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

Phys Chem Chem Phys. 2011 Mar 14;13(10):4514-8. doi: 10.1039/c0cp02364g. Epub 2011 Jan 24.

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.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Dipeptides / chemistry
  • Magnetic Resonance Spectroscopy / methods*

Substances

  • Dipeptides