# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1433 data_cjq3 #----------------------------------------------------------------------- _audit_creation_date '1999-09-13' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_requested_journal ' Chem Comm' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Anthony C. Willis ' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_footnote _publ_author_address ' Rodney J. Geue ' ; Research School of Chemistry and Department of Chemistry, Faculty of Science, Australian National University, Canberra, A. C. T. 0200, Australia ; ' C. Jin Qin ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Stephen F. Ralph ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Alan M. Sargeson ' ; Research School of Chemistry and Department of Chemistry, Faculty of Science, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Allan H. White ' ; Department of Chemistry University of Western Australia, Nedlands, W.A. 6009, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; Sterically induced transmutations in cobalt amine chemistry ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Hall, S. R., King, G. S. D. & Stewart, J. M. (1995). Editors. Xtal3.4 Reference Manual. Univ. of Western Australia: Lamb, Perth, Australia. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #----------------------------------------------------------------------- _computing_data_collection ; Philips PW1100/20 software 1976 ; _computing_cell_refinement xtal_LATCON _computing_data_reduction xtal_DIFDAT_ABSORB_ADDREF _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 10.442(3) _cell_length_b 17.347(6) _cell_length_c 17.830(5) _cell_angle_alpha 90 _cell_angle_beta 105.31(2) _cell_angle_gamma 90 _cell_volume 3115(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.0 _cell_measurement_theta_max 16.5 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, -y, -z' ' +x, -y,1/2+z' ' 1/2+x, 1/2+y, +z' ' 1/2-x, 1/2+y, 1/2-z' ' 1/2-x, 1/2-y, -z' ' 1/2+x, 1/2-y, 1/2+z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'pink' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 639.70 _chemical_formula_analytical ? _chemical_formula_sum 'C25 H56 Co N8 O7 ' _chemical_formula_moiety 'C25 H54 Co N6, 2(N O3), (H2 O)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1380.00 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_correction_T_min 0.757 _exptl_special_details ; ? ; #----------------------------------------------------------------------- _diffrn_special_details ; The scan width was (0.9+0.34tan\q)\% with an \w scan speed of 1.5\% per minute. Stationary background counts were recorded for 10 sec at each end of the scan. ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Philips PW1100/20' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 2 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2114 _reflns_number_total 2114 _reflns_number_gt 1296 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 22.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 100 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 224 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Co 0 4 0.299 0.973 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 32 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 28 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Co(1) 0.5000 0.57780(7) 0.7500 0.0244(4) 1.00 ST Uani d ? O(1) 0.0000 0.3189(3) 0.7500 0.090(3) 1.0 ST Uani d ? O(2) 0.1485(6) 0.4451(3) 0.8421(3) 0.116(3) 1.000 . Uani d ? O(3) 0.3492(5) 0.4501(3) 0.9120(3) 0.075(2) 1.000 . Uani d ? O(4) 0.2268(5) 0.3494(3) 0.9118(3) 0.093(2) 1.000 . Uani d ? N(1) 0.2401(7) 0.4153(4) 0.8899(4) 0.066(3) 1.000 . Uani d ? N(12) 0.3064(4) 0.5882(3) 0.7811(3) 0.029(2) 1.000 . Uani d ? N(16) 0.5794(5) 0.6578(3) 0.8470(3) 0.028(2) 1.000 . Uani d ? N(22) 0.4009(5) 0.4845(3) 0.6696(3) 0.028(2) 1.000 . Uani d ? C(1) 0.0647(5) 0.5807(4) 0.5777(3) 0.048(2) 1.000 . Uani d ? C(2) 0.2061(5) 0.5784(4) 0.6341(3) 0.032(2) 1.000 . Uani d ? C(11) 0.1873(5) 0.5702(4) 0.7163(3) 0.035(2) 1.000 . Uani d ? C(13) 0.2973(6) 0.6670(3) 0.8139(3) 0.037(2) 1.000 . Uani d ? C(14) 0.3803(6) 0.6774(3) 0.8983(3) 0.036(2) 1.000 . Uani d ? C(15) 0.5157(6) 0.6408(4) 0.9105(3) 0.038(2) 1.000 . Uani d ? C(17) 