Direct Generation of Ti-Enolate of α-CF3 Ketone: Theoretical Study and High-Yielding and Diastereoselective Aldol Reaction
Yoshimitsu Itoh; Masahiro Yamanaka; Koichi Mikami; Journal of the American Chemical Society 126 (2004) 13174–13175; doi:10.1021/ja046518a

data_4113060
_publ_section_title
;
 Direct Generation of Ti-Enolate of \a-CF3 Ketone: Theoretical Study and
 High-Yielding and Diastereoselective Aldol Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13174
_journal_page_last               13175
_journal_paper_doi               10.1021/ja046518a
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C20 H21 F3 O2 '
_chemical_formula_sum            'C20 H21 F3 O2'
_chemical_formula_weight         350.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                73.90(2)
_cell_angle_beta                 88.25(3)
_cell_angle_gamma                76.29(2)
_cell_formula_units_Z            2
_cell_length_a                   6.469(4)
_cell_length_b                   10.934(6)
_cell_length_c                   13.371(9)
_cell_measurement_reflns_used    3337
_cell_measurement_temperature    193.1
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.9
_cell_volume                     882.1(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 3.16'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.6070
_diffrn_measured_fraction_theta_max 0.6070
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3713
_diffrn_reflns_theta_full        31.20
_diffrn_reflns_theta_max         31.20
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             368.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3486
_refine_ls_R_factor_gt           0.0960
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0000Fo^2^ + 2.0000\s^2^(Fo) + 0.9800]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1620
_reflns_number_gt                3479
_reflns_number_total             3486
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja046518asi20040612_075431.cif
_cod_data_source_block
'__5-Hydroxy-2,2-dimethyl-1,5-diphenyl-4-trifluoromethyl-3-pentanone'
_cod_original_cell_volume        882.2(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C20 H21 F3 O2 '
_cod_database_code               4113060