0(2) . . . . yes N3 Co1 N5 C11 7.5(2) . . . . yes N2 Co1 N5 C11 95.1(2) . . . . yes N1 Co1 N5 C11 -169.5(2) . . . . yes N4 Co1 N5 C11 -32.1(7) . . . . yes Co1 O1 C1 O2 174.7(2) . . . . yes Co1 O1 C1 C2 -3.6(3) . . . . yes C3 N1 C2 C1 147.2(2) . . . . yes Co1 N1 C2 C1 16.0(3) . . . . yes O2 C1 C2 N1 172.8(2) . . . . yes O1 C1 C2 N1 -8.8(3) . . . . yes C2 N1 C3 C4 176.0(3) . . . . yes Co1 N1 C3 C4 -57.9(3) . . . . yes N1 C3 C4 C5 66.3(4) . . . . yes C6 N2 C5 C4 172.4(3) . . . . yes Co1 N2 C5 C4 46.1(3) . . . . yes C3 C4 C5 N2 -60.1(4) . . . . yes C5 N2 C6 C7 -171.2(3) . . . . yes Co1 N2 C6 C7 -38.2(3) . . . . yes C10 N3 C7 C6 98.9(3) . . . . yes C8 N3 C7 C6 -136.8(3) . . . . yes Co1 N3 C7 C6 -18.9(3) . . . . yes N2 C6 C7 N3 38.0(4) . . . . yes C7 N3 C8 C9 73.8(3) . . . . yes C10 N3 C8 C9 -160.5(2) . . . . yes Co1 N3 C8 C9 -45.7(3) . . . . yes Co1 N4 C9 C8 -25.7(3) . . . . yes N3 C8 C9 N4 46.6(3) . . . . yes C7 N3 C10 C11 -72.6(3) . . . . yes C8 N3 C10 C11 162.9(2) . . . . yes Co1 N3 C10 C11 47.4(3) . . . . yes Co1 N5 C11 C10 17.5(3) . . . . yes N3 C10 C11 N5 -42.4(3) . . . . yes _diffrn_measured_fraction_theta_max .998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full .998 _refine_diff_density_max 2.241 _refine_diff_density_min -1.613 _refine_diff_density_rms .111 data_s-8 _database_code_depnum_ccdc_archive 'CCDC 255282' _audit_creation_method maXus _chemical_compound_source 'Local laboratory' _exptl_crystal_description Cube _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_F_000 1232 _cell_measurement_temperature 122.4(5) _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _computing_data_collection KappaCCD _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.883 _exptl_crystal_density_method 'not measured' _chemical_formula_weight 608.63 _diffrn_radiation_type ' MoK\a' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,+Y,-Z '+X+ 1/2,+Y+ 1/2,+Z' '-X+ 1/2,+Y+ 1/2,-Z' _symmetry_space_group_name_H-M 'C 1 2 1 ' _symmetry_space_group_name_Hall 'C 2y ' _symmetry_cell_setting Monoclinic _chemical_formula_moiety '2(C12 H28 Cl3 Co N5 O2 Zn 1+), Cl4 Zn 2- ' _chemical_formula_sum 'C24 H56 Cl10 Co2 N10 O4 Zn3 ' _chemical_name_common 's-(Co(tren-bngly)ZnCl3)2 ZnCl4' _cell_length_a 13.2627(10) _cell_length_b 11.8214(9) _cell_length_c 13.7098(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.933(10) _cell_angle_gamma 90.00 _cell_volume 