Modulating the guest binding ability within mixed-coordination geometry [Pd(μ-L)<sub>4</sub>RuCl<sub>2</sub>]<sup>2+</sup> and [Pd(μ-L)<sub>4</sub>Pt]<sup>4+</sup> cage architectures.
Gearing, Hayden B.; Söhnel, Tilo; Young, Paul; Lisboa, Lynn; Wright, L. James; Crowley, James D.; Hartinger, Christian G.; Chemical communications (Cambridge, England) 60 (2024) 10950–10953; doi:10.1039/d4cc03613a

data_7133642
_publ_section_title
;
 Modulating the guest binding ability within mixed-coordination geometry
 [Pd(&#x3bc;-L)<sub>4</sub>RuCl<sub>2</sub>]<sup>2+</sup> and
 [Pd(&#x3bc;-L)<sub>4</sub>Pt]<sup>4+</sup> cage architectures.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10950
_journal_page_last               10953
_journal_paper_doi               10.1039/d4cc03613a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C72 H56 N16 O4 Pd Pt, 4(C2 H6 O S), 4(B F4)'
_chemical_formula_sum            'C80 H80 B4 F16 N16 O8 Pd Pt S4'
_chemical_formula_weight         2170.57
_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     direct
_audit_creation_date             2024-06-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-01 deposited with the CCDC.	2024-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.0374(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.89755(20)
_cell_length_b                   18.63351(19)
_cell_length_c                   23.8075(2)
_cell_measurement_reflns_used    55518
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.2020
_cell_measurement_theta_min      2.9970
_cell_volume                     8792.80(15)
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -78.00  29.00   0.50    0.69    --  -46.98  86.00   8.00  214
  2  \w      5.00  32.00   0.50    0.69    --   46.98 -86.00-109.00   54
  3  \w   -168.00-123.00   0.50    2.75    --  -90.25 -86.00-109.00   90
  4  \w    -71.00 -44.00   0.50    2.75    --  -90.25  86.00   8.00   54
  5  \w    122.00 162.00   0.50    2.75    --   97.33  86.00   8.00   80
  6  \w     64.00 103.00   0.50    2.75    --   97.33 -86.00-109.00   78
  7  \w   -122.00 -74.00   0.50    0.69    --  -46.98-125.00 -60.00   96
  8  \w    -93.00 -52.00   0.50    0.69    --  -46.98 -57.00 120.00   82
  9  \w   -120.00 -27.00   0.50    0.69    --  -46.98 -57.00-120.00  186
 10  \w   -113.00 -34.00   0.50    0.69    --  -46.98 -38.00  30.00  158
 11  \w     48.00  97.00   0.50    0.69    --   46.98-125.00  90.00   98
 12  \w    -33.00  23.00   0.50    0.69    --   46.98 -19.00-120.00  112
 13  \w    -25.00   3.00   0.50    0.69    --   46.98 -19.00-180.00   56
 14  \w   -171.00 -72.00   0.50    2.75    --  -90.25 -30.00-180.00  198
 15  \w   -111.00 -70.00   0.50    2.75    --  -90.25 -30.00 -60.00   82
 16  \w    -90.00 -38.00   0.50    2.75    --  -90.25 178.00 120.00  104
 17  \w   -125.00 -95.00   0.50    2.75    --  -90.25 178.00 120.00   60
 18  \w    -66.00 -40.00   0.50    2.75    --  -90.25  61.00-150.00   52
 19  \w   -126.00 -99.00   0.50    2.75    --  -90.25-111.00 150.00   54
 20  \w    -64.00 -36.00   0.50    2.75    --  -90.25  61.00   0.00   56
 21  \w   -170.00-137.00   0.50    2.75    --  -90.25 -30.00 -60.00   66
 22  \w   -120.00 -84.00   0.50    2.75    --  -90.25 -30.00 150.00   72
 23  \w   -169.00 -71.00   0.50    2.75    --  -90.25 -30.00  90.00  196
 24  \w    -49.00 -18.00   0.50    2.75    --  -90.25  45.00   0.00   62
