High yield synthesis of mixed-metal keggin polyoxoanions in non-aqueous solvents: Preparation of (n-Bu4N)4[PMW11O40] (M = V, Nb, Ta)

IF 2.6 3区化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR

Polyhedron Pub Date : 1995-08-01 DOI:10.1016/0277-5387(95)00026-O

Emil Radkov, Robert H. Beer

引用次数: 0

Abstract

The synthesis of (n-Bu₄N)₄[PMW₁₁O₄₀] (M = V, Nb, Ta) in non-aqueous solvents is described using the lacunary compound (n-Bu₄N)₄H₃[PW₁₁O₃₉] and commercially available VOCl₃, NbCl₅ and TaCl₅. The yield and purity of the product vary depending on the solvent and the presence of base. ¹⁸³W NMR spectroscopy of the title compounds reveal six resonances in the ratio 2:2:2:1:2:2 (M, Nb, Ta) consistent withtheir formulation as monosubstituted tungstophosphates with the Keggin structure. Their FAB mass spectra display protonated molecular ions in the positive ion mode and monoanionic fragments MO_x and MW_nO_x(n ⪖ 1, x ⪖ n) (M = Nb, Ta) in the negative ion mode.

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非水溶剂中高收率合成混合金属keggin多氧阴离子：（n-Bu4N）4[PMW11O40] （M = V, Nb, Ta）的制备

以（n-Bu4N）4H3[PW11O39]和市售的VOCl3、NbCl5和TaCl5为原料，在非水溶剂中合成（n-Bu4N）4[PMW11O40] （M = V, Nb, Ta）。产品的收率和纯度取决于溶剂和碱的存在。标题化合物的183W核磁共振谱显示了6个比例为2:2:2:1:2:2 （M, Nb, Ta）的共振，符合它们具有Keggin结构的单取代磷酸钨的分子式。它们的FAB质谱显示质子化分子离子为正离子模式，单阴离子片段MOx和MWnOx(n⪖1,x⪖n) （M = Nb, Ta）为负离子模式。

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来源期刊

Polyhedron 化学-晶体学

CiteScore

4.90

自引率

7.70%

发文量

515

审稿时长

2 months

期刊介绍： Polyhedron publishes original, fundamental, experimental and theoretical work of the highest quality in all the major areas of inorganic chemistry. This includes synthetic chemistry, coordination chemistry, organometallic chemistry, bioinorganic chemistry, and solid-state and materials chemistry. Papers should be significant pieces of work, and all new compounds must be appropriately characterized. The inclusion of single-crystal X-ray structural data is strongly encouraged, but papers reporting only the X-ray structure determination of a single compound will usually not be considered. Papers on solid-state or materials chemistry will be expected to have a significant molecular chemistry component (such as the synthesis and characterization of the molecular precursors and/or a systematic study of the use of different precursors or reaction conditions) or demonstrate a cutting-edge application (for example inorganic materials for energy applications). Papers dealing only with stability constants are not considered.