Crystal structure of ethylenedioxytetrathiafulvalene-4,5-bis(thiolbenzoic acid) 0.25-hydrate
Zhang, Yuanyuan; He, Qiqian; Bao, Huijie; Wang, Lejia; Xiao, Xunwen; Acta Crystallographica Section E 73 (2017) 1275–1278; doi:10.1107/S2056989017011070

data_2242269
_publ_section_title
;
 Crystal structure of ethylenedioxytetrathiafulvalene-4,5-bis(thiolbenzoic
 acid) 0.25-hydrate
;
_journal_coeditor_code           IS5477
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1275
_journal_page_last               1278
_journal_paper_doi               10.1107/S2056989017011070
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C22 H14 O6 S6, 0.25H2 O'
_chemical_formula_moiety         'C22 H14 O6 S6, 0.25(H2 O)'
_chemical_formula_sum            'C22 H14.5 O6.25 S6'
_chemical_formula_weight         571.19
_chemical_name_systematic
'4,4'-{[2-(5,6-Dihydro-[1,3]dithiolo[4,5-<i>b</i>][1,4]dioxin-2-ylidene)-1,3-dithiole-4,5-diyl]bis(sulfanediyl)}dibenzoic acid 0.25-hydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.970(4)
_cell_angle_beta                 92.039(4)
_cell_angle_gamma                110.902(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6995(6)
_cell_length_b                   9.2634(8)
_cell_length_c                   17.9198(14)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.58
_cell_volume                     1192.64(17)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40263
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.597
_diffrn_reflns_theta_min         2.583
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  .91
_exptl_absorpt_correction_T_min  .85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             585
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .16
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5496
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.3142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                4411
_reflns_number_total             5496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5477sup1.cif
_cod_data_source_block           I
_cod_database_code               2242269
_cod_database_fobs_code          2242269
_shelx_hkl_checksum              69279
_shelx_res_checksum              80027