#------------------------------------------------------------------------------
#$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $
#$Revision: 853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1004007.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_tbu

_audit_creation_method            SHELXL
_chemical_name_systematic
;
octakis(\mu~3~-sulfido)-hexakis(tert-butylamine)-hexa-tungsten
tert-butylamine solvate
;
_chemical_name_common             'Tungsten Sulfide cluster'
_chemical_formula_moiety          'W6 S8 (C4H11N)6 (C4H11N)'
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C32 H88 N8 S8 W6'
_chemical_formula_weight          1944.68
_chemical_melting_point           'not measured'
_chemical_compound_source         ?

_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  C2/c
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            monoclinic

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'
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                    23.1036(4)
_cell_length_b                    20.8216(3)
_cell_length_c                    11.497
_cell_angle_alpha                 90.00
_cell_angle_beta                  99.7030(10)
_cell_angle_gamma                 90.00
_cell_volume                      5451.46(12)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(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           0.2
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       'NOT MEASURED'
_exptl_crystal_density_diffrn     2.369
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              3632
_exptl_absorpt_coefficient_mu     12.946
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_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        ?
_diffrn_measurement_method        '\w scans'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             15950
_diffrn_reflns_av_R_equivalents   0.0495
_diffrn_reflns_av_sigmaI/netI     0.0591
_diffrn_reflns_limit_h_min        -29
_diffrn_reflns_limit_h_max        27
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          1.33
_diffrn_reflns_theta_max          28.19
_reflns_number_total              5964
_reflns_number_observed           4914
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'BRUKER SMART'
_computing_cell_refinement        'Bruker SAINT Plus'
_computing_data_reduction         SHELXTL
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     SHELXTL
_computing_publication_material   SHELXTL

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
 or flagged by the user for potential systematic errors.  Weighted R-factors
 wR and all goodnesses 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 observed criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0398P)^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          5964
_refine_ls_number_parameters      248
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0465
_refine_ls_R_factor_obs           0.0325
_refine_ls_wR_factor_all          0.0905
_refine_ls_wR_factor_obs          0.0747
_refine_ls_goodness_of_fit_all    1.061
_refine_ls_goodness_of_fit_obs    0.969
_refine_ls_restrained_S_all       1.061
_refine_ls_restrained_S_obs       0.969
_refine_ls_shift/esd_max          -1.915
_refine_ls_shift/esd_mean         0.039

