#------------------------------------------------------------------------------ #$Date: 2009-05-14 17:03:35 +0300 (Thu, 14 May 2009) $ #$Revision: 725 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/8000000.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_8000000 loop_ _publ_author_name 'Takashi Aridomi' 'Tatsuya Kawamoto' 'Asako Igashira-Kamiyama' 'Takumi Konno' _publ_contact_author ; Takumi Konno Department of Chemistry, Graduate School of Science, Osaka University, Toyonaka, Osaka, 560-0043, Japan ; _publ_section_title ; The First S-Bridged CoIIICdIICoIII and CoIIICdII2CoIII Structures Controlled by Chirality of Mono(thiolato)-Type Cobalt(III) Units ; _journal_issue 3 _journal_name_full 'Chemistry Letters' _journal_page_first 292 _journal_volume 34 _journal_year 2005 _chemical_formula_sum 'C6 H22 Cd0.50 Cl3 Co N5 O4 S' _chemical_formula_weight 481.83 _chemical_name_systematic ; ? ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 96.041(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.5547(14) _cell_length_b 13.8816(14) _cell_length_c 13.5666(13) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 15.0 _cell_measurement_theta_min 14.2 _cell_volume 1602.1(3) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.1372 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 4941 _diffrn_reflns_theta_full 30.01 _diffrn_reflns_theta_max 30.01 _diffrn_reflns_theta_min 2.69 _diffrn_standards_decay_% -0.91 _diffrn_standards_interval_count 0 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.366 _exptl_absorpt_correction_T_max 0.8519 _exptl_absorpt_correction_T_min 0.6490 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 972 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.917 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.156 _refine_ls_extinction_coef 0.0008(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 190 _refine_ls_number_reflns 4661 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.969 _refine_ls_R_factor_all 0.1530 _refine_ls_R_factor_gt 0.0435 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.1230 _reflns_number_gt 2335 _reflns_number_total 4661 _reflns_threshold_expression >2sigma(I) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Cd1 Cd 0.5000 0.0000 0.5000 0.02760(15) Uani 1 2 d S Co1 Co 0.26115(9) 0.22067(5) 0.31166(5) 0.02146(16) Uani 1 1 d . Cl1 Cl 0.2706(2) -0.12426(14) 0.46103(12) 0.0512(5) Uani 1 1 d . Cl2 Cl 0.6693(2) -0.11586(12) 0.39556(11) 0.0439(4) Uani 1 1 d . Cl3 Cl 