Pd(μ-L)4Pt vs. Pd(μ-L)4RuCl2: chlorido ancillary ligands as defining factors in the host–guest interactions of M(μ-L)4M′ heterodimetallic supramolecular architectures
Gearing, Hayden B.; Cziferszky, Monika; Söhnel, Tilo; Wright, L. James; Crowley, James D.; Hartinger, Christian G.; Chemical Science 16 (2025) 7294–7301; doi:10.1039/D5SC00209E

data_1574217
_publ_section_title
;
 Pd(\m-L)4Pt vs. Pd(\m-L)4RuCl2: chlorido ancillary ligands as defining
 factors in the host--guest interactions of M(\m-L)4M&#x2032;
 heterodimetallic supramolecular architectures
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              7294
_journal_page_last               7301
_journal_paper_doi               10.1039/D5SC00209E
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C100 H80 N16 O4 Pd Pt, C10 H6 O6 S2, C3 H7 N O, 2(B F4), 5[C3H7NO]'
_chemical_formula_sum            'C128 H128 B2 F8 N22 O16 Pd Pt S2'
_chemical_formula_weight         2769.75
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2025-03-03
_audit_creation_method
;
Olex2 1.5
(compiled 2025.02.27 svn.r83f5de26 for OlexSys, GUI svn.r7172)
;
_audit_update_record
;
2025-03-08 deposited with the CCDC.	2025-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                79.4685(11)
_cell_angle_beta                 84.6071(10)
_cell_angle_gamma                73.5233(11)
_cell_formula_units_Z            2
_cell_length_a                   15.47952(19)
_cell_length_b                   19.9749(3)
_cell_length_c                   21.2142(3)
_cell_measurement_reflns_used    98249
_cell_measurement_temperature    119.99(13)
_cell_measurement_theta_max      72.1810
_cell_measurement_theta_min      2.9520
_cell_volume                     6177.96(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      119.99(13)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_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    -48.00  26.00   0.50    0.65    --  -46.98  46.00 -57.00  148
  2  \w    -39.00 -13.00   0.50    2.60    --  -90.25  46.00 -57.00   52
  3  \w    -68.00 -22.00   0.50    0.65    --  -46.98 -19.00-180.00   92
  4  \w    -72.00 -46.00   0.50    2.60    --  -74.00 -79.00 -77.14   52
  5  \w    -76.00 -50.00   0.50    2.60    --  -78.00 -78.00 -43.31   52
  6  \w    -72.00 -46.00   0.50    2.60    --  -74.00 -79.00  -7.90   52
  7  \w    -78.00 -50.00   0.50    2.60    --  -78.00 -78.00 -84.09   56
  8  \w    -76.00 -50.00   0.50    2.60    --  -78.00 -78.00-130.21   52
  9  \w    -77.00 -51.00   0.50    2.60    --  -78.00 -76.00-164.96   52
 10  \w    -90.00 -64.00   0.50    2.60    --  -90.25 -74.00 -57.38   52
 11  \w    -94.00 -63.00   0.50    2.60    --  -90.25 -78.00  -5.99   62
 12  \w    -88.00 -62.00   0.50    2.60    --  -90.00 -78.00  58.00   52
 13  \w    -81.00 -55.00   0.50    2.60    --  -82.00 -76.00  82.11   52
 14  \w    -76.00 -50.00   0.50    2.60    --  -78.00 -78.00 131.75   52
 15  \w    -81.00 -55.00   0.50    2.60    --  -82.00 -77.00 112.74   52
 16  \w    -99.00 -63.00   0.50    2.60    --  -90.25 -78.00 138.47   72
 17  \w    -93.00 -63.00   0.50    2.60    --  -90.25 -77.00 150.86   60
 18  \w    -88.00 -63.00   0.50    2.60    --  -90.25 -77.00 114.48   50
 19  \w    -89.00 -64.00   0.50    2.60    --  -90.25 -74.00  44.62   50
 20  \w    -93.00 -63.00   0.50    2.60    --  -90.25 -77.00 -30.00   60
 21  \w    -91.00 -62.00   0.50    2.60    --  -90.25 -80.00 -73.85   58
