Diuranium(IV) Carbide Cluster U<sub>2</sub>C<sub>2</sub> Stabilized Inside Fullerene Cages.
Zhuang, Jiaxin; Abella, Laura; Sergentu, Dumitru-Claudiu; Yao, Yang-Rong; Jin, Meihe; Yang, Wei; Zhang, Xingxing; Li, Xiaomeng; Zhang, Duo; Zhao, Yiming; Li, Xiaohong; Wang, Shuao; Echegoyen, Luis; Autschbach, Jochen; Chen, Ning; Journal of the American Chemical Society 141 (2019) 20249–20260; doi:10.1021/jacs.9b10247

data_4133768
_publ_section_title
;
 Diuranium(IV) Carbide Cluster U<sub>2</sub>C<sub>2</sub> Stabilized
 Inside Fullerene Cages.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20249
_journal_page_last               20260
_journal_paper_doi               10.1021/jacs.9b10247
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'C82 U1.48, C36 H44 N4 Ni0.92, 0.08(Ni), C S2, 1.5(C6 H6), 0.55(U)'
_chemical_formula_sum            'C128 H53 N4 Ni S2 U2'
_chemical_formula_weight         2245.63
_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
_audit_creation_date             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.4380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5980(5)
_cell_length_b                   16.9502(5)
_cell_length_c                   26.7945(7)
_cell_measurement_reflns_used    9529
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      32.00
_cell_measurement_theta_min      2.81
_cell_volume                     7665.8(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD MX300-HE'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82653
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            95532
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        29.730
_diffrn_reflns_theta_max         30.262
_diffrn_reflns_theta_min         1.674
_diffrn_source                   'SSRF, Beamline B17B'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.182
_exptl_absorpt_correction_T_max  0.0252
_exptl_absorpt_correction_T_min  0.0059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1628 before and 0.0802 after correction. The Ratio of minimum to maximum transmission is 0.2341. 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    1.946
_exptl_crystal_description       block
_exptl_crystal_F_000             4372
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.570
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1374
_refine_ls_number_reflns         14461
_refine_ls_number_restraints     1291
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1121P)^2^+38.2554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.1864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13292
_reflns_number_total             14461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10247_si_003.cif
_cod_data_source_block           u2c2c80
_cod_depositor_comments
'Adding full bibliography for 4133768--4133769.cif.'
_cod_database_code               4133768
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.701
_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 C81 \\sim C82 \\sim 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 \\sim Ni1 \\sim Ni2 \\sim N1P \\sim N2P \\sim N3P
\\sim N4P \\sim C1P \\sim C2P \\sim C3P \\sim C4P \\sim C5P \\sim C6P \\sim C7P
\\sim C8P \\sim C9P \\sim C10P \\sim C11P \\sim C12P \\sim C13P \\sim C14P
\\sim C15P \\sim C16P \\sim C17P \\sim C18P \\sim C19P \\sim C20P \\sim C21P
\\sim C22P \\sim C23P \\sim C24P \\sim C25P \\sim C26P \\sim C27P \\sim C28P
\\sim C29P \\sim C30P \\sim C31P \\sim C32P \\sim C33P \\sim C34P \\sim C35P
\\sim C36P \\sim S1S \\sim S2S \\sim C1S \\sim C2S \\sim C3S \\sim C4S \\sim
C5S \\sim C6S \\sim C7S \\sim C8S \\sim C9S \\sim C10S \\sim U3 \\sim U4 \\sim
U5 \\sim U6 \\sim U7 \\sim U8 \\sim U9 \\sim U10 \\sim U11 \\sim U12 \\sim U13
\\sim U14: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
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 0.04 and sigma for terminal atoms of 0.08
3. Others
 1*[Sof(U3)]+1*[Sof(U13)]+1*[Sof(U11)]+1*[Sof(U4)]+1*[Sof(U5)]+1*[Sof(U6)]+1*
 [Sof(U7)]+1*[Sof(U8)]+1*[Sof(U9)]+1*[Sof(U10)]+1*[Sof(U14)]+1*[Sof(U12)]+1*
 [Sof(U1)]+1*[Sof(U2)]=0.0001 with esd of 2
 Sof(Ni2)=1-FVAR(1)
 Sof(Ni1)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5P(H5PA,H5PB), C8P(H8PA,H8PB), C14P(H14A,H14B), C17P(H17A,H17B), C23P(H23A,
 H23B), C26P(H26A,H26B), C32P(H32A,H32B), C35P(H35A,H35B)
4.b Aromatic/amide H refined with riding coordinates:
 C2P(H2P), C11P(H11P), C20P(H20P), C29P(H29P), 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:
 C6P(H6PA,H6PB,H6PC), C9P(H9PA,H9PB,H9PC), C15P(H15A,H15B,H15C), C18P(H18A,
 H18B,H18C), C24P(H24A,H24B,H24C), C27P(H27A,H27B,H27C), C33P(H33A,H33B,H33C),
 C36P(H36A,H36B,H36C)
;
_shelx_res_checksum              63512
_shelx_hkl_checksum              23572
_olex2_submission_special_instructions 'No special instructions were received'