# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2249 data_global #============================================================================== # SUBMISSION DETAILS _publ_requested_journal ' J. Chem. Soc., Dalton Trans ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr ERT Tiekink ' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 8 8303 5943 ' _publ_contact_author_fax ' 61 8 8303 4358 ' _publ_contact_author_email ' etiekink@chemistry.adelaide.edu.au ' #============================================================================== data_[CuL]ClO4 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jun 17 18:29:20 1997' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.981(2) _cell_length_b 15.610(4) _cell_length_c 8.943(2) _cell_angle_alpha 100.06(2) _cell_angle_beta 93.74(2) _cell_angle_gamma 100.16(2) _cell_volume 1343.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 39.9 _cell_measurement_theta_max 44.2 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.160 _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_meas ? _chemical_formula_weight 604.05 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H33 Cl Co N6 O4 S2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 0.934 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.497 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC6R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_decay_% -4.24 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 0 2 -1 1 1 -3 0 _diffrn_reflns_number 6565 _reflns_number_total 6212 _reflns_number_observed 3359 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 4.01 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.01926 _diffrn_orient_matrix_UB_12 -0.03318 _diffrn_orient_matrix_UB_13 0.08252 _diffrn_orient_matrix_UB_21 -0.02126 _diffrn_orient_matrix_UB_22 -0.05690 _diffrn_orient_matrix_UB_23 -0.07602 _diffrn_orient_matrix_UB_31 0.09818 _diffrn_orient_matrix_UB_32 0.00738 _diffrn_orient_matrix_UB_33 -0.02086 #------------------------------------------------------------------------------ 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 44 0.003 0.002 'International Tables' H 0 66 0.000 0.000 'International Tables' Cl 0 2 0.148 0.159 'International Tables' Co 0 2 0.349 0.972 'International Tables' N 0 12 0.006 0.003 'International Tables' O 0 8 0.011 0.006 'International Tables' S 0 4 0.125 0.123 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Co 0.24253(6) 0.18295(4) 0.36507(7) 0.0343(2) Uij ? ? Cl -0.2774(1) 0.38905(9) 0.3200(2) 0.0650(5) Uij ? ? S(1) 0.2952(1) 0.05020(8) 0.2500(2) 0.0490(4) Uij ? ? S(2) 0.1433(2) -0.11890(9) 0.0548(2) 0.0632(5) Uij ? ? O(1) -0.1780(5) 0.4421(3) 0.4335(6) 0.115(2) Uij ? ? O(2) -0.2636(5) 0.4251(4) 0.1861(6) 0.128(2) Uij ? ? O(3) -0.4100(4) 0.3914(3) 0.3612(6) 0.101(2) Uij ? ? O(4) -0.2535(5) 0.3011(3) 0.2993(6) 0.113(2) Uij ? ? N(1) 0.0560(3) 0.1297(2) 0.4151(4) 0.036(1) Uij ? ? N(2) 0.1729(3) 0.3050(2) 0.4895(4) 0.0333(10) Uij ? ? N(3) 0.3984(3) 0.3208(2) 0.6061(4) 0.037(1) Uij ? ? N(4) 0.4006(3) 0.2370(2) 0.5294(4) 0.037(1) Uij ? ? N(5) 0.1672(3) 0.3296(2) 0.2375(4) 0.036(1) Uij ? ? N(6) 0.2461(4) 0.2662(2) 0.2109(4) 0.037(1) Uij ? ? C(1) 0.1426(5) -0.0199(3) 0.1884(5) 0.040(1) Uij ? ? C(2) 0.3170(6) -0.1144(4) 0.0163(7) 0.078(2) Uij ? ? C(3) 0.0151(5) -0.0117(3) 0.2309(5) 0.038(1) Uij ? ? C(4) -0.0223(4) 0.0569(3) 0.3406(5) 0.037(1) Uij ? ? C(5) -0.1723(5) 0.0331(3) 0.3601(5) 0.047(1) Uij ? ? C(6) -0.2257(5) -0.0571(3) 0.2598(7) 0.063(2) Uij ? ? C(7) -0.1131(5) -0.0787(3) 0.1616(5) 0.049(1) Uij ? ? C(8) -0.0100(4) 0.1871(3) 0.5252(5) 0.038(1) Uij ? ? C(9) 0.0892(4) 0.2707(3) 0.6047(5) 0.037(1) Uij ? ? C(10) 0.0125(5) 0.3361(3) 0.6914(5) 0.048(1) Uij ? ? C(11) 0.2978(4) 0.3687(3) 0.5530(5) 0.040(1) Uij ? ? C(12) 0.5391(6) 0.4450(3) 0.7974(6) 0.066(2) Uij ? ? C(13) 0.5093(5) 0.3527(3) 0.7062(5) 0.044(1) Uij ? ? C(14) 0.5846(5) 0.2867(3) 0.6995(6) 0.050(2) Uij ? ? C(15) 0.5147(4) 0.2164(3) 0.5906(6) 0.044(1) Uij ? ? C(16) 0.5533(5) 0.1291(4) 0.5363(7) 0.068(2) Uij ? ? C(17) 0.0949(4) 0.3376(3) 0.3728(5) 0.040(1) Uij ? ? C(18) 0.0979(6) 0.4543(4) 0.1321(6) 0.066(2) Uij ? ? C(19) 0.1741(5) 0.3790(3) 0.1277(5) 0.045(1) Uij ? ? C(20) 0.2610(5) 0.3472(3) 0.0293(5) 0.049(2) Uij ? ? C(21) 0.3047(4) 0.2785(3) 0.0851(5) 0.039(1) Uij ? ? C(22) 0.4106(5) 0.2274(3) 