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_4133503
_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_sum            'C113 H45 Cl3 I0 N4 Ni S0 U'
_chemical_formula_weight         1861.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.390(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.686(5)
_cell_length_b                   15.184(4)
_cell_length_c                   25.496(6)
_cell_measurement_reflns_used    5492
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.004
_cell_measurement_theta_min      5.321
_cell_volume                     7232(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.1259
_diffrn_reflns_Laue_measured_fraction_full 0.889
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19995
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         1.561
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.086
_exptl_transmission_factor_max   0.745685
_exptl_transmission_factor_min   0.449777
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1841
_refine_ls_number_reflns         11652
_refine_ls_number_restraints     11320
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.1754
_refine_ls_R_factor_gt           0.1236
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3435
_refine_ls_wR_factor_ref         0.3750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6682
_reflns_number_total             11652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10435_si_002.cif
_cod_data_source_block           monotwin4S_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4133503
_shelx_estimated_absorpt_t_min   0.357
_shelx_estimated_absorpt_t_max   0.803
_shelxl_version_number           2013-2
_shelx_res_checksum              8788
_shelx_hkl_checksum              72801
_shelx_fab_checksum              64480