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

26 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
Externally published	Yes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

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@article{9417d3d12f8f446d98f9a6dc49d2f6cc,

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\}",

year = "2002",

month = oct,

day = "21",

doi = "10.1021/ic0113146",

language = "English (US)",

volume = "41",

pages = "5426--5432",

journal = "Inorganic Chemistry",

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publisher = "American Chemical Society",

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T1 - Synthesis, purification, and structural characterization of the dimethyldiselenoarsinate anion

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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EP - 5432

JO - Inorganic Chemistry

JF - Inorganic Chemistry

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ER -

Synthesis, purification, and structural characterization of the dimethyldiselenoarsinate anion

Abstract

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