Exploiting reduced-symmetry ligands with pyridyl and imidazole donors to construct a second-generation stimuli-responsive heterobimetallic [PdPtL<sub>4</sub>]<sup>4+</sup> cage.
Pearcy, Aston C.; Lisboa, Lynn S.; Preston, Dan; Page, Nick B.; Lawrence, Tristan; Wright, L. James; Hartinger, Christian G.; Crowley, James D.; Chemical science 14 (2023) 8615–8623; doi:10.1039/d3sc01354e

data_1569523
_publ_section_title
;
 Exploiting reduced-symmetry ligands with pyridyl and imidazole donors to
 construct a second-generation stimuli-responsive heterobimetallic
 [PdPtL<sub>4</sub>]<sup>4+</sup> cage.
;
_journal_issue                   32
_journal_name_full               'Chemical science'
_journal_page_first              8615
_journal_page_last               8623
_journal_paper_doi               10.1039/d3sc01354e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C55 H42 N16 Pd, 2(B F4), 2(C4 H9 O)'
_chemical_formula_sum            'C63 H60 B2 F8 N16 O2 Pd'
_chemical_formula_weight         1353.29
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-22 deposited with the CCDC.	2023-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                74.354(4)
_cell_angle_beta                 86.080(4)
_cell_angle_gamma                61.495(6)
_cell_formula_units_Z            1
_cell_length_a                   10.1145(5)
_cell_length_b                   10.5040(6)
_cell_length_c                   17.3505(7)
_cell_measurement_reflns_used    12585
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      76.4870
_cell_measurement_theta_min      4.9661
_cell_volume                     1555.91(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3449
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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    -70.00  31.00   1.00    1.00    --  -42.04  57.00  60.00  101
  2  \w   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00 -90.00  100
  3  \w     18.00 116.00   1.00    1.00    --   42.04  38.00  30.00   98
  4  \w      9.00  42.00   1.00    1.00    --   42.04  80.00-100.24   33
  5  \w      9.00  42.00   1.00    1.00    --   42.04  79.00 122.18   33
  6  \w    -21.00  75.00   1.00    1.00    --   42.04 -77.00 150.00   96
  7  \w      8.00  34.00   1.00    1.00    --   42.04  83.00  46.03   26
  8  \w     30.00 106.00   1.00    2.00    --  112.00 -95.00  90.00   76
  9  \w     36.00 140.00   1.00    2.00    --  112.00 -30.00 120.00  104
 10  \w     84.00 178.00   1.00    2.00    --  112.00  30.00 120.00   94
 11  \w     36.00 145.00   1.00    2.00    --  112.00 -77.00 -60.00  109
 12  \w     35.00 108.00   1.00    2.00    --  112.00-109.00 -27.00   73
 13  \w     39.00 112.00   1.00    2.00    --  112.00-125.00  90.00   73
 14  \w     39.00 138.00   1.00    2.00    --  112.00 -45.00  30.00   99
 15  \w     97.00 178.00   1.00    2.00    --  112.00 125.00 150.00   81
 16  \w     39.00 112.00   1.00    2.00    --  112.00-125.00  30.00   73
 17  \w     36.00 140.00   1.00    2.00    --  112.00 -30.00-120.00  104
 18  \w     97.00 178.00   1.00    2.00    --  112.00 125.00 120.00   81
 19  \w     39.00 112.00   1.00    2.00    --  112.00-125.00-150.00   73
 20  \w     30.00 106.00   1.00    2.00    --  112.00 -95.00-120.00   76
 21  \w     40.00 141.00   1.00    2.00    --  112.00 -61.00 150.00  101
 22  \w    103.00 178.00   1.00    2.00    --  112.00  77.00 120.00   75
 23  \w     39.00 112.00   1.00    2.00    --  112.00-125.00 -90.00   73
 24  \w     86.00 178.00   1.00    2.00    --  112.00  45.00 -90.00   92
 25  \w     39.00 112.00   1.00    2.00    --  112.00-125.00-180.00   73
 26  \w     30.00 106.00   1.00    2.00    --  112.00 -95.00  30.00   76
 27  \w    103.00 178.00   1.00    2.00    --  112.00  77.00-150.00   75
 28  \w     97.00 178.00   1.00    2.00    --  112.00 125.00  30.00   81
 29  \w   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00-180.00  100
