Alkoxide Route to Mixed Oxides of Rhenium, Niobium, and Tantalum. Preparation and X-ray Single-Crystal Study of a Novel Rhenium−Niobium Methoxo Complex, Nb2(OMe)8(ReO4)2
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Abstract
Thermal decomposition of complex oxomethoxo compounds Nb4O2(OMe)14(ReO4)2 (I) and Ta4O2(OMe)14(ReO4)2 (II) has been investigated. The decomposition of (II) at temperatures exceeding 100 °C results in the formation of MeOMe, MeOCH2OMe, MeOH, and H2O vapor and is accompanied by sublimation at temperatures over 135 °C. Plausible mechanisms of the processes studied are discussed. A new bimetallic methoxo compound, Nb2(OMe)8(ReO4)2 (III), was synthesized by interaction between Re2O7 and Nb2(OMe)10 in toluene solution and its structure was determined by means of an X-ray single-crystal study. The structure can be considered as a product of substitution for terminal methoxo groups with two perrhenate groups in dimeric Nb2(OMe)10 molecules. Decomposition of II in an inert atmosphere at 900 °C gave a Re−Ta mixed oxide phase, supposedly based on the L-Ta2O5 structure. Decomposition of I and III under similar conditions leads to the formation of rhenium−niobium oxide phases. The results obtained provide a basis for the alkoxide approach to the synthesis of oxide and metallic rhenium-based materials.
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