Synthons for Coordinatively Unsaturated Complexes of Tungsten, and Their Use for the Synthesis of High Oxidation-State Silylene Complexes
Benjamin V. Mork; T. Don Tilley; Journal of the American Chemical Society 126 (2004) 4375–4385; doi:10.1021/ja030548g

data_4112383
_publ_section_title
;
 Synthons for Coordinatively Unsaturated Complexes of Tungsten, and Their
 Use for the Synthesis of High Oxidation-State Silylene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4375
_journal_page_last               4385
_journal_paper_doi               10.1021/ja030548g
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C35 H50 P2 Si W '
_chemical_formula_sum            'C35 H50 P2 Si W'
_chemical_formula_weight         744.66
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3293(1)
_cell_length_b                   17.9586(4)
_cell_length_c                   20.4990(1)
_cell_measurement_reflns_used    4057
_cell_measurement_temperature    168
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      4.0
_cell_volume                     6747.63(16)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.052d'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SAPI91
_diffrn_ambient_temperature      168
_diffrn_measurement_device       SMART
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26056
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    3.580
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             3024.00
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.49
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.646
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         2138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0366
_refine_ls_wR_factor_gt          0.0222
_refine_ls_wR_factor_ref         0.0222
_reflns_number_gt                2138
_reflns_number_total             4829
_reflns_threshold_expression     I>3.00sigma
_cod_data_source_file            ja030548g_c2_3.cif
_cod_data_source_block           compound_7
_cod_original_cell_volume        6747.6(2)
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C35 H50 P2 Si W '
_cod_database_code               4112383