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_4127576
_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            'C40 H26 N4 O4'
_chemical_formula_weight         626.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.499(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3461(2)
_cell_length_b                   8.2067(3)
_cell_length_c                   23.9093(8)
_cell_measurement_reflns_used    24133
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      80.342
_cell_measurement_theta_min      3.704
_cell_volume                     1438.74(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Venture CMOS with Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24133
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.342
_diffrn_reflns_theta_min         3.704
_diffrn_source_type              'INCOATEC microfocus sealed tube, Iys 2.0'
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       Block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 2448 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6093
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0341P)^2^+0.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                5686
_reflns_number_total             6093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02207_si_005.cif
_cod_data_source_block           bc12d
_cod_database_code               4127576
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.985
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_shelx_res_checksum              58139
_shelx_hkl_checksum              69709