Structural Insights into Bound Water in Crystalline Amino Acids: Experimental and Theoretical [superscript 17] O NMR
We demonstrate here that the [superscript 17]O NMR properties of bound water in a series of amino acids and dipeptides can be determined with a combination of nonspinning and magic-angle spinning experiments using a range of magnetic field strengths from 9.4 to 21.1 T. Furthermore, we propose a [sup...
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| Format: | Article |
| Language: | en_US |
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American Chemical Society (ACS)
2017
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| Online Access: | http://hdl.handle.net/1721.1/108242 https://orcid.org/0000-0002-6708-7660 https://orcid.org/0000-0003-1589-832X |
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| author | Craigen, Kimberley N. Wren, John E. C. Kroeker, Scott Michaelis, Vladimir K. Keeler, Eric George Ong, Ta-Chung Penzel, Susanne Griffin, Robert Guy |
| author2 | Massachusetts Institute of Technology. Department of Chemistry |
| author_facet | Massachusetts Institute of Technology. Department of Chemistry Craigen, Kimberley N. Wren, John E. C. Kroeker, Scott Michaelis, Vladimir K. Keeler, Eric George Ong, Ta-Chung Penzel, Susanne Griffin, Robert Guy |
| author_sort | Craigen, Kimberley N. |
| collection | MIT |
| description | We demonstrate here that the [superscript 17]O NMR properties of bound water in a series of amino acids and dipeptides can be determined with a combination of nonspinning and magic-angle spinning experiments using a range of magnetic field strengths from 9.4 to 21.1 T. Furthermore, we propose a [superscript 17]O chemical shift fingerprint region for bound water molecules in biological solids that is well outside the previously determined ranges for carbonyl, carboxylic, and hydroxyl oxygens, thereby offering the ability to resolve multiple [superscript 17]O environments using rapid one-dimensional NMR techniques. Finally, we compare our experimental data against quantum chemical calculations using GIPAW and hybrid-DFT, finding intriguing discrepancies between the electric field gradients calculated from structures determined by X-ray and neutron diffraction. |
| first_indexed | 2024-09-23T17:15:06Z |
| format | Article |
| id | mit-1721.1/108242 |
| institution | Massachusetts Institute of Technology |
| language | en_US |
| last_indexed | 2024-09-23T17:15:06Z |
| publishDate | 2017 |
| publisher | American Chemical Society (ACS) |
| record_format | dspace |
| spelling | mit-1721.1/1082422022-09-30T00:45:30Z Structural Insights into Bound Water in Crystalline Amino Acids: Experimental and Theoretical [superscript 17] O NMR Craigen, Kimberley N. Wren, John E. C. Kroeker, Scott Michaelis, Vladimir K. Keeler, Eric George Ong, Ta-Chung Penzel, Susanne Griffin, Robert Guy Massachusetts Institute of Technology. Department of Chemistry Michaelis, Vladimir K. Keeler, Eric George Ong, Ta-Chung Penzel, Susanne Griffin, Robert Guy We demonstrate here that the [superscript 17]O NMR properties of bound water in a series of amino acids and dipeptides can be determined with a combination of nonspinning and magic-angle spinning experiments using a range of magnetic field strengths from 9.4 to 21.1 T. Furthermore, we propose a [superscript 17]O chemical shift fingerprint region for bound water molecules in biological solids that is well outside the previously determined ranges for carbonyl, carboxylic, and hydroxyl oxygens, thereby offering the ability to resolve multiple [superscript 17]O environments using rapid one-dimensional NMR techniques. Finally, we compare our experimental data against quantum chemical calculations using GIPAW and hybrid-DFT, finding intriguing discrepancies between the electric field gradients calculated from structures determined by X-ray and neutron diffraction. National Institute of Biomedical Imaging and Bioengineering (U.S.) (grant number: EB-003151) National Institute of Biomedical Imaging and Bioengineering (U.S.) (grant number: EB-001960) National Institute of Biomedical Imaging and Bioengineering (U.S.) (grant number: EB-002026) 2017-04-19T14:18:45Z 2017-04-19T14:18:45Z 2015-05 2015-05 Article http://purl.org/eprint/type/JournalArticle 1520-6106 1520-5207 http://hdl.handle.net/1721.1/108242 Michaelis, Vladimir K., Eric G. Keeler, Ta-Chung Ong, Kimberley N. Craigen, Susanne Penzel, John E. C. Wren, Scott Kroeker, and Robert G. Griffin. "Structural Insights into Bound Water in Crystalline Amino Acids: Experimental and Theoretical [superscript 17] O NMR." The Journal of Physical Chemistry B 119 (25) (2015): pp. 8024-8036. ©2015. https://orcid.org/0000-0002-6708-7660 https://orcid.org/0000-0003-1589-832X en_US http://dx.doi.org/10.1021/acs.jpcb.5b04647 The Journal of Physical Chemistry B Article is made available in accordance with the publisher's policy and may be subject to US copyright law. Please refer to the publisher's site for terms of use. application/pdf American Chemical Society (ACS) PMC |
| spellingShingle | Craigen, Kimberley N. Wren, John E. C. Kroeker, Scott Michaelis, Vladimir K. Keeler, Eric George Ong, Ta-Chung Penzel, Susanne Griffin, Robert Guy Structural Insights into Bound Water in Crystalline Amino Acids: Experimental and Theoretical [superscript 17] O NMR |
| title | Structural Insights into Bound Water in Crystalline Amino Acids: Experimental and Theoretical [superscript 17] O NMR |
| title_full | Structural Insights into Bound Water in Crystalline Amino Acids: Experimental and Theoretical [superscript 17] O NMR |
| title_fullStr | Structural Insights into Bound Water in Crystalline Amino Acids: Experimental and Theoretical [superscript 17] O NMR |
| title_full_unstemmed | Structural Insights into Bound Water in Crystalline Amino Acids: Experimental and Theoretical [superscript 17] O NMR |
| title_short | Structural Insights into Bound Water in Crystalline Amino Acids: Experimental and Theoretical [superscript 17] O NMR |
| title_sort | structural insights into bound water in crystalline amino acids experimental and theoretical superscript 17 o nmr |
| url | http://hdl.handle.net/1721.1/108242 https://orcid.org/0000-0002-6708-7660 https://orcid.org/0000-0003-1589-832X |
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