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The structure of a new type of polyoxo cluster complex that contains thirteen uranium atoms, {U 13 }, is reported. The complex crystallized from methanol containing tetra-valent uranium (U IV ) with a basic organic ligand, and was characterized as di-chloridoocta-cosa-μ 2 -methano-lato-octa-kis-(methano-lato)octa-μ 4 -oxido-trideca-uranium, [U 13 (CH 3 O) 35.7 Cl 2.3 O 8 ] or [U 13 (μ 4 -O oxo ) 8 Cl  x  (MeO) 38- x  ] ( x = 2.3, MeO = methoxide) ( I ), by single-crystal X-ray diffraction. The characterized {U 13 } 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 UO 2 . The U-O bonds in the cubic polyhedron of I are, however, significantly shorter than those not only in bulk UO 2 but also in another analogue in the {U 38 } 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 penta-valent state (U V ) from the original tetra-valent state (U IV ). Complex I is, hence, the first example of a polyoxo cluster possessing a single cubic coordination polyhedron of U V .

acta crystallographica. section e, crystallographic communications

Structure of the {U13} polyoxo cluster U13O8Cl x (MeO)38–x (x = 2.3, MeO = methoxide)