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_1568307
_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            'C171.25 H142 F10.5 N12 O11.75 Pd2 S3.5'
_chemical_formula_weight         3080.47
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
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_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.
;
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_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      21.964
_cell_measurement_theta_min      0.768
_cell_volume                     15550(5)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
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_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
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'Pilatus 6M fast, High Precision 1-Axis Goniostat with sample changing robot'
_diffrn_measurement_method       '360\deg \p scan'
_diffrn_radiation_type           synchrotron
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_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
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_diffrn_reflns_limit_k_min       -44
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_diffrn_reflns_limit_l_min       -36
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_diffrn_source                   'P11@PETRA III, DESY, Hamburg, Germany'
_exptl_absorpt_coefficient_mu    0.194
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_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       plate
_exptl_crystal_F_000             6360
_exptl_crystal_recrystallization_method
'Diffusion of diisopropyl ether into saturated solution of compound in Acetonitrile.'
_exptl_crystal_size_max          0.100
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_exptl_crystal_size_min          0.010
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_refine_ls_R_factor_all          0.1155
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_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^)+(0.1810P)^2^+35.4273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2854
_refine_ls_wR_factor_ref         0.3076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27912
_reflns_number_total             37560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06629g2.cif
_cod_data_source_block           wb89o_sq
_cod_depositor_comments
'Adding full bibliography for 1568301--1568307.cif.'
_cod_original_cell_volume        15550(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C171.25 H142 F10.50 N12 O11.75 Pd2 S3.50'
_cod_database_code               1568307
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.998
_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              31097
_shelx_hkl_checksum              41568
_shelx_fab_checksum              5861