# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1447 data_1 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 31 14:10:50 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Enraf Nonius CAD4 Diffractometer' _computing_cell_refinement 'Enraf Nonius CAD4 Diffractometer ' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_formula_weight 370.75 _chemical_formula_sum 'C6 H20 Cl Co N4 O4 S2 ' _chemical_formula_moiety 'C6 H20 Cl Co N4 O4 S2 ' _cell_length_a 10.5077(6) _cell_length_b 17.108(1) _cell_length_c 15.7022(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2822.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 11.0 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2 ' _symmetry_Int_Tables_number 43 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z 1/4-x,1/4+y,1/4+z 1/4+x,1/4-y,1/4+z x,1/2+y,1/2+z -x,1/2-y,1/2+z 1/4-x,3/4+y,3/4+z 1/4+x,3/4-y,3/4+z 1/2+x,y,1/2+z 1/2-x,-y,1/2+z 3/4-x,1/4+y,3/4+z 3/4+x,1/4-y,3/4+z 1/2+x,1/2+y,z 1/2-x,1/2-y,z 3/4-x,3/4+y,1/4+z 3/4+x,3/4-y,1/4+z #------------------------------------------------------------------------------ _exptl_crystal_description cubic _exptl_crystal_colour purple _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.380 _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768.00 _exptl_absorpt_coefficient_mu 1.712 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_correction_T_max 0.999 _diffrn_ambient_temperature 296 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source ' Enraf Nonius sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method '\w-\2q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 4312 _reflns_number_total 4312 _reflns_number_observed 3878 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.015 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 60.00 _diffrn_reflns_reduction_process 'Lp corrections applied' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags Co(1) Co 0.0000 0.0000 0.5436 0.01763(6) Uani 1.00 d S Cl(1) Cl -0.2500 0.2500 0.73788(6) 0.0392(2) Uani 1.00 d S S(1) S -0.03304(4) -0.13201(2) 0.53736(3) 0.02611(8) Uani 1.00 d . O(1) O -0.3593(2) 0.2619(2) 0.7908(2) 0.0654(6) Uani 1.00 d . O(2) O -0.2677(3) 0.1821(2) 0.6857(3) 0.086(1) Uani 1.00 d . N(1) N -0.1344(2) 0.00763(9) 0.4561(1) 0.0260(3) Uani 1.00 d . N(2) N -0.1249(2) 0.01474(10) 0.63654(10) 0.0251(3) Uani 1.00 d . C(1) C -0.1649(2) -0.1328(1) 0.4625(1) 0.0348(4) Uani 1.00 d . C(2) C -0.1517(2) -0.0640(1) 0.4032(1) 0.0332(4) Uani 1.00 d . C(3) C -0.0561(2) 0.0275(1) 0.7179(1) 0.0307(4) Uani 1.00 d . H(1) H -0.2127 0.0184 0.4840 0.0312 Uiso 1.00 calc . H(2) H -0.1137 0.0497 0.4191 0.0312 Uiso 1.00 calc . H(5) H -0.1767 0.0589 0.6245 0.0301 Uiso 1.00 calc . H(6) H -0.1769 -0.0305 0.6412 0.0301 Uiso 1.00 calc . H(9) H -0.1635 -0.1800 0.4306 0.0418 Uiso 1.00 calc . H(10) H -0.2430 -0.1292 0.4927 0.0418 Uiso 1.00 calc . H(13) H -0.2262 -0.0591 0.3693 0.0399 Uiso 1.00 calc . H(14) H -0.0799 -0.0711 0.3673 0.0399 Uiso 1.00 calc . H(17) H -0.0276 0.0801 0.7215 0.0368 Uiso 1.00 calc . H(18) H -0.1104 0.0163 0.7648 0.0368 Uiso 1.00 calc . 