Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 1273 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Browne, Julian M.W.' 'Hartshorn, Richard M.' 'Wikaira, Jan' _publ_contact_author_name 'Dr Richard M. Hartshorn' _publ_contact_author_address ; University of Canterbury Christchurch New Zealand ; _publ_contact_author_email r.hartshorn@chem.canterbury.ac.nz data_[Co(tetraenim)Cl]ZnCl4 _database_code_CSD 165266 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H21 Cl5 Co N5 Zn' _chemical_formula_weight 488.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.752(5) _cell_length_b 9.510(4) _cell_length_c 17.268(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.095(5) _cell_angle_gamma 90.00 _cell_volume 1765.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 3.050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8344 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22056 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 26.41 _reflns_number_total 3597 _reflns_number_gt 2910 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3597 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.19817(3) -0.28733(3) 0.447548(15) 0.01651(8) Uani 1 1 d . . . N5 N 0.13675(16) -0.48086(18) 0.43591(10) 0.0210(4) Uani 1 1 d . . . H5B' H 0.1485 -0.5280 0.4820 0.025 Uiso 1 1 calc R . . H5A' H 0.0527 -0.4788 0.4249 0.025 Uiso 1 1 calc R . . N4 N 0.31702(16) -0.33730(18) 0.36718(9) 0.0181(4) Uani 1 1 d . . . H4' H 0.3943 -0.3007 0.3815 0.022 Uiso 1 1 calc R . . N3 N 0.09536(17) -0.20256(18) 0.36578(10) 0.0218(4) Uani 1 1 d . . . H3' H 0.0139 -0.2323 0.3724 0.026 Uiso 1 1 calc R . . N2 N 0.26568(16) -0.10620(18) 0.46211(10) 0.0217(4) Uani 1 1 d . . . N1 N 0.31376(16) -0.33720(19) 0.53340(10) 0.0223(4) Uani 1 1 d . . . H1B' H 0.2749 -0.3963 0.5675 0.027 Uiso 1 1 calc R . . H1A' H 0.3820 -0.3831 0.5144 0.027 Uiso 1 1 calc R . . C8 C 0.2009(2) -0.5588(2) 0.37330(12) 0.0245(5) Uani 1 1 d . . . H8A H 0.1525 -0.5515 0.3241 0.029 Uiso 1 1 calc R . . H8B H 0.2088 -0.6595 0.3871 0.029 Uiso 1 1 calc R . . C7 C 0.3280(2) -0.4943(2) 0.36423(12) 0.0221(5) Uani 1 1 d . . . H7A H 0.3845 -0.5274 0.4063 0.027 Uiso 1 1 calc R . . H7B H 0.3632 -0.5233 0.3141 0.027 Uiso 1 1 calc R . . C6 C 0.2769(2) -0.2705(2) 0.29209(12) 0.0235(5) Uani 1 1 d . . . H6A H 0.3039 -0.3294 0.2483 0.028 Uiso 1 1 calc R . . H6B H 0.3163 -0.1769 0.2872 0.028 Uiso 1 1 calc R . . C5 C 0.1372(2) -0.2550(2) 0.28938(12) 0.0242(5) Uani 1 1 d . . . H5B H 0.1122 -0.1880 0.2481 0.029 Uiso 1 1 calc R . . H5C H 0.0979 -0.3470 0.2778 0.029 Uiso 1 1 calc R . . C4 C 0.0985(2) -0.0455(2) 0.37557(13) 0.0298(5) Uani 1 1 d . . . H4A H 0.0333 -0.0164 0.4120 0.036 Uiso 1 1 calc R . . H4B H 0.0808 0.0002 0.3251 0.036 Uiso 1 1 calc R . . C3 C 0.2246(2) 0.0017(2) 0.40630(14) 0.0323(6) Uani 1 1 d . . . H3A H 0.2843 0.0096 0.3636 0.039 Uiso 1 1 calc R . . H3B H 0.2180 0.0943 0.4320 0.039 Uiso 1 1 calc R . . C2 C 0.3325(2) -0.0839(3) 0.52168(13) 0.0282(5) Uani 1 1 d . . . H2A H 0.368(2) 0.003(3) 0.5345(13) 0.034 Uiso 1 1 d . . . C1 C 0.3537(2) -0.2060(2) 0.57398(13) 0.0309(6) Uani 1 1 d . . . H1B H 0.3056 -0.1939 0.6218 0.037 Uiso 1 1 calc R . . H1C H 0.4430 -0.2123 0.5887 0.037 Uiso 1 1 calc R . . Zn1 Zn 0.29708(2) 0.20952(3) 0.161000(14) 0.02171(8) Uani 1 1 d . . . Cl2 Cl 0.42422(6) 0.15449(8) 0.26017(3) 0.04003(17) Uani 1 1 d . . . Cl3 Cl 0.20474(6) 0.42049(6) 0.16776(3) 0.03074(14) Uani 