Silylation, Sulfidation, and Benzene-1,2-dithiolate Complexation Reactions of Oxo- and Oxosulfidomolybdates(VI) and -Tungstates(VI)
Wang, Jun-Jieh; Holm, R. H.; Inorganic Chemistry 46 (2007) 11156–11164; doi:10.1021/ic701294y

data_4333446
_publ_section_title
;
 Silylation, Sulfidation, and Benzene-1,2-dithiolate Complexation
 Reactions of Oxo- and Oxosulfidomolybdates(VI) and -Tungstates(VI)
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11156
_journal_page_last               11164
_journal_paper_doi               10.1021/ic701294y
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '(C8 H20 N 1+), (C15 H25 O3 S2 Si W 1-)'
_chemical_formula_sum            'C23 H45 N O3 S2 Si W'
_chemical_formula_weight         659.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.9760(10)
_cell_angle_beta                 88.8130(10)
_cell_angle_gamma                89.7990(10)
_cell_formula_units_Z            4
_cell_length_a                   8.4161(4)
_cell_length_b                   17.3262(9)
_cell_length_c                   19.9065(11)
_cell_measurement_temperature    193(2)
_cell_volume                     2891.0(3)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\w scans, 0.3\% rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24509
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.204
_exptl_absorpt_correction_T_max  0.6786
_exptl_absorpt_correction_T_min  0.4196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.545
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         13635
_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+1.2807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                10703
_reflns_number_total             13635
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701294ysup10.cif
_cod_data_source_block           9b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4333446