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_7230241
_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, 3(C4 H8 O), [ solvent]
;
_chemical_formula_sum            'C68 H90 Br2 N2 O3'
_chemical_formula_weight         1143.23
_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           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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            8
_cell_length_a                   22.071(3)
_cell_length_b                   25.991(3)
_cell_length_c                   28.554(4)
_cell_measurement_reflns_used    7855
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.825
_cell_measurement_theta_min      3.00
_cell_volume                     16380(4)
_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      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1380
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30885
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        20.812
_diffrn_reflns_theta_max         20.812
_diffrn_reflns_theta_min         3.135
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.972285
_exptl_absorpt_correction_T_min  0.960439
_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    0.927
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             4848
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran'
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.550
_exptl_crystal_size_min          0.450
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.876
_refine_ls_R_factor_all          0.2964
_refine_ls_R_factor_gt           0.2302
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_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          0.5471
_refine_ls_wR_factor_ref         0.5847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                879
_reflns_number_total             2139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00041g2.cif
_cod_data_source_block           shelx_CCDC2
_cod_database_code               7230241
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.588
_shelx_estimated_absorpt_t_max   0.656
_shelx_res_checksum              92318
_shelx_fab_checksum              65132