0.0300(6) 0.054(2) Uij ? ? H(2a) 0.3242 -0.1669 -0.0565 0.0939 Uij ? ? H(2b) 0.3482 -0.0620 -0.0258 0.0939 Uij ? ? H(2c) 0.3732 -0.1119 0.1102 0.0939 Uij ? ? H(5a) -0.1847 0.0304 0.4660 0.0559 Uij ? ? H(5b) -0.2204 0.0768 0.3285 0.0559 Uij ? ? H(6a) -0.2474 -0.1015 0.3225 0.0761 Uij ? ? H(6b) -0.3070 -0.0554 0.1956 0.0761 Uij ? ? H(7a) -0.1363 -0.0731 0.0572 0.0589 Uij ? ? H(7b) -0.0992 -0.1384 0.1636 0.0589 Uij ? ? H(8a) -0.0856 0.2040 0.4709 0.0458 Uij ? ? H(8b) -0.0443 0.1541 0.6015 0.0458 Uij ? ? H(9) 0.1502 0.2539 0.6786 0.0446 Uij ? ? H(10a) 0.0770 0.3888 0.7421 0.0573 Uij ? ? H(10b) -0.0522 0.3523 0.6207 0.0573 Uij ? ? H(10c) -0.0363 0.3091 0.7670 0.0573 Uij ? ? H(11a) 0.3334 0.3998 0.4749 0.0476 Uij ? ? H(11b) 0.2780 0.4110 0.6378 0.0476 Uij ? ? H(12a) 0.6247 0.4543 0.8614 0.0793 Uij ? ? H(12b) 0.5463 0.4870 0.7289 0.0793 Uij ? ? H(12c) 0.4658 0.4536 0.8611 0.0793 Uij ? ? H(14) 0.6702 0.2890 0.7596 0.0598 Uij ? ? H(16a) 0.4817 0.0819 0.5525 0.0812 Uij ? ? H(16b) 0.5652 0.1224 0.4283 0.0812 Uij ? ? H(16c) 0.6383 0.1261 0.5926 0.0812 Uij ? ? H(17a) 0.0033 0.3022 0.3504 0.0481 Uij ? ? H(17b) 0.0895 0.3991 0.4088 0.0481 Uij ? ? H(18a) 0.1275 0.4971 0.2259 0.0797 Uij ? ? H(18b) 0.1165 0.4826 0.0454 0.0797 Uij ? ? H(18c) 0.0005 0.4315 0.1277 0.0797 Uij ? ? H(20) 0.2870 0.3688 -0.0621 0.0589 Uij ? ? H(22a) 0.3714 0.1646 0.0081 0.0646 Uij ? ? H(22b) 0.4423 0.2455 -0.0619 0.0646 Uij ? ? H(22c) 0.4870 0.2389 0.1082 0.0646 Uij ? ? 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 0.0351(3) 0.0305(3) 0.0376(4) 0.0062(3) 0.0054(3) 0.0066(3) Cl 0.0513(8) 0.0560(8) 0.083(1) 0.0086(7) -0.0056(8) 0.0062(8) S(1) 0.0464(7) 0.0373(6) 0.0621(9) 0.0112(6) 0.0100(6) 0.0009(6) S(2) 0.077(1) 0.0438(7) 0.0632(10) 0.0125(7) 0.0123(8) -0.0065(7) O(1) 0.106(4) 0.063(3) 0.151(5) 0.014(3) -0.068(3) -0.013(3) O(2) 0.113(4) 0.185(6) 0.102(4) 0.025(4) 0.039(3) 0.061(4) O(3) 0.061(3) 0.126(4) 0.135(4) 0.031(3) 0.033(3) 0.059(3) O(4) 0.099(3) 0.057(3) 0.163(5) 0.022(2) -0.027(3) -0.023(3) N(1) 0.039(2) 0.032(2) 0.036(2) 0.004(2) 0.004(2) 0.007(2) N(2) 0.034(2) 0.032(2) 0.034(2) 0.006(2) 0.003(2) 0.008(2) N(3) 0.034(2) 0.036(2) 0.039(2) 0.004(2) 0.002(2) 0.005(2) N(4) 0.035(2) 0.035(2) 0.043(2) 0.007(2) 0.006(2) 0.010(2) N(5) 0.040(2) 0.039(2) 0.032(2) 0.010(2) 0.008(2) 0.012(2) N(6) 0.040(2) 0.033(2) 0.039(2) 0.006(2) 0.007(2) 0.007(2) C(1) 0.059(3) 0.027(2) 0.035(3) 0.008(2) 0.005(2) 0.009(2) C(2) 0.091(4) 0.075(4) 0.068(4) 0.040(4) 0.010(3) -0.013(3) C(3) 0.046(3) 0.032(2) 0.036(3) 0.002(2) 0.001(2) 0.008(2) C(4) 0.039(3) 0.038(2) 0.034(3) 0.004(2) 0.003(2) 0.013(2) C(5) 0.039(3) 0.051(3) 0.047(3) 0.000(2) 0.006(2) 0.009(2) C(6) 0.045(3) 0.057(3) 0.077(4) -0.009(3) 0.002(3) 0.002(3) C(7) 0.056(3) 0.040(3) 0.043(3) -0.006(2) -0.008(2) 0.007(2) C(8) 0.034(2) 0.039(2) 0.041(3) 0.005(2) 0.006(2) 0.008(2) C(9) 0.041(3) 0.040(2) 0.033(3) 0.009(2) 0.006(2) 0.010(2) C(10) 0.054(3) 0.046(3) 0.043(3) 0.014(2) 0.012(2) 0.003(2) C(11) 0.041(3) 0.029(2) 0.047(3) 0.004(2) 0.000(2) 0.006(2) C(12) 0.062(4) 0.056(3) 0.069(4) -0.002(3) -0.014(3) 0.000(3) C(13) 0.037(3) 0.047(3) 0.042(3) -0.006(2) 0.005(2) 0.009(2) C(14) 0.037(3) 0.060(3) 0.050(3) 0.004(2) -0.003(2) 0.011(3) C(15) 0.037(3) 0.050(3) 0.051(3) 0.012(2) 0.008(2) 0.019(2) C(16) 0.056(3) 0.073(4) 0.078(4) 0.033(3) -0.003(3) 0.006(3) C(17) 0.041(3) 0.040(3) 0.041(3) 0.011(2) 0.005(2) 0.009(2) C(18) 0.071(4) 0.077(4) 0.071(4) 0.034(3) 0.014(3) 0.042(3) C(19) 0.049(3) 0.046(3) 0.042(3) 0.006(2) 0.001(2) 0.013(2) C(20) 0.055(3) 0.053(3) 0.040(3) 0.003(3) 0.007(2) 0.017(2) C(21) 0.039(3) 0.041(3) 0.033(3) -0.003(2) 0.007(2) 0.002(2) C(22) 0.052(3) 0.056(3) 0.053(3) 0.007(2) 0.016(3) 0.006(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3359 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0479 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0500 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.690 _refine_ls_shift/esd_max 0.0021 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.49 _refine_diff_density_max 0.33 #------------------------------------------------------------------------------ _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 S(1) 2.311(1) ? ? yes Co N(1) 2.012(4) ? ? yes Co N(2) 2.276(3) ? ? yes Co N(4) 2.038(4) ? ? yes Co N(6) 2.051(3) ? ? yes Cl O(1) 1.409(4) ? ? yes Cl O(2) 