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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
W1 W 0.292491(12) 0.185523(14) 0.93661(3) 0.00931(9) Uani 1 d . .
W2 W 0.196316(12) 0.187726(14) 1.03591(3) 0.00904(9) Uani 1 d . .
W3 W 0.296207(12) 0.237499(14) 1.14942(3) 0.00937(9) Uani 1 d . .
S1 S 0.28309(8) 0.12126(9) 1.1128(2) 0.0140(4) Uani 1 d . .
S2 S 0.19639(8) 0.14488(9) 0.8363(2) 0.0129(4) Uani 1 d . .
S3 S 0.20317(8) 0.24043(9) 1.2294(2) 0.0136(4) Uani 1 d . .
S4 S 0.38082(8) 0.23539(9) 1.0475(2) 0.0133(4) Uani 1 d . .
N1 N 0.3347(3) 0.1055(3) 0.8395(6) 0.019(2) Uani 1 d . .
H1A H 0.3157(15) 0.0783(21) 0.8410(6) 0.023 Uiso 1 calc R .
H1B H 0.3301(5) 0.1158(8) 0.7790(46) 0.023 Uiso 1 calc R .
N2 N 0.1397(3) 0.1075(3) 1.0948(6) 0.0145(14) Uani 1 d . .
H2A H 0.1523(9) 0.0749(22) 1.0714(16) 0.017 Uiso 1 calc R .
H2B H 0.1484(6) 0.1065(3) 1.1654(46) 0.017 Uiso 1 calc R .
N3 N 0.3436(3) 0.2232(3) 1.3408(6) 0.020(2) Uani 1 d . .
H3A H 0.3340(8) 0.2501(20) 1.3731(26) 0.024 Uiso 1 calc R .
H3B H 0.3299(11) 0.1949(22) 1.3613(17) 0.024 Uiso 1 calc R .
C1 C 0.3953(3) 0.0773(4) 0.8595(7) 0.022(2) Uani 1 d . .
C2 C 0.4379(4) 0.1306(5) 0.8450(9) 0.039(3) Uani 1 d . .
H2B H 0.4293(4) 0.1473(5) 0.7642(9) 0.058 Uiso 1 calc R .
H2C H 0.4781(4) 0.1138(5) 0.8604(9) 0.058 Uiso 1 calc R .
H2D H 0.4340(4) 0.1652(5) 0.9009(9) 0.058 Uiso 1 calc R .
C3 C 0.3988(4) 0.0259(5) 0.7655(9) 0.037(2) Uani 1 d . .
H3B H 0.3902(4) 0.0454(5) 0.6869(9) 0.055 Uiso 1 calc R .
H3C H 0.3700(4) -0.0080(5) 0.7718(9) 0.055 Uiso 1 calc R .
H3D H 0.4383(4) 0.0073(5) 0.7776(9) 0.055 Uiso 1 calc R .
C4 C 0.4082(5) 0.0506(5) 0.9839(9) 0.048(3) Uani 1 d . .
H4A H 0.3802(5) 0.0162(5) 0.9922(9) 0.072 Uiso 1 calc R .
H4B H 0.4044(5) 0.0849(5) 1.0405(9) 0.072 Uiso 1 calc R .
H4C H 0.4482(5) 0.0335(5) 0.9993(9) 0.072 Uiso 1 calc R .
C5 C 0.0743(3) 0.0999(4) 1.0704(7) 0.017(2) Uani 1 d . .
C6 C 0.0552(4) 0.0982(4) 0.9366(8) 0.026(2) Uani 1 d . .
H6A H 0.0735(4) 0.0613(4) 0.9040(8) 0.038 Uiso 1 calc R .
H6B H 0.0674(4) 0.1379(4) 0.9021(8) 0.038 Uiso 1 calc R .
H6C H 0.0124(4) 0.0941(4) 0.9178(8) 0.038 Uiso 1 calc R .
C7 C 0.0570(4) 0.0372(4) 1.1258(8) 0.026(2) Uani 1 d . .
H7A H 0.0695(4) 0.0389(4) 1.2115(8) 0.038 Uiso 1 calc R .
H7B H 0.0762(4) 0.0009(4) 1.0935(8) 0.038 Uiso 1 calc R .
H7C H 0.0143(4) 0.0317(4) 1.1076(8) 0.038 Uiso 1 calc R .
C8 C 0.0469(4) 0.1567(4) 1.1258(8) 0.027(2) Uani 1 d . .
H8A H 0.0600(4) 0.1564(4) 1.2114(8) 0.041 Uiso 1 calc R .
H8B H 0.0040(4) 0.1531(4) 1.1086(8) 0.041 Uiso 1 calc R .
H8C H 0.0590(4) 0.1969(4) 1.0927(8) 0.041 Uiso 1 calc R .
C9 C 0.4076(3) 0.2160(4) 1.3897(7) 0.019(2) Uani 1 d . .
C10 C 0.4407(4) 0.2725(5) 1.3531(8) 0.028(2) Uani 1 d . .
H10A H 0.4352(4) 0.2746(5) 1.2667(8) 0.042 Uiso 1 calc R .
H10B H 0.4826(4) 0.2677(5) 1.3849(8) 0.042 Uiso 1 calc R .
H10C H 0.4259(4) 0.3121(5) 1.3837(8) 0.042 Uiso 1 calc R .
C11 C 0.4286(4) 0.1539(5) 1.3394(9) 0.040(3) Uani 1 d . .
H11A H 0.4067(4) 0.1175(5) 1.3639(9) 0.061 Uiso 1 calc R .
