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_7250323
_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 Sn, 2(C6 H6 N)'
_chemical_formula_sum            'C12 H12 Cl6 N2 Sn'
_chemical_formula_weight         515.668
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_Int_Tables_number      15
_audit_creation_date             2025-01-29
_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                 91.529(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.1093(3)
_cell_length_b                   14.9953(5)
_cell_length_c                   32.2219(13)
_cell_measurement_reflns_used    5452
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.7020
_cell_measurement_theta_min      2.2770
_cell_volume                     3433.8(2)
_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 0.9891
_diffrn_measured_fraction_theta_max 0.8377
_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  80.00   0.50    5.00    --  -10.00  45.00   0.00  360
;
_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  0.0188
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.9891
_diffrn_reflns_Laue_measured_fraction_max 0.8377
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            8098
_diffrn_reflns_point_group_measured_fraction_full 0.9891
_diffrn_reflns_point_group_measured_fraction_max 0.8377
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    2.415
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86009
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_description       block
_exptl_crystal_F_000             2002.632
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.1131
_refine_diff_density_min         -1.1052
_refine_diff_density_rms         0.2257
_refine_ls_d_res_high            0.7391
_refine_ls_d_res_low             8.7298
_refine_ls_goodness_of_fit_ref   1.0602
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    22
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0602
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0005P)^2^+40.1562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              0
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              40
_reflns_limit_l_min              -40
_reflns_number_gt                3286
_reflns_number_total             3747
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00203f3.cif
_cod_data_source_block           240527_nnsn_cl_autored
_cod_depositor_comments
'Adding full bibliography for 7250320--7250324.cif.'
_cod_original_sg_symbol_Hall     '-C 2yc (x+z,y,-x)'
_cod_database_code               7250323
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Others
 Fixed Sof: C5(0.5) C4(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N2(H2), C15(H15), C19(H19), C17(H17), C18(H18), C20(H20), C8(H8),
 C2(H2a), C7(H7), C1(H1a)
;
_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
;