Redox-induced reversible metal assembly through translocation and reversible ligand coupling in tetranuclear metal sandwich frameworks.
Murahashi, Tetsuro; Shirato, Katsunori; Fukushima, Azusa; Takase, Kohei; Suenobu, Tomoyoshi; Fukuzumi, Shunichi; Ogoshi, Sensuke; Kurosawa, Hideo; Nature chemistry 4 (2012) 52–58; doi:10.1038/nchem.1202

data_1508166
_publ_section_title
;
 Redox-induced reversible metal assembly through translocation and
 reversible ligand coupling in tetranuclear metal sandwich frameworks.
;
_journal_issue                   1
_journal_name_full               'Nature chemistry'
_journal_page_first              52
_journal_page_last               58
_journal_paper_doi               10.1038/nchem.1202
_journal_volume                  4
_journal_year                    2012
_chemical_formula_moiety         'C120 H76 B2 F48 O4 Pd4'
_chemical_formula_sum            'C120 H76 B2 F48 O4 Pd4'
_chemical_formula_weight         2941.06
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.2296(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   28.2551(5)
_cell_length_b                   19.2999(4)
_cell_length_c                   21.1845(4)
_cell_measurement_reflns_used    57410
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.10
_cell_volume                     11460.5(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0480
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89495
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            deep
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5816.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.940
_refine_diff_density_min         -1.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     840
_refine_ls_number_reflns         9607
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    5.9964    4.1271    4.8701
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                9607
_reflns_number_total             13092
_reflns_threshold_expression     F>3.0\s(F)
_cod_data_source_file            nchem.1202-s2.cif
_cod_data_source_block           fukushima5
_cod_database_code               1508166