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_7230240
_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 H50 N2 2+, (Cl 1-)2'
_chemical_formula_sum            'C48 H50 Cl2 N2'
_chemical_formula_weight         725.80
_chemical_name_systematic
'5,11-dibutyl-1,3,7,9-tetraphenyl-4,5,6,10,11,12-hexahydro-5,11-diazadibenzo[ef,kl]heptalene-5,11-diium dichloride'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 99.050(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4240(8)
_cell_length_b                   23.0450(15)
_cell_length_c                   15.1970(8)
_cell_measurement_reflns_used    34218
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      3.08
_cell_measurement_theta_min      25.34
_cell_volume                     4296.9(5)
_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(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
 Scan : N=1,PHI=90.0,CHI=30.0,OMEGA=110.0,170.0,5.0,COUPLE=0.0
 Scan : N=2,PHI=270.0,CHI=30.0,OMEGA=0.0,160.0,5.0,COUPLE=0.0
 Scan : N=3,PHI=0.0,CHI=30.0,OMEGA=0.0,160.0,5.0,COUPLE=0.0
 Scan : N=4,PHI=180.0,CHI=30.0,OMEGA=0.0,120.0,5.0,COUPLE=0.0
 Orientation Matrix:
 U(1,1)=-0.0226 U(1,2)=-0.0411 U(1,3)= 0.0074
 U(2,1)=-0.0783 U(2,2)= 0.0118 U(2,3)=-0.0136
 U(3,1)= 0.0007 U(3,2)=-0.0072 U(3,3)=-0.0648
;
_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  0.0902
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            70287
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.341
_diffrn_reflns_theta_min         3.081
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_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    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         7826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1007P)^2^+4.6847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5142
_reflns_number_total             7826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00041g2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        4296.9(4)
_cod_database_code               7230240
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.914
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              23896