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The structure of a new type of polyoxo cluster complex that contains thirteen uranium atoms, {U13}, is reported. The complex crystallized from methanol containing tetra­valent uranium (UIV) with a basic organic ligand, and was characterized as di­chloridoocta­cosa-μ2-methano­lato-octa­kis­(methano­lato)octa-μ4-oxido-trideca­uranium, [U13(CH3O)35.7Cl2.3O8] or [U134-Ooxo)8Clx(MeO)38–x] (x = 2.3, MeO = methoxide) (I), by single-crystal X-ray diffraction. The characterized {U13} polyoxo cluster complex (I) possesses a single cubic uranium polyhedron at the centre of the cluster core. To the best of our knowledge, this is the very first example of a polyoxo actinide complex that bears a single cubic polyhedron in its structure. The cubic polyhedron in I is well comparable in shape with those in bulk UO2. The U—O bonds in the cubic polyhedron of I are, however, significantly shorter than those not only in bulk UO2 but also in another analogue in the {U38} cluster. This shortening of U—O bonds, together with BVS calculations and the overall negative charge (2−) of I, suggests that the central uranium atom in I, which forms the single cubic coordination polyhedron, is presumably oxidized to the penta­valent state (UV) from the original tetra­valent state (UIV). Complex I is, hence, the first example of a polyoxo cluster possessing a single cubic coordination polyhedron of UV.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989021007623/yz2009sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989021007623/yz2009Isup2.hkl
Contains datablock I

mol

MDL mol file https://doi.org/10.1107/S2056989021007623/yz2009Isup3.mol
Supplementary material

CCDC reference: 2069007

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](O-C) = 0.027 Å
  • Disorder in main residue
  • R factor = 0.038
  • wR factor = 0.103
  • Data-to-parameter ratio = 15.0

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT971_ALERT_2_A Check Calcd Resid. Dens. 0.87A From U4 5.16 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_A Check Calcd Resid. Dens.  0.81A   From U5              4.04 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement

Alert level B PLAT971_ALERT_2_B Check Calcd Resid. Dens. 0.89A From U2 3.22 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_B Check Calcd Resid. Dens.  2.12A   From C7              3.21 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_B Check Calcd Resid. Dens.  0.84A   From U3              3.20 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_B Check Calcd Resid. Dens.  0.93A   From U1              2.61 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_B Check Calcd Resid. Dens.  0.93A   From U1              2.55 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_B Check Calcd Resid. Dens.  1.05A   From C16             2.51 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT972_ALERT_2_B Check Calcd Resid. Dens.  0.65A   From U5             -3.20 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_B Check Calcd Resid. Dens.  2.01A   From C9             -3.13 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_B Check Calcd Resid. Dens.  0.72A   From U4             -3.04 eA-3
Author Response: See PLAT 971