1.414(5) ? ? yes Cl O(3) 1.402(4) ? ? yes Cl O(4) 1.416(4) ? ? yes S(1) C(1) 1.707(5) ? ? yes S(2) C(1) 1.782(4) ? ? yes S(2) C(2) 1.782(6) ? ? yes N(1) C(4) 1.304(5) ? ? yes N(1) C(8) 1.480(5) ? ? yes N(2) C(9) 1.481(5) ? ? yes N(2) C(11) 1.463(5) ? ? yes N(2) C(17) 1.474(5) ? ? yes N(3) N(4) 1.370(4) ? ? yes N(3) C(11) 1.456(5) ? ? yes N(3) C(13) 1.339(5) ? ? yes N(4) C(15) 1.346(5) ? ? yes N(5) N(6) 1.368(4) ? ? yes N(5) C(17) 1.447(5) ? ? yes N(5) C(19) 1.349(5) ? ? yes N(6) C(21) 1.330(5) ? ? yes C(1) C(3) 1.372(6) ? ? yes C(3) C(4) 1.439(6) ? ? yes C(3) C(7) 1.521(6) ? ? yes C(4) C(5) 1.508(6) ? ? yes C(5) C(6) 1.518(7) ? ? yes C(6) C(7) 1.519(7) ? ? yes C(8) C(9) 1.522(6) ? ? yes C(9) C(10) 1.519(6) ? ? yes C(12) C(13) 1.496(7) ? ? yes C(13) C(14) 1.374(6) ? ? yes C(14) C(15) 1.381(6) ? ? yes C(15) C(16) 1.490(6) ? ? yes C(18) C(19) 1.505(6) ? ? yes C(19) C(20) 1.368(6) ? ? yes C(20) C(21) 1.384(6) ? ? yes C(21) C(22) 1.491(6) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Co N(1) 95.52(10) ? ? ? yes S(1) Co N(2) 173.91(9) ? ? ? yes S(1) Co N(4) 104.70(10) ? ? ? yes S(1) Co N(6) 109.5(1) ? ? ? yes N(1) Co N(2) 78.7(1) ? ? ? yes N(1) Co N(4) 122.3(1) ? ? ? yes N(1) Co N(6) 115.9(1) ? ? ? yes N(2) Co N(4) 77.3(1) ? ? ? yes N(2) Co N(6) 75.0(1) ? ? ? yes N(4) Co N(6) 107.1(1) ? ? ? yes O(1) Cl O(2) 107.2(3) ? ? ? yes O(1) Cl O(3) 111.3(3) ? ? ? yes O(1) Cl O(4) 108.0(3) ? ? ? yes O(2) Cl O(3) 107.8(3) ? ? ? yes O(2) Cl O(4) 112.2(3) ? ? ? yes O(3) Cl O(4) 110.3(3) ? ? ? yes Co S(1) C(1) 106.2(2) ? ? ? yes C(1) S(2) C(2) 105.4(2) ? ? ? yes Co N(1) C(4) 126.2(3) ? ? ? yes Co N(1) C(8) 116.6(3) ? ? ? yes C(4) N(1) C(8) 116.0(4) ? ? ? yes Co N(2) C(9) 103.6(2) ? ? ? yes Co N(2) C(11) 105.9(2) ? ? ? yes Co N(2) C(17) 106.1(2) ? ? ? yes C(9) N(2) C(11) 114.7(3) ? ? ? yes C(9) N(2) C(17) 114.1(3) ? ? ? yes C(11) N(2) C(17) 111.4(3) ? ? ? yes N(4) N(3) C(11) 119.1(3) ? ? ? yes N(4) N(3) C(13) 111.6(3) ? ? ? yes C(11) N(3) C(13) 128.1(4) ? ? ? yes Co N(4) N(3) 115.7(2) ? ? ? yes Co N(4) C(15) 139.5(3) ? ? ? yes N(3) N(4) C(15) 104.8(3) ? ? ? yes N(6) N(5) C(17) 119.7(3) ? ? ? yes N(6) N(5) C(19) 110.9(3) ? ? ? yes C(17) N(5) C(19) 129.4(4) ? ? ? yes Co N(6) N(5) 115.7(3) ? ? ? yes Co N(6) C(21) 138.5(3) ? ? ? yes N(5) N(6) C(21) 105.8(3) ? ? ? yes S(1) C(1) S(2) 118.0(3) ? ? ? yes S(1) C(1) C(3) 128.4(3) ? ? ? yes S(2) C(1) C(3) 113.6(3) ? ? ? yes C(1) C(3) C(4) 128.6(4) ? ? ? yes C(1) C(3) C(7) 122.3(4) ? ? ? yes C(4) C(3) C(7) 109.1(4) ? ? ? yes N(1) C(4) C(3) 127.9(4) ? ? ? yes N(1) C(4) C(5) 122.7(4) ? ? ? yes C(3) C(4) C(5) 109.4(4) ? ? ? yes C(4) C(5) C(6) 106.8(4) ? ? ? yes C(5) C(6) C(7) 107.1(4) ? ? ? yes C(3) C(7) C(6) 106.0(4) ? ? ? yes N(1) C(8) C(9) 112.0(3) ? ? ? yes N(2) C(9) C(8) 108.2(3) ? ? ? yes N(2) C(9) C(10) 115.1(3) ? ? ? yes C(8) C(9) C(10) 110.4(4) ? ? ? yes N(2) C(11) N(3) 108.7(3) ? ? ? yes N(3) C(13) C(12) 123.2(4) ? ? ? yes N(3) C(13) C(14) 106.7(4) ? ? ? yes C(12) C(13) C(14) 130.1(4) ? ? ? yes C(13) C(14) C(15) 106.6(4) ? ? ? yes N(4) C(15) C(14) 110.3(4) ? ? ? yes N(4) C(15) C(16) 121.0(4) ? ? ? yes C(14) C(15) C(16) 128.6(4) ? ? ? yes N(2) C(17) N(5) 107.1(3) ? ? ? yes N(5) C(19) C(18) 121.2(4) ? ? ? yes N(5) C(19) C(20) 106.4(4) ? ? ? yes C(18) C(19) C(20) 132.3(4) ? ? ? yes C(19) C(20) C(21) 106.9(4) ? ? ? yes N(6) C(21) C(20) 110.0(4) ? ? ? yes N(6) C(21) C(22) 121.1(4) ? ? ? yes C(20) C(21) C(22) 128.7(4) ? ? ? yes #------------------------------------------------------------------------------ data_[CoLCl]ClO4 #============================================================================== _audit_creation_date '1999-07-22' _audit_creation_method 'by teXsan for Windows v1.0' _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal ' J. Chem. Soc., Dalton Trans ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr ERT Tiekink ' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 8 8303 5943 ' _publ_contact_author_fax ' 61 8 8303 4358 ' _publ_contact_author_email ' etiekink@chemistry.adelaide.edu.au ' #============================================================================== #============================================================================== data__[CoLCl]ClO4 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 12.86(1) _cell_length_b 13.13(1) _cell_length_c 16.01(2) _cell_angle_alpha 