2146.7(3) _diffrn_reflns_number 76368 _diffrn_reflns_theta_max 45.00 _diffrn_reflns_av_R_equivalents 0.020 _cell_measurement_reflns_used 368 _cell_measurement_theta_min 1.017 _cell_measurement_theta_max 20.362 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.070 0 0 -1 0.040 1 -1 -1 0.090 1 1 -1 0.110 -1 -1 1 0.080 2 0 1 0.140 -2 0 -1 0.110 1 -1 1 0.135 -1 1 1 0.100 1 1 1 0.140 -1 -1 -1 0.090 -1 1 -1 0.100 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.479 _exptl_absorpt_correction_T_max 0.706 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; 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' 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 17569 _reflns_number_gt 16916 _reflns_threshold_expression >2sigma(I) _exptl_absorpt_coefficient_mu 3.076 _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^)+(0.0365P)^2^+1.0759P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(4) _refine_ls_number_reflns 17569 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_restrained_S_all 1.320 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.35664(8) -0.23171(9) -0.44721(7) 0.01099(12) Uani 1 1 d . . . C2 C -0.39604(9) -0.32221(9) -0.38248(8) 0.01330(14) Uani 1 1 d . . . H2A H -0.3569 -0.3896 -0.3904 0.016 Uiso 1 1 d R . . H2B H -0.4652 -0.3367 -0.4024 0.016 Uiso 1 1 d R . . C3 C -0.36646(8) -0.38926(9) -0.21480(8) 0.01265(13) Uani 1 1 d . . . H3A H -0.3908 -0.4560 -0.2482 0.015 Uiso 1 1 d R . . H3B H -0.2948 -0.3951 -0.2019 0.015 Uiso 1 1 d R . . C4 C -0.41532(9) -0.38371(10) -0.11695(8) 0.01493(15) Uani 1 1 d . . . H4A H -0.4127 -0.4594 -0.0915 0.018 Uiso 1 1 d R . . H4B H -0.4844 -0.3628 -0.1316 0.018 Uiso 1 1 d R . . C5 C -0.36814(9) -0.30238(10) -0.04116(8) 0.01446(15) Uani 1 1 d . . . H5A H -0.2981 -0.3228 -0.0344 0.017 Uiso 1 1 d R . . H5B H -0.4001 -0.3191 0.0184 0.017 Uiso 1 1 d R . . C6 C -0.37748(8) -0.17635(10) -0.06291(8) 0.01301(14) Uani 1 1 d . . . H6A H -0.3759 -0.1366 -0.0018 0.016 Uiso 1 1 d R . . H6B H -0.4414 -0.1638 -0.0973 0.016 Uiso 1 1 d R . . C7 C -0.27704(10) -0.01174(10) -0.10159(8) 0.01583(17) Uani 1 1 d . . . H7A H -0.3388 0.0294 -0.1137 0.019 Uiso 1 1 d R . . H7B H -0.2545 -0.0031 -0.0343 0.019 Uiso 1 1 d R . . C8 C -0.19704(10) 0.03003(11) -0.16766(8) 0.01685(18) Uani 1 1 d . . . H8A H -0.1322 0.0037 -0.1430 0.020 Uiso 1 1 d R . . H8B H -0.1976 0.1112 -0.1680 0.020 Uiso 1 1 d R . . C9 