Pillar[5]arene-based ionic single crystals formed by dual self-assemblies through host-guest and ionic interactions for iodine capture.
Zhang, Ting; Wang, Lulu; Li, Hui; Sun, Mingxia; Chen, Jia; Guan, Shuzhe; Qiu, Hongdeng; Chemical communications (Cambridge, England) 61 (2025) 10843–10846; doi:10.1039/d5cc02200b

data_7134710
_publ_section_title
;
 Pillar[5]arene-based ionic single crystals formed by dual self-assemblies
 through host-guest and ionic interactions for iodine capture.
;
_journal_issue                   58
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10843
_journal_page_last               10846
_journal_paper_doi               10.1039/d5cc02200b
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C59 H72 N4 O10, C10 H6 O6 S2, 2(C2 H6 O)'
_chemical_formula_sum            'C73 H90 N4 O18 S2'
_chemical_formula_weight         1375.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2m29hj
_audit_creation_date             2023-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-01-08 deposited with the CCDC.	2025-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                77.270(4)
_cell_angle_beta                 68.987(4)
_cell_angle_gamma                75.532(4)
_cell_formula_units_Z            2
_cell_length_a                   13.938(3)
_cell_length_b                   16.892(4)
_cell_length_c                   18.001(4)
_cell_measurement_reflns_used    2654
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.581
_cell_measurement_theta_min      2.301
_cell_volume                     3790.6(15)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.1178
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19506
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.624
_diffrn_source_current           25.0
_diffrn_source_power             1.125
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1392 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.7196.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         13281
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1828
_refine_ls_R_factor_gt           0.0844
_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^)+(0.1539P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2298
_refine_ls_wR_factor_ref         0.2962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5367
_reflns_number_total             13281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02200b2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7134710.cif.'
_cod_original_cell_volume        3790.4(14)
_cod_database_code               7134710
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.978
_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, All O(H) groups
2. Restrained distances
 C70-C71
 1.5 with sigma of 0.02
 O19-C75 = O18-C73 = O20-C77 = O17-C71
 1.28 with sigma of 0.02
 C75-C74 = C73-C72
 1.5 with sigma of 0.01
 O19-C74
 2.3 with sigma of 0.04
 C72-O18
 2.3 with sigma of 0.04
 C46-C45 \\sim C45-C44
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O19) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C72)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: O17(0.5) H17A(0.5) C71(0.5) H71A(0.5) H71B(0.5) C70(0.5) H70A(0.5)
 H70B(0.5) H70C(0.5) O20(0.5) H20A(0.5) C77(0.5) H77A(0.5) H77B(0.5) C76(0.5)
 H76A(0.5) H76B(0.5) H76C(0.5) C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5) C73(0.5)
 H73A(0.5) H73B(0.5) O19(0.5) H19(0.5) C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5)
 C75(0.5) H75A(0.5) H75B(0.5) O18(0.5) H18(0.5)
5.a Riding coordinates:
 O19(H19), O18(H18)
5.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C28(H28A,H28B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C21(H21A,H21B), C55(H55A,H55B), C7(H7A,H7B), C44(H44A,H44B), C14(H14A,
 H14B), C46(H46A,H46B), C47(H47A,H47B), C45(H45A,H45B), C71(H71A,H71B),
 C77(H77A,H77B), C73(H73A,H73B), C75(H75A,H75B)
5.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C31(H31), C6(H6), C27(H27), C63(H63), C3(H3), C17(H17), C13(H13),
 C20(H20), C10(H10), C68(H68), C61(H61), C24(H24), C66(H66), C58(H58), C67(H67),
  C62(H62), C50(H50), C57(H57), C56(H56), C48(H48), C49(H49)
5.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C39(H39A,H39B,H39C), C51(H51A,H51B,H51C), C38(H38A,H38B,H38C), C43(H43A,
 H43B,H43C), C59(H59A,H59B,H59C), C42(H42A,H42B,H42C), C70(H70A,H70B,H70C),
 C76(H76A,H76B,H76C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C)
5.e Idealised tetrahedral OH refined as rotating group:
 O17(H17A), O20(H20A)
;
_shelx_res_checksum              43637
_shelx_hkl_checksum              14185
_olex2_submission_special_instructions 'No special instructions were received'