A novel technique is described that allows one to measure cross-relaxation rates (Overhauser effects) between 2 selected nuclei in high-resoln. NMR. The 2 chosen sites are irradiated simultaneously with the sidebands of an amplitude-modulated radiofrequency field, so that their magnetization vectors are forced to undergo a simultaneous motion, which is referred to as synchronous nutation. From the time-dependence obsd. for different initial conditions, one may derive cross-relaxation rates, and hence det. internuclear distances. The scalar interactions between the selected spins and other spins belonging to the same coupling network are effectively decoupled. Also, cross relaxation to other spins in the environment does not affect the transient response of the selected spins, which are therefore in effect isolated from their environment in terms of dipolar interactions. The method is particularly suitable to study cases where normal Overhauser effects are perturbed by spin-diffusion effects due to the presence of further spins. The technique is applied to the protein bovine pancreatic trypsin inhibitor. [on SciFinder (R)]