Alert level C PLAT077_ALERT_4_C Unitcell Contains Non-integer Number of Atoms .. Please Check PLAT220_ALERT_2_C NonSolvent Resd 1 O Ueq(max)/Ueq(min) Range 3.1 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) U3 --O4 . 7.3 s.u. PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) U7 --O14 . 7.1 s.u. PLAT234_ALERT_4_C Large Hirshfeld Difference O14 --C14 . 0.17 Ang. PLAT234_ALERT_4_C Large Hirshfeld Difference O16 --C16 . 0.25 Ang. PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of O5 Check PLAT412_ALERT_2_C Short Intra XH3 .. XHn H5B ..H8A . 1.82 Ang. x,y,z = 1_555 Check PLAT413_ALERT_2_C Short Inter XH3 .. XHn H1MB ..H14B . 2.14 Ang. 2-x,1-y,1-z = 2_766 Check PLAT601_ALERT_2_C Unit Cell Contains Solvent Accessible VOIDS of . 66 Ang   3 PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min). 7 Note PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L= 0.595 4 Report PLAT971_ALERT_2_C Check Calcd Resid. Dens. 0.91A From U7 2.31 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.94A   From U6              1.93 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  1.49A   From C11             1.92 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  1.03A   From U7              1.77 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  1.37A   From C13             1.55 eA-3
Author Response: Presumably due to fourier series truncation errors and disorder between methoxide and chloride; see _publ_section_expl_refinement
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  1.67A   From C7             -2.28 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.63A   From U3             -2.13 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.76A   From C16            -1.81 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.81A   From U5             -1.79 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  1.99A   From C9             -1.74 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.93A   From U2             -1.72 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  1.70A   From C11            -1.58 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  1.61A   From C5             -1.55 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.74A   From C16            -1.54 eA-3
Author Response: See PLAT 971
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.67A   From C16            -1.51 eA-3
Author Response: See PLAT 971
PLAT977_ALERT_2_C Check Negative Difference Density on H5A              -0.40 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H7C              -0.69 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H11C             -0.35 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H12A             -0.49 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H12B             -0.41 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H13C             -0.32 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H14B             -0.38 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H15A             -0.55 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H16A             -0.48 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H16C             -0.52 eA-3

