# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2103 data_AJE3_-60_deg_C_-_crystal_#2 #----------------------------------------------------------------------- _audit_creation_date '2000-03-15' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 1994-07-19 Report prepared by ACW for AJE etc 2000-03-15 Cif produced 2000-03-15 ACW modifies cif 2000-03-16 cif passes checkcif with alerts arising from max 2theta ; #----------------------------------------------------------------------- _publ_requested_journal ' test ' _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_address 'Patricia M. Angus ' ; Department of Chemistry, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Anthony J. Elliott ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Alan M. Sargeson ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; 'Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; Template synthesis of amidine- and amide-functionalised cobalt(III) hexaaza cage complexes. ; _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 26.143(1) _cell_length_b 10.794(2) _cell_length_c 17.061(2) _cell_angle_alpha 90 _cell_angle_beta 108.522(6) _cell_angle_gamma 90 _cell_volume 4564.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 213.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 52.2 _cell_measurement_theta_max 54.9 #----------------------------------------------------------------------- _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' ' 1/2+x, 1/2+y, +z' ' -x, +y,1/2-z' ' 1/2-x, 1/2+y, 1/2-z' ' -x, -y, -z' ' 1/2-x, 1/2-y, -z' ' +x, -y,1/2+z' ' 1/2+x, 1/2-y, 1/2+z' #----------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 580.31 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H32 Cl2 Co N7 O8 ' _chemical_formula_moiety 'C16 H32 Co N7 2-, 2(Cl O4 -) ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2416.00 _exptl_absorpt_coefficient_mu 8.588 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.580 _exptl_absorpt_correction_T_min 0.396 _exptl_special_details ; The scan width was (1.10+0.30tan\q)\% with an \w scan speed of 16\% 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. Data can only be collected to 2theta 120 deg on a AFC6R diffractometer when the evacuated beam tunnel in used. Mass attenuation coefficients for absorption from International Tables for X-ray Crystallography, Vol IV (1974) Table 2.1C. ; #----------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 213.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_device_details ; Rigaku AFC6R diffractometer with extended arm and evacuated collimator and beam tunnel. Data cannot be collected beyond \y 60 deg in this configuration. ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.44 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -6 0 2 0 0 4 0 2 0 _diffrn_reflns_number 3734 _reflns_number_total 3385 _reflns_number_gt 2284 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.02839 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 60.