Enhancing the Sensitivity of Solid-State NMR Experiments with Very Low Gyromagnetic Ratio Nuclei with Fast Magic Angle Spinning and Proton Detection
dc.contributor.author | Venkatesh, Amrit | |
dc.contributor.author | Ryan, Matthew | |
dc.contributor.author | Biswas, Abhranil | |
dc.contributor.author | Boteju, Kasuni | |
dc.contributor.author | Sadow, Aaron | |
dc.contributor.author | Rossini, Aaron | |
dc.contributor.department | Ames National Laboratory | |
dc.contributor.department | Chemistry | |
dc.contributor.department | Ames Laboratory | |
dc.date | 2018-07-13T02:45:10.000 | |
dc.date.accessioned | 2020-06-29T23:21:15Z | |
dc.date.available | 2020-06-29T23:21:15Z | |
dc.date.embargo | 2019-06-04 | |
dc.date.issued | 2018-06-04 | |
dc.description.abstract | <p>Many transition metals commonly encountered in inorganic materials and organometallic compounds possess NMR-active nuclei with very low gyromagnetic ratios (γ) such as 89Y, 103Rh, 109Ag, and 183W. A low-γ leads to poor NMR sensitivity and other experimental challenges. Consequently, nuclei with low-γ are often impossible to study with conventional solid-state NMR methods. Here, we combine fast magic angle spinning (MAS) and proton detection to enhance the sensitivity of solid-state NMR experiments with very low-γ nuclei by 1–2 orders of magnitude. Coherence transfer between 1H and low-γ nuclei was performed with low-power double quantum (DQ) or zero quantum (ZQ) cross-polarization (CP) or dipolar refocused insensitive nuclei enhanced by polarization transfer (D-RINEPT). Comparison of the absolute sensitivity of CP NMR experiments performed with proton detection with 1.3 mm rotors and direct detection with 4 mm rotors shows that proton detection with a 1.3 mm rotor provides a significant boost in absolute sensitivity, while requiring approximately 1/40th of the material required to fill a 4 mm rotor. Fast MAS and proton detection were applied to obtain 89Y and 103Rh solid-state NMR spectra of organometallic complexes. These results demonstrate that proton detection and fast MAS represents a general approach to enable and accelerate solid-state NMR experiments with very low-γ nuclei.</p> | |
dc.identifier | archive/lib.dr.iastate.edu/ameslab_manuscripts/194/ | |
dc.identifier.articleid | 1199 | |
dc.identifier.contextkey | 12478897 | |
dc.identifier.s3bucket | isulib-bepress-aws-west | |
dc.identifier.submissionpath | ameslab_manuscripts/194 | |
dc.identifier.uri | https://dr.lib.iastate.edu/handle/20.500.12876/7116 | |
dc.language.iso | en | |
dc.relation.ispartofseries | IS-J 9683 | |
dc.source.bitstream | archive/lib.dr.iastate.edu/ameslab_manuscripts/194/IS_J_9683.pdf|||Fri Jan 14 21:56:21 UTC 2022 | |
dc.source.uri | 10.1021/acs.jpca.8b05107 | |
dc.subject.disciplines | Chemistry | |
dc.subject.disciplines | Physical Chemistry | |
dc.subject.disciplines | Radiochemistry | |
dc.title | Enhancing the Sensitivity of Solid-State NMR Experiments with Very Low Gyromagnetic Ratio Nuclei with Fast Magic Angle Spinning and Proton Detection | |
dc.type | article | |
dc.type.genre | article | |
dspace.entity.type | Publication | |
relation.isAuthorOfPublication | a9d328ff-ec5e-4d1d-8c2f-aed9d5a290ed | |
relation.isAuthorOfPublication | f6703e72-8e9d-40df-b839-5a9ab4da888d | |
relation.isOrgUnitOfPublication | 25913818-6714-4be5-89a6-f70c8facdf7e | |
relation.isOrgUnitOfPublication | 42864f6e-7a3d-4be3-8b5a-0ae3c3830a11 |
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