Piperazine-1,4-diium bis(hydrogen 2-propyl-1<i>H</i>-imidazole-4,5-dicarboxylate) monohydrate
Gao, Zhu-Qing; Gu, Jin-Zhong; Acta Crystallographica Section E 67 (2011) o31–; doi:10.1107/S1600536810049822

data_2228785
_publ_section_title
;
 Piperazine-1,4-diium bis(hydrogen
 2-propyl-1<i>H</i>-imidazole-4,5-dicarboxylate) monohydrate
;
_journal_coeditor_code           JH2238
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o31
_journal_paper_doi               10.1107/S1600536810049822
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C4 H12 N2 2+, 2C8 H9 N2 O4 -, H2 O1'
_chemical_formula_moiety         'C4 H12 N2 2+, 2(C8 H9 N2 O4 -), H2 O1'
_chemical_formula_sum            'C20 H32 N6 O9'
_chemical_formula_weight         500.52
_chemical_name_systematic
;
Piperazine-1,4-diium bis(hydrogen
2-propyl-1<i>H</i>-imidazole-4,5-dicarboxylate) monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 101.296(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.288(2)
_cell_length_b                   15.965(3)
_cell_length_c                   14.449(4)
_cell_measurement_reflns_used    1047
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2553.5(10)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6239
_diffrn_reflns_theta_full        24.27
_diffrn_reflns_theta_max         24.27
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2066
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+1.5738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1358
_reflns_number_gt                1499
_reflns_number_total             2066
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jh2238.cif
_cod_data_source_block           I
_cod_original_cell_volume        2553.6(10)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2228785
_cod_database_fobs_code          2228785