2-Methylsulfanyl-5,6-dihydro-2<i>H</i>-1,3-dithiolo[4,5-<i>b</i>][1,4]dioxin-2-ium tetrafluoroborate
Zhou, Guoquan; Chen, Xinzhi; Acta Crystallographica Section E 68 (2012) o949–; doi:10.1107/S1600536812005326

data_2234371
_publ_section_title
;
 2-Methylsulfanyl-5,6-dihydro-2<i>H</i>-1,3-dithiolo[4,5-<i>b</i>][1,4]dioxin-2-ium
 tetrafluoroborate
;
_journal_coeditor_code           RK2328
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o949
_journal_paper_doi               10.1107/S1600536812005326
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C6 H7 O2 S3 +, B F4 -'
_chemical_formula_moiety         'C6 H7 O2 S3 +, B F4 -'
_chemical_formula_sum            'C6 H7 B F4 O2 S3'
_chemical_formula_weight         294.14
_chemical_name_systematic
;
2-Methylsulfanyl-5,6-dihydro-2<i>H</i>-1,3-dithiolo[4,5-<i>b</i>][1,4]dioxin-
2-ium tetrafluoroborate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.488(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7410(13)
_cell_length_b                   10.1175(10)
_cell_length_c                   10.1874(11)
_cell_measurement_reflns_used    2895
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     1103.7(2)
_computing_cell_refinement       '<i>CrystalClear</i> (Rigaku, 2005)'
_computing_data_collection       '<i>CrystalClear</i> (Rigaku, 2005)'
_computing_data_reduction        '<i>CrystalStructure</i> (Rigaku/MSC, 2005)'
_computing_molecular_graphics    '<i>SHELXTL</i>  (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i>  (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6014
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>REQAB</i>; Jacobson, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.545
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2046
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+1.5661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1743
_reflns_number_gt                1749
_reflns_number_total             2046
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2328.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2234371
_cod_database_fobs_code          2234371