A Dual Arylboronic Acid-Aminothiourea Catalytic System for the Asymmetric Intramolecular Hetero-Michael Reaction of α,β-Unsaturated Carboxylic Acids.
Azuma, Takumi; Murata, Akihiro; Kobayashi, Yusuke; Inokuma, Tsubasa; Takemoto, Yoshiji; Organic letters 16 (2014) 4256–4259; doi:10.1021/ol501954r

data_1517247
_publ_section_title
;
 A Dual Arylboronic Acid-Aminothiourea Catalytic System for the Asymmetric
 Intramolecular Hetero-Michael Reaction of \a,\b-Unsaturated Carboxylic
 Acids.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4256
_journal_page_last               4259
_journal_paper_doi               10.1021/ol501954r
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C21 H23 N O4'
_chemical_formula_sum            'C21 H23 N O4'
_chemical_formula_weight         353.42
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.6158(17)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   9.6514(5)
_cell_length_b                   13.5727(8)
_cell_length_c                   28.8023(14)
_cell_measurement_reflns_used    21653
_cell_measurement_temperature    296
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      3.00
_cell_volume                     3720.0(3)
_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  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29637
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.300
_refine_diff_density_min         -1.190
_refine_ls_extinction_coef       160(29)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         13361
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.065
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                8756
_reflns_number_total             13361
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol501954r_si_002.cif
_cod_data_source_block           azuma140510
_cod_depositor_comments          'Adding full bibliography for 1517247.cif.'
_cod_original_cell_volume        3720.0(4)
_cod_database_code               1517247