Assignments of solid-state 13C resonances for polymorphs of cortisone acetate using shielding tensor components
Carbon-13 CP MAS spectra have been obtained for seven polymorphic and solvated forms of cortisone acetate. For signals in the high-frequency region, the spinning sideband manifolds of the spectra recorded under slow-spinning conditions have been analysed to obtain the shielding tensor components for...
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| Veröffentlicht in: | Solid state nuclear magnetic resonance 1992-06, Vol.1 (2), p.93-101 |
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| container_title | Solid state nuclear magnetic resonance |
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| creator | Christopher, Elizabeth A. Harris, Robin K. Fletton, Richard A. |
| description | Carbon-13
CP
MAS
spectra have been obtained for seven polymorphic and solvated forms of cortisone acetate. For signals in the high-frequency region, the spinning sideband manifolds of the spectra recorded under slow-spinning conditions have been analysed to obtain the shielding tensor components for the five resonances at the highest frequency. These show characteristics values for given types of carbon and have enabled assignments of the C5 and C22 signals to be made with some certainty, providing firm evidence of cross-over between the shifts for these carbons between different polymorphs. Assignments are suggested more tentatively for the resonances from C3, C11 and C20. Comparison of chemical shifts for those forms with published X-ray structures enables conclusions to be drawn regarding hydrogen bonding in the remaining forms. Hydrogen bonding induces a high-frequency change in the isotropic chemical shift of ∼3 ppm. |
| doi_str_mv | 10.1016/0926-2040(92)90021-Z |
| format | Article |
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CP
MAS
spectra have been obtained for seven polymorphic and solvated forms of cortisone acetate. For signals in the high-frequency region, the spinning sideband manifolds of the spectra recorded under slow-spinning conditions have been analysed to obtain the shielding tensor components for the five resonances at the highest frequency. These show characteristics values for given types of carbon and have enabled assignments of the C5 and C22 signals to be made with some certainty, providing firm evidence of cross-over between the shifts for these carbons between different polymorphs. Assignments are suggested more tentatively for the resonances from C3, C11 and C20. Comparison of chemical shifts for those forms with published X-ray structures enables conclusions to be drawn regarding hydrogen bonding in the remaining forms. Hydrogen bonding induces a high-frequency change in the isotropic chemical shift of ∼3 ppm.</description><identifier>ISSN: 0926-2040</identifier><identifier>EISSN: 1527-3326</identifier><identifier>DOI: 10.1016/0926-2040(92)90021-Z</identifier><identifier>PMID: 1365721</identifier><language>eng</language><publisher>Netherlands: Elsevier Inc</publisher><subject>[formula omitted] spectra ; Carbon - chemistry ; Carbon Isotopes ; Cortisone - analogs & derivatives ; Cortisone - chemistry ; cortisone acetate ; Crystallography, X-Ray ; Hydrogen Bonding ; Magnetic Resonance Spectroscopy - methods ; Molecular Structure ; shielding tensor components ; spectral assignment ; spinning sideband analysis</subject><ispartof>Solid state nuclear magnetic resonance, 1992-06, Vol.1 (2), p.93-101</ispartof><rights>1992</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c2041-7b06fe577cfcef214ba66a96366f879474f321fd0e8df0aa78c7027eae191c5d3</citedby><cites>FETCH-LOGICAL-c2041-7b06fe577cfcef214ba66a96366f879474f321fd0e8df0aa78c7027eae191c5d3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/0926-2040(92)90021-Z$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,777,781,3537,27905,27906,45976</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/1365721$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Christopher, Elizabeth A.</creatorcontrib><creatorcontrib>Harris, Robin K.</creatorcontrib><creatorcontrib>Fletton, Richard A.</creatorcontrib><title>Assignments of solid-state 13C resonances for polymorphs of cortisone acetate using shielding tensor components</title><title>Solid state nuclear magnetic resonance</title><addtitle>Solid State Nucl Magn Reson</addtitle><description>Carbon-13
CP
MAS
spectra have been obtained for seven polymorphic and solvated forms of cortisone acetate. For signals in the high-frequency region, the spinning sideband manifolds of the spectra recorded under slow-spinning conditions have been analysed to obtain the shielding tensor components for the five resonances at the highest frequency. These show characteristics values for given types of carbon and have enabled assignments of the C5 and C22 signals to be made with some certainty, providing firm evidence of cross-over between the shifts for these carbons between different polymorphs. Assignments are suggested more tentatively for the resonances from C3, C11 and C20. Comparison of chemical shifts for those forms with published X-ray structures enables conclusions to be drawn regarding hydrogen bonding in the remaining forms. Hydrogen bonding induces a high-frequency change in the isotropic chemical shift of ∼3 ppm.