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Updated: Oct 25, 2025

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
Published on: September 17, 2017
Quantitative rotational-echo double resonance for Carbon-13 spin clusters
Shigeru Matsuoka1, Miriam Sindelar2, Sonal Bansal2
1Department of Chemistry, Washington University, St. Louis, MO 63130, USA; Faculty of Medicine, Oita University, Oita 879-5593, Japan.
Abstract:
By using only half of the total evolution time for dephasing pulses, C{N} rotational-echo double resonance (REDOR) for clusters of 13C spins (RDX) results in the same universal REDOR behavior as observed for isolated 13C-15N pairs. RDX combines Hahn echoes with solid echoes to suppress interference from scalar J couplings. This is crucial for long evolution times. The modified version (which we call RDX24) makes RDX quantitative for 13C clusters. We apply this scheme to human embryonic kidney cells labeled in culture by L-[13C5 -15N2]-glutamine. We quantitatively characterize three separate nitrogen isotopic enrichments for: (i) the alpha nitrogens of glutamine residues in proteins (including the residues of the five amino acids synthesized from glutamine); (ii) the alpha nitrogens of the five amino-acid residues synthesized from glucose, together with those of the nine essential amino acids added to the growth medium; and (iii) the side-chain nitrogens of glutamine (and of asparagine derived from glutamine).
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