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_7128211
_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         'C52 H48 F24 N4 O4 Th, C6 H14'
_chemical_formula_sum            'C58 H62 F24 N4 O4 Th'
_chemical_formula_weight         1567.15
_chemical_name_systematic        Th(ArFTA)4
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-21
_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                 102.024(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7799(2)
_cell_length_b                   14.0321(3)
_cell_length_c                   22.2223(5)
_cell_measurement_reflns_used    33897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7270
_cell_measurement_theta_min      3.2620
_cell_volume                     3287.70(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -45.00  21.00   0.50    6.00    --   -2.02 -77.00 -60.00  132
  2  \w    -45.00  21.00   0.50    6.00    --   -2.02 -77.00  60.00  132
  3  \w    -12.00  36.00   0.50    6.00    --    2.33 -99.00 120.00   96
  4  \w    -75.00  15.00   0.50    6.00    --    2.33 -38.00 -30.00  180
  5  \w    -79.00  11.00   0.50    6.00    --   -2.02 -38.00-150.00  180
  6  \w    -71.00  17.00   0.50    6.00    --    2.33 -57.00-180.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0097602000
_diffrn_orient_matrix_UB_12      -0.0442563000
_diffrn_orient_matrix_UB_13      -0.0156986000
_diffrn_orient_matrix_UB_21      -0.0287312000
_diffrn_orient_matrix_UB_22      0.0240565000
_diffrn_orient_matrix_UB_23      -0.0274513000
_diffrn_orient_matrix_UB_31      0.0600496000
_diffrn_orient_matrix_UB_32      0.0043413000
_diffrn_orient_matrix_UB_33      -0.0080432000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.801
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0219
_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^)+(0.0320P)^2^+1.8207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6324
_reflns_number_total             6726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00867f2.cif
_cod_data_source_block           mds_3_183
_cod_depositor_comments
'Adding full bibliography for 7128209--7128211.cif.'
_cod_database_code               7128211
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Th C80 H80 F24 N4 O4'
_diffrn_oxdiff_digest_frames
;
01167b51101fd2a014d3581e8aa5ab9ee70089612ef
;
_diffrn_oxdiff_digest_hkl
;
017cf3351ddae64a5c6a4cb8d4f9ce119c517b
;
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Fixed Sof: C30(0.5) H30A(0.5) H30B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5) C28(0.5) H28A(0.5) H28B(0.5) C31(0.5) H31A(0.5) H31B(0.5) C29(0.5)
 H29A(0.5) H29B(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C28(H28A,H28B), C31(H31A,H31B), C29(H29A,H29B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C8(H8), C24(H24), C22(H22), C20(H20)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C4(H4A,H4B,H4C), C32(H32A,H32B,H32C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              54995
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.300
_oxdiff_exptl_absorpt_empirical_full_min 0.640