Enantioselective trapping of phosphoramidate ammonium ylides with imino esters for synthesis of 2,3-diaminosuccinic acid derivatives
Jun Jiang; Xiaochu Ma; Shunying Liu; Yu Qian; Fengping Lv; Lin Qiu; Xiang Wu; Wenhao Hu; Chem.Commun. 49 (2013) 4238–; doi:10.1039/c3cc36972b

data_7109241
_publ_section_title
;
 Enantioselective trapping of phosphoramidate ammonium ylides with imino
 esters for synthesis of 2,3-diaminosuccinic acid derivatives
;
_journal_name_full               Chem.Commun.
_journal_page_first              4238
_journal_paper_doi               10.1039/c3cc36972b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C35 H38 Br N2 O8 P'
_chemical_formula_weight         725.55
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 116.6200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9476(6)
_cell_length_b                   14.5627(5)
_cell_length_c                   15.6857(5)
_cell_measurement_temperature    296(2)
_cell_volume                     3460.9(2)
_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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39890
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_correction_T_min  0.8109
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.826
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0752
_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^)+(0.0889P)^2^+8.8222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2318
_reflns_number_gt                3424
_reflns_number_total             6095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc36972b.txt
_cod_data_source_block           z
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7109241