Synthesis, structure and redox properties of single-atom bridged diuranium complexes supported by aryloxides.
Hsueh, Fang-Che; Barluzzi, Luciano; Rajeshkumar, Thayalan; Scopelliti, Rosario; Zivkovic, Ivica; Maron, Laurent; Mazzanti, Marinella; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13416–13426; doi:10.1039/d4dt01819b

data_7716707
_publ_section_title
;
 Synthesis, structure and redox properties of single-atom bridged
 diuranium complexes supported by aryloxides.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13416
_journal_page_last               13426
_journal_paper_doi               10.1039/d4dt01819b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C88 H148 K2 O12 S2 U2'
_chemical_formula_sum            'C88 H148 K2 O12 S2 U2'
_chemical_formula_weight         2016.44
_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             2021-05-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-06-12 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                93.7454(9)
_cell_angle_beta                 113.9243(10)
_cell_angle_gamma                98.2448(8)
_cell_formula_units_Z            1
_cell_length_a                   13.70485(13)
_cell_length_b                   14.20424(13)
_cell_length_c                   15.06289(17)
_cell_measurement_reflns_used    38029
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      72.3890
_cell_measurement_theta_min      3.6820
_cell_volume                     2627.79(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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    -78.00  22.00   1.00    2.00    --  -40.91  93.00  47.00  100
  2  \w     -1.00  64.00   1.00    2.00    --   40.91 -93.00 -64.00   65
  3  \w     78.00 106.00   1.00    8.00    --  105.15 -93.00 -64.00   28
  4  \w    141.00 166.00   1.00    8.00    --  105.15  93.00  47.00   25
  5  \w     -4.00  21.00   1.00    2.00    --   34.00  92.00-134.20   25
  6  \w   -114.00 -17.00   1.00    2.00    --  -40.91 -38.00 -90.00   97
  7  \w     28.00  91.00   1.00    2.00    --   40.91-125.00-180.00   63
  8  \w     18.00 114.00   1.00    2.00    --   40.91  38.00   0.00   96
  9  \w     46.00 113.00   1.00    2.00    --   40.91  57.00  90.00   67
 10  \w      8.00  33.00   1.00    2.00    --   40.91  79.00  69.33   25
 11  \w     13.00  40.00   1.00    2.00    --   40.91  57.00  90.00   27
 12  \w      7.00  33.00   1.00    2.00    --   42.00  84.00 139.54   26
 13  \w     14.00  41.00   1.00    2.00    --   46.00  81.00  35.07   27
 14  \w     17.00  42.00   1.00    2.00    --   50.00  81.00  56.39   25
 15  \w     16.00  41.00   1.00    2.00    --   50.00  82.00-174.79   25
 16  \w     16.00  42.00   1.00    2.00    --   50.00  82.00   7.54   26
 17  \w     16.00  42.00   1.00    2.00    --   50.00  82.00 -65.32   26
 18  \w     16.00  41.00   1.00    2.00    --   50.00  82.00 101.71   25
 19  \w     16.00  41.00   1.00    2.00    --   50.00  81.00-112.18   25
 20  \w     31.00  77.00   1.00    2.00    --   62.00  71.00 113.62   46
 21  \w     33.00  65.00   1.00    2.00    --   62.00  71.00-104.91   32
 22  \w     31.00  84.00   1.00    2.00    --   62.00  71.00-178.16   53
 23  \w     31.00  58.00   1.00    2.00    --   62.00  69.00  67.27   27
 24  \w     36.00  61.00   1.00    2.00    --   66.00  70.00 151.42   25
 25  \w     35.00  62.00   1.00    2.00    --   66.00  71.00  76.21   27
 26  \w     39.00  65.00   1.00    2.00    --   70.00  71.00 -35.91   26
 27  \w     39.00  75.00   1.00    2.00    --   70.00  69.00-142.46   36
 28  \w    117.00 144.00   1.00    2.00    --   70.00  71.00 -35.91   27
 29  \w     43.00  70.00   1.00    8.00    --   74.00  69.00 -83.30   27
 30  \w    110.00 137.00   1.00    8.00    --   74.00  70.00  -4.56   27
 31  \w     43.00  70.00   1.00    8.00    --   74.00  70.00  -4.56   27
 32  \w     47.00  73.00   1.00    8.00    --   78.00  71.00  10.33   26
 33  \w     96.00 150.00   1.00    8.00    --   78.00  71.00  10.33   54
 34  \w     53.00  80.00   1.00    8.00    --   82.00  61.00 114.96   27
 35  \w     51.00  77.00   1.00    8.00    --   82.00  69.00 143.32   26
 36  \w    108.00 135.00   1.00    8.00    --   82.00  68.00 -64.93   27
 37  \w     52.00  78.00   1.00    8.00    --   82.00  68.00 -64.93   26
 38  \w     52.00  80.00   1.00    8.00    --   82.00  70.00-139.79   28
 39  \w     56.00  83.00   1.00    8.00    --   86.00  65.00 -27.19   27
 40  \w     60.00  86.00   1.00    8.00    --   90.00  68.00-122.91   26
 41  \w     60.00  86.00   1.00    8.00    --   90.00  68.00  77.77   26
 42  \w     62.00  98.00   1.00    8.00    --   90.00  60.00  36.30   36
 43  \w     61.00 126.00   1.00    8.00    --   90.00  61.00 132.88   65
 44  \w     59.00 146.00   1.00    8.00    --   90.00  71.00 160.95   87
 45  \w     66.00  91.00   1.00    8.00    --   94.00  63.00 -65.24   25
 46  \w    123.00 150.00   1.00    8.00    --  105.15  61.00-180.00   27
 47  \w     77.00 104.00   1.00    8.00    --  105.15  61.00-180.00   27
 48  \w     39.00 133.00   1.00    8.00    --  105.15 -61.00-150.00   94
 49  \w     77.00 115.00   1.00    8.00    --  105.15  61.00 -90.00   38
 50  \w     76.00 174.00   1.00    8.00    --  105.15  61.00 -30.00   98
