Solvent-induced structural transformation in luminescence-enhanced polymorphic ionic HOFs.
Yang, Yi; Zhou, Bin; Dai, Yu-Ying; Cao, Li-Hui; Chemical communications (Cambridge, England) 62 (2026) 5691–5695; doi:10.1039/d6cc00927a

data_7135465
_publ_section_title
;
 Solvent-induced structural transformation in luminescence-enhanced
 polymorphic ionic HOFs.
;
_journal_issue                   20
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5691
_journal_page_last               5695
_journal_paper_doi               10.1039/d6cc00927a
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety
'2(C34 H36 N10), 2(C26 H16 O12 S4), 11(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C131 H152 N20 O37 S8'
_chemical_formula_weight         2855.20
_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             2026-02-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2026-02-04 deposited with the CCDC.	2026-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                96.6140(10)
_cell_angle_beta                 111.196(2)
_cell_angle_gamma                101.5510(10)
_cell_formula_units_Z            1
_cell_length_a                   13.9046(2)
_cell_length_b                   14.5770(2)
_cell_length_c                   19.1732(3)
_cell_measurement_reflns_used    25253
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.5530
_cell_measurement_theta_min      3.1340
_cell_volume                     3474.23(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.106a 64-bit (release 01-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2025/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -135.00-104.00   0.50    0.05    --  -52.00 179.00   0.00   62
  2  \w   -100.00 -47.00   0.50    0.05    --  -52.00 179.00   0.00  106
  3  \w    -54.00 -24.00   0.50    0.05    --  -39.32 125.00 -60.00   60
  4  \w    -97.00 -24.00   0.50    0.05    --  -39.32 125.00 120.00  146
  5  \w    -90.00 -15.00   0.50    0.05    --  -52.00 111.00  30.00  150
  6  \w    -59.00 -33.00   0.50    0.05    --  -52.00  55.00  11.00   52
  7  \w    -22.00  37.00   0.50    0.05    --  -39.32  55.00  11.00  118
  8  \w     59.00 107.00   0.50    0.18    --  111.82-111.00-180.00   96
  9  \w     48.00 105.00   0.50    0.18    --  111.82-111.00-120.00  114
 10  \w     38.00  64.00   0.50    0.18    --  111.82-111.00-150.00   52
 11  \w     37.00  62.00   0.50    0.18    --  111.82-111.00 -30.00   50
 12  \w     35.00 104.00   0.50    0.18    --  111.82-111.00   0.00  138
 13  \w     46.00  72.00   0.50    0.18    --  111.82-111.00  60.00   52
 14  \w     75.00 104.00   0.50    0.18    --  111.82-111.00 120.00   58
 15  \w     78.00 107.00   0.50    0.18    --  111.82-111.00 150.00   58
 16  \w     36.00  72.00   0.50    0.18    --  111.82-111.00 150.00   72
 17  \w     35.00  62.00   0.50    0.18    --  111.82-111.00 120.00   54
 18  \w     44.00 106.00   0.50    0.18    --  111.82-111.00  90.00  124
 19  \w     35.00 108.00   0.50    0.18    --  111.82-111.00  30.00  146
 20  \w     32.00  63.00   0.50    0.18    --  111.82 -94.00 -30.00   62
 21  \w     76.00 105.00   0.50    0.18    --  111.82-111.00 -30.00   58
 22  \w     60.00 108.00   0.50    0.18    --  111.82-111.00 -60.00   96
 23  \w     33.00  93.00   0.50    0.18    --  111.82 -94.00-120.00  120
 24  \w     80.00 108.00   0.50    0.18    --  111.82-111.00-150.00   56
 25  \w     43.00  69.00   0.50    0.18    --  111.82 -77.00-180.00   52
