Enantioselective synthesis of 4-aminopyrrolidine-2,4-dicarboxylate derivatives via Ag-catalyzed cycloaddition of azomethine ylides with alkylidene azlactones
Maria Gonzalez-Esguevillas; Javier Adrio; Juan C. Carretero; Chem.Commun. 49 (2013) 4649–; doi:10.1039/c3cc41663a

data_7109275
_publ_section_title
;
 Enantioselective synthesis of 4-aminopyrrolidine-2,4-dicarboxylate
 derivatives via Ag-catalyzed cycloaddition of azomethine ylides with
 alkylidene azlactones
;
_journal_name_full               Chem.Commun.
_journal_page_first              4649
_journal_paper_doi               10.1039/c3cc41663a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C27 H25 Br N2 O5'
_chemical_formula_weight         537.40
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.0310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7611(2)
_cell_length_b                   9.9993(2)
_cell_length_c                   25.5619(6)
_cell_measurement_temperature    296(2)
_cell_volume                     2491.46(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41585
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  0.7074
_exptl_absorpt_correction_T_min  0.6490
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                3231
_reflns_number_total             5421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc41663a.txt
_cod_data_source_block           datos_0m
_cod_database_code               7109275