Synthesis, Purification, and Structural Characterization of the Dimethyldiselenoarsinate Anion

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• 作者：Jü ; rgen Gailer ; Graham N. George ; Hugh H. Harris ; Ingrid J. Pickering ; Roger C. Prince ; Arpad Somogyi ; Gavin A. Buttigieg ; Richard S. Glass ; and M. Bonner Denton
• 刊名：Inorganic Chemistry
• 出版年：2002
• 出版时间：October 21, 2002
• 年：2002
• 卷：41
• 期：21
• 页码：5426 - 5432
• 全文大小：132K
• 年卷期：v.41,no.21(October 21, 2002)
• ISSN：1520-510X

文摘

A novel arsenic-selenium solution species was synthesized by reacting equimolar sodium selenite and sodiumdimethylarsinate with 10 mol equiv of glutathione (pH 7.5) in aqueous solution. The solution species showed asingle ⁷⁷Se NMR resonance at 112.8 ppm. Size-exclusion chromatography (SEC) using an inductively coupledplasma atomic emission spectrometer (ICP-AES) as the simultaneous arsenic-, selenium-, sulfur-, and carbon-specific detector revealed an arsenic-selenium moiety with an As:Se molar ratio of 1:2. Electrospray ionizationmass spectrometry (ESI-MS) of the chromatographically purified compound showed a molecular mass peak at m/z263 in the negative ion mode. Fragmentation of the parent ion (ESI-MS-MS) produced (CH₃)₂As^- and Se₂^- fragments.Arsenic and selenium extended X-ray absorption fine structure spectroscopy (EXAFS) of the purified species revealedtwo As-C interactions at 1.943 Å and two As-Se interactions at 2.279 Å. On the basis of these results this novelsolution species is identified as the dimethyldiselenoarsinate anion.