Photosalient effect and reversible photochromic photoluminescence driven by cascade [2 + 2] cycloaddition reaction and water adsorption in a 0D hybrid metal halide.
Chen, Chudong; Li, Ziquan; Xiao, Yonghong; Ye, Chenghao; Wei, Jianwu; Zeng, Ruosheng; Pang, Qi; Luo, Binbin; Chemical science 16 (2025) 13731–13740; doi:10.1039/d5sc03344f

data_1574921
_publ_section_title
;
 Photosalient effect and reversible photochromic photoluminescence driven
 by cascade [2 + 2] cycloaddition reaction and water adsorption in a 0D
 hybrid metal halide.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              13731
_journal_page_last               13740
_journal_paper_doi               10.1039/d5sc03344f
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'Cl5 In, Cl5 H2 In O, 2(C26 H24 N2)'
_chemical_formula_sum            'C52 H50 Cl10 In2 N4 O'
_chemical_formula_weight         1331.10
_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
_audit_creation_date             2025-03-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-03-29 deposited with the CCDC.	2025-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.349(2)
_cell_angle_beta                 91.409(2)
_cell_angle_gamma                95.489(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8121(3)
_cell_length_b                   15.0764(5)
_cell_length_c                   18.0060(4)
_cell_measurement_reflns_used    9598
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.6590
_cell_measurement_theta_min      3.8040
_cell_volume                     2920.67(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.950
_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    -29.00  28.00   0.50    1.17    --    0.00 -38.00  90.00  114
  2  \w     61.00  89.00   0.50    1.17    --    0.00  57.00  90.00   56
  3  \w    -25.00  29.00   0.50    1.17    --    0.00 -38.00-120.00  108
  4  \w    -78.00 -41.00   0.50    1.17    --    0.00 -38.00  90.00   74
  5  \w    -84.00 -48.00   0.50    1.17    --    0.00 -38.00-120.00   72
  6  \w    -24.00  27.00   0.50    1.17    --    0.00  57.00  90.00  102
  7  \w     53.00 130.00   0.50    4.67    --   93.30 -82.00-150.00  154
  8  \w      9.00  38.00   0.50    4.67    --   93.30 -82.00-150.00   58
  9  \w      5.00  31.00   0.50    4.67    --   93.30 -77.00 -60.00   52
 10  \w     34.00 128.00   0.50    4.67    --   93.30 -82.00  90.00  188
 11  \w     26.00  79.00   0.50    4.67    --   93.30  15.00 -30.00  106
 12  \w    104.00 183.00   0.50    4.67    --   93.30  15.00 -30.00  158
 13  \w      4.00  30.00   0.50    4.67    --   93.30 -82.00 -60.00   52
 14  \w      4.00 111.00   0.50    4.67    --   93.30 -61.00  90.00  214
 15  \w      4.00  90.00   0.50    4.67    --   93.30 -30.00 -30.00  172
 16  \w     14.00  99.00   0.50    4.67    --   93.30 -45.00 -30.00  170
 17  \w     62.00  97.00   0.50    4.67    --   93.30 -77.00 -60.00   70
 18  \w      8.00 122.00   0.50    4.67    --   93.30 -61.00-150.00  228
 19  \w    136.00 183.00   0.50    4.67    --   93.30  15.00-120.00   94
 20  \w     65.00 130.00   0.50    4.67    --   93.30 -82.00 -60.00  130
 21  \w     55.00 106.00   0.50    4.67    --   93.30 -82.00  30.00  102
 22  \w     22.00  77.00   0.50    4.67    --   93.30  15.00-120.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1008179000
_diffrn_orient_matrix_UB_12      -0.0592753000
_diffrn_orient_matrix_UB_13      0.0402831000
_diffrn_orient_matrix_UB_21      -0.0569273000
_diffrn_orient_matrix_UB_22      -0.0334845000
_diffrn_orient_matrix_UB_23      -0.0755098000
_diffrn_orient_matrix_UB_31      0.0842483000
_diffrn_orient_matrix_UB_32      -0.0768374000
_diffrn_orient_matrix_UB_33      0.0008604000
_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  0.0786
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28502
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.365
_diffrn_reflns_theta_min         3.819
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    10.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.079
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         11166
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0744P)^2^+5.4551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8118
_reflns_number_total             11166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03344f11.cif
_cod_data_source_block           1i
_cod_depositor_comments
'Adding full bibliography for 1574919--1574921.cif.'
