Crystal structure of 4,4'-[(1,3,5,7-tetraoxo-1,3,3a,4,4a,5,7,7a,8,8a-decahydro-4,8-ethenopyrrolo[3,4-<i>f</i>]isoindole-2,6-diyl)bis(methylene)]bis(pyridin-1-ium) dinitrate
Liu, Zhimin; Acta Crystallographica Section E 71 (2015) o986–o987; doi:10.1107/S2056989015022227

data_2241355
_publ_section_title
;
 Crystal structure of
 4,4'-[(1,3,5,7-tetraoxo-1,3,3a,4,4a,5,7,7a,8,8a-decahydro-4,8-ethenopyrrolo[3,4-<i>f</i>]isoindole-2,6-diyl)bis(methylene)]bis(pyridin-1-ium)
 dinitrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o986
_journal_page_last               o987
_journal_paper_doi               10.1107/S2056989015022227
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C24 H22 N4 O4 2+, 2N O3 -'
_chemical_formula_moiety         'C24 H22 N4 O4 2+, 2(N O3 -)'
_chemical_formula_sum            'C24 H22 N6 O10'
_chemical_formula_weight         554.48
_chemical_name_systematic
'4,4'-[(1,3,5,7-Tetraoxo-1,3,3a,4,4a,5,7,7a,8,8a-decahydro-4,8-ethenopyrrolo[3,4-<i>f</i>]isoindole-2,6-diyl)bis(methylene)]bis(pyridin-1-ium) dinitrate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.861(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0706(6)
_cell_length_b                   14.3587(5)
_cell_length_c                   12.9893(5)
_cell_measurement_reflns_used    4348
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.6819
_cell_measurement_theta_min      2.8272
_cell_volume                     2356.25(17)
_computing_cell_refinement
;
<i>FRAMBO</i> and SAINT (Bruker, 2004)
;
_computing_data_collection
;
<i>FRAMBO</i> (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 16.08
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker MWPC'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13323
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4555
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0861P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                2623
_reflns_number_total             4555
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su5240sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2356.25(16)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               2241355
_cod_database_fobs_code          2241355