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Synthesis and Solid-State NMR Studies of P-Vinylbenzylphosphonic Acid
P‐Vinylbenzylphosphonic acid (2) was synthesized and crystallized in two phases A and B. The latter phase was easily converted into the former. Both phases were investigated by IR and solid‐state 31P and 1H NMR spectroscopy, and X‐ray crystallography. The use of recently developed NMR methods has en...
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Published in: | Chemistry : a European journal 2003-02, Vol.9 (3), p.770-775 |
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container_title | Chemistry : a European journal |
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creator | Frantz, Richard Durand, Jean-Olivier Carré, Francis Lanneau, Gérard F. Bideau, Jean Le Alonso, Bruno Massiot, Dominique |
description | P‐Vinylbenzylphosphonic acid (2) was synthesized and crystallized in two phases A and B. The latter phase was easily converted into the former. Both phases were investigated by IR and solid‐state 31P and 1H NMR spectroscopy, and X‐ray crystallography. The use of recently developed NMR methods has enabled us to increase the usually poor resolution of solid‐state 1H spectra. This gave additional insights on the proton environments. In particular, two dimensional 2D 1H‐31P heteronuclear correlation (HETCOR) experiments, incorporating a Lee–Golburg homonuclear decoupling scheme, allowed description of the mixture of phase A and B.
Recent developments of high‐resolution solid‐state NMR techniques have made it a useful tool for the elucidation of crystalline and amorphous structures of materials. The use of these techniques, in particular, allows a more accurate description of the proton environments in solids. P‐Vinylbenzylphosphonic acid (shown here) was synthesized and crystallized in two phases. Its behavior in the solid state was investigated by X‐ray diffraction and solid‐state NMR spectroscopy. |
doi_str_mv | 10.1002/chem.200390086 |
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Recent developments of high‐resolution solid‐state NMR techniques have made it a useful tool for the elucidation of crystalline and amorphous structures of materials. The use of these techniques, in particular, allows a more accurate description of the proton environments in solids. P‐Vinylbenzylphosphonic acid (shown here) was synthesized and crystallized in two phases. Its behavior in the solid state was investigated by X‐ray diffraction and solid‐state NMR spectroscopy.</description><identifier>ISSN: 0947-6539</identifier><identifier>EISSN: 1521-3765</identifier><identifier>DOI: 10.1002/chem.200390086</identifier><identifier>PMID: 12569470</identifier><language>eng</language><publisher>Weinheim: WILEY-VCH Verlag</publisher><subject>Chemical Sciences ; NMR spectroscopy ; phosphonic acid ; structure elucidation ; styrene</subject><ispartof>Chemistry : a European journal, 2003-02, Vol.9 (3), p.770-775</ispartof><rights>2002 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim</rights><rights>Distributed under a Creative Commons Attribution 4.0 International License</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c4146-368d59d5409c563fe517120cca918e05e72a49205ada00feaa963af0b6353b863</citedby><cites>FETCH-LOGICAL-c4146-368d59d5409c563fe517120cca918e05e72a49205ada00feaa963af0b6353b863</cites><orcidid>0000-0003-1207-7040 ; 0000-0002-3430-1931 ; 0000-0003-4606-2576</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://onlinelibrary.wiley.com/doi/full/10.1002%2Fchem.200390086$$EHTML$$P50$$Gwiley$$H</linktohtml><link.rule.ids>230,315,786,790,891,27957,27958,51032</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/12569470$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink><backlink>$$Uhttps://hal.science/hal-02049167$$DView record in HAL$$Hfree_for_read</backlink></links><search><creatorcontrib>Frantz, Richard</creatorcontrib><creatorcontrib>Durand, Jean-Olivier</creatorcontrib><creatorcontrib>Carré, Francis</creatorcontrib><creatorcontrib>Lanneau, Gérard F.</creatorcontrib><creatorcontrib>Bideau, Jean Le</creatorcontrib><creatorcontrib>Alonso, Bruno</creatorcontrib><creatorcontrib>Massiot, Dominique</creatorcontrib><title>Synthesis and Solid-State NMR Studies of P-Vinylbenzylphosphonic Acid</title><title>Chemistry : a European journal</title><addtitle>Chemistry - A European Journal</addtitle><description>P‐Vinylbenzylphosphonic acid (2) was synthesized and crystallized in two phases A and B. The latter phase was easily converted into the former. Both phases were investigated by IR and solid‐state 31P and 1H NMR spectroscopy, and X‐ray crystallography. The use of recently developed NMR methods has enabled us to increase the usually poor resolution of solid‐state 1H spectra. This gave additional insights on the proton environments. In particular, two dimensional 2D 1H‐31P heteronuclear correlation (HETCOR) experiments, incorporating a Lee–Golburg homonuclear decoupling scheme, allowed description of the mixture of phase A and B.
Recent developments of high‐resolution solid‐state NMR techniques have made it a useful tool for the elucidation of crystalline and amorphous structures of materials. The use of these techniques, in particular, allows a more accurate description of the proton environments in solids. P‐Vinylbenzylphosphonic acid (shown here) was synthesized and crystallized in two phases. 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The latter phase was easily converted into the former. Both phases were investigated by IR and solid‐state 31P and 1H NMR spectroscopy, and X‐ray crystallography. The use of recently developed NMR methods has enabled us to increase the usually poor resolution of solid‐state 1H spectra. This gave additional insights on the proton environments. In particular, two dimensional 2D 1H‐31P heteronuclear correlation (HETCOR) experiments, incorporating a Lee–Golburg homonuclear decoupling scheme, allowed description of the mixture of phase A and B.
Recent developments of high‐resolution solid‐state NMR techniques have made it a useful tool for the elucidation of crystalline and amorphous structures of materials. The use of these techniques, in particular, allows a more accurate description of the proton environments in solids. P‐Vinylbenzylphosphonic acid (shown here) was synthesized and crystallized in two phases. Its behavior in the solid state was investigated by X‐ray diffraction and solid‐state NMR spectroscopy.</abstract><cop>Weinheim</cop><pub>WILEY-VCH Verlag</pub><pmid>12569470</pmid><doi>10.1002/chem.200390086</doi><tpages>6</tpages><orcidid>https://orcid.org/0000-0003-1207-7040</orcidid><orcidid>https://orcid.org/0000-0002-3430-1931</orcidid><orcidid>https://orcid.org/0000-0003-4606-2576</orcidid></addata></record> |
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subjects | Chemical Sciences NMR spectroscopy phosphonic acid structure elucidation styrene |
title | Synthesis and Solid-State NMR Studies of P-Vinylbenzylphosphonic Acid |
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