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_7250324
_publ_section_title
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 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_absolute_configuration unk
_chemical_formula_moiety         '8(Cl5 Sb), 8(C12 H12 N2), 2(H2 O0.5)'
_chemical_formula_sum            'C96 H100 Cl40 N16 O Sb8'
_chemical_formula_weight         3886.151
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_Int_Tables_number      20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2944(5)
_cell_length_b                   37.3407(14)
_cell_length_c                   15.8762(7)
_cell_measurement_reflns_used    11318
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.8010
_cell_measurement_theta_min      2.1760
_cell_volume                     6695.6(5)
_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 0.9991
_diffrn_measured_fraction_theta_max 0.8530
_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  90.00  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  0.0152
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.8530
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16041
_diffrn_reflns_point_group_measured_fraction_full 0.9540
_diffrn_reflns_point_group_measured_fraction_max 0.7767
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    2.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61181
_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    1.928
_exptl_crystal_description       block
_exptl_crystal_F_000             3771.171
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.4068
_refine_diff_density_min         -0.4084
_refine_diff_density_rms         0.0675
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.606(12)
_refine_ls_d_res_high            0.7406
_refine_ls_d_res_low             12.0947
_refine_ls_goodness_of_fit_ref   1.0347
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    63
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6716
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.0301
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.0039
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+14.7614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.684
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              45
_reflns_limit_k_min              -44
_reflns_limit_l_max              21
_reflns_limit_l_min              -20
_reflns_number_gt                6568
_reflns_number_total             6716
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00203f3.cif
_cod_data_source_block           231211_sb_nnore_autored
_cod_depositor_comments
'Adding full bibliography for 7250320--7250324.cif.'
_cod_original_sg_symbol_Hall     ' C 2c 2'
_cod_database_code               7250324
_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. Restrained distances
 C10-C9 \\sim C10-C8
 with sigma of 0.02
 C3-C7 \\sim C3-C6
 with sigma of 0.02
 C3-C9 \\sim C3-C8
 with sigma of 0.04
 C7-C9 \\sim C6-C8
 with sigma of 0.02
 C10-C7 \\sim C10-C6
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C3) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C22) \\sim Ueq, Uanis(C21a) \\sim Ueq, Uanis(C20a) \\sim Ueq, Uanis(C18)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C10) = Uanis(C8) = Uanis(C6) = Uanis(C3)
Uanis(C22) = Uanis(C21a) = Uanis(C20a) = Uanis(C18)
4. Others
 Sof(C8)=Sof(H8)=Sof(C6)=Sof(H6)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(C9)=Sof(H9)=FVAR(1)
 Sof(C21a)=Sof(C20a)=Sof(H21a)=Sof(H20a)=1-FVAR(2)
 Sof(C21)=Sof(C20)=Sof(H21)=Sof(H20)=FVAR(2)
 Fixed Sof: H1b(0.25) H1c(0.25) H1b(0.25) H1c(0.25) O1(0.25) H1b(0.5) H1c(0.5)
5.a Free rotating group:
 O1(H1b,H1c)
5.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N1(H1a), N3(H3), C23(H23), C4(H4a), N2(H2a), C13(H13), C24(H24),
 C25(H25), C12(H12), C26(H26), C17(H17), C11(H11), C14(H14), C2(H2), C1(H1),
 C5(H5), C7(H7), C9(H9), C16(H16), C19(H19), C15(H15), C8(H8), C6(H6), C21(H21),
  C20(H20), C21a(H21a), C20a(H20a)
;
_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
;