Synthesis and characterization of carbene derivatives of Th@<i>C</i> <sub>3v</sub>(8)-C<sub>82</sub> and U@<i>C</i> <sub>2v</sub>(9)-C<sub>82</sub>: exceptional chemical properties induced by strong actinide-carbon cage interaction.
Liu, Xinye; Li, Bo; Yang, Wei; Yao, Yang-Rong; Yang, Le; Zhuang, Jiaxin; Li, Xiaomeng; Jin, Peng; Chen, Ning; Chemical science 12 (2020) 2488–2497; doi:10.1039/d0sc06111e

data_1559846
_publ_section_title
;
 Synthesis and characterization of carbene derivatives of Th@<i>C</i>
 <sub>3v</sub>(8)-C<sub>82</sub> and U@<i>C</i>
 <sub>2v</sub>(9)-C<sub>82</sub>: exceptional chemical properties induced
 by strong actinide-carbon cage interaction.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              2488
_journal_page_last               2497
_journal_paper_doi               10.1039/d0sc06111e
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C92 H14 U, C S2'
_chemical_formula_sum            'C93 H14 S2 U'
_chemical_formula_weight         1433.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-09-14 deposited with the CCDC.	2020-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.257(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3037(7)
_cell_length_b                   21.8879(12)
_cell_length_c                   20.9098(13)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.68
_cell_measurement_theta_min      2.95
_cell_volume                     5073.9(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      119.99
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.982
_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  0.0817
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44485
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.533
_diffrn_reflns_theta_min         2.953
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.273
_exptl_absorpt_correction_T_max  0.440
_exptl_absorpt_correction_T_min  0.262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_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    1.876
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.689
_refine_diff_density_min         -2.502
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         9866
_refine_ls_number_restraints     1216
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0957
_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^)+(0.1489P)^2^+190.0238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2438
_refine_ls_wR_factor_ref         0.2823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7199
_reflns_number_total             9866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06111e2.cif
_cod_data_source_block           UC82Ad
_cod_depositor_comments
;Adding full bibliography for 1559845--1559846.cif.

 Adding full bibliography for 1559845--1559846.cif.
;
_cod_database_code               1559846
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.494
_shelx_estimated_absorpt_t_min   0.308
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C48-C49 = C66-C65 = C72-C71 = C54-C55
 1.38 with sigma of 0.01
 C43-C42 \\sim C42-C66 \\sim C66-C45 \\sim C45-C44 \\sim C44-C43
 with sigma of 0.02
 C43-C66 \\sim C43-C45 \\sim C42-C45 \\sim C42-C44 \\sim C66-C44
 with sigma of 0.02
 C65-C64 \\sim C64-C79 \\sim C79-C80 \\sim C80-C67 \\sim C67-C65
 with sigma of 0.02
 C65-C79 \\sim C65-C80 \\sim C64-C80 \\sim C64-C67 \\sim C79-C67
 with sigma of 0.02
 C53-C72 \\sim C72-C73 \\sim C73-C74 \\sim C74-C54 \\sim C54-C53
 with sigma of 0.02
 C53-C73 \\sim C53-C74 \\sim C72-C74 \\sim C72-C54 \\sim C73-C54
 with sigma of 0.02
 C31-C55 \\sim C55-C56 \\sim C56-C33 \\sim C33-C32 \\sim C32-C31
 with sigma of 0.02
 C31-C56 \\sim C31-C33 \\sim C55-C33 \\sim C55-C32 \\sim C56-C32
 with sigma of 0.02
 C10-C9 \\sim C9-C28 \\sim C28-C29 \\sim C29-C11 \\sim C11-C10
 with sigma of 0.02
 C10-C28 \\sim C10-C29 \\sim C9-C29 \\sim C9-C11 \\sim C28-C11
 with sigma of 0.02
