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_1574216
_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 Cl2 N16 O4 Pd Ru, 5.943(C0.337 H1.01 O0.168 S0.168), 8[C2H6SO]'
_chemical_formula_sum            'C118 H134 Cl2 N16 O13 Pd Ru S9'
_chemical_formula_weight         2551.31
_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_Hall           '-P 4a 2ac'
_space_group_name_H-M_alt        'P 4/n c c :2'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0390(3)
_cell_length_b                   18.0390(3)
_cell_length_c                   41.9278(11)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.6940
_cell_measurement_theta_min      3.4690
_cell_volume                     13643.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_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      100.00(10)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     55.00  85.00   0.25   12.50    --   47.23-157.00 -64.00  120
  2  \w   -106.00 -80.00   0.25   45.00    --  -90.25 157.00 -28.00  104
  3  \w     32.00  90.00   0.25   45.00    --   97.33 -78.00 -23.00  232
  4  \w     19.00  48.00   0.25   45.00    --   97.33 -44.00 159.00  116
  5  \w   -120.00 -74.00   0.25   12.50    --  -47.23-125.00-120.00  184
  6  \w    -23.00  23.00   0.25   12.50    --  -47.23  19.00 -90.00  184
  7  \w    -16.00  14.00   0.25   12.50    --  -47.23  19.00  60.00  120
  8  \w    -51.00 -26.00   0.25   45.00    --  -90.25  45.00-120.00  100
  9  \w    -39.00 -13.00   0.25   45.00    --  -90.25  45.00 -30.00  104
 10  \w    -51.00 -17.00   0.25   45.00    --  -90.25  45.00  90.00  136
 11  \w    -38.00 -12.00   0.25   45.00    --  -90.25  45.00  30.00  104
 12  \w     23.00  49.00   0.25   45.00    --   97.33 -45.00 120.00  104
 13  \w     20.00  46.00   0.25   45.00    --   97.33 -45.00  60.00  104
 14  \w     21.00  46.00   0.25   45.00    --   97.33 -45.00-180.00  100
 15  \w     20.00  45.00   0.25   45.00    --   97.33 -45.00 -90.00  100
 16  \w    106.00 151.00   0.25   45.00    --   97.33 111.00 150.00  180
 17  \w     32.00  64.00   0.25   45.00    --   97.33 -61.00 150.00  128
 18  \w     20.00  45.00   0.25   45.00    --   97.33 -45.00 -30.00  100
;
_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  0.1033
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            46648
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.690
_diffrn_reflns_theta_min         4.057
_exptl_absorpt_coefficient_mu    4.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             5304
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         6182
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0591
_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^)+(0.1308P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3475
_reflns_number_total             6182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00209e2.cif
_cod_data_source_block           hage-226_auto_pl
_cod_depositor_comments
'Adding full bibliography for 1574215--1574217.cif.'
_cod_original_cell_volume        13643.5(6)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               1574216
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.854
_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. Shared sites
{S1A, S1B}
{O2A, O2B}
3. Restrained distances
 C26A-S1A \\sim C26B-S1B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 2A
Uanis(C26A) = Uanis(C26B)
Uanis(S1A) = Uanis(S1B)
Uanis(O2A) = Uanis(O2B)
5. Others
 1*[Sof(S1A)+Sof(O2A)+Sof(C26A)+Sof(H26A)+Sof(H26B)+Sof(H26C)]+1*[Sof(S1B)+
 Sof(O2B)+Sof(C26B)+Sof(H26D)+Sof(H26E)+Sof(H26F)]=0.5 with esd of 0.0001
 Sof(S1A)=Sof(O2A)=0.5*FVAR(2)
 Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Sof(S1B)=Sof(O2B)=0.5*FVAR(3)
 Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=FVAR(2)
6.a Riding coordinates:
 N3(H3), C8(H8), C9(H9), C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
6.c Me refined with riding coordinates:
 C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C5(H5), C6(H6), C11(H11), C15(H15), C16(H16),
 C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25)
;
_smtbx_masks_void_probe_radius   1.5
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              65172
_shelx_fab_checksum              60022
_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
;