Mechanism of Preferential Enrichment, an Unusual Enantiomeric Resolution Phenomenon Caused by Polymorphic Transition during Crystallization of Mixed Crystals Composed of Two Enantiomers
Rui Tamura; Daisuke Fujimoto; Zsolt Lepp; Kentaro Misaki; Hideyuki Miura; Hiroki Takahashi; Takanori Ushio; Tadashi Nakai; Ken Hirotsu; Journal of the American Chemical Society 124 (2002) 13139–13153; doi:10.1021/ja020454r

data_4115235
_publ_section_title
;
 Mechanism of Preferential Enrichment, an Unusual Enantiomeric Resolution
 Phenomenon Caused by Polymorphic Transition during Crystallization of
 Mixed Crystals Composed of Two Enantiomers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13139
_journal_page_last               13153
_journal_paper_doi               10.1021/ja020454r
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C23 H33 N3 O9 S'
_chemical_formula_weight         527.59
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Wed Jul 14 20:00:46 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                96.52(5)
_cell_angle_beta                 92.57(4)
_cell_angle_gamma                107.19(2)
_cell_formula_units_Z            2
_cell_length_a                   9.852(2)
_cell_length_b                   15.148(4)
_cell_length_c                   9.040(9)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      29.4
_cell_volume                     1276.1(14)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.09232
_diffrn_orient_matrix_UB_12      0.01422
_diffrn_orient_matrix_UB_13      0.00966
_diffrn_orient_matrix_UB_21      -0.05149
_diffrn_orient_matrix_UB_22      -0.06813
_diffrn_orient_matrix_UB_23      -0.00657
_diffrn_orient_matrix_UB_31      0.01383
_diffrn_orient_matrix_UB_32      0.00405
_diffrn_orient_matrix_UB_33      0.11111
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4039
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.01
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        -0.86
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.618
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             560.00
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.878
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.0230
_refine_ls_shift/su_mean         0.0050
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00360|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                3242
_reflns_number_total             3780
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            ja020454r_1.cif
_cod_data_source_block           NNMe3
_cod_original_cell_volume        1276(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C23 H33 N3 O9 S '
_cod_database_code               4115235