Palladium-Catalyzed Enantioselective Desymmetrization of Silacyclobutanes: Construction of Silacycles Possessing a Tetraorganosilicon Stereocenter
Ryo Shintani; Kohei Moriya; Tamio Hayashi; Journal of the American Chemical Society 133 (2011) 16440–16443; doi:10.1021/ja208621x

data_4106981
_publ_section_title
;
 Palladium-Catalyzed Enantioselective Desymmetrization of
 Silacyclobutanes: Construction of Silacycles Possessing a
 Tetraorganosilicon Stereocenter
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16440
_journal_page_last               16443
_journal_paper_doi               10.1021/ja208621x
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C25 H27 B O3 Si '
_chemical_formula_sum            'C25 H27 B O3 Si'
_chemical_formula_weight         414.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                81.4897(15)
_cell_angle_beta                 72.9482(13)
_cell_angle_gamma                77.9686(13)
_cell_formula_units_Z            2
_cell_length_a                   8.60096(17)
_cell_length_b                   9.3243(2)
_cell_length_c                   14.1840(3)
_cell_measurement_reflns_used    7992
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.3
_cell_volume                     1059.03(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      93(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10034
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       chip
_exptl_crystal_F_000             440.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.37
_refine_diff_density_min         -1.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7322
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                7267
_reflns_number_total             3748
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja208621x_si_002.cif
_cod_data_source_block           '_10829yuki'
_cod_original_formula_sum        'C25 H27 B O3 Si '
_cod_database_code               4106981