How Does the Synthesis Temperature Impact Hybrid Organic−Inorganic Molybdate Material Design?
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- 作者：Rmi Dessapt ; Daniel Kervern ; Martine Bujoli-Doeuff ; Philippe Deniard ; Michel Evain ; Stphane Jobic
- 刊名：Inorganic Chemistry
- 出版年：2010
- 出版时间：December 20, 2010
- 年：2010
- 卷：49
- 期：24
- 页码：11309-11316
- 全文大小：903K
- 年卷期：v.49,no.24(December 20, 2010)
- ISSN：1520-510X
文摘
We investigate the reactivity of MoO42− toward six organoammonium cations +(Me3−xHxN)(CH2)2(NHyMe3−y)+ (x, y = 1−3) at different synthesis temperatures ranging from 70 to 180 °C. A total of 16 hybrid organic−inorganic materials have been synthesized at an initial pH of 2, via ambient pressure and hydrothermal routes, namely, (H2en)[Mo3O10]·H2O (1), (H2en)[Mo3O10] (2), (H2en)[Mo5O16] (3), (H2MED)2[Mo8O26]·2H2O (4), (H2MED)[Mo5O16] (5), (N,N-H2DMED)2[Mo8O26]·2H2O (6), (N,N-H2DMED)2[Mo8O26]·2H2O (7), (N,N′-H2DMED)2[Mo8O26] (8), (N,N′-H2DMED)[Mo5O16] (9), (H2TriMED)2[Mo8O26]·4H2O (10), (H2TriMED)2[Mo8O26]·2H2O (11), (H2TriMED)[Mo7O22] (12), (H2TMED)2[Mo8O26]·2H2O (13), (H2TMED)2[Mo8O26] (14), (H2TMED)2[Mo8O26] (15), and (H2TMED)[Mo7O22] (16). All of these compounds contain different polyoxomolybdate (Mo-POM) blocks, i.e., discrete β-[Mo8O26]4− blocks in 6, 10, 13, 14, 1/∞[Mo3O10]2−, and 1/∞[Mo8O26]4− polymeric chains in 1, 2, 4, 7, 8, and 15, respectively, and 2/∞[Mo5O16]2− and 2/∞[Mo7O22]2− layers in 3, 5, 9, 12, and 16, respectively. The structures of 5, 9, and 14 have been resolved by single-crystal X-ray analyses. The characterization of the different Mo-POM blocks in 1−16 by Fourier transform Raman spectroscopy is reported. The impact of the synthesis temperature on both the composition and topology of the Mo-POM blocks is highlighted.