Crystal structure of benzene-1,3,5-tricarboxylic acid–4-pyridone (1/3)
Staun, Selena L.; Oliver, Allen G.; Acta Crystallographica Section E 71 (2015) 1283–1286; doi:10.1107/S2056989015017867

data_2241178
_publ_section_title
;
 Crystal structure of benzene-1,3,5-tricarboxylic acid--4-pyridone (1/3)
;
_journal_coeditor_code           ZL2644
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1283
_journal_page_last               1286
_journal_paper_doi               10.1107/S2056989015017867
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C9 H6 O6, 3C5 H5 N O'
_chemical_formula_moiety         'C9 H6 O6, 3(C5 H5 N O)'
_chemical_formula_sum            'C24 H21 N3 O9'
_chemical_formula_weight         495.44
_chemical_name_systematic
;
Benzene-1,3,5-tricarboxylic acid--4-pyridone (1/3)
;
_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   geom
_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                   12.699(3)
_cell_length_b                   26.498(6)
_cell_length_c                   6.6591(14)
_cell_measurement_reflns_used    1078
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      19.15
_cell_measurement_theta_min      3.07
_cell_volume                     2240.8(9)
_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) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'combination of \w and \f-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  0.1086
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            19034
_diffrn_reflns_theta_full        23.362
_diffrn_reflns_theta_max         23.362
_diffrn_reflns_theta_min         1.537
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       rod
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.430
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 801 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013).
;
_refine_ls_abs_structure_Flack   0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         3257
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0689
_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^)+(0.1002P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                2418
_reflns_number_total             3257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2644sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2240.9(8)
_cod_database_code               2241178
_cod_database_fobs_code          2241178
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.994
_shelx_hkl_checksum              78203
_shelx_res_checksum              58995