Fifth-order nonlinear optical properties of through space charge transfer pyridinium salt
Bundulis, Arturs; Leduskrasts, Kaspars; Sapne, Anete; RSC Advances 15 (2025) 48109–48115; doi:10.1039/D5RA07294H

data_7251409
_publ_section_title
;
 Fifth-order nonlinear optical properties of through space charge transfer
 pyridinium salt
;
_journal_issue                   56
_journal_name_full               'RSC Advances'
_journal_page_first              48109
_journal_page_last               48115
_journal_paper_doi               10.1039/D5RA07294H
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C22 H18 N, Cl O4'
_chemical_formula_sum            'C22 H18 Cl N O4'
_chemical_formula_weight         395.84
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2025-11-13
_audit_creation_method
;
Olex2 1.2-ac4
(compiled 2018.05.17 svn.r3504 for Rigaku Oxford Diffraction, GUI svn.r5492)
;
_audit_update_record
;
2025-11-19 deposited with the CCDC.	2025-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7311(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.08322(13)
_cell_length_b                   8.31078(6)
_cell_length_c                   25.0348(2)
_cell_measurement_reflns_used    13278
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      80.1210
_cell_measurement_theta_min      3.6250
_cell_volume                     3669.87(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR97 (Burla et al.,  2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9883
_diffrn_measured_fraction_theta_max 0.9883
_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 -73.00   0.50    1.00    --  -49.98 145.00  57.00   54
  2  \w    -84.00 -42.00   0.50    1.00    --  -49.98 126.00-110.00   84
  3  \w   -111.00 -86.00   0.50    1.00    --  -49.98-145.00   4.00   50
  4  \w   -117.00 -74.00   0.50    1.00    --  -49.98-126.00 172.00   86
  5  \w     46.00  73.00   0.50    1.00    --   49.98-145.00   4.00   54
  6  \w     35.00  63.00   0.50    1.00    --   49.98-126.00 172.00   56
  7  \w    -86.00 -61.00   0.50    4.00    --  -90.00 145.00  57.00   50
  8  \w   -131.00-106.00   0.50    4.00    --  -90.00-145.00   4.00   50
  9  \w    -78.00 -53.00   0.50    4.00    --  -90.00 126.00-110.00   50
 10  \w    101.00 126.00   0.50    4.00    --  111.50 145.00  57.00   50
 11  \w    110.00 135.00   0.50    4.00    --  111.50 126.00-110.00   50
 12  \w     67.00 107.00   0.50    4.00    --  111.50-145.00   4.00   80
 13  \w     73.00  98.00   0.50    4.00    --  111.50-126.00 172.00   50
 14  \w   -116.00 -85.00   0.50    1.00    --  -49.98-125.00-150.00   62
 15  \w   -118.00 -80.00   0.50    1.00    --  -49.98-125.00  30.00   76
 16  \w   -118.00 -87.00   0.50    1.00    --  -49.98-125.00 -30.00   62
 17  \w    -34.00  18.00   0.50    1.00    --  -49.98  19.00  90.00  104
 18  \w   -121.00 -96.00   0.50    1.00    --  -49.98 -77.00 -90.00   50
 19  \w    -44.00 -19.00   0.50    4.00    --  -90.00  30.00  90.00   50
 20  \w     41.00  67.00   0.50    4.00    --  111.50 -61.00 -30.00   52
 21  \w     42.00  67.00   0.50    4.00    --  111.50 -61.00 120.00   50
 22  \w     43.00  68.00   0.50    4.00    --  111.50 -61.00  60.00   50
 23  \w    104.00 177.00   0.50    4.00    --  111.50  15.00 120.00  146
 24  \w    115.00 170.00   0.50    4.00    --  111.50  61.00-180.00  110
 25  \w     46.00  80.00   0.50    4.00    --  111.50 -77.00  90.00   68
 26  \w     95.00 173.00   0.50    4.00    --  111.50 125.00  90.00  156
 27  \w    138.00 164.00   0.50    4.00    --  111.50 125.00-180.00   52
 28  \w    139.00 176.00   0.50    4.00    --  111.50  15.00  90.00   74
 29  \w     41.00  66.00   0.50    4.00    --  111.50 -61.00  30.00   50
 30  \w     42.00  68.00   0.50    4.00    --  111.50 -61.00 150.00   52
 31  \w    104.00 135.00   0.50    4.00    --  111.50  15.00  90.00   62
 32  \w     96.00 161.00   0.50    4.00    --  111.50 125.00 -60.00  130
 33  \w     54.00  94.00   0.50    4.00    --  111.50-125.00 150.00   80
 34  \w     43.00  89.00   0.50    4.00    --  111.50 -77.00   0.00   92
 35  \w     53.00  78.00   0.50    4.00    --  111.50 -77.00  60.00   50
 36  \w     42.00  91.00   0.50    4.00    --  111.50 -77.00 120.00   98
 37  \w    121.00 146.00   0.50    4.00    --  111.50  15.00   0.00   50
 38  \w     52.00  77.00   0.50    4.00    --  111.50 -77.00 -30.00   50
 39  \w    100.00 127.00   0.50    4.00    --  111.50  61.00 120.00   54
 40  \w    134.00 178.00   0.50    4.00    --  111.50  61.00 120.00   88
 41  \w     96.00 123.00   0.50    4.00    --  111.50 125.00-180.00   54
 42  \w     41.00  66.00   0.50    4.00    --  111.50 -61.00 -60.00   50
 43  \w    136.00 161.00   0.50    4.00    --  111.50  77.00 150.00   50
 44  \w    117.00 154.00   0.50    4.00    --  111.50  30.00-180.00   74
 45  \w     94.00 124.00   0.50    4.00    --  111.50  77.00 150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku, XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0121347000
_diffrn_orient_matrix_UB_12      0.0721529000
_diffrn_orient_matrix_UB_13      0.0541006000
_diffrn_orient_matrix_UB_21      0.0496630000
_diffrn_orient_matrix_UB_22      -0.1337550000
_diffrn_orient_matrix_UB_23      0.0322287000
_diffrn_orient_matrix_UB_31      0.0708136000
_diffrn_orient_matrix_UB_32      0.1061376000
_diffrn_orient_matrix_UB_33      0.0038166000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19552
_diffrn_reflns_theta_full        80.3995
_diffrn_reflns_theta_max         80.40
_diffrn_reflns_theta_min         3.62
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.097
_exptl_absorpt_correction_T_max  0.92086
_exptl_absorpt_correction_T_min  0.73349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.4328
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.5121
_refine_diff_density_min         -1.9378
_refine_diff_density_rms         0.0993
_refine_ls_d_res_high            0.7819
_refine_ls_d_res_low             12.2097
_refine_ls_goodness_of_fit_ref   1.2895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.2895
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.0052
_refine_ls_shift/su_mean         0.0016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+11.8236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2319
_refine_ls_wR_factor_ref         0.2346
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                3756
_reflns_number_total             3978
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ra07294h2.cif
_cod_data_source_block           LSK74
_cod_original_cell_volume        3669.88(5)
_cod_database_code               7251409
_chemical_oxdiff_formula         'C176 H144 Cl8 N8 O16'
_chemical_oxdiff_usercomment     'from Kaspars'
_diffrn_oxdiff_digest_frames
;
017458962f0ee61187488269c64f4ad12f000295197
;
_diffrn_oxdiff_digest_hkl
;
01503a2d23d9f905d3a9d337b7e6b6c5a6d8f0
;
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O4(0.75) O3(0.75) O2(0.75) O5(0.75)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
3.b Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.746