Alert level G PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 12 Note PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ... 17 Report PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large 70.43 Why ? PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note) 0.002 Degree PLAT175_ALERT_4_G The CIF-Embedded .res File Contains SAME Records 2 Report PLAT177_ALERT_4_G The CIF-Embedded .res File Contains DELU Records 4 Report PLAT178_ALERT_4_G The CIF-Embedded .res File Contains SIMU Records 4 Report PLAT301_ALERT_3_G Main Residue Disorder ..............(Resd 1 ) 10% Note PLAT304_ALERT_4_G Non-Integer Number of Atoms in ..... (Resd 1 ) 201.64 Check PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 9 Note PLAT794_ALERT_5_G Tentative Bond Valency for U2 (IV) . 4.07 Info PLAT794_ALERT_5_G Tentative Bond Valency for U3 (IV) . 4.44 Info PLAT794_ALERT_5_G Tentative Bond Valency for U6 (V) . 4.76 Info PLAT794_ALERT_5_G Tentative Bond Valency for U7 (IV) . 4.02 Info PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 145 Note PLAT909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still 72% Note PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ... 1 Note
2 ALERT level A = Most likely a serious problem - resolve or explain 9 ALERT level B = A potentially serious problem, consider carefully 37 ALERT level C = Check. Ensure it is not caused by an omission or oversight 17 ALERT level G = General information/check it is not something unexpected 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 47 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 8 ALERT type 4 Improvement, methodology, query or suggestion 4 ALERT type 5 Informative message, check

Computing details top

Data collection: SAINT (Bruker, 2016); cell refinement: APEX3 (Bruker, 2016); data reduction: SAINT (Bruker, 2016); program(s) used to solve structure: SHELXT2014/5 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2015b); molecular graphics: shelXle (Hübschle et al., 2011).

Dichloridooctacosa-µ2-methanolato-octakis(methanolato)octa-µ4-oxido-\ tridecauranium top
Crystal data top
[U13(CH3O)35.7Cl2.3O8]Z = 1
Mr = 4412.01F(000) = 1906
Triclinic, P1Dx = 3.539 Mg m3
a = 12.8598 (6) ÅMo Kα radiation, λ = 0.71073 Å
b = 14.0014 (6) ÅCell parameters from 529 reflections
c = 14.6311 (6) Åθ = 2.2–29.1°
α = 117.339 (2)°µ = 25.48 mm1
β = 113.186 (2)°T = 100 K
γ = 92.373 (2)°Block, black
V = 2069.95 (16) Å30.12 × 0.11 × 0.08 mm
Data collection top
Bruker D8 Venture
diffractometer
6185 reflections with I > 2σ(I)
Detector resolution: 10.4167 pixels mm-1Rint = 0.052
generic φ and ο scansθmax = 25.0°, θmin = 2.7°
Absorption correction: multi-scan
(Krause et al., 2015)
h = 1515
Tmin = 0.394, Tmax = 0.746k = 1616
55319 measured reflectionsl = 1717
7304 independent reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.103H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0373P)2 + 70.429P]
where P = (Fo2 + 2Fc2)/3
7304 reflections(Δ/σ)max = 0.001
488 parametersΔρmax = 5.02 e Å3
145 restraintsΔρmin = 3.41 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
U10.69331 (4)0.29727 (4)0.47526 (4)0.01860 (12)
Cl10.8241 (9)0.1509 (8)0.4746 (9)0.035 (3)0.43 (2)
O1M0.785 (2)0.1771 (16)0.4625 (19)0.030 (4)0.57 (2)
C1M0.841 (2)0.098 (2)0.458 (3)0.036 (5)0.57 (2)
H1MA0.8065130.0502670.4775920.054*0.57 (2)
H1MB0.9243800.1325150.5141460.054*0.57 (2)
H1MC0.8322970.0517650.3797360.054*0.57 (2)
U40.64636 (4)0.81258 (4)0.69281 (4)0.01947 (12)
Cl30.7477 (10)1.0349 (10)0.8252 (9)0.040 (4)0.41 (2)
O3M0.7246 (19)0.9836 (15)0.7937 (19)0.032 (4)0.59 (2)
