Longitudinal nuclear magnetic relaxation in coupled two‐spin systems is discussed in terms of magnetization transfermodes, a generalization of the magnetization modes commonly used in the discussion of one‐dimensional NMR relaxation experiments. The symmetry properties of the transfer modes and their relationship to the elements of the usual Redfield relaxation matrix are discussed. Experimental strategies for measuring the amplitudes of the transfer modes are discussed and various selective two‐dimensional exchange (‘‘soft‐NOESY’’) methods are proposed. Experimental data are presented for Exifone, a small organic molecule, and the auto‐ and cross‐correlation spectral densities, the magnitudes of the proton chemical shift anisotropies, and the strengths of the dipolar interaction are derived from the spectra.

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