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01055 _diffrn_orient_matrix_UB_12 -0.04954 _diffrn_orient_matrix_UB_13 0.05223 _diffrn_orient_matrix_UB_21 0.03886 _diffrn_orient_matrix_UB_22 0.01821 _diffrn_orient_matrix_UB_23 0.00820 _diffrn_orient_matrix_UB_31 -0.00243 _diffrn_orient_matrix_UB_32 0.07614 _diffrn_orient_matrix_UB_33 0.03203 #----------------------------------------------------------------------- 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 0 128 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 256 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.348 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co 0 8 -2.464 3.608 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 56 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 64 0.047 0.032 ;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) 0.36008(2) 0.24600(7) 0.32275(4) 0.0151(2) 1.000 . Uani d ? Cl(1) 0.0000 0.2946(2) 0.2500 0.0364(5) 1. ST Uani d ? Cl(2) 0.12091(5) 0.2995(1) 0.04847(8) 0.0367(4) 1.000 . Uani d ? Cl(3) 0.5000 0.3139(1) 0.2500 0.0346(5) 1. ST Uani d ? O(11) 0.0325(1) 0.3709(3) 0.3159(2) 0.046(1) 1.000 . Uani d ? O(12) 0.0347(1) 0.2206(4) 0.2206(3) 0.090(2) 1.000 . Uani d ? O(21) 0.1148(2) 0.4205(3) 0.0138(2) 0.069(1) 1.000 . Uani d ? O(22) 0.1449(2) 0.2223(3) 0.0032(2) 0.069(1) 1.000 . Uani d ? O(23) 0.0703(1) 0.2529(4) 0.0472(2) 0.077(1) 1.000 . Uani d ? O(24) 0.1553(1) 0.3067(4) 0.1320(2) 0.083(2) 1.000 . Uani d ? O(31) 0.2458(1) -0.0061(3) 0.2091(2) 0.0272(9) 1.000 . Uani d ? O(50) 0.1530(2) 0.2780(4) 0.3060(3) 0.072(2) 1.000 . Uani d ? N(1) 0.2564(1) 0.0120(3) 0.0190(2) 0.036(1) 1.000 . Uani d ? N(12) 0.3986(1) 0.1521(3) 0.2590(2) 0.018(1) 1.000 . Uani d ? N(15) 0.4071(1) 0.1599(3) 0.4212(2) 0.021(1) 1.000 . Uani d ? N(22) 0.3184(1) 0.3358(3) 0.2211(2) 0.019(1) 1.000 . Uani d ? N(25) 0.4121(1) 0.3845(3) 0.3434(2) 0.018(1) 1.000 . Uani d ? N(32) 0.3051(1) 0.1237(3) 0.2987(2) 0.017(1) 1.000 . Uani d ? N(35) 0.3200(1) 0.3137(3) 0.3933(2) 0.017(1) 1.000 . Uani d ? C(1) 0.2776(2) 0.0580(4) 0.0801(3) 0.025(1) 1.000 . Uani d ? C(2) 0.3054(2) 0.1216(4) 0.1589(2) 0.020(1) 1.000 . Uani d ? C(3) 0.4121(2) 0.3682(4) 0.4915(3) 0.022(1) 1.000 . Uani d ? C(4) 0.4368(2) 0.4310(5) 0.5751(3) 0.034(2) 1.000 . Uani d ? C(11) 0.3662(2) 0.1019(4) 0.1766(3) 0.023(1) 1.000 . Uani d ? C(13) 0.4300(2) 0.0532(4) 0.3139(3) 0.027(1) 1.000 . Uani d ? C(14) 0.4532(2) 0.1070(4) 0.3983(3) 0.028(1) 1.000 . Uani d ? C(16) 0.4250(2) 0.2299(5) 0.5015(3) 0.027(1) 1.000 . Uani d ? C(21) 0.2904(2) 0.2605(4) 0.1465(3) 0.023(1) 1.000 . Uani d ? C(23) 0.3556(2) 0.4307(4) 0.2050(3) 0.023(1) 1.000 . Uani d ? C(24) 0.3854(2) 0.4877(4) 0.2868(3) 0.025(1) 1.000 . Uani d ? C(26) 0.4377(2) 0.4241(4) 0.4310(3) 0.027(1) 1.000 . Uani d ? C(31) 0.2839(2) 0.0709(4) 0.2273(3) 0.021(1) 1.000 . Uani d ? C(33) 0.2755(2) 0.1092(4) 0.3582(3) 0.025(1) 1.000 . Uani d ? C(34) 0.2948(2) 0.2074(4) 0.4242(3) 0.024(1) 1.000 . Uani d ? C(36) 0.3515(2) 0.3939(4) 