 51  \w    119.00 176.00   1.00    8.00    --  105.15  61.00 150.00   57
 52  \w     77.00 111.00   1.00    8.00    --  105.15  61.00 150.00   34
 53  \w     75.00 123.00   1.00    8.00    --  105.15  68.00-173.72   48
 54  \w     76.00 176.00   1.00    8.00    --  105.15  61.00   0.00  100
 55  \w     80.00 177.00   1.00    8.00    --  105.15  61.00-150.00   97
 56  \w     38.00 109.00   1.00    8.00    --  105.15-111.00  30.00   71
 57  \w    117.00 154.00   1.00    8.00    --  105.15  61.00 -60.00   37
 58  \w     80.00 114.00   1.00    8.00    --  105.15  61.00 -60.00   34
 59  \w     76.00 176.00   1.00    8.00    --  105.15  61.00  41.96  100
 60  \w    112.00 163.00   1.00    8.00    --  105.15  61.00 120.00   51
 61  \w     76.00 104.00   1.00    8.00    --  105.15  61.00 120.00   28
 62  \w    110.00 172.00   1.00    8.00    --  105.15  66.00-118.37   62
 63  \w    119.00 177.00   1.00    8.00    --  105.15  61.00 -90.00   58
 64  \w     76.00 101.00   1.00    8.00    --  105.15  66.00-118.37   25
 65  \w     79.00 109.00   1.00    8.00    --  105.15-111.00 -90.00   30
 66  \w     79.00 105.00   1.00    8.00    --  105.15 -94.00-180.00   26
 67  \w     23.00 106.00   1.00    8.00    --  105.15 -94.00  60.00   83
 68  \w     24.00  62.00   1.00    8.00    --  105.15 -94.00-180.00   38
 69  \w     78.00 168.00   1.00    8.00    --  105.15  61.00  90.00   90
 70  \w     36.00 138.00   1.00    8.00    --  105.15 -77.00  90.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0341220000
_diffrn_orient_matrix_UB_12      -0.1011457000
_diffrn_orient_matrix_UB_13      -0.0588523000
_diffrn_orient_matrix_UB_21      -0.1182304000
_diffrn_orient_matrix_UB_22      0.0155144000
_diffrn_orient_matrix_UB_23      -0.0492875000
_diffrn_orient_matrix_UB_31      0.0228867000
_diffrn_orient_matrix_UB_32      0.0420350000
_diffrn_orient_matrix_UB_33      -0.0828484000
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50894
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.542
_diffrn_reflns_theta_min         3.173
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.062
_exptl_absorpt_correction_T_max  0.525
_exptl_absorpt_correction_T_min  0.083
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.204
_refine_diff_density_max         1.405
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         10292
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+2.1563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9756
_reflns_number_total             10292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01819b2.cif
_cod_data_source_block           ah109
_cod_depositor_comments
'Adding full bibliography for 7716706--7716710.cif.'
_cod_database_code               7716707
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H84 O7 K1 S1 U1'
_shelx_estimated_absorpt_t_max   0.233
_shelx_estimated_absorpt_t_min   0.131
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-C53 \\sim O8-C56 \\sim O7-C49 \\sim O7-C52
 with sigma of 0.02
 C53-C54 \\sim C49-C50 \\sim C50-C51 \\sim C55-C54 \\sim C55-C56 \\sim C52-C51
 with sigma of 0.02
 O4-C36 \\sim O4-C40 \\sim O4-C33 \\sim O4-C37
 with sigma of 0.02
 C37-C38 \\sim C33-C34 \\sim C39-C38 \\sim C35-C34 \\sim C36-C35 \\sim C39-C40
 with sigma of 0.02
 O6-C44 \\sim O6-C41 \\sim O5-C45 \\sim O5-C48
 with sigma of 0.02
 C44-C47 \\sim C48-C43 \\sim C47-C42 \\sim C46-C43 \\sim C42-C41 \\sim C45-C46
 with sigma of 0.02
 O6-C48 \\sim O5-C44 \\sim O6-C45 \\sim O5-C41
 with sigma of 0.02
 C44-C43 \\sim C47-C48 \\sim C42-C43 \\sim C47-C46 \\sim C45-C46 \\sim C42-C41
 with sigma of 0.02
 K1-O5 \\sim K1-O6 \\sim K1-O8 \\sim K1-O7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O7 \\sim O8 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim
C55 \\sim C56: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
O4 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim
C40: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
O5 \\sim O6 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim
C47 \\sim C48: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
4. Others
 Sof(O8)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=
 Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=1-FVAR(1)
 Sof(O7)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=FVAR(1)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=1-FVAR(2)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(2)
 Sof(O6)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=
 Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=1-FVAR(3)
 Sof(O5)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=
 Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(3)
 Fixed X: U1(0.59015)
 Fixed Y: U1(0.11601)
 Fixed Z: U1(0.584709)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C17(H17), C18(H18), C19(H19)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 83 electrons were 
found in a volume of 386\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H8O], 1[C4H10O] per Asymmetric Unit 
which account for 82 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47400
_shelx_fab_checksum              1219
_olex2_date_sample_data_collection 2021-05-07
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.298
_oxdiff_exptl_absorpt_empirical_full_min 0.546