Synthesis, Structure, and Silylene Exchange Reaction of Base-Stabilized Hydrido(silylene)tungsten Complexes and Rearrangement of Hydrosilyl(pyridine)tungsten Complexes to the Base-Stabilized Hydrido(silylene) Complexes via 1,2-Hydrogen Migration
Hiroyuki Sakaba; Masanori Tsukamoto; Takeshi Hirata; Chizuko Kabuto; Hiroshi Horino; Journal of the American Chemical Society 122 (2000) 11511–11512; doi:10.1021/ja993279w

data_4116241
_publ_section_title
;
 Synthesis, Structure, and Silylene Exchange Reaction of Base-Stabilized
 Hydrido(silylene)tungsten Complexes and Rearrangement of
 Hydrosilyl(pyridine)tungsten Complexes to the Base-Stabilized
 Hydrido(silylene) Complexes via 1,2-Hydrogen Migration
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11511
_journal_page_last               11512
_journal_paper_doi               10.1021/ja993279w
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C29 H31 N O2 Si W'
_chemical_formula_weight         637.50
_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'
_audit_creation_date             'Thu May 25 15:26:27 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   34.226(9)
_cell_length_b                   20.44(1)
_cell_length_c                   15.638(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    286.2
_cell_measurement_theta_max      20.2
_cell_measurement_theta_min      17.7
_cell_volume                     10940(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      286.2
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.01793
_diffrn_orient_matrix_UB_12      0.03437
_diffrn_orient_matrix_UB_13      0.02303
_diffrn_orient_matrix_UB_21      -0.00684
_diffrn_orient_matrix_UB_22      0.01339
_diffrn_orient_matrix_UB_23      -0.05965
_diffrn_orient_matrix_UB_31      -0.02203
_diffrn_orient_matrix_UB_32      -0.03213
_diffrn_orient_matrix_UB_33      -0.00020
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.096
_diffrn_reflns_av_sigmaI/netI    0.084
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11364
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        -7.56
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.296
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5056.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.90
_refine_diff_density_min         -1.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.492
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     621
_refine_ls_number_reflns         5624
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          1.0510
_refine_ls_shift/su_mean         0.0150
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                5624
_reflns_number_total             11250
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja993279w_2.cif
_cod_data_source_block           complex_5
_cod_original_cell_volume        10941(6)
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C29 H31 N O2 Si W '
_cod_database_code               4116241