A solvent-controlled photoresponsive ionic hydrogen-bonded organic framework for encryption applications.
Huang, Ming-Feng; Cao, Li-Hui; Zhou, Bin; Chemical communications (Cambridge, England) 60 (2024) 3437–3440; doi:10.1039/d4cc00701h

data_7132775
_publ_section_title
;
 A solvent-controlled photoresponsive ionic hydrogen-bonded organic
 framework for encryption applications.
;
_journal_issue                   25
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3437
_journal_page_last               3440
_journal_paper_doi               10.1039/d4cc00701h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C26 H16 O12 S4, 2(C4 H9 N O), 2(C14 H16 N4)'
_chemical_formula_sum            'C62 H66 N10 O14 S4'
_chemical_formula_weight         1303.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-02-05 deposited with the CCDC.	2024-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.542(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.9540(19)
_cell_length_b                   10.7480(8)
_cell_length_c                   24.5839(8)
_cell_measurement_reflns_used    4947
_cell_measurement_temperature    212.99(10)
_cell_measurement_theta_max      68.6480
_cell_measurement_theta_min      3.5760
_cell_volume                     10009.3(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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      213.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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   -111.00 -70.00   1.00    0.80    --  -48.42-137.00  48.00   41
  2  \w   -136.00-111.00   1.00    3.00    --  -91.75-137.00  48.00   25
  3  \w   -163.00 -86.00   1.00    3.00    --  -91.75 -99.00   0.00   77
  4  \w   -120.00 -70.00   1.00    0.80    --  -48.42-132.00-134.00   50
  5  \w   -116.00 -91.00   1.00    3.00    --  -91.75-132.00-134.00   25
  6  \w   -161.00 -77.00   1.00    3.00    --  -91.75 -57.00  90.00   84
  7  \w     54.00  99.00   1.00    0.80    --   48.42-137.00  48.00   45
  8  \w     90.00 116.00   1.00    3.00    --  106.65-132.00-134.00   26
  9  \w     54.00 119.00   1.00    3.00    --  106.65-137.00  48.00   65
 10  \w     74.00 106.00   1.00    3.00    --  106.65 -99.00 150.00   32
 11  \w     44.00  70.00   1.00    0.80    --   48.42-132.00-134.00   26
 12  \w     38.00 106.00   1.00    3.00    --  106.65 -99.00-150.00   68
 13  \w     39.00 105.00   1.00    3.00    --  106.65 -77.00-120.00   66
 14  \w     41.00  66.00   1.00    3.00    --  106.65 -57.00-120.00   25
 15  \w     34.00  66.00   1.00    3.00    --  106.65 -57.00 -90.00   32
 16  \w     36.00  89.00   1.00    3.00    --  106.65 -77.00  30.00   53
 17  \w    124.00 173.00   1.00    3.00    --  106.65  38.00 120.00   49
 18  \w    108.00 133.00   1.00    3.00    --  106.65 137.00 111.00   25
 19  \w     92.00 149.00   1.00    3.00    --  106.65 132.00 -65.00   57
 20  \w    -42.00  25.00   1.00    0.80    --  -48.42  38.00-120.00   67
 21  \w    -94.00 -69.00   1.00    0.80    --  -48.42 137.00 111.00   25
 22  \w    -23.00  27.00   1.00    0.80    --  -48.42  19.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31509
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         66.000
_diffrn_reflns_theta_min         3.603
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.865
_exptl_crystal_description       needle
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8619
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0751
_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^)+(0.1384P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2137
_refine_ls_wR_factor_ref         0.2297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5553
_reflns_number_total             8619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00701h2.cif
_cod_data_source_block           hmf20221014_sq
_cod_depositor_comments
'Adding full bibliography for 7132775--7132776.cif.'
_cod_original_cell_volume        10009.4(9)
_cod_database_code               7132775
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.744
_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 C(H,H,H) groups
2. Restrained distances
 N5-C29
 1.55 with sigma of 0.02
 C31-C29
 1.5 with sigma of 0.02
 C31-C30
 3 with sigma of 0.02
 N5-C29 \\sim N5-C30 \\sim N5-C28
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C27(H27), C4(H4), C9(H9), C10(H10), C13(H13), C16(H16), C17(H17), C18(H18),
 C19(H19)
3.b X=CH2 refined with riding coordinates:
 N1(H1a,H1b), N2(H2a,H2b), N3(H3a,H3b), N4(H4a,H4b)
3.c Idealised Me refined as rotating group:
 C28(H28a,H28b,H28c), C30(H30a,H30b,H30c), C31(H31a,H31b,H31c)
;
_shelx_res_checksum              54637
_shelx_hkl_checksum              41687
_shelx_fab_checksum              67595
_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
;