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_7230239
_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)-, 1(C5 H5 N), 1.8(C4 H8 O), [+ solvent]
;
_chemical_formula_sum            'C68.2 H85.4 Br2 N3 O1.8'
_chemical_formula_weight         1135.81
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 110.398(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.465(3)
_cell_length_b                   15.707(3)
_cell_length_c                   25.981(4)
_cell_measurement_reflns_used    17921
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.85
_cell_measurement_theta_min      3.08
_cell_volume                     6680(2)
_computing_cell_refinement       'Crystal Clear V.1.4.1 (Rigaku/MSC, 2007)'
_computing_data_collection       'Crystal Clear V.1.4.1 (Rigaku/MSC, 2007)'
_computing_data_reduction        'Crystal Clear V.1.4.1 (Rigaku/MSC, 2007)'
_computing_molecular_graphics    'Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.'
_computing_publication_material
'Spek, A.L. (2009). Acta Cryst. D65, 148-155.'
_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     0.71075
_diffrn_reflns_av_R_equivalents  0.2525
_diffrn_reflns_av_unetI/netI     0.1141
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        20.859
_diffrn_reflns_theta_max         20.859
_diffrn_reflns_theta_min         3.087
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.977
_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    1.129
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             2400
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran/pyridine'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.2138
_refine_ls_R_factor_gt           0.1276
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3386
_refine_ls_wR_factor_ref         0.3937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2979
_reflns_number_total             6992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00041g2.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C68.20 H85.40 Br2 N3 O1.80'
_cod_database_code               7230239
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.720
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              77525
_shelx_fab_checksum              83073