1 1 d . . . Cl4 Cl 0.14314(5) 0.04294(6) 0.14890(3) 0.02655(13) Uani 1 1 d . . . Cl5 Cl 0.40319(5) 0.19491(6) 0.04525(3) 0.02651(13) Uani 1 1 d . . . Cl1 Cl 0.04630(5) -0.24312(5) 0.53218(3) 0.02393(13) 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 0.01544(15) 0.01770(15) 0.01647(14) 0.00044(11) 0.00276(11) -0.00052(12) N5 0.0204(10) 0.0193(9) 0.0235(9) 0.0001(8) 0.0038(8) -0.0029(8) N4 0.0159(9) 0.0200(9) 0.0183(9) -0.0001(7) 0.0012(7) 0.0005(8) N3 0.0185(9) 0.0225(10) 0.0246(10) 0.0041(8) 0.0018(8) 0.0014(8) N2 0.0209(10) 0.0197(9) 0.0248(10) -0.0007(8) 0.0071(8) -0.0024(8) N1 0.0217(10) 0.0270(10) 0.0183(9) 0.0001(8) 0.0036(7) 0.0025(8) C8 0.0295(13) 0.0192(11) 0.0249(11) -0.0027(9) 0.0057(10) 0.0003(10) C7 0.0244(12) 0.0217(11) 0.0204(10) -0.0027(9) 0.0019(9) 0.0047(10) C6 0.0270(12) 0.0264(12) 0.0173(11) 0.0045(9) 0.0042(9) 0.0017(10) C5 0.0268(13) 0.0281(12) 0.0176(11) 0.0041(9) -0.0001(9) 0.0021(10) C4 0.0356(14) 0.0206(12) 0.0330(13) 0.0045(10) 0.0000(11) 0.0081(11) C3 0.0438(16) 0.0183(12) 0.0351(13) 0.0033(10) 0.0068(11) -0.0025(11) C2 0.0262(13) 0.0287(13) 0.0300(13) -0.0106(10) 0.0093(10) -0.0069(11) C1 0.0318(14) 0.0389(15) 0.0220(12) -0.0092(10) -0.0010(10) -0.0008(12) Zn1 0.01834(14) 0.02659(15) 0.02022(13) -0.00223(10) 0.00077(10) -0.00172(11) Cl2 0.0244(3) 0.0699(5) 0.0256(3) 0.0071(3) -0.0038(2) -0.0018(3) Cl3 0.0346(3) 0.0258(3) 0.0321(3) -0.0043(2) 0.0060(3) -0.0002(3) Cl4 0.0227(3) 0.0258(3) 0.0312(3) -0.0031(2) 0.0017(2) -0.0040(2) Cl5 0.0233(3) 0.0350(3) 0.0213(3) -0.0009(2) 0.0046(2) 0.0028(2) Cl1 0.0229(3) 0.0224(3) 0.0269(3) -0.0004(2) 0.0104(2) 0.0010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.8842(19) . ? Co1 N3 1.9509(18) . ? Co1 N4 1.9628(17) . ? Co1 N5 1.9645(18) . ? Co1 N1 1.9741(18) . ? Co1 Cl1 2.2517(9) . ? N5 C8 1.491(3) . ? N4 C6 1.500(3) . ? N4 C7 1.499(3) . ? N3 C5 1.488(3) . ? N3 C4 1.503(3) . ? N2 C2 1.262(3) . ? N2 C3 1.470(3) . ? N1 C1 1.490(3) . ? C8 C7 1.509(3) . ? C6 C5 1.509(3) . ? C4 C3 1.514(3) . ? C2 C1 1.486(3) . ? Zn1 Cl2 2.2329(9) . ? Zn1 Cl3 2.2426(10) . ? Zn1 Cl4 2.2978(9) . ? Zn1 Cl5 2.3246(9) . ? 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 N3 86.00(8) . . ? N2 Co1 N4 93.52(7) . . ? N3 Co1 N4 87.47(8) . . ? N2 Co1 N5 176.45(8) . . ? N3 Co1 N5 97.38(8) . . ? N4 Co1 N5 85.58(7) . . ? N2 Co1 N1 83.34(8) . . ? N3 Co1 N1 169.33(8) . . ? N4 Co1 N1 93.66(8) . . ? N5 Co1 N1 93.29(8) . . ? N2 Co1 Cl1 91.43(6) . . ? N3 Co1 Cl1 89.12(6) . . ? N4 Co1 Cl1 173.78(5) . . ? N5 Co1 Cl1 89.70(5) . . ? N1 Co1 Cl1 90.66(6) . . ? C8 N5 Co1 112.38(13) . . ? C6 N4 C7 114.47(16) . . ? C6 N4 Co1 109.16(13) . . ? C7 N4 Co1 108.55(12) . . ? C5 N3 C4 115.22(17) . . ? C5 N3 Co1 109.06(13) . . ? C4 N3 Co1 108.53(14) . . ? C2 N2 C3 125.2(2) . . ? C2 N2 Co1 118.34(16) . . ? C3 N2 Co1 116.13(14) . . ? C1 N1 Co1 108.89(14) . . ? N5 C8 C7 107.80(17) . . ? N4 C7 C8 109.22(17) . . ? N4 C6 C5 109.75(17) . . ? N3 C5 C6 108.82(18) . . ? N3 C4 C3 110.62(18) . . ? N2 C3 C4 106.19(18) . . ? N2 C2 C1 116.2(2) . . ? C2 C1 N1 109.21(18) . . ? Cl2 Zn1 Cl3 115.78(3) . . ? Cl2 Zn1 Cl4 109.73(3) . . ? Cl3 Zn1 Cl4 107.62(4) . . ? Cl2 Zn1 Cl5 110.00(4) . . ? Cl3 Zn1 Cl5 108.86(2) . . ? Cl4 Zn1 Cl5 104.19(3) . . ? 