Pd(II) Coordination Sphere Engineering: Pyridine Cages, Quinoline Bowls, and Heteroleptic Pills Binding One or Two Fullerenes.
Chen, Bin; Holstein, Julian J.; Horiuchi, Shinnosuke; Hiller, Wolf G.; Clever, Guido H.; Journal of the American Chemical Society 141 (2019) 8907–8913; doi:10.1021/jacs.9b02207

data_4127573
_publ_section_title
;
 Pd(II) Coordination Sphere Engineering: Pyridine Cages, Quinoline Bowls,
 and Heteroleptic Pills Binding One or Two Fullerenes.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8907
_journal_page_last               8913
_journal_paper_doi               10.1021/jacs.9b02207
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C160 H104 B4 F16 N16 O16 Pd2'
_chemical_formula_weight         3066.63
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.27(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.884(3)
_cell_length_b                   19.386(4)
_cell_length_c                   32.974(7)
_cell_measurement_reflns_used    102108
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      22.790
_cell_measurement_theta_min      1.189
_cell_volume                     10505(4)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'costum designed P11 GUI'
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_computing_molecular_graphics    'shelXle (Huebschle, 2014)'
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_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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     0.6888
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
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_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            102108
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        22.790
_diffrn_reflns_theta_max         22.790
_diffrn_reflns_theta_min         1.189
_diffrn_source                   'P11@PETRA III, DESY, Hamburg, Germany'
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.970
_exptl_crystal_description       plate
_exptl_crystal_F_000             3120
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_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.005
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         15328
_refine_ls_number_restraints     2208
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0791
_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          0.2484
_refine_ls_wR_factor_ref         0.2696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10671
_reflns_number_total             15328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02207_si_004.cif
_cod_data_source_block           bc11c_sq
_cod_database_code               4127573
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.999
_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              12067
_shelx_hkl_checksum              6600
_shelx_fab_checksum              86506