#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1004005.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_1004005 _audit_creation_method SHELXL-97 _chemical_name_systematic ; octakis(\m~3~-sulfido)-hexakis(tert-butylisocyanide)-hexa-tungsten tetrakis(benzene) solvate ; _chemical_name_common 'Tungsten Sulfide cluster' _chemical_melting_point 'not measured' _chemical_formula_moiety 'W6 S8 (C5H9N)6' _chemical_formula_sum 'C54 H78 N6 S8 W6' _chemical_formula_weight 2170.80 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ; octakis(\m~3~-sulfido)-hexakis(tert-butylisocyanide)-hexa-tungsten tetrakis(benzene) solvate ; _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _publ_author_name 'Jin, Song.' 'Zhou, Ran.' 'Scheuer, Ellen. M.' 'Adamchuk, Jennifer.' 'Rayburn, Lori. L.' 'DiSalvo, Francis. J.' _journal_name_full ; Inorganic Chemistry ; _journal_volume 40 _journal_year 2001 _journal_page_first 2666 _journal_page_last 2674 _cell_length_a 12.1751(6) _cell_length_b 12.5456(6) _cell_length_c 12.7678(6) _cell_angle_alpha 111.5324(11) _cell_angle_beta 110.3392(11) _cell_angle_gamma 93.1387(11) _cell_volume 1663.41(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ROD _exptl_crystal_colour RED _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'NOT MEASURED' _exptl_crystal_density_diffrn 2.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 10.619 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.3644 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; Absorption correction was done with SADABS beta Version. This program only gives ratios of max and min absorptions. ; _diffrn_ambient_temperature 173(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 18014 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 26.39 _reflns_number_total 6799 _reflns_number_gt 4978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'Bruker SAINT Plus' _computing_data_reduction SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0418P)^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 6799 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 0.94651(3) -0.07588(3) 0.32710(3) 0.01353(10) Uani 1 1 d . . . W2 W 0.93918(3) 0.13211(3) 0.48498(3) 0.01379(10) Uani 1 1 d . . . W3 W 1.14927(3) 0.06580(3) 0.51048(3) 0.01356(10) Uani 1 1 d . . . S1 S 1.0333(2) 0.1112(2) 0.3388(2) 0.0223(5) Uani 1 1 d . . . S2 S 0.7592(2) -0.0095(2) 0.3189(2) 0.0204(5) Uani 1 1 d . . . S3 S 0.8709(2) -0.2495(2) 0.3460(2) 0.0215(5) Uani 1 1 d . . . S4 S 1.1421(2) -0.1293(2) 0.3651(2) 0.0214(5) Uani 1 1 d . . . C11 C 0.8772(8) -0.1627(8) 0.1308(9) 0.021(2) Uani 1 1 d . . . N1 N 0.8319(7) -0.2104(7) 0.0244(7) 0.0249(19) Uani 1 1 d . . . C12 C 0.7663(9) -0.2639(9) -0.1071(9) 0.027(2) Uani 1 1 d . . . C13 C 0.8428(11) -0.2244(12) -0.1648(11) 0.053(4) Uani 