Bis(dimethylammonium) 3,3'-dicarboxy-5,5'-(5,7,12,14-tetraoxo-6,13-diazatetracyclo[6.6.2.0^4,16^.0^11,15^]hexadeca-1,3,8,10,15-pentaene-6,13-diyl)dibenzoate dihydrate
Xu, Lan-Ping; Qin, Lan; Han, Lei; Acta Crystallographica Section E 68 (2012) o2174–o2175; doi:10.1107/S1600536812025470

data_2235404
_publ_section_title
;
 Bis(dimethylammonium)
 3,3'-dicarboxy-5,5'-(5,7,12,14-tetraoxo-6,13-diazatetracyclo[6.6.2.0^4,16^.0^11,15^]hexadeca-1,3,8,10,15-pentaene-6,13-diyl)dibenzoate
 dihydrate
;
_journal_coeditor_code           FB2246
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2174
_journal_page_last               o2175
_journal_paper_doi               10.1107/S1600536812025470
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '2C2 H8 N +, C30 H12 N2 O12 2-, 2H2 O'
_chemical_formula_moiety         '2(C2 H8 N +), C30 H12 N2 O12 2-, 2(H2 O)'
_chemical_formula_sum            'C34 H32 N4 O14'
_chemical_formula_weight         720.64
_chemical_name_systematic
;
Bis(dimethylammonium) 3,3'-dicarboxy-5,5'-(5,7,12,14-tetraoxo-6,13-
diazatetracyclo[6.6.2.0^4,16^.0^11,15^]hexadeca-1,3,8,10,15-pentaene-
6,13-diyl)dibenzoate dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.956(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.428(13)
_cell_length_b                   8.651(10)
_cell_length_c                   18.40(2)
_cell_measurement_reflns_used    3435
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5476
_cell_measurement_theta_min      2.2149
_cell_volume                     1659(3)
_computing_cell_refinement       '<i>CrystalClear</i> (Rigaku/MSC, 2008)'
_computing_data_collection       '<i>CrystalClear</i> (Rigaku/MSC, 2008)'
_computing_data_reduction        '<i>CrystalClear</i> (Rigaku/MSC, 2008)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXL97</i> (Sheldrick, 2008'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12286
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>CrystalClear</i>; Rigaku/MSC, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube-like
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.358
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3780
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0806
_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^)+(0.1621P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2657
_reflns_number_gt                2137
_reflns_number_total             3780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            fb2246.cif
_cod_data_source_block           I
_cod_original_cell_volume        1659(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2235404
_cod_database_fobs_code          2235404