#------------------------------------------------------------------------------
#$Date: 2009-11-21 12:50:34 +0200 (Sat, 21 Nov 2009) $
#$Revision: 900 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1004004.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_1004004

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
octakis(mu!3$-sulfido)-hexakis(morpholine)
-hexa-tungsten-1.3(morpholine)-3.7(aniline)
;
_chemical_name_common             'Tungsten sulfide cluster with'
_chemical_melting_point           ?
_chemical_formula_moiety          W6S8(C4NOH9)6(C5.2N1.3O1.3H11.7)(C22.2H25.9N3
_chemical_formula_sum            'C51.5 H91.5 N11 O7.25 S8 W6'
_[local]_cod_chemical_formula_sum_orig 'C51.50 H91.50 N11 O7.25 S8 W6'
_chemical_formula_weight          2340.44

_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'
 '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'
 '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                    14.8105(13)
_cell_length_b                    18.5419(17)
_cell_length_c                    25.108(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  104.284(2)
_cell_angle_gamma                 90.00
_cell_volume                      6681.8(10)
_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             dark-red
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       'NOT MEASURED'
_exptl_crystal_density_diffrn     2.327
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              4430
_exptl_absorpt_coefficient_mu     10.593
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.618779
_exptl_absorpt_correction_T_max   1
_exptl_absorpt_process_details    ?

_exptl_special_details
;
octakis(mu!3$-sulfido)-hexakis(morpholine)
-hexa-tungsten-1.3(morpholine)-3.7(aniline)
;

_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             40292
_diffrn_reflns_av_R_equivalents   0.0396
_diffrn_reflns_av_sigmaI/netI     0.0307
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -24
_diffrn_reflns_limit_k_max        24
_diffrn_reflns_limit_l_min        -33
_diffrn_reflns_limit_l_max        33
_diffrn_reflns_theta_min          1.83
_diffrn_reflns_theta_max          28.28
_reflns_number_total              8242
_reflns_number_gt                 7195
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'BRUKER SMART'
_computing_cell_refinement        'Bruker SAINT'
_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^)+(0.0267P)^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          8242
_refine_ls_number_parameters      378
_refine_ls_number_restraints      3
_refine_ls_R_factor_all           0.0389
_refine_ls_R_factor_gt            0.0304
_refine_ls_wR_factor_ref          0.0613
_refine_ls_wR_factor_gt           0.0595
_refine_ls_goodness_of_fit_ref    1.216
_refine_ls_restrained_S_all       1.217
_refine_ls_shift/su_max           0.112
_refine_ls_shift/su_mean          0.003

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 0.533581(13) 0.089461(9) -0.024711(7) 0.01360(5) Uani 1 1 d . . .
W2 W 0.569488(13) -0.048009(9) -0.042656(7) 0.01397(5) Uani 1 1 d . . .
W3 W 0.393746(13) -0.002500(9) -0.059553(7) 0.01391(5) Uani 1 1 d . . .
S4 S 0.69323(8) 0.04062(6) -0.00687(5) 0.0178(2) Uani 1 1 d . . .
S5 S 0.49794(8) 0.03536(6) -0.11713(4) 0.0172(2) Uani 1 1 d . . .
S6 S 0.36929(9) 0.12401(6) -0.03795(5) 0.0190(2) Uani 1 1 d . . .
S7 S 0.56496(9) 0.12921(6) 0.07129(4) 0.0186(2) Uani 1 1 d . . .
N1 N 0.5740(3) 0.1968(2) -0.05888(16) 0.0197(9) Uani 1 1 d . . .
H1Z H 0.614(3) 0.1878(7) -0.0707(8) 0.024 Uiso 1 1 calc R . .
C11 C 0.5024(4) 0.2279(3) -0.1049(2) 0.0313(12) Uani 1 1 d . . .
H11A H 0.4467 0.2405 -0.0917 0.038 Uiso 1 1 calc R . .
