Multi-hydrophilic groups synergistic assembly ionic HOFs with multiple-water clusters and superprotonic single-crystal conductivity.
Li, Shu-Hui; Cao, Li-Hui; Zhang, Wenmin; Bai, Xiang-Tian; Chen, Xu-Yong; Chemical communications (Cambridge, England) 61 (2025) 4034–4037; doi:10.1039/d4cc06654e

data_7134247
_publ_section_title
;
 Multi-hydrophilic groups synergistic assembly ionic HOFs with
 multiple-water clusters and superprotonic single-crystal conductivity.
;
_journal_issue                   20
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4034
_journal_page_last               4037
_journal_paper_doi               10.1039/d4cc06654e
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         '4(C10 H6 O8 S2), 2(C29 H32 N8), 39(H2 O)'
_chemical_formula_sum            'C98 H166 N16 O71 S8'
_chemical_formula_weight         2960.94
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-10-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-11-29 deposited with the CCDC.	2025-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                102.8797(19)
_cell_angle_beta                 95.113(2)
_cell_angle_gamma                95.376(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8167(5)
_cell_length_b                   16.0738(6)
_cell_length_c                   32.1757(12)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.743
_cell_measurement_theta_min      2.836
_cell_volume                     6890.7(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            97888
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.812
_diffrn_reflns_theta_min         2.836
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.95
_diffrn_source_power             0.0475
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.120
_exptl_absorpt_correction_T_max  0.0872
_exptl_absorpt_correction_T_min  0.0091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1335 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.1044.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3124
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1898
_refine_ls_number_reflns         28158
_refine_ls_number_restraints     206
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0809
_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^)+(0.1609P)^2^+0.3473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21340
_reflns_number_total             28158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06654e2.cif
_cod_data_source_block           cu_0821_9_0m
_cod_depositor_comments
'Adding full bibliography for 7134247--7134248.cif.'
_cod_database_code               7134247
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
O54A \\sim O54: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O49A \\sim O49: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O67 \\sim O68 \\sim O68B \\sim O68A \\sim O67A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
O65 \\sim O63 \\sim O63A \\sim O65B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O40A \\sim O40: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O45: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O34A \\sim O34: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O5A \\sim O50: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O37A \\sim O37: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O71 \\sim O71A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O41 \\sim O41A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O62 \\sim O62A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O67) \\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O68B) \\sim Ueq, Uanis(O68A)
\\sim Ueq, Uanis(O67A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O40) \\sim Ueq, Uanis(O40A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O34) \\sim Ueq, Uanis(O34A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O45) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O37) \\sim Ueq, Uanis(O37A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O71A) \\sim Ueq, Uanis(O71) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O41A) \\sim Ueq, Uanis(O41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O62A) \\sim Ueq, Uanis(O62) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O65) \\sim Ueq, Uanis(O65B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