C3M0.781 (3)1.092 (2)0.860 (3)0.049 (7)0.59 (2)
H3MA0.8455761.1058520.8436240.074*0.59 (2)
H3MB0.8135851.1153150.9421530.074*0.59 (2)
H3MC0.7265481.1355210.8430280.074*0.59 (2)
U50.83654 (4)0.60227 (4)0.66263 (4)0.02061 (12)
Cl21.0679 (11)0.6808 (10)0.7997 (11)0.026 (4)0.33 (2)
O2M1.0187 (16)0.6605 (18)0.7652 (17)0.031 (4)0.67 (2)
C2M1.1339 (19)0.710 (2)0.841 (2)0.038 (5)0.67 (2)
H2MA1.1583160.6840200.8958570.056*0.67 (2)
H2MB1.1473840.7910020.8827190.056*0.67 (2)
H2MC1.1797290.6899260.7977590.056*0.67 (2)
C10.6604 (16)0.1259 (13)0.2091 (13)0.042 (4)
H1A0.5803110.0762970.1575100.062*
H1B0.7082470.0948770.2537490.062*
H1C0.6948740.1326140.1626080.062*
O10.6573 (9)0.2307 (8)0.2848 (8)0.027 (2)
U20.53611 (4)0.33105 (4)0.22261 (4)0.01968 (12)
C20.5492 (17)0.1741 (14)0.0359 (14)0.047 (4)
H2A0.6045960.2214690.0388600.071*
H2B0.4717590.1480960.1029950.071*
H2C0.5773770.1096800.0375170.071*
O20.5407 (9)0.2342 (8)0.0640 (8)0.034 (2)
O30.3774 (9)0.3831 (8)0.1168 (7)0.028 (2)
U30.33989 (4)0.53469 (4)0.24238 (4)0.01995 (12)
C30.3303 (17)0.3378 (14)0.0051 (12)0.045 (4)
H3A0.2594050.2763130.0464280.068*
H3B0.3888270.3096620.0298740.068*
H3C0.3103850.3960910.0228610.068*
C40.176 (2)0.564 (2)0.0362 (19)0.072 (7)
H4A0.2109640.5677960.0112110.109*
H4B0.1525550.6317910.0700490.109*
H4C0.1075570.4986540.0125610.109*
O40.2354 (11)0.5561 (10)0.0995 (11)0.050 (3)
C50.299 (3)0.7886 (17)0.341 (2)0.079 (7)
H5A0.3551970.7979340.3147250.119*
H5B0.3165290.8569050.4145660.119*
H5C0.2189740.7739960.2826630.119*
O50.3068 (9)0.6959 (8)0.3598 (8)0.031 (2)
U60.5000000.5000000.5000000.01170 (13)
C60.5010 (17)0.7108 (18)0.2245 (17)0.055 (5)
H6A0.5293740.6710080.1679160.082*
H6B0.5525640.7869310.2808030.082*
H6C0.4207950.7137130.1839900.082*
O60.5011 (9)0.6532 (8)0.2841 (8)0.030 (2)
O80.4733 (8)0.8554 (8)0.6182 (8)0.028 (2)
U70.67893 (4)0.63767 (4)0.41143 (4)0.01923 (12)
C70.674 (2)0.9055 (14)0.5289 (17)0.056 (5)
H7A0.6727160.8820380.4540180.085*
H7B0.7460830.9654250.5916350.085*
H7C0.6054580.9327100.5297030.085*
O70.6722 (9)0.8130 (7)0.5454 (8)0.031 (2)
C80.4640 (16)0.9651 (13)0.6393 (19)0.055 (5)
H8A0.3997520.9581810.5701640.083*
H8B0.5379771.0083200.6563400.083*
H8C0.4479801.0032780.7056120.083*
C90.6967 (15)0.8979 (12)0.9640 (12)0.038 (4)
H9A0.7583410.8673070.9969000.057*
H9B0.6496110.9153291.0054380.057*
H9C0.7329220.9661740.9720650.057*
O90.6228 (8)0.8175 (7)0.8437 (7)0.027 (2)
O100.8303 (9)0.7880 (8)0.7769 (8)0.031 (2)
C100.9266 (13)0.8800 (13)0.8746 (14)0.041 (4)
H10A1.0004380.8608630.8801820.062*
H10B0.9214940.8973870.9454240.062*
H10C0.9242500.9451630.8655980.062*
O110.8253 (9)0.5933 (8)0.8157 (8)0.030 (2)
C110.9024 (16)0.6711 (15)0.9356 (13)0.048 (4)
H11A0.9740370.7089510.9437030.072*
H11B0.9228560.6313070.9777920.072*
H11C0.8632040.7264830.9677940.072*
O120.8746 (9)0.4274 (8)0.6120 (9)0.032 (2)
C120.9709 (14)0.4066 (14)0.6837 (16)0.051 (5)
H12A0.9747630.4378530.7605100.077*
H12B1.0439060.4418310.6916640.077*
H12C0.9606440.3258870.6484040.077*
O130.8658 (9)0.6767 (8)0.5580 (9)0.031 (2)
C130.9615 (15)0.7636 (15)0.6003 (15)0.046 (4)
H13A0.9631140.7664120.5351970.069*
H13B1.0346090.7504420.6424510.069*
H13C0.9536930.8347560.6530220.069*
O140.7675 (11)0.7281 (10)0.3648 (9)0.045 (3)
C140.8158 (16)0.7802 (17)0.3389 (18)0.062 (6)
H14A0.8343640.7285770.2781840.093*
H14B0.8885920.8342290.4075670.093*
