Ultrahigh-resolution phosphorus-31 NMR
The feasibility of ultrahigh-resolution {sup 31}P NMR on both 200- and 500-MHz ({sup 1}H resonance frequency) instruments is demonstrated. Results indicate that temperature gradients within the sample caused by proton decoupling have severely limited the resolution achieved on commercial instruments...
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Veröffentlicht in: | Journal of the American Chemical Society 1989-09, Vol.111 (19), p.7293-7295 |
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container_title | Journal of the American Chemical Society |
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creator | Maple, Steven R Carson, Jennifer E Allerhand, Adam |
description | The feasibility of ultrahigh-resolution {sup 31}P NMR on both 200- and 500-MHz ({sup 1}H resonance frequency) instruments is demonstrated. Results indicate that temperature gradients within the sample caused by proton decoupling have severely limited the resolution achieved on commercial instruments due to the larger temperature dependence of {sup 31}P chemical shifts exhibited by many phosphorous-containing molecules, relative to {sup 13}C chemical shifts. Conditions are described under which instrumental contributions to the observed line width of as little as 15 MHz are observed. Measurements of {sup 31}P-{sup 13}C scalar coupling constants and {sup 13}C isotope effects on {sup 31}P chemical shifts are presented. |
doi_str_mv | 10.1021/ja00201a001 |
format | Article |
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Results indicate that temperature gradients within the sample caused by proton decoupling have severely limited the resolution achieved on commercial instruments due to the larger temperature dependence of {sup 31}P chemical shifts exhibited by many phosphorous-containing molecules, relative to {sup 13}C chemical shifts. Conditions are described under which instrumental contributions to the observed line width of as little as 15 MHz are observed. Measurements of {sup 31}P-{sup 13}C scalar coupling constants and {sup 13}C isotope effects on {sup 31}P chemical shifts are presented.</description><identifier>ISSN: 0002-7863</identifier><identifier>EISSN: 1520-5126</identifier><identifier>DOI: 10.1021/ja00201a001</identifier><identifier>CODEN: JACSAT</identifier><language>eng</language><publisher>Washington, DC: American Chemical Society</publisher><subject>Atomic and molecular physics ; CALCULATION METHODS ; CHEMICAL SHIFT ; DATA ; DATA ANALYSIS ; Exact sciences and technology ; EXPERIMENTAL DATA ; FREQUENCY RANGE ; INFORMATION ; INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY ; ISOTOPES ; LIGHT NUCLEI ; MAGNETIC RESONANCE ; MEASURING INSTRUMENTS ; MEASURING METHODS ; MHZ RANGE ; MHZ RANGE 100-1000 ; Molecular properties and interactions with photons ; NUCLEAR MAGNETIC RESONANCE ; Nuclear resonance and relaxation ; NUCLEI ; NUMERICAL DATA ; ODD-EVEN NUCLEI ; PHOSPHORUS 31 ; PHOSPHORUS ISOTOPES ; Physics ; RESONANCE ; STABLE ISOTOPES 400200 -- Inorganic, Organic, & Physical Chemistry</subject><ispartof>Journal of the American Chemical Society, 1989-09, Vol.111 (19), p.7293-7295</ispartof><rights>1991 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-a273t-ad5097efeda26c64e9a84c7ba82e6b401d77c7ebfce6d1f0bb1c9ecbcc6093193</citedby></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://pubs.acs.org/doi/pdf/10.1021/ja00201a001$$EPDF$$P50$$Gacs$$H</linktopdf><linktohtml>$$Uhttps://pubs.acs.org/doi/10.1021/ja00201a001$$EHTML$$P50$$Gacs$$H</linktohtml><link.rule.ids>230,314,776,780,881,2752,27053,27901,27902,56713,56763</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=19792421$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.osti.gov/biblio/6709049$$D