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_7133644
_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 Cl2 N16 O4 Pd Ru, 4(C4 H7 O2), 4(C3 H7 N O), 4[BF4]'
_chemical_formula_sum            'C100 H112 B4 Cl2 F16 N20 O16 Pd Ru'
_chemical_formula_weight         2475.786
_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'
_symmetry_Int_Tables_number      130
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.90303(5)
_cell_length_b                   18.90303(5)
_cell_length_c                   32.38790(13)
_cell_measurement_reflns_used    177767
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.1830
_cell_measurement_theta_min      2.7350
_cell_volume                     11572.99(6)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_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    -75.00  28.00   0.50    0.45    --  -47.23  81.00 109.00  206
  2  \w      0.00  58.00   0.50    0.45    --   47.23 -81.00 -12.00  116
  3  \w    -69.00 -29.00   0.50    1.79    --  -90.25  81.00 109.00   80
  4  \w   -136.00-102.00   0.50    1.79    --  -90.25 -81.00 -12.00   68
  5  \w    149.00 174.00   0.50    1.79    --   97.33  81.00 109.00   50
  6  \w    101.00 129.00   0.50    1.79    --   97.33  81.00 109.00   56
  7  \w    -61.00 -28.00   0.50    0.45    --   10.00 157.00  14.54   66
  8  \w    -53.00 -25.00   0.50    0.45    --   14.00 151.00 -78.89   56
  9  \w    -64.00 -32.00   0.50    0.45    --   14.00 165.00 165.30   64
 10  \w    -15.00  18.00   0.50    0.45    --   22.00 101.00-108.42   66
 11  \w      2.00  29.00   0.50    0.45    --   34.00  96.00 170.82   54
 12  \w      2.00  27.00   0.50    0.45    --   38.00  98.00  71.16   50
 13  \w     14.00  41.00   0.50    0.45    --   46.00  91.00 118.86   54
 14  \w   -101.00 -23.00   0.50    0.45    --  -47.23 -19.00-150.00  156
 15  \w     41.00 130.00   0.50    0.45    --   47.23  19.00  90.00  178
 16  \w     17.00  42.00   0.50    0.45    --   50.00  90.00-167.77   50
 17  \w     17.00  42.00   0.50    0.45    --   50.00  90.00 -83.61   50
 18  \w     17.00  42.00   0.50    0.45    --   50.00  90.00  33.19   50
 19  \w     16.00  41.00   0.50    0.45    --   50.00  92.00  98.44   50
 20  \w     17.00  42.00   0.50    0.45    --   50.00  90.00 -50.70   50
 21  \w     31.00  86.00   0.50    0.45    --   58.00  77.00  34.19  110
 22  \w     31.00  59.00   0.50    0.45    --   58.00  77.00 -15.82   56
 23  \w     71.00  98.00   0.50    0.45    --   58.00  77.00 -15.82   54
 24  \w     91.00 117.00   0.50    0.45    --   58.00  77.00 176.84   52
 25  \w     35.00 101.00   0.50    0.45    --   58.00  76.00 -68.57  132
 26  \w     31.00  67.00   0.50    0.45    --   58.00  77.00 176.84   72
 27  \w     84.00 132.00   0.50    0.45    --   58.00  76.00 128.22   96
 28  \w     32.00  57.00   0.50    0.45    --   58.00  76.00 128.22   50
 29  \w     35.00  61.00   0.50    0.45    --   62.00  77.00-105.78   52
 30  \w     36.00  77.00   0.50    0.45    --   62.00  76.00-166.09   82
 31  \w   -140.00-114.00   0.50    0.45    --  -66.00 -74.00  49.68   52
 32  \w    -67.00 -41.00   0.50    0.45    --  -66.00 -74.00  49.68   52
 33  \w    -69.00 -41.00   0.50    0.45    --  -66.00 -74.00 -45.67   56
 34  \w     41.00  67.00   0.50    0.45    --   66.00  75.00 127.61   52
 35  \w     41.00  78.00   0.50    0.45    --   66.00  75.00  61.88   74
 36  \w    119.00 145.00   0.50    0.45    --   70.00  77.00-155.44   52
 37  \w    -71.00 -43.00   0.50    0.45    --  -70.00 -76.00 -85.50   56