H14C0.7636660.8198790.3100970.093*
O150.6499 (9)0.4803 (8)0.2400 (8)0.027 (2)
C150.6596 (19)0.4833 (15)0.1523 (15)0.054 (5)
H15A0.6898020.4214270.1148540.082*
H15B0.7139030.5544080.1836150.082*
H15C0.5822260.4761640.0951230.082*
O160.7331 (8)0.4585 (8)0.4341 (8)0.027 (2)
C160.8348 (19)0.4483 (16)0.4207 (16)0.063 (6)
H16A0.8314140.3690290.3783680.094*
H16B0.9040290.4860890.4973370.094*
H16C0.8401620.4826100.3768800.094*
O170.6641 (8)0.4672 (7)0.5997 (7)0.0200 (18)
O180.5061 (8)0.5022 (7)0.3469 (7)0.0191 (18)
O190.4861 (7)0.6687 (7)0.6212 (7)0.0168 (17)
O200.6572 (7)0.6365 (7)0.5677 (7)0.0176 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U10.0266 (3)0.0149 (2)0.0179 (2)0.00949 (19)0.0113 (2)0.01012 (19)
Cl10.035 (6)0.028 (6)0.045 (5)0.017 (4)0.019 (4)0.020 (4)
O1M0.033 (7)0.028 (7)0.032 (6)0.018 (5)0.016 (6)0.016 (6)
C1M0.032 (10)0.034 (11)0.052 (11)0.020 (8)0.030 (9)0.019 (10)
U40.0294 (3)0.0112 (2)0.0149 (2)0.00420 (19)0.0090 (2)0.00584 (18)
Cl30.050 (7)0.023 (7)0.023 (7)0.004 (6)0.012 (5)0.000 (5)
O3M0.036 (7)0.015 (6)0.019 (7)0.002 (7)0.005 (6)0.001 (6)
C3M0.047 (13)0.021 (9)0.032 (12)0.008 (11)0.003 (10)0.007 (11)
U50.0247 (3)0.0175 (2)0.0164 (2)0.00476 (19)0.0066 (2)0.00890 (19)
Cl20.011 (7)0.028 (6)0.024 (7)0.007 (6)0.003 (5)0.007 (5)
O2M0.022 (6)0.032 (7)0.024 (7)0.002 (6)0.004 (6)0.010 (5)
C2M0.013 (7)0.052 (11)0.034 (11)0.002 (9)0.013 (7)0.011 (9)
C10.065 (11)0.034 (9)0.027 (8)0.027 (8)0.026 (8)0.012 (7)
O10.043 (6)0.024 (5)0.029 (5)0.020 (4)0.025 (5)0.016 (4)
U20.0328 (3)0.0153 (2)0.0148 (2)0.0093 (2)0.0140 (2)0.00798 (19)
C20.076 (13)0.035 (9)0.041 (9)0.026 (9)0.046 (10)0.010 (8)
O20.048 (6)0.029 (5)0.030 (5)0.011 (5)0.020 (5)0.017 (5)
O30.045 (6)0.026 (5)0.013 (4)0.012 (4)0.013 (4)0.010 (4)
U30.0284 (3)0.0195 (2)0.0147 (2)0.0087 (2)0.0088 (2)0.01164 (19)
C30.070 (12)0.045 (10)0.012 (7)0.019 (9)0.012 (7)0.014 (7)
C40.089 (17)0.075 (15)0.051 (12)0.002 (13)0.026 (11)0.039 (12)
O40.052 (8)0.042 (7)0.040 (6)0.006 (6)0.023 (6)0.009 (5)
C50.17 (2)0.056 (11)0.081 (14)0.063 (14)0.092 (16)0.056 (11)
O50.051 (6)0.026 (5)0.028 (5)0.017 (5)0.022 (5)0.020 (4)
U60.0178 (3)0.0086 (3)0.0095 (3)0.0054 (2)0.0062 (2)0.0053 (2)
C60.051 (11)0.076 (14)0.065 (12)0.019 (10)0.024 (10)0.058 (12)
O60.044 (6)0.029 (5)0.032 (5)0.015 (5)0.020 (5)0.024 (5)
O80.034 (5)0.023 (5)0.032 (5)0.010 (4)0.014 (5)0.018 (4)
U70.0278 (3)0.0162 (2)0.0172 (2)0.00635 (19)0.0118 (2)0.01013 (19)
C70.103 (16)0.037 (10)0.058 (11)0.025 (10)0.046 (12)0.038 (9)
O70.057 (7)0.011 (4)0.030 (5)0.012 (4)0.024 (5)0.013 (4)
C80.047 (10)0.023 (8)0.085 (14)0.007 (7)0.016 (10)0.031 (9)
C90.053 (10)0.023 (7)0.015 (7)0.010 (7)0.011 (7)0.001 (6)
O90.037 (6)0.018 (5)0.015 (4)0.002 (4)0.006 (4)0.006 (4)
O100.037 (6)0.022 (5)0.014 (4)0.005 (4)0.005 (4)0.001 (4)
C100.030 (8)0.036 (9)0.044 (9)0.006 (7)0.012 (7)0.016 (8)
O110.038 (6)0.029 (5)0.014 (4)0.009 (4)0.006 (4)0.010 (4)
C110.048 (10)0.047 (10)0.027 (8)0.003 (8)0.009 (8)0.011 (8)
O120.032 (5)0.022 (5)0.037 (6)0.012 (4)0.009 (5)0.017 (5)
C120.031 (9)0.037 (9)0.050 (10)0.014 (7)0.000 (8)0.013 (8)
O130.033 (5)0.029 (5)0.038 (6)0.005 (4)0.016 (5)0.022 (5)
C130.044 (10)0.060 (11)0.047 (10)0.004 (8)0.026 (8)0.033 (9)
O140.055 (8)0.043 (7)0.027 (6)0.021 (6)0.015 (6)0.013 (5)
C140.034 (10)0.058 (13)0.055 (12)0.008 (9)0.015 (9)0.004 (10)
O150.045 (6)0.024 (5)0.022 (5)0.012 (4)0.023 (5)0.013 (4)
