Molecular Tiling in the 1:1 Adduct of 1,4-Diazabicyclo[2.2.2]octane and 1,3,5-Benzenetricarboxylic Acid
Meehan, Paul R.; Ferguson, George; Glidewell, Christopher; Patterson, Iain L.J.; Acta Crystallographica Section C 53 (1997) 628–631; doi:10.1107/S0108270197001200

data_2006090
_publ_section_title
;
 Molecular Tiling in the 1:1 Adduct of 1,4-Diazabicyclo[2.2.2]octane
 and 1,3,5-Benzenetricarboxylic Acid
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              628
_journal_page_last               631
_journal_paper_doi               10.1107/S0108270197001200
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C6 H13 N2 1+.C9 H5 O6 1-'
_chemical_formula_sum            'C15 H18 N2 O6'
_chemical_formula_weight         322.31
_chemical_name_systematic
;
1,4-Diazabicyclo[2.2.2]octane--1,3,5-benzenetricarboxylic acid (1/1).
.
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2525(11)
_cell_length_b                   7.0950(12)
_cell_length_c                   18.612(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      23.84
_cell_measurement_theta_min      12.49
_cell_volume                     1485.9(3)
_computing_cell_refinement       'CAD4-PC Software'
_computing_data_collection       'CAD4-PC Software (Enraf-Nonius, 1992)'
_computing_data_reduction
'DATRD2 in NRCVAX96 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics
'NRCVAX96, ORTEPII (Johnson, 1976), PLATON (Spek, 1996a), PLUTON (Spek 1996b)'
_computing_publication_material
'NRCVAX96, SHELXL93  and WordPerfect macro PREPCIF (Ferguson, 1996)'
_computing_structure_refinement  'NRCVAX96 and SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SOLVER in NRCVAX96'
_diffrn_ambient_temperature      294.0(10)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2522
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        'no decay, variation 0.5'
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.185
_refine_ls_extinction_coef       0.0028(12)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.288
_refine_ls_hydrogen_treatment
'H atoms riding (C-H 0.93--0.97, N-H 0.91, O-H 0.82\%A)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.288
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_obs          .0489
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.1098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1531
_refine_ls_wR_factor_obs         .1407
_reflns_number_observed          1380
_reflns_number_total             2323
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ab1456.cif
_cod_data_source_block           96112
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.1098P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.1098P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               2006090