_cod_database_code               1574921
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         InClCNHO
_chemical_oxdiff_usercomment     Stpy-InCl3-450-wushui
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.614
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
N3B \\sim N4B \\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A
\\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39A
\\sim C40A \\sim C41A \\sim C42A \\sim C43A \\sim C44A \\sim C45A \\sim C46A
\\sim C47A \\sim C48A \\sim C49A \\sim C50A \\sim C51A \\sim C52A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N3 \\sim N4 \\sim C27B \\sim C28B \\sim C29B \\sim C30B \\sim C31B \\sim C32B
\\sim C33B \\sim C34B \\sim C35B \\sim C36B \\sim C37B \\sim C38B \\sim C39B
\\sim C40B \\sim C41B \\sim C42B \\sim C43B \\sim C44B \\sim C45B \\sim C46B
\\sim C47B \\sim C48B \\sim C49B \\sim C50B \\sim C51B \\sim C52B: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
 Sof(N3)=Sof(H3A)=Sof(C30B)=Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=Sof(C27B)=
 Sof(H27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29B)=Sof(C33B)=Sof(H33B)=
 Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(C36B)=Sof(H36B)=Sof(C37B)=Sof(H37B)=
 Sof(C38B)=Sof(H38B)=Sof(C39B)=Sof(H39B)=Sof(C43B)=Sof(C44B)=Sof(H44B)=
 Sof(C45B)=Sof(H45B)=Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41B)=Sof(C42B)=
 Sof(H42B)=Sof(C46B)=Sof(H46B)=Sof(C47B)=Sof(H47B)=Sof(C48B)=Sof(C49B)=
 Sof(H49B)=Sof(C50B)=Sof(H50B)=Sof(N4)=Sof(H4)=Sof(C51B)=Sof(H51B)=Sof(C52B)=
 Sof(H52B)=1-FVAR(1)
 Sof(N4B)=Sof(H4B)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=
 Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(N3B)=
 Sof(H3B)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=
 Sof(H41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=
 Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(C49A)=
 Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=Sof(C52A)=Sof(H52A)=FVAR(1)
4.a Rotating group:
 O1(H1B,H1C)
4.b Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C20(H20), C21(H21), C33A(H33A), C33B(H33B), C34A(H34A),
 C34B(H34B), C46A(H46A), C46B(H46B), C47A(H47A), C47B(H47B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C1(H1A), C2(H2A), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C23(H23),
  C24(H24), C25(H25), C26(H26), N3(H3A), N4B(H4B), C27A(H27A), C28A(H28A),
 C29A(H29A), C31B(H31B), C32B(H32B), C27B(H27B), C28B(H28B), C29B(H29B),
 C31A(H31A), C32A(H32A), C36A(H36A), C37A(H37A), N3B(H3B), C38A(H38A),
 C39A(H39A), C36B(H36B), C37B(H37B), C38B(H38B), C39B(H39B), C40A(H40A),
 C41A(H41A), C42A(H42A), C44B(H44B), C45B(H45B), C40B(H40B), C41B(H41B),
 C42B(H42B), C44A(H44A), C45A(H45A), C49B(H49B), C50B(H50B), N4(H4), C51B(H51B),
  C52B(H52B), C49A(H49A), C50A(H50A), C51A(H51A), C52A(H52A)
4.d Fitted hexagon refined as free rotating group:
 C30B(C31B,C32B,C27B,C28B,C29B), C35A(C36A,C37A,N3B,C38A,C39A), C43B(C44B,C45B,
 C40B,C41B,C42B), C48B(C49B,C50B,N4,C51B,C52B)
;
_shelx_res_checksum              49650
_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 1.887
_oxdiff_exptl_absorpt_empirical_full_min 0.595