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_1568305
_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            'C169 H145 F24 N12 O1.5 Pd2 Sb4'
_chemical_formula_weight         3523.76
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 97.42(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.378(5)
_cell_length_b                   25.420(5)
_cell_length_c                   29.183(6)
_cell_measurement_reflns_used    265657
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      21.973
_cell_measurement_theta_min      0.845
_cell_volume                     16462(6)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'costum designed P11 GUI'
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_computing_structure_solution    'SHELXT(Sheldrick, 2015)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Pilatus 6M fast, High Precision 1-Axis Goniostat with sample changing robot'
_diffrn_measurement_method       '360\deg \p scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.5636
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
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_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            265657
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_max         21.973
_diffrn_reflns_theta_min         0.845
_diffrn_source                   'P11@PETRA III, DESY, Hamburg, Germany'
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       plate
_exptl_crystal_F_000             7068
_exptl_crystal_recrystallization_method
'Diffusion of diisopropyl ether into saturated solution of compound in Acetonitrile.'
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
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_refine_ls_number_reflns         40225
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_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0721
_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^)+(0.1399P)^2^+23.4041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2193
_refine_ls_wR_factor_ref         0.2326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31176
_reflns_number_total             40225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06629g2.cif
_cod_data_source_block           wb89s_sq
_cod_depositor_comments
'Adding full bibliography for 1568301--1568307.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C169 H145 F24 N12 O1.50 Pd2 Sb4'
_cod_database_code               1568305
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.985
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_computing_ligand_restraints
'Grade Web Server, http.//grade.globalphasing.org'
_computing_molecular_model       'DSR (Kratzert, 2015)'
_shelx_res_checksum              3115
_shelx_hkl_checksum              4584
_shelx_fab_checksum              13612