Photosalient [2 + 2] photodimerization in metal chloride-templated organic crystals
Kusumoto, Sotaro; Usuda, Kippei; Rakumitsu, Kenta; Kim, Yang; Koide, Yoshihiro; CrystEngComm 27 (2025) 2993–2997; doi:10.1039/D5CE00203F

data_7250322
_publ_section_title
;
 Photosalient [2 + 2] photodimerization in metal chloride-templated
 organic crystals
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              2993
_journal_page_last               2997
_journal_paper_doi               10.1039/D5CE00203F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'Cl6 In, Cl, 4(H2 O), C24 H24 N4'
_chemical_formula_sum            'C24 H32 Cl7 In N4 O4'
_chemical_formula_weight         803.532
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_symmetry_Int_Tables_number      85
_audit_creation_date             2025-02-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-02-19 deposited with the CCDC.	2025-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3333(5)
_cell_length_b                   13.3333(5)
_cell_length_c                   8.8676(6)
_cell_measurement_reflns_used    2520
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.6920
_cell_measurement_theta_min      2.7820
_cell_volume                     1576.45(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'DTREK_VERSION=d*TREK version 9.5W -- May 25 2006'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.9819
_diffrn_measured_fraction_theta_max 0.8396
_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  55.00   0.50   10.00    --  -10.00  45.00  90.00  168
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0098
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.9819
_diffrn_reflns_Laue_measured_fraction_max 0.8396
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3152
_diffrn_reflns_point_group_measured_fraction_full 0.9819
_diffrn_reflns_point_group_measured_fraction_max 0.8396
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       block
_exptl_crystal_F_000             808.934
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.3977
_refine_diff_density_min         -0.9334
_refine_diff_density_rms         0.1289
_refine_ls_d_res_high            0.7412
_refine_ls_d_res_low             7.3837
_refine_ls_goodness_of_fit_ref   1.0207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    15
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0207
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+2.0124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                1645
_reflns_number_total             1701
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00203f3.cif
_cod_data_source_block           240724_nnincl_uv_autored
_cod_depositor_comments
'Adding full bibliography for 7250320--7250324.cif.'
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7250322
_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.a Free rotating group:
 O1(H1b,H1c)
2.b Ternary CH refined with riding coordinates:
 C1(H1a)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C6(H6), C5(H5), C3(H3), C4(H4)
;
_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
;