Polymorphism of a porous hydrogen bond assisted ionic organic framework
Horvath, Daniel Vajk Daniel; Holczbauer, Tamas; Bereczki, Laura; Palko, Roberta; Nagy, Nora V.; Soos, Tibor; Bombicz, Petra Alexandra; CrystEngComm  (2018) –; doi:10.1039/C8CE00041G

data_7230242
_publ_section_title
;
 Polymorphism of a porous hydrogen bond assisted ionic organic framework
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE00041G
_journal_year                    2018
_chemical_formula_moiety
;
C56 H66 N2 2+, (Br-)2, 4(C4 H8 O), [ solvent]
;
_chemical_formula_sum            'C72 H98 Br2 N2 O4'
_chemical_formula_weight         1215.34
_chemical_name_systematic
'5,5,11,11-tetrabutyl-1,3,7,9-tetraphenyl-4,5,6,10,11,12-hexahydro-5,11- diazadibenzo[ef,kl]heptalene-5,11-diium-bromide'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-02-15 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.343(3)
_cell_length_b                   15.987(4)
_cell_length_c                   17.571(5)
_cell_measurement_reflns_used    6786
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.98
_cell_measurement_theta_min      3.045
_cell_volume                     6838(3)
_computing_cell_refinement
'RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)'
_computing_data_collection
'RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)'
_computing_data_reduction
'RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID II'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1625
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26547
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        21.966
_diffrn_reflns_theta_max         21.966
_diffrn_reflns_theta_min         3.045
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.996386
_exptl_absorpt_correction_T_min  0.974096
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
NUMABS, Numerical Absorption correction Program (T.Higashi, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2584
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1862
_refine_ls_R_factor_gt           0.1047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1582P)^2^+4.5433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2801
_refine_ls_wR_factor_ref         0.3288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1864
_reflns_number_total             4151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00041g2.cif
_cod_data_source_block           shelx_CCDC3
_cod_original_formula_sum        'C72 H98 Br2 N2 O4 '
_cod_database_code               7230242
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.578
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              89009
_shelx_fab_checksum              5640