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Issue 10, 2011
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Longer-range distances by spinning-angle-encoding solid-state NMR spectroscopy

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Abstract

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.

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

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Publication details

The article was received on 02 Nov 2010, accepted on 05 Jan 2011 and first published on 24 Jan 2011


Article type: Paper
DOI: 10.1039/C0CP02364G
Citation: Phys. Chem. Chem. Phys., 2011,13, 4514-4518
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    Longer-range distances by spinning-angle-encoding solid-state NMR spectroscopy

    J. Becker-Baldus, T. F. Kemp, J. Past, A. Reinhold, A. Samoson and S. P. Brown, Phys. Chem. Chem. Phys., 2011, 13, 4514
    DOI: 10.1039/C0CP02364G

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