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_7716708
_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
'C84 H126 O7 U2, C16 H32 Li O4, 2(C6 H14), 2(C4 H8 O)'
_chemical_formula_sum            'C120 H202 Li O13 U2'
_chemical_formula_weight         2335.80
_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             2024-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-12 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                102.1051(10)
_cell_angle_beta                 97.5370(10)
_cell_angle_gamma                95.7018(11)
_cell_formula_units_Z            2
_cell_length_a                   14.9084(2)
_cell_length_b                   19.4995(2)
_cell_length_c                   21.0862(2)
_cell_measurement_reflns_used    33211
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      76.0010
_cell_measurement_theta_min      4.1350
_cell_volume                     5890.70(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.108a 64-bit (release 14-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(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 0.970
_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   -115.00 -20.00   1.00    1.00    --  -40.85 -41.00-164.00   95
  2  \w      2.00  33.00   1.00    1.00    --  -40.85  41.00 -11.00   31
  3  \w     16.00 115.00   1.00    1.00    --   40.85  41.00 -11.00   99
  4  \w      0.00  45.00   1.00    1.00    --   40.85 -41.00-164.00   45
  5  \w     88.00 178.00   1.00    4.00    --  112.00  41.00 -11.00   90
  6  \w     63.00 112.00   1.00    4.00    --  112.00 -41.00-164.00   49
  7  \w    -66.00  -7.00   1.00    1.00    --  -40.85 125.00  60.00   59
  8  \w     14.00 113.00   1.00    1.00    --   40.85  57.00  90.00   99
  9  \w     -4.00  39.00   1.00    1.00    --   40.85 -38.00  90.00   43
 10  \w     27.00  95.00   1.00    1.00    --   40.85-125.00-120.00   68
 11  \w     27.00  83.00   1.00    1.00    --   40.85-125.00  60.00   56
 12  \w    103.00 176.00   1.00    4.00    --  112.00  77.00 -60.00   73
 13  \w    113.00 144.00   1.00    4.00    --  112.00  45.00-120.00   31
 14  \w     42.00 137.00   1.00    4.00    --  112.00 -45.00 -60.00   95
 15  \w     78.00 109.00   1.00    4.00    --  112.00-111.00-180.00   31
 16  \w     40.00 109.00   1.00    4.00    --  112.00-111.00 -60.00   69
 17  \w    125.00 152.00   1.00    4.00    --  112.00  77.00-180.00   27
 18  \w    105.00 173.00   1.00    4.00    --  112.00 111.00  60.00   68
 19  \w    104.00 144.00   1.00    4.00    --  112.00  77.00  60.00   40
 20  \w     41.00  68.00   1.00    4.00    --  112.00-111.00 120.00   27
 21  \w     69.00 109.00   1.00    4.00    --  112.00-111.00   0.00   40
 22  \w     29.00  82.00   1.00    4.00    --  112.00 -94.00-150.00   53
 23  \w     40.00 109.00   1.00    4.00    --  112.00-111.00  90.00   69
 24  \w     69.00  98.00   1.00    4.00    --  112.00 -94.00  30.00   29
 25  \w     41.00 108.00   1.00    4.00    --  112.00-111.00  30.00   67
 26  \w     85.00 178.00   1.00    4.00    --  112.00  30.00  60.00   93
 27  \w    105.00 133.00   1.00    4.00    --  112.00 111.00 -90.00   28
 28  \w    147.00 174.00   1.00    4.00    --  112.00 111.00 -90.00   27
 29  \w     30.00  57.00   1.00    4.00    --  112.00 -94.00 120.00   27
 30  \w     79.00 105.00   1.00    4.00    --  112.00 -94.00 120.00   26
 31  \w     84.00 141.00   1.00    4.00    --  112.00  61.00 150.00   57
 32  \w    124.00 169.00   1.00    4.00    --  112.00  30.00  30.00   45
 33  \w     81.00 108.00   1.00    4.00    --  112.00-111.00 120.00   27
 34  \w     29.00  74.00   1.00    4.00    --  112.00 -94.00-120.00   45
 35  \w     50.00 109.00   1.00    4.00    --  112.00-111.00 -90.00   59
 36  \w     75.00 103.00   1.00    4.00    --  112.00-111.00 -30.00   28
