An enantiomerically pure 4-oxo-α-amino acid derivative
Clegg, William; Jackson, Richard F.W.; O'Neil, Paul A.; Wishart, Neil; Acta Crystallographica Section C 50 (1994) 965–967; doi:10.1107/S0108270194000041

data_2009776
_publ_section_title
;
 An enantiomerically pure 4-oxo-\a-amino acid derivative
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              965
_journal_page_last               967
_journal_paper_doi               10.1107/S0108270194000041
_journal_volume                  50
_journal_year                    1994
_chemical_formula_sum            'C24 H27 N O5'
_chemical_formula_weight         409.47
_chemical_name_systematic
'benzyl 2(S)-[(tert-butoxycarbonyl)amino]-4-oxo-6-phenyl-(E)-hex-5-enoate'
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 112.88(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.322(4)
_cell_length_b                   5.367(2)
_cell_length_c                   16.266(5)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    160.0(10)
_cell_measurement_theta_max      12.43
_cell_measurement_theta_min      10.81
_cell_volume                     1071.5(6)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL93 and local programs'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      160.0(10)
_diffrn_measurement_device       'Stoe-Siemens diffractometer'
_diffrn_measurement_method
'\w/\q scans with on-line profile fitting (Clegg, 1981)'
_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  '0.0968 (on F^2^)'
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4308
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        15
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.158
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.8(11)
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_obs          0.0341
_refine_ls_shift/esd_max         <0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[s^2^(Fo^2^) + (0.0383P)^2^ + 0.2454P] where P = (Fo^2^ +
 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0924
_refine_ls_wR_factor_obs         0.0822
_reflns_number_observed          2635
_reflns_number_total             3144
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ha1079.cif
_cod_data_source_block           rfwj30
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2009776