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Comparison of rotational‐echo double‐resonance and double‐cross‐polarization NMR for detection of weak heteronuclear dipolar coupling in solids
Author(s) -
Christensen Allyson M.,
Schaefer Jacob,
Kramer Karl J.
Publication year - 1991
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.1260290503
Subject(s) - homonuclear molecule , heteronuclear molecule , chemistry , magnetic dipole–dipole interaction , magic angle spinning , spins , nuclear magnetic resonance , dipole , resonance (particle physics) , molecular physics , solid state nuclear magnetic resonance , polarization (electrochemistry) , analytical chemistry (journal) , nuclear magnetic resonance spectroscopy , atomic physics , stereochemistry , molecule , physics , condensed matter physics , organic chemistry , chromatography
Abstract Insect exoskeleton, multiply labeled with 13 C and 15 N, was examined by rotational‐echo double‐resonance (REDOR) and double‐cross‐polarization (DCP) magic‐angle spinning 13 C 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 13 C– 15 N 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 13 C or 15 N labels undergoes homonuclear spin flips, DCP gains in relative sensitivity and is easier to use for spin counting than REDOR.