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Synthesis and characterization of an organic-inorganic hybrid compound: [WO3(2,2 '-bipy)] (2,2 '-bipy = 2,2 '-bipyridine)

机译:有机-无机杂化化合物的合成与表征:[WO3(2,2'-联吡啶)](2,2'-联吡啶= 2,2'-联吡啶)

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摘要

The hydrothermal synthesis and characterization of an organic-inorganic hybrid compound [WO3(2,2'-bipy)] (2,2'-bipy = 2,2'-bipyridine) is presented. This compound was characterized by various techniques including Raman and IR spectroscopy, XRD and thermogravimetric analysis. Structural analysis of the compound by Raman and IR data shows that it has a novel tungstate structure with 2,2'-bipy coordinated to tungsten. The X-ray powder diffraction data of the compound are indexed to a monoclinic cell with a = 14.313(4), b = 9.603(2), c = 7.288(2) Angstrom, beta = 102.07(2)degrees. The structure of [WO3(2,2'-bipy)] adopts a chain-like framework consisting of corner-shared distorted octahedra (WO4N2) with 2,2'-bipy acting as a bidentate ligand whose rings fan out from the chain. Upon heating, [WO3(2,2'-bipy)] retains its structural integrity until 300 degrees C, followed by a gradual loss of 2,2'-bipy which leads to the formation of WO3 at ca. 475 degrees C. The thermal decomposition is observed to proceed through a transitional intermediate, [W4O12(2,2'-bipy)], the structure of which is proposed and discussed. [References: 33]
机译:介绍了有机-无机杂化化合物[WO3(2,2'-联吡啶)](2,2'-联吡啶= 2,2'-联吡啶)的水热合成和表征。该化合物通过各种技术进行了表征,包括拉曼光谱和红外光谱,XRD和热重分析。通过拉曼和红外数据对该化合物进行结构分析表明,该化合物具有新颖的钨酸盐结构,其中2,2'-联吡啶与钨配位。该化合物的X射线粉末衍射数据被标为a = 14.313(4),b = 9.603(2),c = 7.288(2)埃,β= 102.07(2)度的单斜细胞。 [WO3(2,2'-bipy)]的结构采用链状构架,该构架由角共享的扭曲八面体(WO4N2)组成,其中2,2'-bipy充当双齿配体,其环扇形展开。加热后,[WO3(2,2'-bipy)]保持其结构完整性,直到300摄氏度,然后逐渐失去2,2'-bipy,这导致大约在200℃形成WO3。 475摄氏度。观察到热分解通过过渡中间体[W4O12(2,2'-bipy)]进行,该中间体的结构已被提出和讨论。 [参考:33]

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