0.7283(6) 0.6558(3) 0.8765(3) 0.034(2) 1.000 . Uani d ? C(21) 0.2780(6) 0.5093(3) 0.6104(3) 0.034(2) 1.000 . Uani d ? C(23) 0.3773(5) 0.4185(4) 0.7167(3) 0.040(2) 1.000 . Uani d ? C(24) 0.5000 0.3677(4) 0.7500 0.030(3) 1.0 ST Uani d ? C(141) 0.3923(6) 0.7635(4) 0.9159(4) 0.054(2) 1.000 . Uani d ? C(142) 0.3102(6) 0.6382(4) 0.9541(3) 0.054(2) 1.000 . Uani d ? C(241) 0.5285(6) 0.3160(3) 0.6868(3) 0.049(2) 1.000 . Uani d ? H(1) 0.309(5) 0.550(3) 0.820(3) 0.04(1) 1.000 . Uiso d ? H(2) 0.556(4) 0.722(3) 0.828(3) 0.043 1.000 . Uiso d ? H(3) 0.455(5) 0.474(3) 0.645(3) 0.043 1.000 . Uiso d ? H(4) 0.0161 0.6222 0.5915 0.058 1.000 . Uiso c ? H(5) 0.0711 0.5878 0.5260 0.058 1.000 . Uiso c ? H(6) 0.0204 0.5335 0.5810 0.058 1.000 . Uiso c ? H(7) 0.1179 0.6040 0.7204 0.042 1.000 . Uiso c ? H(8) 0.1621 0.5185 0.7225 0.042 1.000 . Uiso c ? H(9) 0.3268 0.7035 0.7824 0.045 1.000 . Uiso c ? H(10) 0.2069 0.6767 0.8119 0.045 1.000 . Uiso c ? H(11) 0.4445 0.7713 0.9676 0.065 1.000 . Uiso c ? H(12) 0.4334 0.7882 0.8807 0.065 1.000 . Uiso c ? H(13) 0.3063 0.7847 0.9101 0.065 1.000 . Uiso c ? H(14) 0.2246 0.6602 0.9474 0.065 1.000 . Uiso c ? H(15) 0.3017 0.5846 0.9431 0.065 1.000 . Uiso c ? H(16) 0.3611 0.6457 1.0063 0.065 1.000 . Uiso c ? H(17) 0.5062 0.5865 0.9138 0.046 1.000 . Uiso c ? H(18) 0.5717 0.6595 0.9580 0.046 1.000 . Uiso c ? H(19) 0.7511 0.6674 0.9305 0.041 1.000 . Uiso c ? H(20) 0.7634 0.6944 0.8497 0.041 1.000 . Uiso c ? H(21) 0.3018 0.5225 0.5641 0.041 1.000 . Uiso c ? H(22) 0.2181 0.4670 0.6004 0.041 1.000 . Uiso c ? H(23) 0.3100 0.3871 0.6848 0.048 1.000 . Uiso c ? H(24) 0.3474 0.4380 0.7589 0.048 1.000 . Uiso c ? H(25) 0.5478 0.3471 0.6474 0.058 1.000 . Uiso c ? H(26) 0.6024 0.2839 0.7090 0.058 1.000 . Uiso c ? H(27) 0.4529 0.2850 0.6649 0.058 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0237(7) 0.0264(7) 0.0234(7) 0.0000 0.0068(6) 0.0000 O(1) 0.140(7) 0.047(5) 0.094(6) 0.0000 0.049(5) 0.0000 O(2) 0.103(5) 0.129(6) 0.106(5) 0.037(4) 0.013(4) 0.056(4) O(3) 0.098(5) 0.060(4) 0.072(4) -0.010(3) 0.033(4) -0.006(3) O(4) 0.105(5) 0.076(4) 0.095(5) -0.016(4) 0.022(4) 0.037(4) N(1) 0.081(6) 0.070(6) 0.055(5) 0.009(5) 0.034(4) 0.020(5) N(12) 0.028(3) 0.032(4) 0.027(3) -0.001(3) 0.008(2) -0.002(3) N(16) 0.026(3) 0.035(3) 0.025(3) -0.003(3) 0.010(3) -0.004(3) N(22) 0.030(3) 0.025(3) 0.031(3) 0.000(3) 0.010(3) 0.000(3) C(1) 0.034(4) 0.058(4) 0.044(4) -0.002(5) -0.005(3) -0.001(4) C(2) 0.023(3) 0.040(4) 0.029(4) 0.000(4) 0.000(3) 0.003(4) C(11) 0.028(3) 0.041(4) 0.035(4) 0.000(4) 0.007(3) -0.002(4) C(13) 0.027(4) 0.041(4) 0.047(4) 0.009(3) 0.013(3) -0.006(4) C(14) 0.042(4) 0.039(4) 0.028(4) 0.005(4) 0.013(4) -0.007(3) C(15) 0.036(4) 0.051(5) 0.028(4) 0.002(4) 0.010(3) -0.006(3) C(17) 0.041(5) 0.038(4) 0.023(4) -0.012(4) 0.009(3) -0.001(3) C(21) 0.031(4) 0.031(4) 0.037(4) -0.002(3) 0.004(3) -0.001(3) C(23) 0.041(4) 0.031(4) 0.047(4) -0.003(4) 0.010(3) -0.005(4) C(24) 0.039(6) 0.013(5) 0.041(6) 0.0000 0.014(5) 0.0000 C(141) 0.064(5) 0.051(5) 0.049(5) 0.013(4) 0.018(4) -0.016(4) C(142) 0.056(5) 0.074(6) 0.037(4) 0.003(4) 0.020(4) -0.007(4) C(241) 0.057(5) 0.030(4) 0.059(5) 0.006(4) 0.017(4) -0.006(4) #----------------------------------------------------------------------- _refine_special_details ; H atoms attached to N atoms refxyz, H atoms attached to C atoms noref, H atoms of water not located. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.000004|Fo|^2^]' _refine_ls_hydrogen_treatment 'mixed' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1296 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_number_constraints 2 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0320 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.010 _refine_ls_shift/su_max 0.0580 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.30 _refine_diff_density_max 0.25 #----------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co(1) N(12) 2.240(4) . . yes Co(1) N(12) 2.240(4) . 2_656 yes Co(1) N(16) 2.202(5) . . yes Co(1) N(16) 2.202(5) . 2_656 yes Co(1) N(22) 2.228(5) . . yes Co(1) N(22) 2.228(5) . 