Crystal structure of 4-hydroxypyridin-1-ium 3,5-dicarboxybenzoate
Staun, Selena L.; Oliver, Allen G.; Acta Crystallographica Section E 71 (2015) 861–863; doi:10.1107/S2056989015011780

data_2240875
_publ_section_title
;
 Crystal structure of 4-hydroxypyridin-1-ium 3,5-dicarboxybenzoate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              861
_journal_page_last               863
_journal_paper_doi               10.1107/S2056989015011780
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C5 H6 N O +, C9 H5 O6 -'
_chemical_formula_moiety         'C5 H6 N O +, C9 H5 O6 -'
_chemical_formula_sum            'C14 H11 N O7'
_chemical_formula_weight         305.24
_chemical_name_systematic
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4-Hydroxypyridin-1-ium 3,5dicarboxybenzoate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.3465(10)
_cell_length_b                   12.2113(5)
_cell_length_c                   3.6206(2)
_cell_measurement_reflns_used    2373
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      71.16
_cell_measurement_theta_min      3.42
_cell_volume                     1297.47(10)
_computing_cell_refinement
;
SAINT (Bruker 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker 2012)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009), Mercury (Macrae <i>et al.</i>,
2008) and POVRay (Cason, 2003)
;
_computing_publication_material
;
publCIF (Westrip, 2010) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      122(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            6000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.237
_diffrn_reflns_theta_min         3.012
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
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SADABS (Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       rod
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.186
_refine_ls_abs_structure_details
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Flack <i>x</i> determined using 786 quotients
[(I+)-(I-)]/[(I+)+(I-)] (Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.20(8)
_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     213
_refine_ls_number_reflns         2322
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.1815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                2172
_reflns_number_total             2322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2555sup1.cif
_cod_data_source_block           I
_cod_database_code               2240875
_cod_database_fobs_code          2240875
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.937
_shelx_hkl_checksum              3016
_shelx_res_checksum              22272