#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:06:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179313 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/10/4321059.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_4321059
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 O3 S Si2 W'
_chemical_formula_weight         1019.00
_chemical_name_systematic
;
  [WOS(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                 103.518(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7097(15)
_cell_length_b                   10.3575(6)
_cell_length_c                   27.002(3)
_cell_measurement_temperature    213(2)
_cell_volume                     4543.8(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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            14798
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    2.686
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.086
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0426P)²+6.2373P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                5174
_reflns_number_total             5512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000047l_2.cif
_cod_data_source_block           compound_2
_cod_database_code               4321059
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 0.5000 0.610362(15) 0.7500 0.03074(6) Uani 1 2 d S . .
O1 O 0.5756(4) 0.7213(7) 0.7668(2) 0.0501(16) Uani 0.50 1 d P A 2
O2 O 0.52042(13) 0.5670(2) 0.68478(8) 0.0349(4) Uani 1 1 d . A .
S1 S 0.61140(17) 0.7279(2) 0.78172(9) 0.0494(5) Uani 0.50 1 d P A 1
Si1 Si 0.49610(5) 0.56001(8) 0.62316(3) 0.03058(16) Uani 1 1 d . . .
N1 N 0.4287(12) 0.418(3) 0.7304(11) 0.034(2) Uani 0.50 1 d P A 1
C1 C 0.4723(4) 0.3030(6) 0.7417(2) 0.0311(14) Uiso 0.50 1 d P . 1
C2 C 0.4303(5) 0.1804(7) 0.7317(3) 0.0419(15) Uiso 0.50 1 d P . 1
C3 C 0.3418(6) 0.1753(9) 0.7114(3) 0.0486(16) Uiso 0.50 1 d P A 1
C4 C 0.2950(4) 0.2852(9) 0.7026(2) 0.0336(12) Uiso 0.50 1 d P A 1
C5 C 0.3434(4) 0.4029(7) 0.7133(2) 0.0316(12) Uiso 0.50 1 d P A 1
H5A H 0.3131 0.4802 0.7079 0.038 Uiso 0.50 1 calc PR A 1
C6 C 0.2069(6) 0.2937(10) 0.6832(4) 0.068(2) Uiso 0.50 1 d P A 1
H6A H 0.1838 0.2075 0.6781 0.102 Uiso 0.50 1 calc PR A 1
H6B H 0.1950 0.3397 0.6510 0.102 Uiso 0.50 1 calc PR A 1
H6C H 0.1827 0.3397 0.7074 0.102 Uiso 0.50 1 calc PR A 1
C7 C 0.2994(9) 0.0476(13) 0.6975(5) 0.094(3) Uiso 0.50 1 d P A 1
H7A H 0.3397 -0.0215 0.7051 0.142 Uiso 0.50 1 calc PR A 1
H7B H 0.2733 0.0468 0.6615 0.142 Uiso 0.50 1 calc PR A 1
H7C H 0.2581 0.0352 0.7170 0.142 Uiso 0.50 1 calc PR A 1
C8 C 0.4783(4) 0.0682(7) 0.7435(3) 0.0400(14) Uiso 0.50 1 d P . 1
H8A H 0.4504 -0.0125 0.7344 0.048 Uiso 0.50 1 d PR . 1
N2 N 0.4105(12) 0.430(3) 0.7323(11) 0.034(2) Uani 0.50 1 d P A 2
C9 C 0.4442(4) 0.3141(6) 0.7385(2) 0.0294(12) Uiso 0.50 1 d P . 2
C10 C 0.3947(5) 0.1991(7) 0.7272(3) 0.0432(15) Uiso 0.50 1 d P A 2
C11 C 0.3143(6) 0.2258(11) 0.7087(3) 0.0496(17) Uiso 0.50 1 d P A 2
C12 C 0.2803(5) 0.3437(11) 0.7017(3) 0.0531(18) Uiso 0.50 1 d P A 2
C13 C 0.3334(5) 0.4535(10) 0.7135(3) 0.0479(17) Uiso 0.50 1 d P A 2
H13A H 0.3132 0.5382 0.7077 0.057 Uiso 0.50 1 calc PR A 2
C14 C 0.1902(7) 0.3783(11) 0.6815(5) 0.077(3) Uiso 0.50 1 d P A 2
H14A H 0.1579 0.2999 0.6742 0.116 Uiso 0.50 1 calc PR A 2
H14B H 0.1840 0.4289 0.6506 0.116 Uiso 0.50 1 calc PR A 2
H14C H 0.1712 0.4283 0.7070 0.116 Uiso 0.50 1 calc PR A 2
C15 C 0.2526(9) 0.1098(12) 0.6949(6) 0.091(4) Uiso 0.50 1 d P A 2
H15A H 0.2828 0.0291 0.7012 0.137 Uiso 0.50 1 calc PR A 2
H15B H 0.2243 0.1150 0.6593 0.137 Uiso 0.50 1 calc PR A 2
H15C H 0.2127 0.1137 0.7159 0.137 Uiso 0.50 1 calc PR A 2
C16 C 0.4349(7) 0.0821(10) 0.7368(4) 0.065(2) Uiso 0.50 1 d P A 2
H16A H 0.4021 0.0053 0.7298 0.079 Uiso 0.50 1 d PR A 2
C17 C 0.4780(2) 0.7264(3) 0.59560(12) 0.0391(6) Uani 1 1 d . A .