2_656 yes O(2) N(1) 1.215(7) . . yes O(3) N(1) 1.258(7) . . yes O(4) N(1) 1.228(7) . . yes N(12) C(11) 1.490(6) . . yes N(12) C(13) 1.498(7) . . yes N(12) H(1) 0.94(5) . . no N(16) C(15) 1.486(6) . . yes N(16) C(17) 1.504(7) . . yes N(16) H(2) 1.17(5) . . no N(22) C(21) 1.494(7) . . yes N(22) C(23) 1.478(7) . . yes N(22) H(3) 0.83(5) . . no C(1) C(2) 1.552(6) . . yes C(1) H(4) 0.95 . . no C(1) H(5) 0.95 . . no C(1) H(6) 0.95 . . no C(2) C(11) 1.536(6) . . yes C(2) C(17) 1.541(7) . 2_656 yes C(2) C(21) 1.532(7) . . yes C(11) H(7) 0.95 . . no C(11) H(8) 0.95 . . no C(13) C(14) 1.537(7) . . yes C(13) H(9) 0.95 . . no C(13) H(10) 0.95 . . no C(14) C(15) 1.512(7) . . yes C(14) C(141) 1.524(8) . . yes C(14) C(142) 1.541(7) . . yes C(15) H(17) 0.95 . . no C(15) H(18) 0.95 . . no C(17) H(19) 0.95 . . no C(17) H(20) 0.95 . . no C(21) H(21) 0.95 . . no C(21) H(22) 0.95 . . no C(23) C(24) 1.539(6) . . yes C(23) H(23) 0.95 . . no C(23) H(24) 0.95 . . no C(24) C(241) 1.529(7) . . yes C(24) C(241) 1.529(7) . 2_656 yes C(141) H(11) 0.95 . . no C(141) H(12) 0.95 . . no C(141) H(13) 0.95 . . no C(142) H(14) 0.95 . . no C(142) H(15) 0.95 . . no C(142) H(16) 0.95 . . no C(241) H(25) 0.95 . . no C(241) H(26) 0.95 . . no C(241) H(27) 0.95 . . no #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(12) Co(1) N(12) 170.7(3) . . 2_656 yes N(12) Co(1) N(16) 86.1(2) . . . yes N(12) Co(1) N(16) 88.1(2) . . 2_656 yes N(12) Co(1) N(22) 85.5(2) . . . yes N(12) Co(1) N(22) 101.3(2) . . 2_656 yes N(12) Co(1) N(16) 88.1(2) 2_656 . . yes N(12) Co(1) N(16) 86.1(2) 2_656 . 2_656 yes N(12) Co(1) N(22) 101.3(2) 2_656 . . yes N(12) Co(1) N(22) 85.5(2) 2_656 . 2_656 yes N(16) Co(1) N(16) 101.9(3) . . 2_656 yes N(16) Co(1) N(22) 167.9(2) . . . yes N(16) Co(1) N(22) 86.4(2) . . 2_656 yes N(16) Co(1) N(22) 86.4(2) 2_656 . . yes N(16) Co(1) N(22) 167.9(2) 2_656 . 2_656 yes N(22) Co(1) N(22) 86.8(3) . . 2_656 yes O(2) N(1) O(3) 119.7(8) . . . yes O(2) N(1) O(4) 119.0(8) . . . yes O(3) N(1) O(4) 121.0(8) . . . yes Co(1) N(12) C(11) 114.4(3) . . . yes Co(1) N(12) C(13) 108.9(3) . . . yes Co(1) N(12) H(1) 106(3) . . . no C(11) N(12) C(13) 111.6(5) . . . yes C(11) N(12) H(1) 106(3) . . . no C(13) N(12) H(1) 110(3) . . . no Co(1) N(16) C(15) 108.8(3) . . . yes Co(1) N(16) C(17) 113.6(3) . . . yes Co(1) N(16) H(2) 112(2) . . . no C(15) N(16) C(17) 111.0(4) . . . yes C(15) N(16) H(2) 108(2) . . . no C(17) N(16) H(2) 104(2) . . . no Co(1) N(22) C(21) 114.3(4) . . . yes Co(1) N(22) C(23) 108.5(3) . . . yes Co(1) N(22) H(3) 104(4) . . . no C(21) N(22) C(23) 112.6(4) . . . yes C(21) N(22) H(3) 105(4) . . . no C(23) N(22) H(3) 112(4) . . . no C(2) C(1) H(4) 109.5 . . . no C(2) C(1) H(5) 109.5 . . . no C(2) C(1) H(6) 109.5 . . . no H(4) C(1) H(5) 109.5 . . . no H(4) C(1) H(6) 109.5 . . . no H(5) C(1) H(6) 109.5 . . . no C(1) C(2) C(11) 106.4(4) . . . yes C(1) C(2) C(17) 106.0(5) . . 2_656 yes C(1) C(2) C(21) 107.0(5) . . . yes C(11) C(2) C(17) 111.8(5) . . 2_656 yes C(11) C(2) C(21) 112.7(5) . . . yes C(17) C(2) C(21) 112.4(4) 2_656 . . yes N(12) C(11) C(2) 115.5(4) . . . yes N(12) C(11) H(7) 108.0 . . . no N(12) C(11) H(8) 108.0 . . . no C(2) C(11) H(7) 108.0 . . . no C(2) C(11) H(8) 108.0 . . . no H(7) C(11) H(8) 109.5 . . . no N(12) C(13) C(14) 114.3(5) . . . yes N(12) C(13) H(9) 108.2 . . . no N(12) C(13) H(10) 108.2 . . . no C(14) C(13) H(9) 108.2 . . . no C(14) C(13) H(10) 108.2 . . . no H(9) C(13) H(10) 109.5 . . . no C(13) C(14) C(15) 110.8(5) . . . yes C(13) C(14) C(141) 108.1(5) . . . yes C(13) C(14) C(142) 109.8(5) . . . yes C(15) C(14) C(141) 111.1(5) . . . yes C(15) C(14) C(142) 107.9(5) . . . yes C(141) C(14) C(142) 109.1(5) . . . yes N(16) C(15) C(14) 113.4(5) . . . yes N(16) C(15) H(17) 108.5 . . . no N(16) C(15) H(18) 108.5 . . . no C(14) C(15) H(17) 108.5 . . . no C(14) C(15) H(18) 108.5 . . . no H(17) C(15) H(18) 109.5 . . . no N(16) C(17) C(2) 115.4(5) . . 2_656 yes N(16) C(17) H(19) 108.0 . . . no N(16) C(17) H(20) 108.0 . . . no C(2) C(17) H(19) 108.0 2_656 . . no C(2) C(17) H(20) 108.0 2_656 . . no H(19) C(17) H(20) 109.5 . . . no N(22) C(21) C(2) 115.0(5) . . . yes N(22) C(21) H(21) 108.1 . . . no N(22) C(21) H(22) 108.1 . . . no C(2) C(21) H(21) 108.1 . . . no C(2) C(21) H(22) 108.1 . . . no H(21) C(21) H(22) 109.5 . . . no N(22) C(23) C(24) 114.5(4) . . . yes N(22) C(23) H(23) 108.2 . . . no N(22) C(23) H(24) 108.2 . . . no C(24) C(23) H(23) 108.2 . . . no C(24) C(23) H(24) 108.2 . . . no H(23) C(23) H(24) 109.5 . . . no C(23) C(24) C(23) 110.2(6) . . 