2-Amino-5-methylpyridinium 1<i>H</i>-pyrazole-3,5-dicarboxylate trihydrate
Shahani, Tara; Fun, Hoong-Kun; Hemamalini, Madhukar; Acta Crystallographica Section E 66 (2010) o2876–o2877; doi:10.1107/S1600536810041644

data_2227566
_publ_section_title
;
 2-Amino-5-methylpyridinium 1<i>H</i>-pyrazole-3,5-dicarboxylate
 trihydrate
;
_journal_coeditor_code           HB5681
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2876
_journal_page_last               o2877
_journal_paper_doi               10.1107/S1600536810041644
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '2C6 H9 N2 +, C5 H2 N2 O4 2-, 3H2 O'
_chemical_formula_moiety         '2(C6 H9 N2), C5 H2 N2 O4, 3(H2 O)'
_chemical_formula_sum            'C17 H26 N6 O7'
_chemical_formula_weight         426.44
_chemical_name_systematic
;
2-Amino-5-methylpyridinium 1<i>H</i>-pyrazole-3,5-dicarboxylate trihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.9420(10)
_cell_angle_beta                 93.8830(10)
_cell_angle_gamma                104.6480(10)
_cell_formula_units_Z            2
_cell_length_a                   7.89850(10)
_cell_length_b                   9.21950(10)
_cell_length_c                   15.3922(2)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      35.05
_cell_measurement_theta_min      2.43
_cell_volume                     1052.40(2)
_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) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26056
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.2775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                5085
_reflns_number_total             6103
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5681.cif
_cod_data_source_block           I
_cod_database_code               2227566
_cod_database_fobs_code          2227566