1 1 d . . . H13A H 0.9168 -0.2543 -0.1474 0.079 Uiso 1 1 calc R . . H13B H 0.8627 -0.1386 -0.1302 0.079 Uiso 1 1 calc R . . H13C H 0.7979 -0.2551 -0.2537 0.079 Uiso 1 1 calc R . . C14 C 0.7422(10) -0.3950(9) -0.1485(10) 0.039(3) Uani 1 1 d . . . H14A H 0.6930 -0.4169 -0.1101 0.059 Uiso 1 1 calc R . . H14B H 0.8184 -0.4203 -0.1244 0.059 Uiso 1 1 calc R . . H14C H 0.6997 -0.4330 -0.2379 0.059 Uiso 1 1 calc R . . C15 C 0.6515(10) -0.2193(10) -0.1347(10) 0.046(3) Uani 1 1 d . . . H15A H 0.6027 -0.2453 -0.0981 0.069 Uiso 1 1 calc R . . H15B H 0.6069 -0.2502 -0.2236 0.069 Uiso 1 1 calc R . . H15C H 0.6703 -0.1335 -0.1001 0.069 Uiso 1 1 calc R . . C21 C 0.8689(8) 0.2779(8) 0.4548(8) 0.020(2) Uani 1 1 d . . . N2 N 0.8318(7) 0.3516(7) 0.4294(8) 0.027(2) Uani 1 1 d . . . C22 C 0.7892(8) 0.4351(9) 0.3792(9) 0.026(2) Uani 1 1 d . . . C23 C 0.8077(10) 0.5507(9) 0.4846(10) 0.035(3) Uani 1 1 d . . . H23A H 0.8936 0.5814 0.5344 0.053 Uiso 1 1 calc R . . H23B H 0.7677 0.5390 0.5353 0.053 Uiso 1 1 calc R . . H23C H 0.7738 0.6067 0.4523 0.053 Uiso 1 1 calc R . . C24 C 0.8564(10) 0.4444(10) 0.3028(11) 0.038(3) Uani 1 1 d . . . H24A H 0.9416 0.4767 0.3555 0.056 Uiso 1 1 calc R . . H24B H 0.8245 0.4961 0.2631 0.056 Uiso 1 1 calc R . . H24C H 0.8470 0.3664 0.2401 0.056 Uiso 1 1 calc R . . C25 C 0.6564(9) 0.3859(10) 0.2995(10) 0.037(3) Uani 1 1 d . . . H25A H 0.6462 0.3109 0.2321 0.056 Uiso 1 1 calc R . . H25B H 0.6225 0.4412 0.2661 0.056 Uiso 1 1 calc R . . H25C H 0.6151 0.3739 0.3492 0.056 Uiso 1 1 calc R . . C31 C 1.3189(8) 0.1460(8) 0.5240(8) 0.022(2) Uani 1 1 d . . . N3 N 1.4077(6) 0.1902(7) 0.5336(8) 0.0241(19) Uani 1 1 d . . . C32 C 1.5213(8) 0.2496(8) 0.5475(9) 0.024(2) Uani 1 1 d . . . C33 C 1.5592(9) 0.1671(9) 0.4538(10) 0.035(3) Uani 1 1 d . . . H33A H 1.5722 0.0974 0.4701 0.053 Uiso 1 1 calc R . . H33B H 1.6337 0.2061 0.4582 0.053 Uiso 1 1 calc R . . H33C H 1.4964 0.1440 0.3718 0.053 Uiso 1 1 calc R . . C34 C 1.6099(9) 0.2811(11) 0.6743(11) 0.043(3) Uani 1 1 d . . . H34A H 1.6236 0.2095 0.6866 0.065 Uiso 1 1 calc R . . H34B H 1.5791 0.3292 0.7333 0.065 Uiso 1 1 calc R . . H34C H 1.6856 0.3254 0.6867 0.065 Uiso 1 1 calc R . . C35 C 1.5009(10) 0.3594(10) 0.5278(10) 0.039(3) Uani 1 1 d . . . H35A H 1.4759 0.4108 0.5904 0.058 Uiso 1 1 calc R . . H35B H 1.4381 0.3387 0.4463 0.058 Uiso 1 1 calc R . . H35C H 1.5753 0.4001 0.5338 0.058 Uiso 1 1 calc R . . C1S C 1.8102(16) 0.0920(15) 0.9315(17) 0.089(5) Uiso 1 1 d . . . H1SA H 1.8802 0.0828 0.9148 0.107 Uiso 1 1 calc R . . C2S C 1.8089(17) 0.1075(15) 1.0384(17) 0.091(6) Uiso 1 1 d . . . H2SA H 1.8843 0.1208 1.1026 0.110 Uiso 1 1 calc R . . C3S C 1.7168(14) 0.1068(13) 1.0659(15) 0.076(5) Uiso 1 1 d . . . H3SA H 1.7242 0.1120 1.1442 0.091 Uiso 1 1 calc R . . C4S C 1.5963(14) 0.0975(13) 0.9699(14) 