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) 0.0164(1) 0.0194(1) 0.0170(1) 0.00176(8) 0.0000 0.0000 Cl(1) 0.0238(3) 0.0586(4) 0.0351(3) -0.0006(2) 0.0000 0.0000 S(1) 0.0308(2) 0.0208(1) 0.0267(2) 0.0010(1) -0.0002(2) 0.0018(1) O(1) 0.0268(7) 0.121(2) 0.049(1) 0.0096(8) 0.0080(9) 0.011(1) O(2) 0.077(2) 0.087(2) 0.094(2) -0.002(1) -0.012(1) -0.041(1) N(1) 0.0243(7) 0.0295(6) 0.0243(7) 0.0017(5) -0.0051(6) 0.0040(5) N(2) 0.0219(6) 0.0302(6) 0.0232(6) -0.0004(5) 0.0043(5) -0.0025(5) C(1) 0.0359(9) 0.0319(8) 0.0367(10) -0.0083(7) -0.0058(8) -0.0019(7) C(2) 0.0380(8) 0.0377(8) 0.0240(7) -0.0027(8) -0.0086(7) -0.0030(6) C(3) 0.0373(9) 0.0347(8) 0.0201(7) -0.0061(7) 0.0040(6) -0.0043(6) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|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 3878 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.962 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.15 _refine_diff_density_max 0.38 #------------------------------------------------------------------------------ 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) S(1) 2.2871(4) 1_555 1_555 yes Co(1) S(1) 2.2871(4) 1_555 2_555 yes Co(1) N(1) 1.975(2) 1_555 1_555 yes Co(1) N(1) 1.975(2) 1_555 2_555 yes Co(1) N(2) 1.979(2) 1_555 1_555 yes Co(1) N(2) 1.979(2) 1_555 2_555 yes Cl(1) O(1) 1.432(2) 1_555 1_555 yes Cl(1) O(1) 1.432(2) 1_555 14_455 yes Cl(1) O(2) 1.435(3) 1_555 1_555 yes Cl(1) O(2) 1.435(3) 1_555 14_455 yes S(1) C(1) 1.817(2) 1_555 1_555 yes N(1) C(2) 1.492(2) 1_555 1_555 yes N(2) C(3) 1.484(2) 1_555 1_555 yes C(1) C(2) 1.508(3) 1_555 1_555 yes C(3) C(3) 1.509(4) 1_555 2_555 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(1) S(1) 175.09(3) 1_555 1_555 2_555 yes S(1) Co(1) N(1) 85.81(4) 1_555 1_555 1_555 yes S(1) Co(1) N(1) 90.77(4) 1_555 1_555 2_555 yes S(1) Co(1) N(2) 93.25(5) 1_555 1_555 1_555 yes S(1) Co(1) N(2) 90.37(5) 1_555 1_555 2_555 yes S(1) Co(1) N(1) 90.77(4) 2_555 1_555 1_555 yes S(1) Co(1) N(1) 85.81(4) 2_555 1_555 2_555 yes S(1) Co(1) N(2) 90.37(5) 2_555 1_555 1_555 yes S(1) Co(1) N(2) 93.25(5) 2_555 1_555 2_555 yes N(1) Co(1) N(1) 91.8(1) 1_555 1_555 2_555 yes N(1) Co(1) N(2) 91.73(7) 1_555 1_555 1_555 yes N(1) Co(1) N(2) 174.82(7) 1_555 1_555 2_555 yes N(1) Co(1) N(2) 174.82(7) 2_555 1_555 1_555 yes N(1) Co(1) N(2) 91.73(7) 2_555 1_555 2_555 yes N(2) Co(1) N(2) 84.98(10) 1_555 1_555 2_555 yes O(1) Cl(1) O(1) 109.0(2) 1_555 1_555 14_455 yes O(1) Cl(1) O(2) 110.0(2) 1_555 1_555 1_555 yes O(1) Cl(1) O(2) 108.7(2) 1_555 1_555 14_455 yes O(1) Cl(1) O(2) 108.7(2) 14_455 1_555 1_555 yes O(1) Cl(1) O(2) 110.0(2) 14_455 1_555 14_455 yes O(2) Cl(1) O(2) 110.3(4) 1_555 1_555 14_455 yes Co(1) S(1) C(1) 98.70(6) 1_555 1_555 1_555 yes Co(1) N(1) C(2) 114.9(1) 1_555 1_555 1_555 yes Co(1) N(1) H(1) 108.1(1) 1_555 1_555 1_555 no Co(1) N(1) H(2) 108.1(1) 1_555 1_555 1_555 no C(2) N(1) H(1) 108.1(2) 1_555 1_555 1_555 no C(2) N(1) H(2) 108.1(2) 1_555 1_555 1_555 no H(1) N(1) H(2) 109.5(2) 1_555 1_555 1_555 no