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_7132420
_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 I Mo3 S4 U'
_chemical_formula_sum            'C40 H60 I Mo3 S4 U'
_chemical_formula_weight         1321.87
_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             2023-05-11
_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                79.9966(7)
_cell_angle_beta                 75.1189(7)
_cell_angle_gamma                87.6951(6)
_cell_formula_units_Z            4
_cell_length_a                   11.22430(9)
_cell_length_b                   20.51803(14)
_cell_length_c                   21.54896(19)
_cell_measurement_reflns_used    87058
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.9920
_cell_measurement_theta_min      3.3570
_cell_volume                     4723.32(7)
_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 0.999
_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   -119.00 -57.00   0.50    0.37    --  -47.31-148.00-112.00  124
  2  \w   -103.00 -25.00   0.50    0.37    --  -47.31 148.00 -64.00  156
  3  \w    -85.00 -12.00   0.50    0.37    --  -47.31 124.00 131.00  146
  4  \w     34.00  92.00   0.50    0.37    --   47.31-124.00  52.00  116
  5  \w     47.00 109.00   0.50    0.37    --   47.31-148.00-112.00  124
  6  \w    -85.00 -22.00   0.50    1.50    --  -91.75 124.00 131.00  126
  7  \w   -150.00 -57.00   0.50    1.50    --  -91.75-148.00-112.00  186
  8  \w     47.00 128.00   0.50    1.50    --  113.25-148.00-112.00  162
  9  \w     79.00 167.00   0.50    1.50    --  113.25 148.00 -64.00  176
 10  \w     96.00 178.00   0.50    1.50    --  113.25 124.00 131.00  164
 11  \w     44.00 110.00   0.50    1.50    --  113.25-124.00  52.00  132
 12  \w    -14.00  28.00   0.50    0.37    --  -47.31  19.00-120.00   84
 13  \w    -14.00  28.00   0.50    0.37    --  -47.31  19.00  60.00   84
 14  \w    -14.00  28.00   0.50    0.37    --  -47.31  19.00-150.00   84
 15  \w   -119.00 -32.00   0.50    0.37    --  -47.31 -57.00 -60.00  174
 16  \w    -14.00  28.00   0.50    0.37    --  -47.31  19.00 -60.00   84
 17  \w    -14.00  28.00   0.50    0.37    --  -47.31  19.00-180.00   84
 18  \w    -14.00  28.00   0.50    0.37    --  -47.31  19.00  90.00   84
 19  \w    -27.00  18.00   0.50    0.37    --   47.31 -19.00  60.00   90
 20  \w    -27.00  18.00   0.50    0.37    --   47.31 -19.00-150.00   90
 21  \w   -163.00 -77.00   0.50    1.50    --  -91.75 -55.00 114.52  172
 22  \w    100.00 178.00   0.50    1.50    --  113.25  15.00 -30.00  156
 23  \w     42.00  76.00   0.50    1.50    --  113.25 -61.00   0.00   68
 24  \w     44.00 111.00   0.50    1.50    --  113.25-125.00  90.00  134
 25  \w    101.00 178.00   0.50    1.50    --  113.25  45.00-150.00  154
 26  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00   0.00  128
 27  \w    101.00 178.00   0.50    1.50    --  113.25  45.00 120.00  154
 28  \w     42.00  76.00   0.50    1.50    --  113.25 -61.00-120.00   68
 29  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00 -60.00  128
 30  \w     42.00  76.00   0.50    1.50    --  113.25 -61.00 -60.00   68
 31  \w     44.00 111.00   0.50    1.50    --  113.25-125.00-180.00  134
 32  \w    101.00 178.00   0.50    1.50    --  113.25  30.00-180.00  154
 33  \w    101.00 178.00   0.50    1.50    --  113.25  30.00 -90.00  154
 34  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00  90.00  128
 35  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00-150.00  128
 36  \w     44.00 111.00   0.50    1.50    --  113.25-125.00 120.00  134
 37  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00 -30.00  128
 38  \w    101.00 178.00   0.50    1.50    --  113.25  30.00-120.00  154
 39  \w     97.00 178.00   0.50    1.50    --  113.25  61.00   0.00  162
 40  \w     42.00  76.00   0.50    1.50    --  113.25 -61.00  30.00   68
 41  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00 -45.10  128
 42  \w     42.00 136.00   0.50    1.50    --  113.25 -77.00  90.00  188
 43  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00 -90.00  128
