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 Rossini, Aaron
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 Sadow, Aaron
dc.contributor.author Rossini, Aaron
dc.contributor.department Ames Laboratory
dc.contributor.department Chemistry
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
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relation.isAuthorOfPublication a9d328ff-ec5e-4d1d-8c2f-aed9d5a290ed
relation.isOrgUnitOfPublication 25913818-6714-4be5-89a6-f70c8facdf7e
relation.isOrgUnitOfPublication 42864f6e-7a3d-4be3-8b5a-0ae3c3830a11
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