 26  \w     42.00  68.00   0.50    0.18    --  111.82 -61.00-150.00   52
 27  \w     42.00  68.00   0.50    0.18    --  111.82 -61.00 -60.00   52
 28  \w     42.00  67.00   0.50    0.18    --  111.82 -61.00-120.00   50
 29  \w    -32.00  60.00   0.50    0.05    --   39.32 -55.00-131.00  184
 30  \w     41.00  68.00   0.50    0.18    --  111.82 -61.00   0.00   54
 31  \w     39.00  66.00   0.50    0.18    --  111.82 -61.00 150.00   54
 32  \w     38.00  68.00   0.50    0.18    --  111.82 -61.00 120.00   60
 33  \w    109.00 156.00   0.50    0.18    --  111.82 111.00-120.00   94
 34  \w     85.00 174.00   0.50    0.18    --  111.82 111.00-150.00  178
 35  \w    113.00 173.00   0.50    0.18    --  111.82 111.00-180.00  120
 36  \w     97.00 153.00   0.50    0.18    --  111.82  77.00-120.00  112
 37  \w     84.00 159.00   0.50    0.18    --  111.82  61.00 -60.00  150
 38  \w     84.00 165.00   0.50    0.18    --  111.82  61.00 -90.00  162
 39  \w    104.00 173.00   0.50    0.18    --  111.82  77.00 -30.00  138
 40  \w    101.00 175.00   0.50    0.18    --  111.82  45.00   0.00  148
 41  \w     86.00 136.00   0.50    0.18    --  111.82  55.00  11.00  100
 42  \w    142.00 170.00   0.50    0.18    --  111.82  55.00  11.00   56
 43  \w     83.00 150.00   0.50    0.18    --  111.82  61.00 150.00  134
 44  \w     38.00 174.00   0.50    0.18    --  111.82   0.00 150.00  272
 45  \w     19.00 116.00   0.50    0.05    --   39.32  55.00  11.00  194
 46  \w   -107.00 -13.00   0.50    0.05    --  -39.32 -55.00-131.00  188
 47  \w   -101.00 -76.00   0.50    0.05    --  -52.00 -55.00-131.00   50
 48  \w   -129.00 -89.00   0.50    0.05    --  -52.00 -94.00 -30.00   80
 49  \w   -131.00 -90.00   0.50    0.05    --  -52.00 -94.00   0.00   82
 50  \w   -131.00-105.00   0.50    0.05    --  -52.00 -94.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0835288000
_diffrn_orient_matrix_UB_12      -0.0976756000
_diffrn_orient_matrix_UB_13      -0.0294795000
_diffrn_orient_matrix_UB_21      0.0829579000
_diffrn_orient_matrix_UB_22      -0.0461143000
_diffrn_orient_matrix_UB_23      0.0505249000
_diffrn_orient_matrix_UB_31      -0.0360030000
_diffrn_orient_matrix_UB_32      0.0219298000
_diffrn_orient_matrix_UB_33      0.0658188000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43221
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.799
_diffrn_reflns_theta_min         2.526
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.106a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       needle
_exptl_crystal_F_000             1502
_exptl_crystal_recrystallization_method
'The crystals were growth by means of evaporation of a mixture of DMSO, MeOH and H2O at RT.'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         14122
_refine_ls_number_restraints     763
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0996P)^2^+2.1484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11948
_reflns_number_total             14122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc00927a2.cif
_cod_data_source_block           5194-clh-zb-2
_cod_depositor_comments
'Adding full bibliography for 7135464--7135465.cif.'
_cod_original_cell_volume        3474.23(10)
_cod_database_code               7135465
_shelx_shelxl_version_number     2025/1
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.449
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately coated
 with PDMS (polydimethylsiloxane/Dimethicone, CAS: 9006-65-9 on a glass slide.