View this record in Osti.gov$$Hfree_for_read</backlink></links><search><creatorcontrib>Maple, Steven R</creatorcontrib><creatorcontrib>Carson, Jennifer E</creatorcontrib><creatorcontrib>Allerhand, Adam</creatorcontrib><title>Ultrahigh-resolution phosphorus-31 NMR</title><title>Journal of the American Chemical Society</title><addtitle>J. Am. Chem. Soc</addtitle><description>The feasibility of ultrahigh-resolution {sup 31}P NMR on both 200- and 500-MHz ({sup 1}H resonance frequency) instruments is demonstrated. Results indicate that temperature gradients within the sample caused by proton decoupling have severely limited the resolution achieved on commercial instruments due to the larger temperature dependence of {sup 31}P chemical shifts exhibited by many phosphorous-containing molecules, relative to {sup 13}C chemical shifts. Conditions are described under which instrumental contributions to the observed line width of as little as 15 MHz are observed. Measurements of {sup 31}P-{sup 13}C scalar coupling constants and {sup 13}C isotope effects on {sup 31}P chemical shifts are presented.</description><subject>Atomic and molecular physics</subject><subject>CALCULATION METHODS</subject><subject>CHEMICAL SHIFT</subject><subject>DATA</subject><subject>DATA ANALYSIS</subject><subject>Exact sciences and technology</subject><subject>EXPERIMENTAL DATA</subject><subject>FREQUENCY RANGE</subject><subject>INFORMATION</subject><subject>INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY</subject><subject>ISOTOPES</subject><subject>LIGHT NUCLEI</subject><subject>MAGNETIC RESONANCE</subject><subject>MEASURING INSTRUMENTS</subject><subject>MEASURING METHODS</subject><subject>MHZ RANGE</subject><subject>MHZ RANGE 100-1000</subject><subject>Molecular properties and interactions with photons</subject><subject>NUCLEAR MAGNETIC RESONANCE</subject><subject>Nuclear resonance and relaxation</subject><subject>NUCLEI</subject><subject>NUMERICAL DATA</subject><subject>ODD-EVEN NUCLEI</subject><subject>PHOSPHORUS 31</subject><subject>PHOSPHORUS ISOTOPES</subject><subject>Physics</subject><subject>RESONANCE</subject><subject>STABLE ISOTOPES 400200 -- Inorganic, Organic, & Physical Chemistry</subject><issn>0002-7863</issn><issn>1520-5126</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>1989</creationdate><recordtype>article</recordtype><recordid>eNptkE1LxDAQhoMouK6e_AOLoB4kOknbZHOU9Rs_FndXwUtIp6ntWtsl6YL-e7NU1IOHmWF4n_ngJWSXwTEDzk7mBoADC5mtkR5LONCEcbFOehAEKoci2iRb3s9DG_Mh65GDWdU6U5SvBXXWN9WyLZt6sCgaH8ItPY3Y4P7ucZts5Kbydue79sns4nw6uqK3D5fXo9NbariMWmqyBJS0uc0MFyhiq8wwRpmaIbcijYFlUqK0aY5WZCyHNGWoLKaIAlTEVNQne93exrel9li2Fgts6tpiq4UEBfEKOuogdI33zuZ64cp34z41A73yQf_xIdD7Hb0wHk2VO1Nj6X9HlFQ85iuOdlzpW_vxoxv3Fg5HMtHT8URD_DJ-ej670ZPAH3a8Qa_nzdLVwZh_P_gC43p3rw</recordid><startdate>19890901</startdate><enddate>19890901</enddate><creator>Maple, Steven R</creator><creator>Carson, Jennifer E</creator><creator>Allerhand, Adam</creator><general>American Chemical Society</general><scope>BSCLL</scope><scope>IQODW</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>OTOTI</scope></search><sort><creationdate>19890901</creationdate><title>Ultrahigh-resolution phosphorus-31 NMR</title><author>Maple, Steven R ; Carson, Jennifer E ; Allerhand, Adam</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-a273t-ad5097efeda26c64e9a84c7ba82e6b401d77c7ebfce6d1f0bb1c9ecbcc6093193</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>1989</creationdate><topic>Atomic