H11B H 0.4836 0.1911 -0.1341 0.038 Uiso 1 1 calc R . .
C12 C 0.5362(4) 0.2948(3) -0.1292(2) 0.0320(13) Uani 1 1 d . . .
H12A H 0.5880 0.2815 -0.1458 0.038 Uiso 1 1 calc R . .
H12B H 0.4848 0.3144 -0.1587 0.038 Uiso 1 1 calc R . .
C13 C 0.6410(6) 0.3184(3) -0.0464(3) 0.064(2) Uani 1 1 d . . .
H13A H 0.6648 0.3559 -0.0185 0.077 Uiso 1 1 calc R . .
H13B H 0.6929 0.3034 -0.0625 0.077 Uiso 1 1 calc R . .
C14 C 0.6082(5) 0.2545(3) -0.0194(2) 0.0422(16) Uani 1 1 d . . .
H14A H 0.6604 0.2360 0.0101 0.051 Uiso 1 1 calc R . .
H14B H 0.5578 0.2698 -0.0023 0.051 Uiso 1 1 calc R . .
O1 O 0.5668(3) 0.34795(19) -0.08898(17) 0.0454(11) Uani 1 1 d . . .
N2 N 0.6476(3) -0.1068(2) -0.09875(16) 0.0210(9) Uani 1 1 d . . .
H2Z H 0.612(3) -0.1166(8) -0.1221(17) 0.025 Uiso 1 1 calc R . .
C21 C 0.7121(4) -0.0624(3) -0.1222(2) 0.0324(13) Uani 1 1 d . . .
H21A H 0.7646 -0.0457 -0.0921 0.039 Uiso 1 1 calc R . .
H21B H 0.6786 -0.0193 -0.1403 0.039 Uiso 1 1 calc R . .
C22 C 0.7499(5) -0.1048(3) -0.1637(3) 0.0441(16) Uani 1 1 d . . .
H22A H 0.6979 -0.1181 -0.1952 0.053 Uiso 1 1 calc R . .
H22B H 0.7939 -0.0743 -0.1776 0.053 Uiso 1 1 calc R . .
C23 C 0.7320(4) -0.2137(3) -0.1217(2) 0.0344(13) Uani 1 1 d . . .
H23A H 0.7640 -0.2583 -0.1055 0.041 Uiso 1 1 calc R . .
H23B H 0.6809 -0.2274 -0.1536 0.041 Uiso 1 1 calc R . .
C24 C 0.6917(4) -0.1753(3) -0.0792(2) 0.0332(13) Uani 1 1 d . . .
H24A H 0.6451 -0.2071 -0.0688 0.040 Uiso 1 1 calc R . .
H24B H 0.7422 -0.1665 -0.0458 0.040 Uiso 1 1 calc R . .
O2 O 0.7962(3) -0.1683(2) -0.13948(16) 0.0379(10) Uani 1 1 d . . .
N3 N 0.2604(3) 0.0016(2) -0.13059(16) 0.0223(9) Uani 1 1 d . . .
H3Z H 0.222(3) 0.0121(8) -0.1177(10) 0.027 Uiso 1 1 calc R . .
C31 C 0.2613(4) 0.0573(3) -0.1728(2) 0.0317(13) Uani 1 1 d . . .
H31A H 0.3126 0.0466 -0.1905 0.038 Uiso 1 1 calc R . .
H31B H 0.2742 0.1048 -0.1546 0.038 Uiso 1 1 calc R . .
C32 C 0.1711(4) 0.0617(3) -0.2165(2) 0.0392(14) Uani 1 1 d . . .
H32A H 0.1206 0.0775 -0.1996 0.047 Uiso 1 1 calc R . .
H32B H 0.1771 0.0980 -0.2443 0.047 Uiso 1 1 calc R . .
