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_7133641
_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, C2 H6 O S, 4[BF4]'
_chemical_formula_sum            'C74 H62 B4 Cl2 F16 N16 O5 Pd Ru S'
_chemical_formula_weight         1913.06
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-12-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_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            2
_cell_length_a                   17.58370(10)
_cell_length_b                   17.58370(10)
_cell_length_c                   16.0276(2)
_cell_measurement_reflns_used    14734
_cell_measurement_temperature    109.99(14)
_cell_measurement_theta_max      73.3180
_cell_measurement_theta_min      3.5590
_cell_volume                     4955.52(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (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_environment      N~2~
_diffrn_ambient_temperature      109.99(14)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_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    -24.00  74.00   0.50    1.81    --   -0.62  77.00  90.00  196
  2  \w     82.00 172.00   0.50    7.25    --   97.44  52.00   7.00  180
  3  \w     82.00 174.00   0.50    7.25    --   97.44 108.00  89.00  184
  4  \w     23.00  59.00   0.50    7.25    --   97.44 -52.00-137.00   72
  5  \w     26.00  71.00   0.50    7.25    --   97.44 -61.00 -90.00   90
  6  \w     20.00 106.00   0.50    7.25    --   97.44 -94.00   0.00  172
  7  \w    -23.00  34.00   0.50    1.81    --   -0.62 -99.00 -60.00  114
  8  \w    -73.00  16.00   0.50    1.81    --   -0.62 -57.00 -30.00  178
  9  \w    -51.00 -22.00   0.50    7.25    --  -98.69  45.00-180.00   58
 10  \w    -71.00 -27.00   0.50    7.25    --  -98.69  61.00  60.00   88
 11  \w    -51.00 -22.00   0.50    7.25    --  -98.69  45.00  60.00   58
 12  \w    -80.00  14.00   0.50    1.81    --   -0.62 -19.00 120.00  188
 13  \w   -177.00-139.00   0.50    7.25    --  -98.69 -30.00 -90.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0549593000
_diffrn_orient_matrix_UB_12      -0.0234168000
_diffrn_orient_matrix_UB_13      -0.0703514000
_diffrn_orient_matrix_UB_21      -0.0445247000
_diffrn_orient_matrix_UB_22      0.0502210000
_diffrn_orient_matrix_UB_23      -0.0618929000
_diffrn_orient_matrix_UB_31      0.0517256000
_diffrn_orient_matrix_UB_32      0.0678422000
_diffrn_orient_matrix_UB_33      0.0214343000
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23009
_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         67.712
_diffrn_reflns_theta_min         3.555
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+5.1851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3878
_reflns_number_total             4500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03613a2.cif
_cod_data_source_block           2a_hage180
_cod_depositor_comments
'Adding full bibliography for 7133640--7133644.cif.'
_cod_original_cell_volume        4955.52(8)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7133641
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.598
_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. Others
 Fixed Sof: C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5)
3.a Riding coordinates:
 N3(H3), C6(H6)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C15(H15), C5(H5), C16(H16), C12(H12), C18(H18), C10(H10),
 C17(H17), C2(H2), C3(H3A), C1(H1)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61854
_shelx_fab_checksum              22466
_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 2.045
_oxdiff_exptl_absorpt_empirical_full_min 0.307