5-(1,3-Dithiolo[4,5-<i>d</i>][1,3]dithiol-2-ylidene)-1,3-dithiolo[4,5-<i>c</i>][1,2,5]thiadiazole: an unsymmetrical tetrathiafulvalene with fused 1,2,5-thiadiazole and 1,3-dithiole rings
Tomura, Masaaki; Yamashita, Yoshiro; Acta Crystallographica Section E 65 (2009) o1082–; doi:10.1107/S1600536809014184

data_2221695
_publ_section_title
;5-(1,3-Dithiolo[4,5-<i>d</i>][1,3]dithiol-2-ylidene)-1,3-dithiolo[4,5-<i>c</i>][1,2,5]thiadiazole:
 an unsymmetrical tetrathiafulvalene with fused 1,2,5-thiadiazole and
 1,3-dithiole rings
;
_journal_coeditor_code           HB2951
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1082
_journal_paper_doi               10.1107/S1600536809014184
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C7 H2 N2 S7'
_chemical_formula_moiety         'C7 H2 N2 S7'
_chemical_formula_sum            'C7 H2 N2 S7'
_chemical_formula_weight         338.60
_chemical_name_common
;
4,5-Methylenedithio[1,2,5]thiadiazolotetrathiafulvalene
;
_chemical_name_systematic
;
5-(1,3-Dithiolo[4,5-<i>d</i>][1,3]dithiol-2-ylidene)-1,3-
dithiolo[4,5-<i>c</i>][1,2,5]thiadiazole
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 113.020(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.42(3)
_cell_length_b                   4.051(3)
_cell_length_c                   11.047(10)
_cell_measurement_reflns_used    1272
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      30.3296
_cell_measurement_theta_min      2.0028
_cell_volume                     1129.4(18)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2006)'
_computing_data_reduction        'TEXSAN (Rigaku, 2004)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1758
_diffrn_reflns_av_sigmaI/netI    0.1149
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4788
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green--brown
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.405
_refine_ls_extinction_coef       0.0064(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1639
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.135
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0051P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                737
_reflns_number_total             1639
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2951.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2221695