Synthesis and characterization of a low-valent uranium complex supported by a redox-active molybdenum oxide metalloligand.
Valerio, Leyla R.; Patra, Kamaless; Shiels, Dominic; Brennessel, William W.; Matson, Ellen M.; Chemical communications (Cambridge, England)  (2025) –; doi:10.1039/d5cc05531h

data_7135181
_publ_section_title
;
 Synthesis and characterization of a low-valent uranium complex supported
 by a redox-active molybdenum oxide metalloligand.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d5cc05531h
_journal_year                    2025
_chemical_formula_moiety         'C40 H60 Mo2 O4 U'
_chemical_formula_sum            'C40 H60 Mo2 O4 U'
_chemical_formula_weight         1034.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-10-31
_audit_creation_method
;
Olex2 1.5-ac6-015
(compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873)
;
_audit_update_record
;
2025-09-18 deposited with the CCDC.	2025-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2375(2)
_cell_length_b                   13.63680(10)
_cell_length_c                   17.8447(2)
_cell_measurement_reflns_used    22080
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      79.7180
_cell_measurement_theta_min      4.2400
_cell_volume                     3930.55(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.118a 64-bit (release 27-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(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 0.982
_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    -85.00 -12.00   0.50    0.72    --  -47.26 124.00 116.00  146
  2  \w   -120.00 -58.00   0.50    0.72    --  -47.26-147.00-127.00  124
  3  \w     46.00 107.00   0.50    0.72    --   47.26-147.00-127.00  122
  4  \w     34.00  92.00   0.50    0.72    --   47.26-124.00  37.00  116
  5  \w   -161.00 -74.00   0.50    2.90    --  -91.75-124.00  37.00  174
  6  \w     96.00 178.00   0.50    2.90    --  113.25 124.00 116.00  164
  7  \w     80.00 168.00   0.50    2.90    --  113.25 147.00 -78.00  176
  8  \w     46.00 127.00   0.50    2.90    --  113.25-147.00-127.00  162
  9  \w     44.00 110.00   0.50    2.90    --  113.25-124.00  37.00  132
 10  \w    -14.00  28.00   0.50    0.72    --  -47.26  19.00  90.00   84
 11  \w    -14.00  28.00   0.50    0.72    --  -47.26  19.00 -30.00   84
 12  \w    -14.00  28.00   0.50    0.72    --  -47.26  19.00  60.00   84
 13  \w    -14.00  28.00   0.50    0.72    --  -47.26  19.00  30.00   84
 14  \w    -14.00  28.00   0.50    0.72    --  -47.26  19.00 120.00   84
 15  \w    -30.00  26.00   0.50    0.72    --  -47.26  38.00-120.00  112
 16  \w    -58.00 -19.00   0.50    2.90    --  -91.75  61.00 -30.00   78
 17  \w     42.00 106.00   0.50    2.90    --  113.25 -94.00  60.00  128
 18  \w     42.00 106.00   0.50    2.90    --  113.25 -94.00 120.00  128
 19  \w     42.00 106.00   0.50    2.90    --  113.25 -94.00  90.00  128
 20  \w    101.00 178.00   0.50    2.90    --  113.25  45.00  30.00  154
 21  \w    101.00 178.00   0.50    2.90    --  113.25  30.00 120.00  154
 22  \w     42.00 118.00   0.50    2.90    --  113.25 -77.00  60.00  152
 23  \w     42.00  84.00   0.50    2.90    --  113.25 -61.00  90.00   84
 24  \w     91.00 178.00   0.50    2.90    --  113.25  77.00-180.00  174
 25  \w     44.00 111.00   0.50    2.90    --  113.25-125.00-180.00  134
 26  \w     42.00 118.00   0.50    2.90    --  113.25 -77.00  60.00  152
 27  \w     42.00 106.00   0.50    2.90    --  113.25 -94.00   0.00  128
 28  \w    101.00 178.00   0.50    2.90    --  113.25  45.00 -90.00  154
 29  \w     42.00  84.00   0.50    2.90    --  113.25 -61.00   0.00   84
 30  \w     42.00 106.00   0.50    2.90    --  113.25 -94.00  30.00  128
 31  \w     42.00 106.00   0.50    2.90    --  113.25 -94.00  90.00  128
 32  \w     91.00 178.00   0.50    2.90    --  113.25  77.00-180.00  174
 33  \w     97.00 178.00   0.50    2.90    --  113.25  61.00-150.00  162
 34  \w     42.00 106.00   0.50    2.90    --  113.25 -94.00 120.00  128
 35  \w     44.00 111.00   0.50    2.90    --  113.25-125.00  30.00  134
 36  \w     97.00 178.00   0.50    2.90    --  113.25  61.00-150.00  162
 37  \w     25.00 120.00   0.50    0.72    --   47.26  77.00  90.00  190
 38  \w     25.00 120.00   0.50    0.72    --   47.26  77.00   0.00  190
;
_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      -0.0871627000
_diffrn_orient_matrix_UB_12      0.0253619000
_diffrn_orient_matrix_UB_13      -0.0373605000
_diffrn_orient_matrix_UB_21      0.0229869000
_diffrn_orient_matrix_UB_22      0.1096452000
_diffrn_orient_matrix_UB_23      0.0014936000
_diffrn_orient_matrix_UB_31      0.0312079000
_diffrn_orient_matrix_UB_32      -0.0099016000
_diffrn_orient_matrix_UB_33      -0.0783014000
_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  0.0357
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32741
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.183
_diffrn_reflns_theta_min         4.243
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.118a (Rigaku Oxford Diffraction, 2024)
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    1.749
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.015
_refine_diff_density_max         3.808
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4238
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0210P)^2^+38.5113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4145
_reflns_number_total             4238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05531h2.cif
_cod_data_source_block           matkp29
_cod_database_code               7135181
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.214
_olex2_refinement_description
;
1. Fixed Uiso
 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 1.4A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.4A
All non-hydrogen atoms have similar U: within 0.4A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 0.4A
3. Rigid body (RIGU) restrains
 C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Same fragment restrains
{C12, C13, C14, C15, C11} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C11, C12, C13, C14, C15}
{C11, C12, C13, C14, C15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C11A, C12A, C13A, C14A, C15A}
{C16, C17, C18, C19, C20} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C16A, C17A, C18A, C19A, C20A}
{C17, C18, C19, C20, C16} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C16, C17, C18, C19, C20}
5. Others
 Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=Sof(C15A)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=FVAR(1)
6.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), C16A(H16D,H16E,H16F), C17A(H17D,H17E,
 H17F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F)
;
_shelx_res_checksum              15961
_olex2_submission_original_sample_id matkp29
_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 2.165
_oxdiff_exptl_absorpt_empirical_full_min 0.632