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Zusammenfassung:
Deuteron NMR spectra of both single crystal and powder samples of acetylsalicylic acid-CD 3were measured using the quadrupolar-echo technique. The experiments were done in the temperature range 17-100 K, with a special emphasis on the range 20- 30 K, in which the observable tunneling frequency decreases rapidly from its low-temperature value of 2.7 down to 1.2 MHz. In the tunneling regime, modulations of the line intensities and phases as a function of the echo time tau are observed in the single-crystal spectra. The modulation frequency is equal to the orientation-dependent displacement of the inner satellite pairs (alpha lines) from the Larmor frequency. These effects were confirmed in numerical simulations and fully explain the phase-modulation effects observed previously in quadrupolar-echo spectra of methyl-deuterated methanol and para-xylene guest molecules in some inclusion compounds. By measuring the temperature and orientation dependence of the quadrupolar lineshapes, it was found that the echo spectra are more sensitive to the value of the tunneling frequency than the spectra obtained from the free induction decay. It is pointed out that, because of the modulation effects, special care must be taken when structural parameters are to be extracted from quadrupolar-echo spectra, in particular from spectra of powder samples.
