Tris[(alkylthio)methyl]silanes: Syntheses and Structures of Chromium, Molybdenum, and Tungsten Complexes with a Tripodal Thioether Ligand
Hing W. Yim; Linh M. Tran; Ebern D. Dobbin; Daniel Rabinovich; Louise M. Liable-Sands; Christopher D. Incarvito; Kin-Chung Lam; Arnold L. Rheingold; Inorganic Chemistry 38 (1999) 2211–2215; doi:10.1021/ic981001j

data_4321948
_publ_contact_author
;
     Dr. Daniel Rabinovich
     Department of Chemistry
     University of North Carolina at Charlotte
     9201 University City Blvd.
     Charlotte, NC  28223
     USA
;
_publ_contact_author_email       DRabinov@email.uncc.edu
_publ_contact_author_fax         '+704 547 3151'
_publ_contact_author_phone       '+704 547 4442'
_publ_section_title
;
 Tris[(alkylthio)methyl]silanes: Syntheses and Structures of Chromium,
 Molybdenum, and Tungsten Complexes with a Tripodal Thioether Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2211
_journal_page_last               2215
_journal_paper_doi               10.1021/ic981001j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C10 H18 O3 S3 Si W'
_chemical_formula_weight         494.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.6568(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.1582(2)
_cell_length_b                   14.9903(2)
_cell_length_c                   26.7268(4)
_cell_measurement_reflns_used    7821
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3268.31(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Siemen's P4/CCD'
_diffrn_measurement_method       SMART
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0963
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15140
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    7.522
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.201
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.243
_refine_ls_extinction_coef       0.00015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         7476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                5201
_reflns_number_total             7476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981001j_3.cif
_cod_data_source_block           drab04
_cod_original_cell_volume        3268.30(9)
_cod_database_code               4321948