Statistically disordered short hydrogen bonds in (pipzH~2~)(cdoH)~2~ and a comparison with (pipzH~2~)(cdo)·H~2~O (pipz is piperazine and cdoH~2~ is chelidonic acid)
Ghadermazi, Mohammad; Olmstead, Marilyn M.; Attar Gharamaleki, Jafar; Rostami, Shahideh; Acta Crystallographica Section C 67 (2011) o134–o138; doi:10.1107/S0108270111008110

data_2018046
_publ_section_title
;
 Statistically disordered short hydrogen bonds in (pipzH~2~)(cdoH)~2~
 and a comparison with (pipzH~2~)(cdo)&#x00B7;H~2~O (pipz is piperazine
 and cdoH~2~ is chelidonic acid)
;
_journal_coeditor_code           SK3402
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o134
_journal_page_last               o138
_journal_paper_doi               10.1107/S0108270111008110
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C4 H12 N2 2+ , C7 H2 O6 2- , H2 O'
_chemical_formula_moiety         'C4 H12 N2 2+, C7 H2 O6 2-, H2 O'
_chemical_formula_sum            'C11 H16 N2 O7'
_chemical_formula_weight         288.26
_chemical_name_common            pipzH2(2+)cdo(2-).H2O
_chemical_name_systematic
;
piperazine-1,4-diium 4-oxo-4<i>H</i>-pyran-2,6-dicarboxylate monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.968(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8003(3)
_cell_length_b                   11.3961(5)
_cell_length_c                   16.1548(7)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    87(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.2
_cell_volume                     1250.27(9)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      87(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX DUO'
_diffrn_measurement_method       \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  0.046
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59584
_diffrn_reflns_theta_full        31.53
_diffrn_reflns_theta_max         31.53
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         4609
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0520P)^2^+0.3187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                4303
_reflns_number_total             4609
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3402.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2018046
_cod_database_fobs_code          2018046