and molecular physics</topic><topic>CALCULATION METHODS</topic><topic>CHEMICAL SHIFT</topic><topic>DATA</topic><topic>DATA ANALYSIS</topic><topic>Exact sciences and technology</topic><topic>EXPERIMENTAL DATA</topic><topic>FREQUENCY RANGE</topic><topic>INFORMATION</topic><topic>INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY</topic><topic>ISOTOPES</topic><topic>LIGHT NUCLEI</topic><topic>MAGNETIC RESONANCE</topic><topic>MEASURING INSTRUMENTS</topic><topic>MEASURING METHODS</topic><topic>MHZ RANGE</topic><topic>MHZ RANGE 100-1000</topic><topic>Molecular properties and interactions with photons</topic><topic>NUCLEAR MAGNETIC RESONANCE</topic><topic>Nuclear resonance and relaxation</topic><topic>NUCLEI</topic><topic>NUMERICAL DATA</topic><topic>ODD-EVEN NUCLEI</topic><topic>PHOSPHORUS 31</topic><topic>PHOSPHORUS ISOTOPES</topic><topic>Physics</topic><topic>RESONANCE</topic><topic>STABLE ISOTOPES 400200 -- Inorganic, Organic, & Physical Chemistry</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Maple, Steven R</creatorcontrib><creatorcontrib>Carson, Jennifer E</creatorcontrib><creatorcontrib>Allerhand, Adam</creatorcontrib><collection>Istex</collection><collection>Pascal-Francis</collection><collection>CrossRef</collection><collection>OSTI.GOV</collection><jtitle>Journal of the American Chemical Society</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Maple, Steven R</au><au>Carson, Jennifer E</au><au>Allerhand, Adam</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Ultrahigh-resolution phosphorus-31 NMR</atitle><jtitle>Journal of the American Chemical Society</jtitle><addtitle>J. Am. Chem. Soc</addtitle><date>1989-09-01</date><risdate>1989</risdate><volume>111</volume><issue>19</issue><spage>7293</spage><epage>7295</epage><pages>7293-7295</pages><issn>0002-7863</issn><eissn>1520-5126</eissn><coden>JACSAT</coden><abstract>The feasibility of ultrahigh-resolution {sup 31}P NMR on both 200- and 500-MHz ({sup 1}H resonance frequency) instruments is demonstrated. Results indicate that temperature gradients within the sample caused by proton decoupling have severely limited the resolution achieved on commercial instruments due to the larger temperature dependence of {sup 31}P chemical shifts exhibited by many phosphorous-containing molecules, relative to {sup 13}C chemical shifts. Conditions are described under which instrumental contributions to the observed line width of as little as 15 MHz are observed. Measurements of {sup 31}P-{sup 13}C scalar coupling constants and {sup 13}C isotope effects on {sup 31}P chemical shifts are presented.</abstract><cop>Washington, DC</cop><pub>American Chemical Society</pub><doi>10.1021/ja00201a001</doi><tpages>3</tpages></addata></record> |
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subjects | Atomic and molecular physics CALCULATION METHODS CHEMICAL SHIFT DATA DATA ANALYSIS Exact sciences and technology EXPERIMENTAL DATA FREQUENCY RANGE INFORMATION INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY ISOTOPES LIGHT NUCLEI MAGNETIC RESONANCE MEASURING INSTRUMENTS MEASURING METHODS MHZ RANGE MHZ RANGE 100-1000 Molecular properties and interactions with photons NUCLEAR MAGNETIC RESONANCE Nuclear resonance and relaxation NUCLEI NUMERICAL DATA ODD-EVEN NUCLEI PHOSPHORUS 31 PHOSPHORUS ISOTOPES Physics RESONANCE STABLE ISOTOPES 400200 -- Inorganic, Organic, & Physical Chemistry |
title | Ultrahigh-resolution phosphorus-31 NMR |
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