2_656 yes C(23) C(24) C(241) 110.8(3) . . . yes C(23) C(24) C(241) 108.4(3) . . 2_656 yes C(23) C(24) C(241) 108.4(3) 2_656 . . yes C(23) C(24) C(241) 110.8(3) 2_656 . 2_656 yes C(241) C(24) C(241) 108.2(6) . . 2_656 yes C(14) C(141) H(11) 109.5 . . . no C(14) C(141) H(12) 109.5 . . . no C(14) C(141) H(13) 109.5 . . . no H(11) C(141) H(12) 109.5 . . . no H(11) C(141) H(13) 109.5 . . . no H(12) C(141) H(13) 109.5 . . . no C(14) C(142) H(14) 109.5 . . . no C(14) C(142) H(15) 109.5 . . . no C(14) C(142) H(16) 109.5 . . . no H(14) C(142) H(15) 109.5 . . . no H(14) C(142) H(16) 109.5 . . . no H(15) C(142) H(16) 109.5 . . . no C(24) C(241) H(25) 109.5 . . . no C(24) C(241) H(26) 109.5 . . . no C(24) C(241) H(27) 109.5 . . . no H(25) C(241) H(26) 109.5 . . . no H(25) C(241) H(27) 109.5 . . . no H(26) C(241) H(27) 109.5 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(2) 2.924(7) . . no O(1) O(2) 2.924(7) . 2_556 no O(1) O(4) 3.256(5) . . no O(1) O(4) 3.256(5) . 2_556 no O(1) N(16) 3.277(7) . 5_445 no O(1) N(16) 3.277(7) . 6_546 no O(1) N(1) 3.464(8) . . no O(1) N(1) 3.464(8) . 2_556 no O(1) C(141) 3.562(7) . 5_445 no O(1) C(141) 3.562(7) . 6_546 no O(2) C(11) 3.223(8) . . no O(2) N(12) 3.318(7) . . no O(3) N(12) 3.292(7) . . no O(3) N(22) 3.360(7) . 2_656 no O(3) C(241) 3.366(7) . 2_656 no O(3) C(142) 3.398(8) . . no O(3) C(15) 3.483(8) . 3_667 no O(4) C(17) 3.418(8) . 5_445 no O(4) C(241) 3.512(8) . 2_656 no O(4) C(15) 3.577(8) . 3_667 no N(1) C(241) 3.525(9) . 2_656 no #----------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Co(1) N(12) C(11) C(2) . . . . -22.8(7) no Co(1) N(12) C(13) C(14) . . . . -77.0(5) no Co(1) N(12) C(11) C(2) . 2_656 2_656 2_656 -22.8(7) no Co(1) N(12) C(13) C(14) . 2_656 2_656 2_656 -77.0(5) no Co(1) N(16) C(15) C(14) . . . . -82.1(5) no Co(1) N(16) C(17) C(2) . . . 2_656 -28.2(6) no Co(1) N(16) C(15) C(14) . 2_656 2_656 2_656 -82.1(5) no Co(1) N(16) C(17) C(2) . 2_656 2_656 . -28.2(6) no Co(1) N(22) C(21) C(2) . . . . -26.1(6) no Co(1) N(22) C(23) C(24) . . . . -79.2(4) no Co(1) N(22) C(21) C(2) . 2_656 2_656 2_656 -26.1(6) no Co(1) N(22) C(23) C(24) . 2_656 2_656 . -79.2(4) no N(12) Co(1) N(12) C(11) . . 2_656 2_656 105.5(4) no N(12) Co(1) N(12) C(13) . . 2_656 2_656 -20.1(3) no N(12) Co(1) N(16) C(15) . . . . 35.8(4) no N(12) Co(1) N(16) C(17) . . . . 160.1(4) no N(12) Co(1) N(16) C(15) . . 2_656 2_656 -151.4(4) no N(12) Co(1) N(16) C(17) . . 2_656 2_656 -27.1(4) no N(12) Co(1) N(22) C(21) . . . . 58.2(4) no N(12) Co(1) N(22) C(23) . . . . -68.3(4) no N(12) Co(1) N(22) C(21) . . 2_656 2_656 -115.4(4) no N(12) Co(1) N(22) C(23) . . 2_656 2_656 118.1(3) no N(12) C(11) C(2) C(1) . . . . -163.9(5) no N(12) C(11) C(2) C(17) . . . 2_656 -48.6(7) no N(12) C(11) C(2) C(21) . . . . 79.1(7) no N(12) C(13) C(14) C(15) . . . . 42.6(7) no N(12) C(13) C(14) C(141) . . . . 164.6(5) no N(12) C(13) C(14) C(142) . . . . -76.5(6) no N(16) Co(1) N(12) C(11) . . . . 156.6(4) no N(16) Co(1) N(12) C(13) . . . . 31.0(4) no N(16) Co(1) N(12) C(11) . . 2_656 2_656 54.6(4) no N(16) Co(1) N(12) C(13) . . 2_656 2_656 -71.1(4) no N(16) Co(1) N(16) C(15) . . 2_656 2_656 123.0(4) no N(16) Co(1) N(16) C(17) . . 2_656 2_656 -112.7(4) no N(16) Co(1) N(22) C(21) . . . . 104(1) no N(16) Co(1) N(22) C(23) . . . . -22(1) no N(16) Co(1) N(22) C(21) . . 2_656 2_656 -30.1(4) no N(16) Co(1) N(22) C(23) . . 2_656 2_656 -156.6(4) no N(16) C(15) C(14) C(13) . . . . 44.4(7) no N(16) C(15) C(14) C(141) . . . . -75.9(6) no N(16) C(15) C(14) C(142) . . . . 164.6(5) no N(16) C(17) C(2) C(1) . . 2_656 2_656 -162.0(4) no N(16) C(17) C(2) C(11) . . 2_656 2_656 82.5(6) no N(16) C(17) C(2) C(21) . . 2_656 2_656 -45.4(6) no N(22) Co(1) N(12) C(11) . . . . -32.0(4) no N(22) Co(1) N(12) C(13) . . . . -157.6(4) no N(22) Co(1) N(12) C(11) . . 2_656 2_656 -117.8(4) no N(22) Co(1) N(12) C(13) . . 2_656 2_656 116.6(4) no N(22) Co(1) N(16) C(15) . . . . -10(1) no N(22) Co(1) N(16) C(17) . . . . 114.2(9) no N(22) Co(1) N(16) C(15) . . 2_656 2_656 -65.7(4) no N(22) Co(1) N(16) C(17) . . 2_656 2_656 58.5(4) no N(22) Co(1) N(22) C(21) . . 2_656 2_656 159.8(5) no N(22) Co(1) N(22) C(23) . . 