 38  \w    -71.00 -45.00   0.50    0.45    --  -70.00 -73.00 -62.55   52
 39  \w     43.00  70.00   0.50    0.45    --   70.00  77.00-155.44   54
 40  \w    -79.00 -48.00   0.50    1.79    --  -74.00 -76.00  14.10   62
 41  \w     47.00  76.00   0.50    1.79    --   74.00  77.00  13.79   58
 42  \w    -73.00 -47.00   0.50    1.79    --  -74.00 -77.00  86.19   52
 43  \w    -87.00 -51.00   0.50    1.79    --  -78.00 -77.00-125.12   72
 44  \w    -78.00 -53.00   0.50    1.79    --  -78.00 -72.00-117.86   50
 45  \w   -144.00-119.00   0.50    1.79    --  -78.00 -72.00-117.86   50
 46  \w    -77.00 -52.00   0.50    1.79    --  -78.00 -75.00 -94.70   50
 47  \w    -76.00 -51.00   0.50    1.79    --  -78.00 -76.00  54.59   50
 48  \w    -77.00 -51.00   0.50    1.79    --  -78.00 -76.00 143.34   52
 49  \w    -85.00 -51.00   0.50    1.79    --  -78.00 -76.00 158.57   68
 50  \w   -139.00-113.00   0.50    1.79    --  -78.00 -75.00 -94.70   52
 51  \w    -87.00 -56.00   0.50    1.79    --  -82.00 -75.00 130.41   62
 52  \w   -153.00-105.00   0.50    1.79    --  -86.00 -77.00-145.50   96
 53  \w    -84.00 -59.00   0.50    1.79    --  -86.00 -77.00-145.50   50
 54  \w    -88.00 -59.00   0.50    1.79    --  -86.00 -77.00 -14.23   58
 55  \w   -166.00 -63.00   0.50    1.79    --  -90.25 -77.00  53.26  206
 56  \w   -131.00 -63.00   0.50    1.79    --  -90.25 -77.00   7.92  136
 57  \w   -165.00 -64.00   0.50    1.79    --  -90.25 -74.00 -52.88  202
 58  \w    -92.00 -63.00   0.50    1.79    --  -90.25 -77.00  90.00   58
 59  \w   -164.00 -63.00   0.50    1.79    --  -90.25 -77.00 -60.00  202
 60  \w   -156.00-104.00   0.50    1.79    --  -90.25 -77.00  90.00  104
 61  \w    -89.00 -63.00   0.50    1.79    --  -90.25 -77.00  30.00   52
 62  \w   -146.00-106.00   0.50    1.79    --  -90.25 -77.00  30.00   80
 63  \w   -103.00 -64.00   0.50    1.79    --  -90.25 -76.00 165.15   78
 64  \w   -166.00-110.00   0.50    1.79    --  -90.25 -76.00 165.15  112
 65  \w   -158.00 -66.00   0.50    1.79    --  -90.25 -71.00  97.16  184
 66  \w   -146.00 -64.00   0.50    1.79    --  -90.25 -77.00-150.00  164
 67  \w   -128.00 -64.00   0.50    1.79    --  -90.25 -76.00-115.75  128
 68  \w   -163.00 -63.00   0.50    1.79    --  -90.25 -77.00-131.22  200
 69  \w   -144.00 -71.00   0.50    1.79    --  -90.25 -70.00  12.57  146
 70  \w    -89.00 -64.00   0.50    1.79    --  -90.25 -76.00-173.88   50
 71  \w   -153.00 -66.00   0.50    1.79    --  -90.25 -73.00 -25.50  174
 72  \w   -130.00-104.00   0.50    1.79    --  -90.25 -76.00-173.88   52
 73  \w   -166.00-141.00   0.50    1.79    --  -90.25 -76.00-115.75   50
 74  \w   -158.00 -64.00   0.50    1.79    --  -90.25 -76.00 117.44  188
 75  \w    -89.00 -64.00   0.50    1.79    --  -90.25 -74.00  37.11   50
 76  \w    -82.00 -36.00   0.50    1.79    --  -90.25 111.00  90.00   92
 77  \w    -98.00 -65.00   0.50    1.79    --  -90.25 -73.00 148.75   66
 78  \w   -165.00-102.00   0.50    1.79    --  -90.25 -74.00  37.11  126
 79  \w   -138.00 -64.00   0.50    1.79    --  -90.25 -76.00-101.58  148
 80  \w   -156.00-125.00   0.50    1.79    --  -90.25 -73.00 148.75   62
 81  \w    -96.00 -63.00   0.50    1.79    --  -90.25 -77.00 -30.00   66
 82  \w   -154.00 -64.00   0.50    1.79    --  -90.25 -77.00-180.00  180
 83  \w   -157.00-125.00   0.50    1.79    --  -90.25 -77.00 -30.00   64
 84  \w    -89.00 -64.00   0.50    1.79    --  -90.25 -76.00 -78.65   50
 85  \w   -117.00 -91.00   0.50    1.79    --  -90.25 -76.00 -78.65   52
 86  \w    -99.00 -64.00   0.50    1.79    --  -90.25 -75.00  63.39   70
