#------------------------------------------------------------------------------
#$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