New, General, and Stereoselective Synthesis of CF3-Containing Tri- and Tetrasubstituted Oxiranes and Tetrasubstituted Alkenes
Masaki Shimizu; Takuya Fujimoto; Hiroshi Minezaki; Takeshi Hata; Tamejiro Hiyama; Journal of the American Chemical Society 123 (2001) 6947–6948; doi:10.1021/ja016077k

data_4115620
_publ_contact_author             'Masaki Shimizu'
_publ_contact_author_email       shimizu@npc05.kuic.Kyoto-u.ac.jp
_publ_contact_author_fax         +81-75-753-5555
_publ_contact_author_phone       +81-75-753-5535
_publ_section_title
;
 New, General, and Stereoselective Synthesis of CF3-Containing Tri- and
 Tetrasubstituted Oxiranes and Tetrasubstituted Alkenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6947
_journal_page_last               6948
_journal_paper_doi               10.1021/ja016077k
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C21 H19 F3'
_chemical_formula_weight         328.36
_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                 104.289(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.9675(5)
_cell_length_b                   17.1070(13)
_cell_length_c                   9.1531(7)
_cell_measurement_reflns_used    2946
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.6795
_cell_measurement_theta_min      2.5865
_cell_volume                     905.50(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7275
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        -0.05
_diffrn_standards_interval_time  583
_diffrn_standards_number         99
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.971871
_exptl_absorpt_correction_T_min  0.294928
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       prism
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(11)
_refine_ls_extinction_coef       0.023(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3497
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2127
_reflns_number_gt                2351
_reflns_number_total             3497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016077k_s2_3.cif
_cod_data_source_block           4b
_cod_database_code               4115620