Three sandglass-type molybdophosphates obtained via a new route: Synthesis and characterization of X

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• 作者：Yan-Chun Bai ; Li-Ping Liu ; Xing-Juan Yan ; Wei Chu ; Ying-Ying Zhu ; Yu-Ting Song ; Ru-Dan Huang
• 关键词：Molybdophosphates ; Polyoxometalates ; Phosphorus pentachloride ; Sandglass-type ; Hydrothermal treatment
• 刊名：Journal of Solid State Chemistry
• 出版年：2009
• 出版时间：January 2009
• 年：2009
• 卷：182
• 期：1
• 页码：89-94
• 全文大小：758 K

文摘

Three new polyoxometalates X₇[PMo₈O₃₀] (X=Na⁺, 1; K⁺, 2; NH₄⁺, 3) have been synthesized with the classical Keggin and/or Dawson heteropolymolybdophosphates and PCl₅ in acetonitrile-water solutions via hydrothermal treatment. The three compounds were characterized by different analyses including IR, ³¹P NMR spectroscopy, elemental analysis, electrochemistry, thermogravimetric analysis (TGA) and powder X-ray diffraction (XRD). Single crystal X-ray analyses were carried out on Na₇[PMo₈O₃₀] (1) and (NH₄)₇[PMo₈O₃₀] (3). Compound 1 and 3 crystallize in the orthorhombic system. The structure of compound 2 was confirmed by the IR spectra and powder XRD. All the three compounds contain the same octamolybdophosphate polyoxoanion [PMo₈O₃₀]⁷⁻, which consists of two Mo₄O₁₅ moieties linked by one central PO₄ tetrahedron, leading to a remarkable sandglass-like structure.