The crystal structure of 3,3′-disulfanediyldi(1H-1,2,4-triazol-5-amine) monohydrate, C4H8N8OS2
Khayrullaev, Giyosiddin; Torambetov, Batirbay; Kadirova, Shakhnoza; Vaksler, Yevhenii; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 141–144; doi:10.1515/ncrs-2022-0519

data_8107376
_publ_section_title
;
 The crystal structure of
 3,3&#x2032;-disulfanediyldi(1H-1,2,4-triazol-5-amine) monohydrate,
 C4H8N8OS2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              141
_journal_page_last               144
_journal_paper_doi               10.1515/ncrs-2022-0519
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C4 H6 N8 S2, H2 O'
_chemical_formula_sum            'C4 H8 N8 O S2'
_chemical_formula_weight         248.30
_chemical_melting_point          553.15
_chemical_name_common
;
'3,3'-disulfanediyldi(1H-1,2,4-triazol-5-amine) monohydrate'
;
_chemical_name_systematic
;
'3,3'-disulfanediyldi(1H-1,2,4-triazol-5-amine) monohydrate'
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                91.481(5)
_cell_angle_beta                 108.906(5)
_cell_angle_gamma                110.678(6)
_cell_formula_units_Z            2
_cell_length_a                   7.4377(5)
_cell_length_b                   7.5032(5)
_cell_length_c                   10.0964(6)
_cell_measurement_reflns_used    2337
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.7380
_cell_measurement_theta_min      4.3370
_cell_volume                     492.41(6)
_computing_cell_refinement       'CrysAlis^Pro^, Ver. 1.171.39.46 [1]'
_computing_data_collection       'CrysAlis^Pro^, Ver. 1.171.39.46 [1]'
_computing_data_reduction        'CrysAlis^Pro^, Ver. 1.171.39.46 [1]'
_computing_molecular_graphics    'Olex2 1.5 [4]'
_computing_publication_material  'Olex2 1.5 [4]'
_computing_structure_refinement  'SHELXL-2017/1 [3]'
_computing_structure_solution    'SHELXT-2014/5 [2]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -76.00 -50.00   1.00   10.00    --  -30.68-178.00  30.00   26
  2  \w    -99.00  -2.00   1.00   10.00    --  -30.68 -77.00  60.00   97
  3  \w     21.00  69.00   1.00   10.00    --   32.08 -99.00   0.00   48
  4  \w     74.00 109.00   1.00   10.00    --   32.08-178.00 -90.00   35
  5  \w    -35.00  42.00   1.00   10.00    --   32.08 -57.00-180.00   77
  6  \w     26.00  74.00   1.00   10.00    --   32.08 -99.00-120.00   48
  7  \w    -41.00  74.00   1.00   10.00    --   32.08 -19.00-120.00  115
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6011
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.572
_diffrn_reflns_theta_min         3.133
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       block
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.12(2)
_refine_ls_extinction_method     'SHELXL-2017/1 [3]'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1002P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1888
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2735
_reflns_number_total             3756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0519_suppl.cif
_cod_data_source_block           exp_1115
_cod_database_code               8107376
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              25521