Abstract
AbstractInsect exoskeleton, multiply labeled with 13C and 15N, was examined by rotational‐echo double‐resonance (REDOR) and double‐cross‐polarization (DCP) magic‐angle spinning 13C NMR. Low levels of incorporation of label make the analysis of these samples a practical test of the relative advantages of REDOR and DCP for the detection of weak, heteronuclear dipolar coupling between rare spins in solids. The sensitivity of REDOR for the detection of directly bonded 13C–15N pairs is an order of magnitude greater than that of DCP when neither label is involved in homonuclear dipolar coupling of strength comparable to the spinning frequency. However, if either of the 13C or 15N labels undergoes homonuclear spin flips, DCP gains in relative sensitivity and is easier to use for spin counting than REDOR.
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