C -0.12192(9) -0.04752(12) -0.31532(10) 0.01825(19) Uani 1 1 d . . . H9A H -0.1343 -0.0574 -0.3844 0.022 Uiso 1 1 d R . . H9B H -0.0718 0.0102 -0.3037 0.022 Uiso 1 1 d R . . C10 C -0.08659(9) -0.15811(14) -0.26870(13) 0.0228(2) Uani 1 1 d . . . H10A H -0.0608 -0.1453 -0.2029 0.027 Uiso 1 1 d R . . H10B H -0.0349 -0.1919 -0.3057 0.027 Uiso 1 1 d R . . C11 C -0.27390(9) 0.07179(9) -0.33272(8) 0.01375(15) Uani 1 1 d . . . H11A H -0.2418 0.1443 -0.3253 0.016 Uiso 1 1 d R . . H11B H -0.2737 0.0486 -0.3998 0.016 Uiso 1 1 d R . . C12 C -0.38148(9) 0.07820(9) -0.30057(9) 0.01559(16) Uani 1 1 d . . . H12A H -0.4245 0.1127 -0.3506 0.019 Uiso 1 1 d R . . H12B H -0.3839 0.1214 -0.2414 0.019 Uiso 1 1 d R . . N1 N -0.38914(6) -0.28709(7) -0.27770(6) 0.00949(10) Uani 1 1 d . . . H21 H -0.4543 -0.2626 -0.2587 0.011 Uiso 1 1 d R . . N2 N -0.29445(7) -0.13382(8) -0.12333(6) 0.01061(11) Uani 1 1 d . . . H22 H -0.2333 -0.1742 -0.1059 0.013 Uiso 1 1 d R . . N3 N -0.21756(7) -0.01326(8) -0.27018(6) 0.01160(12) Uani 1 1 d . . . N4 N -0.17603(7) -0.23570(9) -0.26789(8) 0.01406(13) Uani 1 1 d . . . H24A H -0.1699 -0.2824 -0.2107 0.017 Uiso 1 1 d R . . H24B H -0.1770 -0.2826 -0.3251 0.017 Uiso 1 1 d R . . N5 N -0.41746(7) -0.04057(8) -0.28239(7) 0.01162(12) Uani 1 1 d . . . H25A H -0.4611 -0.0633 -0.3369 0.014 Uiso 1 1 d R . . H25B H -0.4545 -0.0406 -0.2241 0.014 Uiso 1 1 d R . . O1 O -0.30608(6) -0.15172(8) -0.40601(5) 0.01235(10) Uani 1 1 d . . . O2 O -0.37240(7) -0.23894(8) -0.53789(6) 0.01492(13) Uani 1 1 d . . . Cl1 Cl -0.38157(2) -0.18992(2) -0.766587(18) 0.01261(3) Uani 1 1 d . . . Cl2 Cl -0.14140(2) -0.13246(3) -0.60190(3) 0.01852(5) Uani 1 1 d . . . Cl3 Cl -0.37189(2) 0.04960(3) -0.58661(2) 0.01670(4) Uani 1 1 d . . . Cl4 Cl 0.12471(3) -0.19226(4) -0.05558(4) 0.02934(8) Uani 1 1 d . . . Cl5 Cl -0.07166(2) -0.41738(3) -0.11693(2) 0.01655(4) Uani 1 1 d . . . Co1 Co -0.302108(9) -0.148221(14) -0.266774(9) 0.00754(2) Uani 1 1 d . . . Zn1 Zn -0.308103(9) -0.1208 -0.624043(9) 0.01097(2) Uani 1 1 d . . . Zn2 Zn 0.0000 -0.3020 0.0000 0.01423(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0117(3) 0.0118(3) 0.0095(3) 0.0001(2) 0.0005(2) -0.0018(2) C2 0.0181(4) 0.0111(3) 0.0105(3) -0.0001(2) -0.0009(3) -0.0048(3) C3 0.0149(3) 0.0099(3) 0.0131(3) 0.0031(3) 0.0001(3) -0.0004(3) C4 0.0185(4) 0.0135(4) 0.0128(3) 0.0037(3) 0.0006(3) -0.0049(3) C5 0.0174(4) 0.0146(4) 