Iodination of Stanna-closo-dodecaborate
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- 作者：Torben Gä ; dt ; Falko M. Schappacher ; Rainer Pö ; ttgen ; Lars Wesemann
- 刊名：Inorganic Chemistry
- 出版年：2007
- 出版时间：April 2, 2007
- 年：2007
- 卷：46
- 期：7
- 页码：2864 - 2869
- 全文大小：111K
- 年卷期：v.46,no.7(April 2, 2007)
- ISSN：1520-510X
文摘
The dianionic stannaborate [SnB11H11]2- oxidatively adds iodine at the tin vertex to give the iodinated cluster[I2SnB11H11]2- which maintains a closo structure, albeit having a nido electron count. The iodo-stannaborate[I2SnB11H11]2- is unstable at room temperature, but its structure was elucidated via single-crystal X-ray diffractionat low temperatures. The low-temperature 11B NMR spectrum exhibits a 5:1:5 signal pattern, and the 119Sn NMRshows a resonance at -1039 ppm. Iodination of the zwitterionic stannaborate iron complex Fe(SnB11H11)(triphos)leads to the formation of the corresponding iodo-stannaborate iron complex Fe(I2SnB11H11)(triphos) which featuresan iodinated stannaborate moiety that has a structure analogous to that of [I2SnB11H11]2-. The zwitterionic iodo-stannaborate complex is stable at room temperature, and the crystal structure and the 1H, 11B, 31P, and 119Sn NMRparameters were determined. 119Sn Mössbauer spectroscopy supports the assignment of a tin oxidation state of +IIfor Fe(SnB11H11)(triphos) (
= 2.71 mm s-1) and +IV for Fe(I2SnB11H11)(triphos) ( = 1.22 mm s-1). Additional57Fe Mössbauer spectra confirm the iron oxidation state +II for both compounds.
= 2.71 mm s-1) and +IV for Fe(I2SnB11H11)(triphos) ( = 1.22 mm s-1). Additional57Fe Mössbauer spectra confirm the iron oxidation state +II for both compounds.