Proton transfer and hydrogen bonding in the organic solid state: a combined XRD/XPS/ssNMR study of 17 organic acid-base complexes.
Stevens, Joanna S.; Byard, Stephen J.; Seaton, Colin C.; Sadiq, Ghazala; Davey, Roger J.; Schroeder, Sven L. M.; Physical chemistry chemical physics : PCCP 16 (2014) 1150–1160; doi:10.1039/c3cp53907e

data_7214134
_publ_section_title
;
 Proton transfer and hydrogen bonding in the organic solid state: a
 combined XRD/XPS/ssNMR study of 17 organic acid-base complexes.
;
_journal_issue                   3
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              1150
_journal_page_last               1160
_journal_paper_doi               10.1039/c3cp53907e
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C7 H5 O5, C6 H7 N2 O'
_chemical_formula_sum            'C13 H12 N2 O6'
_chemical_formula_weight         292.25
_chemical_name_systematic
; 
  pyridinium-4-carboxamide 2,4,6-trihydroxybenzoate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8093(14)
_cell_length_b                   13.1563(12)
_cell_length_c                   7.4708(8)
_cell_measurement_temperature    100(2)
_cell_volume                     1259.0(2)
_computing_cell_refinement
;
 CrysAlis CCD, Oxford Diffraction Ltd.,
 Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
 (compiled Jan 8 2009,16:24:04)
;
_computing_data_collection
;
 CrysAlis CCD, Oxford Diffraction Ltd.,
 Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
 (compiled Jan 8 2009,16:24:04)
;
_computing_data_reduction
;
 CrysAlis CCD, Oxford Diffraction Ltd.,
 Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
 (compiled Jan 8 2009,16:24:04)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Oxford Diffraction Xcaliber'
_diffrn_measurement_method       '\w 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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3392
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.200
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         1817
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                1244
_reflns_number_total             1817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cp53907e.txt
_cod_data_source_block           246_thba_isonic
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_database_code               7214134