Molybdenum sulphide clusters as redox-active supports for low-valent uranium.
Patra, Kamaless; Brennessel, William W.; Matson, Ellen M.; Chemical communications (Cambridge, England) 60 (2024) 530–533; doi:10.1039/d3cc05561b

data_7132418
_publ_section_title
;
 Molybdenum sulphide clusters as redox-active supports for low-valent
 uranium.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              530
_journal_page_last               533
_journal_paper_doi               10.1039/d3cc05561b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C40 H60 I2 Mo3 S4 U, 2(C6 D6)'
_chemical_formula_sum            'C52 H60 D12 I2 Mo3 S4 U'
_chemical_formula_weight         1617.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-04-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-11-08 deposited with the CCDC.	2023-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.0360(10)
_cell_angle_beta                 109.1620(10)
_cell_angle_gamma                110.9690(10)
_cell_formula_units_Z            2
_cell_length_a                   13.30840(10)
_cell_length_b                   13.3384(3)
_cell_length_c                   17.3783(3)
_cell_measurement_reflns_used    64472
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.4550
_cell_measurement_theta_min      3.5710
_cell_volume                     2696.47(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.980
_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    -81.00   3.00   0.50    0.20    --  -47.28 104.00 -25.00  168
  2  \w     18.00  83.00   0.50    0.20    --   47.28-104.00-126.00  130
  3  \w   -162.00 -84.00   0.50    0.81    --  -91.75-104.00-126.00  156
  4  \w    -81.00 -21.00   0.50    0.81    --  -91.75 104.00 -25.00  120
  5  \w    106.00 178.00   0.50    0.81    --  113.25 104.00 -25.00  144
  6  \w     43.00 107.00   0.50    0.81    --  113.25-104.00-126.00  128
  7  \w    -14.00  28.00   0.50    0.20    --  -47.28  19.00 120.00   84
  8  \w    -14.00  28.00   0.50    0.20    --  -47.28  19.00-120.00   84
  9  \w    -86.00 -13.00   0.50    0.20    --  -47.28 125.00-120.00  146
 10  \w   -119.00 -25.00   0.50    0.20    --  -47.28 -77.00-150.00  188
 11  \w    -14.00  28.00   0.50    0.20    --  -47.28  19.00 -30.00   84
 12  \w    -38.00  26.00   0.50    0.20    --  -47.28  38.00   0.00  128
 13  \w    -14.00  28.00   0.50    0.20    --  -47.28  19.00 -90.00   84
 14  \w     34.00  93.00   0.50    0.20    --   47.28-125.00-120.00  118
 15  \w    -27.00  18.00   0.50    0.20    --   47.28 -19.00 -30.00   90
 16  \w    -47.00 -20.00   0.50    0.81    --  -91.75  45.00 120.00   54
 17  \w    -47.00 -20.00   0.50    0.81    --  -91.75  45.00 -90.00   54
 18  \w   -163.00 -76.00   0.50    0.81    --  -91.75 -60.00 -45.92  174
 19  \w     42.00 106.00   0.50    0.81    --  113.25 -94.00 -90.00  128
 20  \w     42.00 106.00   0.50    0.81    --  113.25 -94.00   0.00  128
 21  \w     44.00 111.00   0.50    0.81    --  113.25-125.00-150.00  134
 22  \w     42.00  76.00   0.50    0.81    --  113.25 -61.00 120.00   68
 23  \w     42.00  76.00   0.50    0.81    --  113.25 -61.00  30.00   68
 24  \w     91.00 178.00   0.50    0.81    --  113.25  77.00 120.00  174
 25  \w     42.00 106.00   0.50    0.81    --  113.25 -94.00-120.00  128
 26  \w     42.00 106.00   0.50    0.81    --  113.25 -94.00  30.00  128
 27  \w    100.00 178.00   0.50    0.81    --  113.25  15.00 -90.00  156
 28  \w     42.00  76.00   0.50    0.81    --  113.25 -61.00 150.00   68
 29  \w     42.00 106.00   0.50    0.81    --  113.25 -94.00 120.00  128
 30  \w    100.00 178.00   0.50    0.81    --  113.25  15.00 -60.00  156
 31  \w    100.00 178.00   0.50    0.81    --  113.25  15.00 150.00  156
 32  \w     42.00  76.00   0.50    0.81    --  113.25 -61.00   0.00   68
 33  \w     42.00  76.00   0.50    0.81    --  113.25 -61.00 -90.00   68
 34  \w     42.00  76.00   0.50    0.81    --  113.25 -61.00-180.00   68
 35  \w    101.00 178.00   0.50    0.81    --  113.25  45.00   0.00  154
 36  \w    101.00 178.00   0.50    0.81    --  113.25  30.00  60.00  154
 37  \w     42.00 106.00   0.50    0.81    --  113.25 -94.00 -30.00  128
 38  \w    101.00 178.00   0.50    0.81    --  113.25  30.00 120.00  154
 39  \w     44.00 111.00   0.50    0.81    --  113.25-125.00 120.00  134
 40  \w     42.00 106.00   0.50    0.81    --  113.25 -94.00  90.00  128
 41  \w     42.00 106.00   0.50    0.81    --  113.25 -94.00-180.00  128
 42  \w     91.00 178.00   0.50    0.81    --  113.25  77.00  30.00  174
