A dynamic covalent approach to [Pt<sub><i>n</i></sub>L<sub>2<i>n</i></sub>]<sup>2<i>n</i>+</sup> cages.
van Hilst, Quinn V. C.; Pearcy, Aston C.; Preston, Dan; Wright, L. James; Hartinger, Christian G.; Brooks, Heather J. L.; Crowley, James D.; Chemical communications (Cambridge, England) 60 (2024) 4302–4305; doi:10.1039/d4cc00323c

data_7132869
_publ_section_title
;
 A dynamic covalent approach to
 [Pt<sub><i>n</i></sub>L<sub>2<i>n</i></sub>]<sup>2<i>n</i>+</sup> cages.
;
_journal_issue                   32
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4302
_journal_page_last               4305
_journal_paper_doi               10.1039/d4cc00323c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C100 H80 N16 Pt2, 4(B F4)'
_chemical_formula_sum            'C100 H80 B4 F16 N16 Pt2'
_chemical_formula_weight         2243.22
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-27 deposited with the CCDC.	2024-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                87.192(3)
_cell_angle_beta                 75.514(3)
_cell_angle_gamma                86.266(3)
_cell_formula_units_Z            1
_cell_length_a                   11.1598(4)
_cell_length_b                   14.8934(5)
_cell_length_c                   17.8869(6)
_cell_measurement_reflns_used    12525
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.0460
_cell_measurement_theta_min      4.0580
_cell_volume                     2870.67(18)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(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 0.981
_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   -114.00 -14.00   1.00    1.00    --  -41.67 -57.00 -60.00  100
  2  \w    -70.00  31.00   1.00    1.00    --  -41.67  57.00-150.00  101
  3  \w   -114.00 -14.00   1.00    1.00    --  -41.67 -57.00  60.00  100
  4  \w    -21.00  74.00   1.00    1.00    --   41.67 -77.00 -60.00   95
  5  \w      8.00  42.00   1.00    1.00    --   41.67  82.00 -70.10   34
  6  \w     31.00 112.00   1.00    1.00    --  104.32-125.00  90.00   81
  7  \w     22.00 106.00   1.00    1.00    --  104.32 -95.00-120.00   84
  8  \w     22.00 106.00   1.00    1.00    --  104.32 -95.00 150.00   84
  9  \w     22.00 106.00   1.00    1.00    --  104.32 -95.00-180.00   84
 10  \w     31.00 130.00   1.00    1.00    --  104.32 -45.00-120.00   99
 11  \w     22.00 106.00   1.00    1.00    --  104.32 -95.00   0.00   84
 12  \w     28.00 133.00   1.00    1.00    --  104.32 -30.00 -30.00  105
 13  \w    103.00 178.00   1.00    1.00    --  104.32  77.00 -30.00   75
 14  \w     16.00 178.00   1.00    1.00    --  104.32   0.00 150.00  162
 15  \w    103.00 178.00   1.00    1.00    --  104.32  77.00-120.00   75
 16  \w     22.00 106.00   1.00    1.00    --  104.32 -95.00 -90.00   84
 17  \w     28.00 109.00   1.00    1.00    --  104.32-111.00 119.10   81
 18  \w   -116.00 -17.00   1.00    1.00    --  -41.67 -38.00-180.00   99
 19  \w      8.00  42.00   1.00    1.00    --   41.67  82.00  36.49   34
 20  \w      6.00  83.00   1.00    1.00    --   41.67 -99.00  60.00   77
 21  \w      8.00  42.00   1.00    1.00    --   41.67  81.00-174.98   34
 22  \w      9.00  42.00   1.00    1.00    --   41.67  76.00-152.77   33
 23  \w     75.00 177.00   1.00    1.00    --  104.32  61.00-180.00  102
 24  \w     52.00 178.00   1.00    1.00    --  104.32  15.00 -60.00  126
 25  \w     75.00 177.00   1.00    1.00    --  104.32  61.00 -60.00  102
 26  \w     75.00 177.00   1.00    1.00    --  104.32  61.00  60.00  102
 27  \w     75.00 116.00   1.00    1.00    --  104.32  61.00 120.00   41
 28  \w     75.00 177.00   1.00    1.00    --  104.32  61.00   0.00  102
;
_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      -0.1210325000
_diffrn_orient_matrix_UB_12      0.0069631000
_diffrn_orient_matrix_UB_13      -0.0270596000
_diffrn_orient_matrix_UB_21      0.0572614000
_diffrn_orient_matrix_UB_22      -0.0674367000
_diffrn_orient_matrix_UB_23      -0.0635305000
_diffrn_orient_matrix_UB_31      -0.0496159000
_diffrn_orient_matrix_UB_32      -0.0784946000
_diffrn_orient_matrix_UB_33      0.0561599000
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42580
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.776
_diffrn_reflns_theta_min         3.855
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.112
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   gaussian
_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 light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_recrystallization_method
'Slow diffusion of diethyl ether into a concentrated nitromethane solution of the cage'
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.201
_refine_diff_density_max         2.560
_refine_diff_density_min         -2.639
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         11226
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1192P)^2^+3.5381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.1998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8987
_reflns_number_total             11226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00323c2.cif
_cod_data_source_block           C4_4
_cod_depositor_comments
'Adding full bibliography for 7132868--7132869.cif.'
_cod_database_code               7132869
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNPtBFO
_chemical_oxdiff_usercomment     M694
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Restrained distances
 B2-F5 \\sim B2-F6 \\sim B2-F7 \\sim B2-F8
 with sigma of 0.02
 F5-F6 \\sim F5-F7 \\sim F5-F8 \\sim F6-F7 \\sim F6-F8 \\sim F7-F8
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
B2 \\sim F5 \\sim F6 \\sim F7 \\sim F8: within 2.5A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2.5A
Uanis(B2) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim
Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of
0.01
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C38(H38A,H38B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C33(H33),
 C34(H34), C36(H36), C37(H37), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
  C47(H47), C48(H48), C49(H49), C50(H50)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83525
_shelx_fab_checksum              32319
_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 2.717
_oxdiff_exptl_absorpt_empirical_full_min 0.715