Maximized axial helicity in a Pd<sub>2</sub>L<sub>4</sub> cage: inverse guest size-dependent compression and mesocate isomerism.
Bloch, Witold M.; Horiuchi, Shinnosuke; Holstein, Julian J.; Drechsler, Christoph; Wuttke, Axel; Hiller, Wolf; Mata, Ricardo A.; Clever, Guido H.; Chemical science 14 (2023) 1524–1531; doi:10.1039/d2sc06629g

data_1568302
_publ_section_title
;
 Maximized axial helicity in a Pd<sub>2</sub>L<sub>4</sub> cage: inverse
 guest size-dependent compression and mesocate isomerism.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              1524
_journal_page_last               1531
_journal_paper_doi               10.1039/d2sc06629g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_sum            'C161 H124.5 Cl2.5 N13.5 O13 Pd2'
_chemical_formula_weight         2757.66
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           106
_space_group_name_Hall           'P 4c -2ab'
_space_group_name_H-M_alt        'P 42 b c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-22 deposited with the CCDC.	2023-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.020(4)
_cell_length_b                   30.020(4)
_cell_length_c                   29.369(6)
_cell_measurement_reflns_used    108011
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.564
_cell_measurement_theta_min      2.081
_cell_volume                     26467(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'shelXle (Huebschle, 2014)'
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
_computing_structure_refinement  'SHELXL-2016/5 (Sheldrick, 2016)'
_computing_structure_solution
'SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture CMOS with Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            108011
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        44.564
_diffrn_reflns_theta_max         44.564
_diffrn_reflns_theta_min         2.081
_diffrn_source                   'INCOATEC microfocus sealed tube, Iys 2.0'
_exptl_absorpt_coefficient_mu    3.229
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_correction_T_min  0.5438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       plate
_exptl_crystal_F_000             11388
_exptl_crystal_recrystallization_method
'Diffusion of diisopropyl ether into saturated solution of compound in Acetonitrile.'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 4102 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1877
_refine_ls_number_reflns         10378
_refine_ls_number_restraints     2348
_refine_ls_restrained_S_all      1.676
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0891
_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^)+(0.1715P)^2^+151.5785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2449
_refine_ls_wR_factor_ref         0.2527
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9531
_reflns_number_total             10378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06629g2.cif
_cod_data_source_block           sola_a
_cod_depositor_comments
'Adding full bibliography for 1568301--1568307.cif.'
_cod_original_cell_volume        26467(9)
_cod_original_formula_sum        'C161 H124.50 Cl2.50 N13.50 O13 Pd2'
_cod_database_code               1568302
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.564
_shelx_estimated_absorpt_t_max   0.738
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_computing_ligand_restraints
'Grade Web Server, http.//grade.globalphasing.org'
_shelx_res_checksum              85288
_shelx_hkl_checksum              80418