 87  \w   -100.00 -64.00   0.50    1.79    --  -90.25 -74.00 126.97   72
 88  \w   -165.00-117.00   0.50    1.79    --  -90.25 -74.00 126.97   96
 89  \w   -156.00 -64.00   0.50    1.79    --  -90.25 -77.00 -90.00  184
 90  \w   -149.00-104.00   0.50    1.79    --  -90.25 -75.00  63.39   90
 91  \w     51.00 103.00   0.50    1.79    --   97.33-111.00  60.00  104
 92  \w     26.00  62.00   0.50    1.79    --   97.33-111.00 -30.00   72
 93  \w     43.00 100.00   0.50    1.79    --   97.33-111.00   0.00  114
 94  \w     34.00 108.00   0.50    1.79    --   97.33-111.00  90.00  148
 95  \w     21.00  47.00   0.50    1.79    --   97.33 -45.00  30.00   52
 96  \w     32.00 109.00   0.50    1.79    --   97.33-111.00-120.00  154
 97  \w     18.00  96.00   0.50    1.79    --   97.33 -95.00-180.00  156
 98  \w     34.00  98.00   0.50    1.79    --   97.33 -95.00-120.00  128
 99  \w     82.00 109.00   0.50    1.79    --   97.33-111.00 -60.00   54
100  \w     54.00  80.00   0.50    1.79    --   97.33-111.00 -60.00   52
101  \w     54.00 103.00   0.50    1.79    --   97.33-111.00 120.00   98
102  \w    107.00 133.00   0.50    1.79    --   97.33 178.00 120.00   52
103  \w     62.00  87.00   0.50    1.79    --   97.33 178.00 120.00   50
104  \w     29.00 107.00   0.50    1.79    --   97.33-111.00-180.00  156
105  \w     42.00 100.00   0.50    1.79    --   97.33 -77.00-120.00  116
106  \w     67.00 109.00   0.50    1.79    --   97.33-111.00 -30.00   84
107  \w     87.00 112.00   0.50    1.79    --   97.33 -81.00 -12.00   50
108  \w     49.00  78.00   0.50    1.79    --   97.33 -81.00 -12.00   58
;
_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      -0.0339247000
_diffrn_orient_matrix_UB_12      0.0574852000
_diffrn_orient_matrix_UB_13      0.0272851000
_diffrn_orient_matrix_UB_21      0.0620834000
_diffrn_orient_matrix_UB_22      -0.0060812000
_diffrn_orient_matrix_UB_23      0.0306571000
_diffrn_orient_matrix_UB_31      0.0404888000
_diffrn_orient_matrix_UB_32      0.0574172000
_diffrn_orient_matrix_UB_33      -0.0240533000
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0065
_diffrn_reflns_Laue_measured_fraction_full 0.9990
_diffrn_reflns_Laue_measured_fraction_max 0.9990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            349032
_diffrn_reflns_point_group_measured_fraction_full 0.9990
_diffrn_reflns_point_group_measured_fraction_max 0.9990
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         67.72
_diffrn_reflns_theta_min         4.29
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.550
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68004
_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    1.421
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5095.860
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.7312
_refine_diff_density_min         -0.7206
_refine_diff_density_rms         0.0878
_refine_ls_d_res_high            0.8331
_refine_ls_d_res_low             10.3085
_refine_ls_goodness_of_fit_ref   1.0677
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    65
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5252
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.0634
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+25.7787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                5088
_reflns_number_total             5252
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc03613a2.cif
_cod_data_source_block           HAGE-179
_cod_depositor_comments
'Adding full bibliography for 7133640--7133644.cif.'
