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_1574704
_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         '2(C40 H38 P2), 2(C12 H8 O6 S2), 3(H2 O)'
_chemical_formula_sum            'C104 H98 O15 P4 S4'
_chemical_formula_weight         1839.94
_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     iterative
_audit_creation_date             2023-12-20
_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                70.458(2)
_cell_angle_beta                 77.061(2)
_cell_angle_gamma                71.936(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5835(13)
_cell_length_b                   14.1726(18)
_cell_length_c                   17.216(2)
_cell_measurement_reflns_used    5036
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.228
_cell_measurement_theta_min      2.534
_cell_volume                     2292.7(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15820
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.200
_diffrn_reflns_theta_min         1.577
_diffrn_source_current           25.0
_diffrn_source_power             1.125
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1440 before and 0.0338 after correction.
The Ratio of minimum to maximum transmission is 0.8278.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             966
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         11857
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0822P)^2^+0.5893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8309
_reflns_number_total             11857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02039e2.cif
_cod_data_source_block           smx_231217
_cod_depositor_comments
'Adding full bibliography for 1574702--1574705.cif.'
_cod_database_code               1574704
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.963
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
S1 \\sim O3 \\sim O1 \\sim O2 \\sim O3A \\sim O1A \\sim O2A: within 3A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3A
3. Others
 Sof(O3A)=Sof(O1A)=Sof(O2A)=1-FVAR(1)
 Sof(O3)=Sof(O1)=Sof(O2)=FVAR(1)
 Fixed Sof: O8(0.5) H8A(0.5) H8B(0.5)
4.a Riding coordinates:
 O7(H7A,H7B)
4.b Free rotating group:
 O8(H8A,H8B)
4.c Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B)
4.d Aromatic/amide H refined with riding coordinates:
 C24(H24), C6(H6), C20(H20), C36(H36), C32(H32), C49(H49), C51(H51), C5(H5),
 C12(H12), C30(H30), C18(H18), C45(H45), C48(H48), C2(H2), C26(H26), C52(H52),
 C34(H34), C14(H14), C33(H33), C35(H35), C23(H23), C21(H21), C8(H8), C43(H43),
 C42(H42), C46(H46), C22(H22), C27(H27), C4(H4), C16(H16), C15(H15), C10(H10),
 C17(H17), C29(H29), C11(H11), C3(H3), C28(H28), C9(H9)
;
_shelx_res_checksum              11178
_olex2_submission_special_instructions 'No special instructions were received'