Organocatalytic Asymmetric Conjugate Addition and Cascade Acyl Transfer Reaction of α-Nitroketones
Rui-jiong Lu; Yun-yun Yan; Jin-jia Wang; Quan-sheng Du; Shao-zhen Nie; Ming Yan; Journal of Organic Chemistry 76 (2011) 6230–6239; doi:10.1021/jo2009752

data_4026491
_publ_section_title
;
 Organocatalytic Asymmetric Conjugate Addition and Cascade Acyl Transfer
 Reaction of \a-Nitroketones
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6230
_journal_page_last               6239
_journal_paper_doi               10.1021/jo2009752
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C19 H16 Cl N O6'
_chemical_formula_weight         389.78
_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                 102.5386(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.39286(12)
_cell_length_b                   7.87082(8)
_cell_length_c                   12.69168(17)
_cell_measurement_temperature    104(2)
_cell_volume                     915.91(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      104(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17793
_diffrn_reflns_theta_full        71.39
_diffrn_reflns_theta_max         71.39
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    2.174
_exptl_absorpt_correction_T_max  0.8991
_exptl_absorpt_correction_T_min  0.4768
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3547
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0397P)^2^+0.1574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                3463
_reflns_number_total             3547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2009752_si_001.cif
_cod_data_source_block           lyj_101216_2
_cod_database_code               4026491