Catalytic Asymmetric [4 + 2] Cycloadditions and Hosomi-Sakurai Reactions of α-Alkylidene β-Keto Imides.
Orimoto, Kohei; Oyama, Harufumi; Namera, Yuki; Niwa, Takashi; Nakada, Masahisa; Organic letters 15 (2013) 768–771; doi:10.1021/ol303381c

data_1508933
_publ_section_title
;
 Catalytic Asymmetric [4 + 2] Cycloadditions and Hosomi-Sakurai Reactions
 of \a-Alkylidene \b-Keto Imides.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              768
_journal_page_last               771
_journal_paper_doi               10.1021/ol303381c
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C9 H12 N2 O4'
_chemical_formula_sum            'C9 H12 N2 O4'
_chemical_formula_weight         212.20
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.8985(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.7215(3)
_cell_length_b                   7.90305(19)
_cell_length_c                   16.5104(4)
_cell_measurement_reflns_used    9420
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.21
_cell_measurement_theta_min      5.47
_cell_volume                     985.87(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9872
_diffrn_reflns_theta_full        68.21
_diffrn_reflns_theta_max         68.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.560
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448.00
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.600
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     144
_refine_ls_number_reflns         1792
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0795P)^2^+0.3987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1430
_reflns_number_gt                1608
_reflns_number_total             1792
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol303381c_si_002.cif
_cod_data_source_block           2012-6-6-imide
_cod_database_code               1508933