0.4632(3) 0.025(1) 1.000 . Uani d ? H(4A) 0.424(2) 0.393(4) 0.616(2) 0.040 1.000 . Uiso d ? H(4B) 0.429(2) 0.518(4) 0.570(2) 0.040 1.000 . Uiso d ? H(4C) 0.472(2) 0.417(4) 0.595(2) 0.040 1.000 . Uiso d ? H(11A) 0.372(1) 0.011(4) 0.174(2) 0.027 1.000 . Uiso d ? H(11B) 0.378(1) 0.146(3) 0.135(2) 0.027 1.000 . Uiso d ? H(12) 0.422(1) 0.203(3) 0.250(2) 0.022 1.000 . Uiso d ? H(13A) 0.457(1) 0.026(3) 0.293(2) 0.032 1.000 . Uiso d ? H(13B) 0.403(1) -0.015(3) 0.314(2) 0.032 1.000 . Uiso d ? H(14A) 0.472(2) 0.052(4) 0.436(2) 0.034 1.000 . Uiso d ? H(14B) 0.483(1) 0.181(3) 0.401(2) 0.034 1.000 . Uiso d ? H(15) 0.391(2) 0.098(3) 0.427(2) 0.025 1.000 . Uiso d ? H(16A) 0.411(1) 0.194(3) 0.544(2) 0.032 1.000 . Uiso d ? H(16B) 0.461(1) 0.221(4) 0.522(2) 0.032 1.000 . Uiso d ? H(21A) 0.250(1) 0.274(3) 0.134(2) 0.028 1.000 . Uiso d ? H(21B) 0.299(1) 0.291(3) 0.100(2) 0.028 1.000 . Uiso d ? H(22) 0.293(1) 0.373(3) 0.235(2) 0.022 1.000 . Uiso d ? H(23A) 0.381(1) 0.388(3) 0.177(2) 0.027 1.000 . Uiso d ? H(23B) 0.335(1) 0.487(3) 0.165(2) 0.027 1.000 . Uiso d ? H(24A) 0.360(1) 0.530(3) 0.309(2) 0.030 1.000 . Uiso d ? H(24B) 0.410(1) 0.546(4) 0.282(2) 0.030 1.000 . Uiso d ? H(25) 0.437(1) 0.355(3) 0.326(2) 0.021 1.000 . Uiso d ? H(26A) 0.475(1) 0.398(3) 0.449(2) 0.032 1.000 . Uiso d ? H(26B) 0.435(1) 0.512(4) 0.432(2) 0.032 1.000 . Uiso d ? H(33A) 0.238(1) 0.123(4) 0.331(2) 0.030 1.000 . Uiso d ? H(33B) 0.284(1) 0.025(3) 0.384(2) 0.030 1.000 . Uiso d ? H(34A) 0.325(1) 0.176(3) 0.475(2) 0.028 1.000 . Uiso d ? H(34B) 0.264(1) 0.237(4) 0.440(2) 0.028 1.000 . Uiso d ? H(35) 0.293(1) 0.366(3) 0.359(2) 0.021 1.000 . Uiso d ? H(36A) 0.339(1) 0.384(4) 0.509(2) 0.030 1.000 . Uiso d ? H(36B) 0.346(1) 0.488(3) 0.444(2) 0.030 1.000 . Uiso d ? H(50A) 0.117(2) 0.277(5) 0.294(3) 0.085 1.000 . Uiso d ? H(50B) 0.161(2) 0.291(5) 0.253(3) 0.085 1.000 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0140(3) 0.0136(3) 0.0187(3) 0.0002(3) 0.0066(3) 0.0011(3) Cl(1) 0.0300(9) 0.0256(9) 0.056(1) 0.0000 0.0165(9) 0.0000 Cl(2) 0.0418(7) 0.0299(7) 0.0443(8) 0.0027(6) 0.0219(6) 0.0004(6) Cl(3) 0.0245(9) 0.033(1) 0.055(1) 0.0000 0.0248(8) 0.0000 O(11) 0.050(2) 0.048(2) 0.031(2) -0.005(2) -0.002(2) 0.000(2) O(12) 0.061(3) 0.076(3) 0.139(4) 0.026(2) 0.038(3) -0.044(3) O(21) 0.123(4) 0.021(2) 0.085(3) 0.009(2) 0.064(3) 0.003(2) O(22) 0.110(3) 0.036(2) 0.083(3) 0.020(2) 0.062(3) -0.003(2) O(23) 0.042(2) 0.082(3) 0.107(3) -0.015(2) 0.026(2) 0.010(3) O(24) 0.065(3) 0.135(4) 0.047(2) 0.007(3) 0.012(2) 0.000(3) O(31) 0.027(2) 0.030(2) 0.026(2) -0.017(1) 0.010(1) -0.007(2) O(50) 0.053(3) 0.064(3) 0.094(3) 0.006(3) 0.018(3) -0.001(3) N(1) 0.037(3) 0.047(3) 0.028(3) -0.009(2) 0.015(2) -0.011(2) N(12) 0.014(2) 0.016(2) 0.025(2) 0.000(2) 0.009(2) -0.002(2) N(15) 0.021(2) 0.014(2) 0.027(2) -0.002(2) 0.006(2) 0.000(2) N(22) 0.018(2) 0.019(2) 0.020(2) 0.002(2) 0.008(2) 0.002(2) N(25) 0.017(2) 0.015(2) 0.024(2) 0.000(2) 0.008(2) 0.001(2) N(32) 0.020(2) 0.018(2) 0.017(2) -0.006(2) 0.010(2) 