Solvent-induced conformational changes in color-tunable hydrogen-bonded organic frameworks.
Hu, Longhao; Lin, Chaohui; Zeng, Dailin; Qin, Xianjiao; Lai, Xiao-Li; Gong, Lingshan; Ye, Yingxiang; AlShahrani, Thamraa; Ma, Shengqian; Chemical communications (Cambridge, England) 61 (2025) 17882–17885; doi:10.1039/d5cc03791c

data_7135075
_publ_section_title
;
 Solvent-induced conformational changes in color-tunable hydrogen-bonded
 organic frameworks.
;
_journal_issue                   91
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              17882
_journal_page_last               17885
_journal_paper_doi               10.1039/d5cc03791c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C38 H30 N2 O8, 1[C4H8O]'
_chemical_formula_sum            'C42 H38 N2 O9'
_chemical_formula_weight         714.74
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-10-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-10-07 deposited with the CCDC.	2025-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                83.657(5)
_cell_angle_beta                 78.757(5)
_cell_angle_gamma                84.862(5)
_cell_formula_units_Z            1
_cell_length_a                   5.9506(4)
_cell_length_b                   11.9443(8)
_cell_length_c                   13.0049(8)
_cell_measurement_reflns_used    3124
_cell_measurement_temperature    293.4(2)
_cell_measurement_theta_max      72.7110
_cell_measurement_theta_min      3.4310
_cell_volume                     898.85(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.4(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.964
_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    -75.00  33.00   1.00    1.00    --  -40.32  86.00 144.00  108
  2  \w      6.00  54.00   1.00    1.00    --   40.32 -86.00  26.00   48
  3  \w    114.00 139.00   1.00    5.00    --  103.24  86.00 144.00   25
  4  \w     64.00 104.00   1.00    5.00    --  103.24 -86.00  26.00   40
  5  \w    -86.00 -16.00   1.00    1.00    --  -40.32 -38.00-150.00   70
  6  \w   -100.00 -13.00   1.00    1.00    --  -40.32 -57.00 -30.00   87
  7  \w     73.00 113.00   1.00    1.00    --   40.32  57.00 -90.00   40
  8  \w     15.00  52.00   1.00    1.00    --   40.32  57.00 -90.00   37
  9  \w     30.00 116.00   1.00    5.00    --  103.24-125.00  60.00   86
 10  \w     77.00 167.00   1.00    5.00    --  103.24  45.00 -30.00   90
 11  \w     21.00 102.00   1.00    5.00    --  103.24 -94.00-180.00   81
 12  \w     30.00  69.00   1.00    5.00    --  103.24-125.00 -30.00   39
 13  \w     31.00 131.00   1.00    5.00    --  103.24 -30.00   0.00  100
 14  \w     73.00 108.00   1.00    5.00    --  103.24-125.00 -30.00   35
 15  \w    129.00 170.00   1.00    5.00    --  103.24  45.00-180.00   41
 16  \w     38.00 116.00   1.00    5.00    --  103.24-125.00-180.00   78
 17  \w    126.00 151.00   1.00    5.00    --  103.24 125.00-150.00   25
 18  \w    127.00 158.00   1.00    5.00    --  103.24 125.00  90.00   31
 19  \w     75.00 177.00   1.00    5.00    --  103.24  30.00-120.00  102
 20  \w     38.00 106.00   1.00    5.00    --  103.24 -45.00-180.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1212003000
_diffrn_orient_matrix_UB_12      0.1189993000
_diffrn_orient_matrix_UB_13      0.0086942000
_diffrn_orient_matrix_UB_21      0.0677047000
_diffrn_orient_matrix_UB_22      0.0029614000
_diffrn_orient_matrix_UB_23      0.1080746000
_diffrn_orient_matrix_UB_31      0.2252562000
_diffrn_orient_matrix_UB_32      0.0524771000
_diffrn_orient_matrix_UB_33      -0.0544538000
_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  0.0451
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6823
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.753
_diffrn_reflns_theta_min         3.481
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane and Tetrahydrofuran'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1173P)^2^+0.0439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2632
_reflns_number_total             3445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03791c2.cif
_cod_data_source_block           4E-THF
_cod_depositor_comments
'Adding full bibliography for 7135075--7135076.cif.'
_cod_database_code               7135075
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N'
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C14(H14), C15(H15), C4(H4), C16(H16), C9(H9), C6(H6), C13(H13), C5(H5)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 43 electrons were 
found in a volume of 170\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H8O] per formula unit 
which account for 40 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85051
_shelx_hkl_checksum              6460
_shelx_fab_checksum              55208
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.280
_oxdiff_exptl_absorpt_empirical_full_min 0.406