Piperazine-1,4-diium bis(2,4,5-tricarboxybenzoate) dihydrate
Narayanam, Nagaraju; Gangu, Kranthi Kumar; Kurra, Balakrishna; Mukkamala, Saratchandra Babu; Acta Crystallographica Section E 69 (2013) o574–o575; doi:10.1107/S160053681300723X

data_2237739
_publ_section_title
;
 Piperazine-1,4-diium bis(2,4,5-tricarboxybenzoate) dihydrate
;
_journal_coeditor_code           YK2086
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o574
_journal_page_last               o575
_journal_paper_doi               10.1107/S160053681300723X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C4 H12 N2 2+, 2C10 H5 O8 -, 2H2 O'
_chemical_formula_moiety         'C4 H12 N2 2+, 2(C10 H5 O8 -), 2H2 O'
_chemical_formula_sum            'C24 H26 N2 O18'
_chemical_formula_weight         630.46
_chemical_melting_point          560
_chemical_name_systematic
;
Piperazine-1,4-diium bis(2,4,5-tricarboxybenzoate) dihydrate
;
_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                87.117(5)
_cell_angle_beta                 89.527(5)
_cell_angle_gamma                70.962(4)
_cell_formula_units_Z            1
_cell_length_a                   8.2521(2)
_cell_length_b                   8.4810(2)
_cell_length_c                   9.6369(2)
_cell_measurement_reflns_used    7490
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.988
_cell_measurement_theta_min      2.544
_cell_volume                     636.73(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
;
ORTEP-3 for Windows
(Farrugia, 2012) and <i>Mercury</i> (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and DIAMOND (Brandenburg, 2007)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11108
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.9853
_exptl_absorpt_correction_T_min  0.9453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.198
_refine_ls_extinction_coef       0.075(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2234
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0431P)^2^+0.2345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                2061
_reflns_number_total             2234
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            yk2086.cif
_cod_data_source_block           I
_cod_database_code               2237739
_cod_database_fobs_code          2237739