Synthesis, purification, and structural characterization of the dimethyldiselenoarsinate anion

Jurgen Gailer; Graham N. George; Hugh H. Harris; Ingrid J. Pickering; Roger C. Prince; Arpad Somogyi; Gavin A. Buttigieg; Richard S. Glass; M. Bonner Denton

doi:10.1021/ic0113146

Synthesis, purification, and structural characterization of the dimethyldiselenoarsinate anion

Jurgen Gailer, Graham N. George, Hugh H. Harris, Ingrid J. Pickering, Roger C. Prince, Arpad Somogyi, Gavin A. Buttigieg, Richard S. Glass, M. Bonner Denton

Research output: Contribution to journal › Article › peer-review

24 Scopus citations

Abstract

A novel arsenic-selenium solution species was synthesized by reacting equimolar sodium selenite and sodium dimethylarsinate with 10 mol equiv of glutathione (pH 7.5) in aqueous solution. The solution species showed a single ⁷⁷Se NMR resonance at 112.8 ppm. Size-exclusion chromatography (SEC) using an inductively coupled plasma 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 ionization mass spectrometry (ESI-MS) of the chromatographically purified compound showed a molecular mass peak at m/z 263 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 revealed two As-C interactions at 1.943 Å and two As-Se interactions at 2.279 Å. On the basis of these results this novel solution species is identified as the dimethyldiselenoarsinate anion.

Original language	English (US)
Pages (from-to)	5426-5432
Number of pages	7
Journal	Inorganic Chemistry
Volume	41
Issue number	21
DOIs	https://doi.org/10.1021/ic0113146
State	Published - Oct 21 2002

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

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Synthesis, purification, and structural characterization of the dimethyldiselenoarsinate anion. / Gailer, Jurgen; George, Graham N.; Harris, Hugh H.; Pickering, Ingrid J.; Prince, Roger C.; Somogyi, Arpad; Buttigieg, Gavin A.; Glass, Richard S.; Denton, M. Bonner.

In: Inorganic Chemistry, Vol. 41, No. 21, 21.10.2002, p. 5426-5432.

Research output: Contribution to journal › Article › peer-review

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title = "Synthesis, purification, and structural characterization of the dimethyldiselenoarsinate anion",

abstract = "A novel arsenic-selenium solution species was synthesized by reacting equimolar sodium selenite and sodium dimethylarsinate with 10 mol equiv of glutathione (pH 7.5) in aqueous solution. The solution species showed a single 77Se NMR resonance at 112.8 ppm. Size-exclusion chromatography (SEC) using an inductively coupled plasma 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 ionization mass spectrometry (ESI-MS) of the chromatographically purified compound showed a molecular mass peak at m/z 263 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 revealed two As-C interactions at 1.943 {\AA} and two As-Se interactions at 2.279 {\AA}. On the basis of these results this novel solution species is identified as the dimethyldiselenoarsinate anion.",

author = "Jurgen Gailer and George, {Graham N.} and Harris, {Hugh H.} and Pickering, {Ingrid J.} and Prince, {Roger C.} and Arpad Somogyi and Buttigieg, {Gavin A.} and Glass, {Richard S.} and Denton, {M. Bonner}",

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AU - Gailer, Jurgen

AU - George, Graham N.

AU - Harris, Hugh H.

AU - Pickering, Ingrid J.

AU - Prince, Roger C.

AU - Somogyi, Arpad

AU - Buttigieg, Gavin A.

AU - Glass, Richard S.

AU - Denton, M. Bonner

PY - 2002/10/21

Y1 - 2002/10/21

N2 - A novel arsenic-selenium solution species was synthesized by reacting equimolar sodium selenite and sodium dimethylarsinate with 10 mol equiv of glutathione (pH 7.5) in aqueous solution. The solution species showed a single 77Se NMR resonance at 112.8 ppm. Size-exclusion chromatography (SEC) using an inductively coupled plasma 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 ionization mass spectrometry (ESI-MS) of the chromatographically purified compound showed a molecular mass peak at m/z 263 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 revealed two As-C interactions at 1.943 Å and two As-Se interactions at 2.279 Å. On the basis of these results this novel solution species is identified as the dimethyldiselenoarsinate anion.

AB - A novel arsenic-selenium solution species was synthesized by reacting equimolar sodium selenite and sodium dimethylarsinate with 10 mol equiv of glutathione (pH 7.5) in aqueous solution. The solution species showed a single 77Se NMR resonance at 112.8 ppm. Size-exclusion chromatography (SEC) using an inductively coupled plasma 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 ionization mass spectrometry (ESI-MS) of the chromatographically purified compound showed a molecular mass peak at m/z 263 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 revealed two As-C interactions at 1.943 Å and two As-Se interactions at 2.279 Å. On the basis of these results this novel solution species is identified as the dimethyldiselenoarsinate anion.

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Synthesis, purification, and structural characterization of the dimethyldiselenoarsinate anion

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