Facile separation of cyclic aliphatic and aromatic vapors using crystalline thiacalixarene assemblies with preorganized channels.
Yamada, Manabu; Yoshizaki, Ruka; Uemura, Fumiya; Katagiri, Hiroshi; Kato, Sumio; Akimoto, Kazuhiko; Hamada, Fumio; Chemical communications (Cambridge, England) 59 (2023) 2604–2607; doi:10.1039/d2cc05647j

data_7131341
_publ_section_title
;
 Facile separation of cyclic aliphatic and aromatic vapors using
 crystalline thiacalixarene assemblies with preorganized channels.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2604
_journal_page_last               2607
_journal_paper_doi               10.1039/d2cc05647j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C36 H36 Br4 O4 S4, 0.63[C7H14]'
_chemical_formula_sum            'C40.41 H44.82 Br4 O4 S4'
_chemical_formula_weight         1042.38
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-11-17 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   31.1921(6)
_cell_length_b                   31.1921(6)
_cell_length_c                   24.1196(5)
_cell_measurement_reflns_used    28801
_cell_measurement_temperature    223
_cell_measurement_theta_max      26.1960
_cell_measurement_theta_min      2.1840
_cell_volume                     20323.1(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'PLATON (Spek, 2020)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL2018 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT2014 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            84595
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.497
_diffrn_reflns_theta_min         2.847
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    3.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       Prism
_exptl_crystal_F_000             9419
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methylcyclohexane and chloroform (= 1:1 v/v)'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4691
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+62.5902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3425
_reflns_number_total             4691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05647j2.cif
_cod_data_source_block           20201104_yamada_no3_-50__sq
_cod_original_cell_volume        20323.1(9)
_cod_database_code               7131341
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.313
_shelx_estimated_absorpt_t_max   0.313
_oxdiff_exptl_absorpt_empirical_full_min 0.755
_oxdiff_exptl_absorpt_empirical_full_max 1.588
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelx_res_checksum              71058
_shelx_hkl_checksum              423
_shelx_fab_checksum              59586