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 N5 C8 -78.8(12) . . . . ? N3 Co1 N5 C8 83.45(15) . . . . ? N4 Co1 N5 C8 -3.43(14) . . . . ? N1 Co1 N5 C8 -96.84(15) . . . . ? Cl1 Co1 N5 C8 172.52(14) . . . . ? N2 Co1 N4 C6 -78.47(14) . . . . ? N3 Co1 N4 C6 7.36(14) . . . . ? N5 Co1 N4 C6 104.97(14) . . . . ? N1 Co1 N4 C6 -162.01(14) . . . . ? Cl1 Co1 N4 C6 64.2(5) . . . . ? N2 Co1 N4 C7 156.14(13) . . . . ? N3 Co1 N4 C7 -118.03(14) . . . . ? N5 Co1 N4 C7 -20.42(13) . . . . ? N1 Co1 N4 C7 72.60(14) . . . . ? Cl1 Co1 N4 C7 -61.2(5) . . . . ? N2 Co1 N3 C5 110.18(14) . . . . ? N4 Co1 N3 C5 16.48(14) . . . . ? N5 Co1 N3 C5 -68.73(14) . . . . ? N1 Co1 N3 C5 112.8(4) . . . . ? Cl1 Co1 N3 C5 -158.32(13) . . . . ? N2 Co1 N3 C4 -16.07(14) . . . . ? N4 Co1 N3 C4 -109.77(15) . . . . ? N5 Co1 N3 C4 165.01(14) . . . . ? N1 Co1 N3 C4 -13.4(5) . . . . ? Cl1 Co1 N3 C4 75.43(14) . . . . ? N3 Co1 N2 C2 168.31(18) . . . . ? N4 Co1 N2 C2 -104.48(17) . . . . ? N5 Co1 N2 C2 -29.3(13) . . . . ? N1 Co1 N2 C2 -11.20(17) . . . . ? Cl1 Co1 N2 C2 79.29(17) . . . . ? N3 Co1 N2 C3 -5.54(15) . . . . ? N4 Co1 N2 C3 81.68(16) . . . . ? N5 Co1 N2 C3 156.8(11) . . . . ? N1 Co1 N2 C3 174.95(16) . . . . ? Cl1 Co1 N2 C3 -94.55(15) . . . . ? N2 Co1 N1 C1 17.25(14) . . . . ? N3 Co1 N1 C1 14.6(5) . . . . ? N4 Co1 N1 C1 110.37(14) . . . . ? N5 Co1 N1 C1 -163.85(14) . . . . ? Cl1 Co1 N1 C1 -74.12(13) . . . . ? Co1 N5 C8 C7 26.2(2) . . . . ? C6 N4 C7 C8 -81.9(2) . . . . ? Co1 N4 C7 C8 40.28(18) . . . . ? N5 C8 C7 N4 -42.9(2) . . . . ? C7 N4 C6 C5 92.4(2) . . . . ? Co1 N4 C6 C5 -29.5(2) . . . . ? C4 N3 C5 C6 85.7(2) . . . . ? Co1 N3 C5 C6 -36.6(2) . . . . ? N4 C6 C5 N3 43.5(2) . . . . ? C5 N3 C4 C3 -88.4(2) . . . . ? Co1 N3 C4 C3 34.2(2) . . . . ? C2 N2 C3 C4 -148.2(2) . . . . ? Co1 N2 C3 C4 25.1(2) . . . . ? N3 C4 C3 N2 -37.6(2) . . . . ? C3 N2 C2 C1 174.7(2) . . . . ? Co1 N2 C2 C1 1.4(3) . . . . ? N2 C2 C1 N1 13.2(3) . . . . ? Co1 N1 C1 C2 -20.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.499 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.064 #===END data_[Co(trien)(NH2CH2CH(OEt)2)Cl]Br2 _database_code_CSD 165267 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H33 Br2 Cl Co N5 O2' _chemical_formula_weight 533.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 14.618(7) _cell_length_b 18.114(9) _cell_length_c 7.712(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2041.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 4.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7522 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995)A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22915 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.40 _reflns_number_total 3577 _reflns_number_gt 2751 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.110(17) _refine_ls_number_reflns 3577 _refine_ls_number_parameters 209 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.03227(6) 0.56304(5) 0.80391(14) 0.0338(2) Uani 1 1 d . . . Co Co 0.97524(6) 0.31490(5) 0.78971(14) 0.0117(2) Uani 1 1 d . . . Cl1 Cl 0.86542(11) 0.25096(10) 0.9407(3) 0.0195(4) Uani 1 1 d . . . N1 N 1.0722(4) 0.3746(3) 0.6823(8) 0.0156(15) Uani 1 1 d . . . H1A H 1.0879 0.3545 0.5769 0.019 Uiso 1 1 calc R . . H1B H 1.0511 0.4217 0.6634 0.019 Uiso 1 1 calc R . . N2 N 1.0554(4) 0.3099(3) 0.9914(8) 0.0161(15) Uani 1 1 d . . . H2 H 1.0203 0.3155 1.0912 0.019 Uiso 1 1 calc R . . N3 N 1.0352(4) 0.2247(3) 0.7169(9) 0.0167(15) Uani 1 1 d . . . H3 H 1.0889 0.2382 0.6606 0.020 Uiso 1 1 calc R . . N4 N 0.9069(4) 0.3036(4) 0.5718(8) 0.0172(15) Uani 1 1 d . . . H4A H 0.8463 0.2947 0.5965 0.021 Uiso 1 1 calc R . . H4B H 0.9102 0.3469 0.5095 0.021 Uiso 1 1 calc R . . N5 N 0.9117(4) 0.4071(3) 0.8705(8) 0.0149(15) Uani 1 1 d . . . H5A H 0.9030 0.4035 0.9884 0.018 Uiso 1 1 calc R . . H5B H 0.9501 0.4465 0.8513 0.018 Uiso 1 1 calc R . . O1A O 0.6906(3) 0.4915(3) 0.7820(9) 0.0231(12) Uani 1 1 d . . . O1B O 0.7695(4) 0.4915(3) 1.0473(6) 0.0174(13) Uani 1 1 d . . . C1 C 1.1530(5) 0.3771(4) 0.7953(13) 0.0182(15) Uani 1 1 d . . . H1C H 1.1872 0.4235 0.7756 0.022 Uiso 1 1 calc R . . H1D H 1.1941 0.3351 0.7688 0.022 Uiso 1 1 calc R . . C2 C 1.1219(5) 0.3729(4) 0.9798(10) 0.0171(18) Uani 1 1 d . . . H2A H 1.0919 0.4197 1.0143 0.021 Uiso 1 1 calc R . . H2B H 1.1747 0.3642 1.0576 0.021 Uiso 1 1 calc R . . C3 C 1.1063(6) 0.2362(4) 1.0009(11) 0.0212(19) Uani 1 1 d . . . H3A H 1.1031 0.2162 1.1202 0.025 Uiso 1 1 calc R . . H3B H 1.1715 0.2434 0.9704 0.025 Uiso 1 1 calc R . . C4 C 1.0620(6) 0.1818(5) 0.8737(10) 0.0206(19) Uani 1 1 d . . . H4C H 1.1059 0.1424 0.8421 0.025 Uiso 1 1 calc R . . H4D H 1.0075 0.1586 0.9270 0.025 Uiso 1 1 calc R . . C5 C 0.9791(6) 0.1852(5) 0.5913(11) 0.0226(19) Uani 1 1 d . . . H5C H 0.9278 0.1598 0.6502 0.027 Uiso 1 1 calc R . . H5D H 1.0161 0.1479 0.5290 0.027 Uiso 1 1 calc R . . C6 C 0.9432(6) 0.2427(4) 0.4662(11) 0.021(2) Uani 1 1 d . . . H6A H 0.9931 0.2607 0.3903 0.025 Uiso 1 1 calc R . . H6B H 0.8944 0.2215 0.3925 0.025 Uiso 1 1 calc R . . C10 C 0.8229(5) 0.4236(4) 0.7896(14) 0.0200(17) Uani 1 1 d . . . H10A H 0.7822 0.3803 0.8033 0.024 Uiso 1 1 calc R . . H10B H 0.8323 0.4316 0.6638 0.024 Uiso 1 1 calc R . . C11 C 0.7751(5) 0.4915(4) 0.8656(10) 0.0162(18) Uani 1 1 d . . . H11A H 0.8096 0.5365 0.8285 0.019 Uiso 1 1 calc R . . C12A C 0.6405(6) 0.5594(5) 0.8075(17) 0.037(2) Uani 1 1 d . . . H12A H 0.6765 0.6019 0.7639 0.045 Uiso 1 1 calc R . . H12B H 0.6281 0.5672 0.9324 0.045 Uiso 1 1 calc R . . C12B C 0.7200(6) 0.4323(5) 1.1269(11) 0.024(2) Uani 1 1 d . . . H12C H 0.7556 0.3860 1.1178 0.028 Uiso 1 1 calc R . . H12D H 0.6609 0.4251 1.0665 0.028 Uiso 1 1 calc R . . C13A C 0.5532(6) 0.5531(6) 0.7103(14) 0.043(3) Uani 1 1 d . . . H13D H 0.5171 0.5982 0.7266 0.064 Uiso 1 1 calc R . . H13E H 0.5185 0.5106 0.7536 0.064 Uiso 1 1 calc R . . H13F H 0.5662 0.5464 0.5867 0.064 Uiso 1 1 calc R . . Br2 Br 0.69902(6) 0.24069(5) 1.43454(15) 0.0344(2) Uani 1 1 d . . . C13B C 0.7033(6) 0.4502(5) 1.3132(14) 0.032(2) Uani 1 1 d . . . H13A H 0.6688 0.4099 1.3674 0.048 Uiso 1 1 calc R . . H13B H 0.6680 0.4961 1.3215 0.048 Uiso 1 1 calc R . . H13C H 0.7620 0.4563 1.3729 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0377(5) 0.0332(5) 0.0306(5) -0.0018(5) 0.0025(6) -0.0005(4) Co 0.0096(5) 0.0130(5) 0.0125(5) -0.0006(5) -0.0004(5) 0.0004(4) Cl1 0.0118(8) 0.0229(10) 0.0237(9) 0.0005(10) 0.0037(10) -0.0032(7) N1 0.012(3) 0.020(4) 0.015(4) 0.001(3) 0.001(3) 0.002(3) N2 0.015(3) 0.015(3) 0.018(4) -0.002(3) 0.003(3) 0.003(3) N3 0.012(3) 0.010(3) 0.029(4) 0.001(3) 0.000(3) -0.003(3) N4 0.012(4) 0.020(4) 0.019(4) -0.002(3) 0.002(3) 0.004(3) N5 0.013(3) 0.014(3) 0.018(3) 0.000(3) -0.001(3) 0.004(3) O1A 0.017(3) 0.026(3) 0.027(3) -0.013(3) -0.009(3) 0.011(2) O1B 0.021(3) 0.023(3) 0.009(3) -0.003(2) 0.000(2) -0.001(2) C1 0.013(4) 0.022(4) 0.019(4) 0.005(4) -0.007(4) -0.007(3) C2 0.012(4) 0.018(4) 0.022(5) -0.003(3) -0.002(3) -0.004(3) C3 0.027(5) 0.020(4) 0.017(4) 0.006(3) -0.006(4) 