 22  \w   -104.00 -63.00   0.50    2.60    --  -90.25 -77.00-120.00   82
 23  \w   -111.00 -77.00   0.50    0.65    --  -46.98 -19.00-180.00   68
 24  \w   -124.00 -29.00   0.50    0.65    --  -46.98 -46.00 -44.70  190
 25  \w   -111.00 -24.00   0.50    0.65    --  -46.98 -19.00  30.00  174
 26  \w    -27.00  42.00   0.50    0.65    --   46.98 -46.00 153.00  138
 27  \w     20.00  52.00   0.50    2.60    --   97.33 -46.00 153.00   64
 28  \w     29.00  71.00   0.50    2.60    --   97.33 -61.00 150.00   84
 29  \w     20.00 101.00   0.50    2.60    --   97.33 -95.00 150.00  162
 30  \w     77.00 108.00   0.50    2.60    --   97.33-111.00  30.00   62
 31  \w     41.00  67.00   0.50    2.60    --   97.33-111.00  30.00   52
 32  \w     36.00 106.00   0.50    2.60    --   97.33 -95.00  30.00  140
 33  \w     37.00 109.00   0.50    2.60    --   97.33-111.00 -60.00  144
 34  \w     40.00  99.00   0.50    0.65    --   46.98-125.00-180.00  118
 35  \w     45.00 107.00   0.50    2.60    --   97.33-111.00-120.00  124
 36  \w     35.00  64.00   0.50    2.60    --   97.33 -61.00-180.00   58
 37  \w     32.00  98.00   0.50    2.60    --   97.33 -95.00-120.00  132
 38  \w     29.00  70.00   0.50    2.60    --   97.33 -61.00 -60.00   82
 39  \w     19.00 106.00   0.50    2.60    --   97.33 -95.00 -60.00  174
 40  \w     32.00 100.00   0.50    2.60    --   97.33 -77.00  30.00  136
 41  \w     23.00 109.00   0.50    2.60    --   97.33-111.00 150.00  172
 42  \w     28.00 120.00   0.50    0.65    --   46.98  46.00 -57.00  184
 43  \w    107.00 134.00   0.50    2.60    --   97.33  46.00 -57.00   54
 44  \w     85.00 111.00   0.50    0.65    --   62.00  77.00  36.38   52
 45  \w     72.00 121.00   0.50    2.60    --   97.33  77.00 120.00   98
 46  \w    107.00 134.00   0.50    0.65    --   66.00  80.00 171.32   54
 47  \w     63.00 126.00   0.50    2.60    --   97.33 178.00  90.00  126
 48  \w     43.00  68.00   0.50    0.65    --   70.00  80.00  70.19   50
 49  \w     38.00  65.00   0.50    0.65    --   66.00  80.00  55.91   54
 50  \w     35.00  67.00   0.50    0.65    --   62.00  80.00  -7.36   64
 51  \w     35.00  65.00   0.50    0.65    --   62.00  77.00  36.38   60
 52  \w     35.00  60.00   0.50    0.65    --   62.00  80.00 -32.98   50
 53  \w     46.00  72.00   0.50    2.60    --   74.00  80.00 -85.71   52
 54  \w     43.00  68.00   0.50    0.65    --   70.00  80.00-104.62   50
 55  \w     41.00  66.00   0.50    0.65    --   66.00  76.00-164.13   50
 56  \w     38.00  64.00   0.50    0.65    --   66.00  79.00-143.09   52
 57  \w     34.00  60.00   0.50    0.65    --   62.00  79.00 -98.65   52
 58  \w      8.00  33.00   0.50    0.65    --   42.00  92.00   1.63   50
 59  \w     16.00  41.00   0.50    0.65    --   50.00  92.00  20.13   50
 60  \w     17.00  42.00   0.50    0.65    --   50.00  90.00 -40.10   50
 61  \w     16.00  41.00   0.50    0.65    --   50.00  92.00-106.05   50
 62  \w     16.00  41.00   0.50    0.65    --   50.00  92.00-149.17   50
 63  \w    -13.00  12.00   0.50    0.65    --   26.00 102.00-129.29   50
 64  \w    -16.00  12.00   0.50    0.65    --   22.00 102.00 -25.74   56
 65  \w    -23.00   2.00   0.50    0.65    --   18.00 106.00  77.00   50
 66  \w      9.00  34.00   0.50    0.65    --   42.00  91.00 127.83   50
 67  \w     17.00  42.00   0.50    0.65    --   50.00  90.00 138.16   50
 68  \w     32.00  91.00   0.50    0.65    --   58.00  78.00 138.33  118
