Bis(5-amino-3-carboxy-1<i>H</i>-1,2,4-triazol-4-ium) dihydrogenphosphate nitrate 5-amino-1<i>H</i>-1,2,4-triazol-4-ium-3-carboxylate
Berrah, Fadila; Bouchene, Rafika; Bouacida, Sofiane; Daran, Jean-Claude; Acta Crystallographica Section E 68 (2012) o1333–o1334; doi:10.1107/S1600536812014481

data_2234596
_publ_section_title
;
 Bis(5-amino-3-carboxy-1<i>H</i>-1,2,4-triazol-4-ium) dihydrogenphosphate
 nitrate 5-amino-1<i>H</i>-1,2,4-triazol-4-ium-3-carboxylate
;
_journal_coeditor_code           FJ2538
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1333
_journal_page_last               o1334
_journal_paper_doi               10.1107/S1600536812014481
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'2C3 H5 N4 O2 +, N O3-, H2 P O4 -, C3 H4 N4 O2'
_chemical_formula_moiety
'2(C3 H5 N4 O2 +), N O3 -, H2 P O4 -, C3 H4 N4 O2'
_chemical_formula_structural     'C9 H14 N12 O6, H2 O4 P, N O3'
_chemical_formula_sum            'C9 H16 N13 O13 P'
_chemical_formula_weight         545.32
_chemical_name_systematic
;
Bis(5-amino-3-carboxy-1<i>H</i>-1,2,4-triazol-4-ium) dihydrogenphosphate
nitrate 5-amino-1<i>H</i>-1,2,4-triazol-4-ium-3-carboxylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.079(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2249(13)
_cell_length_b                   13.2036(7)
_cell_length_c                   7.7468(5)
_cell_measurement_reflns_used    8428
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      3.08
_cell_volume                     1929.8(2)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997) and
DIAMOND (Brandenburg & Berndt, 2001)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire1 long-nozzle'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10050
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       box
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.265
_refine_ls_abs_structure_details 'Flack (1983), 1858 Friedel pairs'
_refine_ls_abs_structure_Flack   0.33(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3836
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.9492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                3735
_reflns_number_total             3836
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fj2538.cif
_cod_data_source_block           I
_cod_database_code               2234596
_cod_database_fobs_code          2234596