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_original_formula_sum        'C100 H112 B4 Cl2 F16 N20 O16 Pd1 Ru1'
_cod_database_code               7133644
_chemical_oxdiff_formula         C72H56B2Cl2F8N18O4PdRu
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1Ia,H1Ib,H1Ic} of C1I, {H1Da,H1Db,H1Dc} of C1D, All N(H)
  groups
 At 1.5 times of:
  {H22a,H22b,H22c} of C22, {H1Aa,H1Ab,H1Ac} of C1A, {H1Ca,H1Cb,H1Cc} of C1C,
  {H19a,H19b,H19c} of C19
2. Restrained distances
 N6-C1B \\sim N6A-C23
 with sigma of 0.02
 N6-C1C \\sim N6A-C1A
 with sigma of 0.02
 C1C-C1D \\sim C1A-C1I
 with sigma of 0.04
 N6-C1D \\sim N6A-C1I
 with sigma of 0.02
 H1Db-H1Da \\sim H1Ib-H1Ia
 with sigma of 0.04
 C1B-C1C \\sim C23-C1A
 with sigma of 0.04
 O1A-C1B \\sim O1B-C23
 with sigma of 0.02
 C1D-H1Db \\sim C1I-H1Ib
 with sigma of 0.02
 C1B-C1D \\sim C23-C1I
 with sigma of 0.04
 C1D-H1Dc \\sim C1I-H1Ic
 with sigma of 0.02
 C1D-H1Da \\sim C1I-H1Ia
 with sigma of 0.02
 H1Db-H1Dc \\sim H1Ib-H1Ic
 with sigma of 0.04
 N6-O1A \\sim N6A-O1B
 with sigma of 0.04
 N6-H1Db \\sim N6A-H1Ib
 with sigma of 0.04
 H1Dc-H1Da \\sim H1Ic-H1Ia
 with sigma of 0.04
 N6-H1Dc \\sim N6A-H1Ic
 with sigma of 0.04
 N6-H1Da \\sim N6A-H1Ia
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C13 \\sim C11: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C1I) = Uanis(C1D)
Uanis(N6) = Uanis(N6A)
Uanis(C1A) = Uanis(C1C)
Uanis(C1B) = Uanis(C23)
Uanis(O1B) = Uanis(O1A)
4. Others
 Sof(O1B)=Sof(N6A)=Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(C1I)=Sof(H1Ia)=
 Sof(H1Ib)=Sof(H1Ic)=Sof(C23)=Sof(H23)=1-FVAR(1)
 Sof(O1A)=Sof(N6)=Sof(C1B)=Sof(H1B)=Sof(C1C)=Sof(H1Ca)=Sof(H1Cb)=Sof(H1Cc)=
 Sof(C1D)=Sof(H1Da)=Sof(H1Db)=Sof(H1Dc)=FVAR(1)
5.a Free rotating group:
 C13(C1)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C3(H3a), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12),
 C1(H1), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C1B(H1B), C23(H23)
5.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C22(H22a,H22b,H22c), C1C(H1Ca,H1Cb,H1Cc), C1D(H1Da,H1Db,
 H1Dc), C1A(H1Aa,H1Ab,H1Ac), C1I(H1Ia,H1Ib,H1Ic)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.939
_oxdiff_exptl_absorpt_empirical_full_min 0.612