Diastereo- and enantioselective conjugate addition of a-substituted nitroacetates to maleimides under base-free neutral phase-transfer conditions
Seiji Shirakawa; Shogo J. Terao; Rongjun He; Keiji Maruoka; Chem.Commun. 47 (2011) 10557–; doi:10.1039/c1cc14043d

data_7106878
_publ_section_title
;
 Diastereo- and enantioselective conjugate addition of a-substituted
 nitroacetates to maleimides under base-free neutral phase-transfer
 conditions
;
_journal_name_full               Chem.Commun.
_journal_page_first              10557
_journal_paper_doi               10.1039/c1cc14043d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C22 H21 Br N2 O6 '
_chemical_formula_sum            'C22 H21 Br N2 O6'
_chemical_formula_weight         489.32
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.21622(15)
_cell_length_b                   14.1578(3)
_cell_length_c                   24.7401(7)
_cell_measurement_reflns_used    12318
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.1
_cell_volume                     2177.33(9)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 5.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.121
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21656
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_exptl_absorpt_coefficient_mu    2.936
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1000.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.41
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1671 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3992
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                3609
_reflns_number_total             3992
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c1cc14043d.txt
_cod_data_source_block           '_0731'
_cod_original_cell_volume        2177.32(9)
_cod_original_formula_sum        'C22 H21 Br N2 O6 '
_cod_database_code               7106878