C150.080 (14)0.036 (9)0.045 (10)0.006 (9)0.040 (10)0.011 (8)
O160.030 (5)0.030 (5)0.030 (5)0.012 (4)0.019 (4)0.016 (4)
C160.086 (16)0.047 (12)0.042 (11)0.002 (11)0.030 (11)0.015 (9)
O170.027 (5)0.020 (4)0.015 (4)0.007 (4)0.007 (4)0.014 (4)
O180.029 (5)0.016 (4)0.014 (4)0.011 (4)0.010 (4)0.009 (4)
O190.026 (5)0.011 (4)0.014 (4)0.007 (3)0.010 (4)0.007 (3)
O200.022 (4)0.017 (4)0.017 (4)0.008 (4)0.008 (4)0.012 (4)
Geometric parameters (Å, º) top
U1—O1M2.076 (19)C4—H4B0.9800
U1—O122.320 (10)C4—H4C0.9800
U1—O12.326 (9)C5—O51.441 (19)
U1—O5i2.371 (9)C5—H5A0.9800
U1—O8i2.378 (9)C5—H5B0.9800
U1—O19i2.385 (8)C5—H5C0.9800
U1—O172.399 (9)U6—O17i2.249 (8)
U1—O162.668 (9)U6—O172.249 (8)
U1—Cl12.704 (11)U6—O20i2.255 (8)
O1M—C1M1.34 (3)U6—O202.255 (8)
C1M—H1MA0.9800U6—O19i2.279 (8)
C1M—H1MB0.9800U6—O192.279 (8)
C1M—H1MC0.9800U6—O18i2.287 (8)
U4—O3M2.076 (18)U6—O182.287 (8)
U4—O82.303 (9)C6—O61.432 (17)
U4—O72.310 (9)C6—H6A0.9800
U4—O92.315 (9)C6—H6B0.9800
U4—O102.322 (10)C6—H6C0.9800
U4—O192.328 (8)O6—U72.410 (10)
U4—O202.352 (8)O8—C81.442 (17)
U4—Cl32.698 (11)U7—O142.157 (14)
O3M—C3M1.34 (3)U7—O152.324 (9)
C3M—H3MA0.9800U7—O132.330 (10)
C3M—H3MB0.9800U7—O72.368 (9)
C3M—H3MC0.9800U7—O182.404 (9)
U5—O2M2.086 (18)U7—O202.417 (8)
U5—O132.337 (9)U7—O162.759 (9)
U5—O122.346 (9)C7—O71.423 (17)
U5—O112.359 (9)C7—H7A0.9800
U5—O202.379 (8)C7—H7B0.9800
U5—O102.387 (10)C7—H7C0.9800
U5—O172.406 (9)C8—H8A0.9800
U5—Cl22.662 (12)C8—H8B0.9800
U5—O162.664 (9)C8—H8C0.9800
O2M—C2M1.35 (3)C9—O91.429 (16)
C2M—H2MA0.9800C9—H9A0.9800
C2M—H2MB0.9800C9—H9B0.9800
C2M—H2MC0.9800C9—H9C0.9800
C1—O11.389 (16)O10—C101.420 (17)
C1—H1A0.9800C10—H10A0.9800
C1—H1B0.9800C10—H10B0.9800
C1—H1C0.9800C10—H10C0.9800
O1—U22.339 (9)O11—C111.426 (18)
U2—O22.110 (10)C11—H11A0.9800
U2—O152.353 (9)C11—H11B0.9800
U2—O9i2.383 (9)C11—H11C0.9800
U2—O32.401 (9)O12—C121.416 (18)
U2—O19i2.411 (8)C12—H12A0.9800
U2—O182.413 (8)C12—H12B0.9800
U2—O162.749 (10)C12—H12C0.9800
C2—O21.363 (17)O13—C131.400 (18)
C2—H2A0.9800C13—H13A0.9800
C2—H2B0.9800C13—H13B0.9800
C2—H2C0.9800C13—H13C0.9800
O3—C31.425 (15)O14—C141.21 (2)
O3—U32.305 (9)C14—H14A0.9800
U3—O42.160 (14)C14—H14B0.9800
U3—O62.284 (10)C14—H14C0.9800
U3—O182.293 (8)O15—C151.356 (18)
U3—O11i2.305 (10)C15—H15A0.9800
U3—O52.307 (9)C15—H15B0.9800
U3—O17i2.344 (8)C15—H15C0.9800
C3—H3A0.9800O16—C161.40 (2)
C3—H3B0.9800C16—H16A0.9800
C3—H3C0.9800C16—H16B0.9800
C4—O40.99 (2)C16—H16C0.9800
C4—H4A0.9800
O1M—U1—O1286.1 (7)C4—O4—U3170.5 (18)
O1M—U1—O183.1 (7)O5—C5—H5A109.5
O12—U1—O1113.1 (4)O5—C5—H5B109.5
O12—U1—O5i83.0 (4)H5A—C5—H5B109.5
O1—U1—O5i161.1 (3)O5—C5—H5C109.5
O12—U1—O8i160.6 (3)H5A—C5—H5C109.5
O1—U1—O8i82.2 (3)H5B—C5—H5C109.5
O5i—U1—O8i80.1 (3)C5—O5—U3123.3 (9)
O12—U1—O19i127.3 (3)C5—O5—U1i122.8 (9)
O1—U1—O19i72.2 (3)U3—O5—U1i113.6 (4)
O5i—U1—O19i106.7 (3)O17i—U6—O17180.0 (5)
O8i—U1—O19i67.4 (3)O17i—U6—O20i71.0 (3)
O1M—U1—O17147.4 (6)O17—U6—O20i109.0 (3)
O12—U1—O1771.0 (3)O17i—U6—O20109.0 (3)
O1—U1—O17126.8 (3)O17—U6—O2071.0 (3)
O5i—U1—O1766.5 (3)O20i—U6—O20180.0
O8i—U1—O17110.3 (3)O17i—U6—O19i108.9 (3)
O19i—U1—O1766.8 (3)O17—U6—O19i71.1 (3)
O1M—U1—O16124.2 (7)O20i—U6—O19i70.0 (3)
O12—U1—O1667.0 (3)O20—U6—O19i110.0 (3)
O1—U1—O1666.4 (3)O17i—U6—O1971.1 (3)
O5i—U1—O16131.6 (3)O17—U6—O19108.9 (3)
O8i—U1—O16132.1 (3)O20i—U6—O19110.0 (3)
O19i—U1—O1669.0 (3)O20—U6—O1970.0 (3)
O17—U1—O1668.1 (3)O19i—U6—O19180.0