2_656 2_656 33.3(3) no N(22) C(21) C(2) C(1) . . . . -164.3(5) no N(22) C(21) C(2) C(11) . . . . -47.8(7) no N(22) C(21) C(2) C(17) . . . 2_656 79.7(6) no N(22) C(23) C(24) C(23) . . . 2_656 44.0(3) no N(22) C(23) C(24) C(241) . . . . -76.0(6) no N(22) C(23) C(24) C(241) . . . 2_656 165.4(5) no C(2) C(11) N(12) C(13) . . . . 101.4(6) no C(2) C(17) N(16) C(15) . 2_656 2_656 2_656 94.8(5) no C(2) C(21) N(22) C(23) . . . . 98.3(5) no C(11) N(12) C(13) C(14) . . . . 155.7(5) no C(14) C(15) N(16) C(17) . . . . 152.2(5) no C(21) N(22) C(23) C(24) . . . . 153.3(5) no #----------------------------------------------------------------------- #===END data_cjq14 #----------------------------------------------------------------------- _audit_creation_date '1999-09-13' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------- _publ_requested_journal ' Chem Comm' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Anthony C. Willis ' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_footnote _publ_author_address ' Rodney J. Geue ' ; Research School of Chemistry and Department of Chemistry, Faculty of Science, Australian National University, Canberra, A. C. T. 0200, Australia ; ' C. Jin Qin ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Stephen F. Ralph ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Alan M. Sargeson ' ; Research School of Chemistry and Department of Chemistry, Faculty of Science, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Allan H. White ' ; Department of Chemistry University of Western Australia, Nedlands, W.A. 6009, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; Sterically induced transmutations in cobalt amine chemistry ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------- _cell_length_a 10.733(4) _cell_length_b 19.038(4) _cell_length_c 15.678(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3204(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.9 _cell_measurement_theta_max 15.8 #----------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_Int_Tables_number 60 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2-y,1/2+z' '1/2+x,1/2-y, -z' ' -x, +y,1/2-z' ' -x, -y, -z' '1/2+x,1/2+y,1/2-z' '1/2-x,1/2+y, +z' ' +x, -y,1/2+z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'wedge' _exptl_crystal_colour 'violet' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 704.87 _chemical_formula_analytical ? _chemical_formula_sum 'C25 H54 Cl4 Co N6 Zn ' _chemical_formula_moiety 'C25 H54 Co N6, (Cl4 Zn)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1484.00 _exptl_absorpt_coefficient_mu 1.626 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_correction_T_min 0.788 _exptl_special_details ; The scan width was (1.20+0.34tan\q)\% with an \w scan speed of 2\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #----------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.97 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 5 2 -2 0 6 2 0 6 _diffrn_reflns_number 3218 _reflns_number_total 3218 _reflns_number_gt 1609 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.07200 _diffrn_orient_matrix_UB_12 0.03161 _diffrn_orient_matrix_UB_13 0.01289 _diffrn_orient_matrix_UB_21 0.05840 _diffrn_orient_matrix_UB_22 -0.04063 _diffrn_orient_matrix_UB_23 -0.00593 _diffrn_orient_matrix_UB_31 0.00935 _diffrn_orient_matrix_UB_32 0.01043 _diffrn_orient_matrix_UB_33 -0.06218 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 100 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 216 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co 0 4 0.299 0.973 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 24 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Zn 0 4 0.222 1.431 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Zn(1) 0.0000 0.14791(4) 0.7500 0.0286(2) 1.0 ST Uani d ? Co(1) 0.0000 0.16264(4) 0.2500 0.0235(3) 1.0 ST Uani d ? Cl(1) 0.1072(1) 0.21579(7) 0.65565(9) 0.0424(4) 1.000 . Uani d ? Cl(2) 0.1238(1) 0.07645(7) 0.82964(9) 0.0439(5) 1.000 . Uani d ? N(12) 0.0077(5) 0.1347(2) 0.1182(3) 0.026(1) 1.000 . Uani d ? N(16) 0.1755(4) 0.0887(2) 0.2570(3) 0.025(1) 1.000 . Uani d ? N(22) -0.1372(4) 0.2454(2) 0.2205(3) 0.024(1) 1.000 . Uani d ? C(1) -0.3222(5) 0.1615(3) 0.0379(3) 0.037(2) 1.000 . Uani d ? C(2) -0.2217(5) 0.1603(3) 0.1072(3) 0.025(2) 1.000 . Uani d ? C(11) -0.0949(5) 0.1604(3) 0.0630(3) 0.030(2) 1.000 . Uani d ? C(13) 0.1281(5) 0.1405(3) 0.0714(3) 0.033(2) 1.000 . Uani d ? C(14) 0.2242(5) 0.0857(3) 0.0973(3) 0.028(2) 1.000 . Uani d ? C(15) 0.2689(5) 0.0966(3) 0.1886(3) 0.030(2) 1.000 . Uani d ? C(17) 0.2398(5) 0.0920(3) 0.3414(3) 0.031(2) 1.000 . Uani d ? C(21) -0.2417(5) 0.2249(2) 0.1620(3) 0.028(1) 1.000 . Uani d ? C(23) -0.0673(5) 0.3061(3) 0.1837(3) 0.031(2) 1.000 . Uani d ? C(24) 0.0000 0.3510(3) 0.2500 0.032(2) 1.0 ST Uani d ? C(141) 0.1737(5) 0.0114(3) 0.0826(3) 0.040(2) 1.000 . Uani d ? C(142) 0.3373(6) 0.0972(3) 0.0383(4) 0.047(2) 1.000 . Uani d ? C(241) -0.0922(6) 0.3980(3) 0.2987(4) 0.047(2) 1.000 . Uani d ? H(1) -0.007(6) 0.095(2) 0.129(3) 0.031 1.000 . Uiso d ? H(2) 0.152(4) 0.042(2) 0.251(3) 0.029 1.000 . Uiso d ? H(3) -0.172(4) 0.260(2) 0.264(3) 0.029 1.000 . Uiso d ? H(4) -0.3144 0.2034 0.0053 0.045 1.000 . Uiso c ? H(5) -0.3122 0.1220 0.0017 0.045 1.000 . Uiso c ? H(6) -0.4022 0.1601 0.0638 0.045 1.000 . Uiso c ? H(7) -0.0763 0.2071 0.0459 0.037 1.000 . Uiso c ? H(8) -0.0997 0.1311 0.0141 0.037 1.000 . Uiso c ? H(9) 0.1118 0.1354 0.0122 0.040 1.000 . Uiso c ? H(10) 0.1620 0.1858 0.0820 0.040 1.000 . Uiso c ? H(11) 0.1041 0.0035 0.1188 0.048 1.000 . Uiso c ? H(12) 0.1487 0.0065 0.0248 0.048 1.000 . Uiso c ? H(13) 0.2369 -0.0220 0.0952 0.048 1.000 . Uiso c ? H(14) 0.4004 0.0640 0.0518 0.056 1.000 . Uiso c ? H(15) 0.3125 0.0914 -0.0194 0.056 1.000 . Uiso c ? H(16) 0.3689 0.1434 0.0463 0.056 1.000 . Uiso c ? H(17) 0.3018 0.1428 0.1924 0.036 1.000 . Uiso c ? H(18) 0.3333 0.0635 0.1991 0.036 1.000 . Uiso c ? H(19) 0.3265 0.0862 0.3317 0.037 1.000 . Uiso c ? H(20) 0.2098 0.0542 0.3752 0.037 1.000 . Uiso c ? H(21) -0.3133 0.2167 0.1962 0.033 1.000 . Uiso c ? H(22) -0.2568 0.2633 0.1248 0.033 1.000 . Uiso c ? H(23) -0.0072 0.2883 0.1449 0.037 1.000 . Uiso c ? H(24) -0.1247 0.3351 0.1540 0.037 1.000 . Uiso c ? H(25) -0.1498 0.3694 0.3288 0.057 1.000 . Uiso c ? H(26) -0.0479 0.4267 0.3378 0.057 1.000 . Uiso c ? H(27) -0.1359 0.4269 0.2593 0.057 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn(1) 0.0311(5) 0.0233(4) 0.0314(5) 0.0000 -0.0010(6) 0.0000 Co(1) 0.0274(6) 0.0216(5) 0.0215(5) 0.0000 0.0000(6) 0.0000 Cl(1) 0.050(1) 0.0455(9) 0.0321(8) -0.0185(8) 0.0006(8) 0.0025(7) Cl(2) 0.046(1) 0.0370(8) 0.0487(9) 0.0108(8) -0.0051(9) 0.0078(8) N(12) 0.027(3) 0.027(2) 0.025(2) 0.007(3) 0.003(3) 0.005(2) N(16) 0.030(2) 0.020(2) 0.023(2) 0.000(2) 0.000(3) 0.001(3) N(22) 0.026(3) 0.018(2) 0.029(2) -0.001(2) 0.001(2) -0.002(2) C(1) 0.035(4) 0.043(4) 0.034(3) 0.000(3) -0.011(3) -0.002(3) C(2) 0.029(3) 0.026(3) 0.021(3) 0.002(3) -0.002(3) -0.002(3) C(11) 0.039(4) 0.031(3) 0.022(3) 0.004(3) -0.005(3) -0.004(3) C(13) 0.036(4) 0.033(3) 0.031(3) -0.001(3) 0.005(3) 0.007(3) C(14) 0.026(3) 0.029(3) 0.030(3) 0.003(3) 0.003(3) -0.003(3) C(15) 0.025(3) 0.029(3) 0.035(3) 0.003(3) 0.001(3) 0.002(3) C(17) 0.033(3) 0.030(3) 0.029(3) 0.004(3) -0.004(3) 0.006(3) C(21) 0.026(3) 0.026(3) 0.031(3) 0.004(3) -0.002(3) 0.001(3) C(23) 0.033(4) 0.026(3) 0.034(3) 0.002(3) -0.007(3) 0.005(3) C(24) 0.033(4) 0.015(3) 0.048(5) 0.0000 -0.006(6) 0.0000 C(141) 0.040(4) 0.033(3) 0.047(4) 0.003(3) 0.002(3) -0.008(3) C(142) 0.038(4) 0.059(4) 0.044(4) 0.003(4) 0.006(3) -0.003(3) C(241) 0.049(4) 0.032(3) 0.062(4) 0.008(3) -0.002(4) -0.016(3) #----------------------------------------------------------------------- _refine_special_details ; H atoms attached to N atoms refxyz, H atoms attached to C atoms noref. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.000006|Fo|^2^]' _refine_ls_hydrogen_treatment 'mixed' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1609 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0289 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.748 _refine_ls_shift/su_max 0.0720 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.46 _refine_diff_density_max 0.35 #----------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn(1) Cl(1) 2.276(1) . . yes Zn(1) Cl(1) 2.276(1) . 4_556 yes Zn(1) Cl(2) 2.275(2) . . yes Zn(1) Cl(2) 2.275(2) . 4_556 yes Co(1) N(12) 2.135(4) . . yes Co(1) N(12) 2.135(4) . 4 yes Co(1) N(16) 2.355(4) . . yes Co(1) N(16) 2.355(4) . 4 yes Co(1) N(22) 2.206(4) . . yes Co(1) N(22) 2.206(4) . 