Peroxouranyl-Containing W<sub>48</sub> Wheel: Synthesis, Structure, and Detailed Infrared and Raman Spectroscopy Study
Joydeb Goura, Anusree Sundar, Bassem S. Bassil, Gordana Ćirić‐Marjanović, Danica Bajuk‐Bogdanović, Ulrich Kortz
Abstract
We report on the first example of a peroxouranium-containing {P8W48} wheel, [{(UO2)4(O2)4}2(P8W48O184)]40– (1), which was synthesized by a one-pot reaction of UO2(NO3)2·6H2O with the 48-tungsto-8-phosphate wheel [H7P8W48O184]33− and aqueous hydrogen peroxide in a pH 6 lithium acetate solution at 50 °C. Polyanion 1 comprises two tetrauranyl squares with side-on peroxo bridging ligands in the cavity of the {P8W48} wheel, and was isolated as the hydrated potassium–lithium salt K18Li22[{(UO2)4(O2)4}2(P8W48O184)]·133H2O (KLi-1), which was characterized in the solid state by single-crystal X-ray diffraction, as well as thermogravimetric and elemental analyses. A detailed Fourier transform infrared and Raman spectroscopy study was also performed.