C18 C 0.4917(3) 0.8369(4) 0.62511(15) 0.0527(9) Uani 1 1 d . . .
H18A H 0.5119 0.8297 0.6605 0.063 Uiso 1 1 calc R A .
C19 C 0.4760(4) 0.9595(4) 0.6030(2) 0.0739(14) Uani 1 1 d . A .
H19A H 0.4851 1.0336 0.6236 0.089 Uiso 1 1 calc R . .
C20 C 0.4479(3) 0.9714(5) 0.5519(2) 0.0766(15) Uani 1 1 d . . .
H20A H 0.4388 1.0539 0.5371 0.092 Uiso 1 1 calc R A .
C21 C 0.4325(3) 0.8630(5) 0.52143(19) 0.0716(13) Uani 1 1 d . A .
H21A H 0.4122 0.8714 0.4861 0.086 Uiso 1 1 calc R . .
C22 C 0.4470(2) 0.7423(4) 0.54321(14) 0.0521(8) Uani 1 1 d . . .
H22A H 0.4359 0.6688 0.5223 0.062 Uiso 1 1 calc R A .
C23 C 0.39933(19) 0.4652(3) 0.59937(11) 0.0348(6) Uani 1 1 d . A .
C24 C 0.3985(2) 0.3348(4) 0.58803(17) 0.0561(9) Uani 1 1 d . . .
H24A H 0.4487 0.2907 0.5914 0.067 Uiso 1 1 calc R A .
C25 C 0.3246(3) 0.2673(5) 0.5716(2) 0.0682(12) Uani 1 1 d . A .
H25A H 0.3255 0.1782 0.5651 0.082 Uiso 1 1 calc R . .
C26 C 0.2512(2) 0.3304(5) 0.56501(15) 0.0605(10) Uani 1 1 d . . .
H26A H 0.2016 0.2856 0.5528 0.073 Uiso 1 1 calc R A .
C27 C 0.2500(2) 0.4607(5) 0.57636(15) 0.0564(10) Uani 1 1 d . A .
H27A H 0.1996 0.5044 0.5724 0.068 Uiso 1 1 calc R . .
C28 C 0.3231(2) 0.5258(4) 0.59351(13) 0.0448(7) Uani 1 1 d . . .
H28A H 0.3215 0.6140 0.6015 0.054 Uiso 1 1 calc R A .
C30 C 0.58439(18) 0.4798(3) 0.60377(11) 0.0343(6) Uani 1 1 d . A .
C31 C 0.6234(2) 0.3740(3) 0.63114(15) 0.0480(8) Uani 1 1 d . . .
H31A H 0.6036 0.3420 0.6586 0.058 Uiso 1 1 calc R A .
C32 C 0.6909(3) 0.3148(4) 0.61888(18) 0.0617(10) Uani 1 1 d . A .
H32A H 0.7155 0.2425 0.6374 0.074 Uiso 1 1 calc R . .
C33 C 0.7216(3) 0.3626(4) 0.5793(2) 0.0650(12) Uani 1 1 d . . .
H33A H 0.7679 0.3240 0.5713 0.078 Uiso 1 1 calc R A .
C34 C 0.6841(2) 0.4674(4) 0.55135(15) 0.0538(9) Uani 1 1 d . A .
H34A H 0.7047 0.4997 0.5242 0.065 Uiso 1 1 calc R . .