0.0112(3) 0.0043(3) -0.0011(3) -0.0036(3) C6 0.0143(3) 0.0140(3) 0.0110(3) 0.0012(3) 0.0024(3) -0.0022(3) C7 0.0242(5) 0.0123(3) 0.0109(3) -0.0011(3) -0.0009(3) -0.0058(3) C8 0.0220(4) 0.0157(4) 0.0123(3) 0.0017(3) -0.0043(3) -0.0103(3) C9 0.0117(3) 0.0210(5) 0.0222(5) 0.0050(4) 0.0027(3) -0.0049(3) C10 0.0093(3) 0.0247(6) 0.0344(6) 0.0078(5) 0.0012(4) -0.0014(3) C11 0.0167(4) 0.0110(3) 0.0133(3) 0.0033(3) -0.0025(3) -0.0051(3) C12 0.0173(4) 0.0088(3) 0.0204(4) 0.0032(3) -0.0018(3) -0.0006(3) N1 0.0098(2) 0.0087(3) 0.0099(2) 0.0013(2) 0.00040(19) -0.0008(2) N2 0.0125(3) 0.0110(3) 0.0083(2) 0.0011(2) -0.00050(19) -0.0026(2) N3 0.0115(3) 0.0123(3) 0.0108(3) 0.0023(2) -0.0017(2) -0.0051(2) N4 0.0098(3) 0.0147(3) 0.0178(3) 0.0018(3) 0.0016(2) 0.0013(2) N5 0.0111(3) 0.0091(3) 0.0146(3) 0.0021(2) -0.0003(2) -0.0003(2) O1 0.0154(3) 0.0134(3) 0.0082(2) 0.0001(2) 0.00056(19) -0.0053(2) O2 0.0184(3) 0.0176(3) 0.0087(2) -0.0003(2) 0.0002(2) -0.0051(3) Cl1 0.01387(8) 0.01291(8) 0.01088(7) -0.00134(6) -0.00116(6) 0.00278(7) Cl2 0.01108(8) 0.01921(12) 0.02537(12) -0.00024(9) 0.00188(8) 0.00051(8) Cl3 0.01997(11) 0.01398(9) 0.01580(9) -0.00188(7) -0.00242(8) 0.00468(8) Cl4 0.02346(14) 0.02726(16) 0.03595(18) 0.01475(14) -0.01170(13) -0.01242(12) Cl5 0.01988(10) 0.01521(10) 0.01407(9) -0.00212(7) -0.00382(8) -0.00082(8) Co1 0.00743(4) 0.00754(4) 0.00758(4) 0.00081(3) -0.00024(3) -0.00163(3) Zn1 0.01102(4) 0.01094(4) 0.01093(4) -0.00028(3) 0.00036(3) -0.00050(3) Zn2 0.01451(7) 0.01104(6) 0.01652(7) 0.000 -0.00538(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.2529(13) . yes C1 O1 1.2744(13) . yes C1 C2 1.5008(14) . yes C2 N1 1.4936(13) . yes C2 H2A 0.9598 . yes C2 H2B 0.9593 . yes C3 N1 1.5055(13) . yes C3 C4 1.5208(16) . yes C3 H3A 0.9605 . yes C3 H3B 0.9597 . yes C4 C5 1.5261(17) . yes C4 H4A 0.9598 . yes C4 H4B 0.9602 . yes C5 C6 1.5233(16) . yes C5 H5A 0.9594 . yes C5 H5B 0.9599 . yes C6 N2 1.4983(13) . yes C6 H6A 0.9594 . yes C6 H6B 0.9603 . yes C7 N2 1.4893(14) . yes C7 C8 1.5127(17) . yes C7 H7A 0.9596 . yes C7 H7B 0.9606 . yes C8 N3 1.5075(14) . yes C8 H8A 0.9593 . yes C8 H8B 0.9601 . yes C9 N3 1.4954(16) . yes C9 C10 1.519(2) . yes C9 H9A 0.9600 . yes C9 H9B 0.9598 . yes C10 N4 1.5000(17) . yes C10 H10A 0.9596 . yes C10 H10B 0.9603 . yes C11 N3 1.4963(14) . yes C11 C12 1.5166(18) . yes C11 H11A 0.9601 . yes C11 H11B 0.9602 . yes C12 N5 