#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000189.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_4000189 _journal_name_full 'Chemistry of Materials' _journal_year 2002 _chemical_name_systematic ; tri iron(II) octakis(mu!3$-sulfido)-hexakis(cyanide) -hexa-tungsten- 24.6(water)solvate ; _chemical_name_common 'linked tugsten sulfido cyanide cluster' _chemical_formula_moiety [Fe(H2O)4]3[W6S8(CN)6](H2O)24.5 _chemical_formula_sum 'C6 H0 Fe3 N6 O36.50 S8 W6' _chemical_formula_weight 2267.25 _symmetry_cell_setting Monoclinic _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.6008(15) _cell_length_b 21.968(2) _cell_length_c 18.286(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.940(6) _cell_angle_gamma 90.00 _cell_volume 5843.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 165(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'brown red' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'NOT MEASURED' _exptl_crystal_density_diffrn 2.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 12.848 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.693193 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 165(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15533 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 20.81 _reflns_number_total 3027 _reflns_number_gt 2375 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3027 _refine_ls_number_parameters 248 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.002 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 _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.25577(5) 0.29357(3) 0.08969(4) 0.0135(2) Uani 1 1 d . . . W2 W 0.25709(5) 0.17560(3) 0.05241(4) 0.0123(2) Uani 1 1 d . . . W3 W 0.12038(5) 0.24778(3) -0.00214(4) 0.0144(2) Uani 1 1 d . . . S4 S 0.1437(3) 0.2198(2) 0.1286(3) 0.0258(13) Uani 1 1 d . . . S5 S 0.3809(3) 0.2231(2) 0.1325(3) 0.0274(13) Uani 1 1 d . . . S6 S 0.1295(3) 0.3554(2) 0.0319(3) 0.0266(13) Uani 1 1 d . . . S7 S 0.3678(3) 0.35977(19) 0.0352(3) 0.0224(12) Uani 1 1 d . . . Fe1 Fe 0.25527(19) -0.04006(11) 0.19598(15) 0.0242(7) Uani 1 1 d . . . Fe2 Fe -0.2500 0.2500 0.0000 0.0525(15) Uani 1 2 d S . . O11 O 0.3293(9) -0.0911(5) 0.1182(7) 0.043(4) Uani 1 1 d . . . O12 O 0.3809(10) -0.0185(6) 0.2559(8) 0.057(4) Uani 1 1 d . . . O13 O 0.1251(10) -0.0566(6) 0.1318(7) 0.053(4) Uani 1 1 d . . . O14 O 0.1855(9) 0.0124(5) 0.2765(7) 0.043(4) Uani 1 1 d . . . O21 O -0.2492(10) 0.1603(6) 0.0451(10) 0.077(6) Uani 1 1 d . . . O22 O -0.2250(9) 0.2858(5) 0.1118(8) 0.053(4) Uani 1 1 d . . . C1 C 0.2600(11) 0.3494(7) 0.1885(9) 0.013(4) Uiso 1 1 d . . . N1 N 0.2399(10) -0.1178(6) 0.2621(8) 0.027(4) Uiso 1 1 d . . . C2 C 0.2625(12) 0.0886(8) 