Mono- and Bimetallic Homo- and Heterodinuclear Pd and Pt Complexes Bridged by Diphosphines: Synthesis, Characterisation and Cytotoxicity
Blom, Burgert; Prince, Sharon; Roufosse, Basile; Brice, Thomas; Papaldo, Marco; Macharia, Lucy; Serala, Karabo; Mlaza, Vuyo; Medupe, Thato; Marschner, Christoph; Cleij, Thomas; Dalton Transactions  (2026) –; doi:10.1039/D5DT02044A

data_7720007
_publ_section_title
;
 Mono- and Bimetallic Homo- and Heterodinuclear Pd and Pt Complexes
 Bridged by Diphosphines: Synthesis, Characterisation and Cytotoxicity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02044A
_journal_year                    2026
_chemical_formula_moiety         'C64 H66 Cl3 P4 Pd Ru, C F3 O3 S'
_chemical_formula_sum            'C65 H66 Cl3 F3 O3 P4 Pd Ru S'
_chemical_formula_weight         1421.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-07
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.29070(10)
_cell_length_b                   17.9374(2)
_cell_length_c                   34.5299(5)
_cell_measurement_reflns_used    32347
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      78.2750
_cell_measurement_theta_min      4.5880
_cell_volume                     6311.98(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.129a 64-bit (release 29-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.954
_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      6.00  32.00   0.50    4.00    --   24.00  71.00  25.69   52
  2  \w     12.00  39.00   0.50    4.00    --   28.00  66.00 131.16   54
  3  \w    -26.00  20.00   0.50    4.00    --  -54.67  19.00  60.00   92
  4  \w   -123.00 -87.00   0.50    4.00    --  -54.67-125.00   0.00   72
  5  \w    -66.00  -4.00   0.50    4.00    --  -76.64  57.00   0.00  124
  6  \w   -154.00 -66.00   0.50    4.00    --  -80.00 -51.00 -68.01  176
  7  \w     35.00 105.00   0.50   16.00    --  101.05 -77.00-180.00  140
  8  \w     28.00  66.00   0.50   16.00    --  101.05 -57.00-180.00   76
  9  \w     40.00 131.00   0.50   16.00    --  105.75 -82.00 178.55  182
 10  \w     41.00 129.00   0.50   16.00    --  105.75 -79.00 -64.53  176
 11  \w     55.00 178.00   0.50   16.00    --  105.75  13.00 162.35  246
 12  \w     55.00 178.00   0.50   16.00    --  105.75  13.00 162.35  246
 13  \w     40.00 110.00   0.50   16.00    --  105.75 -84.00   8.90  140
 14  \w     42.00  97.00   0.50   16.00    --  105.75 -85.00 -47.31  110
 15  \w     61.00 102.00   0.50   16.00    --  105.75  14.00  48.05   82
 16  \w    120.00 177.00   0.50   16.00    --  105.75  16.00 -45.22  114
 17  \w     41.00  77.00   0.50   16.00    --  105.75 -85.00  40.99   72
 18  \w    145.00 178.00   0.50   16.00    --  105.75  14.00  48.05   66
 19  \w     96.00 122.00   0.50   16.00    --  105.75 -80.00-121.35   52
 20  \w     40.00  66.00   0.50   16.00    --  105.75 -77.00  -3.22   52
 21  \w     64.00 102.00   0.50   16.00    --  105.75  15.00 -62.65   76
 22  \w    117.00 143.00   0.50   16.00    --  105.75  15.00 -62.65   52
 23  \w     71.00  99.00   0.50   16.00    --  105.75 -87.00  71.98   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1278212000
_diffrn_orient_matrix_UB_12      -0.0390138000
_diffrn_orient_matrix_UB_13      -0.0071956000
_diffrn_orient_matrix_UB_21      0.0566460000
_diffrn_orient_matrix_UB_22      0.0112225000
_diffrn_orient_matrix_UB_23      0.0433158000
_diffrn_orient_matrix_UB_31      -0.0575105000
_diffrn_orient_matrix_UB_32      -0.0756617000
_diffrn_orient_matrix_UB_33      0.0101390000
_diffrn_radiation_collimation    0.3
_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  0.0765
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            61163
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.942
_diffrn_reflns_theta_min         2.782
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.110
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.053
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       plate
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.515
_refine_diff_density_min         -1.864
_refine_diff_density_rms         0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         13330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0881
_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^)+(0.0921P)^2^+78.1781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12282
_reflns_number_total             13330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02044a2.cif
_cod_data_source_block           chm_15_cu_2_chmfinabs
_cod_original_cell_volume        6311.97(13)
_cod_database_code               7720007
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         P3PdRuClC20H40SF3O3
_chemical_oxdiff_usercomment     overnight
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.102
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9894(4)
 0.0106(4)
2. 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
3.a Ternary CH refined with riding coordinates:
 C62(H62)
3.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C42(H42A,H42B), C14(H14A,H14B), C41(H41A,H41B), C13(H13A,
 H13B), C39(H39A,H39B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C38(H38), C2(H2), C50(H50), C32(H32), C44(H44), C5(H5), C26(H26),
 C35(H35), C53(H53), C3(H3), C45(H45), C52(H52), C22(H22), C9(H9), C56(H56),
 C46(H46), C54(H54), C36(H36), C28(H28), C25(H25), C29(H29), C59(H59), C37(H37),
  C48(H48), C10(H10), C31(H31), C20(H20), C30(H30), C23(H23), C47(H47),
 C60(H60), C24(H24), C51(H51), C4(H4), C8(H8), C57(H57), C12(H12), C34(H34),
 C11(H11), C16(H16), C19(H19), C18(H18), C17(H17)
3.d Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C61(H61A,H61B,H61C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              25465
_olex2_date_sample_data_collection 2024-07-15
_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 1.850
_oxdiff_exptl_absorpt_empirical_full_min 0.559