Oxo/Sulfidotungstate(VI) as Precursors to WVIO2, WVIOS, and WVIS2 Complexes and WIV-Dithiolene Chelate Rings
Mingming Miao; Michael W. Willer; R. H. Holm; Inorganic Chemistry 39 (2000) 2843–2849; doi:10.1021/ic000047l

data_4321059
_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/[\s^2^(Fo^2^)+(0.0426P)^2^+6.2373P] where P=(Fo^2^+2Fc^2^)/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