n Bu 3 SnF and Mes 3 SnF (Mes = mesityl) are organotin fluorides that have direct Sn–F bonds. The 119 Sn and 19 F NMR spectra of these compounds have been measured using a selection of CPMAS probes. Doubly decoupled { 1 H, 19 F} as well as singly decoupled { 1 H} 119 Sn NMR spectra are shown. Double decoupling gives higher resolution spectra and allows the sample of Mes 3 SnF to be spun slower to give more spinning-sidebands without overlapping of signals, giving improved analysis. The doubly decoupled spectra are sensitive to the power and offset of the decouplers. The effect of off-resonance decoupling has been observed for 119 Sn NMR through reduced splittings when the 19 F decoupler power and offset were varied. Proton-decoupled 19 F spectra have been measured using a new HF double-resonance probe. In addition, two-dimensional heteronuclear correlation spectra are presented for Mes 3 SnF, allowing a full assignment for the 19 F and 119 Sn chemical shifts of the two sites. Full shielding tensor data are reported for both compounds. Values have been derived for the effective ( 119 Sn, 19 F) dipolar coupling constants from both 119 Sn and 19 F experiments, yielding estimates of coupling anisotropy.