Palladium(II) complexes of 5-acetylmethyl-1,2,4-oxadiazole: versatile ditopic acceptors for halogen bonding
Abulkhaev, Jacob U.; Semenov, Artem V.; Ivanov, Daniil; Ignatov, Eugene V.; Baykov, Sergey; Bokach, Nadezhda A.; CrystEngComm  (2026) –; doi:10.1039/D6CE00085A

data_7251800
_publ_section_title
;
 Palladium(ii) complexes of 5-acetylmethyl-1,2,4-oxadiazole: versatile
 ditopic acceptors for halogen bonding
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2443
_journal_page_last               2454
_journal_paper_doi               10.1039/D6CE00085A
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C6 F3 I3, C12 H14 N4 O4 Pd'
_chemical_formula_sum            'C18 H14 F3 I3 N4 O4 Pd'
_chemical_formula_weight         894.43
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-12-17
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-01-16 deposited with the CCDC.	2026-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.086(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.27490(10)
_cell_length_b                   17.9506(4)
_cell_length_c                   30.5282(8)
_cell_measurement_reflns_used    5741
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      79.4130
_cell_measurement_theta_min      2.8990
_cell_volume                     2342.64(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.136a 64-bit (release 23-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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     42.00  67.00   0.50    1.00    --  113.25 -61.00-180.00   50
  2  \w     43.00  70.00   0.50    1.00    --  113.25 -61.00 -90.00   54
  3  \w     45.00  70.00   0.50    1.00    --  113.25 -61.00  90.00   50
  4  \w     13.00  93.00   0.50    0.25    --   47.39-125.00 120.00  160
  5  \w    -27.00  26.00   0.50    0.25    --   47.39 -19.00   0.00  106
  6  \w    -64.00  25.00   0.50    0.25    --  -47.39  62.00 117.00  178
  7  \w    -64.00  25.00   0.50    0.25    --  -47.39  62.00 117.00  178
  8  \w   -100.00 -39.00   0.50    1.00    -- -106.00  77.00   0.00  122
  9  \w    -73.00 -33.00   0.50    1.00    -- -106.00  62.00 117.00   80
 10  \w   -106.00 -70.00   0.50    1.00    -- -106.00  77.00   0.00   72
 11  \w    -67.00 -37.00   0.50    1.00    -- -106.00  61.00  90.00   60
 12  \w   -103.00 -76.00   0.50    1.00    -- -106.00  77.00 -60.00   54
 13  \w    -71.00 -33.00   0.50    1.00    -- -106.00  77.00 -60.00   76
 14  \w    -26.00  28.00   0.50    0.25    --  -47.39  19.00-150.00  108
 15  \w   -177.00 -85.00   0.50    1.00    -- -106.00-102.00-109.00  184
 16  \w   -177.00 -88.00   0.50    1.00    -- -106.00 -64.00 128.00  178
 17  \w   -177.00 -88.00   0.50    1.00    -- -106.00 -64.00 128.00  178
 18  \w     81.00 107.00   0.50    0.25    --   47.39  19.00 -90.00   52
 19  \w    -19.00   7.00   0.50    0.25    --   47.39 -19.00 -30.00   52
 20  \w    -76.00 -39.00   0.50    1.00    -- -106.00  77.00-150.00   74
 21  \w   -124.00 -94.00   0.50    1.00    -- -106.00 -45.00  90.00   60
 22  \w    -71.00 -46.00   0.50    1.00    -- -106.00  61.00  30.00   50
 23  \w   -106.00 -80.00   0.50    1.00    -- -106.00  77.00-150.00   52
 24  \w   -171.00-146.00   0.50    1.00    -- -106.00 -45.00  90.00   50
 25  \w     42.00  67.00   0.50    1.00    --  113.25 -61.00 120.00   50
 26  \w     85.00 134.00   0.50    1.00    --  113.25 102.00  -5.00   98
 27  \w     99.00 137.00   0.50    1.00    --  113.25  61.00-180.00   76
 28  \w    138.00 164.00   0.50    1.00    --  113.25 102.00  -5.00   52
 29  \w     42.00  67.00   0.50    1.00    --  113.25 -61.00-150.00   50
 30  \w    110.00 177.00   0.50    1.00    --  113.25  45.00 150.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1720574000
_diffrn_orient_matrix_UB_12      0.0441080000
_diffrn_orient_matrix_UB_13      0.0358919000
_diffrn_orient_matrix_UB_21      -0.1984840000
_diffrn_orient_matrix_UB_22      -0.0693346000
_diffrn_orient_matrix_UB_23      0.0107572000
_diffrn_orient_matrix_UB_31      0.2467391000
_diffrn_orient_matrix_UB_32      -0.0247943000
_diffrn_orient_matrix_UB_33      0.0337885000
_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  0.0841
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9146
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.467
_diffrn_reflns_theta_max         67.467
_diffrn_reflns_theta_min         2.895
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    37.962
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.536
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-dichloroethane'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0801P)^2^+9.7142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1799
_reflns_number_total             2057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6ce00085a2.cif
_cod_data_source_block           096-097_cpii
_cod_depositor_comments
'Adding full bibliography for 7251800--7251802.cif.'
_cod_database_code               7251800
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Pd '
_shelx_estimated_absorpt_t_max   0.209
_shelx_estimated_absorpt_t_min   0.083
_reflns_odcompleteness_completeness 97.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.93
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
1.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              23914
_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 2.635
_oxdiff_exptl_absorpt_empirical_full_min 0.436