 37  \w     51.00 107.00   1.00    4.00    --  112.00 -94.00-180.00   56
 38  \w    105.00 168.00   1.00    4.00    --  112.00 111.00  90.00   63
 39  \w    108.00 135.00   1.00    4.00    --  112.00  77.00 -90.00   27
 40  \w    148.00 173.00   1.00    4.00    --  112.00  77.00 -90.00   25
 41  \w     38.00  65.00   1.00    4.00    --  112.00 -94.00  90.00   27
 42  \w     65.00 133.00   1.00    4.00    --  112.00 178.00-150.00   68
;
_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      -0.0821137000
_diffrn_orient_matrix_UB_12      0.0420780000
_diffrn_orient_matrix_UB_13      -0.0015911000
_diffrn_orient_matrix_UB_21      -0.0472026000
_diffrn_orient_matrix_UB_22      -0.0474732000
_diffrn_orient_matrix_UB_23      0.0390694000
_diffrn_orient_matrix_UB_31      0.0456472000
_diffrn_orient_matrix_UB_32      0.0511707000
_diffrn_orient_matrix_UB_33      0.0647615000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28682
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.497
_diffrn_reflns_theta_min         2.808
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.110
_exptl_absorpt_correction_T_max  0.377
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.109a (Rigaku Oxford Diffraction, 2024)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       prism
_exptl_crystal_F_000             2426
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.206
_refine_diff_density_max         1.756
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1542
_refine_ls_number_reflns         28682
_refine_ls_number_restraints     1401
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0949P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24674
_reflns_number_total             28682
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9855\% 
around [1.00 -0.00 -0.00] (reciprocal) or [0.99 0.10 0.11] (direct)
;
_cod_data_source_file            d4dt01819b2.cif
_cod_data_source_block           ah739
_cod_depositor_comments
'Adding full bibliography for 7716706--7716710.cif.'
_cod_database_code               7716708
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C120 H202 Li1 O13 U2'
_shelx_estimated_absorpt_t_max   0.286
_shelx_estimated_absorpt_t_min   0.130
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8790(11)
 0.1210(11)
2. 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
3. Restrained distances
 C107-C106
 1.54 with sigma of 0.02
 O16-C113
 1.43 with sigma of 0.02
 C110-C111
 1.54 with sigma of 0.02
 O11-Li1 \\sim O15-Li1 \\sim O12-Li1 \\sim O16-Li1 \\sim O9-Li1 \\sim O13-Li1
\\sim O14-Li1 \\sim O10-Li1
 with sigma of 0.02
 O9-C88 \\sim O9-C85 \\sim O13-C104 \\sim O13-C101 \\sim O15-C108 \\sim
O15-C105 \\sim O11-C96 \\sim O11-
 C93 \\sim O10-C89 \\sim O10-C92 \\sim O14-C112 \\sim O14-C109 \\sim O16-C113
\\sim O16-C116 \\sim O12-C100
 \\sim O12-C97
 with sigma of 0.02
 C103-C104 \\sim C102-C103 \\sim C102-C101 \\sim C85-C86 \\sim C86-C87 \\sim
C88-C87 \\sim C108-C107 ~
 C107-C106 \\sim C94-C93 \\sim C105-C106 \\sim C95-C96 \\sim C94-C95 \\sim
C90-C89 \\sim C91-C92 \\sim C91-
 C90 \\sim C110-C109 \\sim C112-C111 \\sim C114-C113 \\sim C115-C114 \\sim
C100-C99 \\sim C115-C116 ~
 C98-C97 \\sim C98-C99
 with sigma of 0.02
 O20-C129 \\sim O19-C128 \\sim O20-C132 \\sim O19-C125
 with sigma of 0.02
 C126-C125 \\sim C126-C127 \\sim C128-C127 \\sim C130-C129 \\sim C131-C130
\\sim C131-C132
 with sigma of 0.02
 O17-C117 \\sim O18-C121 \\sim O17-C120 \\sim O18-C124
 with sigma of 0.02
 C121-C122 \\sim C118-C117 \\sim C122-C123 \\sim C119-C118 \\sim C124-C123
\\sim C119-C120
 with sigma of 0.02
 C120-C117 \\sim C124-C121
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim
C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim
