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_7128209
_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         'C32 H64 N4 O4 Th'
_chemical_formula_sum            'C32 H64 N4 O4 Th'
_chemical_formula_weight         800.91
_chemical_name_systematic        Th(ITA)4
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-12-18
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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                 113.0550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.6755(11)
_cell_length_b                   12.3970(5)
_cell_length_c                   8.8081(4)
_cell_measurement_reflns_used    16912
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.466
_cell_measurement_theta_min      2.077
_cell_volume                     1876.38(16)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0314
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16912
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         31.466
_diffrn_reflns_theta_min         2.077
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.274
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
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_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
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_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     211
_refine_ls_number_reflns         2994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0187
_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^)+(0.0322P)^2^+3.0242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2994
_reflns_number_total             2994
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_depositor_comments
'Adding full bibliography for 7128209--7128211.cif.'
_cod_database_code               7128209
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.700
_shelx_estimated_absorpt_t_min   0.513
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C5)
Uanis(C10) = Uanis(C8)
Uanis(C11) = Uanis(C6)
3. Others
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(H12B)=1-FVAR(1)
 Sof(O2)=Sof(N2)=Sof(C2)=Sof(C9)=Sof(H9)=Sof(C11)=Sof(C12)=Sof(H12A)=0.5*(1-
 FVAR(2))
 Sof(O1)=Sof(N1)=Sof(C1)=Sof(C4)=Sof(H4)=Sof(C6)=Sof(C7)=Sof(H7A)=0.5*FVAR(2)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
 Sof(H7B)=FVAR(1)
 Fixed Sof: O3(0.5) N3(0.5) C14(0.5) H14(0.5) C15(0.5) H15A(0.5) H15B(0.5)
 H15C(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C17(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) C3(0.5)
4.a Ternary CH refined with riding coordinates:
 C4(H4), C9(H9), C14(H14)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              40901
_olex2_submission_special_instructions 'No special instructions were received'