 C6-C5 \\sim C5-C21 \\sim C21-C22 \\sim C22-C7 \\sim C7-C6
 with sigma of 0.02
 C6-C21 \\sim C6-C22 \\sim C5-C22 \\sim C5-C7 \\sim C21-C7
 with sigma of 0.02
 C17-C39 \\sim C39-C40 \\sim C40-C19 \\sim C19-C18 \\sim C18-C17
 with sigma of 0.02
 C17-C40 \\sim C17-C19 \\sim C39-C19 \\sim C39-C18 \\sim C40-C18
 with sigma of 0.02
 C58-C59 \\sim C59-C37 \\sim C37-C36 \\sim C36-C35 \\sim C35-C58
 with sigma of 0.02
 C58-C37 \\sim C58-C36 \\sim C59-C36 \\sim C59-C35 \\sim C37-C35
 with sigma of 0.02
 C77-C78 \\sim C78-C61 \\sim C61-C60 \\sim C60-C76 \\sim C76-C77
 with sigma of 0.02
 C77-C61 \\sim C77-C60 \\sim C78-C60 \\sim C78-C76 \\sim C61-C76
 with sigma of 0.02
 C49-C69 \\sim C69-C70 \\sim C70-C71 \\sim C71-C50 \\sim C50-C49
 with sigma of 0.02
 C49-C70 \\sim C49-C71 \\sim C69-C71 \\sim C69-C50 \\sim C70-C50
 with sigma of 0.02
 C25-C24 \\sim C24-C47 \\sim C47-C48 \\sim C48-C26 \\sim C26-C25
 with sigma of 0.02
 C25-C47 \\sim C25-C48 \\sim C24-C48 \\sim C24-C26 \\sim C47-C26
 with sigma of 0.02
 C23-C22 \\sim C23-C24 \\sim C23-C44
 with sigma of 0.02
 C22-C24 \\sim C24-C44 \\sim C44-C22
 with sigma of 0.02
 C27-C26 \\sim C27-C28 \\sim C27-C51
 with sigma of 0.02
 C26-C28 \\sim C28-C51 \\sim C51-C26
 with sigma of 0.02
 C30-C29 \\sim C30-C31 \\sim C30-C52
 with sigma of 0.02
 C29-C31 \\sim C31-C52 \\sim C52-C29
 with sigma of 0.02
 C34-C33 \\sim C34-C35 \\sim C34-C14
 with sigma of 0.02
 C33-C35 \\sim C35-C14 \\sim C14-C33
 with sigma of 0.02
 C38-C37 \\sim C38-C39 \\sim C38-C62
 with sigma of 0.02
 C37-C39 \\sim C39-C62 \\sim C62-C37
 with sigma of 0.02
 C41-C40 \\sim C41-C42 \\sim C41-C63
 with sigma of 0.02
 C40-C42 \\sim C42-C63 \\sim C63-C40
 with sigma of 0.02
 C46-C45 \\sim C46-C47 \\sim C46-C68
 with sigma of 0.02
 C45-C47 \\sim C47-C68 \\sim C68-C45
 with sigma of 0.02
 C48-C50 \\sim C48-C69 \\sim C49-C47 \\sim C49-C26
 with sigma of 0.02
 C51-C50 \\sim C51-C27 \\sim C51-C52
 with sigma of 0.02
 C50-C52 \\sim C52-C27 \\sim C27-C50
 with sigma of 0.02
 C52-C51 \\sim C52-C53 \\sim C52-C30
 with sigma of 0.02
 C51-C53 \\sim C53-C30 \\sim C30-C51
 with sigma of 0.02
 C54-C56 \\sim C54-C31 \\sim C55-C53 \\sim C55-C74
 with sigma of 0.02
 C57-C56 \\sim C57-C58 \\sim C57-C75
 with sigma of 0.02
 C56-C58 \\sim C58-C75 \\sim C75-C56
 with sigma of 0.02
 C59-C61 \\sim C59-C76 \\sim C60-C58 \\sim C60-C37
 with sigma of 0.02
 C62-C61 \\sim C62-C63 \\sim C62-C38
 with sigma of 0.02
 C61-C63 \\sim C63-C38 \\sim C38-C61
 with sigma of 0.02
 C63-C62 \\sim C63-C64 \\sim C63-C41
 with sigma of 0.02
 C62-C64 \\sim C64-C41 \\sim C41-C62
 with sigma of 0.02
 C66-C64 \\sim C66-C67 \\sim C65-C42 \\sim C65-C45
 with sigma of 0.02
 C68-C67 \\sim C68-C69 \\sim C68-C46
 with sigma of 0.02
 C67-C69 \\sim C69-C46 \\sim C46-C67
 with sigma of 0.02
3. Restrained planarity
 C43, C42, C66, C45, C44
 with sigma of 0.1
 C65, C64, C79, C80, C67
 with sigma of 0.1
 C53, C54, C72, C73, C74
 with sigma of 0.1
 C31, C32, C33, C55, C56
 with sigma of 0.1
 C9, C10, C11, C28, C29
 with sigma of 0.1
 C5, C6, C7, C21, C22
 with sigma of 0.1
 C17, C18, C19, C39, C40
 with sigma of 0.1
 C35, C36, C37, C58, C59
 with sigma of 0.1
 C60, C61, C76, C77, C78
 with sigma of 0.1
 C49, C50, C69, C70, C71
 with sigma of 0.1
 C24, C25, C26, C47, C48
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
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 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 C64 \\sim C63 \\sim C41 \\sim C42 \\sim C66
\\sim C65 \\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 C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 C84(H84), C86(H86), C88(H88), C90(H90)
5.b Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C87(H87A,H87B), C89(H89A,H89B), C91(H91A,H91B), C92(H92A,H92B)
;
_shelx_res_checksum              53156
_shelx_fab_checksum              26221
_olex2_submission_special_instructions 'No special instructions were received'