Thorium amidates function as single-source molecular precursors for thorium dioxide.
Straub, Mark D.; Ouellette, Erik T.; Boreen, Michael A.; Branson, Jacob A.; Ditter, Alex; Kilcoyne, A. L. David; Lohrey, Trevor D.; Marcus, Matthew A.; Paley, Maria; Ramirez, José; Shuh, David K.; Minasian, Stefan G.; Arnold, John; Chemical communications (Cambridge, England) 57 (2021) 4954–4957; doi:10.1039/d1cc00867f

data_7128210
_publ_section_title
;
 Thorium amidates function as single-source molecular precursors for
 thorium dioxide.
;
_journal_issue                   40
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4954
_journal_page_last               4957
_journal_paper_doi               10.1039/d1cc00867f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C60 H88 N4 O4 Th'
_chemical_formula_sum            'C60 H88 N4 O4 Th'
_chemical_formula_weight         1161.38
_chemical_name_systematic        Th(TPTA)4
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-19 deposited with the CCDC.	2021-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.646(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.5272(17)
_cell_length_b                   11.0968(7)
_cell_length_c                   21.0598(13)
_cell_measurement_reflns_used    25021
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.042
_cell_measurement_theta_min      1.040
_cell_volume                     5907.6(7)
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_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
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.343
_diffrn_measurement_device_type  'Bruker D8 with PHOTON-II CPAD detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.343
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25021
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.343
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         1.040
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    2.739
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             2392
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.865
_refine_diff_density_min         -4.197
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.489
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5433
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.488
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+84.8249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5253
_reflns_number_total             5433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00867f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7128209--7128211.cif.'
_cod_database_code               7128210
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.536
_shelx_estimated_absorpt_t_min   0.204
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.952(2)
 0.0142(19) 0.0334(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C21) = Uanis(C21A)
Uanis(C23) = Uanis(C23A)
4. Others
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C21A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(2)
 Sof(C21)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C11(H11), C18(H18), C19(H19), C25(H25), C26(H26)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C24A(H24D,H24E,H24F), C13A(H13D,H13E,H13F), C15A(H15D,H15E,H15F), C22A(H22D,
 H22E,H22F), C14A(H14D,H14E,H14F), C23A(H23D,H23E,H23F), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              52827
_olex2_submission_special_instructions 'No special instructions were received'