Selective separation of branched alkane vapor by thiacalixarene supramolecular crystals having shape-recognition properties.
Yamada, Manabu; Uemure, Fumiya; Katagiri, Hiroshi; Akimoto, Kazuhiko; Hamada, Fumio; Chemical communications (Cambridge, England) 57 (2021) 6237–6240; doi:10.1039/d1cc01931g

data_7128470
_publ_section_title
;
 Selective separation of branched alkane vapor by thiacalixarene
 supramolecular crystals having shape-recognition properties.
;
_journal_issue                   51
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6237
_journal_page_last               6240
_journal_paper_doi               10.1039/d1cc01931g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C36 H36 Br4 O4 S4, 0.5(C8 H18)'
_chemical_formula_sum            'C40 H45 Br4 O4 S4'
_chemical_formula_weight         1037.64
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-05-12 deposited with the CCDC.	2021-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.624(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
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_cell_length_b                   31.1812(6)
_cell_length_c                   19.7005(5)
_cell_measurement_reflns_used    46061
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.0940
_cell_measurement_theta_min      1.8900
_cell_volume                     13489.9(6)
_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    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            26470
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.602
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    3.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69792
_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             6252
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform and isooctane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1568
_refine_ls_number_reflns         26470
_refine_ls_number_restraints     534
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0753P)^2^+30.2725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17431
_reflns_number_total             26470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01931g2.cif
_cod_data_source_block           20200704_yamada_no3_-100__tw
_cod_depositor_comments          'Adding full bibliography for 7128470.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7128470
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.450
_shelx_estimated_absorpt_t_max   0.517
_oxdiff_exptl_absorpt_empirical_full_min 0.837
_oxdiff_exptl_absorpt_empirical_full_max 1.406
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelx_res_checksum              32291
_shelx_hkl_checksum              92156