#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:06:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179313 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/10/4321060.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_4321060
loop_
_publ_author_name
'Mingming Miao'
'Michael W. Willer'
'R. H. Holm'
_publ_contact_author             R.H.Holm
_publ_contact_author_address
;
    Dept. of Chemistry and Chemical Biology
    Harvard University
    Cambridge, MA 02138
    USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_section_title
;
 Oxo/Sulfidotungstate(VI) as Precursors to WVIO2, WVIOS, and WVIS2
 Complexes and WIV-Dithiolene Chelate Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2843
_journal_page_last               2849
_journal_paper_doi               10.1021/ic000047l
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C52 H46 N2 O2 S2 Si2 W'
_chemical_formula_weight         1035.06
_chemical_name_systematic
;
  [WS2(OSiPh3)2(Me4phen)]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.5170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.93510(10)
_cell_length_b                   10.49630(10)
_cell_length_c                   26.8896(2)
_cell_measurement_temperature    213(2)
_cell_volume                     4627.18(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            15099
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    2.681
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       prism
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.072
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0459P)²+1.2831P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                5146
_reflns_number_total             5612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000047l_3.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        4627.18(6)
_cod_database_code               4321060
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_
_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 0.0000 0.112813(16) 0.7500 0.02532(6) Uani 1 2 d S . .
O1 O 0.02217(14) 0.0699(2) 0.68539(8) 0.0309(4) Uani 1 1 d . . .
Si1 Si -0.00141(5) 0.06067(9) 0.62303(3) 0.02823(17) Uani 1 1 d . . .
S1 S 0.10282(6) 0.23638(10) 0.78008(4) 0.0440(2) Uani 1 1 d . . .
N1 N -0.08064(17) -0.0704(3) 0.72994(10) 0.0318(6) Uani 1 1 d . . .
C1 C -0.1609(2) -0.0687(4) 0.71155(14) 0.0418(8) Uani 1 1 d . . .
H1A H -0.1871 0.0108 0.7052 0.050 Uiso 1 1 calc R . .
C2 C -0.2095(3) -0.1800(6) 0.70099(15) 0.0565(13) Uani 1 1 d . . .
C3 C -0.1732(3) -0.2964(5) 0.71025(17) 0.0653(15) Uani 1 1 d . . .
C4 C -0.0871(3) -0.3026(4) 0.72998(15) 0.0535(11) Uani 1 1 d . . .
C5 C -0.0433(2) -0.1854(3) 0.73936(12) 0.0373(8) Uani 1 1 d . . .
C6 C -0.0414(4) -0.4178(5) 0.7405(2) 0.082(2) Uani 1 1 d . . .
C7 C -0.2231(5) -0.4165(7) 0.6993(3) 0.110(3) Uani 1 1 d . . .
H7A H -0.2802 -0.3947 0.6862 0.165 Uiso 1 1 calc R . .
H7B H -0.2161 -0.4654 0.7307 0.165 Uiso 1 1 calc R . .
H7C H -0.2051 -0.4668 0.6739 0.165 Uiso 1 1 calc R . .
C8 C -0.3007(3) -0.1601(8) 0.6796(2) 0.092(2) Uani 1 1 d . . .
H8A H -0.3278 -0.2422 0.6737 0.137 Uiso 1 1 calc R . .
H8B H -0.3104 -0.1137 0.6475 0.137 Uiso 1 1 calc R . .
H8C H -0.3222 -0.1118 0.7041 0.137 Uiso 1 1 calc R . .
C9 C -0.0203(2) 0.2240(4) 0.59399(14) 0.0369(7) Uani 1 1 d . . .
C10 C -0.0528(3) 0.2359(5) 0.54121(16) 0.0513(9) Uani 1 1 d . . .
H10A H -0.0638 0.1621 0.5208 0.062 Uiso 1 1 calc R . .
C11 C -0.0690(3) 0.3543(6) 0.5182(2) 0.0684(14) Uani 1 1 d . . .
H11A H -0.0906 0.3602 0.4825 0.082 Uiso 1 1 calc R . .