C35 C 0.6162(2) 0.5244(3) 0.56360(12) 0.0425(7) Uani 1 1 d . . .
H35A H 0.5910 0.5951 0.5443 0.051 Uiso 1 1 calc R A .
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 94.3(5) . 2_656 ?
O1 W1 O2 97.0(2) . . ?
O1 W1 O2 101.2(2) 2_656 . ?
O1 W1 O2 101.2(2) . 2_656 ?
O1 W1 O2 97.0(2) 2_656 2_656 ?
O2 W1 O2 153.01(13) . 2_656 ?
O1 W1 S1 10.6(3) . . ?
O1 W1 S1 103.7(3) 2_656 . ?
O2 W1 S1 99.72(9) . . ?
O2 W1 S1 94.99(9) 2_656 . ?
O1 W1 S1 103.7(3) . 2_656 ?
O1 W1 S1 10.6(3) 2_656 2_656 ?
O2 W1 S1 94.99(9) . 2_656 ?
O2 W1 S1 99.72(9) 2_656 2_656 ?
S1 W1 S1 113.53(15) . 2_656 ?
O1 W1 N1 163.3(5) . . ?
O1 W1 N1 102.2(6) 2_656 . ?
O2 W1 N1 77.4(6) . . ?
O2 W1 N1 79.4(7) 2_656 . ?
S1 W1 N1 153.9(6) . . ?
S1 W1 N1 92.5(6) 2_656 . ?
O1 W1 N1 102.2(6) . 2_656 ?
O1 W1 N1 163.3(6) 2_656 2_656 ?
O2 W1 N1 79.4(7) . 2_656 ?
O2 W1 N1 77.4(6) 2_656 2_656 ?
S1 W1 N1 92.5(6) . 2_656 ?
S1 W1 N1 153.9(6) 2_656 2_656 ?
N1 W1 N1 61.4(11) . 2_656 ?
O1 W1 N2 170.8(7) . . ?
O1 W1 N2 94.8(6) 2_656 . ?
O2 W1 N2 82.6(6) . . ?
O2 W1 N2 76.2(7) 2_656 . ?
S1 W1 N2 160.4(7) . . ?
S1 W1 N2 85.5(6) 2_656 . ?
N1 W1 N2 8.4(8) . . ?
N1 W1 N2 68.6(2) 2_656 . ?
O1 W1 N2 94.8(6) . 2_656 ?
O1 W1 N2 170.8(7) 2_656 2_656 ?
O2 W1 N2 76.2(7) . 2_656 ?
O2 W1 N2 82.6(6) 2_656 2_656 ?
S1 W1 N2 85.5(6) . 2_656 ?
S1 W1 N2 160.4(7) 2_656 2_656 ?
N1 W1 N2 68.6(2) . 2_656 ?
N1 W1 N2 8.4(8) 2_656 2_656 ?
N2 W1 N2 76.1(11) . 2_656 ?
Si1 O2 W1 153.57(14) . . ?
O2 Si1 C30 106.41(13) . . ?
O2 Si1 C23 111.42(13) . . ?
C30 Si1 C23 110.19(13) . . ?
O2 Si1 C17 110.20(14) . . ?
C30 Si1 C17 111.24(14) . . ?
C23 Si1 C17 107.43(14) . . ?
C1 N1 C5 115(3) . . ?
C1 N1 W1 118.0(14) . . ?
C5 N1 W1 126.7(18) . . ?
C1 C1 N1 121.2(13) 2_656 . ?
C1 C1 C2 118.4(4) 2_656 . ?
N1 C1 C2 120.2(14) . . ?
C8 C2 C1 117.2(7) . . ?
C8 C2 C3 122.2(7) . . ?
C1 C2 C3 120.6(7) . . ?
C8 C2 C8 18.4(3) . 2_656 ?
C1 C2 C8 98.9(5) . 2_656 ?
C3 C2 C8 140.3(6) . 2_656 ?
C4 C3 C2 121.6(7) . . ?
C4 C3 C7 118.1(9) . . ?
C2 C3 C7 120.2(9) . . ?
C3 C4 C6 127.2(8) . . ?
C3 C4 C5 113.2(6) . . ?
C6 C4 C5 119.5(9) . . ?
N1 C5 C4 129.2(16) . . ?
C8 C8 C2 124.1(4) 2_656 . ?
C8 C8 C2 37.5(3) 2_656 2_656 ?
