Palladium-catalyzed asymmetric synthesis of 2-pyrrolidinones with a quaternary carbon stereocenter
Ryo Shintani; Tomoaki Ito; Midori Nagamoto; Haruka Otomo; Tamio Hayashi; Chem.Commun. 48 (2012) 9936–; doi:10.1039/c2cc35259a

data_7108399
_publ_section_title
;
 Palladium-catalyzed asymmetric synthesis of 2-pyrrolidinones with a
 quaternary carbon stereocenter
;
_journal_name_full               Chem.Commun.
_journal_page_first              9936
_journal_paper_doi               10.1039/c2cc35259a
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C19 H24 Cl N O3 '
_chemical_formula_sum            'C19 H24 Cl N O3'
_chemical_formula_weight         349.86
_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                 104.9876(14)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   8.71555(18)
_cell_length_b                   8.71796(19)
_cell_length_c                   12.4456(3)
_cell_measurement_reflns_used    9073
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.7
_cell_volume                     913.47(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.057
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9740
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  0.673
_exptl_absorpt_correction_T_min  0.564
_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    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             372.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1446 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.040(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3224
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.0040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.0256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                2892
_reflns_number_total             3224
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2cc35259a.txt
_cod_data_source_block           '_20623yuki'
_cod_original_cell_volume        913.47(3)
_cod_original_formula_sum        'C19 H24 Cl N O3 '
_cod_database_code               7108399