 A suitable single crystal was selected and mounted on a glass fiber using
 vacuum silicone grease as adhesive. The glass fiber with single crystal was
 mounted on copper pin with solid paraffin. Operator: DJ_Tokyo.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O14-C61 = O14A-C61A = C61B-O14B = O14C-C61C = O14D-C61D = O14F-C61F = C61E-
 O14E = O14G-C61G = O14H-C61H
 1.43 with sigma of 0.01
 O15D-C62D = O15C-C62C = O15E-C62E = O15F-C62F = O15-C62 = O15A-C62A = O15B-C62B
 1.43 with sigma of 0.01
 O15D-C62D
 1.43 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O15C \\sim C62C \\sim O15D \\sim C62D \\sim O15E \\sim C62E \\sim O15F \\sim
C62F \\sim O15 \\sim C62 \\sim C62A \\sim O15A \\sim O15B \\sim C62B: within 3A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3A
C61A \\sim O14A \\sim C61 \\sim O14 \\sim C61B \\sim O14B \\sim O14C \\sim C61C
\\sim O14D \\sim C61D \\sim O14F \\sim C61F \\sim C61E \\sim O14E \\sim O14G
\\sim C61G \\sim O14H \\sim C61H: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3A
O13A \\sim O13: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
4. Others
 1*[Sof(O14)+Sof(C61)]+1*[Sof(C61A)+Sof(O14A)]+1*[Sof(C61B)+Sof(O14B)]+1*
 [Sof(O14E)+Sof(C61E)]+1*[Sof(O14C)+Sof(C61C)]+1*[Sof(C61D)+Sof(O14D)]+1*
 [Sof(C61F)+Sof(O14F)]+1*[Sof(C61G)+Sof(O14G)]+1*[Sof(C61H)+Sof(O14H)]=3 with
 esd of 0
 1*[Sof(O15C)+Sof(C62C)]+1*[Sof(O15D)+Sof(C62D)]+1*[Sof(C62E)+Sof(O15E)]+1*
 [Sof(O15F)+Sof(C62F)]+1*[Sof(O15)+Sof(C62)]+1*[Sof(C62A)+Sof(O15A)]+1*
 [Sof(O15B)+Sof(C62B)]=2.5 with esd of 0
 Sof(O15)=Sof(C62)=FVAR(1)
 Sof(O14)=Sof(C61)=FVAR(2)
 Sof(C61A)=Sof(O14A)=FVAR(3)
 Sof(O15C)=Sof(C62C)=FVAR(4)
 Sof(C61B)=Sof(O14B)=FVAR(5)
 Sof(O15D)=Sof(C62D)=FVAR(6)
 Sof(O14E)=Sof(C61E)=FVAR(7)
 Sof(O13A)=Sof(H13C)=Sof(H13D)=1-FVAR(8)
 Sof(O13)=Sof(H13A)=Sof(H13B)=FVAR(8)
 Sof(O14C)=Sof(C61C)=FVAR(9)
 Sof(C61D)=Sof(O14D)=FVAR(10)
 Sof(C61F)=Sof(O14F)=FVAR(11)
 Sof(C61G)=Sof(O14G)=FVAR(12)
 Sof(C61H)=Sof(O14H)=FVAR(13)
 Sof(C62A)=Sof(O15A)=FVAR(14)
 Sof(O15B)=Sof(C62B)=FVAR(15)
 Sof(C62E)=Sof(O15E)=FVAR(16)
 Sof(O15F)=Sof(C62F)=FVAR(17)
5.a Riding coordinates:
 O13(H13A,H13B), O13A(H13C,H13D)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C11(H11), C25(H25), C22(H22), C6(H6), C19(H19), C26(H26), C10(H10),
 C4(H4), C7(H7), C17(H17), C14(H14), C3(H3), C16(H16), C23(H23), C20(H20),
 C45(H45), C55(H55), C58(H58), C46(H46), C51(H51), C48(H48), C56(H56), C52(H52),
  C59(H59), C49(H49), C29(H29), C42(H42), C31(H31), C35(H35), C41(H41),
 C38(H38), C39(H39), C28(H28), C32(H32), C34(H34)
5.c X=CH2 refined with riding coordinates:
 N7(H7A,H7B), N8(H8A,H8B), N9(H9A,H9B), N10(H10A,H10B), N4(H4A,H4B), N3(H3A,
 H3B), N2(H2A,H2B), N5(H5A,H5B)
;
_shelx_res_checksum              54632
_shelx_hkl_checksum              90137
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.954
_oxdiff_exptl_absorpt_empirical_full_min 0.374