Longer-range distances by spinning-angle-encoding solid-state NMR spectroscopy

A new spinning-angle-encoding spin-echo solid-state NMR approach is used to accurately determine the dipolar coupling corresponding to a C-C distance over 4 Å in a fully labelled dipeptide. The dipolar coupling dependent spin-echo modulation was recorded off magic angle, switching back to the magic...

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Veröffentlicht in:Physical chemistry chemical physics : PCCP 2011-03, Vol.13 (10), p.4514-4518
Hauptverfasser: BECKER-BALDUS, Johanna, KEMP, Thomas F, PAST, Jaan, REINHOLD, Andres, SAMOSON, Ago, BROWN, Steven P
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Sprache:eng
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Zusammenfassung:A new spinning-angle-encoding spin-echo solid-state NMR approach is used to accurately determine the dipolar coupling corresponding to a C-C distance over 4 Å in a fully labelled dipeptide. The dipolar coupling dependent spin-echo modulation was recorded off magic angle, switching back to the magic angle for the acquisition of the free-induction decay, so as to obtain optimum sensitivity. The retention of both ideal resolution and long-range distance sensitivity was achieved by redesigning a 600 MHz HX MAS NMR probe to provide fast angle switching during the NMR experiment: for 1.8 mm rotors, angle changes of up to ∼5° in ∼10 ms were achieved at 12 kHz MAS. A new experimental design that combines a reference and a dipolar-modulated experiment and a master-curve approach to data interpretation is presented.
ISSN:1463-9076
1463-9084
DOI:10.1039/c0cp02364g