Adaptive crystals of homothiacalix[4]arene capable of molecular recognition, with preferential uptake of benzene over cyclohexane.
Losus, Renny Maria; Bleus, Sem; Bon, Volodymyr; Kaskel, Stefan; Dehaen, Wim; Dobrzańska, Liliana; Chemical communications (Cambridge, England)  (2025) –; doi:10.1039/d5cc05862g

data_7135157
_publ_section_title
;
 Adaptive crystals of homothiacalix[4]arene capable of molecular
 recognition, with preferential uptake of benzene over cyclohexane.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d5cc05862g
_journal_year                    2025
_chemical_formula_moiety         'C52 H72 O4 S4, 2(C6 H6)'
_chemical_formula_sum            'C64 H84 O4 S4'
_chemical_formula_weight         1045.55
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-02-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-01 deposited with the CCDC.	2025-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.37523(14)
_cell_length_b                   28.37523(14)
_cell_length_c                   14.57079(13)
_cell_measurement_reflns_used    14309
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.3540
_cell_measurement_theta_min      3.3970
_cell_volume                     11731.73(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.120a 64-bit (release 16-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -57.00  -1.00   0.50    7.00    --  -46.54  55.00  68.00  112
  2  \w    -79.00 -34.00   0.50   21.00    --  -91.75  69.00 -90.00   90
  3  \w   -152.00 -75.00   0.50   21.00    --  -91.75 -69.00 137.00  154
  4  \w     50.00 105.00   0.50   21.00    --  113.25-108.00  53.00  110
  5  \w   -116.00 -88.00   0.50    7.00    --  -46.54 -77.00-180.00   56
  6  \w   -119.00 -90.00   0.50    7.00    --  -46.54 -77.00   0.00   58
  7  \w    -26.00   3.00   0.50    7.00    --   46.54 -19.00   0.00   58
  8  \w    -47.00 -21.00   0.50   21.00    --  -91.75  45.00  30.00   52
  9  \w    -46.00 -20.00   0.50   21.00    --  -91.75  45.00 120.00   52
 10  \w    -51.00 -26.00   0.50   21.00    --  -91.75  45.00 -90.00   50
 11  \w    -51.00 -26.00   0.50   21.00    --  -91.75  45.00  60.00   50
 12  \w     47.00  97.00   0.50   21.00    --  113.25 -95.00  90.00  100
 13  \w     48.00  97.00   0.50   21.00    --  113.25 -95.00 120.00   98
 14  \w     41.00  67.00   0.50   21.00    --  113.25 -61.00  60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0391093000
_diffrn_orient_matrix_UB_12      0.0358732000
_diffrn_orient_matrix_UB_13      -0.0222232000
_diffrn_orient_matrix_UB_21      0.0170341000
_diffrn_orient_matrix_UB_22      -0.0021937000
_diffrn_orient_matrix_UB_23      0.1003329000
_diffrn_orient_matrix_UB_31      0.0335705000
_diffrn_orient_matrix_UB_32      -0.0406958000
_diffrn_orient_matrix_UB_33      -0.0249224000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21691
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.710
_diffrn_reflns_theta_min         4.407
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.835
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0681P)^2^+16.8403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5399
_reflns_number_total             5870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05862g5.cif
_cod_data_source_block           htca13sol
_cod_original_cell_volume        11731.72(15)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7135157
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C64H84O4S4
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.849
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C15(H15A,H15B), C17(H17A,H17B), C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C19(H19), C21(H21), C32(H32), C31(H31), C36(H36), C35(H35),
 C34(H34), C33(H33)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C)
;
_shelx_res_checksum              59835
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.041
_oxdiff_exptl_absorpt_empirical_full_min 0.963