A cyclic manipulation of cage isomers <i>via</i> anion exchange and thermal isomerism.
Park, Seonghyeon; Kim, Dongwon; Kim, Doheon; Kim, Dongwook; Jung, Ok-Sang; Chemical communications (Cambridge, England) 57 (2021) 2919–2922; doi:10.1039/d0cc08303h

data_7127946
_publ_section_title
;
 A cyclic manipulation of cage isomers <i>via</i> anion exchange and
 thermal isomerism.
;
_journal_issue                   23
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2919
_journal_page_last               2922
_journal_paper_doi               10.1039/d0cc08303h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'C140 H188 Cl8 N16 O34 Pd4 S2 Si8'
_chemical_formula_weight         3637.09
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                105.10(3)
_cell_angle_beta                 108.18(3)
_cell_angle_gamma                107.22(3)
_cell_formula_units_Z            1
_cell_length_a                   18.335(4)
_cell_length_b                   19.458(4)
_cell_length_c                   20.980(4)
_cell_measurement_reflns_used    42483
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.203
_cell_volume                     6258(4)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_refinement  SHELXL
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49077
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.253
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    0.965
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.827
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.395
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         24835
_refine_ls_number_restraints     952
_refine_ls_restrained_S_all      1.424
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.1030
_refine_ls_shift/su_max          0.004
_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          0.3269
_refine_ls_wR_factor_ref         0.3446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18174
_reflns_number_total             24835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08303h3.cif
_cod_data_source_block           PdL4ClO4_exchange_sq
_cod_depositor_comments
'Adding full bibliography for 7127941--7127948.cif.'
_cod_original_cell_volume        6257(3)
_cod_database_code               7127946
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              19144
_shelx_hkl_checksum              83724
_shelx_fab_checksum              13022