Unique Four-Electron Metal-to-Cage Charge Transfer of Th to a C<sub>82</sub> Fullerene Cage: Complete Structural Characterization of Th@C<sub>3v</sub>(8)-C<sub>82</sub>.
Wang, Yaofeng; Morales-Martínez, Roser; Zhang, Xingxing; Yang, Wei; Wang, Yaxing; Rodríguez-Fortea, Antonio; Poblet, Josep M.; Feng, Lai; Wang, Shuao; Chen, Ning; Journal of the American Chemical Society 139 (2017) 5110–5116; doi:10.1021/jacs.6b13383

data_4131223
_publ_section_title
;
 Unique Four-Electron Metal-to-Cage Charge Transfer of Th to a
 C<sub>82</sub> Fullerene Cage: Complete Structural Characterization of
 Th@C<sub>3v</sub>(8)-C<sub>82</sub>.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5110
_journal_page_last               5116
_journal_paper_doi               10.1021/jacs.6b13383
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'Th C82, Ni N4 C36 H44, 1.5(bz), 1.0(CS2)'
_chemical_formula_sum            'C128 H53 I0 N4 Ni O0 S2 Th'
_chemical_formula_weight         2001.61
_chemical_name_common            Th@C82/NiOEP/1.5bz/CS2
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 106.7590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1225(6)
_cell_length_b                   17.0996(5)
_cell_length_c                   17.6908(4)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.50
_cell_measurement_theta_min      5.22
_cell_volume                     7856.2(3)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31154
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.373
_diffrn_reflns_theta_min         3.094
_exptl_absorpt_coefficient_mu    7.379
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5977
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       block
_exptl_crystal_F_000             3996
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.247
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.00033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         7452
_refine_ls_number_restraints     943
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0739P)^2^+17.7140P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6897
_reflns_number_total             7452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b13383_si_002.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4131223
_shelx_estimated_absorpt_t_min   0.320
_shelx_estimated_absorpt_t_max   0.320
_shelxl_version_number           2013-2
_shelx_res_checksum              6486
_shelx_hkl_checksum              43009