A Metallo-molecular Cage That Can Close the Apertures with Coordination Bonds.
Akine, Shigehisa; Miyashita, Masato; Nabeshima, Tatsuya; Journal of the American Chemical Society 139 (2017) 4631–4634; doi:10.1021/jacs.7b00840

data_4126149
_publ_section_title
;
 A Metallo-molecular Cage That Can Close the Apertures with Coordination
 Bonds.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4631
_journal_page_last               4634
_journal_paper_doi               10.1021/jacs.7b00840
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         C217.50H196B3Co3F72N12O15.50
_chemical_formula_sum            'C217.5 H196 B3 Co3 F72 N12 O15.5'
_chemical_formula_weight         4803.08
_chemical_name_common            '[LCo3(C6H16N2)3]_3TFPB_2H2O_1.5MeOH'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.8030(10)
_cell_angle_beta                 82.6610(10)
_cell_angle_gamma                74.2470(10)
_cell_formula_units_Z            2
_cell_length_a                   19.2543(4)
_cell_length_b                   20.7309(4)
_cell_length_c                   29.5488(6)
_cell_measurement_reflns_used    81717
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      1.02
_cell_volume                     11249.5(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2009)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer confocal mirror'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            81717
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         1.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.9049
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4906
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3537
_refine_ls_number_reflns         50235
_refine_ls_number_restraints     1094
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+23.6731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.2166
_reflns_number_gt                27484
_reflns_number_total             50235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b00840_si_002.cif
_cod_data_source_block           miy068
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C217.50 H196 B3 Co3 F72 N12 O15.50'
_cod_database_code               4126149