Electroreductive Intramolecular Coupling of Chiral α-Imino Esters: Stereoselective Synthesis of Mixed Ketals of cis-2,4-Disubstituted Azetidine-3-ones
Naoki Kise; Hiroshi Ozaki; Noriaki Moriyama; Yasuo Kitagishi; Nasuo Ueda; Journal of the American Chemical Society 125 (2003) 11591–11596; doi:10.1021/ja036975b

data_4114203
_publ_section_title
;
 Electroreductive Intramolecular Coupling of Chiral \a-Imino Esters:
 Stereoselective Synthesis of Mixed Ketals of cis-2,4-Disubstituted
 Azetidine-3-ones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11591
_journal_page_last               11596
_journal_paper_doi               10.1021/ja036975b
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C26 H37 N O3 Si '
_chemical_formula_sum            'C26 H37 N O3 Si'
_chemical_formula_weight         439.67
_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
_cell_angle_beta                 95.347(2)
_cell_angle_gamma                90
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_cell_length_b                   9.6213(1)
_cell_length_c                   13.4593(5)
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_cell_measurement_temperature    296.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.0
_cell_volume                     1339.69(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 2.00'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9979
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12456
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.784
_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    1.090
_exptl_crystal_description       block
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.11
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5876
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.006Fo^2^ + 1.000\s^2^(Fo)]/(4Fo^2^)'
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_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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_cod_data_source_block           '_NK020815_________________'
_cod_original_cell_volume        1339.69(3)
_cod_original_formula_sum        'C26 H37 N O3 Si '
_cod_database_code               4114203