C33 C 0.1405(4) -0.0594(3) -0.2033(2) 0.0402(15) Uani 1 1 d . . .
H33A H 0.1244 -0.1061 -0.2224 0.048 Uiso 1 1 calc R . .
H33B H 0.0898 -0.0465 -0.1857 0.048 Uiso 1 1 calc R . .
C34 C 0.2300(4) -0.0674(3) -0.1599(2) 0.0317(13) Uani 1 1 d . . .
H34A H 0.2217 -0.1042 -0.1329 0.038 Uiso 1 1 calc R . .
H34B H 0.2793 -0.0846 -0.1771 0.038 Uiso 1 1 calc R . .
O3 O 0.1477(3) -0.0056(2) -0.24229(15) 0.0399(10) Uani 1 1 d . . .
N1S N 0.7491(3) 0.3507(3) 0.10068(17) 0.0366(12) Uani 1 1 d . . .
H1SA H 0.7789 0.3865 0.0896 0.044 Uiso 1 1 calc R . .
H1SB H 0.7032 0.3290 0.0773 0.044 Uiso 1 1 calc R . .
C11S C 0.7746(4) 0.3286(3) 0.1551(2) 0.0252(11) Uani 1 1 d . . .
C12S C 0.7330(4) 0.2687(3) 0.1722(2) 0.0271(11) Uani 1 1 d . . .
H12C H 0.6852 0.2438 0.1466 0.033 Uiso 1 1 calc R . .
C13S C 0.7603(4) 0.2451(3) 0.2254(2) 0.0293(12) Uani 1 1 d . . .
H13C H 0.7301 0.2047 0.2366 0.035 Uiso 1 1 calc R . .
C14S C 0.8311(4) 0.2792(3) 0.2628(2) 0.0297(12) Uani 1 1 d . . .
H14C H 0.8500 0.2626 0.2997 0.036 Uiso 1 1 calc R . .
C15S C 0.8741(4) 0.3380(3) 0.2461(2) 0.0326(13) Uani 1 1 d . . .
H15A H 0.9229 0.3619 0.2716 0.039 Uiso 1 1 calc R . .
C16S C 0.8468(4) 0.3622(3) 0.1926(2) 0.0299(12) Uani 1 1 d . . .
H16A H 0.8777 0.4022 0.1814 0.036 Uiso 1 1 calc R . .
N2S N 0.5000 -0.0238(4) -0.2500 0.060(3) Uani 1 2 d S . .
H2SA H 0.4811 0.0000 -0.2244 0.073 Uiso 0.50 1 calc PR . .
H2SB H 0.5189 0.0000 -0.2756 0.073 Uiso 0.50 1 calc PR . .
C21S C 0.5000 -0.0964(5) -0.2500 0.0313(18) Uani 1 2 d S . .
C22S C 0.4705(4) -0.1350(3) -0.2098(2) 0.0328(13) Uani 1 1 d . . .
H22C H 0.4492 -0.1099 -0.1823 0.039 Uiso 1 1 calc R . .
C23S C 0.4719(4) -0.2084(4) -0.2098(2) 0.0424(15) Uani 1 1 d . . .
H23C H 0.4531 -0.2340 -0.1816 0.051 Uiso 1 1 calc R . .
C24S C 0.5000 -0.2458(5) -0.2500 0.050(2) Uani 1 2 d S . .
H24C H 0.5000 -0.2971 -0.2500 0.060 Uiso 1 2 calc SR . .