90 _cell_angle_beta 92.50(7) _cell_angle_gamma 90 _cell_volume 2701(4) _cell_formula_units_Z 4 _cell_measurement_temperature 135 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.1 _cell_measurement_theta_max 23.1 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'wedge' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 639.50 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H33 Cl2 Co N6 O4 S2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.029 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.894 _exptl_special_details ; The scan width was (1.15+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 3 scans to achieve I/\s(I) > 20). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 135 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_decay_% -8.11 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 1 0 -3 0 0 -3 -1 0 _diffrn_reflns_number 6801 _reflns_number_total 6525 _reflns_number_gt 3603 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.13043 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.63 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06196 _diffrn_orient_matrix_UB_12 -0.01192 _diffrn_orient_matrix_UB_13 -0.03869 _diffrn_orient_matrix_UB_21 -0.00143 _diffrn_orient_matrix_UB_22 -0.07305 _diffrn_orient_matrix_UB_23 0.01756 _diffrn_orient_matrix_UB_31 -0.04707 _diffrn_orient_matrix_UB_32 0.01791 _diffrn_orient_matrix_UB_33 0.04588 #------------------------------------------------------------------------------ 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 88 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 132 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 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, Table 6.1.1.2) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 8 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.25480(5) 0.12506(5) 0.24784(4) 0.0138(1) 1.000 . Uani d ? Cl(1) 0.20692(9) 0.28567(8) 0.20628(8) 0.0216(3) 1.000 . Uani d ? Cl(2) 0.1495(1) -0.3011(1) 0.4388(1) 0.0431(5) 1.000 . Uani d ? S(1) 0.38518(9) 0.20900(9) 0.31044(8) 0.0188(3) 1.000 . Uani d ? S(2) 0.5942(1) 0.1688(1) 0.3911(1) 0.0359(4) 1.000 . Uani d ? O(1) 0.0844(5) -0.2195(4) 0.4113(4) 0.089(2) 1.000 . Uani d ? O(2) 0.0831(3) -0.3809(3) 0.4628(2) 0.043(1) 1.000 . Uani d ? O(3) 0.2021(4) -0.3293(4) 0.3649(4) 0.079(2) 1.000 . Uani d ? O(4) 0.1958(7) -0.2538(7) 0.5126(5) 0.065(2) 0.580 S Uiso d ? O(4) 0.247(1) -0.320(1) 0.4880(9) 0.085(4) 0.420 S Uiso d ? N(1) 0.2906(3) -0.0088(3) 0.2859(2) 0.017(1) 1.000 . Uani d ? N(2) 0.1316(3) 0.0634(3) 0.1842(2) 0.019(1) 1.000 . Uani d ? N(3) 0.2492(3) 0.0948(3) 0.0770(2) 0.018(1) 1.000 . Uani d ? N(4) 0.3210(3) 0.1008(3) 0.1420(2) 0.017(1) 1.000 . Uani d ? N(5) 0.0589(3) 0.1108(3) 0.3084(3) 0.022(1) 1.000 . Uani d ? N(6) 0.1586(3) 0.1322(3) 0.3376(2) 0.017(1) 1.000 . Uani d ? C(1) 0.4733(3) 0.1219(4) 0.3512(3) 0.021(1) 1.000 . Uani d ? C(2) 0.5901(5) 0.3032(5) 0.3736(5) 0.055(2) 1.000 . Uani d ? C(3) 0.4621(4) 0.0189(4) 0.3552(3) 0.020(1) 1.000 . Uani d ? C(4) 0.3735(4) -0.0402(3) 0.3301(3) 0.019(1) 1.000 . Uani d ? C(5) 0.3877(5) -0.1468(4) 0.3627(4) 0.038(2) 1.000 . Uani d ? C(6) 0.5028(4) -0.1561(4) 0.3833(4) 0.037(2) 1.000 . Uani d ? C(7) 0.5442(4) -0.0501(4) 0.3957(4) 0.033(2) 1.000 . Uani d ? C(8) 0.1998(4) -0.0770(4) 0.2714(4) 0.030(2) 1.000 . Uani d ? C(9) 0.1433(4) -0.0508(3) 0.1922(4) 0.029(1) 1.000 . Uani d ? C(10) 0.0459(4) -0.1115(4) 0.1736(3) 0.029(1) 1.000 . Uani d ? C(11) 0.1405(4) 0.0962(4) 0.0950(3) 0.022(1) 1.000 . Uani d ? C(12) 0.2312(4) 0.0835(4) -0.0772(3) 0.033(2) 1.000 . Uani d ? C(13) 0.2923(4) 0.0849(4) 0.0038(3) 0.023(1) 1.000 . Uani d ? C(14) 0.3984(4) 0.0826(4) 0.0204(3) 0.027(1) 1.000 . Uani d ? C(15) 0.4138(4) 0.0919(3) 0.1084(3) 0.022(1) 1.000 . Uani d ? C(16) 0.5155(4) 0.0863(4) 0.1548(3) 0.027(1) 1.000 . Uani d ? C(17) 0.0397(4) 0.1075(4) 0.2191(3) 0.026(1) 1.000 . Uani d ? C(18) -0.1198(4) 0.0776(5) 0.3554(4) 0.038(2) 1.000 . Uani d ? C(19) -0.0070(4) 0.0997(4) 0.3711(3) 0.025(1) 1.000 . Uani d ? C(20) 0.0527(4) 0.1134(4) 0.4433(3) 0.028(1) 1.000 . Uani d ? C(21) 0.1547(4) 0.1294(4) 0.4218(3) 0.019(1) 1.000 . Uani d ? C(22) 0.2486(4) 0.1389(4) 0.4792(3) 0.028(1) 1.000 . Uani d ? H(2a) 0.6529 0.3332 0.3951 0.066 1.000 . Uiso c ? H(2b) 0.5825 0.3162 0.3152 0.066 1.000 . Uiso c ? H(2c) 0.5329 