 25  \w   -169.00-140.00   0.50    2.75    --  -90.25 -30.00 150.00   58
 26  \w     25.00 109.00   0.50    2.75    --   97.33-111.00 -30.00  168
 27  \w     78.00 140.00   0.50    2.75    --   97.33  45.00 -60.00  124
 28  \w     20.00  55.00   0.50    2.75    --   97.33 -95.00  30.00   70
 29  \w     25.00  71.00   0.50    2.75    --   97.33 -61.00  90.00   92
 30  \w     23.00  51.00   0.50    2.75    --   97.33 -45.00  90.00   56
 31  \w     61.00 100.00   0.50    2.75    --   97.33 -95.00  30.00   78
 32  \w     80.00 109.00   0.50    2.75    --   97.33-111.00 120.00   58
 33  \w     25.00  50.00   0.50    2.75    --   97.33 -61.00  30.00   50
 34  \w    122.00 172.00   0.50    2.75    --   97.33  45.00 -30.00  100
 35  \w     26.00  67.00   0.50    2.75    --   97.33 -61.00-120.00   82
 36  \w     79.00 113.00   0.50    2.75    --   97.33  45.00 -30.00   68
 37  \w     20.00  47.00   0.50    2.75    --   97.33 -45.00 -30.00   54
 38  \w     96.00 135.00   0.50    2.75    --   97.33  30.00 -60.00   78
 39  \w     21.00  48.00   0.50    2.75    --   97.33 -45.00   0.00   54
 40  \w     18.00 105.00   0.50    2.75    --   97.33 -95.00-120.00  174
 41  \w     20.00  45.00   0.50    2.75    --   97.33 -45.00  60.00   50
 42  \w    148.00 173.00   0.50    2.75    --   97.33  30.00 -60.00   50
 43  \w     20.00  49.00   0.50    2.75    --   97.33 -45.00-120.00   58
 44  \w     73.00 103.00   0.50    2.75    --   97.33 -95.00 -30.00   60
 45  \w    139.00 166.00   0.50    2.75    --   97.33  45.00 120.00   54
 46  \w     86.00 165.00   0.50    2.75    --   97.33  61.00  90.00  158
 47  \w     20.00  46.00   0.50    2.75    --   97.33 -45.00-180.00   52
 48  \w     26.00  71.00   0.50    2.75    --   97.33-111.00 120.00   90
 49  \w     97.00 124.00   0.50    2.75    --   97.33  45.00 120.00   54
 50  \w     64.00 101.00   0.50    2.75    --   97.33 -77.00 -60.00   74
 51  \w     31.00  66.00   0.50    2.75    --   97.33 -95.00 -30.00   70
 52  \w     26.00  51.00   0.50    2.75    --   97.33 -45.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0507081000
_diffrn_orient_matrix_UB_12      0.0477504000
_diffrn_orient_matrix_UB_13      0.0279169000
_diffrn_orient_matrix_UB_21      -0.0556670000
_diffrn_orient_matrix_UB_22      -0.0565568000
_diffrn_orient_matrix_UB_23      -0.0136026000
_diffrn_orient_matrix_UB_31      0.0192904000
_diffrn_orient_matrix_UB_32      -0.0368098000
_diffrn_orient_matrix_UB_33      0.0570580000
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            121705
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.740
_diffrn_reflns_theta_min         3.728
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77304
_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_density_diffrn    1.640
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.509
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.092
_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     1242
_refine_ls_number_reflns         15924
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0495P)^2^+23.7342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13969
_reflns_number_total             15924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03613a2.cif
_cod_data_source_block           2b_hage-110
_cod_depositor_comments
'Adding full bibliography for 7133640--7133644.cif.'
