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_7720006
_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
'C40 H38 Cl P3 Pd, C0.5 H1.989 Cl1.52, C0.783 F2.356 O2.387 S0.781, C0.187 F0.549 O0.663 S0.193'
_chemical_formula_sum            'C41.8 H39.6 Cl2.53 F3.06 O2.86 P3 Pd S0.95'
_chemical_formula_weight         965.20
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-24
_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                 105.1110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.08760(10)
_cell_length_b                   15.34030(10)
_cell_length_c                   19.8791(2)
_cell_measurement_reflns_used    40316
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3100
_cell_measurement_theta_min      3.6760
_cell_volume                     4147.49(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.106a 64-bit (release 01-02-2024))'
_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  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(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 0.999
_diffrn_measured_fraction_theta_max 0.992
_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     95.00 170.00   0.50    1.00    --  101.05 125.00-180.00  150
  2  \w     95.00 170.00   0.50    1.00    --  101.05 125.00  30.00  150
  3  \w     35.00 105.00   0.50    1.00    --  101.05 -77.00 150.00  140
  4  \w     35.00 105.00   0.50    1.00    --  101.05 -77.00 120.00  140
  5  \w     28.00  66.00   0.50    1.00    --  101.05 -57.00 150.00   76
  6  \w     28.00  66.00   0.50    1.00    --  101.05 -57.00  60.00   76
  7  \w     28.00  66.00   0.50    1.00    --  101.05 -57.00   0.00   76
  8  \w     28.00  66.00   0.50    1.00    --  101.05 -57.00 -30.00   76
  9  \w    -21.00  26.00   0.50    0.20    --   53.17 -19.00 -90.00   94
 10  \w     28.00  66.00   0.50    1.00    --  101.05 -57.00-150.00   76
 11  \w     35.00 105.00   0.50    1.00    --  101.05 -77.00-150.00  140
 12  \w     28.00  66.00   0.50    1.00    --  101.05 -57.00 -90.00   76
 13  \w     89.00 177.00   0.50    1.00    --  101.05  38.00  60.00  176
 14  \w    100.00 167.00   0.50    1.00    --  101.05  77.00  90.00  134
 15  \w    100.00 167.00   0.50    1.00    --  101.05  77.00  90.00  134
 16  \w    100.00 167.00   0.50    1.00    --  101.05  77.00  60.00  134
 17  \w     87.00 174.00   0.50    1.00    --  101.05  57.00   0.00  174
 18  \w    100.00 167.00   0.50    1.00    --  101.05  77.00 -60.00  134
 19  \w    100.00 167.00   0.50    1.00    --  101.05  77.00 -90.00  134
 20  \w    100.00 167.00   0.50    1.00    --  101.05  77.00-120.00  134
 21  \w     89.00 177.00   0.50    1.00    --  101.05  38.00-180.00  176
 22  \w     42.00 129.00   0.50    0.20    --   53.17  38.00-150.00  174
 23  \w     42.00 129.00   0.50    0.20    --   53.17  38.00 -60.00  174
 24  \w    -26.00  20.00   0.50    0.20    --  -54.67  19.00-180.00   92
 25  \w    -43.00  -1.00   0.50    0.20    --  -76.64  38.00-180.00   84
 26  \w    -43.00  -1.00   0.50    0.20    --  -76.64  38.00 -60.00   84
 27  \w    -86.00 -13.00   0.50    0.20    --  -54.67 125.00  30.00  146
 28  \w     36.00 101.00   0.50    1.00    --  101.05 -99.00 -30.00  130
 29  \w   -126.00 -39.00   0.50    0.20    --  -54.67 -63.00 175.00  174
 30  \w   -130.00 -43.00   0.50    0.20    --  -54.67 -38.00  60.00  174
 31  \w   -127.00 -82.00   0.50    0.20    --  -54.67 -57.00  30.00   90
 32  \w   -126.00 -40.00   0.50    0.20    --  -54.67 -60.00 -26.00  172
 33  \w   -145.00 -87.00   0.50    0.20    --  -76.64-125.00  90.00  116
 34  \w   -123.00 -87.00   0.50    0.20    --  -54.67-125.00 120.00   72
 35  \w   -123.00 -87.00   0.50    0.20    --  -54.67-125.00 -30.00   72
;
_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      -0.1017818000
_diffrn_orient_matrix_UB_12      -0.0327295000
_diffrn_orient_matrix_UB_13      -0.0415741000
_diffrn_orient_matrix_UB_21      0.0497220000
_diffrn_orient_matrix_UB_22      -0.0660131000
_diffrn_orient_matrix_UB_23      -0.0383125000
_diffrn_orient_matrix_UB_31      0.0007434000
_diffrn_orient_matrix_UB_32      -0.0682121000
_diffrn_orient_matrix_UB_33      0.0569918000
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            69734
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.565
_diffrn_reflns_theta_min         4.344
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.090
_exptl_absorpt_correction_T_max  0.39935
_exptl_absorpt_correction_T_min  0.32831
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.546
_exptl_crystal_description       plate
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         8768
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0384P)^2^+5.2012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8305
_reflns_number_total             8768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02044a2.cif
_cod_data_source_block           chm_10_cu_chmfin
_cod_original_formula_sum        'C41.80 H39.60 Cl2.53 F3.06 O2.86 P3 Pd S0.95'
_cod_database_code               7720006
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C20H40PtP4
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.509
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C41-Cl2B \\sim C41-Cl3B \\sim C41-Cl2A \\sim C41-Cl3A
 with sigma of 0.02
 F2-F3A \\sim F2-O2A \\sim F2-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S1A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 F2A, S1A, F1A, O3A, F2, F3A, O1A, O2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3, S1, O1, O2, O3, C31, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2A, C41, Cl2B, Cl3A, Cl3B, H41C, H41D, H41A, H41B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C41(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C41(H41C,
 H41D), C41(H41A,H41B)
6.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00J(H00J), C00N(H00N), C00S(H00S), C00W(H00W), C00X(H00X),
 C01C(H01C), C01G(H01G), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9),
  C010(H010), C10(H10), C11(H11), C12(H12), C015(H015), C17(H17), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C32(H32)
;
_shelx_res_checksum              86045
_olex2_submission_original_sample_id chm_10_Cu
_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 1.848
_oxdiff_exptl_absorpt_empirical_full_min 0.593