0.000(2) N(35) 0.016(2) 0.019(2) 0.019(2) 0.000(2) 0.007(2) 0.002(2) C(1) 0.026(3) 0.029(3) 0.028(3) -0.002(2) 0.018(2) -0.001(2) C(2) 0.021(2) 0.022(3) 0.018(2) -0.003(2) 0.007(2) -0.006(2) C(3) 0.023(3) 0.021(3) 0.021(3) -0.003(2) 0.006(2) -0.003(2) C(4) 0.030(3) 0.039(3) 0.030(3) -0.005(3) 0.006(2) -0.004(3) C(11) 0.025(3) 0.025(3) 0.020(3) -0.002(2) 0.011(2) -0.002(2) C(13) 0.027(3) 0.020(3) 0.033(3) 0.008(2) 0.010(2) -0.001(2) C(14) 0.023(3) 0.028(3) 0.030(3) 0.015(2) 0.003(2) 0.006(2) C(16) 0.024(3) 0.032(3) 0.019(3) 0.001(2) -0.002(2) -0.005(2) C(21) 0.023(3) 0.026(3) 0.019(2) 0.001(2) 0.005(2) 0.002(2) C(23) 0.021(3) 0.020(3) 0.029(3) 0.000(2) 0.012(2) 0.008(2) C(24) 0.027(3) 0.014(3) 0.038(3) -0.004(2) 0.015(2) 0.003(2) C(26) 0.023(3) 0.026(3) 0.033(3) -0.003(2) 0.009(2) -0.006(2) C(31) 0.018(2) 0.020(3) 0.025(3) 0.001(2) 0.008(2) 0.001(2) C(33) 0.027(3) 0.027(3) 0.026(3) -0.006(2) 0.014(2) -0.003(2) C(34) 0.026(3) 0.023(3) 0.028(3) -0.006(2) 0.016(2) -0.002(2) C(36) 0.026(3) 0.026(3) 0.024(3) 0.003(2) 0.009(2) -0.006(2) #----------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2284 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0260 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.640 _refine_ls_shift/su_max 0.0410 _refine_ls_shift/su_mean 0.001 _refine_diff_density_min -0.32 _refine_diff_density_max 0.30 #----------------------------------------------------------------------- _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) 1.980(3) . . yes Co(1) N(15) 1.971(4) . . yes Co(1) N(22) 1.983(3) . . yes Co(1) N(25) 1.976(3) . . yes Co(1) N(32) 1.898(3) . . yes Co(1) N(35) 1.971(3) . . yes Cl(1) O(11) 1.434(3) . . yes Cl(1) O(11) 1.434(3) . 2 yes Cl(1) O(12) 1.416(3) . . yes Cl(1) O(12) 1.416(3) . 2 yes Cl(2) O(21) 1.421(3) . . yes Cl(2) O(22) 1.412(3) . . yes Cl(2) O(23) 1.410(3) . . yes Cl(2) O(24) 1.426(4) . . yes O(31) C(31) 1.259(4) . . yes O(50) H(50A) 0.89(5) . . no O(50) H(50B) 1.00(5) . . no N(1) C(1) 1.129(5) . . yes N(12) C(11) 1.495(5) . . yes N(12) C(13) 1.482(5) . . yes N(12) H(12) 0.87(3) . . no N(15) C(14) 1.493(5) . . yes N(15) C(16) 1.503(5) . . yes N(15) H(15) 0.81(3) . . no N(22) C(21) 1.491(5) . . yes N(22) C(23) 1.497(5) . . yes N(22) H(22) 0.88(3) . . no N(25) C(24) 1.495(5) . . yes N(25) C(26) 1.494(5) . . yes N(25) H(25) 0.85(3) . . no N(32) C(31) 1.298(5) . . yes N(32) C(33) 1.467(5) . . yes N(35) C(34) 1.499(5) . . yes N(35) C(36) 1.492(5) . . yes N(35) H(35) 0.95(3) . . no C(1) C(2) 1.479(5) . . yes C(2) C(11) 1.534(5) . . yes C(2) C(21) 1.548(6) . . yes C(2) C(31) 1.548(5) . . yes C(3) C(4) 1.525(6) . . yes C(3) C(16) 1.527(6) . . yes C(3) C(26) 1.523(6) . . yes C(3) C(36) 1.527(5) . . yes C(4) H(4A) 0.95(4) . . no C(4) H(4B) 0.96(4) . . no C(4) H(4C) 0.88(4) . . no C(11) H(11A) 1.00(4) . . no C(11) H(11B) 0.98(3) . . no C(13) C(14) 1.492(6) . . yes C(13) H(13A) 0.93(4) . . no C(13) H(13B) 1.03(4) . . no C(14) H(14A) 0.90(4) . . no C(14) H(14B) 1.10(4) . . no C(16) H(16A) 