U<sub>2</sub>N@<i>I</i> <sub>h</sub>(7)-C<sub>80</sub>: fullerene cage encapsulating an unsymmetrical U(iv)[double bond, length as m-dash]N[double bond, length as m-dash]U(v) cluster.
Li, Xiaomeng; Roselló, Yannick; Yao, Yang-Rong; Zhuang, Jiaxin; Zhang, Xingxing; Rodríguez-Fortea, Antonio; de Graaf, Coen; Echegoyen, Luis; Poblet, Josep M.; Chen, Ning; Chemical science 12 (2020) 282–292; doi:10.1039/d0sc04677a

data_1559998
_publ_section_title
;
 U<sub>2</sub>N@<i>I</i> <sub>h</sub>(7)-C<sub>80</sub>: fullerene cage
 encapsulating an unsymmetrical U(iv)[double bond, length as
 m-dash]N[double bond, length as m-dash]U(v) cluster.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              282
_journal_page_last               292
_journal_paper_doi               10.1039/d0sc04677a
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C80 N U2, C36 H44 N4 Ni, C S2, 3(C3 H3)'
_chemical_formula_sum            'C126 H53 N5 Ni S2 U2'
_chemical_formula_weight         2235.62
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-10-15 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.76
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6663(2)
_cell_length_b                   16.9578(2)
_cell_length_c                   26.7308(3)
_cell_measurement_reflns_used    9675
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.97
_cell_measurement_theta_min      2.63
_cell_volume                     7667.88(15)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker MX300-HE CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77484
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            102345
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        27.704
_diffrn_reflns_theta_max         28.574
_diffrn_reflns_theta_min         1.570
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.575
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0980 before and 0.0602 after correction. The Ratio of minimum to maximum transmission is 0.5858. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_description       block
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.688
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1305
_refine_ls_number_reflns         14315
_refine_ls_number_restraints     888
_refine_ls_restrained_S_all      1.456
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0472P)^2^+46.0519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13730
_reflns_number_total             14315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04677a2.cif
_cod_data_source_block           u2nc80
_cod_depositor_comments          'Adding full bibliography for 1559998.cif.'
_cod_original_cell_volume        7667.84(15)
_cod_database_code               1559998
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.654
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
U1 \\sim U2 \\sim U3 \\sim U4 \\sim U5 \\sim U6 \\sim N1 \\sim U7 \\sim U8
\\sim U9 \\sim U10: within 2A with sigma of 0.001 and sigma for terminal atoms
of 0.002
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within
2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(U3) \\sim Ueq, Uanis(U4) \\sim Ueq, Uanis(U5) \\sim Ueq, Uanis(U6) \\sim
Ueq, Uanis(U7) \\sim Ueq, Uanis(U8) \\sim Ueq, Uanis(U9) \\sim Ueq, Uanis(U10)
\\sim Ueq, Uanis(Ni1N) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(U1) \\sim Ueq, Uanis(U2) \\sim Ueq: with sigma of 0.0003 and sigma for
terminal atoms of 0.0006
3. Others
 Fixed Sof: U1(0.86) U2(0.86) U3(0.05) U4(0.05) U5(0.03) U6(0.03) U7(0.05)
 U8(0.05) U9(0.01) U10(0.01)
4.a Secondary CH2 refined with riding coordinates:
 C21N(H21A,H21B), C23N(H23A,H23B), C25N(H25A,H25B), C27N(H27A,H27B), C29N(H29A,
 H29B), C31N(H31A,H31B), C33N(H33A,H33B), C35N(H35A,H35B)
4.b Aromatic/amide H refined with riding coordinates:
 C2N(H2N), C7N(H7N), C12N(H12N), C17N(H17N), C2S(H2S), C3S(H3S), C4S(H4S),
 C5S(H5S), C6S(H6S), C7S(H7S), C8S(H8S), C9S(H9S), C10S(H10S)
4.c Idealised Me refined as rotating group:
 C22N(H22A,H22B,H22C), C24N(H24A,H24B,H24C), C26N(H26A,H26B,H26C), C28N(H28A,
 H28B,H28C), C30N(H30A,H30B,H30C), C32N(H32A,H32B,H32C), C34N(H34A,H34B,H34C),
 C36N(H36A,H36B,H36C)
;
_shelx_res_checksum              96008
_olex2_submission_special_instructions 'No special instructions were received'