London dispersion driven compaction of coordination cages in the gas-phase - a combined ion mobility and theoretical study.
Drechsler, Christoph; Baksi, Ananya; Platzek, André; Acar, Mert; Holstein, Julian J.; Stein, Christopher J.; Clever, Guido H.; Chemical science 15 (2024) 19264–19272; doi:10.1039/d4sc04786a

data_1572872
_publ_section_title
;
 London dispersion driven compaction of coordination cages in the
 gas-phase - a combined ion mobility and theoretical study.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              19264
_journal_page_last               19272
_journal_paper_doi               10.1039/d4sc04786a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C168 H92 B3.5 F14 N12 Pd2'
_chemical_formula_weight         2795.17
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif by Daniel Kratzert, Freiburg 2019,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2023-03-31 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.151(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.58(3)
_cell_length_b                   37.13(3)
_cell_length_c                   38.88(4)
_cell_measurement_reflns_used    144173
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.650
_cell_measurement_theta_min      0.961
_cell_volume                     35644(6)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'costum designed P11 GUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
;
Eiger 2X 16M, High Precision 1-Axis Goniostat with Sta\"ubli sample changing
robot
;
_diffrn_measurement_method       '360\deg \p scan'
_diffrn_radiation_monochromator
'double crystal monochromator (Si-111 and Si-113 reflections)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            144173
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        21.650
_diffrn_reflns_theta_max         21.650
_diffrn_reflns_theta_min         0.961
_diffrn_source                   'P11@PETRA III, DESY, Hamburg, Germany'
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_description       plate
_exptl_crystal_F_000             11356
_exptl_crystal_recrystallization_method
'Slow vapour diffusion of 3ml Di-isopropylether into solution 150 yl of 0.2 mM solution of compound in Nitromethan for two weeks.'
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.456
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.678
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3592
_refine_ls_number_reflns         21294
_refine_ls_number_restraints     8052
_refine_ls_restrained_S_all      1.475
_refine_ls_R_factor_all          0.1964
_refine_ls_R_factor_gt           0.1520
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4177
_refine_ls_wR_factor_ref         0.4491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11487
_reflns_number_total             21294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04786a2.cif
_cod_data_source_block           cd248d_sq
_cod_depositor_comments          'Adding full bibliography for 1572872.cif.'
_cod_original_cell_volume        35649(58)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C168 H92 B3.50 F14 N12 Pd2'
_cod_database_code               1572872
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              43754
_shelx_hkl_checksum              28357
_shelx_fab_checksum              34108