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The high-temperature/high-pressure treatment of the K-Te-U oxo-family at 1100 °C and 3.5 GPa results in the crystallization of a series of novel uranyl tellurium compounds, K 2 [(UO 2 ) 3 (Te IV O 3 ) 4 ], K 2 [(UO 2 )TeO 14 ], α-K 2 [(UO 2 )Te VI O 5 ] and β-K 2 [(UO 2 )Te VI O 5 ]. In contrast to most of the reported uranyl compounds which are favorable in layered structures, we found that under extreme conditions, the potassium uranyl oxo-tellurium compounds preferably crystallized in three-dimensional (3D) framework structures with complex topologies. Anion topology analysis indicates that the 3D uranyl tellurite anionic framework observed in K 2 [(UO 2 ) 3 (Te IV O 3 ) 4 ] is attributable to the additional linkages of TeO 3 polyhedra connecting with TeO 4 disphenoids from the neighboring U-Te layers. The structure of K 2 [(UO 2 )TeO 14 ] can be described based on [UTe 6 O 26 ] 22- clusters, where six TeO 5 polyhedra enclose a hexagonal cavity in which a UO 8 polyhedron is located. The [UTe 6 O 26 ] 22- clusters are further linked by TeO 5 square pyramids to form the 3D network. Similar to uranyl tellurates, both α-K 2 [(UO 2 )Te VI O 5 ] and β-K 2 [(UO 2 )Te VI O 5 ] contain TeO 6 octahedra which share a common face to form a dimeric Te 2 O 10 unit. However, in α-K 2 [(UO 2 )Te VI O 5 ], these Te 2 O 10 units connect with UO 6 tetragonal bipyramids to form a 3D structural framework, while in β-K 2 [(UO 2 )Te VI O 5 ], the same Te 2 O 10 dimers are observed to link with UO 7 pentagonal bipyramids, forming 2D layers. Raman measurements were carried out and the vibration bands related to Te IV -O, Te VI -O and U VI -O bonds are discussed.

Investigation of reactivity and structure formation in a K–Te–U oxo-system under high-temperature/high-pressure conditions