Novel η3-1-Silaallyl Tungsten Complexes via Si-H Bond Activation of Hydrovinylsilanes: Structure and Reactivity toward Methanol
Hiroyuki Sakaba; Sanae Watanabe; Chizuko Kabuto; Kuninobu Kabuto; Journal of the American Chemical Society 125 (2003) 2842–2843; doi:10.1021/ja028432s

data_4113529
_publ_section_title
;
 Novel \h3-1-Silaallyl Tungsten Complexes via Si-H Bond Activation of
 Hydrovinylsilanes: Structure and Reactivity toward Methanol
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2842
_journal_page_last               2843
_journal_paper_doi               10.1021/ja028432s
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C19 H32 O3 Si W '
_chemical_formula_sum            'C19 H32 O3 Si W'
_chemical_formula_weight         520.40
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 102.802(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.805(3)
_cell_length_b                   8.606(2)
_cell_length_c                   15.728(3)
_cell_measurement_reflns_used    7837
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     2086.1(7)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16331
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_exptl_absorpt_coefficient_mu    5.615
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         3621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0642
_reflns_number_gt                3172
_reflns_number_total             3621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028432ssi20021230_063738_2.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        2085.9(7)
_cod_original_formula_sum        'C19 H32 O3 Si W '
_cod_database_code               4113529