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A new rubidium uranyl silicate, Rb 2 (UO 2 ) 2 O(Si 3 O 8 ) ( 1 ), was obtained using high-temperature approach from the melt in silica tubes. Its crystal structure was solved by direct methods: hexagonal,  P 6/ m ,  a  = 27.7992(7),  c  = 7.2346(2) Å,  V  = 4841.8(3) Å 3 ,  R  1  = 0.033. The structure of  1  represents a new structure type with unprecedented topology not observed before among U(VI) oxides and oxysalts. It is comprised of layers with large voids derived from the U 3 O 8  structure formed exclusively by pentagonal  Ur O 5  bipyramids. The low-occupied Rb sites are located in the interlayer space. The SiO 4  silicate tetrahedra in the structure of  1  share vertices to form rolled [Si 6 O 16 ] 8−  chains. The nanotubules [(UO 2 )(Si 6 O 16 )] 6−  penetrate through both U 3 O 8 -derived layers and Rb interlayer. These tubules are attached to the U 3 O 8  derived sheets via uranyl-uranyl interactions and edge-sharing between silicate tetrahedra and  Ur O 5  bipyramids.

Uranyl silicate nanotubules in Rb 2 [(UO 2 ) 2 O(Si 3 O 8 )]: synthesis and crystal structure