Synthesis, Purification, and Structural Characterization of the Dimethyldiselenoarsinate Anion
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 a...
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| Veröffentlicht in: | Inorganic Chemistry 2002-10, Vol.41 (21), p.5426-5432 |
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| container_title | Inorganic Chemistry |
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| creator | Gailer, Jürgen George, Graham N Harris, Hugh H Pickering, Ingrid J Prince, Roger C Somogyi, Arpad Buttigieg, Gavin A Glass, Richard S Denton, M. Bonner |
| description | 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. |
| doi_str_mv | 10.1021/ic0113146 |
| format | Article |
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Bonner</creator><creatorcontrib>Gailer, Jürgen ; George, Graham N ; Harris, Hugh H ; Pickering, Ingrid J ; Prince, Roger C ; Somogyi, Arpad ; Buttigieg, Gavin A ; Glass, Richard S ; Denton, M. Bonner ; Stanford Synchrotron Radiation Lab. (US) ; Stanford Linear Accelerator Center, Menlo Park, CA (US)</creatorcontrib><description>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.</description><identifier>ISSN: 0020-1669</identifier><identifier>EISSN: 1520-510X</identifier><identifier>DOI: 10.1021/ic0113146</identifier><identifier>PMID: 12377037</identifier><language>eng</language><publisher>United States: American Chemical Society</publisher><subject>ANIONS ; ARSENIC OXIDES ; Chromatography, Gel ; Environmental Pollutants - analysis ; Hydrogen-Ion Concentration ; Indicators and Reagents ; INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY ; Magnetic Resonance Spectroscopy ; Mass Spectrometry ; MOLECULAR STRUCTURE ; ORGANOMETALLIC COMPOUNDS ; PURIFICATION ; SELENIUM COMPOUNDS ; Selenium Radioisotopes - chemistry ; Solutions ; STANFORD SYNCHROTRON RADIATION LABORATORY ; SYNTHESIS</subject><ispartof>Inorganic Chemistry, 2002-10, Vol.41 (21), p.5426-5432</ispartof><rights>Copyright © 2002 American Chemical Society</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-a441t-f23fd03c735e84f6d0d8a10ac5ece27cae2bd24b36ef83110331511989c435053</citedby><cites>FETCH-LOGICAL-a441t-f23fd03c735e84f6d0d8a10ac5ece27cae2bd24b36ef83110331511989c435053</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://pubs.acs.org/doi/pdf/10.1021/ic0113146$$EPDF$$P50$$Gacs$$H</linktopdf><linktohtml>$$Uhttps://pubs.acs.org/doi/10.1021/ic0113146$$EHTML$$P50$$Gacs$$H</linktohtml><link.rule.ids>314,780,784,885,2765,27076,27924,27925,56738,56788</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/12377037$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink><backlink>$$Uhttps://www.osti.gov/biblio/815855$$D View this record in Osti.gov$$Hfree_for_read</backlink></links><search><creatorcontrib>Gailer, Jürgen</creatorcontrib><creatorcontrib>George, Graham N</creatorcontrib><creatorcontrib>Harris, Hugh H</creatorcontrib><creatorcontrib>Pickering, Ingrid J</creatorcontrib><creatorcontrib>Prince, Roger C</creatorcontrib><creatorcontrib>Somogyi, Arpad</creatorcontrib><creatorcontrib>Buttigieg, Gavin A</creatorcontrib><creatorcontrib>Glass, Richard S</creatorcontrib><creatorcontrib>Denton, M. Bonner</creatorcontrib><creatorcontrib>Stanford Synchrotron Radiation Lab. (US)</creatorcontrib><creatorcontrib>Stanford Linear Accelerator Center, Menlo Park, CA (US)</creatorcontrib><title>Synthesis, Purification, and Structural Characterization of the Dimethyldiselenoarsinate Anion</title><title>Inorganic Chemistry</title><addtitle>Inorg. Chem</addtitle><description>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.</description><subject>ANIONS</subject><subject>ARSENIC OXIDES</subject><subject>Chromatography, Gel</subject><subject>Environmental Pollutants - analysis</subject><subject>Hydrogen-Ion Concentration</subject><subject>Indicators and Reagents</subject><subject>INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY</subject><subject>Magnetic Resonance Spectroscopy</subject><subject>Mass Spectrometry</subject><subject>MOLECULAR STRUCTURE</subject><subject>ORGANOMETALLIC COMPOUNDS</subject><subject>PURIFICATION</subject><subject>SELENIUM COMPOUNDS</subject><subject>Selenium Radioisotopes - chemistry</subject><subject>Solutions</subject><subject>STANFORD SYNCHROTRON RADIATION