Unfunctionalized, α-Epimerizable Nonracemic Ketones and Aldehydes Can Be Accessed by Crystallization-Induced Dynamic Resolution of Imines
Janez Košmrlj; Leland O. Weigel; David A. Evans; C. Wade Downey; Jimmy Wu; Journal of the American Chemical Society 125 (2003) 3208–3209; doi:10.1021/ja029715n

data_4113569
_publ_section_title
;
 Unfunctionalized, \a-Epimerizable Nonracemic Ketones and Aldehydes Can Be
 Accessed by Crystallization-Induced Dynamic Resolution of Imines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3208
_journal_page_last               3209
_journal_paper_doi               10.1021/ja029715n
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C17 H24 N2 O3'
_chemical_formula_weight         304.38
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.7719(12)
_cell_length_b                   12.980(3)
_cell_length_c                   27.034(6)
_cell_measurement_temperature    213(2)
_cell_volume                     1674.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.1357
_diffrn_reflns_av_sigmaI/netI    0.1611
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6960
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.083
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_F_000             656
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2093
_reflns_number_gt                2890
_reflns_number_total             3925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029715nsi20030122_022156.cif
_cod_data_source_block           jwu33t
_cod_database_code               4113569