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_4112378
_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         'C16 H31 Cl P2 W '
_chemical_formula_sum            'C16 H31 Cl P2 W'
_chemical_formula_weight         504.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Fri Jun 15 09:26:40 2001'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 102.536(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7200(2)
_cell_length_b                   16.6120(3)
_cell_length_c                   13.9440(1)
_cell_measurement_reflns_used    4163
_cell_measurement_temperature    169.2
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      1.5
_cell_volume                     1971.73(6)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.0'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.9781
_diffrn_measured_fraction_theta_max 0.9781
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3534
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_exptl_absorpt_coefficient_mu    13.243
_exptl_absorpt_correction_T_max  0.560
_exptl_absorpt_correction_T_min  0.230
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       blocks
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         2.88
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.411
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2433
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.0216
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0371
_reflns_number_gt                2433
_reflns_number_total             3400
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ja030548g_1.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C16 H31 Cl P2 W '
_cod_database_code               4112378