_cod_original_cell_volume        8792.79(15)
_cod_database_code               7133642
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C72H56B4F16N16O4PdPt
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.494
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{O8, O8A}
3. Restrained distances
 B3-F20 = B3-F21 = B3-F22 = B3-F23 = B3A-F20A = B3A-F21A = B3A-F22A = B3A-F23A
 1.4 with sigma of 0.002
 C75-S3 \\sim C75A-S3A
 with sigma of 0.02
 S3-C73 \\sim S3A-C6A
 with sigma of 0.02
 S3-C75 \\sim S3A-C75A
 with sigma of 0.02
 S3-O76 \\sim S3A-O76A
 with sigma of 0.02
 O73-S1 \\sim O73A-S1A
 with sigma of 0.02
 C82-S1 \\sim C83-S1A
 with sigma of 0.02
 S1-C74 \\sim S1A-C81
 with sigma of 0.02
 C77-S5 \\sim C77A-S5A
 with sigma of 0.02
 C78-S5 \\sim C78A-S5A
 with sigma of 0.02
 C77-C78 \\sim C77A-C78A
 with sigma of 0.02
 S5-O8 \\sim S5A-O8A
 with sigma of 0.02
 B2-F7 \\sim B2-F8 \\sim B2-F9 \\sim B2-F10
 with sigma of 0.002
 F20-F21 \\sim F21-F22 \\sim F22-F23 \\sim F23-F20
 with sigma of 0.04
 F20A-F21A \\sim F21A-F22A \\sim F22A-F23A \\sim F23A-F20A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C75 \\sim O76 \\sim S3 \\sim C73: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
C82 \\sim O73 \\sim S1 \\sim C74: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
Uanis(C75) = Uanis(C75A)
Uanis(O76) = Uanis(O76A)
Uanis(C73) = Uanis(C6A)
Uanis(S3) = Uanis(S3A)
Uanis(O73) = Uanis(O73A)
Uanis(C82) = Uanis(C83)
Uanis(C74) = Uanis(C81)
Uanis(S1) = Uanis(S1A)
Uanis(C77) = Uanis(C77A)
Uanis(C78) = Uanis(C78A)
Uanis(S5) = Uanis(S5A)
Uanis(O8) = Uanis(O8A)
Uanis(F7) = Uanis(F8)
Uanis(F9) = Uanis(F10)
Uanis(B3) = Uanis(B3A)
Uanis(F20) = Uanis(F20A)
Uanis(F21) = Uanis(F21A)
Uanis(F22) = Uanis(F22A)
Uanis(F23) = Uanis(F23A)
5. Others
 Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(O76A)=Sof(S3A)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(H6AC)=1-FVAR(1)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(O76)=Sof(S3)=Sof(C73)=Sof(H73A)=
 Sof(H73B)=Sof(H73C)=FVAR(1)
 Sof(O73A)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=Sof(S1A)=Sof(C81)=Sof(H81A)=
 Sof(H81B)=Sof(H81C)=Sof(B3A)=Sof(F23A)=Sof(F20A)=Sof(F22A)=Sof(F21A)=1-FVAR(2)
 Sof(O73)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(S1)=Sof(C74)=Sof(H74A)=
 Sof(H74B)=Sof(H74C)=Sof(B3)=Sof(F20)=Sof(F21)=Sof(F22)=Sof(F23)=FVAR(2)
 Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=Sof(C78A)=Sof(H78D)=Sof(H78E)=
 Sof(H78F)=Sof(S5A)=Sof(O8A)=Sof(F7)=Sof(F10)=1-FVAR(3)
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=
 Sof(S5)=Sof(O8)=Sof(F8)=Sof(F9)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N7(H7), N11(H11), N15(H15), C1(H1), C2(H2), C3(H3A), C5(H5), C6(H6),
 C8(H8), C9(H9), C10(H10), C12(H12), C15(H15A), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C30(H30), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C48(H48), C51(H51),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59),
 C60(H60), C62(H62), C63(H63), C64(H64), C66(H66), C69(H69), C70(H70), C71(H71),
  C72(H72)
6.b Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C74(H74A,H74B,H74C), C83(H83A,H83B,H83C), C81(H81A,H81B,
 H81C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C77A(H77D,H77E,H77F),
 C78A(H78D,H78E,H78F), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C75(H75A,H75B,
 H75C), C73(H73A,H73B,H73C), C75A(H75D,H75E,H75F), C6A(H6AA,H6AB,H6AC)
;
_shelx_res_checksum              15077
_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 1.982
_oxdiff_exptl_absorpt_empirical_full_min 0.569