C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100
\\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107
\\sim C108 \\sim C109 \\sim C110 \\sim C111 \\sim C112 \\sim C113 \\sim C114
\\sim C115 \\sim C116 \\sim Li1: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
O17 \\sim C117 \\sim C118 \\sim C119 \\sim C120 \\sim O18 \\sim C121 \\sim C122
\\sim C123 \\sim C124 \\sim O19 \\sim C125 \\sim C126 \\sim C127 \\sim C128
\\sim O20 \\sim C129 \\sim C130 \\sim C131 \\sim C132: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
5. Others
 Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=Sof(C101)=Sof(H10F)=Sof(H10G)=Sof(C102)=
 Sof(H10H)=Sof(H10I)=Sof(C103)=Sof(H10J)=Sof(H10K)=Sof(C104)=Sof(H10L)=
 Sof(H10M)=Sof(C105)=Sof(H10N)=Sof(H10O)=Sof(C106)=Sof(H10P)=Sof(H10Q)=
 Sof(C107)=Sof(H10R)=Sof(H10S)=Sof(C108)=Sof(H10T)=Sof(H10U)=Sof(C109)=
 Sof(H10V)=Sof(H10W)=Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(C111)=Sof(H11C)=
 Sof(H11D)=Sof(C112)=Sof(H11E)=Sof(H11F)=Sof(C113)=Sof(H11G)=Sof(H11H)=
 Sof(C114)=Sof(H11I)=Sof(H11J)=Sof(C115)=Sof(H11K)=Sof(H11L)=Sof(C116)=
 Sof(H11M)=Sof(H11N)=1-FVAR(1)
 Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=
 Sof(H86A)=Sof(H86B)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=
 Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(C91)=Sof(H91A)=
 Sof(H91B)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=
 Sof(H94A)=Sof(H94B)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=
 Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=
 Sof(H99B)=Sof(C100)=Sof(H10D)=Sof(H10E)=FVAR(1)
 Sof(O18)=Sof(C121)=Sof(H12F)=Sof(H12G)=Sof(C122)=Sof(H12H)=Sof(H12I)=
 Sof(C123)=Sof(H12J)=Sof(H12K)=Sof(C124)=Sof(H12L)=Sof(H12M)=1-FVAR(2)
 Sof(O17)=Sof(C117)=Sof(H11O)=Sof(H11P)=Sof(C118)=Sof(H11Q)=Sof(H11R)=
 Sof(C119)=Sof(H11S)=Sof(H11T)=Sof(C120)=Sof(H12D)=Sof(H12E)=FVAR(2)
 Sof(O20)=Sof(C129)=Sof(H12V)=Sof(H12W)=Sof(C130)=Sof(H13U)=Sof(H13V)=
 Sof(C131)=Sof(H13W)=Sof(H13X)=Sof(C132)=Sof(H13Y)=Sof(H)=1-FVAR(3)
 Sof(O19)=Sof(C125)=Sof(H12N)=Sof(H12O)=Sof(C126)=Sof(H12P)=Sof(H12Q)=
 Sof(C127)=Sof(H12R)=Sof(H12S)=Sof(C128)=Sof(H12T)=Sof(H12U)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,
 H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B),
 C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B),
  C99(H99A,H99B), C100(H10D,H10E), C101(H10F,H10G), C102(H10H,H10I), C103(H10J,
 H10K), C104(H10L,H10M), C105(H10N,H10O), C106(H10P,H10Q), C107(H10R,H10S),
 C108(H10T,H10U), C109(H10V,H10W), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,
 H11F), C113(H11G,H11H), C114(H11I,H11J), C115(H11K,H11L), C116(H11M,H11N),
 C117(H11O,H11P), C118(H11Q,H11R), C119(H11S,H11T), C120(H12D,H12E), C121(H12F,
 H12G), C122(H12H,H12I), C123(H12J,H12K), C124(H12L,H12M), C125(H12N,H12O),
 C126(H12P,H12Q), C127(H12R,H12S), C128(H12T,H12U), C129(H12V,H12W), C130(H13U,
 H13V), C131(H13W,H13X), C132(H13Y,H), C134(H13G,H13H), C135(H13I,H13J),
 C136(H13K,H13L), C137(H13M,H13N), C140(H14D,H14E), C141(H14F,H14G), C142(H14H,
 H14I), C143(H14J,H14K)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C17(H17), C18(H18), C19(H19), C31(H31), C32(H32),
 C33(H33), C45(H45), C46(H46), C47(H47), C59(H59), C60(H60), C61(H61), C73(H73),
  C74(H74), C75(H75)
6.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), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,
 H70C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C82(H82A,
 H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C133(H13D,H13E,H13F),
 C138(H13O,H13P,H13Q), C139(H13R,H13S,H13T), C144(H14L,H14M,H14N)
;
_shelx_res_checksum              40224
_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 22.150
_oxdiff_exptl_absorpt_empirical_full_min 0.203
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2