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_1568304
_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            'C160 H124 N13 O11 Pd2 Re2'
_chemical_formula_weight         2989.91
_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.
;
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   30.0723(9)
_cell_length_c                   29.2855(18)
_cell_measurement_reflns_used    133584
_cell_measurement_temperature    100(2)
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_computing_structure_solution
'SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0560
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -38
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_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            133584
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.816
_diffrn_reflns_theta_min         1.391
_exptl_absorpt_coefficient_mu    2.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             12040
_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          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.369
_refine_diff_density_min         -4.030
_refine_diff_density_rms         0.195
_refine_ls_abs_structure_details
;
 Flack x determined using 9362 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1741
_refine_ls_number_reflns         27659
_refine_ls_number_restraints     3570
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.1069
_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^)+(0.1982P)^2^+126.6828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3030
_refine_ls_wR_factor_ref         0.3144
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                23651
_reflns_number_total             27659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06629g2.cif
_cod_data_source_block           sol2_a_sq
_cod_depositor_comments
'Adding full bibliography for 1568301--1568307.cif.'
_cod_database_code               1568304
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.674
_diffrn_measurement_detector     'CCD Plate'
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_computing_ligand_restraints
'Grade Web Server, http.//grade.globalphasing.org'
_shelx_res_checksum              12318
_shelx_hkl_checksum              20412
_shelx_fab_checksum              80634