0.99(4) . . no C(16) H(16B) 0.90(4) . . no C(21) H(21A) 1.01(4) . . no C(21) H(21B) 0.95(4) . . no C(23) C(24) 1.497(6) . . yes C(23) H(23A) 1.04(3) . . no C(23) H(23B) 0.96(4) . . no C(24) H(24A) 0.98(4) . . no C(24) H(24B) 0.94(4) . . no C(26) H(26A) 0.98(4) . . no C(26) H(26B) 0.95(4) . . no C(33) C(34) 1.512(6) . . yes C(33) H(33A) 0.96(4) . . no C(33) H(33B) 1.01(4) . . no C(34) H(34A) 1.03(4) . . no C(34) H(34B) 0.97(3) . . no C(36) H(36A) 0.94(4) . . no C(36) H(36B) 1.06(4) . . 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(15) 86.5(1) . . . yes N(12) Co(1) N(22) 90.2(1) . . . yes N(12) Co(1) N(25) 92.5(1) . . . yes N(12) Co(1) N(32) 90.5(1) . . . yes N(12) Co(1) N(35) 170.9(1) . . . yes N(15) Co(1) N(22) 175.1(1) . . . yes N(15) Co(1) N(25) 89.9(1) . . . yes N(15) Co(1) N(32) 94.6(1) . . . yes N(15) Co(1) N(35) 87.9(1) . . . yes N(22) Co(1) N(25) 86.7(1) . . . yes N(22) Co(1) N(32) 89.0(1) . . . yes N(22) Co(1) N(35) 95.9(1) . . . yes N(25) Co(1) N(32) 174.8(1) . . . yes N(25) Co(1) N(35) 94.6(1) . . . yes N(32) Co(1) N(35) 82.9(1) . . . yes O(11) Cl(1) O(11) 110.0(3) . . 2 yes O(11) Cl(1) O(12) 108.3(2) . . . yes O(11) Cl(1) O(12) 109.5(2) . . 2 yes O(11) Cl(1) O(12) 109.5(2) 2 . . yes O(11) Cl(1) O(12) 108.3(2) 2 . 2 yes O(12) Cl(1) O(12) 111.2(4) . . 2 yes O(21) Cl(2) O(22) 109.0(2) . . . yes O(21) Cl(2) O(23) 109.9(2) . . . yes O(21) Cl(2) O(24) 108.5(3) . . . yes O(22) Cl(2) O(23) 111.1(2) . . . yes O(22) Cl(2) O(24) 109.3(2) . . . yes O(23) Cl(2) O(24) 109.0(2) . . . yes H(50A) O(50) H(50B) 107(5) . . . no Co(1) N(12) C(11) 117.8(3) . . . yes Co(1) N(12) C(13) 107.3(3) . . . yes Co(1) N(12) H(12) 107(3) . . . no C(11) N(12) C(13) 111.6(3) . . . yes C(11) N(12) H(12) 106(3) . . . no C(13) N(12) H(12) 107(3) . . . no Co(1) N(15) C(14) 107.1(3) . . . yes Co(1) N(15) C(16) 117.9(3) . . . yes Co(1) N(15) H(15) 106(3) . . . no C(14) N(15) C(16) 112.8(3) . . . yes C(14) N(15) H(15) 102(3) . . . no C(16) N(15) H(15) 109(3) . . . no Co(1) N(22) C(21) 117.7(3) . . . yes Co(1) N(22) C(23) 106.7(3) . . . yes Co(1) N(22) H(22) 104(3) . . . no C(21) N(22) C(23) 112.9(3) . . . yes C(21) N(22) H(22) 106(3) . . . no C(23) N(22) H(22) 109(3) . . . no Co(1) N(25) C(24) 107.2(3) . . . yes Co(1) N(25) C(26) 117.3(3) . . . yes Co(1) N(25) H(25) 102(3) . . . no C(24) N(25) C(26) 113.7(3) . . . yes C(24) N(25) H(25) 108(3) . . . no C(26) N(25) H(25) 108(3) . . . no Co(1) N(32) C(31) 125.1(3) . . . yes Co(1) N(32) C(33) 117.1(3) . . . yes C(31) N(32) C(33) 116.2(3) . . . yes Co(1) N(35) C(34) 107.9(2) . . . yes Co(1) N(35) C(36) 115.9(3) . . . yes Co(1) N(35) H(35) 106(2) . . . no C(34) N(35) C(36) 110.9(3) . . . yes C(34) N(35) H(35) 110(2) . . . no C(36) N(35) H(35) 106(2) . . . no N(1) C(1) C(2) 178.4(5) . . . yes C(1) C(2) C(11) 107.1(3) . . . yes C(1) C(2) C(21) 107.2(4) . . . yes C(1) C(2) C(31) 109.3(3) . . . yes C(11) C(2) C(21) 111.3(3) . . . yes C(11) C(2) C(31) 113.8(3) . . . yes C(21) C(2) C(31) 107.9(3) . . . yes