A dihydrogen phosphate anionic network as a host lattice for cations in 1-methylpiperazine-1,4-diium bis(dihydrogen phosphate) and 2-(pyridin-2-yl)pyridinium dihydrogen phosphate–orthophosphoric acid (1/1)
Jagan, R.; Sathya, D.; Sivakumar, K.; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615006518

data_2019927
_publ_section_title
;
 A dihydrogen phosphate anionic network as a host lattice for cations in
 1-methylpiperazine-1,4-diium bis(dihydrogen phosphate) and
 2-(pyridin-2-yl)pyridinium dihydrogen phosphate--orthophosphoric acid
 (1/1)
;
_journal_coeditor_code           UK3112
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615006518
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C10 H9 N2 + , H2 P O4 - , H3 P O4'
_chemical_formula_moiety         'C10 H9 N2 +, H2 O4 P -, H3 O4 P'
_chemical_formula_sum            'C10 H14 N2 O8 P2'
_chemical_formula_weight         352.17
_chemical_name_systematic
;
2-(Pyridin-2-yl)pyridinium dihydrogen phosphate--orthophosphoric acid (1/1)
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.881(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3885(7)
_cell_length_b                   10.4019(5)
_cell_length_c                   8.3927(3)
_cell_measurement_reflns_used    3870
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.149
_cell_measurement_theta_min      2.281
_cell_volume                     1507.08(11)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT and XPREP (Bruker, 2004)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1993)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13052
_diffrn_reflns_theta_full        25.79
_diffrn_reflns_theta_max         25.79
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.9470
_exptl_absorpt_correction_T_min  0.8975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2889
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0384P)^2^+1.3728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                2096
_reflns_number_total             2889
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            uk3112sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019927
_cod_database_fobs_code          2019927