Three-Dimensional Sandwich Nanocubes Composed of 13-Atom Palladium Core and Hexakis-Carbocycle Shell.
Teramoto, Masahiro; Iwata, Kosuke; Yamaura, Hiroshige; Kurashima, Kenta; Miyazawa, Koshi; Kurashige, Yuki; Yamamoto, Koji; Murahashi, Tetsuro; Journal of the American Chemical Society 140 (2018) 12682–12686; doi:10.1021/jacs.8b07430

data_4132929
_publ_section_title
;
 Three-Dimensional Sandwich Nanocubes Composed of 13-Atom Palladium Core
 and Hexakis-Carbocycle Shell.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12682
_journal_page_last               12686
_journal_paper_doi               10.1021/jacs.8b07430
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C140 H82 B3 Cl4 F72 Pd13'
_chemical_formula_sum            'C140 H82 B3 Cl4 F72 Pd13'
_chemical_formula_weight         4689.51
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.6402(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   23.2475(4)
_cell_length_b                   22.7475(4)
_cell_length_c                   28.3112(5)
_cell_measurement_reflns_used    131584
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.02
_cell_volume                     14965.5(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            209615
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.015
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.732
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9004.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.37
_refine_diff_density_min         -1.90
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     2068
_refine_ls_number_reflns         34178
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0612P)^2^+43.0711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25374
_reflns_number_total             34178
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8b07430_si_003.cif
_cod_data_source_block           KI-287-retry_
_cod_database_code               4132929
_shelx_res_checksum              90858
_shelx_hkl_checksum              13941
_shelx_fab_checksum              36248