Hydrogen-bonding behaviour of benzene-1,2,4,5-tetracarboxylic acid: supramolecular structures of different dimensionality in the 2:1 adducts formed with 4,4'-bipyridyl and hexamethylenetetramine
Lough, Alan J.; Wheatley, Paul S.; Ferguson, George; Glidewell, Christopher; Acta Crystallographica Section B 56 (2000) 261–272; doi:10.1107/S0108768199012860

data_2102027
_publ_section_title
;
 Hydrogen-bonding behaviour of benzene-1,2,4,5-tetracarboxylic acid:
 supramolecular structures of different dimensionality in the 2:1
 adducts formed with 4,4'-bipyridyl and hexamethylenetetramine
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              261
_journal_page_last               272
_journal_paper_doi               10.1107/S0108768199012860
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C10 H4 O8, 2(C6 H13 N4)'
_chemical_formula_sum            'C22 H30 N8 O8'
_chemical_formula_weight         534.54
_chemical_name_systematic
;
Benzeme-1,2,4,5-tetracarboxylic acid--hexamethylenetetramine (1/2)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                84.271(3)
_cell_angle_beta                 79.399(3)
_cell_angle_gamma                75.264(3)
_cell_formula_units_Z            3
_cell_length_a                   9.7029(6)
_cell_length_b                   10.9369(7)
_cell_length_c                   16.7647(11)
_cell_measurement_reflns_used    6124
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      4.09
_cell_volume                     1688.55(19)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'NRCVAX-96, ORTEP (Johnson, 1976), PLATON (Spek, 1999)'
_computing_publication_material
'NRCVAX-96, SHELXL-97  and WordPerfect macro PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'NRCVAX-96 and SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full .989
_diffrn_measured_fraction_theta_max .989
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .078
_diffrn_reflns_av_sigmaI/netI    .1266
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14292
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         4.09
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .122
_exptl_absorpt_correction_T_max  .9759
_exptl_absorpt_correction_T_min  .9701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             846
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .20
_refine_diff_density_max         .275
_refine_diff_density_min         -.269
_refine_ls_extinction_coef       .0016(5)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   .839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         6124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .839
_refine_ls_R_factor_all          .1262
_refine_ls_R_factor_gt           .0482
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1142
_reflns_number_gt                2853
_reflns_number_total             6124
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            fr0006.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_database_code               2102027