Creation of a ternary complex between a crown ether, 4-aminobenzoic acid and 3,5-dinitrobenzoic acid
Boardman, Nicole D.; Munshi, Tasnim; Scowen, Ian J.; Seaton, Colin C.; Acta Crystallographica Section B 70 (2014) 132–140; doi:10.1107/S2052520613026036

data_2105761
_publ_section_title
;
 Creation of a ternary complex between a crown ether, 4-aminobenzoic acid
 and 3,5-dinitrobenzoic acid
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              132
_journal_page_last               140
_journal_paper_doi               10.1107/S2052520613026036
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety
;
C12 H24 O6, C7 H3 N2 O6, C7 H4 N2 O6, C7 H8 N O2
;
_chemical_formula_sum            'C33 H39 N5 O20'
_chemical_formula_weight         825.69
_chemical_name_systematic
;
 18-crown-6/4-aminobenzoic acid/bis(3,5-dinitrobenzoic acid)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                73.156(2)
_cell_angle_beta                 85.540(2)
_cell_angle_gamma                89.5620(10)
_cell_formula_units_Z            2
_cell_length_a                   7.6055(2)
_cell_length_b                   16.0157(4)
_cell_length_c                   16.4476(4)
_cell_measurement_reflns_used    9094
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.55
_cell_volume                     1911.45(9)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2005) and Mercury (Macrae et al., 2006)
;
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50498
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         10356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.3350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                6336
_reflns_number_total             10356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bi5005sup1.cif
_cod_data_source_block           2
_cod_database_code               2105761
_shelxl_version_number           .2013