1.5077(14) . yes C12 H12A 0.9603 . yes C12 H12B 0.9605 . yes N1 Co1 2.0081(8) . yes N1 H21 0.9603 . yes N2 Co1 1.9713(8) . yes N2 H22 0.9604 . yes N3 Co1 1.9520(9) . yes N4 Co1 1.9668(10) . yes N4 H24A 0.9594 . yes N4 H24B 0.9598 . yes N5 Co1 1.9931(9) . yes N5 H25A 0.9599 . yes N5 H25B 0.9597 . yes O1 Co1 1.9073(8) . yes O2 Zn1 2.0435(9) . yes Cl1 Zn1 2.2894(4) . yes Cl2 Zn1 2.2206(3) . yes Cl3 Zn1 2.2542(3) . yes Cl4 Zn2 2.2645(4) . yes Cl5 Zn2 2.2755(3) . yes Zn2 Cl4 2.2644(4) 2 yes Zn2 Cl5 2.2755(3) 2 yes 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 O2 C1 O1 123.21(10) . . yes O2 C1 C2 119.52(9) . . yes O1 C1 C2 117.25(9) . . yes N1 C2 C1 111.38(8) . . yes N1 C2 H2A 109.4 . . yes C1 C2 H2A 108.6 . . yes N1 C2 H2B 109.5 . . yes C1 C2 H2B 108.4 . . yes H2A C2 H2B 109.5 . . yes N1 C3 C4 112.89(9) . . yes N1 C3 H3A 109.5 . . yes C4 C3 H3A 107.9 . . yes N1 C3 H3B 109.3 . . yes C4 C3 H3B 107.7 . . yes H3A C3 H3B 109.5 . . yes C3 C4 C5 116.71(9) . . yes C3 C4 H4A 105.7 . . yes C5 C4 H4A 109.5 . . yes C3 C4 H4B 105.7 . . yes C5 C4 H4B 109.5 . . yes H4A C4 H4B 109.5 . . yes C6 C5 C4 117.16(9) . . yes C6 C5 H5A 109.5 . . yes C4 C5 H5A 105.6 . . yes C6 C5 H5B 109.4 . . yes C4 C5 H5B 105.5 . . yes H5A C5 H5B 109.5 . . yes N2 C6 C5 112.44(9) . . yes N2 C6 H6A 109.5 . . yes C5 C6 H6A 108.1 . . yes N2 C6 H6B 109.4 . . yes C5 C6 H6B 108.0 . . yes H6A C6 H6B 109.4 . . yes N2 C7 C8 107.62(10) . . yes N2 C7 H7A 109.5 . . yes C8 C7 H7A 110.4 . . yes N2 C7 H7B 109.4 . . yes C8 C7 H7B 110.3 . . yes H7A C7 H7B 109.5 . . yes N3 C8 C7 110.41(9) . . yes N3 C8 H8A 109.5 . . yes C7 C8 H8A 109.1 . . yes N3 C8 H8B 109.5 . . yes C7 C8 H8B 108.9 . . yes H8A C8 H8B 109.4 . . yes N3 C9 C10 107.99(10) . . yes N3 C9 H9A 109.6 . . yes C10 C9 H9A 110.1 . . yes N3 C9 H9B 109.5 . . yes C10 C9 H9B 110.2 . . yes H9A C9 H9B 109.4 . . yes N4 C10 C9 107.60(10) . . yes N4 C10 H10A 109.5 . . yes C9 C10 H10A 110.3 . . yes N4 C10 H10B 109.6 . . yes C9 C10 H10B 110.4 . . yes H10A C10 H10B 109.5 . . yes N3 C11 C12 108.46(9) . . yes N3 C11 H11A 109.5 . . yes C12 C11 H11A 110.1 . . yes N3 C11 H11B 109.4 . . yes C12 C11 H11B 110.0 . . yes H11A C11 H11B 109.5 . . yes N5 C12 C11 108.18(9) . . yes N5 C12 H12A 109.4 . . yes C11 C12 H12A 110.3 . . yes N5 C12 H12B 109.3 . . yes C11 C12 H12B 110.1 . . yes H12A C12 H12B 109.5 . . yes C2 N1 C3 109.18(8) . . yes C2 N1 Co1 107.80(6) . . yes C3 