 30  \w   -122.00  -1.00   1.00    1.00    --  -42.04 -19.00  60.00  121
 31  \w      9.00  42.00   1.00    1.00    --   42.04  80.00-173.91   33
 32  \w     61.00 131.00   1.00    1.00    --   42.04 178.00  30.00   70
 33  \w      9.00  42.00   1.00    1.00    --   42.04  80.00  63.11   33
 34  \w      8.00  34.00   1.00    1.00    --   42.04  83.00-139.75   26
 35  \w     59.00 119.00   1.00    2.00    --  112.00  15.00  30.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0140216000
_diffrn_orient_matrix_UB_12      0.0227128000
_diffrn_orient_matrix_UB_13      0.0848482000
_diffrn_orient_matrix_UB_21      0.1322486000
_diffrn_orient_matrix_UB_22      -0.1598079000
_diffrn_orient_matrix_UB_23      0.0323282000
_diffrn_orient_matrix_UB_31      0.1118054000
_diffrn_orient_matrix_UB_32      0.0632214000
_diffrn_orient_matrix_UB_33      -0.0173283000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24535
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.287
_diffrn_reflns_theta_min         4.967
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.107
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       plate
_exptl_crystal_F_000             694
_exptl_crystal_preparation
'Slow vapour diffusion of diethyl ether into acetonitrile'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.168
_refine_diff_density_max         3.089
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6461
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0948
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2490
_refine_ls_wR_factor_ref         0.2592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6141
_reflns_number_total             6461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01354e2.cif
_cod_data_source_block           jdc007
_cod_depositor_comments
'Adding full bibliography for 1569522--1569526.cif.'
_cod_original_cell_volume        1555.92(16)
_cod_database_code               1569523
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C56H48N16PdB2F8
_chemical_oxdiff_usercomment     M404
_olex2_refinement_description
;
1. Restrained planarity
 C4, C00X, C017, C019, C015, C1AA
 with sigma of 0.01
 C00X, C017, C019, C015, C1AA
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C1AA \\sim C015 \\sim C019 \\sim C017 \\sim C4: within 1.7A with sigma of 0.03
and sigma for terminal atoms of 0.06 within 1.7A
Uanis(C1AA) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 C1AA, C019, C015, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, C017, C019, C1AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N00N(0.5) H00W(0.5) H00D(0.5) C4(0.5) H4(0.5) H017(0.5) N11(0.5)
 F1(0.5) F0AA(0.5) F5(0.5) F19(0.5)
 Fixed X: Pd01(0) H008(0.28846) H009(0.165221) H00A(0.11658) H00E(0.52477)
 H00G(0.22974) H00H(0.584829) H00B(0.48502) H00C(0.323071) H00K(0.00034)
 H00L(0.0514) H00Q(0.13402) H00R(0.31704) H00V(0.300361) H00Y(0.19523)
 H00Z(0.15058) H01A(0.482029) H01B(0.46076) H011(0.204909)
 Fixed Y: Pd01(0.5) H008(0.24515) H009(0.674399) H00A(0.318271) H00E(0.19458)
 H00G(0.877419) H00H(0.39029) H00B(1.045) H00C(1.090488) H00K(0.741961)
 H00L(0.774889) H00Q(0.5758) H00R(0.976499) H00V(1.331161) H00Y(1.476688)
 H00Z(1.377041) H01A(-0.13046) H01B(-0.11571) H011(1.128132)
 Fixed Z: Pd01(0.5) H008(0.482889) H009(0.437479) H00A(0.667101)
 H00E(0.439629) H00G(0.40078) H00H(0.39681) H00B(0.355081) H00C(0.38521)
 H00K(0.56091) H00L(0.680241) H00Q(0.793981) H00R(0.22285) H00V(0.27638)
 H00Y(0.14809) H00Z(0.05856) H01A(0.891721) H01B(0.979809) H011(0.0962)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C00W(H00D), C4(H4), C1AA(H1AA), C017(H017), C0AA(H0AA)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C2AA(H2AA,H2AB,H2AC)
;
_shelx_res_checksum              51829
_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 2.644
_oxdiff_exptl_absorpt_empirical_full_min 0.640