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_7132419
_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_absolute_configuration ad
_chemical_formula_moiety         'C52 H70 Mo3 N2 S4 U, C7 H8'
_chemical_formula_sum            'C59 H78 Mo3 N2 S4 U'
_chemical_formula_weight         1469.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-05-26
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.01510(10)
_cell_length_b                   20.26860(10)
_cell_length_c                   24.6766(2)
_cell_measurement_reflns_used    37491
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.3830
_cell_measurement_theta_min      3.5760
_cell_volume                     5509.31(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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -79.00  24.00   0.50    3.03    --  -47.07  98.00-139.00  206
  2  \w   -161.00 -82.00   0.50   12.12    --  -91.75-110.00-146.00  158
  3  \w    103.00 178.00   0.50   12.12    --  113.25 110.00 -51.00  150
  4  \w     43.00 106.00   0.50   12.12    --  113.25 -98.00 113.00  126
  5  \w    101.00 178.00   0.50   12.12    --  113.25  30.00 101.00  154
  6  \w     -9.00  28.00   0.50    3.03    --  -47.07  19.00  90.00   74
  7  \w   -119.00 -65.00   0.50    3.03    --  -47.07   0.00 -30.00  108
  8  \w   -119.00 -32.00   0.50    3.03    --  -47.07 -57.00 120.00  174
  9  \w     -9.00  28.00   0.50    3.03    --  -47.07  19.00 -90.00   74
 10  \w     97.00 178.00   0.50   12.12    --  113.25  61.00   0.00  162
 11  \w     44.00 111.00   0.50   12.12    --  113.25-125.00-150.00  134
 12  \w     42.00  83.00   0.50   12.12    --  113.25 -61.00-180.00   82
 13  \w     44.00 111.00   0.50   12.12    --  113.25-125.00 -90.00  134
 14  \w     42.00  83.00   0.50   12.12    --  113.25 -61.00  30.00   82
 15  \w     42.00  83.00   0.50   12.12    --  113.25 -61.00  90.00   82
 16  \w    101.00 178.00   0.50   12.12    --  113.25  45.00 150.00  154
 17  \w     42.00  83.00   0.50   12.12    --  113.25 -61.00 120.00   82
 18  \w    101.00 178.00   0.50   12.12    --  113.25  45.00 -90.00  154
 19  \w    101.00 178.00   0.50   12.12    --  113.25  45.00-180.00  154
 20  \w     42.00 106.00   0.50   12.12    --  113.25 -94.00-180.00  128
 21  \w     41.00 178.00   0.50   12.12    --  113.25   0.00-120.00  274
 22  \w     42.00  83.00   0.50   12.12    --  113.25 -61.00 -90.00   82
 23  \w     42.00  83.00   0.50   12.12    --  113.25 -61.00-120.00   82
 24  \w     42.00  83.00   0.50   12.12    --  113.25 -61.00   0.00   82
 25  \w   -119.00 -32.00   0.50    3.03    --  -47.07 -57.00 -60.00  174
 26  \w   -120.00 -24.00   0.50    3.03    --  -47.07 -77.00  60.00  192
 27  \w   -119.00 -32.00   0.50    3.03    --  -47.07 -57.00-150.00  174
 28  \w     34.00  93.00   0.50    3.03    --   47.07-125.00 120.00  118
;
_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      0.0510886000
_diffrn_orient_matrix_UB_12      0.0698450000
_diffrn_orient_matrix_UB_13      -0.0093149000
_diffrn_orient_matrix_UB_21      0.0204973000
_diffrn_orient_matrix_UB_22      -0.0163268000
_diffrn_orient_matrix_UB_23      -0.0602917000
_diffrn_orient_matrix_UB_31      -0.1285656000
_diffrn_orient_matrix_UB_32      0.0251469000
_diffrn_orient_matrix_UB_33      -0.0132598000
_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  0.0598
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            70003
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.287
_diffrn_reflns_theta_min         3.582
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60078
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.081
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.269
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
;
 Flack x determined using 4720 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.036(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         11882
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0268P)^2^+28.6488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                11276
_reflns_number_total             11882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05561b2.cif
_cod_data_source_block           matkp10
_cod_depositor_comments
'Adding full bibliography for 7132418--7132420.cif.'
_cod_database_code               7132419
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.370
_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. Restrained distances
 C53-C54
 1.52 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C53, C54, C55, C56, C57, C58, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59)
4.b Fitted hexagon refined as free rotating group:
 C54(C55,C56,C57,C58,C59)
4.c 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), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              1476
_shelx_hkl_checksum              33643
_olex2_submission_original_sample_id matkp10
_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 1.678
_oxdiff_exptl_absorpt_empirical_full_min 0.720