N1 Co1 121.06(6) . . yes C2 N1 H21 109.4 . . yes C3 N1 H21 104.1 . . yes Co1 N1 H21 104.8 . . yes C7 N2 C6 108.98(9) . . yes C7 N2 Co1 106.43(6) . . yes C6 N2 Co1 121.38(7) . . yes C7 N2 H22 108.1 . . yes C6 N2 H22 109.3 . . yes Co1 N2 H22 101.9 . . yes C9 N3 C11 110.74(9) . . yes C9 N3 C8 111.18(9) . . yes C11 N3 C8 111.54(9) . . yes C9 N3 Co1 106.80(8) . . yes C11 N3 Co1 106.99(6) . . yes C8 N3 Co1 109.37(6) . . yes C10 N4 Co1 110.58(8) . . yes C10 N4 H24A 108.9 . . yes Co1 N4 H24A 109.4 . . yes C10 N4 H24B 109.0 . . yes Co1 N4 H24B 109.5 . . yes H24A N4 H24B 109.4 . . yes C12 N5 Co1 111.39(7) . . yes C12 N5 H25A 108.4 . . yes Co1 N5 H25A 109.5 . . yes C12 N5 H25B 108.5 . . yes Co1 N5 H25B 109.5 . . yes H25A N5 H25B 109.5 . . yes C1 O1 Co1 116.53(7) . . yes C1 O2 Zn1 118.27(7) . . yes O1 Co1 N3 88.87(4) . . yes O1 Co1 N4 87.75(4) . . yes N3 Co1 N4 86.55(4) . . yes O1 Co1 N2 176.04(4) . . yes N3 Co1 N2 87.30(4) . . yes N4 Co1 N2 93.02(4) . . yes O1 Co1 N5 85.67(4) . . yes N3 Co1 N5 85.08(4) . . yes N4 Co1 N5 169.46(4) . . yes N2 Co1 N5 92.99(4) . . yes O1 Co1 N1 85.48(4) . . yes N3 Co1 N1 174.35(4) . . yes N4 Co1 N1 93.17(4) . . yes N2 Co1 N1 98.34(3) . . yes N5 Co1 N1 94.52(4) . . yes O2 Zn1 Cl2 108.70(3) . . yes O2 Zn1 Cl3 107.85(3) . . yes Cl2 Zn1 Cl3 114.019(13) . . yes O2 Zn1 Cl1 94.45(3) . . yes Cl2 Zn1 Cl1 118.153(15) . . yes Cl3 Zn1 Cl1 111.406(11) . . yes Cl4 Zn2 Cl4 110.10(3) 2 . yes Cl4 Zn2 Cl5 107.130(14) 2 . yes Cl4 Zn2 Cl5 113.097(17) . . yes Cl4 Zn2 Cl5 113.096(17) 2 2 yes Cl4 Zn2 Cl5 107.128(14) . 2 yes Cl5 Zn2 Cl5 106.337(18) . 2 yes _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 45.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.671 _refine_diff_density_min -1.672 _refine_diff_density_rms 0.184 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 O2 C1 C2 N1 -167.96(10) . . . . yes O1 C1 C2 N1 13.64(14) . . . . yes N1 C3 C4 C5 -73.97(13) . . . . yes C3 C4 C5 C6 67.70(14) . . . . yes C4 C5 C6 N2 -86.38(12) . . . . yes N2 C7 C8 N3 44.23(13) . . . . yes N3 C9 C10 N4 46.96(15) . . . . yes N3 C11 C12 N5 -42.33(12) . . . . yes C1 C2 N1 C3 -145.57(9) . . . . yes C1 C2 N1 Co1 -12.31(11) . . . . yes C4 C3 N1 C2 -146.40(9) . . . . yes C4 C3 N1 Co1 87.64(10) . . . . yes C8 C7 N2 C6 -176.92(9) . . . . yes C8 C7 N2 Co1 -44.42(10) . . . . yes C5 C6 N2 C7 -152.36(9) . . . . yes C5 C6 N2 Co1 83.57(10) . . . . yes C10 C9 