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_4112379
_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_sum            'C40 H31 B F20 P2 W'
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_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 13:13:33 2001'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 96.322(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2193(2)
_cell_length_b                   15.9706(2)
_cell_length_c                   17.2664(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      4.0
_cell_volume                     4171.27(11)
_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    SIR92
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
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_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
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_diffrn_reflns_av_R_equivalents  0.0570
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_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_theta_max         24.72
_diffrn_standards_decay_%        0.00
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_exptl_absorpt_coefficient_mu    2.970
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       plate
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_exptl_crystal_size_mid          0.250
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0500
_refine_ls_wR_factor_gt          0.0449
_reflns_number_gt                4575
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_reflns_threshold_expression     I>3.00sigma
_cod_data_source_file            ja030548g_2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        4171.27(9)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C40 H31 B F20 P2 W '
_cod_database_code               4112379