Synthesis and crystal structure of 1H-1,2,4-triazole-3,5-diamine monohydrate
Inoue, Kazuki; Nakami, Shun; Kumasaki, Mieko; Matsumoto, Shinya; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 1161–1164; doi:10.1107/S2056989024009265

data_2023286
_publ_section_title
;
 Synthesis and crystal structure of 1H-1,2,4-triazole-3,5-diamine
 monohydrate
;
_journal_coeditor_code           DX2060
_journal_issue                   11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1161
_journal_page_last               1164
_journal_paper_doi               10.1107/S2056989024009265
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C2 H5 N5, H2 O'
_chemical_formula_moiety         'C2 H5 N5, H2 O'
_chemical_formula_sum            'C2 H7 N5 O'
_chemical_formula_weight         117.13
_chemical_name_systematic
;
1<i>H</i>-1,2,4-Triazole-3,5-diamine monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.9639(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.80560(5)
_cell_length_b                   9.49424(11)
_cell_length_c                   14.01599(15)
_cell_measurement_reflns_used    2506
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      72.5260
_cell_measurement_theta_min      6.3240
_cell_volume                     505.738(10)
_computing_cell_refinement
;
CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
PublCIF (Westrip, 2010) and OLEX2 1.5 (Dolomanov <i>et al.</i>,
2009)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2894
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.669
_diffrn_reflns_theta_min         5.631
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             248
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.220
_refine_ls_extinction_coef       0.0108(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0403P)^2^+0.1848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                956
_reflns_number_total             989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dx2060.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023286.cif.'
_cod_database_code               2023286
_shelx_estimated_absorpt_t_min   0.814
_shelx_estimated_absorpt_t_max   0.901