</description><subject>[formula omitted] spectra</subject><subject>Carbon - chemistry</subject><subject>Carbon Isotopes</subject><subject>Cortisone - analogs & derivatives</subject><subject>Cortisone - chemistry</subject><subject>cortisone acetate</subject><subject>Crystallography, X-Ray</subject><subject>Hydrogen Bonding</subject><subject>Magnetic Resonance Spectroscopy - methods</subject><subject>Molecular Structure</subject><subject>shielding tensor components</subject><subject>spectral assignment</subject><subject>spinning sideband analysis</subject><issn>0926-2040</issn><issn>1527-3326</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>1992</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNp9kEtLAzEUhYMotVb_gcKsRBejSWYm6WyEUnxBwY1uuglp5qaNzEzG3KnQf2_6QHducgPnnPv4CLlk9I5RJu5pyUXKaU5vSn5bUspZOj8iQ1ZwmWYZF8dk-Gs5JWeIn5RSyTIxIIP4FpKzIfETRLdsG2h7TLxN0NeuSrHXPSQsmyYB0Le6NYCJ9SHpfL1pfOhWO7PxoXdRh0Qb2EXW6NplgisHdbX99dBijBnfdNEWZ5yTE6trhItDHZGPp8f36Us6e3t-nU5mqYnrslQuqLBQSGmsActZvtBC6FJkQtixLHOZ24wzW1EYV5ZqLcdGUi5BAyuZKapsRK73fbvgv9aAvWocGqhr3YJfo5JFwcuxpNGY740meMQAVnXBNTpsFKNqy1ltIaotRFVyteOs5jF2dei_XjRQ_YX2YKP-sNchHvntICg0DiLHygUwvaq8-3_AD7DUjrw</recordid><startdate>199206</startdate><enddate>199206</enddate><creator>Christopher, Elizabeth A.</creator><creator>Harris, Robin K.</creator><creator>Fletton, Richard A.</creator><general>Elsevier Inc</general><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>7X8</scope></search><sort><creationdate>199206</creationdate><title>Assignments of solid-state 13C resonances for polymorphs of cortisone acetate using shielding tensor components</title><author>Christopher, Elizabeth A. ; Harris, Robin K. ; Fletton, Richard A.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c2041-7b06fe577cfcef214ba66a96366f879474f321fd0e8df0aa78c7027eae191c5d3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>1992</creationdate><topic>[formula omitted] spectra</topic><topic>Carbon - chemistry</topic><topic>Carbon Isotopes</topic><topic>Cortisone - analogs & derivatives</topic><topic>Cortisone - chemistry</topic><topic>cortisone acetate</topic><topic>Crystallography, X-Ray</topic><topic>Hydrogen Bonding</topic><topic>Magnetic Resonance Spectroscopy - methods</topic><topic>Molecular Structure</topic><topic>shielding tensor components</topic><topic>spectral assignment</topic><topic>spinning sideband analysis</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Christopher, Elizabeth A.</creatorcontrib><creatorcontrib>Harris, Robin K.</creatorcontrib><creatorcontrib>Fletton, Richard A.</creatorcontrib><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><jtitle>Solid state nuclear magnetic resonance</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Christopher, Elizabeth A.</au><au>Harris, Robin K.</au><au>Fletton, Richard A.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Assignments of solid-state 13C resonances for polymorphs of cortisone acetate using shielding tensor components</atitle><jtitle>Solid state nuclear magnetic resonance</jtitle><addtitle>Solid State Nucl Magn Reson</addtitle><date>1992-06</date><risdate>1992</risdate><volume>1</volume><issue>2</issue><spage>93</spage><epage>101</epage><pages>93-101</pages><issn>0926-2040</issn><eissn>1527-3326</eissn><abstract>Carbon-13
CP
MAS
spectra have been obtained for seven polymorphic and solvated forms of cortisone acetate. For signals in the high-frequency region, the spinning sideband manifolds of the spectra recorded under slow-spinning conditions have been analysed to obtain the shielding tensor components for the five resonances at the highest frequency. These show characteristics values for given types of carbon and have enabled assignments of the C5 and C22 signals to be made with some certainty, providing firm evidence of cross-over between the shifts for these carbons between different polymorphs. Assignments are suggested more tentatively for the resonances from C3, C11 and C20. Comparison of chemical shifts for those forms with published X-ray structures enables conclusions to be drawn regarding hydrogen bonding in the remaining forms. Hydrogen bonding induces a high-frequency change in the isotropic chemical shift of ∼3 ppm.</abstract><cop>Netherlands</cop><pub>Elsevier Inc</pub><pmid>1365721</pmid><doi>10.1016/0926-2040(92)90021-Z</doi><tpages>9</tpages></addata></record> |
| fulltext | fulltext |
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| ispartof | Solid state nuclear magnetic resonance, 1992-06, Vol.1 (2), p.93-101 |
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| language | eng |
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| source | MEDLINE; Elsevier ScienceDirect Journals |
| subjects | [formula omitted] spectra Carbon - chemistry Carbon Isotopes Cortisone - analogs & derivatives Cortisone - chemistry cortisone acetate Crystallography, X-Ray Hydrogen Bonding Magnetic Resonance Spectroscopy - methods Molecular Structure shielding tensor components spectral assignment spinning sideband analysis |
| title | Assignments of solid-state 13C resonances for polymorphs of cortisone acetate using shielding tensor components |
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