0.3316 0.4009 0.066 1.000 . Uiso c ? H(5a) 0.3662 -0.1951 0.3212 0.045 1.000 . Uiso c ? H(5b) 0.3491 -0.1568 0.4113 0.045 1.000 . Uiso c ? H(6a) 0.5143 -0.1947 0.4331 0.044 1.000 . Uiso c ? H(6b) 0.5362 -0.1884 0.3386 0.044 1.000 . Uiso c ? H(7a) 0.5538 -0.0351 0.4535 0.040 1.000 . Uiso c ? H(7b) 0.6085 -0.0424 0.3693 0.040 1.000 . Uiso c ? H(8a) 0.1544 -0.0699 0.3162 0.036 1.000 . Uiso c ? H(8b) 0.2233 -0.1455 0.2688 0.036 1.000 . Uiso c ? H(9) 0.1890 -0.0694 0.1497 0.035 1.000 . Uiso c ? H(10a) -0.0035 -0.0971 0.2144 0.035 1.000 . Uiso c ? H(10b) 0.0175 -0.0938 0.1197 0.035 1.000 . Uiso c ? H(10c) 0.0621 -0.1821 0.1748 0.035 1.000 . Uiso c ? H(11a) 0.1030 0.0506 0.0588 0.027 1.000 . Uiso c ? H(11c) 0.1134 0.1631 0.0876 0.027 1.000 . Uiso c ? H(12a) 0.1936 0.1455 -0.0838 0.040 1.000 . Uiso c ? H(12b) 0.2771 0.0762 -0.1218 0.040 1.000 . Uiso c ? H(12c) 0.1838 0.0280 -0.0779 0.040 1.000 . Uiso c ? H(14) 0.4509 0.0761 -0.0192 0.032 1.000 . Uiso c ? H(16a) 0.5178 0.0271 0.1889 0.032 1.000 . Uiso c ? H(16b) 0.5695 0.0834 0.1163 0.032 1.000 . Uiso c ? H(16c) 0.5245 0.1450 0.1891 0.032 1.000 . Uiso c ? H(17a) -0.0196 0.0666 0.2055 0.031 1.000 . Uiso c ? H(17b) 0.0285 0.1744 0.1978 0.031 1.000 . Uiso c ? H(18a) -0.1276 0.0152 0.3258 0.046 1.000 . Uiso c ? H(18b) -0.1526 0.0723 0.4073 0.046 1.000 . Uiso c ? H(18c) -0.1511 0.1310 0.3233 0.046 1.000 . Uiso c ? H(20) 0.0284 0.1121 0.4985 0.034 1.000 . Uiso c ? H(22a) 0.2811 0.2028 0.4705 0.034 1.000 . Uiso c ? H(22b) 0.2285 0.1345 0.5355 0.034 1.000 . Uiso c ? H(22c) 0.2960 0.0856 0.4683 0.034 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 0.0139(3) 0.0147(3) 0.0129(3) 0.0016(3) 0.0015(2) -0.0008(3) Cl(1) 0.0286(6) 0.0174(5) 0.0189(6) 0.0047(5) 0.0016(5) 0.0027(5) Cl(2) 0.0366(8) 0.0476(9) 0.045(1) -0.0127(7) -0.0008(7) -0.0069(8) S(1) 0.0196(6) 0.0171(6) 0.0197(7) -0.0012(5) -0.0005(5) -0.0018(5) S(2) 0.0236(7) 0.0396(8) 0.043(1) -0.0062(6) -0.0113(7) -0.0012(7) O(1) 0.133(5) 0.044(3) 0.096(4) 0.010(3) 0.067(4) 0.007(3) O(2) 0.024(2) 0.061(3) 0.045(3) -0.013(2) 0.006(2) 0.012(2) O(3) 0.071(4) 0.049(3) 0.120(5) -0.010(3) 0.057(4) -0.018(3) N(1) 0.020(2) 0.013(2) 0.016(2) -0.001(2) -0.004(2) 0.003(2) N(2) 0.016(2) 0.020(2) 0.021(2) 0.003(2) -0.001(2) -0.000(2) N(3) 0.016(2) 0.025(2) 0.013(2) 0.003(2) 0.003(2) -0.003(2) N(4) 0.017(2) 0.020(2) 0.013(2) 0.000(2) 0.001(2) -0.008(2) N(5) 0.015(2) 0.027(2) 0.024(2) 0.003(2) -0.004(2) 0.002(2) N(6) 0.017(2) 0.014(2) 0.020(2) 0.003(2) 0.001(2) -0.001(2) C(1) 0.015(2) 0.032(3) 0.018(3) -0.003(2) 0.002(2) -0.003(2) C(2) 0.045(4) 0.040(4) 0.079(5) -0.018(3) -0.009(4) -0.008(4) C(3) 0.021(3) 0.026(3) 0.014(3) 0.006(2) 0.001(2) -0.004(2) C(4) 0.029(3) 0.018(2) 0.011(3) 0.003(2) 0.002(2) -0.003(2) C(5) 0.048(4) 0.021(3) 0.042(4) 0.006(2) -0.015(3) 0.007(3) C(6) 0.043(4) 0.029(3) 0.038(4) 0.014(3) -0.010(3) 0.007(3) C(7) 0.025(3) 0.036(3) 0.037(4) 0.011(2) -0.008(3) 0.001(3) C(8) 0.030(3) 0.020(3) 0.039(4) -0.005(2) -0.001(3) 0.006(3) C(9) 0.026(3) 0.013(2) 0.047(4) -0.001(2) -0.008(3) -0.003(2) C(10) 0.024(3) 0.033(3) 0.032(3) -0.008(2) 0.001(2) -0.001(3) C(11) 0.020(2) 0.033(3) 0.013(3) 0.007(2) -0.002(2) -0.003(2) C(12) 0.041(3) 0.042(3) 0.017(3) -0.001(3) -0.001(3) -0.003(3) C(13) 0.035(3) 0.024(3) 0.011(3) 0.004(2) 0.003(2) -0.004(2) C(14) 0.027(3) 0.034(3) 0.019(3) -0.000(2) 0.012(2) -0.001(2) C(15) 0.025(3) 0.016(2) 0.025(3) 0.002(2) 0.006(2) -0.004(2) C(16) 0.025(3) 0.030(3) 0.027(3) -0.001(2) 0.007(2) -0.014(2) C(17) 0.016(2) 0.029(3) 0.032(3) 0.007(2) 0.002(2) -0.001(2) C(18) 0.029(3) 0.048(4) 0.038(4) -0.004(3) 0.010(3) 0.006(3) C(19) 0.021(3) 0.020(3) 0.035(3) 0.003(2) 0.015(2) 0.009(2) C(20) 0.028(3) 0.028(3) 0.028(3) 0.006(2) 0.010(2) 0.011(3) C(21) 0.025(3) 0.018(2) 0.016(3) 0.005(2) 0.009(2) 0.007(2) C(22) 0.033(3) 0.033(3) 0.019(3) 0.006(2) -0.001(2) 0.000(2) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00036|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3603 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0810 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.140 _refine_ls_shift/su_max 0.0100 _refine_ls_shift/su_mean 0.0004 _refine_diff_density_min -0.77 _refine_diff_density_max 0.97 #============================================================================== # MOLECULAR GEOMETRY _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 Cl(1) 2.288(2) . . ? Co S(1) 2.210(2) . . ? Co N(1) 1.911(5) . . ? Co N(2) 2.016(5) . . ? Co N(4) 1.955(6) . . ? Co N(6) 1.939(6) . . ? Cl(2) O(1) 1.418(8) . . ? Cl(2) O(2) 1.415(6) . . ? Cl(2) O(3) 1.437(8) . . ? Cl(2) O(4) 1.44(1) . . ? Cl(2) O(4') 1.47(2) . . ? S(1) C(1) 1.719(7) . . ? S(2) C(1) 1.767(7) . . ? S(2) C(2) 1.787(9) . . ? O(4) O(4') 1.17(2) . . ? N(1) C(4) 1.320(8) . . ? N(1) C(8) 1.481(9) . . ? N(2) C(9) 1.512(9) . . ? N(2) C(11) 1.501(9) . . ? N(2) C(17) 1.450(9) . . ? N(3) N(4) 1.363(7) . . ? N(3) C(11) 1.439(9) . . ? N(3) C(13) 1.323(9) . . ? N(4) C(15) 1.335(9) . . ? N(5) N(6) 1.375(7) . . ? N(5) C(17) 1.441(9) . . ? N(5) C(19) 1.349(9) . . ? N(6) C(21) 1.352(9) . . ? C(1) C(3) 1.36(1) . . ? C(2) H(2a) 0.95 . . no C(2) H(2b) 0.95 . . no C(2) H(2c) 0.95 . . no C(3) C(4) 1.421(9) . . ? C(3) C(7) 1.515(9) . . ? C(4) C(5) 1.50(1) . . ? C(5) C(6) 1.51(1) . . ? C(5) H(5b) 0.95 . . no C(5) H(5a) 0.95 . . no C(6) C(7) 1.50(1) . . ? C(6) H(6b) 0.95 . . no C(6) H(6a) 0.95 . . no C(7) H(7b) 0.95 . . no C(7) H(7a) 0.95 . . no C(8) C(9) 1.47(1) . . ? C(8) H(8b) 0.95 . . no C(8) H(8a) 0.95 . . no C(9) C(10) 1.504(9) . . ? C(9) H(9) 0.95 . . no C(10) H(10a) 0.95 . . no C(10) H(10b) 0.95 . . no C(10) H(10c) 0.95 . . no C(11) H(11a) 0.95 . . no C(11) H(11b) 0.95 . . no C(12) C(13) 1.49(1) . . ? C(12) H(12a) 0.95 . . no C(12) H(12b) 0.95 . . no C(12) H(12c) 0.95 . . no C(13) C(14) 1.38(1) . . ? C(14) C(15) 1.42(1) . . ? C(14) H(14) 0.95 . . no C(15) C(16) 1.48(1) . . ? C(16) H(16a) 0.95 . . no C(16) H(16b) 0.95 . . no C(16) H(16c) 0.95 . . no C(17) H(17a) 0.95 . . no C(17) H(17b) 0.95 . . no C(18) C(19) 1.49(1) . . ? C(18) H(18c) 0.95 . . no C(18) H(18a) 0.95 . . no C(18) H(18b) 0.95 . . no C(19) C(20) 1.37(1) . . ? C(20) C(21) 1.39(1) . . ? C(20) H(20) 0.95 . . no C(21) C(22) 1.490(9) . . ? C(22) H(22c) 0.95 . . no C(22) H(22a) 0.95 . . no C(22) H(22b) 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) Co S(1) 82.03(8) . . . ? Cl(1) Co N(1) 177.7(2) . . . ? Cl(1) Co N(2) 91.6(2) . . . ? Cl(1) Co N(4) 91.2(2) . . . ? Cl(1) Co N(6) 89.9(2) . . . ? S(1) Co N(1) 98.4(2) . . . ? S(1) Co N(2) 173.5(2) . . . ? S(1) Co N(4) 97.1(2) . . . ? S(1) Co N(6) 97.8(2) . . . ? N(1) Co N(2) 88.0(2) . . . ? N(1) Co N(4) 91.1(2) . . . ? N(1) Co N(6) 87.7(2) . . . ? N(2) Co N(4) 81.9(2) . . . ? N(2) Co N(6) 83.2(2) . . . ? N(4) Co N(6) 165.1(2) . . . ? O(1) Cl(2) O(2) 106.8(4) . . . ? O(1) Cl(2) O(3) 103.4(5) . . . ? O(1) Cl(2) O(4) 98.4(6) . . . ? O(1) Cl(2) O(4') 140.5(8) . . . ? O(2) Cl(2) O(3) 110.1(4) . . . ? O(2) Cl(2) O(4) 109.2(6) . . . ? O(2) Cl(2) O(4') 103.8(8) . . . ? O(3) Cl(2) O(4) 126.4(6) . . . ? O(3) Cl(2) O(4') 88.7(9) . . . ? O(4) Cl(2) O(4') 47.3(8) . . . ? Co S(1) C(1) 108.4(2) . . . ? C(1) S(2) C(2) 105.6(4) . . . ? Cl(2) O(4) O(4') 68(1) . . . ? Cl(2) O(4') O(4) 65(1) . . . ? Co N(1) C(4) 129.5(4) . . . ? Co N(1) C(8) 109.2(4) . . . ? C(4) N(1) C(8) 120.6(6) . . . ? Co N(2) C(9) 106.4(4) . . . ? Co N(2) C(11) 105.9(4) . . . ? Co N(2) C(17) 106.3(4) . . . ? C(9) N(2) C(11) 110.8(6) . . . ? C(9) N(2) C(17) 116.3(6) . . . ? C(11) N(2) C(17) 110.5(5) . . . ? N(4) N(3) C(11) 118.5(6) . . . ? N(4) N(3) C(13) 112.6(6) . . . ? C(11) N(3) C(13) 128.8(6) . . . ? Co N(4) N(3) 111.4(4) . . . ? Co N(4) C(15) 142.5(5) . . . ? N(3) N(4) C(15) 106.0(6) . . . ? N(6) N(5) C(17) 117.4(6) . . . ? N(6) N(5) C(19) 112.1(6) . . . ? C(17) N(5) C(19) 130.4(6) . . . ? Co N(6) N(5) 110.7(4) . . . ? Co N(6) C(21) 142.3(5) . . . ? N(5) N(6) C(21) 105.0(6) . . . ? S(1) C(1) S(2) 117.4(4) . . . ? S(1) C(1) C(3) 127.6(5) . . . ? S(2) C(1) C(3) 115.0(5) . . . ? S(2) C(2) H(2a) 109.5 . . . no S(2) C(2) H(2b) 109.5 . . . no S(2) C(2) H(2c) 109.5 . . . no H(2a) C(2) H(2b) 109.5 . . . no H(2a) C(2) H(2c) 109.5 . . . no H(2b) C(2) H(2c) 109.5 . . . no C(1) C(3) C(4) 127.9(6) . . . ? C(1) C(3) C(7) 122.7(6) . . . ? C(4) C(3) C(7) 109.2(6) . . . ? N(1) C(4) C(3) 126.9(6) . . . ? N(1) C(4) C(5) 124.0(6) . . . ? C(3) C(4) C(5) 109.1(6) . . . ? C(4) C(5) C(6) 104.7(7) . . . ? C(4) C(5) H(5b) 110.6 . . . no C(4) C(5) H(5a) 110.6 . . . no C(6) C(5) H(5b) 110.6 . . . no C(6) C(5) H(5a) 110.6 . . . no H(5b) C(5) H(5a) 109.5 . . . no C(5) C(6) C(7) 107.1(6) . . . ? C(5) C(6) H(6b) 110.1 . . . no C(5) C(6) H(6a) 110.1 . . . no C(7) C(6) H(6b) 