An X-(X) over bar pulse train with stepped modulation frequency was employed to enhance the multiple-quantum to single-quantum coherence transfer in the mixing period of the multiple-quantum magic-angle spinning (MQ-MAS) experiment for spin I = 5/2 nuclei. Two MQ-MAS pulse sequences employing this mixing scheme for the triple-to-single and quintuple-to-single quantum coherence transfers have been designed and their performance is demonstrated for Al-27 on samples of NaSi3AlO8 and 9Al(2)O(3) . 2B(2)O(3). Compared to the standard single-pulse mixing sequences, the sensitivity is approximately doubled in the present experiments. (C) 2000 Elsevier Science B.V. All rights reserved.