Two-dimensional hydrogen-bonded supramolecular networks in the compounds of benzene-1,2,4,5-tetracarboxylic acid (pyromellitic acid) with 2,2'-biimidazole and 4,4'-dimethyl-2,2'-bipyridine
Zhong, Kai-Long; Acta Crystallographica Section C 69 (2013) 1537–1540; doi:10.1107/S0108270113030801

data_2019319
_publ_section_title
;
 Two-dimensional hydrogen-bonded supramolecular networks in the compounds
 of benzene-1,2,4,5-tetracarboxylic acid (pyromellitic acid) with
 2,2'-biimidazole and 4,4'-dimethyl-2,2'-bipyridine
;
_journal_coeditor_code           SF3209
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1537
_journal_page_last               1540
_journal_paper_doi               10.1107/S0108270113030801
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C12 H13 N2 +, C10 H5 O8 -, H2 O'
_chemical_formula_moiety         'C12 H13 N2 +, C10 H5 O8 -, H2 O'
_chemical_formula_sum            'C22 H20 N2 O9'
_chemical_formula_weight         456.40
_chemical_name_systematic
;
4-Methyl-2-(4-methylpyridin-2-yl)pyridinium 2,4,5-tricarboxybenzoate
monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.979(6)
_cell_angle_beta                 73.421(6)
_cell_angle_gamma                62.655(8)
_cell_formula_units_Z            2
_cell_length_a                   9.5166(7)
_cell_length_b                   9.9970(8)
_cell_length_c                   12.4106(8)
_cell_measurement_reflns_used    2637
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      29.2190
_cell_measurement_theta_min      3.4810
_cell_volume                     1001.03(15)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9371
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB: Jacobson, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.395
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3516
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0474P)^2^+0.9963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                2681
_reflns_number_total             3516
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3209.cif
_cod_data_source_block           II
_cod_original_cell_volume        1001.03(13)
_cod_database_code               2019319