O12—U1—Cl182.5 (3)O17i—U6—O18i110.4 (3)
O1—U1—Cl186.4 (3)O17—U6—O18i69.6 (3)
O5i—U1—Cl186.0 (3)O20i—U6—O18i70.8 (3)
O8i—U1—Cl186.8 (3)O20—U6—O18i109.2 (3)
O19i—U1—Cl1148.1 (3)O19i—U6—O18i109.3 (3)
O17—U1—Cl1143.4 (3)O19—U6—O18i70.7 (3)
O16—U1—Cl1124.0 (3)O17i—U6—O1869.6 (3)
C1M—O1M—U1176 (2)O17—U6—O18110.4 (3)
O1M—C1M—H1MA109.5O20i—U6—O18109.2 (3)
O1M—C1M—H1MB109.5O20—U6—O1870.8 (3)
H1MA—C1M—H1MB109.5O19i—U6—O1870.7 (3)
O1M—C1M—H1MC109.5O19—U6—O18109.3 (3)
H1MA—C1M—H1MC109.5O18i—U6—O18180.0
H1MB—C1M—H1MC109.5O6—C6—H6A109.5
O3M—U4—O886.4 (7)O6—C6—H6B109.5
O3M—U4—O788.1 (7)H6A—C6—H6B109.5
O8—U4—O785.1 (3)O6—C6—H6C109.5
O3M—U4—O990.3 (7)H6A—C6—H6C109.5
O8—U4—O994.8 (3)H6B—C6—H6C109.5
O7—U4—O9178.4 (3)C6—O6—U3125.1 (10)
O3M—U4—O1087.9 (7)C6—O6—U7122.8 (10)
O8—U4—O10174.3 (3)U3—O6—U7110.7 (3)
O7—U4—O1093.9 (4)C8—O8—U4124.9 (9)
O9—U4—O1086.1 (3)C8—O8—U1i122.9 (9)
O3M—U4—O19146.4 (7)U4—O8—U1i111.7 (4)
O8—U4—O1969.6 (3)O14—U7—O1585.3 (4)
O7—U4—O19112.0 (3)O14—U7—O1385.2 (4)
O9—U4—O1969.4 (3)O15—U7—O13109.0 (3)
O10—U4—O19115.9 (3)O14—U7—O786.7 (4)
O3M—U4—O20146.0 (7)O15—U7—O7162.5 (3)
O8—U4—O20115.1 (3)O13—U7—O785.8 (4)
O7—U4—O2069.1 (3)O14—U7—O18146.0 (3)
O9—U4—O20112.3 (3)O15—U7—O1872.6 (3)
O10—U4—O2069.5 (3)O13—U7—O18126.0 (3)
O19—U4—O2067.6 (3)O7—U7—O18106.7 (3)
O8—U4—Cl386.4 (3)O14—U7—O685.3 (4)
O7—U4—Cl388.5 (3)O15—U7—O683.1 (3)
O9—U4—Cl389.9 (3)O13—U7—O6163.9 (3)
O10—U4—Cl388.0 (3)O7—U7—O680.7 (3)
O19—U4—Cl3146.1 (3)O18—U7—O667.0 (3)
O20—U4—Cl3146.3 (3)O14—U7—O20145.9 (3)
C3M—O3M—U4177 (3)O15—U7—O20125.5 (3)
O3M—C3M—H3MA109.5O13—U7—O2072.0 (3)
O3M—C3M—H3MB109.5O7—U7—O2067.1 (3)
H3MA—C3M—H3MB109.5O18—U7—O2066.2 (3)
O3M—C3M—H3MC109.5O6—U7—O20110.2 (3)
H3MA—C3M—H3MC109.5O14—U7—O16125.7 (4)
H3MB—C3M—H3MC109.5O15—U7—O1665.7 (3)
O2M—U5—O1385.7 (7)O13—U7—O1664.9 (3)
O2M—U5—O1282.7 (6)O7—U7—O16131.1 (3)
O13—U5—O12113.4 (4)O18—U7—O1668.1 (3)
O2M—U5—O1187.6 (7)O6—U7—O16131.1 (3)
O13—U5—O11160.2 (3)O20—U7—O1666.9 (3)
O12—U5—O1184.1 (3)O7—C7—H7A109.5
O2M—U5—O20148.5 (6)O7—C7—H7B109.5
O13—U5—O2072.5 (3)H7A—C7—H7B109.5
O12—U5—O20126.5 (3)O7—C7—H7C109.5
O11—U5—O20105.1 (3)H7A—C7—H7C109.5
O2M—U5—O1086.8 (6)H7B—C7—H7C109.5
O13—U5—O1081.6 (3)C7—O7—U4124.4 (9)
O12—U5—O10160.8 (3)C7—O7—U7122.0 (9)
O11—U5—O1079.4 (3)U4—O7—U7113.5 (3)
O20—U5—O1068.0 (3)O8—C8—H8A109.5
O2M—U5—O17143.9 (7)O8—C8—H8B109.5
O13—U5—O17126.7 (3)H8A—C8—H8B109.5
O12—U5—O1770.4 (3)O8—C8—H8C109.5
O11—U5—O1766.5 (3)H8A—C8—H8C109.5
O20—U5—O1766.3 (3)H8B—C8—H8C109.5
O10—U5—O17111.1 (3)O9—C9—H9A109.5
O13—U5—Cl286.7 (4)O9—C9—H9B109.5
O12—U5—Cl283.9 (4)H9A—C9—H9B109.5
O11—U5—Cl286.2 (4)O9—C9—H9C109.5
O20—U5—Cl2147.9 (4)H9A—C9—H9C109.5
O10—U5—Cl285.3 (4)H9B—C9—H9C109.5
O17—U5—Cl2143.6 (4)C9—O9—U4124.5 (8)
O2M—U5—O16123.0 (6)C9—O9—U2i123.0 (8)
O13—U5—O1666.4 (3)U4—O9—U2i112.5 (3)
O12—U5—O1666.7 (3)C10—O10—U4121.1 (9)
O11—U5—O16132.0 (3)C10—O10—U5127.1 (9)
O20—U5—O1669.0 (3)U4—O10—U5111.2 (4)
O10—U5—O16132.2 (3)O10—C10—H10A109.5
O17—U5—O1668.1 (3)O10—C10—H10B109.5
Cl2—U5—O16124.9 (3)H10A—C10—H10B109.5
C2M—O2M—U5173 (2)O10—C10—H10C109.5
O2M—C2M—H2MA109.5H10A—C10—H10C109.5
O2M—C2M—H2MB109.5H10B—C10—H10C109.5
H2MA—C2M—H2MB109.5C11—O11—U3i121.4 (9)
O2M—C2M—H2MC109.5C11—O11—U5123.7 (9)
H2MA—C2M—H2MC109.5U3i—O11—U5114.2 (4)
H2MB—C2M—H2MC109.5O11—C11—H11A109.5
O1—C1—H1A109.5O11—C11—H11B109.5
O1—C1—H1B109.5H11A—C11—H11B109.5
