Neutron diffraction studies of the 1:1 and 2:1 cocrystals of benzene-1,2,4,5-tetracarboxylic acid and 4,4'-bipyridine
Cowan, John A.; Howard, Judith A. K.; Mason, Sax A.; McIntyre, Garry J.; Lo, Samuel M.-F.; Mak, Toby; Chui, Stephen S.-Y.; Cai, Jiwen; Cha, John A.; Williams, Ian D.; Acta Crystallographica Section C 62 (2006) o157–o161; doi:10.1107/S0108270106004008

data_2015236
_publ_section_title
;
 Neutron diffraction studies of the 1:1 and 2:1 cocrystals of
 benzene-1,2,4,5-tetracarboxylic acid and 4,4'-bipyridine
;
_journal_coeditor_code           FG1884
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o157
_journal_page_last               o161
_journal_paper_doi               10.1107/S0108270106004008
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C10 H10 N2 2+ , C10 H4 O8 2- , 1.8H2 O'
_chemical_formula_moiety         'C10 H10 N2 2+ , C10 H4 O8 2- , 1.8H2 O'
_chemical_formula_sum            'C20 H17.6 N2 O9.8'
_chemical_formula_weight         442.40
_chemical_name_systematic
;
4,4'-bipyridinium 2,5-dicarboxybenzene-1,4-dicarboxylate 1.8-hydrate
;
_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           SHELXL97
_cell_angle_alpha                99.626(3)
_cell_angle_beta                 97.726(3)
_cell_angle_gamma                95.515(3)
_cell_formula_units_Z            1
_cell_length_a                   3.7747(2)
_cell_length_b                   10.8587(5)
_cell_length_c                   11.9519(6)
_cell_measurement_reflns_used    1196
_cell_measurement_temperature    215(2)
_cell_measurement_theta_max      55
_cell_measurement_theta_min      5
_cell_volume                     475.07(4)
_computing_cell_refinement       'RAFD19 (Filhol, 1998)'
_computing_data_collection       'MAD (Barthelemy <i>et al.</i>,  1984)'
_computing_data_reduction        'RETREAT (Wilkinson <i>et al.</i>,  1988)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1999)'
_computing_publication_material
'Please provide missing details and reference'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'Please provide missing details and reference'
_diffrn_ambient_temperature      215(2)
_diffrn_measured_fraction_theta_full 0.847
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  D19
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Germanium
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL high-flux reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.302
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1983
_diffrn_reflns_theta_full        55.04
_diffrn_reflns_theta_max         55.04
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.9332
_exptl_absorpt_correction_T_min  0.8608
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(D19ABS; Matthewmann <i>et al.</i>,  1982)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             143
_exptl_crystal_size_max          2.0
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.549
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         1654
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0297P)^2^+1.6121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                1426
_reflns_number_total             1654
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1884.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C20 H17.60 N2 O9.80'
_cod_database_code               2015236
_cod_database_fobs_code          2015236