Hiding and recovering electrons in a dimetallic endohedral fullerene: air-stable products from radical additions.
Yamada, Michio; Kurihara, Hiroki; Suzuki, Mitsuaki; Saito, Masayoshi; Slanina, Zdenek; Uhlik, Filip; Aizawa, Toshihiro; Kato, Tatsuhisa; Olmstead, Marilyn M.; Balch, Alan L.; Maeda, Yutaka; Nagase, Shigeru; Lu, Xing; Akasaka, Takeshi; Journal of the American Chemical Society 137 (2015) 232–238; doi:10.1021/ja509956y

data_4123162
_publ_section_title
;
 Hiding and recovering electrons in a dimetallic endohedral fullerene:
 air-stable products from radical additions.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              232
_journal_page_last               238
_journal_paper_doi               10.1021/ja509956y
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'La2 C95 N3 H10, 1.5(CS2)'
_chemical_formula_sum            'C96.5 H10 La2 N3 S3'
_chemical_formula_weight         1585.07
_chemical_name_common            La2@D5h-C80(C3N3(C6H5)2)
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 112.174(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.242(11)
_cell_length_b                   10.988(5)
_cell_length_c                   22.219(10)
_cell_measurement_reflns_used    6539
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      4.30
_cell_volume                     5255(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1192
_diffrn_reflns_av_unetI/netI     0.1145
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46953
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         4.375
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.9156
_exptl_absorpt_correction_T_min  0.6626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_description       plate
_exptl_crystal_F_000             3088
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_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.050
_refine_diff_density_max         4.356
_refine_diff_density_min         -2.850
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1622
_refine_ls_number_reflns         11803
_refine_ls_number_restraints     5069
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.2144
_refine_ls_R_factor_gt           0.1652
_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^)+372.4605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3419
_refine_ls_wR_factor_ref         0.3680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8020
_reflns_number_total             11803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja509956y_si_003.cif
_cod_data_source_block           D5h
_cod_depositor_comments
'Adding full bibliography for 4123161--4123163.cif.'
_cod_original_formula_sum        'C96.50 H10 La2 N3 S3'
_cod_database_code               4123162
_shelx_estimated_absorpt_t_min   0.663
_shelx_estimated_absorpt_t_max   0.916
_shelxl_version_number           2014-1
_shelx_res_checksum              86423
_shelx_hkl_checksum              26705