C12 C -0.0535(4) 0.4640(5) 0.5476(2) 0.0713(15) Uani 1 1 d . . .
H12A H -0.0643 0.5445 0.5321 0.086 Uiso 1 1 calc R . .
C13 C -0.0223(3) 0.4536(4) 0.5997(2) 0.0612(12) Uani 1 1 d . . .
H13A H -0.0122 0.5277 0.6199 0.073 Uiso 1 1 calc R . .
C14 C -0.0054(2) 0.3342(4) 0.62301(16) 0.0430(8) Uani 1 1 d . . .
H14A H 0.0164 0.3289 0.6587 0.052 Uiso 1 1 calc R . .
C15 C 0.08719(19) -0.0188(3) 0.60534(12) 0.0322(6) Uani 1 1 d . . .
C16 C 0.1200(2) 0.0255(4) 0.56607(14) 0.0423(8) Uani 1 1 d . . .
H16A H 0.0954 0.0954 0.5463 0.051 Uiso 1 1 calc R . .
C17 C 0.1884(3) -0.0307(5) 0.55519(18) 0.0549(11) Uani 1 1 d . . .
H17A H 0.2104 0.0027 0.5291 0.066 Uiso 1 1 calc R . .
C18 C 0.2233(3) -0.1351(5) 0.5828(2) 0.0600(12) Uani 1 1 d . . .
H18A H 0.2688 -0.1743 0.5752 0.072 Uiso 1 1 calc R . .
C19 C 0.1920(3) -0.1832(4) 0.6217(2) 0.0560(11) Uani 1 1 d . . .
H19A H 0.2162 -0.2548 0.6405 0.067 Uiso 1 1 calc R . .
C20 C 0.1247(2) -0.1252(4) 0.63298(16) 0.0425(8) Uani 1 1 d . . .
H20A H 0.1039 -0.1580 0.6597 0.051 Uiso 1 1 calc R . .
C21 C -0.0967(2) -0.0346(3) 0.59870(12) 0.0338(7) Uani 1 1 d . . .
C22 C -0.0971(2) -0.1650(4) 0.58899(18) 0.0516(10) Uani 1 1 d . . .
H22A H -0.0469 -0.2077 0.5940 0.062 Uiso 1 1 calc R . .
C23 C -0.1685(3) -0.2341(5) 0.5723(2) 0.0652(13) Uani 1 1 d . . .
H23A H -0.1665 -0.3223 0.5666 0.078 Uiso 1 1 calc R . .
C24 C -0.2428(3) -0.1717(5) 0.56400(16) 0.0577(11) Uani 1 1 d . . .
H24A H -0.2917 -0.2172 0.5520 0.069 Uiso 1 1 calc R . .
C25 C -0.2448(2) -0.0429(5) 0.57336(16) 0.0537(11) Uani 1 1 d . . .
H25A H -0.2952 -0.0006 0.5680 0.064 Uiso 1 1 calc R . .
C26 C -0.1731(2) 0.0245(4) 0.59062(15) 0.0453(9) Uani 1 1 d . . .
H26A H -0.1756 0.1122 0.5971 0.054 Uiso 1 1 calc R . .
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'
Si Si 0.0817 0.0704 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 W1 O1 152.91(14) . 2_556 ?
O1 W1 S1 99.06(7) . . ?
O1 W1 S1 97.12(7) 2_556 . ?
O1 W1 S1 97.12(7) . 2_556 ?
O1 W1 S1 99.06(7) 2_556 2_556 ?
S1 W1 S1 106.16(6) . 2_556 ?
O1 W1 N1 80.46(10) . . ?
O1 W1 N1 77.35(10) 2_556 . ?
S1 W1 N1 161.53(8) . . ?
S1 W1 N1 92.17(8) 2_556 . ?
O1 W1 N1 77.35(10) . 2_556 ?
O1 W1 N1 80.46(10) 2_556 2_556 ?
S1 W1 N1 92.17(8) . 2_556 ?
S1 W1 N1 161.53(8) 2_556 2_556 ?