LABORATORY</subject><subject>SYNTHESIS</subject><issn>0020-1669</issn><issn>1520-510X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2002</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNpt0E1Lw0AQBuBFFK3Vg39A4sGDYHQmm03SY6nfKBar4Mllu5nQ1XYjuxuw_npTI3rxNAPzzAy8jO0hnCAkeGo0IHJMszXWQ5FALBCe11kPoO0xywZbbNv7VwAY8DTbZFuY8DwHnvfYy2Rpw4y88cfRuHGmMloFU9vjSNkymgTX6NA4NY9GM-WUDuTM5zeI6ipqF6Mzs6AwW85L42lOtlbOG6sCRUPbqh22Uam5p92f2mdPF-ePo6v49v7yejS8jVWaYoirhFclcJ1zQUVaZSWUhUJQWpCmJNeKkmmZpFOeUVVwROAcBeKgGOiUCxC8zw66u7UPRnptAumZrq0lHWSBohArc9QZ7WrvHVXy3ZmFckuJIFc5yt8cW7vf2fdmuqDyT_4E14K4A8YH-vidK_cms5znQj6OJ_Lh7ELcjO_GMm39YeeV9vK1bpxt4_jn8RcRcYjX</recordid><startdate>20021021</startdate><enddate>20021021</enddate><creator>Gailer, Jürgen</creator><creator>George, Graham N</creator><creator>Harris, Hugh H</creator><creator>Pickering, Ingrid J</creator><creator>Prince, Roger C</creator><creator>Somogyi, Arpad</creator><creator>Buttigieg, Gavin A</creator><creator>Glass, Richard S</creator><creator>Denton, M. Bonner</creator><general>American Chemical Society</general><scope>BSCLL</scope><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>OTOTI</scope></search><sort><creationdate>20021021</creationdate><title>Synthesis, Purification, and Structural Characterization of the Dimethyldiselenoarsinate Anion</title><author>Gailer, Jürgen ; George, Graham N ; Harris, Hugh H ; Pickering, Ingrid J ; Prince, Roger C ; Somogyi, Arpad ; Buttigieg, Gavin A ; Glass, Richard S ; Denton, M. Bonner</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-a441t-f23fd03c735e84f6d0d8a10ac5ece27cae2bd24b36ef83110331511989c435053</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2002</creationdate><topic>ANIONS</topic><topic>ARSENIC OXIDES</topic><topic>Chromatography, Gel</topic><topic>Environmental Pollutants - analysis</topic><topic>Hydrogen-Ion Concentration</topic><topic>Indicators and Reagents</topic><topic>INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY</topic><topic>Magnetic Resonance Spectroscopy</topic><topic>Mass Spectrometry</topic><topic>MOLECULAR STRUCTURE</topic><topic>ORGANOMETALLIC COMPOUNDS</topic><topic>PURIFICATION</topic><topic>SELENIUM COMPOUNDS</topic><topic>Selenium Radioisotopes - chemistry</topic><topic>Solutions</topic><topic>STANFORD SYNCHROTRON RADIATION LABORATORY</topic><topic>SYNTHESIS</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Gailer, Jürgen</creatorcontrib><creatorcontrib>George, Graham N</creatorcontrib><creatorcontrib>Harris, Hugh H</creatorcontrib><creatorcontrib>Pickering, Ingrid J</creatorcontrib><creatorcontrib>Prince, Roger C</creatorcontrib><creatorcontrib>Somogyi, Arpad</creatorcontrib><creatorcontrib>Buttigieg, Gavin A</creatorcontrib><creatorcontrib>Glass, Richard S</creatorcontrib><creatorcontrib>Denton, M. Bonner</creatorcontrib><creatorcontrib>Stanford Synchrotron Radiation Lab. (US)</creatorcontrib><creatorcontrib>Stanford Linear Accelerator Center, Menlo Park, CA (US)</creatorcontrib><collection>Istex</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>OSTI.GOV</collection><jtitle>Inorganic Chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Gailer, Jürgen</au><au>George, Graham N</au><au>Harris, Hugh H</au><au>Pickering, Ingrid J</au><au>Prince, Roger C</au><au>Somogyi, Arpad</au><au>Buttigieg, Gavin A</au><au>Glass, Richard S</au><au>Denton, M. Bonner</au><aucorp>Stanford Synchrotron Radiation Lab. (US)</aucorp><aucorp>Stanford Linear Accelerator Center, Menlo Park, CA (US)</aucorp><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Synthesis, Purification, and Structural Characterization of the Dimethyldiselenoarsinate Anion</atitle><jtitle>Inorganic Chemistry</jtitle><addtitle>Inorg. Chem</addtitle><date>2002-10-21</date><risdate>2002</risdate><volume>41</volume><issue>21</issue><spage>5426</spage><epage>5432</epage><pages>5426-5432</pages><issn>0020-1669</issn><eissn>1520-510X</eissn><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.</abstract><cop>United States</cop><pub>American Chemical Society</pub><pmid>12377037</pmid><doi>10.1021/ic0113146</doi><tpages>7</tpages></addata></record> |
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| subjects | ANIONS ARSENIC OXIDES Chromatography, Gel Environmental Pollutants - analysis Hydrogen-Ion Concentration Indicators and Reagents INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY Magnetic Resonance Spectroscopy Mass Spectrometry MOLECULAR STRUCTURE ORGANOMETALLIC COMPOUNDS PURIFICATION SELENIUM COMPOUNDS Selenium Radioisotopes - chemistry Solutions STANFORD SYNCHROTRON RADIATION LABORATORY SYNTHESIS |
| title | Synthesis, Purification, and Structural Characterization of the Dimethyldiselenoarsinate Anion |
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