U2@Ih(7)-C80: Crystallographic characterization of a long-sought dimetallic actinide endohedral fullerene.
Zhang, Xingxing; Wang, Yaofeng; Morales-Martínez, Roser; Zhong, Jun; de Graaf, Coen; Rodríguez-Fortea, Antonio; Poblet, Josep M.; Echegoyen, Luis; Feng, Lai; Chen, Ning; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b10865

data_4127171
_publ_section_title
;
 U2@Ih(7)-C80: Crystallographic characterization of a long-sought
 dimetallic actinide endohedral fullerene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10865
_journal_year                    2018
_chemical_formula_moiety         'U2 C80, Ni N4 C36 H44, 1.0(CHCl3)'
_chemical_formula_sum            'C117 H46 Cl5 N4 Ni U2'
_chemical_formula_weight         2219.60
_chemical_name_common            U2@C80/NiOEP/CHCl3
_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'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.492(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1208(9)
_cell_length_b                   15.5044(6)
_cell_length_c                   19.5147(6)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.23
_cell_measurement_theta_min      3.35
_cell_volume                     7565.8(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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0684
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57816
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.641
_diffrn_reflns_theta_min         3.354
_exptl_absorpt_coefficient_mu    14.338
_exptl_absorpt_correction_T_max  0.211
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_description       block
_exptl_crystal_F_000             4292
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         1.653
_refine_diff_density_min         -2.353
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.576
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1032
_refine_ls_number_reflns         8027
_refine_ls_number_restraints     1232
_refine_ls_restrained_S_all      1.699
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.1169
_refine_ls_shift/su_max          0.005
_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          0.3419
_refine_ls_wR_factor_ref         0.3706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6060
_reflns_number_total             8027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10865_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4127171
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.4714
_shelx_estimated_absorpt_t_max   0.7531
_iucr_refine_squeeze_details
;
TITL t_a.res in C2/m
CELL   25.1208   15.5044   19.5147     90.00     95.49     90.00
SPGR C2/m
Q101 0.523 0.498 0.422 !       4.87 eA-3
C102 0.435 0.124 0.986 !       3.10 eA-3
C103 1.000 0.364 0.095 !       2.75 eA-3
C104 1.000 0.250-0.004 !       2.25 eA-3
C105 1.000 0.312 0.004 !       1.25 eA-3
Q106 0.897 0.139 0.720 !       1.12 eA-3
Q107 0.297 0.353 0.638 !       1.06 eA-3
Q108 0.211 0.270 0.184 !       1.04 eA-3
Q109 0.180 0.363 0.904 !       1.02 eA-3
Q110 0.890 0.217 0.825 !       0.89 eA-3
C111 0.998 0.389 0.027 !       0.86 eA-3
Q112 0.793 0.498 0.844 !       0.81 eA-3
Q113 0.189 0.291 0.783 !       0.78 eA-3
Q114 0.828 0.212 0.925 !       0.77 eA-3
C115 0.993 0.450 0.932 !       0.72 eA-3
Q116 0.322 0.476 0.909 !       0.72 eA-3
Q117 0.436 0.499 0.734 !       0.71 eA-3
Q118 0.785 0.509 0.188 !       0.68 eA-3
Q119 0.748 0.506 0.688 !       0.67 eA-3
Q120 0.764 0.280 0.298 !       0.66 eA-3
Q121 0.674 0.505 0.703 !       0.64 eA-3
Q122 0.273 0.357 0.987 !       0.61 eA-3
Q123 0.601 0.074 0.062 !       0.60 eA-3
Q124 0.360 0.506 0.625 !       0.57 eA-3
Q125 0.203 0.507 0.984 !       0.57 eA-3
Q126 0.477 0.500 0.422 !       0.57 eA-3
Q127 0.180 0.495 0.219 !       0.56 eA-3
Q128 0.501 0.492 0.531 !       0.56 eA-3
Q129 0.452 0.350 0.966 !       0.55 eA-3
Q130 0.876 0.359 0.345 !       0.55 eA-3
Q131 0.142 0.507 0.703 !       0.54 eA-3
Q132 0.555 0.425 0.170 !       0.53 eA-3
C133 1.000 0.499 0.001 !       0.53 eA-3
Q134 0.367 0.072 0.224 !       0.53 eA-3
Q135 0.249 0.284 0.905 !       0.52 eA-3
Q136 0.878 0.500 0.545 !       0.51 eA-3
Q137 0.212 0.039 0.132 !       0.51 eA-3
Q138 0.572 0.502 0.078 !       0.50 eA-3
;
_shelx_res_checksum              5259
_shelx_hkl_checksum              60813
_shelx_fab_checksum              90628