C(4) C(3) C(16) 108.5(4) . . . yes C(4) C(3) C(26) 108.1(4) . . . yes C(4) C(3) C(36) 107.6(4) . . . yes C(16) C(3) C(26) 109.5(4) . . . yes C(16) C(3) C(36) 112.5(4) . . . yes C(26) C(3) C(36) 110.4(4) . . . yes C(3) C(4) H(4A) 110(3) . . . no C(3) C(4) H(4B) 110(3) . . . no C(3) C(4) H(4C) 112(3) . . . no H(4A) C(4) H(4B) 112(4) . . . no H(4A) C(4) H(4C) 102(4) . . . no H(4B) C(4) H(4C) 111(4) . . . no N(12) C(11) C(2) 112.2(3) . . . yes N(12) C(11) H(11A) 110(2) . . . no N(12) C(11) H(11B) 107(2) . . . no C(2) C(11) H(11A) 107(2) . . . no C(2) C(11) H(11B) 109(2) . . . no H(11A) C(11) H(11B) 112(3) . . . no N(12) C(13) C(14) 107.6(4) . . . yes N(12) C(13) H(13A) 109(2) . . . no N(12) C(13) H(13B) 106(2) . . . no C(14) C(13) H(13A) 112(3) . . . no C(14) C(13) H(13B) 111(2) . . . no H(13A) C(13) H(13B) 112(3) . . . no N(15) C(14) C(13) 106.7(4) . . . yes N(15) C(14) H(14A) 111(3) . . . no N(15) C(14) H(14B) 109(2) . . . no C(13) C(14) H(14A) 113(3) . . . no C(13) C(14) H(14B) 113(2) . . . no H(14A) C(14) H(14B) 104(3) . . . no N(15) C(16) C(3) 113.3(4) . . . yes N(15) C(16) H(16A) 113(2) . . . no N(15) C(16) H(16B) 106(3) . . . no C(3) C(16) H(16A) 110(2) . . . no C(3) C(16) H(16B) 108(3) . . . no H(16A) C(16) H(16B) 105(3) . . . no N(22) C(21) C(2) 112.1(3) . . . yes N(22) C(21) H(21A) 107(2) . . . no N(22) C(21) H(21B) 110(2) . . . no C(2) C(21) H(21A) 112(2) . . . no C(2) C(21) H(21B) 110(2) . . . no H(21A) C(21) H(21B) 106(3) . . . no N(22) C(23) C(24) 106.6(3) . . . yes N(22) C(23) H(23A) 109(2) . . . no N(22) C(23) H(23B) 108(2) . . . no C(24) C(23) H(23A) 113(2) . . . no C(24) C(23) H(23B) 115(2) . . . no H(23A) C(23) H(23B) 105(3) . . . no N(25) C(24) C(23) 107.0(3) . . . yes N(25) C(24) H(24A) 109(2) . . . no N(25) C(24) H(24B) 112(2) . . . no C(23) C(24) H(24A) 110(2) . . . no C(23) C(24) H(24B) 111(2) . . . no H(24A) C(24) H(24B) 108(3) . . . no N(25) C(26) C(3) 114.3(4) . . . yes N(25) C(26) H(26A) 108(2) . . . no N(25) C(26) H(26B) 107(2) . . . no C(3) C(26) H(26A) 107(2) . . . no C(3) C(26) H(26B) 110(2) . . . no H(26A) C(26) H(26B) 110(3) . . . no O(31) C(31) N(32) 126.1(4) . . . yes O(31) C(31) C(2) 119.7(4) . . . yes N(32) C(31) C(2) 113.9(3) . . . yes N(32) C(33) C(34) 108.3(3) . . . yes N(32) C(33) H(33A) 110(2) . . . no N(32) C(33) H(33B) 108(2) . . . no C(34) C(33) H(33A) 107(2) . . . no C(34) C(33) H(33B) 110(2) . . . no H(33A) C(33) H(33B) 114(3) . . . no N(35) C(34) C(33) 110.9(3) . . . yes N(35) C(34) H(34A) 104(2) . . . no N(35) C(34) H(34B) 109(2) . . . no C(33) C(34) H(34A) 112(2) . . . no C(33) C(34) H(34B) 109(2) . . . no H(34A) C(34) H(34B) 111(3) . . . no N(35) C(36) C(3) 113.7(4) . . . yes N(35) C(36) H(36A) 110(2) . . . no N(35) C(36) H(36B) 109(2) . . . no C(3) C(36) H(36A) 108(2) . . . no C(3) C(36) H(36B) 107(2) . . . no H(36A) C(36) H(36B) 109(3) . . . 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(3) N(12) 3.219(3) . . no Cl(3) N(12) 3.219(3) . 2_655 no Cl(3) N(25) 3.275(3) . . no Cl(3) N(25) 3.275(3) . 