 69  \w     38.00  63.00   0.50    0.65    --   66.00  80.00 171.32   50
 70  \w     39.00  70.00   0.50    0.65    --   66.00  77.00 113.77   62
 71  \w     38.00  65.00   0.50    0.65    --   66.00  80.00 131.31   54
 72  \w     17.00  42.00   0.50    0.65    --   50.00  90.00  65.80   50
 73  \w    -57.00 -31.00   0.50    0.65    --   14.00 158.00 -84.74   52
 74  \w    -79.00 -53.00   0.50    2.60    --  -90.25 111.00  60.00   52
 75  \w   -125.00 -26.00   0.50    0.65    --  -46.98 -46.00 153.00  198
 76  \w   -108.00 -63.00   0.50    2.60    --  -90.25 -78.00 166.56   90
 77  \w   -131.00-105.00   0.50    2.60    --  -90.25 -46.00 153.00   52
 78  \w   -130.00 -62.00   0.50    2.60    --  -90.25 -80.00 106.46  136
 79  \w   -144.00-106.00   0.50    2.60    --  -90.25 -78.00 138.47   76
 80  \w   -146.00-109.00   0.50    2.60    --  -90.00 -78.00  58.00   74
 81  \w   -140.00 -62.00   0.50    2.60    --  -90.25 -80.00  42.80  156
 82  \w   -142.00 -93.00   0.50    2.60    --  -90.25 -74.00  44.62   98
 83  \w   -150.00 -63.00   0.50    2.60    --  -90.25 -77.00  86.73  174
 84  \w   -141.00-105.00   0.50    2.60    --  -90.25 -78.00  -5.99   72
 85  \w   -142.00 -98.00   0.50    2.60    --  -90.25 -77.00 -30.00   88
 86  \w   -153.00-119.00   0.50    2.60    --  -90.25 -74.00 -57.38   68
 87  \w   -157.00 -64.00   0.50    2.60    --  -90.25 -76.00  16.09  186
 88  \w   -144.00-101.00   0.50    2.60    --  -90.25 -77.00 150.86   86
 89  \w   -140.00 -63.00   0.50    2.60    --  -90.25 -77.00  78.29  154
 90  \w   -152.00 -62.00   0.50    2.60    --  -90.25 -79.00 -99.74  180
 91  \w   -143.00 -64.00   0.50    2.60    --  -90.25 -76.00-146.22  158
 92  \w   -156.00-118.00   0.50    2.60    --  -90.25 -77.00-120.00   76
 93  \w   -162.00-133.00   0.50    2.60    --  -90.25 -80.00 -73.85   58
 94  \w   -163.00 -62.00   0.50    2.60    --  -90.25 -79.00 -61.49  202
 95  \w   -164.00-133.00   0.50    2.60    --  -90.25 -80.00 106.46   62
 96  \w   -165.00-107.00   0.50    2.60    --  -90.25 -77.00 114.48  116
 97  \w   -157.00 -65.00   0.50    2.60    --  -90.25 -72.00   0.18  184
 98  \w   -164.00 -62.00   0.50    2.60    --  -90.25 -79.00-129.57  204
 99  \w   -166.00 -63.00   0.50    2.60    --  -90.25 -77.00-167.68  206
100  \w   -162.00 -63.00   0.50    2.60    --  -90.25 -77.00 -90.00  198
101  \w   -165.00 -63.00   0.50    2.60    --  -90.25 -77.00-180.00  204
102  \w   -166.00 -63.00   0.50    2.60    --  -90.25 -77.00 -44.16  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            191459
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.739
_diffrn_reflns_theta_min         3.735
_exptl_absorpt_coefficient_mu    4.301
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       plank
_exptl_crystal_F_000             2832
_exptl_crystal_recrystallization_method 'Dimethylsulfoxide and Ethyl acetate'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.094
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1390
_refine_ls_number_reflns         22345
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0766P)^2^+14.3416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20221
_reflns_number_total             22345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00209e2.cif
_cod_data_source_block           hage128_05g
_cod_depositor_comments
'Adding full bibliography for 1574215--1574217.cif.'
