Accurate heteronuclear distance measurements at all magic-angle spinning frequencies in solid-state NMR spectroscopy |
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Authors: | Lixin Liang Yi Ji Zhenchao Zhao Caitlin M. Quinn Xiuwen Han Xinhe Bao Tatyana Polenova Guangjin Hou |
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Affiliation: | State Key Laboratory of Catalysis, National Laboratory for Clean Energy, 2011-Collaborative Innovation Center of Chemistry for Energy Materials, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Zhongshan Road 457, Dalian 116023 China.; University of Chinese Academy of Sciences, Beijing 100049 China ; Department of Chemistry and Biochemistry, University of Delaware, Newark Delaware 19716 USA |
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Abstract: | Heteronuclear dipolar coupling is indispensable in revealing vital information related to the molecular structure and dynamics, as well as intermolecular interactions in various solid materials. Although numerous approaches have been developed to selectively reintroduce heteronuclear dipolar coupling under MAS, most of them lack universality and can only be applied to limited spin systems. Herein, we introduce a new and robust technique dubbed phase modulated rotary resonance (PMRR) for reintroducing heteronuclear dipolar couplings while suppressing all other interactions under a broad range of MAS conditions. The standard PMRR requires the radiofrequency (RF) field strength of only twice the MAS frequency, can efficiently recouple the dipolar couplings with a large scaling factor of 0.50, and is robust to experimental imperfections. Moreover, the adjustable window modification of PMRR, dubbed wPMRR, can improve its performance remarkably, making it well suited for the accurate determination of dipolar couplings in various spin systems. The robust performance of such pulse sequences has been verified theoretically and experimentally via model compounds, at different MAS frequencies. The application of the PMRR technique was demonstrated on the H-ZSM-5 zeolite, where the interaction between the Brønsted acidic hydroxyl groups of H-ZSM-5 and the absorbed trimethylphosphine oxide (TMPO) were probed, revealing the detailed configuration of super acid sites.A new and robust technique dubbed phase modulated rotary resonance (PMRR) was proposed for the accurate determination of heteronuclear dipolar coupling under a broad range of MAS conditions in solid-state NMR spectroscopy. |
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