Formation of uranium disulfide from a uranium thioamidate single-source precursor.
Kelly, Sheridon N.; Russo, Dominic R.; Ouellette, Erik T.; Roy, Debashree; Swift, Andrew J.; Boreen, Michael A.; Smith, Patrick W.; Moreau, Liane M.; Arnold, John; Minasian, Stefan G.; Chemical science 15 (2024) 13325–13332; doi:10.1039/d4sc03422h

data_1572160
_publ_section_title
;
 Formation of uranium disulfide from a uranium thioamidate single-source
 precursor.
;
_journal_issue                   33
_journal_name_full               'Chemical science'
_journal_page_first              13325
_journal_page_last               13332
_journal_paper_doi               10.1039/d4sc03422h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C32 H64 N4 S4 U'
_chemical_formula_sum            'C32 H64 N4 S4 U'
_chemical_formula_weight         871.14
_chemical_melting_point          483.15
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-05-04 deposited with the CCDC.	2024-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6654(2)
_cell_length_b                   11.61050(10)
_cell_length_c                   15.62010(10)
_cell_measurement_reflns_used    45033
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      77.2280
_cell_measurement_theta_min      4.1000
_cell_volume                     3905.57(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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     82.00 119.00   0.50    0.10    --   47.95  57.00   0.00   74
  2  \w     82.00 119.00   0.50    0.10    --   47.95  57.00 150.00   74
  3  \w     82.00 119.00   0.50    0.10    --   47.95  57.00 -30.00   74
  4  \w     82.00 119.00   0.50    0.10    --   47.95  57.00 -60.00   74
  5  \w     82.00 119.00   0.50    0.10    --   47.95  57.00 -90.00   74
  6  \w    102.00 178.00   0.50    0.34    --  107.75  77.00-180.00  152
  7  \w     96.00 176.00   0.50    0.34    --  107.75  66.00-106.02  160
  8  \w    142.00 168.00   0.50    0.34    --  107.75  77.00 -90.00   52
  9  \w    135.00 174.00   0.50    0.34    --  107.75  30.00-120.00   78
 10  \w     93.00 178.00   0.50    0.34    --  107.75  56.00  -9.87  170
 11  \w    101.00 178.00   0.50    0.34    --  107.75  30.00 -30.00  154
 12  \w    107.00 133.00   0.50    0.34    --  107.75  30.00  60.00   52
 13  \w    101.00 174.00   0.50    0.34    --  107.75  77.00 150.00  146
 14  \w     94.00 176.00   0.50    0.34    --  107.75  15.00 120.00  164
 15  \w    142.00 170.00   0.50    0.34    --  107.75  30.00  60.00   56
 16  \w     94.00 178.00   0.50    0.34    --  107.75  15.00-180.00  168
 17  \w    107.00 178.00   0.50    0.34    --  107.75 101.00-172.00  142
 18  \w    126.00 163.00   0.50    0.34    --  107.75 125.00 -60.00   74
 19  \w    106.00 132.00   0.50    0.34    --  107.75 125.00  60.00   52
 20  \w     37.00  87.00   0.50    0.34    --  107.75 -77.00  30.00  100
 21  \w     35.00  71.00   0.50    0.34    --  107.75 -61.00  60.00   72
 22  \w     43.00  73.00   0.50    0.34    --  107.75 -61.00 120.00   60
 23  \w     36.00  64.00   0.50    0.34    --  107.75 -61.00-150.00   56
 24  \w     35.00  72.00   0.50    0.34    --  107.75 -61.00-180.00   74
 25  \w    -26.00  24.00   0.50    0.10    --   47.95 -19.00-180.00  100
 26  \w     56.00 106.00   0.50    0.34    --  107.75 -94.00 -46.76  100
 27  \w     34.00  96.00   0.50    0.10    --   47.95-125.00-180.00  124
 28  \w     40.00  73.00   0.50    0.34    --  107.75-125.00 -90.00   66
 29  \w     76.00 106.00   0.50    0.34    --  107.75-125.00 -90.00   60
 30  \w     39.00  96.00   0.50    0.34    --  107.75-109.00  21.30  114
 31  \w     49.00 107.00   0.50    0.34    --  107.75-105.00  29.30  116
 32  \w     36.00  63.00   0.50    0.34    --  107.75-125.00  90.00   54
 33  \w     35.00 106.00   0.50    0.34    --  107.75-101.00  82.00  142
 34  \w     35.00 106.00   0.50    0.34    --  107.75 -94.00 120.00  142
 35  \w     55.00  81.00   0.50    0.34    --  107.75-125.00 150.00   52
 36  \w      4.00  82.00   0.50    0.10    --   47.95-101.00  82.00  156
 37  \w     64.00 106.00   0.50    0.34    --  107.75 -94.00  30.00   84
 38  \w     36.00  90.00   0.50    0.34    --  107.75 -94.00 -60.00  108
 39  \w     44.00 106.00   0.50    0.34    --  107.75 -98.00 -70.90  124
 40  \w     43.00 106.00   0.50    0.34    --  107.75 -94.00-150.00  126
 41  \w     78.00 106.00   0.50    0.34    --  107.75 -94.00-180.00   56
 42  \w     42.00  74.00   0.50    0.34    --  107.75 -94.00-180.00   64
 43  \w     68.00 105.00   0.50    0.34    --  107.75 -94.00-120.00   74
 44  \w     35.00  77.00   0.50    0.34    --  107.75 -94.00 -90.00   84
 45  \w     35.00 105.00   0.50    0.34    --  107.75 -94.00 -30.00  140
 46  \w     47.00 106.00   0.50    0.34    --  107.75 -94.00  90.00  118
 47  \w     79.00 106.00   0.50    0.34    --  107.75 -94.00 150.00   54
 48  \w     38.00  71.00   0.50    0.34    --  107.75 -94.00 150.00   66
 49  \w   -119.00 -35.00   0.50    0.10    --  -47.95 -48.00 -64.30  168
 50  \w   -159.00 -91.00   0.50    0.34    --  -86.25 -61.00-180.00  136
 51  \w   -159.00 -85.00   0.50    0.34    --  -86.25-101.00  82.00  148
 52  \w   -119.00 -82.00   0.50    0.10    --  -47.95 -57.00 -30.00   74
 53  \w    -40.00  25.00   0.50    0.10    --  -47.95  37.00 120.00  130
 54  \w    -49.00 -14.00   0.50    0.34    --  -86.25  45.00 -60.00   70
 55  \w    -80.00  18.00   0.50    0.10    --  -47.95 101.00-172.00  196
 56  \w    -81.00 -13.00   0.50    0.34    --  -86.25 101.00-172.00  136
 57  \w    -49.00 -14.00   0.50    0.34    --  -86.25  45.00-180.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            79768
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.463
_diffrn_reflns_theta_min         4.106
_exptl_absorpt_coefficient_mu    13.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.366
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         8264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+4.4174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7522
_reflns_number_total             8264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03422h2.cif
_cod_data_source_block           ja21002
_cod_depositor_comments          'Adding full bibliography for 1572160.cif.'
_cod_database_code               1572160
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.490
_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.a Ternary CH refined with riding coordinates:
 C26(H26), C12(H12), C19(H19), C5(H5)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C16(H16A,H16B,
 H16C), C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C25(H25A,
 H25B,H25C), C27(H27A,H27B,H27C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C11(H11A,H11B,
 H11C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C6(H6A,H6B,H6C), C13(H13A,
 H13B,H13C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              42051
_shelx_hkl_checksum              93844
_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
;