H1A—C1—H1B109.5O11—C11—H11C109.5
O1—C1—H1C109.5H11A—C11—H11C109.5
H1A—C1—H1C109.5H11B—C11—H11C109.5
H1B—C1—H1C109.5C12—O12—U1124.1 (9)
C1—O1—U1126.0 (8)C12—O12—U5125.1 (9)
C1—O1—U2123.2 (9)U1—O12—U5105.3 (4)
U1—O1—U2105.4 (3)O12—C12—H12A109.5
O2—U2—O184.8 (3)O12—C12—H12B109.5
O2—U2—O1584.7 (3)H12A—C12—H12B109.5
O1—U2—O15109.8 (3)O12—C12—H12C109.5
O2—U2—O9i88.0 (3)H12A—C12—H12C109.5
O1—U2—O9i85.5 (3)H12B—C12—H12C109.5
O15—U2—O9i162.4 (3)C13—O13—U7124.0 (9)
O2—U2—O386.0 (3)C13—O13—U5125.9 (9)
O1—U2—O3164.1 (3)U7—O13—U5105.2 (4)
O15—U2—O382.2 (3)O13—C13—H13A109.5
O9i—U2—O381.3 (3)O13—C13—H13B109.5
O2—U2—O19i146.2 (3)H13A—C13—H13B109.5
O1—U2—O19i71.5 (3)O13—C13—H13C109.5
O15—U2—O19i125.4 (3)H13A—C13—H13C109.5
O9i—U2—O19i66.9 (3)H13B—C13—H13C109.5
O3—U2—O19i110.7 (3)C14—O14—U7178.8 (13)
O2—U2—O18146.1 (3)O14—C14—H14A109.5
O1—U2—O18125.7 (3)O14—C14—H14B109.5
O15—U2—O1871.9 (3)H14A—C14—H14B109.5
O9i—U2—O18106.9 (3)O14—C14—H14C109.5
O3—U2—O1867.1 (3)H14A—C14—H14C109.5
O19i—U2—O1866.4 (3)H14B—C14—H14C109.5
O2—U2—O16124.0 (3)C15—O15—U7124.3 (9)
O1—U2—O1664.9 (3)C15—O15—U2126.2 (9)
O15—U2—O1665.5 (3)U7—O15—U2105.7 (3)
O9i—U2—O16131.2 (3)O15—C15—H15A109.5
O3—U2—O16130.9 (3)O15—C15—H15B109.5
O19i—U2—O1667.2 (3)H15A—C15—H15B109.5
O18—U2—O1668.2 (3)O15—C15—H15C109.5
O2—C2—H2A109.5H15A—C15—H15C109.5
O2—C2—H2B109.5H15B—C15—H15C109.5
H2A—C2—H2B109.5C16—O16—U598.1 (9)
O2—C2—H2C109.5C16—O16—U1103.3 (10)
H2A—C2—H2C109.5U5—O16—U188.2 (3)
H2B—C2—H2C109.5C16—O16—U2110.3 (9)
C2—O2—U2177.3 (11)U5—O16—U2151.6 (4)
C3—O3—U3125.8 (9)U1—O16—U286.5 (3)
C3—O3—U2122.6 (9)C16—O16—U7105.4 (10)
U3—O3—U2110.7 (3)U5—O16—U786.3 (3)
O4—U3—O689.5 (4)U1—O16—U7151.3 (4)
O4—U3—O18151.1 (4)U2—O16—U785.2 (3)
O6—U3—O1871.0 (3)O16—C16—H16A109.5
O4—U3—O11i87.5 (4)O16—C16—H16B109.5
O6—U3—O11i175.1 (3)H16A—C16—H16B109.5
O18—U3—O11i110.3 (3)O16—C16—H16C109.5
O4—U3—O389.2 (4)H16A—C16—H16C109.5
O6—U3—O391.3 (3)H16B—C16—H16C109.5
O18—U3—O370.7 (3)U6—O17—U3i111.0 (4)
O11i—U3—O384.9 (3)U6—O17—U1111.2 (3)
O4—U3—O586.8 (4)U3i—O17—U1111.3 (3)
O6—U3—O584.5 (4)U6—O17—U5110.8 (3)
O18—U3—O5111.4 (3)U3i—O17—U5111.0 (3)
O11i—U3—O599.2 (4)U1—O17—U5101.1 (3)
O3—U3—O5174.2 (3)U6—O18—U3111.5 (4)
O4—U3—O17i141.1 (4)U6—O18—U7111.1 (3)
O6—U3—O17i116.2 (3)U3—O18—U7110.6 (3)
O18—U3—O17i67.9 (3)U6—O18—U2111.2 (3)
O11i—U3—O17i68.3 (3)U3—O18—U2110.7 (3)
O3—U3—O17i117.1 (3)U7—O18—U2101.4 (3)
O5—U3—O17i68.5 (3)U6—O19—U4111.2 (3)
O3—C3—H3A109.5U6—O19—U1i110.7 (3)
O3—C3—H3B109.5U4—O19—U1i110.6 (3)
H3A—C3—H3B109.5U6—O19—U2i111.5 (3)
O3—C3—H3C109.5U4—O19—U2i111.0 (3)
H3A—C3—H3C109.5U1i—O19—U2i101.4 (3)
H3B—C3—H3C109.5U6—O20—U4111.2 (3)
O4—C4—H4A109.5U6—O20—U5111.6 (3)
O4—C4—H4B109.5U4—O20—U5110.5 (3)
H4A—C4—H4B109.5U6—O20—U7111.7 (3)
O4—C4—H4C109.5U4—O20—U7110.2 (3)
H4A—C4—H4C109.5U5—O20—U7101.3 (3)
H4B—C4—H4C109.5
Symmetry code: (i) x+1, y+1, z+1.
Summary of bond-valence-sum (BVS) calculations on the uranium atoms U1–U7 in (I) top
AtomAtomic charge calculated by BVS (v.u.)
U13.73
U23.99
U34.34
U43.86
U53.77
U65.16
U73.93
Average4.11
Geometrical parameters (Å, °) of cubic uranium polyhedra in different compounds top
U—O distanceO—U—O angle
CompoundShortestLongestAverageSmallestLargestAverageReference
UO22.36870.5Cooper (1982)
{U38}2.2292.5202.35768.176.570.5Falaise et al. (2013c)
{U13}2.2432.2902.26469.871.270.5This work
 

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