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_7132868
_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         'C88 H64 N16 Pt2, [+ solvents]'
_chemical_formula_sum            'C88 H64 N16 Pt2'
_chemical_formula_weight         1735.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 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                90
_cell_angle_beta                 98.888(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2019(9)
_cell_length_b                   21.4417(13)
_cell_length_c                   19.1515(13)
_cell_measurement_reflns_used    2940
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.9630
_cell_measurement_theta_min      4.1090
_cell_volume                     5761.9(6)
_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 0.995
_diffrn_measured_fraction_theta_max 0.963
_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    -63.00  30.00   1.00   75.00    --  -42.04  38.00 150.00   93
  2  \w     20.00  59.00   1.00   75.00    --   42.04 -99.00 -90.00   39
  3  \w     62.00  99.00   1.00   75.00    --   42.04 178.00 -60.00   37
  4  \w     13.00  54.00   1.00   75.00    --   42.04 -99.00  30.00   41
  5  \w    100.00 178.00   1.00  100.00    --  104.32 125.00-150.00   78
  6  \w     97.00 177.00   1.00  100.00    --  104.32 125.00 150.00   80
  7  \w     76.00 144.00   1.00  100.00    --  104.32  30.00 -60.00   68
  8  \w    121.00 168.00   1.00  100.00    --  104.32  77.00 -60.00   47
  9  \w     71.00 109.00   1.00  100.00    --  104.32 -61.00-150.00   38
 10  \w     45.00 125.00   1.00  100.00    --  104.32 -77.00 150.00   80
 11  \w     32.00  59.00   1.00  100.00    --  104.32 -61.00-150.00   27
;
_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      0.0753721000
_diffrn_orient_matrix_UB_12      -0.0508500000
_diffrn_orient_matrix_UB_13      -0.0047280000
_diffrn_orient_matrix_UB_21      -0.0522196000
_diffrn_orient_matrix_UB_22      -0.0440831000
_diffrn_orient_matrix_UB_23      0.0448264000
_diffrn_orient_matrix_UB_31      -0.0603476000
_diffrn_orient_matrix_UB_32      -0.0253891000
_diffrn_orient_matrix_UB_33      -0.0677553000
_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  0.0793
_diffrn_reflns_av_unetI/netI     0.1076
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11232
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.726
_diffrn_reflns_theta_min         4.674
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1720
_exptl_crystal_preparation
'Slow diffusion of diethyl ether into nitromethane'
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.965
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         5690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4067
_reflns_number_total             5690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00323c2.cif
_cod_data_source_block           Cnap
_cod_depositor_comments
'Adding full bibliography for 7132868--7132869.cif.'
_cod_original_cell_volume        5761.8(6)
_cod_database_code               7132868
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNPtBF
_chemical_oxdiff_usercomment     M701
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a 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),
 C14(H14), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55360
_shelx_fab_checksum              72747
_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 2.509
_oxdiff_exptl_absorpt_empirical_full_min 0.814