A nanoscale chemical oscillator: reversible formation of palladium nanoparticles in ionic liquid.
Lodge, Rhys W.; Cull, William J.; Weilhard, Andreas; Argent, Stephen P.; Alves Fernandes, Jesum; Khlobystov, Andrei N.; Nanoscale 17 (2025) 10105–10116; doi:10.1039/d4nr04150j

data_1574242
_publ_section_title
;
 A nanoscale chemical oscillator: reversible formation of palladium
 nanoparticles in ionic liquid.
;
_journal_issue                   16
_journal_name_full               Nanoscale
_journal_page_first              10105
_journal_page_last               10116
_journal_paper_doi               10.1039/d4nr04150j
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C22 H24 Br2 N4 Pd, C H2 Cl2'
_chemical_formula_sum            'C23 H26 Br2 Cl2 N4 Pd'
_chemical_formula_weight         695.60
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-24 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.968(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4693(4)
_cell_length_b                   9.1908(3)
_cell_length_c                   19.4408(6)
_cell_measurement_reflns_used    17274
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.6490
_cell_measurement_theta_min      4.2430
_cell_volume                     2546.30(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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    -44.00  49.00   1.00   30.00    --  -23.76  40.00 127.00   93
  2  \w    -58.00 -31.00   1.00   30.00    --  -23.76 -40.00 -25.00   27
  3  \w    -49.00  49.00   1.00   30.00    --   24.70 -40.00 -25.00   98
  4  \w     14.00  97.00   1.00   30.00    --   24.70  40.00 127.00   83
  5  \w    -41.00   9.00   1.00   30.00    --  -23.76 -77.00 -60.00   50
  6  \w    -39.00   9.00   1.00   30.00    --  -23.76 -77.00  90.00   48
  7  \w    -42.00   9.00   1.00   30.00    --  -23.76 -77.00 150.00   51
  8  \w   -100.00 -67.00   1.00   30.00    --  -23.76 155.00 -27.04   33
  9  \w    -65.00 -15.00   1.00   30.00    --  -23.76  19.00 -30.00   50
 10  \w     12.00  48.00   1.00   30.00    --  -23.76  19.00 -30.00   36
 11  \w     38.00 112.00   1.00   30.00    --   24.70-178.00 -90.00   74
 12  \w      0.00  94.00   1.00   30.00    --   24.70  38.00 -60.00   94
 13  \w      2.00  99.00   1.00   30.00    --   24.70  38.00  30.00   97
 14  \w      9.00  79.00   1.00   30.00    --   24.70-123.00 -47.36   70
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0255839000
_diffrn_orient_matrix_UB_12      0.0637277000
_diffrn_orient_matrix_UB_13      0.0118640000
_diffrn_orient_matrix_UB_21      0.0390088000
_diffrn_orient_matrix_UB_22      -0.0434346000
_diffrn_orient_matrix_UB_23      0.0145841000
_diffrn_orient_matrix_UB_31      0.0173246000
_diffrn_orient_matrix_UB_32      0.0037825000
_diffrn_orient_matrix_UB_33      -0.0319073000
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38462
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.096
_diffrn_reflns_theta_min         3.541
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    4.096
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.815
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         5432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0216P)^2^+9.3601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4544
_reflns_number_total             5432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr04150j10.cif
_cod_data_source_block           pdrlla
_cod_depositor_comments          'Adding full bibliography for 1574242.cif.'
_cod_database_code               1574242
_nottingham_internal_coll_name   PDRLLA
_nottingham_internal_coll_number 19091
_nottingham_internal_coll_client RL/ANK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time 30.00
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   01/11/2021
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017-09'
_nottingham_internal_process_date 02/11/2021
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 02/11/2021
_nottingham_internal_solution_user pczspa
_nottingham_internal_refinement_date 02/11/2021
_nottingham_internal_refinement_user pczspa
_nottingham_internal_validation_date 02/11/2021
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 02/11/2021
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C23H26Br2Cl2N4Pd
_chemical_oxdiff_usercomment
'PDRLLA #19091 SN-1644 for RL/ANK fomblin micromount'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_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
2. Others
 Fixed Sof: H1SA(0.5) H1SB(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C1S(H1SA,H1SB)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              64770
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_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 1.120
_oxdiff_exptl_absorpt_empirical_full_min 0.909