110.1 . . . no C(7) C(6) H(6a) 110.1 . . . no H(6b) C(6) H(6a) 109.5 . . . no C(3) C(7) C(6) 105.1(6) . . . ? C(3) C(7) H(7b) 110.5 . . . no C(3) C(7) H(7a) 110.5 . . . no C(6) C(7) H(7b) 110.6 . . . no C(6) C(7) H(7a) 110.5 . . . no H(7b) C(7) H(7a) 109.5 . . . no N(1) C(8) C(9) 110.5(6) . . . ? N(1) C(8) H(8b) 109.2 . . . no N(1) C(8) H(8a) 109.2 . . . no C(9) C(8) H(8b) 109.2 . . . no C(9) C(8) H(8a) 109.2 . . . no H(8b) C(8) H(8a) 109.5 . . . no N(2) C(9) C(8) 110.4(6) . . . ? N(2) C(9) C(10) 115.5(6) . . . ? N(2) C(9) H(9) 104.9 . . . no C(8) C(9) C(10) 115.0(7) . . . ? C(8) C(9) H(9) 104.9 . . . no C(10) C(9) H(9) 104.9 . . . no C(9) C(10) H(10a) 109.5 . . . no C(9) C(10) H(10b) 109.5 . . . no C(9) C(10) H(10c) 109.5 . . . no H(10a) C(10) H(10b) 109.5 . . . no H(10a) C(10) H(10c) 109.5 . . . no H(10b) C(10) H(10c) 109.5 . . . no N(2) C(11) N(3) 107.6(5) . . . ? N(2) C(11) H(11a) 109.9 . . . no N(2) C(11) H(11b) 109.9 . . . no N(3) C(11) H(11a) 109.9 . . . no N(3) C(11) H(11b) 109.9 . . . no H(11a) C(11) H(11b) 109.5 . . . no C(13) C(12) H(12a) 109.5 . . . no C(13) C(12) H(12b) 109.5 . . . no C(13) C(12) H(12c) 109.5 . . . no H(12a) C(12) H(12b) 109.5 . . . no H(12a) C(12) H(12c) 109.5 . . . no H(12b) C(12) H(12c) 109.5 . . . no N(3) C(13) C(12) 123.1(7) . . . ? N(3) C(13) C(14) 106.4(6) . . . ? C(12) C(13) C(14) 130.4(8) . . . ? C(13) C(14) C(15) 106.4(7) . . . ? C(13) C(14) H(14) 126.8 . . . no C(15) C(14) H(14) 126.8 . . . no N(4) C(15) C(14) 108.6(6) . . . ? N(4) C(15) C(16) 126.1(7) . . . ? C(14) C(15) C(16) 125.2(7) . . . ? C(15) C(16) H(16a) 109.5 . . . no C(15) C(16) H(16b) 109.5 . . . no C(15) C(16) H(16c) 109.5 . . . no H(16a) C(16) H(16b) 109.5 . . . no H(16a) C(16) H(16c) 109.5 . . . no H(16b) C(16) H(16c) 109.5 . . . no N(2) C(17) N(5) 106.7(5) . . . ? N(2) C(17) H(17a) 110.2 . . . no N(2) C(17) H(17b) 110.2 . . . no N(5) C(17) H(17a) 110.2 . . . no N(5) C(17) H(17b) 110.2 . . . no H(17a) C(17) H(17b) 109.5 . . . no C(19) C(18) H(18c) 109.5 . . . no C(19) C(18) H(18a) 109.5 . . . no C(19) C(18) H(18b) 109.5 . . . no H(18c) C(18) H(18a) 109.5 . . . no H(18c) C(18) H(18b) 109.5 . . . no H(18a) C(18) H(18b) 109.5 . . . no N(5) C(19) C(18) 122.3(7) . . . ? N(5) C(19) C(20) 105.4(6) . . . ? C(18) C(19) C(20) 132.3(8) . . . ? C(19) C(20) C(21) 108.2(7) . . . ? C(19) C(20) H(20) 125.9 . . . no C(21) C(20) H(20) 125.9 . . . no N(6) C(21) C(20) 109.1(6) . . . ? N(6) C(21) C(22) 123.2(6) . . . ? C(20) C(21) C(22) 127.6(7) . . . ? C(21) C(22) H(22c) 109.5 . . . no C(21) C(22) H(22a) 109.5 . . . no C(21) C(22) H(22b) 109.5 . . . no H(22c) C(22) H(22a) 109.5 . . . no H(22c) C(22) H(22b) 109.5 . . . no H(22a) C(22) H(22b) 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 S(2) O(4) 3.25(1) . 3_656 no S(2) O(4') 3.39(2) . 3_656 no O(1) C(20) 3.29(1) . 3_556 no O(1) C(8) 3.32(1) . . no O(1) C(17) 3.43(1) . 2_545 no O(2) C(11) 2.998(8) . 2_545 no O(2) C(17) 3.254(9) . 2_545 no O(2) C(12) 3.35(1) . 4_545 no O(2) C(10) 3.43(1) . 4_545 no O(2) C(11) 3.589(9) . 4_545 no O(3) C(5) 3.38(1) . . no O(3) C(17) 3.43(1) . 2_545 no O(3) C(12) 3.48(1) . 4_545 no O(4) C(2) 3.30(1) . 3_656 no O(4) C(18) 3.31(2) . 3_556 no O(4') C(2) 2.99(2) . 3_656 no O(4') C(13) 3.54(2) . 4_545 no O(4') C(5) 3.58(2) . . no C(6) C(16) 3.44(1) . 2_645 no C(6) C(15) 3.48(1) . 2_645 no C(7) C(22) 3.47(1) . 3_656 no C(14) C(14) 3.48(2) . 3_655 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 S(1) C(1) S(2) . . . . 170.8(3) no Co S(1) C(1) C(3) . . . . -7.7(8) no Co N(1) C(4) C(3) . . . . -5(1) no Co N(1) C(4) C(5) . . . . 174.2(6) no Co N(1) C(8) C(9) . . . . 37.0(7) no Co N(2) C(9) C(8) . . . . 29.0(8) no Co N(2) C(9) C(10) . . . . 161.5(6) no Co N(2) C(11) N(3) . . . . 37.7(6) no Co N(2) C(17) N(5) . . . . -41.3(6) no Co N(4) N(3) C(11) . . . . -6.1(7) no Co N(4) N(3) C(13) . . . . 176.0(5) no Co N(4) C(15) C(14) . . . . -174.6(6) no Co N(4) C(15) C(16) . . . . 9(1) no Co N(6) N(5) C(17) . . . . -11.9(7) no Co N(6) N(5) C(19) . . . . 170.5(4) no Co N(6) C(21) C(20) . . . . -164.7(6) no Co N(6) C(21) C(22) . . . . 13(1) no Cl(1) Co S(1) C(1) . . . . -172.7(3) no Cl(1) Co N(1) C(4) . . . . -107(4) no Cl(1) Co N(1) C(8) . . . . 63(4) no Cl(1) Co N(2) C(9) . . . . 175.3(5) no Cl(1) Co N(2) C(11) . . . . 