Flexible phosphonium and sulfonate pair-to-pair self-assembled ionic organic single crystals for iodine capture
Sun, Mingxia; Chen, Jia; Zhang, Ting; Xu, Wei; He, Jing; Zhang, Yunyun; Liu, Huifeng; Zhang, Shuang; Wang, Juanjuan; Li, Xin; Yang, Yali; Qiu, Hongdeng; Chemical Science 16 (2025) 11858–11869; doi:10.1039/D5SC02039E

data_1574705
_publ_section_title
;
 Flexible phosphonium and sulfonate pair-to-pair self-assembled ionic
 organic single crystals for iodine capture
;
_journal_issue                   26
_journal_name_full               'Chemical Science'
_journal_page_first              11858
_journal_page_last               11869
_journal_paper_doi               10.1039/D5SC02039E
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C32 H14 O25 S8, 4(C38 H34 P2), 4(C H4 O), 4(H2 O)'
_chemical_formula_sum            'C188 H174 O33 P8 S8'
_chemical_formula_weight         3465.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-11-11
_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.	2025-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.5610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.9946(10)
_cell_length_b                   20.2180(17)
_cell_length_c                   17.2493(14)
_cell_measurement_reflns_used    6675
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.433
_cell_measurement_theta_min      2.344
_cell_volume                     4125.0(6)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.936
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27343
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.550
_diffrn_reflns_theta_min         1.564
_diffrn_source_current           25.0
_diffrn_source_power             1.125
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1241 before and 0.0443 after correction.
The Ratio of minimum to maximum transmission is 0.8728.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             1814
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         10817
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0593P)^2^+0.9091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7526
_reflns_number_total             10817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02039e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1574702--1574705.cif.'
_cod_database_code               1574705
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.959
_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, All O(H,H) groups
2. Restrained distances
 C16A-C14A \\sim C15A-C13A
 with sigma of 0.02
 C14A-C18A \\sim C13A-C17A
 with sigma of 0.02
 C17A-C14A \\sim C16A-C13A \\sim C18A-C15A
 with sigma of 0.02
 C16A-C15A \\sim C17A-C16A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C13 \\sim C13A \\sim C14 \\sim C14A \\sim C15 \\sim C15A \\sim C16 \\sim C16A
\\sim C17 \\sim C17A \\sim C18A \\sim C18: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=1-FVAR(1)
 Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=
 Sof(H17)=Sof(C18)=Sof(H18)=FVAR(1)
 Fixed Sof: O9(0.25) H9A(0.25) H9B(0.25)
5.a Free rotating group:
 O8(H8A,H8B), O9(H9A,H9B)
5.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B)
5.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C45(H45), C46(H46), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C14A(H14A), C15(H15),
 C15A(H15A), C16(H16), C16A(H16A), C17(H17), C17A(H17A), C18A(H18A), C18(H18),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
5.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C)
5.e Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_shelx_res_checksum              83465
_olex2_submission_special_instructions 'No special instructions were received'