Photosalient effect and photodimerization of mono- and dicationic organic salts incorporated in 4-styrylpyridine
Kusumoto, Sotaro; Wakabayashi, Kaede; Rakumitsu, Kenta; Kim, Yang; Koide, Yoshihiro; CrystEngComm 26 (2024) 3791–3794; doi:10.1039/D4CE00538D

data_7248926
_publ_section_title
;
 Photosalient effect and photodimerization of mono- and dicationic organic
 salts incorporated in 4-styrylpyridine
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              3791
_journal_page_last               3794
_journal_paper_doi               10.1039/D4CE00538D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '2(Br), 1.5(H2 O), C38 H38 N2'
_chemical_formula_sum            'C38 H41 Br2 N2 O1.5'
_chemical_formula_weight         709.55
_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             2024-04-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-14 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                69.469(3)
_cell_angle_beta                 73.203(3)
_cell_angle_gamma                89.616(3)
_cell_formula_units_Z            4
_cell_length_a                   12.1902(4)
_cell_length_b                   15.9154(5)
_cell_length_c                   18.7119(7)
_cell_measurement_reflns_used    10401
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.1370
_cell_measurement_theta_min      1.7620
_cell_volume                     3236.5(2)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.780
_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
  2  \w   -100.00 -10.00   0.50    5.00    --  -10.00  45.00  90.00  180
;
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.780
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23882
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.780
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.683
_diffrn_reflns_theta_min         1.755
_exptl_absorpt_coefficient_mu    2.540
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81172
_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    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.693
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         13043
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0633P)^2^+6.7739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9198
_reflns_number_total             13043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00538d4.cif
_cod_data_source_block           2300509_1256br_nore_no_sun_autored
_cod_depositor_comments
'Adding full bibliography for 7248924--7248927.cif.'
_cod_original_formula_sum        'C38 H41 Br2 N2 O1.50'
_cod_database_code               7248926
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.785
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C40)
3.a Free rotating group:
 O3(H3A,H3B), O1(H1A,H1B), O2(H2A,H2B)
3.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C15(H15A,H15B), C01F(H01A,H01B), C47(H47A,H47B)
3.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C63(H63), C33(H33), C31(H31), C67(H67), C55(H55), C13(H13),
 C58(H58), C12(H12), C28(H28), C56(H56), C64(H64), C54(H54), C30(H30), C8(H8),
 C61(H61), C11(H11), C50(H50), C59(H59), C27(H27), C9(H9), C32(H32), C62(H62),
 C14(H14), C60(H60), C39(H39), C35(H35), C66(H66), C38(H38), C51(H51), C37(H37),
  C36(H36), C68(H68), C6(H6), C69(H69), C7(H7), C71(H71), C4(H4), C73(H73),
 C2(H2), C72(H72), C3(H3), C75(H75), C74(H74)
3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C49(H49A,H49B,H49C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C76(H76A,
 H76B,H76C)
;
_shelx_res_checksum              94069
_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
;