Structures of tetrathiabenzoquinone derivatives and the order–disorder phase transition
Matsumoto, Shinya; Mizuguchi, Jin; Acta Crystallographica Section B 57 (2001) 82–87; doi:10.1107/S0108768100014087

data_2103572
_publ_section_title
;
 Structures of tetrathiabenzoquinone derivatives and the
 order--disorder phase transition
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              82
_journal_page_last               87
_journal_paper_doi               10.1107/S0108768100014087
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C12 H12 O2 S4 '
_chemical_formula_sum            'C12 H12 O2 S4'
_chemical_formula_weight         316.47
_chemical_name_systematic
;
3,4,9,10-tetrahydro-2H,8H-benzo[1,2-b:4,5-b']bis[1,4] dithiepin-6,12-dione
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.758(2)
_cell_length_b                   16.846(2)
_cell_length_c                   7.981(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.7
_cell_volume                     1311.9(5)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    'ORTEP II(Johnson, 1976)'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'SIR92(Altomare et al, 1994)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .7107
_diffrn_reflns_av_R_equivalents  .000
_diffrn_reflns_av_sigmaI/netI    .026
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1510
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        -.13
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .713
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  .836
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             656.00
_exptl_crystal_size_max          .800
_exptl_crystal_size_mid          .300
_exptl_crystal_size_min          .150
_refine_diff_density_max         .35
_refine_diff_density_min         -.28
_refine_ls_extinction_coef       .027(5)
_refine_ls_extinction_method
;
Zachariasen(1967) type 2 Gaussian isotropic
;
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .0377
_refine_ls_R_factor_gt           .0377
_refine_ls_shift/su_max          .0338
_refine_ls_shift/su_mean         .0023
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
w = 1/[\s^2^(Fo) + 0.00346|Fo|^2^]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .0724
_refine_ls_wR_factor_ref         .0659
_reflns_number_gt                1264
_reflns_number_total             1510
_reflns_threshold_expression     I>2.0sigma(I)
_cod_data_source_file            oa0031.cif
_cod_data_source_block           2
_cod_original_cell_volume        1312.0(3)
_cod_original_formula_sum        'C12 H12 O2 S4 '
_cod_database_code               2103572
_cod_database_fobs_code          2103572