2_655 no O(11) C(16) 3.151(5) . 7_556 no O(11) C(13) 3.317(5) . 5_455 no O(11) C(13) 3.334(5) . 6 no O(11) O(50) 3.361(5) . . no O(12) O(50) 3.034(5) . . no O(12) C(24) 3.296(5) . 6_545 no O(12) C(4) 3.370(7) . 8_454 no O(12) O(23) 3.389(5) . . no O(21) N(15) 2.939(4) . 6 no O(21) C(14) 3.340(6) . 6 no O(21) C(11) 3.447(5) . 7 no O(21) C(16) 3.483(6) . 6 no O(22) C(21) 3.488(5) . 7 no O(22) C(11) 3.539(6) . 7 no O(22) C(36) 3.588(6) . 6_545 no O(23) C(26) 3.582(6) . 6_545 no O(24) O(50) 3.004(6) . . no O(24) C(21) 3.496(6) . . no O(31) N(35) 2.808(4) . 6_545 no O(31) N(22) 2.902(4) . 6_545 no O(31) C(36) 3.396(5) . 6_545 no O(31) C(24) 3.454(5) . 6_545 no O(31) C(23) 3.481(5) . 6_545 no O(31) O(50) 3.594(5) . 6_545 no O(50) C(24) 3.510(6) . 6_545 no O(50) C(33) 3.542(6) . . no O(50) C(11) 3.558(6) . 6 no N(1) C(36) 3.197(6) . 6_545 no N(1) C(34) 3.204(6) . 4_554 no N(1) C(33) 3.218(6) . 4_554 no N(1) N(35) 3.563(5) . 6_545 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) . . . . -6.0(5) no Co(1) N(12) C(13) C(14) . . . . -39.9(4) no Co(1) N(15) C(14) C(13) . . . . -42.4(4) no Co(1) N(15) C(16) C(3) . . . . -10.6(5) no Co(1) N(22) C(21) C(2) . . . . -7.8(5) no Co(1) N(22) C(23) C(24) . . . . -42.7(4) no Co(1) N(25) C(24) C(23) . . . . -41.1(4) no Co(1) N(25) C(26) C(3) . . . . -11.1(5) no Co(1) N(32) C(31) O(31) . . . . -176.6(3) no Co(1) N(32) C(31) C(2) . . . . -3.2(5) no Co(1) N(32) C(33) C(34) . . . . 4.2(5) no Co(1) N(35) C(34) C(33) . . . . -37.3(4) no Co(1) N(35) C(36) C(3) . . . . -24.6(5) no O(31) C(31) N(32) C(33) . . . . -11.7(6) no O(31) C(31) C(2) C(1) . . . . -4.4(5) no O(31) C(31) C(2) C(11) . . . . -124.1(4) no O(31) C(31) C(2) C(21) . . . . 111.8(4) no N(1) C(1) C(2) C(11) . . . . -90.8(2) no N(1) C(1) C(2) C(21) . . . . 28.8(2) no N(1) C(1) C(2) C(31) . . . . 145.5(2) no N(12) Co(1) N(15) C(14) . . . . 16.5(3) no N(12) Co(1) N(15) C(16) . . . . 144.9(3) no N(12) Co(1) N(22) C(21) . . . . 51.5(3) no N(12) Co(1) N(22) C(23) . . . . -76.4(3) no N(12) Co(1) N(25) C(24) . . . . 103.9(3) no N(12) Co(1) N(25) C(26) . . . . -126.8(3) no N(12) Co(1) N(32) C(31) . . . . -42.3(3) no N(12) Co(1) N(32) C(33) . . . . 153.0(3) no N(12) Co(1) N(35) C(34) . . . . -12(1) no N(12) Co(1) N(35) C(36) . . . . 113.0(9) no N(12) C(11) C(2) C(1) . . . . -174.6(3) no N(12) C(11) C(2) C(21) . . . . 68.5(5) no N(12) C(11) C(2) C(31) . . . . -53.7(5) no N(12) C(13) C(14) N(15) . . . . 54.7(5) no N(15) Co(1) N(12) C(11) . . . . 139.8(3) no N(15) Co(1) N(12) C(13) . . . . 12.9(3) no N(15) Co(1) N(22) C(21) . . . . 99(2) no N(15) Co(1) N(22) C(23) . . . . -29(2) no N(15) Co(1) N(25) C(24) . . . . -169.6(3) no N(15) Co(1) N(25) C(26) . . . . -40.4(3) no N(15) Co(1) N(32) C(31) . . . . -128.7(3) no N(15) Co(1) N(32) C(33) . . . . 66.5(3) no N(15) Co(1) N(35) C(34) . . . . -63.5(3) no N(15) Co(1) N(35) C(36) . . . . 61.6(3) no N(15) C(16) C(3) C(4) . . . . -174.6(4) no N(15) C(16) C(3) C(26) . . . . -56.8(5) no N(15) C(16) C(3) C(36) . . . . 