O3S O 0.0815(6) 0.0194(4) -0.0791(4) 0.062(3) Uiso 0.646(11) 1 d PD A 1
N3S N -0.0359(6) 0.1388(5) -0.0911(3) 0.045(2) Uiso 0.646(11) 1 d PD A 1
H3SA H -0.0805 0.1628 -0.0814 0.054 Uiso 0.646(11) 1 calc PR A 1
C31S C 0.1040(13) 0.0771(8) -0.0392(7) 0.051(4) Uiso 0.646(11) 1 d PD A 1
H31C H 0.1724 0.0812 -0.0250 0.062 Uiso 0.646(11) 1 calc PR A 1
H31D H 0.0763 0.0673 -0.0078 0.062 Uiso 0.646(11) 1 calc PR A 1
C32S C 0.0638(10) 0.1482(8) -0.0683(7) 0.079(5) Uiso 0.646(11) 1 d PD A 1
H32C H 0.0750 0.1885 -0.0416 0.095 Uiso 0.646(11) 1 calc PR A 1
H32D H 0.0947 0.1597 -0.0979 0.095 Uiso 0.646(11) 1 calc PR A 1
C33S C -0.0485(9) 0.0852(7) -0.1311(5) 0.059(3) Uiso 0.646(11) 1 d PD A 1
H33C H -0.0135 0.0975 -0.1588 0.070 Uiso 0.646(11) 1 calc PR A 1
H33C H -0.1153 0.0811 -0.1501 0.070 Uiso 0.646(11) 1 calc PR A 1
C34S C -0.0143(10) 0.0160(8) -0.1042(7) 0.060(4) Uiso 0.646(11) 1 d PD A 1
H34C H -0.0489 0.0046 -0.0762 0.072 Uiso 0.646(11) 1 calc PR A 1
H34D H -0.0262 -0.0231 -0.1319 0.072 Uiso 0.646(11) 1 calc PR A 1
N3T N -0.0558(14) -0.0167(10) -0.1334(8) 0.067(6) Uiso 0.354(11) 1 d P A 2
H3TA H -0.1012 -0.0121 -0.1633 0.080 Uiso 0.354(11) 1 calc PR A 2
H3TB H -0.0390 -0.0598 -0.1198 0.080 Uiso 0.354(11) 1 calc PR A 2
C31T C -0.0134(15) 0.0403(12) -0.1092(9) 0.038(5) Uiso 0.354(11) 1 d P A 2
C32T C 0.0522(19) 0.0279(15) -0.0517(12) 0.076(8) Uiso 0.354(11) 1 d P A 2
H32E H 0.0610 -0.0187 -0.0356 0.091 Uiso 0.354(11) 1 calc PR A 2
C33T C 0.092(3) 0.080(2) -0.0282(18) 0.096(14) Uiso 0.354(11) 1 d P A 2
H33D H 0.1392 0.0710 0.0042 0.115 Uiso 0.354(11) 1 calc PR A 2
C34T C 0.0763(16) 0.1496(13) -0.0425(10) 0.052(6) Uiso 0.354(11) 1 d P A 2
H34E H 0.1089 0.1871 -0.0200 0.063 Uiso 0.354(11) 1 calc PR A 2
C35T C 0.0138(15) 0.1645(11) -0.0896(7) 0.041(5) Uiso 0.354(11) 1 d P A 2
H35A H -0.0009 0.2137 -0.0981 0.049 Uiso 0.354(11) 1 calc PR A 2
C36T C -0.0252(14) 0.1195(11) -0.1218(9) 0.046(5) Uiso 0.354(11) 1 d P A 2
H36A H -0.0643 0.1344 -0.1559 0.055 Uiso 0.354(11) 1 calc PR A 2

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 0.01935(10) 0.01069(9) 0.01164(9) 0.00080(6) 0.00549(7) -0.00171(7)
W2 0.01937(10) 0.01191(9) 0.01210(9) -0.00017(6) 0.00667(7) -0.00027(7)
W3 0.01873(10) 0.01261(9) 0.01101(9) 0.00076(6) 0.00482(7) -0.00154(7)
