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Measurement of Internuclear Distances in Solid-State NMR by a Background-Filtered REDOR Experiment

✍ Scribed by Frederick G Vogt; Susan M Mattingly; James M Gibson; Karl T Mueller

Publisher
Elsevier Science
Year
2000
Tongue
English
Weight
106 KB
Volume
147
Category
Article
ISSN
1090-7807

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✦ Synopsis

A background-filtered version of the rotational-echo double resonance (REDOR) experiment is demonstrated. The experiment combines a traditional REDOR pulse sequence with a double-cross-polarization (DCP) sequence to select only those signals coming from spin pairs of interest. The relatively inefficient DCP sequence, which transfers polarization from (1)H to (15)N and subsequently to (13)C, is improved by the use of adiabatic passages through the (-1) sideband of the Hartmann-Hahn matching condition. The result is an efficient 2D-REDOR pulse sequence that does not require a reference experiment for removal of background signals. The data produced by the experiment are ideally suited to analysis by newly developed dipolar transform methods, such as the REDOR transform. The relevant features of the experiment are demonstrated on simple labeled amino acids. Relative efficiencies of several other potential filtering methods are also compared. Copyright 2000 Academic Press.

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