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

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Becker-Baldus, Johanna ; Kemp, Thomas F. ; Past, Jaan ; Reinhold, Andres ; Samoson, Ago ; Brown, Steven P. (2011)

A new spinning-angle-encoding spin-echo solid-state NMR approach is used to accurately determine the\ud dipolar coupling corresponding to a C-C distance over 4 Å in a fully labelled dipeptide. The dipolar coupling\ud dependent spin-echo modulation was recorded off magic angle, switching back to the magic angle for the\ud acquisition of the free-induction decay, so as to obtain optimum sensitivity. The retention of both ideal\ud resolution and long-range distance sensitivity was achieved by redesigning a 600MHz HXMAS NMR probe\ud to provide fast angle switching during the NMR experiment: For 1.8 mm rotors, angle changes of up to ~5\ud degrees in ~10 ms were achieved at 12 kHzMAS. A new experimental design that combines a reference and a\ud dipolar-modulated experiment and a master-curve approach to data interpretation is presented.
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