0.76670(19) 0.39933(11) 0.41106(11) 0.0354(3) Uani 1 1 d . S1 S 0.39593(17) 0.08114(10) 0.32302(9) 0.0252(3) Uani 1 1 d . O1 O 0.6338(8) 0.4139(6) 0.3377(5) 0.095(2) Uani 1 1 d . O2 O 0.7045(8) 0.3892(4) 0.5029(4) 0.0735(19) Uani 1 1 d . O3 O 0.8593(8) 0.4836(4) 0.4069(4) 0.0734(19) Uani 1 1 d . O4 O 0.8481(10) 0.3168(5) 0.3873(7) 0.118(3) Uani 1 1 d . N1 N 0.4164(6) 0.2682(3) 0.2255(3) 0.0292(10) Uani 1 1 d . H5 H 0.3644 0.2964 0.1720 0.035 Uiso 1 1 calc R H6 H 0.4754 0.3139 0.2587 0.035 Uiso 1 1 calc R N2 N 0.1563(6) 0.3495(3) 0.3004(3) 0.0303(10) Uani 1 1 d . H7 H 0.1557 0.3722 0.2383 0.036 Uiso 1 1 calc R H8 H 0.0562 0.3444 0.3146 0.036 Uiso 1 1 calc R N3 N 0.3799(6) 0.2718(3) 0.4308(3) 0.0285(10) Uani 1 1 d . H13 H 0.3849 0.2274 0.4794 0.034 Uiso 1 1 calc R H14 H 0.4787 0.2857 0.4182 0.034 Uiso 1 1 calc R N4 N 0.1211(6) 0.1742(3) 0.1968(3) 0.0296(10) Uani 1 1 d . H15 H 0.1033 0.2218 0.1520 0.035 Uiso 1 1 calc R H16 H 0.1669 0.1249 0.1677 0.035 Uiso 1 1 calc R N5 N 0.1042(5) 0.1643(3) 0.3927(3) 0.0284(10) Uani 1 1 d . H21 H 0.1532 0.1339 0.4458 0.034 Uiso 1 1 calc R H22 H 0.0433 0.2111 0.4141 0.034 Uiso 1 1 calc R C1 C 0.5727(7) 0.1272(5) 0.2767(4) 0.0328(13) Uani 1 1 d . H1 H 0.6357 0.1621 0.3286 0.039 Uiso 1 1 calc R H2 H 0.6351 0.0745 0.2550 0.039 Uiso 1 1 calc R C2 C 0.5235(7) 0.1936(5) 0.1909(4) 0.0355(14) Uani 1 1 d . H3 H 0.6151 0.2240 0.1680 0.043 Uiso 1 1 calc R H4 H 0.4697 0.1574 0.1364 0.043 Uiso 1 1 calc R C3 C 0.2452(8) 0.4159(4) 0.3715(5) 0.0383(15) Uani 1 1 d . H9 H 0.1777 0.4681 0.3887 0.046 Uiso 1 1 calc R H10 H 0.3335 0.4433 0.3419 0.046 Uiso 1 1 calc R C4 C 0.3029(8) 0.3593(4) 0.4628(4) 0.0374(15) Uani 1 1 d . H11 H 0.3768 0.3975 0.5056 0.045 Uiso 1 1 calc R H12 H 0.2153 0.3423 0.4993 0.045 Uiso 1 1 calc R C5 C -0.0296(7) 0.1420(5) 0.2305(4) 0.0360(14) Uani 1 1 d . H17 H -0.0814 0.0967 0.1835 0.043 Uiso 1 1 calc R H18 H -0.0987 0.1967 0.2358 0.043 Uiso 1 1 calc R C6 C 0.0067(7) 0.0950(4) 0.3297(4) 0.0348(13) Uani 1 1 d . H19 H -0.0896 0.0808 0.3587 0.042 Uiso 1 1 calc R H20 H 0.0637 0.0353 0.3232 0.042 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0359(3) 0.0218(3) 0.0235(2) -0.0019(2) -0.0044(2) 0.0027(3) Co1 0.0237(4) 0.0224(3) 0.0175(3) 0.0017(3) -0.0013(3) 0.0012(3) Cl1 0.0569(11) 0.0578(11) 0.0364(8) -0.0024(8) -0.0072(8) -0.0270(9) Cl2 0.0597(11) 0.0457(9) 0.0267(7) 0.0044(6) 0.0071(7) 0.0217(8) Cl3 0.0376(8) 0.0325(7) 0.0372(7) -0.0029(6) 0.0091(6) -0.0030(6) S1 0.0285(7) 0.0249(6) 0.0216(6) -0.0007(5) -0.0003(5) 