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_1574703
_publ_section_title
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 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
'C40 H38 P2, 0.5(C16 H6 O12 S4), 2(C H4 O), 3(H2 O)'
_chemical_formula_sum            'C50 H55 O11 P2 S2'
_chemical_formula_weight         958.00
_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     dual
_audit_creation_date             2024-01-05
_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                 106.827(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4375(15)
_cell_length_b                   19.787(2)
_cell_length_c                   18.4255(19)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      31.017
_cell_measurement_theta_min      2.213
_cell_volume                     4689.4(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0246
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28540
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.547
_diffrn_source_current           25.0
_diffrn_source_power             1.125
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1298 before and 0.0417 after correction.
The Ratio of minimum to maximum transmission is 0.8132.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         10711
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0572P)^2^+2.9471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8934
_reflns_number_total             10711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02039e2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1574702--1574705.cif.'
_cod_database_code               1574703
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.962
_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
 O10-C50 \\sim O10A-C50A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O10 \\sim C50 \\sim O10A \\sim C50A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O10A \\sim C50A: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
4. Others
 Sof(O10A)=Sof(H10B)=Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(1)
 Sof(O10)=Sof(H10A)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1)
5.a Riding coordinates:
 C50(H50A,H50B,H50C), C50A(H50D,H50E,H50F)
5.b Free rotating group:
 O11(H11A,H11B), O9(H9A,H9B), O7(H7A,H7B)
5.c Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C20(H20A,H20B), C21(H21A,H21B), C19(H19A,H19B)
5.d Aromatic/amide H refined with riding coordinates:
 C48(H48), C47(H47), C42(H42), C18(H18), C6(H6), C12(H12), C17(H17), C8(H8),
 C28(H28), C2(H2), C15(H15), C36(H36), C40(H40), C14(H14), C27(H27), C38(H38),
 C37(H37), C26(H26), C16(H16), C30(H30), C3(H3), C4(H4), C11(H11), C24(H24),
 C39(H39), C9(H9), C34(H34), C5(H5), C31(H31), C32(H32), C25(H25), C10(H10),
 C33(H33)
5.e Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C)
5.f Idealised tetrahedral OH refined as rotating group:
 O8(H8A), O10(H10A), O10A(H10B)
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_shelx_res_checksum              20090
_olex2_submission_special_instructions 'No special instructions were received'