Chiral Discrimination of Cryptochiral Saturated Quaternary and Tertiary Hydrocarbons by Asymmetric Autocatalysis
Tsuneomi Kawasaki; Hiroyuki Tanaka; Takashi Tsutsumi; Toshinari Kasahara; Itaru Sato; Kenso Soai; Journal of the American Chemical Society 128 (2006) 6032–6033; doi:10.1021/ja061429e

data_4110598
_publ_section_title
;
 Chiral Discrimination of Cryptochiral Saturated Quaternary and Tertiary
 Hydrocarbons by Asymmetric Autocatalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6032
_journal_page_last               6033
_journal_paper_doi               10.1021/ja061429e
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C22 H24 N4 O4 S2'
_chemical_formula_sum            'C22 H24 N4 O4 S2'
_chemical_formula_weight         472.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0187(5)
_cell_length_b                   23.4465(14)
_cell_length_c                   12.3357(7)
_cell_measurement_reflns_used    4169
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.48
_cell_measurement_theta_min      2.40
_cell_volume                     2313.4(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_sigmaI/netI    0.0906
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15704
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_correction_T_min  0.9079
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         7635
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                5045
_reflns_number_total             7635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061429esi20060301_082218.cif
_cod_data_source_block           hyd3
_cod_database_code               4110598