0.0038(5) O1 0.063(4) 0.120(6) 0.093(5) 0.010(5) -0.027(4) -0.022(4) O2 0.107(5) 0.074(4) 0.046(3) -0.001(3) 0.037(3) -0.018(4) O3 0.092(5) 0.057(4) 0.076(4) -0.004(3) 0.030(4) -0.036(3) O4 0.129(7) 0.057(4) 0.185(9) 0.024(5) 0.101(6) 0.040(4) N1 0.031(3) 0.031(2) 0.026(2) 0.0077(19) 0.0033(19) -0.002(2) N2 0.034(3) 0.026(2) 0.029(2) -0.0022(19) -0.004(2) 0.002(2) N3 0.031(3) 0.030(2) 0.023(2) 0.0002(19) -0.0060(18) 0.001(2) N4 0.032(3) 0.030(2) 0.027(2) 0.0030(19) 0.0019(19) 0.003(2) N5 0.027(2) 0.032(2) 0.026(2) 0.0036(19) 0.0028(19) 0.002(2) C1 0.026(3) 0.044(3) 0.028(3) 0.000(2) 0.002(2) 0.007(3) C2 0.035(3) 0.048(4) 0.026(3) -0.004(3) 0.009(2) 0.007(3) C3 0.052(4) 0.021(3) 0.040(3) -0.006(2) -0.003(3) 0.003(3) C4 0.051(4) 0.030(3) 0.029(3) -0.008(2) -0.004(3) 0.009(3) C5 0.033(3) 0.042(3) 0.031(3) 0.000(3) -0.007(2) -0.006(3) C6 0.029(3) 0.035(3) 0.040(3) 0.001(3) 0.002(3) -0.005(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 Cl1 Cd1 Cl1 180.00(6) 3_656 Cl1 Cd1 Cl2 86.16(6) . Cl2 Cd1 Cl2 180.0 3_656 Cl1 Cd1 S1 85.75(5) . Cl2 Cd1 S1 85.77(4) . S1 Cd1 S1 180.00(3) 3_656 N3 Co1 N4 174.0(2) . N3 Co1 N1 92.5(2) . N4 Co1 N1 91.8(2) . N3 Co1 N5 90.5(2) . N4 Co1 N5 85.34(19) . N1 Co1 N5 175.9(2) . N3 Co1 N2 85.87(19) . N4 Co1 N2 90.13(19) . N1 Co1 N2 88.9(2) . N5 Co1 N2 94.1(2) . N3 Co1 S1 92.18(14) . N4 Co1 S1 92.10(14) . N1 Co1 S1 87.50(14) . N5 Co1 S1 89.67(14) . N2 Co1 S1 175.80(16) . O4 Cl3 O2 111.5(4) . O4 Cl3 O3 111.9(4) . O2 Cl3 O3 112.4(4) . O4 Cl3 O1 109.3(5) . O2 Cl3 O1 106.3(4) . O3 Cl3 O1 105.1(4) . C1 S1 Co1 96.5(2) . C1 S1 Cd1 104.16(19) . Co1 S1 Cd1 122.36(6) . C2 N1 Co1 115.4(4) . C3 N2 Co1 108.1(4) . C4 N3 Co1 109.5(3) . C5 N4 Co1 109.3(3) . C6 N5 Co1 108.0(3) . C2 C1 S1 107.9(4) . N1 C2 C1 108.2(5) . N2 C3 C4 108.2(5) . N3 C4 C3 107.9(5) . N4 C5 C6 107.7(5) . N5 C6 C5 106.6(5) . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cd1 Cl1 2.6243(17) Cd1 Cl2 2.6692(15) Cd1 S1 2.7160(13) Co1 N3 1.950(4) Co1 N4 1.972(5) Co1 N1 1.973(5) Co1 N5 1.983(5) Co1 N2 1.999(5) Co1 S1 2.2511(15) Cl3 O4 1.396(6) Cl3 O2 1.413(5) Cl3 O3 1.417(5) Cl3 O1 1.444(6) S1 C1 1.814(6) N1 C2 1.490(7) N2 C3 1.484(7) N3 C4 1.469(7) N4 C5 1.481(7) N5 C6 1.484(7) C1 C2 1.510(8) C3 C4 1.505(8) C5 C6 1.499(8) loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 Cl1 N1 3.216(5) 2_545 Cl2 N3 3.259(5) 3_656 Cl2 N5 3.359(5) 3_656 O1 N1 3.044(8) . O1 N3 3.283(9) . O2 N4 2.931(7) 4_666 O2 N3 3.279(8) . O4 N2 3.033(9) 1_655 O4 N5 3.042(8) 1_655