Abstract 13 C, 17 O, 29 Si, 119 Sn NMR spectra of acyloxysilanes,-germanesand-stannanes R 1 R 2 R 3 MOCOR (M= Si, Ge, Sn) have been investigated. The character of substituent effects ion the 13 C and 17 O chemical shifts of these compounds is almost the same for Si, Ge and Sn. 17 O and 119 Sn NMR spectra establish the predominance of the intermolecular exchange processes in acyloxystannanes.