{"title":"Highly sensitive measurements of methylene dynamics with a frequency-selective double-quantum sideband method","authors":"Jacob Mayer , Frédéric A. Perras","doi":"10.1016/j.ssnmr.2025.101994","DOIUrl":null,"url":null,"abstract":"<div><div>Probing the fast dynamics of surface sites using NMR spectroscopy is highly challenging owing to the sites' high dilution and the difficulties often associated with isotopic enrichment. Intra-CH<sub>2</sub> <sup>1</sup>H–<sup>1</sup>H dipolar couplings are ideal probes of motions given that they only involve <sup>1</sup>H's and the tensor has a well-defined size and orientation. We introduce a frequency-selective variant of the double-quantum sideband method to measure like-spin <sup>1</sup>H–<sup>1</sup>H dipolar coupling constants. The experiment dramatically reduces the instrument time required to measure dynamically-averaged intra-CH<sub>2</sub> dipolar couplings. We demonstrate the performance of the sequence using silica-supported silanes as model highly-mobile surface species.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"136 ","pages":"Article 101994"},"PeriodicalIF":1.8000,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Solid state nuclear magnetic resonance","FirstCategoryId":"92","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0926204025000104","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CHEMISTRY, PHYSICAL","Score":null,"Total":0}
引用次数: 0
Abstract
Probing the fast dynamics of surface sites using NMR spectroscopy is highly challenging owing to the sites' high dilution and the difficulties often associated with isotopic enrichment. Intra-CH21H–1H dipolar couplings are ideal probes of motions given that they only involve 1H's and the tensor has a well-defined size and orientation. We introduce a frequency-selective variant of the double-quantum sideband method to measure like-spin 1H–1H dipolar coupling constants. The experiment dramatically reduces the instrument time required to measure dynamically-averaged intra-CH2 dipolar couplings. We demonstrate the performance of the sequence using silica-supported silanes as model highly-mobile surface species.
期刊介绍：
The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.
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