Planar chiral [2.2]paracyclophane-based bis(thiourea) catalyst: application to asymmetric Henry reaction
Shinji Kitagaki; Takahiro Ueda; Chisato Mukai; Chem.Commun. 49 (2013) 4030–; doi:10.1039/c3cc41789a

data_7109175
_publ_section_title
;
 Planar chiral [2.2]paracyclophane-based bis(thiourea) catalyst:
 application to asymmetric Henry reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              4030
_journal_paper_doi               10.1039/c3cc41789a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C46 H48 F12 N4 O3 S2'
_chemical_formula_sum            'C46 H48 F12 N4 O3 S2'
_chemical_formula_weight         997.01
_chemical_melting_point          402
_chemical_name_systematic
4,12-Bis{N?-[3,5-bis(trifluoromethyl)phenyl]thioureido}[2.2]paracyclophane
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 108.682(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.5099(12)
_cell_length_b                   15.3119(11)
_cell_length_c                   23.0134(18)
_cell_measurement_reflns_used    17339
_cell_measurement_temperature    243
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      3.02
_cell_volume                     4843.6(7)
_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    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      243
_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_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41855
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_source_type              'Rigaku R-AXIS RAPID II'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2064.00
_exptl_crystal_recrystallization_method THF-hexane
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.686
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.324
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     660
_refine_ls_number_reflns         10947
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0014Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2481
_reflns_number_gt                4429
_reflns_number_total             10947
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3cc41789a.txt
_cod_data_source_block           seimitsu62-2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7109175