Palladium-Catalyzed Desymmetrization of Silacyclobutanes with Alkynes: Enantioselective Synthesis of Silicon-Stereogenic 1-Sila-2-cyclohexenes and Mechanistic Considerations.
Shintani, Ryo; Moriya, Kohei; Hayashi, Tamio; Organic letters 14 (2012) 2902–2905; doi:10.1021/ol301191u

data_1507752
_publ_section_title
;
 Palladium-Catalyzed Desymmetrization of Silacyclobutanes with Alkynes:
 Enantioselective Synthesis of Silicon-Stereogenic 1-Sila-2-cyclohexenes
 and Mechanistic Considerations.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2902
_journal_page_last               2905
_journal_paper_doi               10.1021/ol301191u
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C42 H36 O4 P2 Pd '
_chemical_formula_sum            'C42 H36 O4 P2 Pd'
_chemical_formula_weight         773.09
_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                77.9626(10)
_cell_angle_beta                 72.5847(9)
_cell_angle_gamma                71.1590(10)
_cell_formula_units_Z            2
_cell_length_a                   10.26586(19)
_cell_length_b                   10.7910(2)
_cell_length_c                   18.0287(3)
_cell_measurement_reflns_used    15957
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      4.4
_cell_volume                     1789.64(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    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      93(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.070
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18707
_diffrn_reflns_theta_full        68.20
_diffrn_reflns_theta_max         68.20
_exptl_absorpt_coefficient_mu    5.358
_exptl_absorpt_correction_T_max  0.342
_exptl_absorpt_correction_T_min  0.261
_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    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             792.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.80
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6351
_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^)+(0.0093P)^2^+2.2450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                5910
_reflns_number_total             6351
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol301191u_si_005.cif
_cod_data_source_block           '_20324yuki'
_cod_original_formula_sum        'C42 H36 O4 P2 Pd '
_cod_database_code               1507752