2. Others
 1*[Sof(O67)+Sof(H67A)+Sof(H67B)]+1*[Sof(H68A)+Sof(H68B)+Sof(O68)]+1*
 [Sof(O68A)+Sof(H68C)+Sof(H68D)]+1*[Sof(O68B)+Sof(H68E)+Sof(H68F)]+1*[Sof(O67A)+
 Sof(H67C)+Sof(H67D)]=2 with esd of 0.00001
 1*[Sof(O65)+Sof(H65A)+Sof(H65B)]+1*[Sof(O63)+Sof(H63A)+Sof(H63B)]+1*
 [Sof(O63A)+Sof(H63C)+Sof(H63D)]+1*[Sof(O65B)+Sof(H65C)+Sof(H65D)]+1*[Sof(O45)+
 Sof(H45A)+Sof(H45B)]=2 with esd of 0.00001
 Sof(O54A)=Sof(H54C)=Sof(H54D)=1-FVAR(1)
 Sof(O54)=Sof(H54A)=Sof(H54B)=FVAR(1)
 Sof(O67)=Sof(H67A)=Sof(H67B)=FVAR(2)
 Sof(O65)=Sof(H65A)=Sof(H65B)=FVAR(3)
 Sof(O5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(4)
 Sof(O50)=Sof(H50A)=Sof(H50B)=FVAR(4)
 Sof(O49A)=Sof(H49C)=Sof(H49D)=1-FVAR(5)
 Sof(O49)=Sof(H49A)=Sof(H49B)=FVAR(5)
 Sof(H68A)=Sof(H68B)=Sof(O68)=FVAR(6)
 Sof(O63)=Sof(H63A)=Sof(H63B)=FVAR(7)
 Sof(O40A)=Sof(H40C)=Sof(H40D)=1-FVAR(8)
 Sof(O40)=Sof(H40A)=Sof(H40B)=FVAR(8)
 Sof(O37A)=Sof(H37C)=Sof(H37D)=1-FVAR(9)
 Sof(O37)=Sof(H37A)=Sof(H37B)=FVAR(9)
 Sof(O71A)=Sof(H71C)=Sof(H71D)=1-FVAR(10)
 Sof(O71)=Sof(H71A)=Sof(H71B)=FVAR(10)
 Sof(O34A)=Sof(H34C)=Sof(H34D)=1-FVAR(11)
 Sof(O34)=Sof(H34A)=Sof(H34B)=FVAR(11)
 Sof(O41A)=Sof(H41C)=Sof(H41D)=1-FVAR(12)
 Sof(O41)=Sof(H41A)=Sof(H41B)=FVAR(12)
 Sof(O62A)=Sof(H62C)=Sof(H62D)=1-FVAR(13)
 Sof(O62)=Sof(H62A)=Sof(H62B)=FVAR(13)
 Sof(O68A)=Sof(H68C)=Sof(H68D)=FVAR(14)
 Sof(O68B)=Sof(H68E)=Sof(H68F)=FVAR(15)
 Sof(O67A)=Sof(H67C)=Sof(H67D)=FVAR(16)
 Sof(O63A)=Sof(H63C)=Sof(H63D)=FVAR(17)
 Sof(O65B)=Sof(H65C)=Sof(H65D)=FVAR(18)
 Sof(O45)=Sof(H45A)=Sof(H45B)=FVAR(19)
 Fixed X: O49(0.648971) O68A(0.261981)
3.a Riding coordinates:
 O24(H24A), O12(H12), O28(H28A), O8(H8), O16(H16C), O32(H32), O33(H33A,H33B),
 O69(H69A,H69B), O36(H36A,H36B), O47(H47A,H47B), O51(H51A,H51B), O42(H42A,H42B),
  O43(H43A,H43B), O56(H56A,H56B), O49(H49A,H49B), O48(H48A,H48B), O58(H58A,
 H58B), O52(H52A,H52B), O59(H59A,H59B), O57(H57A,H57B), O38(H38A,H38B),
 O46(H46A,H46B), O53(H53A,H53B), O44(H44A,H44B), O54(H54A,H54B), O61(H61A,H61B),
  O60(H60A,H60B), O34(H34A,H34B), O55(H55A,H55B), O70(H70A,H70B), O62(H62A,
 H62B), O72(H72A,H72B), O64(H64A,H64B), O67(H67A,H67B), O66(H66A,H66B),
 O50(H50A,H50B), O41(H41A,H41B), O37(H37A,H37B), O71(H71A,H71B), O39(H39A,H39B),
  O45(H45A,H45B), O40(H40A,H40B), O40(H68A,H68B), O65(H65A,H65B), O63(H63A,
 H63B), O54A(H54C,H54D), O67A(H67C,H67D), O49A(H49C,H49D), O68A(H68C,H68D),
 O63A(H63C,H63D), O40A(H40C,H40D), O37A(H37C,H37D), O71A(H71C,H71D), O34A(H34C,
 H34D), O41A(H41C,H41D), O62A(H62C,H62D), O68B(H68E,H68F), O65B(H65C,H65D)
3.b Free rotating group:
 O3AA(H3AA,H3AB), O5A(H5AA,H5AB)
3.c Aromatic/amide H refined with riding coordinates:
 C79(H79), C46(H46), C1(H1), C56(H56), C67(H67), C7(H7), C63(H63), C43(H43),
 C88(H88), C89(H89), C85(H85), C62(H62), C74(H74), C95(H95), C76(H76), C49(H49),
  C40(H40), C21(H21), C52(H52), C4(H4C), C59(H59), C10(H10), C82(H82), C66(H66),
  C70(H70), C77(H77), C69(H69), C53(H53), C30(H30), C17(H17), C27(H27),
 C20(H20), C55(H55), C38(H38), C73(H73), C23(H23), C60(H60), C34(H34), C24(H24),
  C31(H31), C37(H37), C92(H92), C16(H16), C98(H98), C14(H14), C28(H28),
 C13(H13), C35(H35)
3.d X=CH2 refined with riding coordinates:
 N15(H15A,H15B), N16(H16A,H16B), N10(H10A,H10B), N6(H6A,H6B), N3(H3A,H3B),
 N14(H14A,H14B), N12(H12A,H12B), N2(H2A,H2B), N5(H5A,H5B), N9(H9A,H9B), N4(H4A,
 H4B), N1(H1A,H1B), N13(H13A,H13B), N11(H11A,H11B), N8(H8A,H8B), N7(H7A,H7B)
3.e Idealised tetrahedral OH refined as rotating group:
 O20(H20A), O4(H4)
;
_shelx_res_checksum              18602
_shelx_hkl_checksum              27067
_olex2_submission_special_instructions 'No special instructions were received'