4 yes N(12) C(11) 1.485(7) . . yes N(12) C(13) 1.490(7) . . yes N(12) H(1) 0.79(4) . . no N(16) C(15) 1.476(7) . . yes N(16) C(17) 1.494(7) . . yes N(16) H(2) 0.93(4) . . no N(22) C(21) 1.500(6) . . yes N(22) C(23) 1.493(6) . . yes N(22) H(3) 0.82(4) . . no C(1) C(2) 1.531(7) . . yes C(1) H(4) 0.95 . . no C(1) H(5) 0.95 . . no C(1) H(6) 0.95 . . no C(2) C(11) 1.528(7) . . yes C(2) C(17) 1.542(7) . 4 yes C(2) C(21) 1.514(6) . . yes C(11) H(7) 0.95 . . no C(11) H(8) 0.95 . . no C(13) C(14) 1.521(7) . . yes C(13) H(9) 0.95 . . no C(13) H(10) 0.95 . . no C(14) C(15) 1.524(7) . . yes C(14) C(141) 1.533(7) . . yes C(14) C(142) 1.542(7) . . yes C(15) H(17) 0.95 . . no C(15) H(18) 0.95 . . no C(17) H(19) 0.95 . . no C(17) H(20) 0.95 . . no C(21) H(21) 0.95 . . no C(21) H(22) 0.95 . . no C(23) C(24) 1.527(6) . . yes C(23) H(23) 0.95 . . no C(23) H(24) 0.95 . . no C(24) C(241) 1.536(6) . . yes C(24) C(241) 1.536(6) . 4 yes C(141) H(11) 0.95 . . no C(141) H(12) 0.95 . . no C(141) H(13) 0.95 . . no C(142) H(14) 0.95 . . no C(142) H(15) 0.95 . . no C(142) H(16) 0.95 . . no C(241) H(25) 0.95 . . no C(241) H(26) 0.95 . . no C(241) H(27) 0.95 . . no #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Zn(1) Cl(1) 110.82(8) . . 4_556 yes Cl(1) Zn(1) Cl(2) 113.63(6) . . . yes Cl(1) Zn(1) Cl(2) 106.14(5) . . 4_556 yes Cl(1) Zn(1) Cl(2) 106.14(5) 4_556 . . yes Cl(1) Zn(1) Cl(2) 113.63(6) 4_556 . 4_556 yes Cl(2) Zn(1) Cl(2) 106.56(8) . . 4_556 yes N(12) Co(1) N(12) 151.1(2) . . 4 yes N(12) Co(1) N(16) 82.2(2) . . . yes N(12) Co(1) N(16) 80.6(2) . . 4 yes N(12) Co(1) N(22) 90.1(2) . . . yes N(12) Co(1) N(22) 110.8(2) . . 4 yes N(12) Co(1) N(16) 80.6(2) 4 . . yes N(12) Co(1) N(16) 82.2(2) 4 . 4 yes N(12) Co(1) N(22) 110.8(2) 4 . . yes N(12) Co(1) N(22) 90.1(2) 4 . 4 yes N(16) Co(1) N(16) 106.5(2) . . 4 yes N(16) Co(1) N(22) 166.2(2) . . . yes N(16) Co(1) N(22) 83.3(1) . . 4 yes N(16) Co(1) N(22) 83.3(1) 4 . . yes N(16) Co(1) N(22) 166.2(2) 4 . 4 yes N(22) Co(1) N(22) 88.8(2) . . 4 yes Co(1) N(12) C(11) 117.0(3) . . . yes Co(1) N(12) C(13) 119.5(4) . . . yes Co(1) N(12) H(1) 91(3) . . . no C(11) N(12) C(13) 109.4(4) . . . yes C(11) N(12) H(1) 107(4) . . . no C(13) N(12) H(1) 110(4) . . . no Co(1) N(16) C(15) 116.7(3) . . . yes Co(1) N(16) C(17) 112.7(3) . . . yes Co(1) N(16) H(2) 110(3) . . . no C(15) N(16) C(17) 109.0(4) . . . yes C(15) N(16) H(2) 102(3) . . . no C(17) N(16) H(2) 105(3) . . . no Co(1) N(22) C(21) 116.2(3) . . . yes Co(1) N(22) C(23) 107.3(3) . . . yes Co(1) N(22) H(3) 112(3) . . . no C(21) N(22) C(23) 110.0(4) . . . yes C(21) N(22) H(3) 104(3) . . . no C(23) N(22) H(3) 106(3) . . . no C(2) C(1) H(4) 109.4 . . . no C(2) C(1) H(5) 109.5 . . . no C(2) C(1) H(6) 109.5 . . . no H(4) C(1) H(5) 109.5 . . . no H(4) C(1) H(6) 109.4 . . . no H(5) C(1) H(6) 109.5 . . . no C(1) C(2) C(11) 107.8(4) . . . yes C(1) C(2) C(17) 107.1(4) . . 4 yes C(1) C(2) C(21) 106.9(4) . . . yes C(11) C(2) C(17) 110.5(4) . . 4 yes C(11) C(2) C(21) 112.5(4) . . . yes C(17) C(2) C(21) 111.8(4) 4 . . yes N(12) C(11) C(2) 113.3(4) . . . yes N(12) C(11) H(7) 108.5 . . . no N(12) C(11) H(8) 108.5 . . . no C(2) C(11) H(7) 108.5 . . . no C(2) C(11) H(8) 108.5 . . . no H(7) C(11) H(8) 109.4 . . . no N(12) C(13) C(14) 113.9(4) . . . yes N(12) C(13) H(9) 108.3 . . . no N(12) C(13) H(10) 108.3 . . . no C(14) C(13) H(9) 108.4 . . . no C(14) C(13) H(10) 108.4 . . . no H(9) C(13) H(10) 109.5 . . . no C(13) C(14) C(15) 111.8(4) . . . yes C(13) C(14) C(141) 110.7(4) . . . yes C(13) C(14) C(142) 106.1(4) . . . yes C(15) C(14) C(141) 112.2(4) . . . yes C(15) C(14) C(142) 107.2(4) . . . yes C(141) C(14) C(142) 108.6(4) . . . yes N(16) C(15) C(14) 117.1(5) . . . yes N(16) C(15) H(17) 107.5 . . . no N(16) C(15) H(18) 107.5 . . . no C(14) C(15) H(17) 107.6 . . . no C(14) C(15) H(18) 107.6 . . . no H(17) C(15) H(18) 109.4 . . . no N(16) C(17) C(2) 116.1(4) . . 4 yes N(16) C(17) H(19) 107.8 . . . no N(16) C(17) H(20) 107.8 . . . no C(2) C(17) H(19) 107.8 4 . . no C(2) C(17) H(20) 107.8 4 . . no H(19) C(17) H(20) 109.5 . . . no N(22) C(21) C(2) 116.9(4) . . . yes N(22) C(21) H(21) 107.6 . . . no N(22) C(21) H(22) 107.6 . . . no C(2) C(21) H(21) 107.6 . . . no C(2) C(21) H(22) 107.6 . . . no H(21) C(21) H(22) 109.4 . . . no N(22) C(23) C(24) 114.1(4) . . . yes N(22) C(23) H(23) 108.3 . . . no N(22) C(23) H(24) 108.3 . . . no C(24) C(23) H(23) 108.3 . . . no C(24) C(23) H(24) 108.3 . . . no H(23) C(23) H(24) 109.4 . . . no C(23) C(24) C(23) 111.9(5) . . 