Triple-quantum (TQ) NMR spectroscopy in dipolar solids under fast magi
c-angle spinning is introduced. Proton dipolar connectivities derived
from two-dimensional high-resolution TQ NMR spectra are shown for bisp
henol-A-polycarbonate, fully protonated and OH-deuterated dimethylglyo
xime and acetonitrile trapped in the cages of perdeuterated hydroquino
ne. For spin-1/2-triads, fast rotating about their threefold symmetry
axis, MAS-induced TQ spinning-sideband patterns are evaluated. Analyti
cal treatment of isolated spin-1/2-triads is compared to numerical spi
n-dynamics simulations including influences of surrounding spins with
respect to effects on both the integral intensities of TQ coherences a
nd the signal distribution on TQ sideband patterns. Using the above sa
mples, which contain methyl groups in different surroundings, the pert
urbing effects of neighboring protons are elucidated. (C) 1998 Publish
ed by Elsevier Science B.V.