Construction of Chiral α-Amino Quaternary Stereogenic Centers via Phase-Transfer Catalyzed Enantioselective α-Alkylation of α-Amidomalonates.
Ha, Min Woo; Lee, Myungmo; Choi, Sujee; Kim, Seek; Hong, Suckchang; Park, Yohan; Kim, Mi-Hyun; Kim, Taek-Soo; Lee, Jihoon; Lee, Jae Kyun; Park, Hyeung-Geun; The Journal of organic chemistry 80 (2015) 3270–3279; doi:10.1021/jo502791d

data_4030725
_publ_section_title
;
 Construction of Chiral \a-Amino Quaternary Stereogenic Centers via
 Phase-Transfer Catalyzed Enantioselective \a-Alkylation of
 \a-Amidomalonates.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3270
_journal_page_last               3279
_journal_paper_doi               10.1021/jo502791d
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C24 H30 N2 O4'
_chemical_formula_sum            'C24 H30 N2 O4'
_chemical_formula_weight         410.51
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.0770(5)
_cell_length_b                   10.5732(8)
_cell_length_c                   26.8277(18)
_cell_measurement_reflns_used    13087
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.04
_cell_volume                     2291.1(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22473
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5211
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0635P)^2^+0.0490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                3014
_reflns_number_total             5211
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo502791d_si_002.cif
_cod_data_source_block           1413c
_cod_depositor_comments          'Adding full bibliography for 4030725.cif.'
_cod_database_code               4030725