4 yes C(23) C(24) C(241) 111.0(3) . . . yes C(23) C(24) C(241) 107.0(3) . . 4 yes C(23) C(24) C(241) 107.0(3) 4 . . yes C(23) C(24) C(241) 111.0(3) 4 . 4 yes C(241) C(24) C(241) 108.9(6) . . 4 yes C(14) C(141) H(11) 109.5 . . . no C(14) C(141) H(12) 109.5 . . . no C(14) C(141) H(13) 109.5 . . . no H(11) C(141) H(12) 109.5 . . . no H(11) C(141) H(13) 109.5 . . . no H(12) C(141) H(13) 109.5 . . . no C(14) C(142) H(14) 109.5 . . . no C(14) C(142) H(15) 109.5 . . . no C(14) C(142) H(16) 109.5 . . . no H(14) C(142) H(15) 109.5 . . . no H(14) C(142) H(16) 109.4 . . . no H(15) C(142) H(16) 109.5 . . . no C(24) C(241) H(25) 109.5 . . . no C(24) C(241) H(26) 109.5 . . . no C(24) C(241) H(27) 109.4 . . . no H(25) C(241) H(26) 109.5 . . . no H(25) C(241) H(27) 109.5 . . . no H(26) C(241) H(27) 109.5 . . . no #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) N(22) 3.441(4) . 3_556 no Cl(1) C(21) 3.476(5) . 3_556 no Cl(1) C(11) 3.589(5) . 4 no Cl(2) N(16) 3.389(4) . 8 no Cl(2) C(17) 3.444(6) . 8 no #----------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Co(1) N(12) C(11) C(2) . . . . -37.1(5) no Co(1) N(12) C(13) C(14) . . . . 70.9(5) no Co(1) N(12) C(11) C(2) . 4 4 4 -37.1(5) no Co(1) N(12) C(13) C(14) . 4 4 4 70.9(5) no Co(1) N(16) C(15) C(14) . . . . -58.3(5) no Co(1) N(16) C(17) C(2) . . . 4 -25.1(5) no Co(1) N(16) C(15) C(14) . 4 4 4 -58.3(5) no Co(1) N(16) C(17) C(2) . 4 4 . -25.1(5) no Co(1) N(22) C(21) C(2) . . . . -19.5(5) no Co(1) N(22) C(23) C(24) . . . . -78.1(4) no Co(1) N(22) C(21) C(2) . 4 4 4 -19.5(5) no Co(1) N(22) C(23) C(24) . 4 4 . -78.1(4) no N(12) Co(1) N(12) C(11) . . 4 4 120.9(4) no N(12) Co(1) N(12) C(13) . . 4 4 -103.5(3) no N(12) Co(1) N(16) C(15) . . . . 43.4(4) no N(12) Co(1) N(16) C(17) . . . . 170.6(3) no N(12) Co(1) N(16) C(15) . . 4 4 -159.9(4) no N(12) Co(1) N(16) C(17) . . 4 4 -32.7(3) no N(12) Co(1) N(22) C(21) . . . . 45.6(3) no N(12) Co(1) N(22) C(23) . . . . -77.9(3) no N(12) Co(1) N(22) C(21) . . 4 4 -114.0(3) no N(12) Co(1) N(22) C(23) . . 4 4 122.6(3) no N(12) C(11) C(2) C(1) . . . . -159.8(4) no N(12) C(11) C(2) C(17) . . . 4 -43.1(6) no N(12) C(11) C(2) C(21) . . . . 82.6(5) no N(12) C(13) C(14) C(15) . . . . -67.1(6) no N(12) C(13) C(14) C(141) . . . . 58.7(6) no N(12) C(13) C(14) C(142) . . . . 176.4(4) no N(16) Co(1) N(12) C(11) . . . . 174.9(4) no N(16) Co(1) N(12) C(13) . . . . -49.5(3) no N(16) Co(1) N(12) C(11) . . 4 4 66.6(4) no N(16) Co(1) N(12) C(13) . . 4 4 -157.8(4) no N(16) Co(1) N(16) C(15) . . 4 4 121.1(4) no N(16) Co(1) N(16) C(17) . . 4 4 -111.6(3) no N(16) Co(1) N(22) C(21) . . . . 101.4(7) no N(16) Co(1) N(22) C(23) . . . . -22.1(8) no N(16) Co(1) N(22) C(21) . . 4 4 -34.9(3) no N(16) Co(1) N(22) C(23) . . 4 4 -158.4(3) no N(16) C(15) C(14) C(13) . . . . 63.8(6) no N(16) C(15) C(14) C(141) . . . . -61.2(6) no N(16) C(15) C(14) C(142) . . . . 179.6(4) no N(16) C(17) C(2) C(1) . . 4 4 -164.0(4) no N(16) C(17) C(2) C(11) . . 4 4 78.8(5) no N(16) C(17) C(2) C(21) . . 4 4 -47.2(6) no N(22) Co(1) N(12) C(11) . . . . -16.6(4) no N(22) Co(1) N(12) C(13) . . . . 119.0(4) no N(22) Co(1) N(12) C(11) . . 4 4 -105.4(4) no N(22) Co(1) N(12) C(13) . . 4 4 30.2(4) no N(22) Co(1) N(16) C(15) . . . . -13.2(8) no N(22) Co(1) N(16) C(17) . . . . 114.0(7) no N(22) Co(1) N(16) C(15) . . 4 4 -68.8(3) no N(22) Co(1) N(16) C(17) . . 4 4 58.5(3) no N(22) Co(1) N(22) C(21) . . 4 4 156.4(4) no N(22) Co(1) N(22) C(23) . . 4 4 32.9(2) no N(22) C(21) C(2) C(1) . . . . -165.1(4) no N(22) C(21) C(2) C(11) . . . . -47.0(6) no N(22) C(21) C(2) C(17) . . . 4 77.9(6) no N(22) C(23) C(24) C(23) . . . 4 43.9(3) no N(22) C(23) C(24) C(241) . . . . -75.6(6) no N(22) C(23) C(24) C(241) . . . 4 165.8(4) no C(2) C(11) N(12) C(13) . . . . -176.9(4) no C(2) C(17) N(16) C(15) . 4 4 4 106.1(5) no C(2) C(21) N(22) C(23) . . . . 102.6(5) no C(11) N(12) C(13) C(14) . . . . -150.4(4) no C(14) C(15) N(16) C(17) . . . . 172.7(4) no C(21) N(22) C(23) C(24) . . . . 154.7(4) no #----------------------------------------------------------------------- #===END