Enantiomerically Puretrans-β-Lactams from α-Amino Acids via Compact Fluorescent Light (CFL) Continuous-Flow Photolysis
Yvette S. Mimieux Vaske; Maximillian E. Mahoney; Joseph P. Konopelski; David L. Rogow; William J. McDonald; Journal of the American Chemical Society 132 (2010) 11379–11385; doi:10.1021/ja1050023

data_4102843
_publ_contact_author_address     '379A PSB'
_publ_contact_author_email       mimieux@chemistry
_publ_contact_author_name        'Yvette Mimieux-Vaske'
_publ_contact_author_phone       9-5056
_publ_section_title
;
 Enantiomerically Puretrans-\b-Lactams from \a-Amino Acids via Compact
 Fluorescent Light (CFL) Continuous-Flow Photolysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11379
_journal_page_last               11385
_journal_paper_doi               10.1021/ja1050023
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C33 H31 N2 O4'
_chemical_formula_weight         519.60
_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                 92.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.510(3)
_cell_length_b                   11.941(6)
_cell_length_c                   23.992(8)
_cell_measurement_reflns_used    3164
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      42.341
_cell_measurement_theta_min      4.814
_cell_volume                     2722.6(19)
_computing_cell_refinement       'Bruker SAINT v7.34'
_computing_data_collection       'Bruker APEX-II v2.1-4'
_computing_data_reduction        'Bruker SAINT v7.34'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       \w/2\q-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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23617
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6733
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular blocks'
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         9242
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0403P)^2^+0.0553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                6933
_reflns_number_total             9242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1050023_si_003.cif
_cod_data_source_block           xsc09005
_cod_original_cell_volume        2722.8(18)
_cod_database_code               4102843