Crystal structure of bis(5-amino-1,2,4-triazol-4-ium-3-yl)methane sulfate, C5H10N8O4S
Zhang, Guo-Tao; Wang, Hua; Li, Hong-Ya; Yan, Biao; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 571–572; doi:10.1515/ncrs-2022-0133

data_8105753
_publ_section_title
;
 Crystal structure of bis(5-amino-1,2,4-triazol-4-ium-3-yl)methane
 sulfate, C5H10N8O4S
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              571
_journal_page_last               572
_journal_paper_doi               10.1515/ncrs-2022-0133
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety
;
C5 H10 N8 2+,S1 O4 2-
;
_chemical_formula_sum            'C5 H10 N8 O4 S'
_chemical_formula_weight         278.27
_chemical_name_systematic
; 
 bis(5-amino-1,2,4-triazol-4-ium-3-yl)methane sulfate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           32
_space_group_name_Hall           'P 2 -2ab'
_space_group_name_H-M_alt        'P b a 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7320(11)
_cell_length_b                   12.8686(19)
_cell_length_c                   5.0657(8)
_cell_measurement_reflns_used    1518
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.24
_cell_measurement_theta_min      3.07
_cell_volume                     504.04(13)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2909
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.946
_diffrn_reflns_theta_min         3.074
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
; 
 Flack x determined using 428 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.13(4)
_refine_ls_extinction_coef       0.061(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1218
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0265P)^2^+0.2035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.655
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.740
_reflns_number_gt                1144
_reflns_number_total             1218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0133_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105753
_shelx_estimated_absorpt_t_min   0.883
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              42626
_shelx_hkl_checksum              13887