0.009(4) C4 0.028(5) 0.021(5) 0.012(4) 0.004(3) -0.001(3) 0.006(4) C5 0.022(5) 0.023(5) 0.023(5) -0.003(4) 0.004(4) 0.001(4) C6 0.025(4) 0.024(4) 0.014(5) 0.005(4) -0.006(3) 0.003(3) C10 0.014(4) 0.024(4) 0.022(4) -0.008(4) -0.007(4) 0.007(3) C11 0.015(4) 0.012(4) 0.021(4) 0.000(3) -0.006(3) 0.000(3) C12A 0.030(5) 0.031(5) 0.051(6) 0.002(5) -0.010(6) 0.014(4) C12B 0.027(5) 0.021(5) 0.024(5) -0.010(4) -0.001(4) -0.010(4) C13A 0.035(6) 0.052(7) 0.042(6) -0.012(5) -0.024(5) 0.026(5) Br2 0.0241(4) 0.0479(6) 0.0313(5) 0.0074(5) 0.0004(5) -0.0054(4) C13B 0.023(4) 0.036(5) 0.036(6) 0.003(5) 0.008(5) -0.014(4) _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 N3 1.937(6) . ? Co N2 1.950(6) . ? Co N1 1.965(6) . ? Co N4 1.966(7) . ? Co N5 2.010(6) . ? Co Cl1 2.296(2) . ? N1 C1 1.469(9) . ? N2 C2 1.502(9) . ? N2 C3 1.530(10) . ? N3 C5 1.457(10) . ? N3 C4 1.490(10) . ? N4 C6 1.470(10) . ? N5 C10 1.472(10) . ? O1A C11 1.394(9) . ? O1A C12A 1.445(9) . ? O1B C11 1.404(9) . ? O1B C12B 1.433(10) . ? C1 C2 1.496(13) . ? C3 C4 1.533(11) . ? C5 C6 1.514(11) . ? C10 C11 1.530(11) . ? C12A C13A 1.484(12) . ? C12B C13B 1.493(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co N2 85.4(3) . . ? N3 Co N1 90.9(3) . . ? N2 Co N1 85.9(3) . . ? N3 Co N4 83.9(3) . . ? N2 Co N4 169.4(3) . . ? N1 Co N4 93.6(3) . . ? N3 Co N5 178.5(3) . . ? N2 Co N5 93.9(3) . . ? N1 Co N5 90.4(3) . . ? N4 Co N5 96.7(3) . . ? N3 Co Cl1 92.2(2) . . ? N2 Co Cl1 89.6(2) . . ? N1 Co Cl1 174.3(2) . . ? N4 Co Cl1 91.5(2) . . ? N5 Co Cl1 86.48(19) . . ? C1 N1 Co 110.3(5) . . ? C2 N2 C3 110.6(6) . . ? C2 N2 Co 107.8(5) . . ? C3 N2 Co 111.7(5) . . ? C5 N3 C4 115.6(6) . . ? C5 N3 Co 110.6(5) . . ? C4 N3 Co 108.9(5) . . ? C6 N4 Co 111.5(5) . . ? C10 N5 Co 116.5(5) . . ? C11 O1A C12A 112.7(6) . . ? C11 O1B C12B 117.2(6) . . ? N1 C1 C2 108.5(6) . . ? C1 C2 N2 107.0(6) . . ? N2 C3 C4 109.0(6) . . ? N3 C4 C3 107.2(6) . . ? N3 C5 C6 106.2(7) . . ? N4 C6 C5 106.8(7) . . ? N5 C10 C11 113.8(6) . . ? O1A C11 O1B 114.2(7) . . ? O1A C11 C10 103.2(6) . . ? O1B C11 C10 114.2(7) . . ? O1A C12A C13A 107.5(8) . . ? O1B C12B C13B 109.4(6) . . ? 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 Co N1 C1 -79.5(5) . . . . ? N2 Co N1 C1 5.9(5) . . . . ? N4 Co N1 C1 -163.5(5) . . . . ? N5 Co N1 C1 99.8(5) . . . . ? Cl1 Co N1 C1 43(2) . . . . ? N3 Co N2 C2 112.0(5) . . . . ? N1 Co N2 C2 20.8(5) . . . . ? N4 Co N2 C2 108.5(15) . . . . ? N5 Co N2 C2 -69.4(5) . . . . ? Cl1 Co N2 C2 -155.8(4) . . . . ? N3 Co N2 C3 -9.8(5) . . . . ? N1 Co N2 C3 -101.0(5) . . . . ? N4 Co N2 C3 -13.2(18) . . . . ? N5 Co N2 C3 168.9(5) . . . . ? Cl1 Co N2 C3 82.5(5) . . . . ? N2 Co N3 C5 159.5(5) . . . . ? N1 Co N3 C5 -114.7(5) . . . . ? N4 Co N3 C5 -21.1(5) . . . . ? N5 Co N3 C5 94(11) . . . . ? Cl1 Co N3 C5 70.1(5) . . . . ? N2 Co N3 C4 31.5(5) . . . . ? N1 Co N3 C4 117.3(5) . . . . ? N4 Co N3 C4 -149.1(5) . . . . ? N5 Co N3 C4 -34(11) . . . . ? Cl1 Co N3 C4 -57.9(5) . . . . ? N3 Co N4 C6 -7.0(5) . . . . ? N2 Co N4 C6 -3.5(18) . . . . ? N1 Co N4 C6 83.5(5) . . . . ? N5 Co N4 C6 174.3(5) . . . . ? Cl1 Co N4 C6 -99.0(5) . . . . ? N3 Co N5 C10 -96(11) . . . . ? N2 Co N5 C10 -161.6(6) . . . . ? N1 Co N5 C10 112.5(6) . . . . ? N4 Co N5 C10 18.8(6) . . . . ? Cl1 Co N5 C10 -72.3(6) . . . . ? Co N1 C1 C2 -31.5(7) . . . . ? N1 C1 C2 N2 48.4(8) . . . . ? C3 N2 C2 C1 79.6(7) . . . . ? Co N2 C2 C1 -42.8(7) . . . . ? C2 N2 C3 C4 -133.5(7) . . . . ? Co N2 C3 C4 -13.3(8) . . . . ? C5 N3 C4 C3 -170.9(7) . . . . ? Co N3 C4 C3 -45.7(7) . . . . ? N2 C3 C4 N3 37.4(9) . . . . ? C4 N3 C5 C6 167.8(7) . . . . ? Co N3 C5 C6 43.5(7) . . . . ? Co N4 C6 C5 32.0(8) . . . . ? N3 C5 C6 N4 -48.1(8) . . . . ? Co N5 C10 C11 176.0(6) . . . . ? C12A O1A C11 O1B 67.3(10) . . . . ? C12A O1A C11 C10 -168.2(8) . . . . ? C12B O1B C11 O1A 57.4(9) . . . . ? C12B O1B C11 C10 -61.0(10) . . . . ? N5 C10 C11 O1A -174.4(7) . . . . ? N5 C10 C11 O1B -49.9(10) . . . . ? C11 O1A C12A C13A 179.0(8) . . . . ? C11 O1B C12B C13B -167.3(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.638 _refine_diff_density_min -1.333 _refine_diff_density_rms 0.139 #===END data_exo-ffms-[Co(tetraenol)Cl]ZnCl4 _database_code_CSD 165268 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H29 Cl5 Co N5 O2 Zn' _chemical_formula_weight 552.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.548(3) _cell_length_b 8.838(2) _cell_length_c 22.210(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.980(4) _cell_angle_gamma 90.00 _cell_volume 2045.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 2.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8806 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 pp33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15317 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.38 _reflns_number_total 4154 _reflns_number_gt 3273 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4154 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 Zn1 Zn 0.23877(3) 0.76832(3) 0.393922(14) 0.01921(9) Uani 1 1 d . . . Co1 Co 0.32210(3) 0.87212(3) 0.675368(16) 0.01352(9) Uani 1 1 d . . . Cl5 Cl 0.22729(6) 0.97337(7) 0.33035(3) 0.02285(16) Uani 1 1 d . . . Cl1 Cl 0.48471(6) 0.78772(7) 0.74630(3) 0.02238(15) Uani 1 1 d . . . Cl4 Cl 0.14709(7) 0.83214(8) 0.47950(3) 0.02554(16) Uani 1 1 d . . . Cl3 Cl 0.10762(7) 0.59412(7) 0.34062(3) 0.02811(17) Uani 1 1 d . . . Cl2 Cl 0.43643(7) 0.67907(8) 0.42434(4) 0.03285(18) Uani 1 1 d . . . N3 N 0.2051(2) 0.7177(2) 0.69958(10) 0.0168(5) Uani 1 1 d . . . H3' H 0.2250 0.7016 0.7414 0.020 Uiso 1 1 calc R . . N5 N 0.4453(2) 1.0005(2) 0.64095(10) 0.0179(5) Uani 1 1 d . . . H5B' H 0.4115 1.0957 0.6332 0.022 Uiso 1 1 calc R . . H5A' H 0.5199 1.0093 0.6684 0.022 Uiso 1 1 calc R . . N1 N 0.2877(2) 1.0236(2) 0.73611(9) 0.0172(5) Uani 1 1 d . . . H1A' H 0.2767 0.9746 0.7715 0.021 Uiso 1 1 calc R . . H1B' H 0.3578 1.0861 0.7449 0.021 Uiso 1 1 calc R . . N4 N 0.3532(2) 0.7266(2) 0.61401(10) 0.0181(5) Uani 1 1 d . . . H4' H 0.2874 0.7377 0.5812 0.022 Uiso 1 1 calc R . . O1 O 0.24105(18) 1.2121(2) 0.62508(9) 0.0277(5) Uani 1 1 d . . . H1" H 0.2059 1.2587 0.5939 0.042 Uiso 1 1 calc R . . N2 N 0.17103(19) 0.9607(2) 0.62450(10) 0.0159(5) Uani 1 1 d . . . H2' H 0.1876 0.9666 0.5847 0.019 Uiso 1 1 calc R . . C6 C 0.3416(3) 0.5720(3) 0.63871(14) 0.0270(7) Uani 1 1 d . . . H6B H 0.4169 0.5484 0.6698 0.032 Uiso 1 1 calc R . . H6A H 0.3366 0.4960 0.6057 0.032 Uiso 1 1 calc R . . C4 C 0.0708(2) 0.7740(3) 0.68517(13) 0.0204(6) Uani 1 1 d . . . H4A H 0.0515 0.8425 0.7178 0.024 Uiso 1 1 calc R . . H4B H 0.0099 0.6881 0.6819 0.024 Uiso 1 1 calc R . . C5 C 0.2208(3) 0.5703(3) 0.66671(14) 0.0261(7) Uani 1 1 d . . . H5B H 0.2239 0.4851 0.6959 0.031 Uiso 1 1 calc R . . H5A H 0.1459 0.5547 0.6344 0.031 Uiso 1 1 calc R . . C3 C 0.0580(2) 0.8580(3) 0.62529(12) 0.0195(6) Uani 1 