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_7250320
_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         'Cl5 H2 In O, H2 O, C12 H12 N2'
_chemical_formula_sum            'C12 H16 Cl5 In N2 O2'
_chemical_formula_weight         512.354
_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'
_symmetry_Int_Tables_number      15
_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                 95.665(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6884(5)
_cell_length_b                   13.4365(4)
_cell_length_c                   14.1149(4)
_cell_measurement_reflns_used    5718
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.7790
_cell_measurement_theta_min      2.2710
_cell_volume                     3527.04(17)
_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 1.3 (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 0.9837
_diffrn_measured_fraction_theta_max 0.8112
_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   -100.00  68.00   0.50    5.00    --  -10.00  45.00  90.00  336
;
_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  0.0129
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.9837
_diffrn_reflns_Laue_measured_fraction_max 0.8112
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7689
_diffrn_reflns_point_group_measured_fraction_full 0.9837
_diffrn_reflns_point_group_measured_fraction_max 0.8112
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83320
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_description       block
_exptl_crystal_F_000             2016.894
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.5230
_refine_diff_density_min         -0.5037
_refine_diff_density_rms         0.0795
_refine_ls_d_res_high            0.7451
_refine_ls_d_res_low             10.8912
_refine_ls_goodness_of_fit_ref   1.0446
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0446
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0169
_refine_ls_shift/su_max          0.0022
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+3.6211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0418
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3444
_reflns_number_total             3623
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00203f3.cif
_cod_data_source_block           231130_nnno3_incl_autored
_cod_depositor_comments
'Adding full bibliography for 7250320--7250324.cif.'
_cod_database_code               7250320
_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:
 O2(H2b,H2c)
2.b Rotating group:
 O1(H1b,H1c)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C6(H6), C9(H9), C7(H7), C2(H2a), C11(H11), C3(H3), C10(H10),
 C5(H5), C1(H1a), C12(H12)
;
_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
;