C2 C8 C2 86.8(6) . 2_656 ?
C13 N2 C9 125(3) . . ?
C13 N2 W1 117(2) . . ?
C9 N2 W1 117.5(13) . . ?
N2 C9 C10 121.3(13) . . ?
N2 C9 C9 114.4(12) . 2_656 ?
C10 C9 C9 124.2(5) . 2_656 ?
C11 C10 C16 130.5(9) . . ?
C11 C10 C9 112.4(8) . . ?
C16 C10 C9 117.1(8) . . ?
C12 C11 C10 126.2(8) . . ?
C12 C11 C15 115.6(9) . . ?
C10 C11 C15 118.2(11) . . ?
C11 C12 C13 118.2(8) . . ?
C11 C12 C14 128.1(9) . . ?
C13 C12 C14 113.7(10) . . ?
N2 C13 C12 116.7(18) . . ?
C18 C17 C22 117.2(3) . . ?
C18 C17 Si1 122.9(3) . . ?
C22 C17 Si1 119.9(3) . . ?
C17 C18 C19 121.0(4) . . ?
C20 C19 C18 120.2(5) . . ?
C19 C20 C21 120.3(4) . . ?
C22 C21 C20 119.6(4) . . ?
C21 C22 C17 121.7(4) . . ?
C24 C23 C28 116.9(3) . . ?
C24 C23 Si1 123.4(3) . . ?
C28 C23 Si1 119.7(2) . . ?
C23 C24 C25 121.4(4) . . ?
C26 C25 C24 120.1(4) . . ?
C25 C26 C27 119.8(4) . . ?
C28 C27 C26 119.6(4) . . ?
C27 C28 C23 122.1(4) . . ?
C35 C30 C31 117.2(3) . . ?
C35 C30 Si1 122.7(2) . . ?
C31 C30 Si1 120.1(2) . . ?
C32 C31 C30 121.7(4) . . ?
C33 C32 C31 119.7(4) . . ?
C32 C33 C34 120.0(4) . . ?
C33 C34 C35 119.7(4) . . ?
C34 C35 C30 121.8(3) . . ?
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 1.689(6) . ?
W1 O1 1.689(6) 2_656 ?
W1 O2 1.924(2) . ?
W1 O2 1.924(2) 2_656 ?
W1 S1 2.222(2) . ?
W1 S1 2.222(2) 2_656 ?
W1 N1 2.32(4) . ?
W1 N1 2.32(4) 2_656 ?
W1 N2 2.37(3) . ?
W1 N2 2.37(3) 2_656 ?
O2 Si1 1.620(2) . ?
Si1 C30 1.872(3) . ?
Si1 C23 1.872(3) . ?
Si1 C17 1.873(3) . ?
N1 C1 1.39(3) . ?
N1 C5 1.40(2) . ?
C1 C1 0.928(13) 2_656 ?
C1 C2 1.446(9) . ?
C2 C8 1.405(10) . ?
C2 C3 1.452(11) . ?
C2 C8 1.912(10) 2_656 ?
C3 C4 1.370(11) . ?
C3 C7 1.506(16) . ?
C4 C6 1.447(12) . ?
C4 C5 1.454(10) . ?
C8 C8 0.730(12) 2_656 ?
C8 C2 1.912(10) 2_656 ?
N2 C13 1.29(2) . ?
N2 C9 1.32(3) . ?
C9 C10 1.442(10) . ?
C9 C9 1.823(15) 2_656 ?
C10 C11 1.349(13) . ?
C10 C16 1.379(13) . ?
C11 C12 1.341(13) . ?
C11 C15 1.569(15) . ?
C12 C13 1.432(13) . ?
C12 C14 1.520(15) . ?
C17 C18 1.383(5) . ?
C17 C22 1.398(5) . ?
C18 C19 1.402(5) . ?
C19 C20 1.356(7) . ?
C20 C21 1.379(8) . ?
C21 C22 1.379(6) . ?
C23 C24 1.384(5) . ?
C23 C28 1.396(4) . ?
C24 C25 1.398(5) . ?
C25 C26 1.364(7) . ?
C26 C27 1.385(7) . ?
C27 C28 1.376(5) . ?
C30 C35 1.394(4) . ?
C30 C31 1.395(5) . ?
C31 C32 1.389(5) . ?
C32 C33 1.382(6) . ?
C33 C34 1.385(7) . ?
C34 C35 1.386(5) . ?