H11B H 0.4706(4) 0.1481(5) 1.3690(9) 0.061 Uiso 1 calc R .
H11C H 0.4221(4) 0.1564(5) 1.2531(9) 0.061 Uiso 1 calc R .
C12 C 0.4154(4) 0.2117(5) 1.5245(8) 0.031(2) Uani 1 d . .
H12A H 0.3934(4) 0.1747(5) 1.5468(8) 0.046 Uiso 1 calc R .
H12B H 0.4006(4) 0.2511(5) 1.5558(8) 0.046 Uiso 1 calc R .
H12C H 0.4571(4) 0.2064(5) 1.5571(8) 0.046 Uiso 1 calc R .
N1S N 0.2051(3) -0.0259(4) 1.0874(8) 0.028(2) Uani 1 d D .
H1SA H 0.2331(33) -0.0066(44) 1.1027(87) 0.033 Uiso 1 d D .
H1SB H 0.1889(38) -0.0412(45) 1.1463(72) 0.033 Uiso 1 d D .
C1S C 0.2079(4) -0.0726(4) 0.9920(7) 0.022(2) Uani 1 d . .
C2S C 0.1477(4) -0.1021(4) 0.9568(9) 0.034(2) Uani 1 d . .
H2SA H 0.1364(4) -0.1242(4) 1.0248(9) 0.051 Uiso 1 calc R .
H2SB H 0.1485(4) -0.1330(4) 0.8928(9) 0.051 Uiso 1 calc R .
H2SC H 0.1191(4) -0.0683(4) 0.9298(9) 0.051 Uiso 1 calc R .
C3S C 0.2526(4) -0.1254(5) 1.0320(9) 0.039(3) Uani 1 d . .
H3SA H 0.2917(4) -0.1063(5) 1.0546(9) 0.058 Uiso 1 calc R .
H3SB H 0.2533(4) -0.1559(5) 0.9672(9) 0.058 Uiso 1 calc R .
H3SC H 0.2417(4) -0.1480(5) 1.0998(9) 0.058 Uiso 1 calc R .
C4S C 0.2274(4) -0.0375(5) 0.8903(9) 0.043(3) Uiso 1 d . .
H4SA H 0.2664(4) -0.0189(5) 0.9163(9) 0.064 Uiso 1 calc R .
H4SB H 0.1994(4) -0.0031(5) 0.8631(9) 0.064 Uiso 1 calc R .
H4SC H 0.2290(4) -0.0676(5) 0.8254(9) 0.064 Uiso 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 0.00766(15) 0.0094(2) 0.0116(2) 0.00001(11) 0.00384(12) -0.00098(11)
W2 0.00700(15) 0.0094(2) 0.0115(2) 0.00034(11) 0.00390(12) -0.00250(11)
W3 0.00729(15) 0.01067(15) 0.0105(2) 0.00099(12) 0.00258(11) -0.00159(11)
S1 0.0127(9) 0.0122(9) 0.0176(10) 0.0019(8) 0.0036(8) -0.0006(7)
S2 0.0118(9) 0.0123(9) 0.0148(10) -0.0012(8) 0.0029(7) -0.0035(7)
S3 0.0148(9) 0.0152(9) 0.0118(10) 0.0006(7) 0.0048(7) -0.0018(7)
S4 0.0070(9) 0.0159(9) 0.0177(10) 0.0001(8) 0.0041(7) -0.0014(7)
N1 0.021(4) 0.019(4) 0.018(4) -0.008(3) 0.007(3) 0.000(3)
N2 0.012(3) 0.016(3) 0.018(4) 0.000(3) 0.011(3) -0.007(3)
N3 0.021(4) 0.025(4) 0.015(4) 0.009(3) 0.003(3) -0.006(3)
C1 0.020(4) 0.028(5) 0.019(5) 0.000(4) 0.008(4) 0.007(4)
C2 0.026(5) 0.045(6) 0.051(7) -0.022(5) 0.025(5) -0.009(4)
C3 0.035(6) 0.030(6) 0.047(7) -0.014(5) 0.013(5) 0.007(4)
C4 0.047(7) 0.055(7) 0.047(7) 0.017(6) 0.022(6) 0.028(5)
C5 0.010(4) 0.019(4) 0.023(5) 0.001(3) 0.008(3) -0.003(3)
C6 0.021(4) 0.022(5) 0.032(5) 0.003(4) 0.001(4) -0.011(4)
C7 0.026(5) 0.022(5) 0.031(5) 0.006(4) 0.011(4) -0.012(4)
C8 0.022(5) 0.027(5) 0.036(6) 0.002(4) 0.016(4) -0.002(4)
C9 0.011(4) 0.025(5) 0.021(5) 0.002(4) 0.000(3) 0.007(3)
C10 0.013(4) 0.045(6) 0.025(5) -0.007(4) 0.004(4) -0.011(4)
C11 0.050(6) 0.029(6) 0.039(6) 0.001(5) -0.002(5) 0.020(5)
C12 0.027(5) 0.045(6) 0.019(5) 0.007(4) -0.004(4) -0.002(4)
N1S 0.030(5) 0.023(4) 0.032(5) -0.006(4) 0.011(4) -0.002(3)
C1S 0.033(5) 0.019(4) 0.015(4) 0.005(3) 0.005(4) -0.001(4)
C2S 0.034(5) 0.033(6) 0.034(6) -0.011(5) 0.006(4) -0.008(4)
C3S 0.038(6) 0.045(7) 0.032(6) -0.006(5) 0.004(5) 0.021(5)


_refine_diff_density_max    1.354
_refine_diff_density_min   -3.972
_refine_diff_density_rms    0.542