66.4(5) no N(22) Co(1) N(12) C(11) . . . . -43.8(3) no N(22) Co(1) N(12) C(13) . . . . -170.8(3) no N(22) Co(1) N(15) C(14) . . . . -31(2) no N(22) Co(1) N(15) C(16) . . . . 97(2) no N(22) Co(1) N(25) C(24) . . . . 13.8(3) no N(22) Co(1) N(25) C(26) . . . . 143.1(3) no N(22) Co(1) N(32) C(31) . . . . 47.9(3) no N(22) Co(1) N(32) C(33) . . . . -116.8(3) no N(22) Co(1) N(35) C(34) . . . . 119.7(3) no N(22) Co(1) N(35) C(36) . . . . -115.2(3) no N(22) C(21) C(2) C(1) . . . . -177.2(3) no N(22) C(21) C(2) C(11) . . . . -60.3(5) no N(22) C(21) C(2) C(31) . . . . 65.3(4) no N(22) C(23) C(24) N(25) . . . . 55.8(4) no N(25) Co(1) N(12) C(11) . . . . -130.5(3) no N(25) Co(1) N(12) C(13) . . . . 102.6(3) no N(25) Co(1) N(15) C(14) . . . . -76.0(3) no N(25) Co(1) N(15) C(16) . . . . 52.4(3) no N(25) Co(1) N(22) C(21) . . . . 144.0(3) no N(25) Co(1) N(22) C(23) . . . . 16.1(3) no N(25) Co(1) N(32) C(31) . . . . 82(2) no N(25) Co(1) N(32) C(33) . . . . -82(2) no N(25) Co(1) N(35) C(34) . . . . -153.1(3) no N(25) Co(1) N(35) C(36) . . . . -28.1(3) no N(25) C(26) C(3) C(4) . . . . -171.9(4) no N(25) C(26) C(3) C(16) . . . . 70.1(5) no N(25) C(26) C(3) C(36) . . . . -54.4(5) no N(32) Co(1) N(12) C(11) . . . . 45.2(3) no N(32) Co(1) N(12) C(13) . . . . -81.7(3) no N(32) Co(1) N(15) C(14) . . . . 106.7(3) no N(32) Co(1) N(15) C(16) . . . . -124.9(3) no N(32) Co(1) N(22) C(21) . . . . -38.9(3) no N(32) Co(1) N(22) C(23) . . . . -166.9(3) no N(32) Co(1) N(25) C(24) . . . . -21(2) no N(32) Co(1) N(25) C(26) . . . . 109(2) no N(32) Co(1) N(35) C(34) . . . . 31.5(3) no N(32) Co(1) N(35) C(36) . . . . 156.5(3) no N(32) C(31) C(2) C(1) . . . . -178.3(4) no N(32) C(31) C(2) C(11) . . . . 62.1(5) no N(32) C(31) C(2) C(21) . . . . -62.0(4) no N(32) C(33) C(34) N(35) . . . . 21.8(5) no N(35) Co(1) N(12) C(11) . . . . 88.3(9) no N(35) Co(1) N(12) C(13) . . . . -39(1) no N(35) Co(1) N(15) C(14) . . . . -170.6(3) no N(35) Co(1) N(15) C(16) . . . . -42.2(3) no N(35) Co(1) N(22) C(21) . . . . -121.7(3) no N(35) Co(1) N(22) C(23) . . . . 110.4(3) no N(35) Co(1) N(25) C(24) . . . . -81.8(3) no N(35) Co(1) N(25) C(26) . . . . 47.5(3) no N(35) Co(1) N(32) C(31) . . . . 144.0(4) no N(35) Co(1) N(32) C(33) . . . . -20.7(3) no N(35) C(36) C(3) C(4) . . . . -165.7(4) no N(35) C(36) C(3) C(16) . . . . -46.3(5) no N(35) C(36) C(3) C(26) . . . . 76.5(5) no C(2) C(11) N(12) C(13) . . . . 118.8(4) no C(2) C(21) N(22) C(23) . . . . 117.2(4) no C(2) C(31) N(32) C(33) . . . . 161.6(3) no C(3) C(16) N(15) C(14) . . . . 115.0(4) no C(3) C(26) N(25) C(24) . . . . 115.0(4) no C(3) C(36) N(35) C(34) . . . . 98.9(4) no C(11) N(12) C(13) C(14) . . . . -170.3(3) no C(13) C(14) N(15) C(16) . . . . -173.8(4) no C(21) N(22) C(23) C(24) . . . . -173.5(3) no C(23) C(24) N(25) C(26) . . . . -172.5(3) no C(31) N(32) C(33) C(34) . . . . -161.9(4) no C(33) C(34) N(35) C(36) . . . . -165.2(4) no #----------------------------------------------------------------------- #===END