Optimal 2H rf pulses and 2H-13C cross-polarization methods for solid-state 2H MAS NMR of perdeuterated proteins

Daxiu Wei, Ümit Akbey, Berit Paaske, Hartmut Oschkinat, Bernd Reif, Morten Bjerring, Niels Chr Nielsen

Research output: Contribution to journalArticlepeer-review

37 Scopus citations

Abstract

We present a novel concept for rf pulses and optimal control designed cross-polarization experiments for quadrupolar nuclei. The methods are demonstrated for 2H CP-MAS and 2H multiple-pulse NMR of perdeuterated proteins, for which sensitivity enhancements up to an order of magnitude are presented relative to commonly used approaches. The so-called RESPIRATION rf pulses combines the concept of short broad-band pulses with generation of pulses with large flip angles through distribution of the rf pulse over several rotor echoes. This lead to close-to-ideal rf pulses, facilitating implementation of experiments relying on the ability to realize high-performance 90 and 180° pulses, as, for example, in refocused INEPT and double-to-single quantum coherence experiments, or just pulses that provide a true representation of the quadrupolar powder pattern to extract information about the structure or dynamics. The optimal control 2H ↔ 13C CP-MAS method demonstrates transfer efficiencies up to around 85% while being extremely robust toward rf inhomogeneity and resonance offsets.

Original languageEnglish
Pages (from-to)1289-1294
Number of pages6
JournalJournal of Physical Chemistry Letters
Volume2
Issue number11
DOIs
StatePublished - 2 Jun 2011

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