Complex Topology of Uranyl Polyphosphate Frameworks: Crystal Structures of α‐, β‐K[(UO2)(P3O9)] and K[(UO2)2(P3O10)]

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Abstract
Three new uranyl polyphosphates, α‐K[(UO2)(P3O9)] (1), β‐K[(UO2)(P3O9)] (2), and K[(UO2)2(P3O10)] (3), were prepared by high‐temperature solid‐state reactions. The crystal structures of the compounds have been solved by direct methods: 1 – monoclinic, P21/m, a = 8.497(1), b = 15.1150(1), c = 14.7890(1) Å, β = 91.911(5)°, V = 1898.3(3) Å3, Z = 4, R1 = 0.0734 for 4181 unique reflections with |F0| ≥ 4σF; 2 – monoclinic, P21/n, a = 8.607(1), b = 14.842(2), c = 14.951(1) Å, β = 95.829(5)°, V = 1900.0(4) Å3, Z = 4, R1 = 0.0787 for 3185 unique reflections with |F0| ≥ 4σF; 3 – Pbcn, a = 10.632(1), b = 10.325(1), c = 11.209(1) Å, V = 1230.5(2) Å3, Z = 4, R1 = 0.0364 for 1338 unique reflections with |F0| ≥ 4σF. In the structures of 1 and 2, phosphate tetrahedra share corners to form infinite [PO3]− chains, whereas, in the structure of 3, tetrahedra form linear [P3O10]5− trimers. The structures are based upon 3‐D frameworks of U and P polyhedra linked by sharing common O corners. The infinite [PO3]− chains in the structures of 1 and 2 are parallel to [100] and [–101], respectively. The uranyl polyphosphate frameworks are occupied by host K+ cations.

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