Sterically crowded hydrogen-bonded hexagonal network frameworks
Hisaki, Ichiro; Ikenaka, Nobuaki; Tsuzuki, Seiji; Tohnai, Norimitsu; Materials Chemistry Frontiers 2 (2018) 338–; doi:10.1039/C7QM00544J

data_1553710
_publ_section_title
;
 Sterically crowded hydrogen-bonded hexagonal network frameworks
;
_journal_issue                   2
_journal_name_full               'Materials Chemistry Frontiers'
_journal_page_first              338
_journal_paper_doi               10.1039/C7QM00544J
_journal_volume                  2
_journal_year                    2018
_chemical_formula_moiety         'C72 H60 O12, C8 H8 O2'
_chemical_formula_sum            'C80 H68 O14'
_chemical_formula_weight         1253.41
_chemical_name_systematic
'hexakis(4-carboxy-3,5-dimethylphenyl)triphenylene, methyl benzoate solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-10-06 deposited with the CCDC.
2017-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3352(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.8455(3)
_cell_length_b                   22.4501(2)
_cell_length_c                   29.8331(3)
_cell_measurement_reflns_used    24397
_cell_measurement_temperature    213
_cell_measurement_theta_max      75.80
_cell_measurement_theta_min      4.03
_cell_volume                     18568.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.5a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.5a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.5a (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      213
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  XtaLAB200
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            54132
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         76.119
_diffrn_reflns_theta_min         3.794
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.5a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7456.00
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF, methyl benzoate'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     950
_refine_ls_number_reflns         18891
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1811P)^2^+18.0017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2811
_refine_ls_wR_factor_ref         0.2926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15382
_reflns_number_total             18891
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7qm00544j2.cif
_cod_data_source_block           TpMe-1
_cod_database_code               1553710
_shelx_res_checksum              9424
_shelx_hkl_checksum              75727
_shelx_fab_checksum              9378