Proton location in acid⋯pyridine hydrogen bonds of multi-component crystals
Seaton, Colin C.; CrystEngComm 16 (2014) 5878–; doi:10.1039/c4ce00043a

data_7215669
_publ_section_title
;
 Proton location in acid&#x22EF;pyridine hydrogen bonds of multi-component
 crystals
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              5878
_journal_paper_doi               10.1039/c4ce00043a
_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_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Sir92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0816
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.896
_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            3389
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.573
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         28.419
_diffrn_reflns_theta_min         3.136
_diffrn_source
;
'Enhance (Mo) X-ray Source'  
;
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.542
_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         0.180
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 187 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.4(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.825
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         1815
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.825
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0136P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0482
_reflns_Friedel_coverage         0.189
_reflns_Friedel_fraction_full    0.236
_reflns_Friedel_fraction_max     0.197
_reflns_number_gt                1244
_reflns_number_total             1815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00043a2.cif
_cod_data_source_block           246thba_ina
_cod_depositor_comments
'Adding full bibliography for 7215667--7215669.cif.'
_cod_database_code               7215669
_shelxl_version_number           2013-4
_shelx_res_checksum              41678
_shelx_hkl_checksum              65718