Co(1) N(2) C(3) 109.3(1) 1_555 1_555 1_555 yes Co(1) N(2) H(5) 109.5(1) 1_555 1_555 1_555 no Co(1) N(2) H(6) 109.5(1) 1_555 1_555 1_555 no C(3) N(2) H(5) 109.5(1) 1_555 1_555 1_555 no C(3) N(2) H(6) 109.5(1) 1_555 1_555 1_555 no H(5) N(2) H(6) 109.5(2) 1_555 1_555 1_555 no S(1) C(1) C(2) 108.9(1) 1_555 1_555 1_555 yes S(1) C(1) H(9) 109.6(2) 1_555 1_555 1_555 no S(1) C(1) H(10) 109.6(2) 1_555 1_555 1_555 no C(2) C(1) H(9) 109.6(2) 1_555 1_555 1_555 no C(2) C(1) H(10) 109.6(2) 1_555 1_555 1_555 no H(9) C(1) H(10) 109.5(2) 1_555 1_555 1_555 no N(1) C(2) C(1) 108.0(2) 1_555 1_555 1_555 yes N(1) C(2) H(13) 109.8(2) 1_555 1_555 1_555 no N(1) C(2) H(14) 109.8(2) 1_555 1_555 1_555 no C(1) C(2) H(13) 109.8(2) 1_555 1_555 1_555 no C(1) C(2) H(14) 109.8(2) 1_555 1_555 1_555 no H(13) C(2) H(14) 109.5(2) 1_555 1_555 1_555 no N(2) C(3) C(3) 106.8(1) 1_555 1_555 2_555 yes N(2) C(3) H(17) 110.1(2) 1_555 1_555 1_555 no N(2) C(3) H(18) 110.1(2) 1_555 1_555 1_555 no C(3) C(3) H(17) 110.1(2) 2_555 1_555 1_555 no C(3) C(3) H(18) 110.1(2) 2_555 1_555 1_555 no H(17) C(3) H(18) 109.5(2) 1_555 1_555 1_555 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co(1) S(1) C(1) C(2) 30.3(1) 1_555 1_555 1_555 1_555 yes Co(1) S(1) C(1) C(2) 30.3(1) 1_555 2_555 2_555 2_555 yes Co(1) N(1) C(2) C(1) 50.8(2) 1_555 1_555 1_555 1_555 yes Co(1) N(1) C(2) C(1) 50.8(2) 1_555 2_555 2_555 2_555 yes Co(1) N(2) C(3) C(3) -39.9(2) 1_555 1_555 1_555 2_555 yes Co(1) N(2) C(3) C(3) -39.9(2) 1_555 2_555 2_555 1_555 yes S(1) Co(1) S(1) C(1) -49.58(7) 1_555 1_555 2_555 2_555 yes S(1) Co(1) N(1) C(2) -24.6(1) 1_555 1_555 1_555 1_555 yes S(1) Co(1) N(1) C(2) 151.9(1) 1_555 1_555 2_555 2_555 yes S(1) Co(1) N(2) C(3) 104.6(1) 1_555 1_555 1_555 1_555 yes S(1) Co(1) N(2) C(3) -78.7(1) 1_555 1_555 2_555 2_555 yes S(1) C(1) C(2) N(1) -51.6(2) 1_555 1_555 1_555 1_555 yes N(1) Co(1) S(1) C(1) -3.62(8) 1_555 1_555 1_555 1_555 yes N(1) Co(1) S(1) C(1) -95.39(10) 1_555 1_555 2_555 2_555 yes N(1) Co(1) N(1) C(2) 66.1(1) 1_555 1_555 2_555 2_555 yes N(1) Co(1) N(2) C(3) -169.5(1) 1_555 1_555 1_555 1_555 yes N(1) Co(1) N(2) C(3) -36.3(9) 1_555 1_555 2_555 2_555 yes N(2) Co(1) S(1) C(1) 87.88(9) 1_555 1_555 1_555 1_555 yes N(2) Co(1) S(1) C(1) 172.87(9) 1_555 1_555 2_555 2_555 yes N(2) Co(1) N(1) C(2) -117.7(1) 1_555 1_555 1_555 1_555 yes N(2) Co(1) N(1) C(2) -67.1(9) 1_555 1_555 2_555 2_555 yes N(2) Co(1) N(2) C(3) 14.50(9) 1_555 1_555 2_555 2_555 yes N(2) C(3) C(3) N(2) 51.9(3) 1_555 1_555 2_555 2_555 yes #------------------------------------------------------------------------------ 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(1) N(1) 3.367(2) 1_555 15_445 ? O(1) N(1) 3.005(3) 1_555 3_455 ? O(1) N(2) 3.172(3) 1_555 3_455 ? O(1) C(1) 3.493(3) 1_555 10_455 ? O(1) C(2) 3.559(3) 1_555 3_455 ? O(2) N(2) 3.323(4) 1_555 1_555 ? O(2) C(3) 3.492(4) 1_555 1_555 ? O(2) C(2) 3.511(4) 1_555 3_455 ? O(2) C(3) 3.511(5) 1_555 12_454 ? O(2) C(1) 3.540(4) 1_555 3_455 ? #------------------------------------------------------------------------------