Polyhalogenated BEDT-TTF through chlorination (SO2Cl2, Cl2) and fluorination (®Selectfluor, XeF2) of 5,6-dihydro[1,3]dithiolo[4,5-b][1,4]dithiin-2-one
Olivier J. Dautel; Marc Fourmigué; J. Chem. Soc., Perkin Trans. 1  (2001) 3399–3402; doi:10.1039/b106144p

data_7204211
_publ_section_title
;
 Polyhalogenated BEDT-TTF through chlorination (SO2Cl2, Cl2) and
 fluorination (&#x00AE;Selectfluor, XeF2) of
 5,6-dihydro[1,3]dithiolo[4,5-b][1,4]dithiin-2-one
;
_journal_issue                   24
_journal_name_full               'J. Chem. Soc., Perkin Trans. 1'
_journal_page_first              3399
_journal_page_last               3402
_journal_paper_doi               10.1039/b106144p
_journal_year                    2001
_chemical_formula_sum            'C5 H Cl5 O S4'
_chemical_formula_weight         382.55
_chemical_name_systematic
; 
3a,5,5,6,7a-pentachloro-tetrahydro(1,3)dithiolo(4,5-b)(1,4)dithiin-2-one 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5432(13)
_cell_length_b                   16.283(3)
_cell_length_c                   11.420(2)
_cell_measurement_reflns_used    5929
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      2.5
_cell_volume                     1212.4(4)
_computing_cell_refinement       'SELECT, CELL, Stoe-IPDS'
_computing_data_collection       'EXPOSE, Stoe-IPDS'
_computing_data_reduction        'INTEGRATE, Stoe-IPDS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       'oscillation, phi incr. 1.4 deg.'
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9445
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  0.9228
_exptl_absorpt_correction_T_min  0.6714
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                1493
_reflns_number_total             2315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106144p.txt
_cod_data_source_block           dop195mer
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7204211