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_7230243
_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         'C48 H48 N2'
_chemical_formula_sum            'C48 H48 N2'
_chemical_formula_weight         652.88
_chemical_name_systematic
N-((6-butyl-2,4,8,10-tetraphenyl-6,7-dihydro-5H-dibenzo[c,e]azepin-1-yl)methyl)-N-ethylbutan-1-amine
_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
;
2017-12-22 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.421(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0148(17)
_cell_length_b                   9.6841(11)
_cell_length_c                   25.874(3)
_cell_measurement_reflns_used    17214
_cell_measurement_temperature    123(3)
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      3.195
_cell_volume                     3700.1(7)
_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      123(3)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.2009
_diffrn_reflns_av_unetI/netI     0.1266
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32947
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        21.967
_diffrn_reflns_theta_max         21.967
_diffrn_reflns_theta_min         3.113
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.994830
_exptl_absorpt_correction_T_min  0.969220
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
T.Higashi, Numerical Absorption Correction, NUMABS, 2002
T.Higashi, Empirical Absorption Correction, 2001
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         4488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0574P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2726
_reflns_number_total             4488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00041g2.cif
_cod_data_source_block           shelx_CCDC4
_cod_database_code               7230243
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              74182