1 d . . . H3B H 0.0529 0.7846 0.5913 0.023 Uiso 1 1 calc R . . H3A H -0.0220 0.9184 0.6196 0.023 Uiso 1 1 calc R . . C2 C 0.1509(3) 1.1189(3) 0.64654(13) 0.0202(6) Uani 1 1 d . . . H2A H 0.0619 1.1543 0.6307 0.024 Uiso 1 1 calc R . . C8 C 0.4737(3) 0.9307(3) 0.58312(12) 0.0231(6) Uani 1 1 d . . . H8B H 0.5583 0.9653 0.5745 0.028 Uiso 1 1 calc R . . H8A H 0.4074 0.9600 0.5485 0.028 Uiso 1 1 calc R . . C1 C 0.1727(3) 1.1167(3) 0.71503(12) 0.0212(6) Uani 1 1 d . . . H1B H 0.1859 1.2210 0.7310 0.025 Uiso 1 1 calc R . . H1A H 0.0970 1.0733 0.7301 0.025 Uiso 1 1 calc R . . C7 C 0.4742(3) 0.7624(3) 0.59171(14) 0.0256(7) Uani 1 1 d . . . H7B H 0.4782 0.7101 0.5527 0.031 Uiso 1 1 calc R . . H7A H 0.5488 0.7309 0.6218 0.031 Uiso 1 1 calc R . . O2 O 0.1110(2) 1.3837(2) 0.53921(10) 0.0374(5) Uani 1 1 d . . . H2" H 0.0416 1.3354 0.5331 0.056 Uiso 1 1 calc R . . C21 C 0.1607(3) 1.3985(4) 0.48318(15) 0.0419(9) Uani 1 1 d . . . H21A H 0.2183 1.4875 0.4858 0.050 Uiso 1 1 calc R . . H21B H 0.0887 1.4169 0.4497 0.050 Uiso 1 1 calc R . . C20 C 0.2331(3) 1.2617(4) 0.46836(18) 0.0558(11) Uani 1 1 d . . . H20A H 0.2661 1.2782 0.4300 0.084 Uiso 1 1 calc R . . H20B H 0.1758 1.1738 0.4642 0.084 Uiso 1 1 calc R . . H20C H 0.3050 1.2432 0.5012 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01899(17) 0.02119(16) 0.01781(19) -0.00177(12) 0.00400(14) -0.00106(12) Co1 0.01335(19) 0.01272(16) 0.0145(2) -0.00018(13) 0.00218(15) -0.00076(13) Cl5 0.0232(4) 0.0235(3) 0.0227(4) 0.0017(3) 0.0061(3) 0.0011(3) Cl1 0.0213(4) 0.0222(3) 0.0217(4) 0.0015(3) -0.0030(3) 0.0040(3) Cl4 0.0276(4) 0.0323(4) 0.0177(4) -0.0047(3) 0.0066(3) 0.0006(3) Cl3 0.0347(4) 0.0273(4) 0.0227(4) -0.0064(3) 0.0056(3) -0.0112(3) Cl2 0.0235(4) 0.0380(4) 0.0375(5) 0.0060(3) 0.0062(3) 0.0087(3) N3 0.0214(12) 0.0150(10) 0.0143(12) -0.0015(9) 0.0032(10) -0.0023(9) N5 0.0174(12) 0.0176(10) 0.0189(13) -0.0005(9) 0.0033(10) -0.0004(9) N1 0.0201(12) 0.0162(10) 0.0156(12) -0.0003(8) 0.0031(10) -0.0025(9) N4 0.0163(12) 0.0181(10) 0.0195(13) -0.0019(9) 0.0013(10) 0.0010(9) O1 0.0296(12) 0.0228(10) 0.0308(13) 0.0077(8) 0.0053(10) -0.0014(8) N2 0.0168(12) 0.0178(11) 0.0134(12) -0.0002(9) 0.0037(9) -0.0001(9) C6 0.0323(17) 0.0152(13) 0.0342(19) -0.0021(12) 0.0072(14) 0.0006(12) C4 0.0173(14) 0.0214(13) 0.0237(16) -0.0041(11) 0.0073(12) -0.0084(11) C5 0.0340(18) 0.0120(12) 0.0337(18) -0.0025(11) 0.0096(14) -0.0030(11) C3 0.0155(14) 0.0221(13) 0.0211(16) -0.0036(11) 0.0035(12) -0.0023(11) C2 0.0180(15) 0.0149(12) 0.0281(17) 0.0015(11) 0.0052(12) 0.0016(10) C8 0.0214(15) 0.0308(14) 0.0183(16) -0.0031(12) 0.0062(13) -0.0065(12) C1 0.0247(15) 0.0163(12) 0.0236(17) -0.0017(11) 0.0069(13) 0.0028(11) C7 0.0251(16) 0.0263(14) 0.0275(18) -0.0052(12) 0.0104(14) 0.0010(12) O2 0.0335(13) 0.0454(13) 0.0335(14) 0.0073(10) 0.0057(11) 0.0001(10) C21 0.051(2) 0.0391(18) 0.036(2) 0.0017(15) 0.0072(18) -0.0066(16) C20 0.036(2) 0.076(3) 0.053(3) -0.018(2) 0.0000(19) 0.0095(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl2 2.2327(9) . ? Zn1 Cl3 2.2747(8) . ? Zn1 Cl5 2.2890(8) . ? Zn1 Cl4 2.3323(9) . ? Co1 N4 1.939(2) . ? Co1 N2 1.966(2) . ? Co1 N5 1.968(2) . ? Co1 N3 1.970(2) . ? Co1 N1 1.974(2) . ? Co1 Cl1 2.2664(8) . ? N3 C4 1.488(3) . ? N3 C5 1.515(3) . ? N5 C8 1.497(3) . ? N1 C1 1.480(3) . ? N4 C7 1.474(3) . ? N4 C6 1.484(3) . ? O1 C2 1.397(3) . ? N2 C3 1.501(3) . ? N2 C2 1.508(3) . ? C6 C5 1.503(4) . ? C4 C3 