Piperazine-1,4-diium bis(2-carboxy-1<i>H</i>-pyrazole-4-carboxylate) tetrahydrate
Zhou, Xin-Hui; Acta Crystallographica Section E 66 (2010) o2578–; doi:10.1107/S160053681003655X

data_2227872
_publ_section_title
;
 Piperazine-1,4-diium bis(2-carboxy-1<i>H</i>-pyrazole-4-carboxylate)
 tetrahydrate
;
_journal_coeditor_code           OM2361
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2578
_journal_paper_doi               10.1107/S160053681003655X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C4 H12 N2, 2C5 H3 N2 O4, 4H2 O'
_chemical_formula_moiety         'C4 H12 N2, 2(C5 H3 N2 O4), 4(H2 O)'
_chemical_formula_sum            'C14 H26 N6 O12'
_chemical_formula_weight         470.41
_chemical_name_systematic
;
Piperazine-1,4-diium bis(2-carboxy-1<i>H</i>-pyrazole-4-carboxylate)
tetrahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.812(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.3363(13)
_cell_length_b                   16.246(3)
_cell_length_c                   7.3930(11)
_cell_measurement_reflns_used    1373
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.7
_cell_volume                     1001.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'phi and omega 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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5265
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.9798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                1524
_reflns_number_total             1946
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2361.cif
_cod_data_source_block           I
_cod_original_cell_volume        1001.2(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2227872
_cod_database_fobs_code          2227872