N3 C11 -161.70(11) . . . . yes C10 C9 N3 C8 73.70(13) . . . . yes C10 C9 N3 Co1 -45.55(12) . . . . yes C12 C11 N3 C9 163.87(10) . . . . yes C12 C11 N3 C8 -71.73(11) . . . . yes C12 C11 N3 Co1 47.84(10) . . . . yes C7 C8 N3 C9 -139.97(11) . . . . yes C7 C8 N3 C11 95.88(11) . . . . yes C7 C8 N3 Co1 -22.27(12) . . . . yes C9 C10 N4 Co1 -26.33(14) . . . . yes C11 C12 N5 Co1 17.70(11) . . . . yes O2 C1 O1 Co1 174.01(9) . . . . yes C2 C1 O1 Co1 -7.65(13) . . . . yes O1 C1 O2 Zn1 3.04(15) . . . . yes C2 C1 O2 Zn1 -175.25(8) . . . . yes C1 O1 Co1 N3 179.94(9) . . . . yes C1 O1 Co1 N4 93.35(9) . . . . yes C1 O1 Co1 N2 -165.3(5) . . . . yes C1 O1 Co1 N5 -94.90(9) . . . . yes C1 O1 Co1 N1 -0.01(8) . . . . yes C9 N3 Co1 O1 -63.05(8) . . . . yes C11 N3 Co1 O1 55.57(7) . . . . yes C8 N3 Co1 O1 176.53(8) . . . . yes C9 N3 Co1 N4 24.77(8) . . . . yes C11 N3 Co1 N4 143.39(8) . . . . yes C8 N3 Co1 N4 -95.65(8) . . . . yes C9 N3 Co1 N2 117.96(8) . . . . yes C11 N3 Co1 N2 -123.42(7) . . . . yes C8 N3 Co1 N2 -2.46(8) . . . . yes C9 N3 Co1 N5 -148.81(8) . . . . yes C11 N3 Co1 N5 -30.18(7) . . . . yes C8 N3 Co1 N5 90.78(8) . . . . yes C9 N3 Co1 N1 -62.6(4) . . . . yes C11 N3 Co1 N1 56.0(4) . . . . yes C8 N3 Co1 N1 177.0(4) . . . . yes C10 N4 Co1 O1 90.06(9) . . . . yes C10 N4 Co1 N3 1.06(9) . . . . yes C10 N4 Co1 N2 -86.05(9) . . . . yes C10 N4 Co1 N5 38.6(3) . . . . yes C10 N4 Co1 N1 175.41(9) . . . . yes C7 N2 Co1 O1 11.7(6) . . . . yes C6 N2 Co1 O1 137.0(5) . . . . yes C7 N2 Co1 N3 26.52(8) . . . . yes C6 N2 Co1 N3 151.77(8) . . . . yes C7 N2 Co1 N4 112.92(8) . . . . yes C6 N2 Co1 N4 -121.83(8) . . . . yes C7 N2 Co1 N5 -58.41(8) . . . . yes C6 N2 Co1 N5 66.84(8) . . . . yes C7 N2 Co1 N1 -153.43(7) . . . . yes C6 N2 Co1 N1 -28.18(8) . . . . yes C12 N5 Co1 O1 -82.27(8) . . . . yes C12 N5 Co1 N3 6.97(8) . . . . yes C12 N5 Co1 N4 -30.7(3) . . . . yes C12 N5 Co1 N2 94.00(8) . . . . yes C12 N5 Co1 N1 -167.38(8) . . . . yes C2 N1 Co1 O1 7.20(7) . . . . yes C3 N1 Co1 O1 133.79(8) . . . . yes C2 N1 Co1 N3 6.7(4) . . . . yes C3 N1 Co1 N3 133.3(4) . . . . yes C2 N1 Co1 N4 -80.30(7) . . . . yes C3 N1 Co1 N4 46.30(8) . . . . yes C2 N1 Co1 N2 -173.82(7) . . . . yes C3 N1 Co1 N2 -47.22(8) . . . . yes C2 N1 Co1 N5 92.49(7) . . . . yes C3 N1 Co1 N5 -140.92(8) . . . . yes C1 O2 Zn1 Cl2 61.54(9) . . . . yes C1 O2 Zn1 Cl3 -62.55(9) . . . . yes C1 O2 Zn1 Cl1 -176.73(9) . . . . yes