Synthesis of 1,2,2-trifluorovinyl sulphides and selenides from trifluorovinylation of organic thiocyanates and selenocyanates
Zhang, Yunxiao; Wu, Dongping; Weng, Zhiqiang; Organic Chemistry Frontiers 4 (2017) 2226–; doi:10.1039/C7QO00595D

data_1553847
_publ_section_title
;
 Synthesis of 1,2,2-trifluorovinyl sulphides and selenides from
 trifluorovinylation of organic thiocyanates and selenocyanates
;
_journal_issue                   11
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              2226
_journal_paper_doi               10.1039/C7QO00595D
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C8 H6 Br F3 O S'
_chemical_formula_weight         287.10
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-06-09 deposited with the CCDC.
2017-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.906(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.993(7)
_cell_length_b                   3.9406(12)
_cell_length_c                   12.147(4)
_cell_measurement_temperature    296(2)
_cell_volume                     999.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0642
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3253
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    4.328
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+1.0967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                1426
_reflns_number_total             1736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7qo00595d2.cif
_cod_data_source_block           P21_c
_cod_original_cell_volume        999.5(5)
_cod_database_code               1553847