1.510(4) . ? C2 C1 1.503(4) . ? C8 C7 1.499(4) . ? O2 C21 1.430(4) . ? C21 C20 1.494(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Zn1 Cl3 112.44(3) . . ? Cl2 Zn1 Cl5 115.05(3) . . ? Cl3 Zn1 Cl5 104.21(3) . . ? Cl2 Zn1 Cl4 108.98(3) . . ? Cl3 Zn1 Cl4 106.97(3) . . ? Cl5 Zn1 Cl4 108.81(3) . . ? N4 Co1 N2 94.07(9) . . ? N4 Co1 N5 85.13(9) . . ? N2 Co1 N5 94.17(9) . . ? N4 Co1 N3 85.07(9) . . ? N2 Co1 N3 86.93(9) . . ? N5 Co1 N3 170.19(8) . . ? N4 Co1 N1 178.46(9) . . ? N2 Co1 N1 84.48(9) . . ? N5 Co1 N1 94.45(9) . . ? N3 Co1 N1 95.36(9) . . ? N4 Co1 Cl1 94.45(7) . . ? N2 Co1 Cl1 171.09(7) . . ? N5 Co1 Cl1 89.17(7) . . ? N3 Co1 Cl1 91.19(7) . . ? N1 Co1 Cl1 87.03(6) . . ? C4 N3 C5 110.8(2) . . ? C4 N3 Co1 108.98(15) . . ? C5 N3 Co1 110.12(16) . . ? C8 N5 Co1 109.19(15) . . ? C1 N1 Co1 112.95(15) . . ? C7 N4 C6 116.6(2) . . ? C7 N4 Co1 110.11(16) . . ? C6 N4 Co1 108.57(17) . . ? C3 N2 C2 113.87(19) . . ? C3 N2 Co1 109.08(15) . . ? C2 N2 Co1 108.98(15) . . ? N4 C6 C5 106.6(2) . . ? N3 C4 C3 107.8(2) . . ? C6 C5 N3 110.7(2) . . ? N2 C3 C4 110.2(2) . . ? O1 C2 C1 110.4(2) . . ? O1 C2 N2 107.4(2) . . ? C1 C2 N2 108.0(2) . . ? N5 C8 C7 107.2(2) . . ? N1 C1 C2 108.4(2) . . ? N4 C7 C8 105.7(2) . . ? O2 C21 C20 112.8(3) . . ? 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 N4 Co1 N3 C4 -112.36(17) . . . . ? N2 Co1 N3 C4 -18.00(16) . . . . ? N5 Co1 N3 C4 -114.7(5) . . . . ? N1 Co1 N3 C4 66.15(17) . . . . ? Cl1 Co1 N3 C4 153.28(15) . . . . ? N4 Co1 N3 C5 9.43(17) . . . . ? N2 Co1 N3 C5 103.79(17) . . . . ? N5 Co1 N3 C5 7.1(6) . . . . ? N1 Co1 N3 C5 -172.06(17) . . . . ? Cl1 Co1 N3 C5 -84.93(16) . . . . ? N4 Co1 N5 C8 9.85(17) . . . . ? N2 Co1 N5 C8 -83.89(17) . . . . ? N3 Co1 N5 C8 12.2(6) . . . . ? N1 Co1 N5 C8 -168.67(16) . . . . ? Cl1 Co1 N5 C8 104.38(16) . . . . ? N4 Co1 N1 C1 21(3) . . . . ? N2 Co1 N1 C1 1.52(17) . . . . ? N5 Co1 N1 C1 95.29(17) . . . . ? N3 Co1 N1 C1 -84.86(17) . . . . ? Cl1 Co1 N1 C1 -175.78(16) . . . . ? N2 Co1 N4 C7 112.84(17) . . . . ? N5 Co1 N4 C7 19.00(17) . . . . ? N3 Co1 N4 C7 -160.60(18) . . . . ? N1 Co1 N4 C7 93(3) . . . . ? Cl1 Co1 N4 C7 -69.79(17) . . . . ? N2 Co1 N4 C6 -118.44(18) . . . . ? N5 Co1 N4 C6 147.72(18) . . . . ? N3 Co1 N4 C6 -31.88(18) . . . . ? N1 Co1 N4 C6 -138(3) . . . . ? Cl1 Co1 N4 C6 58.93(17) . . . . ? N4 Co1 N2 C3 78.11(17) . . . . ? N5 Co1 N2 C3 163.51(16) . . . . ? N3 Co1 N2 C3 -6.72(16) . . . . ? N1 Co1 N2 C3 -102.41(17) . . . . ? Cl1 Co1 N2 C3 -84.7(4) . . . . ? N4 Co1 N2 C2 -157.02(16) . . . . ? N5 Co1 N2 C2 -71.62(16) . . . . ? N3 Co1 N2 C2 118.15(16) . . . . ? N1 Co1 N2 C2 22.46(16) . . . . ? Cl1 Co1 N2 C2 40.1(5) . . . . ? C7 N4 C6 C5 171.7(2) . . . . ? Co1 N4 C6 C5 46.8(3) . . . . ? C5 N3 C4 C3 -83.0(2) . . . . ? Co1 N3 C4 C3 38.4(2) . . . . ? N4 C6 C5 N3 -39.3(3) . . . . ? C4 N3 C5 C6 135.3(2) . . . . ? Co1 N3 C5 C6 14.7(3) . . . . ? C2 N2 C3 C4 -91.9(2) . . . . ? Co1 N2 C3 C4 30.1(2) . . . . ? N3 C4 C3 N2 -45.0(3) . . . . ? C3 N2 C2 O1 -160.8(2) . . . . ? Co1 N2 C2 O1 77.2(2) . . . . ? C3 N2 C2 C1 80.2(3) . . . . ? Co1 N2 C2 C1 -41.8(2) . . . . ? Co1 N5 C8 C7 -36.0(2) . . . . ? Co1 N1 C1 C2 -25.2(2) . . . . ? O1 C2 C1 N1 -74.2(2) . . . . ? N2 C2 C1 N1 42.9(3) . . . . ? C6 N4 C7 C8 -167.4(2) . . . . ? Co1 N4 C7 C8 -43.2(3) . . . . ? N5 C8 C7 N4 50.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.408 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.078