N1 W1 N1 69.62(15) . 2_556 ?
Si1 O1 W1 153.32(15) . . ?
O1 Si1 C21 111.09(14) . . ?
O1 Si1 C9 110.26(15) . . ?
C21 Si1 C9 107.46(16) . . ?
O1 Si1 C15 106.39(14) . . ?
C21 Si1 C15 110.34(15) . . ?
C9 Si1 C15 111.34(15) . . ?
C1 N1 C5 117.9(3) . . ?
C1 N1 W1 124.0(3) . . ?
C5 N1 W1 118.0(2) . . ?
N1 C1 C2 123.6(5) . . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 C8 124.2(5) . . ?
C1 C2 C8 116.5(6) . . ?
C2 C3 C4 118.9(4) . . ?
C2 C3 C7 120.6(6) . . ?
C4 C3 C7 120.5(6) . . ?
C3 C4 C6 124.6(4) . . ?
C3 C4 C5 117.7(4) . . ?
C6 C4 C5 117.7(5) . . ?
N1 C5 C4 122.5(4) . . ?
N1 C5 C5 117.15(19) . 2_556 ?
C4 C5 C5 120.3(3) . 2_556 ?
C6 C6 C4 122.0(3) 2_556 . ?
C14 C9 C10 118.0(4) . . ?
C14 C9 Si1 122.8(3) . . ?
C10 C9 Si1 119.2(3) . . ?
C11 C10 C9 121.3(5) . . ?
C12 C11 C10 120.2(4) . . ?
C13 C12 C11 119.2(4) . . ?
C12 C13 C14 120.8(5) . . ?
C9 C14 C13 120.5(4) . . ?
C16 C15 C20 117.0(3) . . ?
C16 C15 Si1 122.7(3) . . ?
C20 C15 Si1 120.2(3) . . ?
C15 C16 C17 121.9(4) . . ?
C18 C17 C16 119.5(4) . . ?
C17 C18 C19 120.5(4) . . ?
C18 C19 C20 119.7(4) . . ?
C19 C20 C15 121.3(4) . . ?
C22 C21 C26 116.4(3) . . ?
C22 C21 Si1 123.6(3) . . ?
C26 C21 Si1 120.0(3) . . ?
C23 C22 C21 122.6(4) . . ?
C22 C23 C24 119.2(5) . . ?
C25 C24 C23 119.8(4) . . ?
C24 C25 C26 120.3(4) . . ?
C25 C26 C21 121.7(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 1.921(2) . ?
W1 O1 1.921(2) 2_556 ?
W1 S1 2.1592(9) . ?
W1 S1 2.1592(9) 2_556 ?
W1 N1 2.342(3) . ?
W1 N1 2.342(3) 2_556 ?
O1 Si1 1.626(2) . ?
Si1 C21 1.871(3) . ?
Si1 C9 1.878(4) . ?
Si1 C15 1.879(3) . ?
N1 C1 1.325(4) . ?
N1 C5 1.357(5) . ?
C1 C2 1.416(6) . ?
C2 C3 1.362(8) . ?
C2 C8 1.522(7) . ?
C3 C4 1.421(7) . ?
C3 C7 1.505(7) . ?
C4 C6 1.425(8) . ?
C4 C5 1.426(5) . ?
C5 C5 1.435(7) 2_556 ?
C6 C6 1.368(15) 2_556 ?
C9 C14 1.383(6) . ?
C9 C10 1.393(5) . ?
C10 C11 1.385(6) . ?
C11 C12 1.385(8) . ?
C12 C13 1.370(8) . ?
C13 C14 1.399(6) . ?
C15 C16 1.391(5) . ?
C15 C20 1.402(5) . ?
C16 C17 1.394(6) . ?
C17 C18 1.372(7) . ?
C18 C19 1.380(7) . ?
C19 C20 1.392(5) . ?
C21 C22 1.394(6) . ?
C21 C26 1.401(5) . ?
C22 C23 1.385(6) . ?
C23 C24 1.387(7) . ?
C24 C25 1.378(8) . ?
C25 C26 1.381(6) . ?
