Influence of Size, Shape, Heteroatom Content and Dispersive Contributions on Guest Binding in a Coordination Cage
Löffler, Susanne; Wuttke, Axel; Zhang, Bo; Holstein, Julian J.; Mata, Ricardo A.; Clever, Guido H.; Chem. Commun.  (2017) –; doi:10.1039/C7CC04855F

data_7120741
_publ_section_title
;
 Influence of Size, Shape, Heteroatom Content and Dispersive Contributions
 on Guest Binding in a Coordination Cage
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04855F
_journal_year                    2017
_chemical_formula_moiety
'4(C66 H54 N6 O2), C6 H12 N2, 4Pd, 3(BF4), 2Cl, I, [+ solvent]'
_chemical_formula_sum            'C270 H228 B3 Cl2 F12 I N26 O8 Pd4'
_chemical_formula_weight         4848.60
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_Hall           '-P 4a 2ac'
_space_group_name_H-M_alt        'P 4/n c c'
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-19 deposited with the CCDC.
2017-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.064(3)
_cell_length_b                   22.064(3)
_cell_length_c                   62.075(12)
_cell_measurement_reflns_used    249159
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      17.631
_cell_measurement_theta_min      0.520
_cell_volume                     30219(8)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'costum designed P11 GUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'shelXle (Huebschle, 2014)'
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT(Sheldrick, 2015)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            249159
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        17.631
_diffrn_reflns_theta_max         17.631
_diffrn_reflns_theta_min         0.520
_diffrn_source                   'P11@PETRA III, DESY, Hamburg, Germany'
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_description       plate
_exptl_crystal_F_000             9952
_exptl_crystal_recrystallization_method
'Crystallized from slow diffusion of Ethanol into a saturated solution of cage in Acetonitrile.'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.664
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.632
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         9732
_refine_ls_number_restraints     1644
_refine_ls_restrained_S_all      1.673
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0950
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3564
_refine_ls_wR_factor_ref         0.3840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6813
_reflns_number_total             9732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04855f2.cif
_cod_data_source_block           sl324a_sq
_cod_original_cell_volume        30219(10)
_cod_database_code               7120741
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.996
_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              15804
_shelx_fab_checksum              71894