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_4116240
_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            'C31 H34 N2 O2 Si W'
_chemical_formula_weight         678.56
_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             'Thu May 25 15:24:01 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90.84(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.018(2)
_cell_length_b                   16.244(4)
_cell_length_c                   20.737(2)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    286.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      26.4
_cell_volume                     3037.4(10)
_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-2\q
_diffrn_orient_matrix_UB_11      -0.04377
_diffrn_orient_matrix_UB_12      -0.05534
_diffrn_orient_matrix_UB_13      -0.00943
_diffrn_orient_matrix_UB_21      0.00956
_diffrn_orient_matrix_UB_22      0.01043
_diffrn_orient_matrix_UB_23      -0.04728
_diffrn_orient_matrix_UB_31      0.10145
_diffrn_orient_matrix_UB_32      -0.02486
_diffrn_orient_matrix_UB_33      0.00116
_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  0.080
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7615
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        -6.21
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.875
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1352.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.553
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4241
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.4040
_refine_ls_shift/su_mean         0.0240
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00112|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                4241
_reflns_number_total             7163
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja993279w_1.cif
_cod_data_source_block           complex_4a.CH3CN
_cod_original_cell_volume        3037.4(9)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C31 H34 N2 O2 Si W '
_cod_database_code               4116240