S4 0.0196(6) 0.0182(6) 0.0170(5) 0.0022(4) 0.0072(5) -0.0022(5)
S5 0.0242(6) 0.0167(6) 0.0125(5) 0.0011(4) 0.0079(5) -0.0015(5)
S6 0.0241(7) 0.0155(6) 0.0182(6) 0.0019(4) 0.0065(5) 0.0010(5)
S7 0.0264(7) 0.0141(5) 0.0160(5) -0.0024(4) 0.0065(5) -0.0036(5)
N1 0.022(2) 0.014(2) 0.023(2) 0.0002(16) 0.0048(17) -0.0035(16)
C11 0.033(3) 0.025(3) 0.030(3) 0.013(2) -0.003(2) -0.005(2)
C12 0.035(3) 0.024(3) 0.033(3) 0.013(2) -0.001(2) -0.003(2)
C13 0.094(6) 0.033(4) 0.042(4) 0.012(3) -0.023(4) -0.037(4)
C14 0.071(5) 0.023(3) 0.022(3) 0.004(2) -0.010(3) -0.017(3)
O1 0.071(3) 0.0130(19) 0.046(3) 0.0048(17) 0.003(2) -0.005(2)
N2 0.021(2) 0.026(2) 0.016(2) -0.0052(16) 0.0064(17) 0.0012(18)
C21 0.044(4) 0.028(3) 0.036(3) 0.001(2) 0.029(3) 0.003(3)
C22 0.062(5) 0.037(3) 0.044(4) 0.000(3) 0.034(3) 0.014(3)
C23 0.042(4) 0.024(3) 0.041(3) -0.002(2) 0.016(3) 0.011(3)
C24 0.047(4) 0.018(3) 0.040(3) 0.004(2) 0.021(3) 0.012(2)
O2 0.030(2) 0.046(2) 0.041(2) -0.0093(19) 0.0154(18) 0.0080(19)
N3 0.023(2) 0.025(2) 0.018(2) 0.0025(17) 0.0051(17) 0.0004(18)
C31 0.038(3) 0.027(3) 0.028(3) 0.013(2) 0.003(2) -0.007(2)
C32 0.035(4) 0.043(4) 0.034(3) 0.008(3) -0.003(3) 0.002(3)
C33 0.043(4) 0.042(4) 0.028(3) -0.002(3) -0.008(3) -0.011(3)
C34 0.033(3) 0.029(3) 0.026(3) -0.003(2) -0.005(2) -0.010(2)
O3 0.045(3) 0.046(3) 0.021(2) -0.0019(18) -0.0060(18) -0.004(2)
N1S 0.048(3) 0.042(3) 0.022(2) 0.008(2) 0.014(2) -0.001(2)
C11S 0.029(3) 0.029(3) 0.022(3) 0.003(2) 0.014(2) 0.002(2)
C12S 0.028(3) 0.031(3) 0.023(3) 0.000(2) 0.007(2) -0.007(2)
C13S 0.031(3) 0.030(3) 0.027(3) 0.006(2) 0.007(2) -0.007(2)
C14S 0.029(3) 0.042(3) 0.017(2) 0.003(2) 0.003(2) -0.005(3)
C15S 0.026(3) 0.039(3) 0.034(3) -0.003(2) 0.009(2) -0.004(2)
C16S 0.031(3) 0.026(3) 0.037(3) 0.004(2) 0.017(2) -0.005(2)
N2S 0.114(8) 0.044(5) 0.029(4) 0.000 0.029(5) 0.000
C21S 0.026(4) 0.047(5) 0.015(3) 0.000 -0.004(3) 0.000
C22S 0.023(3) 0.054(4) 0.021(3) -0.004(3) 0.005(2) 0.000(3)
C23S 0.032(3) 0.061(4) 0.036(3) 0.009(3) 0.010(3) -0.006(3)
C24S 0.044(6) 0.042(5) 0.063(6) 0.000 0.013(5) 0.000

_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              28.28
_diffrn_measured_fraction_theta_full   0.993
_refine_diff_density_max    1.472
_refine_diff_density_min   -1.393
_refine_diff_density_rms    0.179