A convenient stereoselective synthesis of trifluoromethyl-substituted polyfunctionalized cyclopropane: synthesis of (±)-trans-trifluoronorcoronamic acid
Jiang, Biao; Zhang, Fangjiang; Xiong, Wennan; Chemical Communications (Cambridge, United Kingdom)  (2003) 536–537; doi:10.1039/b210642f

data_7113541
_publ_section_title
;
 A convenient stereoselective synthesis of trifluoromethyl-substituted
 polyfunctionalized cyclopropane: synthesis of
 (+-)-trans-trifluoronorcoronamic acid
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   4
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              536
_journal_page_last               537
_journal_paper_doi               10.1039/b210642f
_journal_year                    2003
_chemical_formula_sum            'C11 H8 F3 N O2 S'
_chemical_formula_weight         275.24
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 118.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.596(8)
_cell_length_b                   5.881(3)
_cell_length_c                   20.446(7)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      18.4
_cell_volume                     2386.6(18)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  afc7r
_diffrn_measurement_method       'omega/2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_sigmaI/netI    0.0942
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2074
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.27
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  -0.01
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8567
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0032(7)
_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   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+1.8652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                1657
_reflns_number_total             2030
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103976
_cod_data_source_file            b210642f.txt
_cod_data_source_block           shelxs
_cod_original_cell_volume        2386.7(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7113541