An unsymmetrical tetrathiafulvalene with a fused 1,2,5-thiadiazole ring and an ethylenedioxy group
Tomura, Masaaki; Yamashita, Yoshiro; Acta Crystallographica Section E 59 (2003) o145–o147; doi:10.1107/S1600536802023723

data_2202104
_publ_section_title
;
 An unsymmetrical tetrathiafulvalene with a fused 1,2,5-thiadiazole
 ring and an ethylenedioxy group
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o145
_journal_page_last               o147
_journal_paper_doi               10.1107/S1600536802023723
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C8 H4 N2 O2 S5'
_chemical_formula_sum            'C8 H4 N2 O2 S5'
_chemical_formula_weight         320.43
_chemical_name_common
;
4,5-ethylenedioxy[1,2,5]thiadiazolotetrathiafulvalene
;
_chemical_name_systematic
;
5-(4,5-ethylenedioxy-1,3-dithiol-2-ylidene)-1,3,2,4,6-diazatrithiapentalene
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7363(10)
_cell_length_b                   12.9552(6)
_cell_length_c                   3.9938(5)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      42.66
_cell_measurement_theta_min      14.11
_cell_volume                     1124.65(16)
_computing_cell_refinement       'CAD4 Express Software'
_computing_data_collection       'CAD4 Express Software (Enraf-Nonius, 1992)'
_computing_data_reduction
;
teXsan (Molecular Structure Corporation/Rigaku Corporation, 2000)
;
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.001
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1271
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1303
_diffrn_reflns_theta_full        74.15
_diffrn_reflns_theta_max         74.15
_diffrn_reflns_theta_min         3.97
_diffrn_standards_decay_%        0.40
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.434
_exptl_absorpt_correction_T_max  0.8337
_exptl_absorpt_correction_T_min  0.1164
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.867
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.03(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1303
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0859P)^2^] where P = (Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1735
_reflns_number_gt                791
_reflns_number_total             1303
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6206.cif
_cod_data_source_block           I
_cod_database_code               2202104
_cod_database_fobs_code          2202104