 43  \w     42.00  76.00   0.50    0.81    --  113.25 -61.00-120.00   68
 44  \w    101.00 178.00   0.50    0.81    --  113.25  45.00 -30.00  154
 45  \w     42.00 106.00   0.50    0.81    --  113.25 -94.00  60.00  128
 46  \w     42.00  76.00   0.50    0.81    --  113.25 -61.00 -30.00   68
 47  \w    100.00 178.00   0.50    0.81    --  113.25  15.00   0.00  156
 48  \w     42.00 106.00   0.50    0.81    --  113.25 -95.00 -61.10  128
 49  \w     42.00  76.00   0.50    0.81    --  113.25 -61.00  90.00   68
 50  \w   -119.00 -25.00   0.50    0.20    --  -47.28 -77.00 -90.00  188
 51  \w   -119.00 -25.00   0.50    0.20    --  -47.28 -77.00 -30.00  188
 52  \w   -119.00 -25.00   0.50    0.20    --  -47.28 -77.00-180.00  188
 53  \w   -119.00 -32.00   0.50    0.20    --  -47.28 -57.00  30.00  174
 54  \w   -119.00 -25.00   0.50    0.20    --  -47.28 -77.00   0.00  188
 55  \w   -119.00 -25.00   0.50    0.20    --  -47.28 -77.00 120.00  188
 56  \w     25.00 120.00   0.50    0.20    --   47.28  77.00  90.00  190
 57  \w     35.00 120.00   0.50    0.20    --   47.28  38.00  30.00  170
 58  \w     35.00 120.00   0.50    0.20    --   47.28  38.00 150.00  170
 59  \w     35.00 120.00   0.50    0.20    --   47.28  38.00 -60.00  170
 60  \w     35.00 120.00   0.50    0.20    --   47.28  38.00-120.00  170
 61  \w   -163.00 -77.00   0.50    0.81    --  -91.75 -77.00   0.00  172
 62  \w   -163.00 -69.00   0.50    0.81    --  -91.75 -76.00-159.51  188
 63  \w   -163.00 -69.00   0.50    0.81    --  -91.75 -77.00 -90.00  188
 64  \w   -163.00 -71.00   0.50    0.81    --  -91.75 -73.00  98.58  184
 65  \w   -163.00 -69.00   0.50    0.81    --  -91.75 -77.00  60.00  188
 66  \w   -163.00 -69.00   0.50    0.81    --  -91.75 -77.00 -60.00  188
 67  \w   -163.00 -69.00   0.50    0.81    --  -91.75 -77.00-120.00  188
 68  \w   -163.00 -71.00   0.50    0.81    --  -91.75 -72.00 147.02  184
 69  \w   -163.00 -69.00   0.50    0.81    --  -91.75 -77.00  30.00  188
 70  \w    101.00 178.00   0.50    0.81    --  113.25  30.00-150.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1286026000
_diffrn_orient_matrix_UB_12      -0.0216589000
_diffrn_orient_matrix_UB_13      -0.0223096000
_diffrn_orient_matrix_UB_21      0.0084303000
_diffrn_orient_matrix_UB_22      -0.0233905000
_diffrn_orient_matrix_UB_23      0.0882238000
_diffrn_orient_matrix_UB_31      0.0304781000
_diffrn_orient_matrix_UB_32      0.1206749000
_diffrn_orient_matrix_UB_33      0.0262122000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            91758
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.527
_diffrn_reflns_theta_min         3.581
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.087
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.796
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         11563
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+14.3048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11205
_reflns_number_total             11563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05561b2.cif
_cod_data_source_block           matkp07
_cod_depositor_comments
'Adding full bibliography for 7132418--7132420.cif.'
_cod_database_code               7132418
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.497
_shelx_estimated_absorpt_t_min   0.223
_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
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.2A
3. Same fragment restrains
{C48, C49, C50, C51, C52, C47} sigma for 1-2: 0.02, 1-3: 0.04
{C52, C51, C50, C49, C48, C47} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C47, C48, C49, C50, C51, C52}
{C47, C48, C49, C50, C51, C52} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C47', C48', C49', C50', C51', C52'}
4. Others
 Sof(C47')=Sof(D47')=Sof(C48')=Sof(D48')=Sof(C49')=Sof(D49')=Sof(C50')=
 Sof(D50')=Sof(C51')=Sof(D51')=Sof(C52')=Sof(D52')=1-FVAR(1)
 Sof(C47)=Sof(D47)=Sof(C48)=Sof(D48)=Sof(C49)=Sof(D49)=Sof(C50)=Sof(D50)=
 Sof(C51)=Sof(D51)=Sof(C52)=Sof(D52)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C47'(D47'), C48'(D48'), C49'(D49'), C50'(D50'), C51'(D51'), C52'(D52'),
 C47(D47), C48(D48), C49(D49), C50(D50), C51(D51), C52(D52), C41(D41), C42(D42),
  C43(D43), C44(D44), C45(D45), C46(D46)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              36637
_shelx_hkl_checksum              40258
_olex2_submission_original_sample_id matkp07
_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 2.139
_oxdiff_exptl_absorpt_empirical_full_min 0.702