Catalytic Enantioselective Synthesis of α,β-Diamino Acid Derivatives
Le Li; Madhu Ganesh; Daniel Seidel; Journal of the American Chemical Society 131 (2009) 11648–11649; doi:10.1021/ja9034494

data_4104895
_publ_section_title
;
 Catalytic Enantioselective Synthesis of \a,\b-Diamino Acid Derivatives
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11648
_journal_page_last               11649
_journal_paper_doi               10.1021/ja9034494
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         '(C21 H19 N3 O5 S2), 0.75(C H2 CL2)'
_chemical_formula_sum            'C21.75 H20.5 Cl1.5 N3 O5 S2'
_chemical_formula_weight         521.21
_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                 100.941(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.5766(5)
_cell_length_b                   7.3289(3)
_cell_length_c                   14.2420(7)
_cell_measurement_reflns_used    7265
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.64
_cell_measurement_theta_min      2.91
_cell_volume                     1186.38(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w 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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14297
_diffrn_reflns_theta_full        30.67
_diffrn_reflns_theta_max         30.67
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       rod
_exptl_crystal_F_000             539
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(6)
_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     385
_refine_ls_number_reflns         7153
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                6443
_reflns_number_total             7153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9034494_si_002.cif
_cod_data_source_block           cinnamyl
_cod_original_formula_sum        'C21.75 H20.50 Cl1.50 N3 O5 S2'
_cod_database_code               4104895