2,5-Diaminothiophene-3,4-dicarbonitrile
Ziegler, Christopher J.; Nemykin, Victor N.; Acta Crystallographica Section E 68 (2012) o2693–; doi:10.1107/S1600536812034678

data_2236787
_publ_section_title
;
 2,5-Diaminothiophene-3,4-dicarbonitrile
;
_journal_coeditor_code           ZS2223
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2693
_journal_paper_doi               10.1107/S1600536812034678
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C6 H4 N4 S'
_chemical_formula_moiety         'C6 H4 N4 S'
_chemical_formula_sum            'C6 H4 N4 S'
_chemical_formula_weight         164.19
_chemical_melting_point          513
_chemical_name_common            2,5-diamino-3,4-dicyanothiophene
_chemical_name_systematic        2,5-Diaminothiophene-3,4-dicarbonitrile
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.9231(2)
_cell_length_b                   13.8213(12)
_cell_length_c                   12.6465(11)
_cell_measurement_reflns_used    783
_cell_measurement_temperature    123
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     685.72(9)
_computing_cell_refinement       'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'CrystalClear (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear (Rigaku, 2009)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Rigaku RAPID II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Mo Ka'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2260
_diffrn_reflns_theta_full        26.931
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.360
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  2
_diffrn_standards_number         783
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.63
_refine_ls_extinction_coef       0.0
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         769
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.0000992
_refine_ls_shift/su_mean         0.0000128
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994; Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:  57.9 74.5 21.5
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1162
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                492
_reflns_number_total             783
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zs2223.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P b c n '
_cod_database_code               2236787
_cod_database_fobs_code          2236787