0.1078(9) 0.021(5) Uiso 1 1 d . . . N2 N 0.2684(11) 0.0419(7) 0.1356(8) 0.034(4) Uiso 1 1 d . . . C3 C -0.0277(15) 0.2445(9) -0.0047(11) 0.039(6) Uiso 1 1 d . . . N3 N -0.1072(13) 0.2444(8) -0.0055(10) 0.054(5) Uiso 1 1 d . . . O1S O 0.2419(9) -0.0149(6) 0.4197(7) 0.050(4) Uiso 1 1 d . . . O2S O 0.0206(10) -0.1479(6) 0.1779(8) 0.057(4) Uiso 1 1 d . . . O3S O 0.1321(10) -0.0688(7) -0.0197(8) 0.065(5) Uiso 1 1 d . . . O4S O 0.3703(10) 0.2518(6) 0.3118(8) 0.058(4) Uiso 1 1 d . . . O5S O -0.3962(16) 0.0339(10) 0.0000(13) 0.143(9) Uiso 1 1 d . . . O6S O 0.0338(14) 0.0666(9) 0.1122(10) 0.051(8) Uiso 0.73(3) 1 d P . . O6T O -0.019(4) 0.115(3) 0.102(3) 0.07(3) Uiso 0.27(3) 1 d P . . O7S O -0.204(3) 0.1338(10) 0.2230(17) 0.055(10) Uiso 0.74(11) 1 d P . . O7T O -0.242(6) 0.138(2) 0.238(3) 0.01(3) Uiso 0.26(11) 1 d P . . O8S O 0.4774(16) -0.1136(13) 0.3249(13) 0.058(10) Uiso 0.65(4) 1 d P . . O8T O 0.488(2) -0.0720(19) 0.355(2) 0.030(16) Uiso 0.35(4) 1 d P . . O9S O 0.5000 0.0754(17) 0.2500 0.075(17) Uiso 0.60(4) 2 d SP . . O9T O 0.572(3) 0.1009(17) 0.219(2) 0.07(2) Uiso 0.40(4) 1 d P . . O10S O -0.0912(15) 0.2176(10) 0.1718(12) 0.086(10) Uiso 0.79(3) 1 d P . . O10T O -0.044(4) 0.279(3) 0.192(3) 0.04(3) Uiso 0.21(3) 1 d P . . O10U O 0.0000 0.2970(19) 0.2500 0.140(16) Uiso 0.79(3) 2 d SP . . O11S O -0.5083(19) 0.0653(12) 0.0885(15) 0.030(11) Uiso 0.42(3) 1 d P . . O13S O -0.370(4) 0.140(2) 0.138(3) 0.099(18) Uiso 0.42(3) 1 d P . . O12S O -0.432(4) 0.120(2) 0.072(4) 0.06(3) Uiso 0.29(6) 1 d P . . O12T O -0.453(5) 0.135(3) 0.121(4) 0.07(3) Uiso 0.29(6) 1 d P . . O14S O 0.0000 0.113(3) 0.2500 0.19(4) Uiso 0.61(7) 2 d SP . . O15S O 0.0000 0.008(3) 0.2500 0.34(5) Uiso 0.98(10) 2 d SP . . 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 W1 0.0138(5) 0.0099(4) 0.0168(4) -0.0011(4) 0.0022(3) 0.0000(4) W2 0.0105(5) 0.0083(4) 0.0182(4) 0.0015(4) 0.0016(3) 0.0006(4) W3 0.0058(5) 0.0130(4) 0.0248(5) 0.0022(4) 0.0032(3) 0.0006(4) S4 0.025(3) 0.027(3) 0.028(3) 0.003(3) 0.016(2) -0.001(2) S5 0.030(4) 0.026(3) 0.024(3) 0.006(2) -0.011(2) -0.005(3) S6 0.025(3) 0.018(3) 0.039(3) -0.004(3) 0.015(3) 0.007(2) S7 0.017(3) 0.015(3) 0.034(3) 0.000(2) -0.005(2) -0.007(2) Fe1 0.0289(19) 0.0137(14) 0.0286(17) 0.0072(13) -0.0054(13) -0.0014(13) Fe2 0.012(3) 0.015(2) 0.134(5) -0.007(3) 0.022(3) -0.001(2) O11 0.050(11) 0.031(8) 0.048(9) 0.004(7) 0.009(8) 0.002(7) O12 0.048(11) 0.051(10) 0.067(11) 0.005(8) -0.025(8) -0.003(8) O13 0.059(11) 0.051(10) 0.046(10) 0.017(8) -0.017(8) -0.025(8) O14 0.044(10) 0.039(8) 0.048(9) 0.009(8) 0.015(8) 0.016(7) O21 0.047(11) 0.023(8) 0.164(18) 0.007(10) 0.024(11) -0.025(8) O22 0.029(10) 0.024(8) 0.108(13) -0.019(9) 0.008(9) -0.003(7)