57.4(4) no Cl(1) Co N(2) C(17) . . . . -60.1(4) no Cl(1) Co N(4) N(3) . . . . -68.5(4) no Cl(1) Co N(4) C(15) . . . . 107.4(8) no Cl(1) Co N(6) N(5) . . . . 81.1(4) no Cl(1) Co N(6) C(21) . . . . -118.8(8) no S(1) Co N(1) C(4) . . . . -5.2(7) no S(1) Co N(1) C(8) . . . . 164.8(5) no S(1) Co N(2) C(9) . . . . 166(1) no S(1) Co N(2) C(11) . . . . 48(2) no S(1) Co N(2) C(17) . . . . -70(2) no S(1) Co N(4) N(3) . . . . -150.6(4) no S(1) Co N(4) C(15) . . . . 25.3(8) no S(1) Co N(6) N(5) . . . . 163.0(4) no S(1) Co N(6) C(21) . . . . -36.9(8) no S(1) C(1) S(2) C(2) . . . . -1.5(6) no S(1) C(1) C(3) C(4) . . . . -3(1) no S(1) C(1) C(3) C(7) . . . . -177.7(6) no S(2) C(1) C(3) C(4) . . . . 178.3(6) no S(2) C(1) C(3) C(7) . . . . 4(1) no O(1) Cl(2) O(4) O(4') . . . . -158(1) no O(1) Cl(2) O(4') O(4) . . . . 36(2) no O(2) Cl(2) O(4) O(4') . . . . 91(1) no O(2) Cl(2) O(4') O(4) . . . . -104(1) no O(3) Cl(2) O(4) O(4') . . . . -44(2) no O(3) Cl(2) O(4') O(4) . . . . 146(1) no N(1) Co S(1) C(1) . . . . 9.6(3) no N(1) Co N(2) C(9) . . . . -7.0(5) no N(1) Co N(2) C(11) . . . . -124.9(4) no N(1) Co N(2) C(17) . . . . 117.6(5) no N(1) Co N(4) N(3) . . . . 110.7(4) no N(1) Co N(4) C(15) . . . . -73.4(8) no N(1) Co N(6) N(5) . . . . -98.7(4) no N(1) Co N(6) C(21) . . . . 61.4(8) no N(1) C(4) C(3) C(1) . . . . 12(1) no N(1) C(4) C(3) C(7) . . . . -173.2(7) no N(1) C(4) C(5) C(6) . . . . 162.3(7) no N(1) C(8) C(9) N(2) . . . . -43.9(9) no N(1) C(8) C(9) C(10) . . . . -176.7(6) no N(2) Co S(1) C(1) . . . . -163(2) no N(2) Co N(1) C(4) . . . . 174.0(7) no N(2) Co N(1) C(8) . . . . -16.0(5) no N(2) Co N(4) N(3) . . . . 22.9(4) no N(2) Co N(4) C(15) . . . . -161.2(8) no N(2) Co N(6) N(5) . . . . -10.5(4) no N(2) Co N(6) C(21) . . . . 149.6(8) no N(2) C(11) N(3) N(4) . . . . -22.0(8) no N(2) C(11) N(3) C(13) . . . . 155.6(7) no N(2) C(17) N(5) N(6) . . . . 36.6(8) no N(2) C(17) N(5) C(19) . . . . -146.3(7) no N(3) N(4) Co N(6) . . . . 26(1) no N(3) N(4) C(15) C(14) . . . . 1.4(7) no N(3) N(4) C(15) C(16) . . . . -175.3(6) no N(3) C(11) N(2) C(9) . . . . -77.2(7) no N(3) C(11) N(2) C(17) . . . . 152.4(5) no N(3) C(13) C(14) C(15) . . . . 0.0(8) no N(4) Co S(1) C(1) . . . . -82.5(3) no N(4) Co N(1) C(4) . . . . 92.2(6) no N(4) Co N(1) C(8) . . . . -97.9(5) no N(4) Co N(2) C(9) . . . . 84.3(5) no N(4) Co N(2) C(11) . . . . -33.6(4) no N(4) Co N(2) C(17) . . . . -151.1(5) no N(4) Co N(6) N(5) . . . . -13(1) no N(4) Co N(6) C(21) . . . . 147.0(8) no N(4) N(3) C(13) C(12) . . . . -175.9(6) no N(4) N(3) C(13) C(14) . . . . 0.9(8) no N(4) C(15) C(14) C(13) . . . . -0.9(8) no N(5) N(6) C(21) C(20) . . . . -4.0(8) no N(5) N(6) C(21) C(22) . . . . 174.1(6) no N(5) C(17) N(2) C(9) . . . . 76.9(7) no N(5) C(17) N(2) C(11) . . . . -155.8(5) no N(5) C(19) C(20) C(21) . . . . -1.8(8) no N(6) Co S(1) C(1) . . . . 98.5(3) no N(6) Co N(1) C(4) . . . . -102.7(6) no N(6) Co N(1) C(8) . . . . 67.2(5) no N(6) Co N(2) C(9) . . . . -95.0(5) no N(6) Co N(2) C(11) . . . . 147.1(4) no N(6) Co N(2) C(17) . . . . 29.6(4) no N(6) Co N(4) C(15) . . . . -158.6(8) no N(6) N(5) C(19) C(18) . . . . 179.2(6) no N(6) N(5) C(19) C(20) . . . . -0.7(8) no N(6) C(21) C(20) C(19) . . . . 3.7(8) no C(1) C(3) C(4) C(5) . . . . -167.8(8) no C(1) C(3) C(7) C(6) . . . . -177.9(8) no C(2) S(2) C(1) C(3) . . . . 177.1(7) no C(3) C(4) N(1) C(8) . . . . -174.2(7) no C(3) C(4) C(5) C(6) . . . . -18.2(9) no C(3) C(7) C(6) C(5) . . . . -17.9(9) no C(4) N(1) C(8) C(9) . . . . -152.0(7) no C(4) C(3) C(7) C(6) . . . . 6.7(9) no C(4) C(5) C(6) C(7) . . . . 22.1(9) no C(5) C(4) N(1) C(8) . . . . 5(1) no C(5) C(4) C(3) C(7) . . . . 7.3(9) no C(8) C(9) N(2) C(11) . . . . 143.7(6) no C(8) C(9) N(2) C(17) . . . . -89.1(8) no C(10) C(9) N(2) C(11) . . . . -83.8(8) no C(10) C(9) N(2) C(17) . . . . 43.4(9) no C(11) N(3) N(4) C(15) . . . . 176.5(6) no C(11) N(3) C(13) C(12) . . . . 6(1) no C(11) N(3) C(13) C(14) . . . . -176.8(7) no C(12) C(13) C(14) C(15) . . . . 176.5(7) no C(13) N(3) N(4) C(15) . . . . -1.4(7) no C(13) C(14) C(15) C(16) . . . . 175.8(7) no C(17) N(5) N(6) C(21) . . . . -179.4(6) no C(17) N(5) C(19) C(18) . . . . 2(1) no C(17) N(5) C(19) C(20) . . . . -178.0(7) no C(18) C(19) C(20) C(21) . . . . 178.3(8) no C(19) N(5) N(6) C(21) . . . . 2.9(7) no C(19) C(20) C(21) C(22) . . . . -174.3(7) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================