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_7251801
_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 F4 I2, C22 H18 N4 O4 Pd'
_chemical_formula_sum            'C28 H18 F4 I2 N4 O4 Pd'
_chemical_formula_weight         910.66
_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   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                80.628(4)
_cell_angle_beta                 88.278(3)
_cell_angle_gamma                76.719(4)
_cell_formula_units_Z            1
_cell_length_a                   6.0196(2)
_cell_length_b                   10.5726(5)
_cell_length_c                   11.3896(5)
_cell_measurement_reflns_used    6400
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2380
_cell_measurement_theta_min      3.5840
_cell_volume                     696.04(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -22.00  15.00   1.00   31.40    --  -16.78 -77.00-180.00   37
  2  \w   -103.00 -61.00   1.00   31.40    --  -16.78-178.00  60.00   42
  3  \w    -38.00  16.00   1.00   31.40    --  -16.78 -77.00  30.00   54
  4  \w     39.00  67.00   1.00   31.40    --   18.97 178.00 120.00   28
  5  \w     39.00  69.00   1.00   31.40    --   18.97 178.00-120.00   30
  6  \w     -6.00  92.00   1.00   31.40    --   18.97  38.00  30.00   98
  7  \w     -6.00  93.00   1.00   31.40    --   18.97  38.00 -60.00   99
  8  \w    -17.00  52.00   1.00   31.40    --   18.97 -77.00 -60.00   69
  9  \w    -43.00  28.00   1.00   31.40    --   18.97 -38.00-150.00   71
 10  \w      2.00  91.00   1.00   31.40    --   18.97  38.00-180.00   89
 11  \w     40.00  67.00   1.00   31.40    --   18.97-111.00-153.00   27
 12  \w      3.00  60.00   1.00   31.40    --   18.97 -99.00  90.00   57
 13  \w    -57.00 -13.00   1.00   31.40    --   18.97 -19.00   0.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0519917000
_diffrn_orient_matrix_UB_12      -0.0613166000
_diffrn_orient_matrix_UB_13      -0.0175070000
_diffrn_orient_matrix_UB_21      -0.0381513000
_diffrn_orient_matrix_UB_22      0.0253791000
_diffrn_orient_matrix_UB_23      -0.0593146000
_diffrn_orient_matrix_UB_31      0.1024695000
_diffrn_orient_matrix_UB_32      0.0217498000
_diffrn_orient_matrix_UB_33      -0.0126297000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13876
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         3.478
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.955
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021)
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    2.173
_exptl_crystal_description       prism
_exptl_crystal_F_000             434
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-dichloroethane'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.433
_refine_diff_density_min         -1.610
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3173
_reflns_number_total             3701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6ce00085a2.cif
_cod_data_source_block           ask-9
_cod_depositor_comments
'Adding full bibliography for 7251800--7251802.cif.'
_cod_database_code               7251801
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H18 F8 I4 N4 O4 Pd '
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.700
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C7(H7), C11(H11), C10(H10), C8(H8)
1.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              63065
_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 2.001
_oxdiff_exptl_absorpt_empirical_full_min 0.699