Catalytic Asymmetric Rearrangement of α,α-Disubstituted α-Siloxy Aldehydes to Optically Active Acyloins Using Axially Chiral Organoaluminum Lewis Acids
Takashi Ooi; Kohsuke Ohmatsu; Keiji Maruoka; Journal of the American Chemical Society 129 (2007) 2410–2411; doi:10.1021/ja063051q

data_4109130
_publ_section_title
;
 Catalytic Asymmetric Rearrangement of \a,\a-Disubstituted \a-Siloxy
 Aldehydes to Optically Active Acyloins Using Axially Chiral
 Organoaluminum Lewis Acids
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2410
_journal_page_last               2411
_journal_paper_doi               10.1021/ja063051q
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C42 H23 F12 N O3 S '
_chemical_formula_sum            'C42 H23 F12 N O3 S'
_chemical_formula_weight         849.69
_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                 103.364(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.029(4)
_cell_length_b                   13.029(3)
_cell_length_c                   17.866(6)
_cell_measurement_reflns_used    32806
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3630.1(17)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16618
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             1720.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.80
_refine_ls_extinction_coef       976(69)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.326
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     1122
_refine_ls_number_reflns         15200
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.0036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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_cod_data_source_block           '_ohmatsu'
_cod_original_formula_sum        'C42 H23 F12 N O3 S '
_cod_database_code               4109130