From molecular architecture to environmental action: a new palladium-based perovskite catalyst as a cathodic modifier for electro-Fenton degradation
Khlifi, Houyem; Guesmi, Ahlem; Rabaaoui, Nejmeddine; Cherif, Mourad; Mhadhbi, Noureddine; El-Fattah, Wesam Abd; Ben Hamadi, Naoufel; Naïli, Houcine; RSC Advances 15 (2025) 30326–30338; doi:10.1039/D5RA03275J

data_7250815
_publ_section_title
;
 From molecular architecture to environmental action: a new
 palladium-based perovskite catalyst as a cathodic modifier for
 electro-Fenton degradation
;
_journal_issue                   37
_journal_name_full               'RSC Advances'
_journal_page_first              30326
_journal_page_last               30338
_journal_paper_doi               10.1039/D5RA03275J
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'Cl3 H2 O Pd, C9 H8 N'
_chemical_formula_sum            'C9 H10 Cl3 N O Pd'
_chemical_formula_weight         360.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-12
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2025-04-15 deposited with the CCDC.	2025-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3380(2)
_cell_length_b                   7.47850(10)
_cell_length_c                   20.6528(4)
_cell_measurement_reflns_used    27301
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      30.0790
_cell_measurement_theta_min      2.5650
_cell_volume                     2340.37(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (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-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.877
_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     -7.00  39.00   0.50    1.99    --    8.76  57.00-180.00   92
  2  \w     -7.00  39.00   0.50    1.99    --    8.76  57.00-150.00   92
  3  \w     -7.00  25.00   0.50    1.99    --    8.76  57.00-120.00   64
  4  \w     -7.00  39.00   0.50    1.99    --    8.76  57.00 -30.00   92
  5  \w     -7.00  39.00   0.50    1.99    --    8.76  57.00  60.00   92
  6  \w    -61.00 -35.00   0.50    1.99    --   -7.66 126.00 -11.25   52
  7  \w    -58.00 -31.00   0.50    1.99    --   -7.66 121.00  26.79   54
  8  \w    -39.00 -11.00   0.50    1.99    --   -7.66  90.00 171.45   56
  9  \w    -89.00 -40.00   0.50    1.99    --   -7.66 -19.00 -60.00   98
 10  \w    -89.00 -40.00   0.50    1.99    --   -7.66 -19.00-150.00   98
 11  \w    -72.00 -40.00   0.50    1.99    --    8.76 -19.00-120.00   64
 12  \w    -72.00 -40.00   0.50    1.99    --    8.76 -19.00-150.00   64
 13  \w    -72.00 -40.00   0.50    1.99    --    8.76 -19.00 -90.00   64
 14  \w    -72.00 -40.00   0.50    1.99    --    8.76 -19.00 -60.00   64
 15  \w    -26.00  29.00   0.50    1.99    --    8.76 -72.00 -29.00  110
 16  \w    -72.00 -40.00   0.50    1.99    --    8.76 -19.00  30.00   64
 17  \w    -72.00 -40.00   0.50    1.99    --    8.76 -19.00 120.00   64
 18  \w     -4.00  46.00   0.50    1.99    --    8.76 -99.00 120.00  100
 19  \w     14.00  62.00   0.50    1.99    --    8.76-126.00  -4.75   96
 20  \w     14.00  64.00   0.50    1.99    --   10.00-127.00-119.96  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0072465000
_diffrn_orient_matrix_UB_12      0.0616210000
_diffrn_orient_matrix_UB_13      0.0247178000
_diffrn_orient_matrix_UB_21      -0.0324233000
_diffrn_orient_matrix_UB_22      0.0441447000
_diffrn_orient_matrix_UB_23      -0.0226530000
_diffrn_orient_matrix_UB_31      -0.0330481000
_diffrn_orient_matrix_UB_32      -0.0568754000
_diffrn_orient_matrix_UB_33      0.0091581000
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            52278
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.532
_diffrn_reflns_theta_min         2.574
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.241
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6286
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+4.2855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5273
_reflns_number_total             6286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03275j2.cif
_cod_data_source_block           qpdcl_needle_autored
_cod_original_cell_volume        2340.36(6)
_cod_database_code               7250815
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H19 Cl2 N2 Pd2'
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.558
_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
 Pd1-H1B \\sim Pd1-H1C
 with sigma of 0.02
3.a Free rotating group:
 O1(H1B,H1C)
3.b Rotating group:
 O2(H2B,H2C)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), N2(H2A),
 C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17)
;
_shelx_res_checksum              43852
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id QPdCl
_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 1.480
_oxdiff_exptl_absorpt_empirical_full_min 0.610