2-(4-Methoxybenzylidene)-2<i>H</i>-1,3-benzodithiole 1,1,3,3-tetraoxide
Asahara, Haruyasu; Mayer, Peter; Mayr, Herbert; Acta Crystallographica Section E 68 (2012) o567–; doi:10.1107/S1600536812002826

data_2233918
_publ_section_title
;
 2-(4-Methoxybenzylidene)-2<i>H</i>-1,3-benzodithiole 1,1,3,3-tetraoxide
;
_journal_coeditor_code           LD2042
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o567
_journal_paper_doi               10.1107/S1600536812002826
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C15 H12 O5 S2'
_chemical_formula_moiety         'C15 H12 O5 S2'
_chemical_formula_sum            'C15 H12 O5 S2'
_chemical_formula_weight         336.385
_chemical_name_systematic
;
2-(4-Methoxybenzylidene)-2<i>H</i>-1,3-benzodithiole 1,1,3,3-tetraoxide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                84.345(2)
_cell_angle_beta                 84.631(2)
_cell_angle_gamma                71.711(2)
_cell_formula_units_Z            4
_cell_length_a                   7.3649(2)
_cell_length_b                   11.4723(3)
_cell_length_c                   17.6114(5)
_cell_measurement_reflns_used    5056
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      3.134
_cell_volume                     1402.89(7)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 2004)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and OLEX2 (Dolomanov <i>et al.</i>,
2004)
;
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_radiation_monochromator  'MONTEL, graded multilayered X-ray optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9496
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.59268(8)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0250P)^2^+1.7791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                4435
_reflns_number_total             5124
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ld2042.cif
_cod_data_source_block           I
_cod_database_code               2233918
_cod_database_fobs_code          2233918