Rhodium-Catalyzed Asymmetric Synthesis of Silicon-Stereogenic Dibenzooxasilines via Enantioselective Transmetalation
Ryo Shintani; Eleanor E. Maciver; Fumiko Tamakuni; Tamio Hayashi; Journal of the American Chemical Society 134 (2012) 16955–16958; doi:10.1021/ja3076555

data_4118769
_publ_section_title
;
 Rhodium-Catalyzed Asymmetric Synthesis of Silicon-Stereogenic
 Dibenzooxasilines via Enantioselective Transmetalation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16955
_journal_page_last               16958
_journal_paper_doi               10.1021/ja3076555
_journal_volume                  134
_journal_year                    2012
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C23 H26 O Si '
_chemical_formula_sum            'C23 H26 O Si'
_chemical_formula_weight         346.54
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.1108(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.68805(18)
_cell_length_b                   10.08629(18)
_cell_length_c                   20.5544(4)
_cell_measurement_reflns_used    19164
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      4.4
_cell_volume                     1983.16(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      93(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.034
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20020
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.627
_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    1.161
_exptl_crystal_description       prism
_exptl_crystal_F_000             744.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.22
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2586 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6415
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.4406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                6128
_reflns_number_total             6415
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja3076555_si_003.cif
_cod_data_source_block           '_20703yuki'
_cod_original_formula_sum        'C23 H26 O Si '
_cod_database_code               4118769