Ma. Dellabona et al., MAGNETIC-RESONANCE SPECTROSCOPIC STUDIES OF A TETRAARYL-DISTANNENE AND TETRAARYL-DIGERMENE [M2R4] (R = C6HBUT-2-ME-3-4,5,6 AND M = SN OR GE), Journal of the Chemical Society. Dalton transactions, (7), 1998, pp. 1187-1190
Tin-119 NMR spectral studies in the solid state and in solution of [Sn
2R4] (R = C6HBu'-2-Me-3-4,5,6) 3 are presented. The ambient temperatur
e Sn-119 CP-MAS NMR spectrum displayed a single resonance at delta(iso
) 819, while variable-temperature spectra in toluene clearly indicated
the existence of a rapid equilibrium between the loosely held dimer 3
and its monomer SnR2. Photolysis of either 3 or its digermanium analo
gue in benzene yielded the persistent radicals [MR3](.) (M = Ge or Sn)
, which were studied by ESR spectroscopy. The ESR parameters are compa
red with other trialkyl-and triamido-tin(III)- and -germanium(III)-cen
tred radicals. Noteworthy is the first observation of C-13 hyperfine c
oupling for a Group 14 metal-centred radical, 18(1) G for [SnR3](.) an
d 10(1) G for [GeR3](.).