Epimerization of diastereomeric alpha-amino nitriles to single stereoisomers in the solid state.
Sakurai, Rumiko; Suzuki, Shuji; Hashimoto, Junichi; Baba, Manabu; Itoh, Osamu; Uchida, Akira; Hattori, Tetsutaro; Miyano, Sotaro; Yamaura, Masanori; Organic letters 6 (2004) 2241–2244; doi:10.1021/ol049256q

data_1507083
_publ_section_title
;
 Epimerization of diastereomeric alpha-amino nitriles to single
 stereoisomers in the solid state.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              2241
_journal_page_last               2244
_journal_paper_doi               10.1021/ol049256q
_journal_volume                  6
_journal_year                    2004
_chemical_formula_moiety         'C17 H16 N2 O'
_chemical_formula_sum            'C17 H16 N2 O'
_chemical_formula_weight         264.32
_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                 109.070(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9347(14)
_cell_length_b                   5.099(3)
_cell_length_c                   13.547(2)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      10.78
_cell_volume                     713.9(4)
_computing_cell_refinement
; 
MSC/AFC Diffractometer Control Software 
;
_computing_data_collection
;MSC/AFC Diffractometer Control Software 
(Molecular Structure Corporation, 1996) 
;
_computing_data_reduction
'TEXSAN     (Molecular Structure Corporation, 2000)'
_computing_molecular_graphics
'PLATON (Spek, 2001) and ORTEPIII (Burnett et al., 1996)'
_computing_publication_material  'SHELXL97, PLATON and PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1952
_diffrn_reflns_theta_full        75.04
_diffrn_reflns_theta_max         75.04
_diffrn_reflns_theta_min         3.45
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.133
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(9)
_refine_ls_extinction_coef       0.0083(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         1614
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.1347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                930
_reflns_number_total             1614
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ol049256qsi20040422_101348.cif
_cod_data_source_block           R-1a
_cod_original_cell_volume        713.8(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1507083