 44  \w     91.00 178.00   0.50    1.50    --  113.25  77.00  30.00  174
 45  \w    101.00 178.00   0.50    1.50    --  113.25  45.00  60.00  154
 46  \w     95.00 178.00   0.50    1.50    --  113.25 125.00 -90.00  166
 47  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00  60.00  128
 48  \w     95.00 178.00   0.50    1.50    --  113.25 125.00 -60.00  166
 49  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00-120.00  128
 50  \w     42.00  76.00   0.50    1.50    --  113.25 -61.00-180.00   68
 51  \w     42.00 106.00   0.50    1.50    --  113.25 -94.00 120.00  128
 52  \w     44.00 111.00   0.50    1.50    --  113.25-125.00 150.00  134
 53  \w     42.00  76.00   0.50    1.50    --  113.25 -61.00  60.00   68
 54  \w   -119.00 -25.00   0.50    0.37    --  -47.31 -77.00  60.00  188
 55  \w   -119.00 -25.00   0.50    0.37    --  -47.31 -77.00  30.00  188
 56  \w   -119.00 -25.00   0.50    0.37    --  -47.31 -77.00 -60.00  188
 57  \w   -119.00 -25.00   0.50    0.37    --  -47.31 -77.00-120.00  188
 58  \w   -119.00 -32.00   0.50    0.37    --  -47.31 -57.00 150.00  174
 59  \w   -119.00 -25.00   0.50    0.37    --  -47.31 -77.00 120.00  188
 60  \w     25.00 120.00   0.50    0.37    --   47.31  77.00-150.00  190
 61  \w     35.00 120.00   0.50    0.37    --   47.31  38.00  60.00  170
 62  \w     25.00 120.00   0.50    0.37    --   47.31  77.00 150.00  190
 63  \w     25.00 120.00   0.50    0.37    --   47.31  77.00  30.00  190
 64  \w     35.00 120.00   0.50    0.37    --   47.31  38.00 150.00  170
 65  \w     35.00 120.00   0.50    0.37    --   47.31  38.00 -30.00  170
 66  \w   -163.00-104.00   0.50    1.50    --  -91.75 -71.00 -81.00  118
 67  \w   -163.00 -69.00   0.50    1.50    --  -91.75 -76.00  78.66  188
 68  \w   -163.00 -69.00   0.50    1.50    --  -91.75 -77.00-180.00  188
 69  \w   -163.00 -71.00   0.50    1.50    --  -91.75 -72.00 -23.24  184
;
_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      0.0545305000
_diffrn_orient_matrix_UB_12      -0.0699044000
_diffrn_orient_matrix_UB_13      -0.0022391000
_diffrn_orient_matrix_UB_21      -0.0451665000
_diffrn_orient_matrix_UB_22      -0.0171482000
_diffrn_orient_matrix_UB_23      0.0747518000
_diffrn_orient_matrix_UB_31      -0.1231032000
_diffrn_orient_matrix_UB_32      -0.0250617000
_diffrn_orient_matrix_UB_33      -0.0064112000
_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  0.076
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            260733
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.446
_diffrn_reflns_theta_min         3.319
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.867
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11183
_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            green-black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_description       needle
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.023
_refine_diff_density_max         2.942
_refine_diff_density_min         -3.500
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         47571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0846P)^2^+14.7790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                43990
_reflns_number_total             47571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05561b2.cif
_cod_data_source_block           matkp08
_cod_depositor_comments
'Adding full bibliography for 7132418--7132420.cif.'
_cod_database_code               7132420
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.621
_shelx_estimated_absorpt_t_min   0.058
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5948(5)
 0.4052(5)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3.a 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), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C)
;
_shelx_res_checksum              93967
_shelx_hkl_checksum              6886
_shelx_fab_checksum              50661
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id matkp08
_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 5.681
_oxdiff_exptl_absorpt_empirical_full_min 0.449