0.068(4) Uiso 1 1 d . . . H4SA H 1.5249 0.0972 0.9844 0.082 Uiso 1 1 calc R . . C5S C 1.5981(11) 0.0894(10) 0.8589(11) 0.044(3) Uiso 1 1 d . . . H5SA H 1.5269 0.0836 0.7933 0.053 Uiso 1 1 calc R . . C6S C 1.7057(13) 0.0900(12) 0.8473(14) 0.064(4) Uiso 1 1 d . . . H6SA H 1.7065 0.0889 0.7728 0.077 Uiso 1 1 calc R . . C7S C 1.0614(9) -0.3865(10) 0.0724(10) 0.035(3) Uiso 1 1 d . . . H7SA H 1.1040 -0.3078 0.1227 0.052 Uiso 1 1 calc R . . C8S C 0.9914(9) -0.4408(10) 0.1094(10) 0.036(3) Uiso 1 1 d . . . H8SA H 0.9854 -0.3996 0.1855 0.043 Uiso 1 1 calc R . . C9S C 0.9299(10) -0.5544(10) 0.0373(10) 0.036(3) Uiso 1 1 d . . . H9SA H 0.8815 -0.5919 0.0635 0.053 Uiso 1 1 calc R . . C10S C 0.5506(11) -0.3837(11) 0.0717(11) 0.047(3) Uiso 1 1 d . . . H10A H 0.5854 -0.3028 0.1209 0.071 Uiso 1 1 calc R . . C11S C 0.6228(11) -0.4650(10) 0.0601(11) 0.043(3) Uiso 1 1 d . . . H11A H 0.7074 -0.4406 0.1022 0.051 Uiso 1 1 calc R . . C12S C 0.5722(10) -0.5794(11) -0.0114(11) 0.043(3) Uiso 1 1 d . . . H12A H 0.6218 -0.6352 -0.0203 0.064 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 W1 0.01222(18) 0.0150(2) 0.01235(19) 0.00511(15) 0.00424(14) 0.00334(14) W2 0.01264(18) 0.0134(2) 0.01627(19) 0.00730(15) 0.00524(15) 0.00485(14) W3 0.00963(18) 0.0156(2) 0.01595(19) 0.00708(15) 0.00502(14) 0.00223(14) S1 0.0257(13) 0.0233(13) 0.0206(13) 0.0123(11) 0.0094(10) 0.0015(10) S2 0.0157(12) 0.0249(13) 0.0188(12) 0.0105(11) 0.0032(10) 0.0052(10) S3 0.0235(13) 0.0124(12) 0.0224(13) 0.0042(10) 0.0057(10) -0.0008(10) S4 0.0204(12) 0.0249(14) 0.0206(13) 0.0066(11) 0.0123(10) 0.0089(10) C11 0.024(5) 0.020(5) 0.019(5) 0.008(4) 0.008(4) 0.008(4) N1 0.022(4) 0.024(5) 0.022(5) 0.004(4) 0.007(4) 0.009(4) C12 0.026(5) 0.027(6) 0.014(5) -0.004(4) 0.006(4) 0.000(4) C13 0.054(8) 0.059(9) 0.028(7) 0.009(6) 0.008(6) 0.001(7) C14 0.044(7) 0.031(7) 0.023(6) -0.002(5) 0.005(5) 0.000(5) C15 0.041(7) 0.042(8) 0.030(7) 0.006(6) -0.004(5) 0.006(6) C21 0.022(5) 0.013(5) 0.022(5) 0.007(4) 0.007(4) -0.002(4) N2 0.020(4) 0.022(5) 0.045(6) 0.021(4) 0.012(4) 0.007(4) C22 0.021(5) 0.032(6) 0.035(6) 0.023(5) 0.012(5) 0.008(4) C23 0.038(6) 0.025(6) 0.053(7) 0.020(6) 0.023(6) 0.019(5) C24 0.038(6) 0.038(7) 0.047(7) 0.021(6) 0.025(6) 0.010(5) C25 0.033(6) 0.042(7) 0.039(7) 0.022(6) 0.011(5) 0.012(5) C31 0.023(5) 0.029(6) 0.018(5) 0.015(4) 0.006(4) 0.004(4) N3 0.007(4) 0.029(5) 0.036(5) 0.014(4) 0.008(4) 0.000(3) C32 0.011(5) 0.023(5) 0.035(6) 0.013(5) 0.005(4) -0.002(4) C33 0.028(6) 0.033(7) 0.043(7) 0.014(6) 0.012(5) 0.011(5) C34 0.028(6) 0.051(8) 0.046(7) 0.023(6) 0.007(5) 0.002(6) C35 0.039(7) 0.048(8) 0.032(6) 0.018(6) 0.015(5) 0.010(6) _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.277 _refine_diff_density_min -2.039 _refine_diff_density_rms 0.256 _cod_database_code 1004005