Tris(5-amino-1<i>H</i>-1,2,4-triazol-4-ium) dihydrogenphosphate hydrogenphosphate trihydrate
Mrad, Mohamed Lahbib; Zeller, Matthias; Hernandez, Kristen J.; Rzaigui, Mohamed; Ben Nasr, Cherif; Acta Crystallographica Section E 68 (2012) o3257–o3258; doi:10.1107/S1600536812044492

data_2237009
_publ_section_title
;
 Tris(5-amino-1<i>H</i>-1,2,4-triazol-4-ium) dihydrogenphosphate
 hydrogenphosphate trihydrate
;
_journal_coeditor_code           RU2044
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3257
_journal_page_last               o3258
_journal_paper_doi               10.1107/S1600536812044492
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '3C2 H5 N4 +, H O4 P 2-, H2 O4 P -, 3H2 O'
_chemical_formula_moiety         '3(C2 H5 N4 +), H O4 P 2-, H2 O4 P -, 3(H2 O)'
_chemical_formula_sum            'C6 H24 N12 O11 P2'
_chemical_formula_weight         502.31
_chemical_name_systematic
;
Tris(5-amino-1<i>H</i>-1,2,4-triazol-4-ium) dihydrogenphosphate
hydrogenphosphate trihydrate
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.489(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4793(13)
_cell_length_b                   8.7655(11)
_cell_length_c                   11.4536(14)
_cell_measurement_reflns_used    5573
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.82
_cell_measurement_theta_min      2.98
_cell_volume                     1003.5(2)
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2011)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXLE (H\"ubschle <i>et al.</i>, 2011)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13833
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.190
_refine_ls_abs_structure_details 'Flack (1983), 2950 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6229
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.0562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                6132
_reflns_number_total             6229
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ru2044.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               2237009
_cod_database_fobs_code          2237009