Synthesis and Characterization of Non-Isolated-Pentagon-Rule Actinide Endohedral Metallofullerenes U@ C<sub>1</sub>(17418)-C<sub>76</sub>, U@ C<sub>1</sub>(28324)-C<sub>80</sub>, and Th@ C<sub>1</sub>(28324)-C<sub>80</sub>: Low-Symmetry Cage Selection Directed by a Tetravalent Ion.
Cai, Wenting; Abella, Laura; Zhuang, Jiaxin; Zhang, Xingxing; Feng, Lai; Wang, Yaofeng; Morales-Martínez, Roser; Esper, Ronda; Boero, Mauro; Metta-Magaña, Alejandro; Rodríguez-Fortea, Antonio; Poblet, Josep M.; Echegoyen, Luis; Chen, Ning; Journal of the American Chemical Society 140 (2018) 18039–18050; doi:10.1021/jacs.8b10435

data_4133504
_publ_section_title
;
 Synthesis and Characterization of Non-Isolated-Pentagon-Rule Actinide
 Endohedral Metallofullerenes U@ C<sub>1</sub>(17418)-C<sub>76</sub>, U@
 C<sub>1</sub>(28324)-C<sub>80</sub>, and Th@
 C<sub>1</sub>(28324)-C<sub>80</sub>: Low-Symmetry Cage Selection Directed
 by a Tetravalent Ion.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18039
_journal_page_last               18050
_journal_paper_doi               10.1021/jacs.8b10435
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'Th C80, Ni N4 C36 H44, C12Hl2'
_chemical_formula_sum            'C128 H56 N4 Ni Th'
_chemical_formula_weight         1940.51
_chemical_name_common            Th@C80/NiOEP/2(C6H6)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 120.3020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.4289(8)
_cell_length_b                   15.0655(3)
_cell_length_c                   25.2663(4)
_cell_measurement_reflns_used    7158
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.12
_cell_measurement_theta_min      28.45
_cell_volume                     14930.0(5)
_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-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            86356
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.479
_diffrn_reflns_theta_min         2.253
_exptl_absorpt_coefficient_mu    7.234
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       block
_exptl_crystal_F_000             7760
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.6401
_refine_diff_density_max         2.506
_refine_diff_density_min         -2.412
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         13701
_refine_ls_number_restraints     1149
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0967
_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^)+(0.1706P)^2^+206.5160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2672
_refine_ls_wR_factor_ref         0.2743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12504
_reflns_number_total             13701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10435_si_004.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        14929.9(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4133504
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              77403
_shelx_hkl_checksum              38977