_cod_original_cell_volume        6177.96(14)
_cod_database_code               1574217
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.480
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-C84 = O7A-C84A
 1.21 with sigma of 0.001
 N8-C80 = N8A-C80
 1.42 with sigma of 0.001
 C84-C85 \\sim C84A-C85
 with sigma of 0.02
 C84-N8 \\sim C84A-N8
 with sigma of 0.02
 N8-C84 \\sim N8A-C84A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.01 within 2A
N4 \\sim C85 \\sim C86 \\sim C88 \\sim C89 \\sim C90: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.01 within 2A
Uanis(O7) = Uanis(O7A)
Uanis(C84) = Uanis(C84A)
Uanis(C85) = Uanis(C85A)
Uanis(C88) = Uanis(C88A)
Uanis(C89) = Uanis(C89A)
Uanis(C90) = Uanis(C90A)
Uanis(N4) = Uanis(N4A)
Uanis(N8) = Uanis(N8A)
Uanis(C86) = Uanis(C86A)
4. Others
 Sof(O7A)=Sof(N8A)=Sof(H8A)=Sof(C84A)=Sof(C85A)=Sof(C86A)=Sof(H86A)=Sof(N4A)=
 Sof(C88A)=Sof(H88A)=Sof(C89A)=Sof(H89A)=Sof(C90A)=Sof(H90A)=1-FVAR(1)
 Sof(O7)=Sof(N8)=Sof(H8)=Sof(C84)=Sof(C85)=Sof(C86)=Sof(H86)=Sof(N4)=Sof(C88)=
 Sof(H88)=Sof(C89)=Sof(H89)=Sof(C90)=Sof(H90)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C47(H47A,H47B), C76(H76A,H76B), C102(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N7(H7), C1(H1), C13(H13), C14(H14), C16(H16), C17(H17),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29),
  C30(H30), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
 C42(H42), C43(H43), C45(H45), C46(H46), C49(H49), C50(H50), C52(H52), C53(H53),
  C54(H54), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C64(H64),
 C65(H65), C66(H66), C68(H68), C71(H71), C72(H72), C74(H74), C75(H75), C78(H78),
  C79(H79), C81(H81), C82(H82), N8(H8), C86(H86), C88(H88), C89(H89), C90(H90),
 N8A(H8A), C86A(H86A), C88A(H88A), C89A(H89A), C90A(H90A), C92(H92), C94(H94),
 C96(H96), C99(H99), C100(H100), C104(H104), C105(H105), C110(H110), C111(H111),
  C112(H112), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120), C121(H121), C5(H5A), C6(H6A), C7(H7A), C9(H9),
 C10(H10), C11(H11), C32(H32)
5.c Fitted hexagon refined as free rotating group:
 C77(C78,C79,C80,C81,C82), C85(C86,N4,C88,C89,C90), C85A(C86A,N4A,C88A,C89A,
 C90A)
5.d Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C31(H31A,H31B,H31C)
;
_smtbx_masks_void_probe_radius   1.3
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51639
_shelx_fab_checksum              59303
_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
;