Ot. Beachley et al., Synthesis of an organogallium(I) compound [Ga(CH2CMe2Ph)](n) with EPR spectral evidence for gallium clusters, J ORGMET CH, 582(1), 1999, pp. 32-39
The organogallium(I) compound [Ga(CH2CMe2Ph)](n) has been prepared by the r
eduction of Ga(CH2CMe2Ph)(2)Cl by using either sodium or lithium with napht
halene in THF. The yellow dihydronaphthalene gallium(III) intermediate M-2(
C10H8[Ga(CH2CMe2Ph)(2)Cl](2)) initially formed at -78 degrees C but then de
composed at higher temperatures to form [Ga(CH2CMe2Ph)](n), Ga(CH2CMe2Ph)(3
) and MCl. EPR spectra, which were recorded as the two yellow intermediates
Na-2(C10H8[Ga(CH2CMe2R)(2)Cl](2)) (R = Ph, Me) decomposed, indicated the p
resence of radicals. The first and second derivatives of the EPR signals, l
ine-widths, g-values and hyperfine coupling constants are consistent with t
he radicals being clusters of organogallium species. The experimental spect
ra were simulated by the superposition of two spectra, a single Gaussian sh
aped line with a peak-to-peak width of 14 mT (92%) with the spectrum of fiv
e equivalent gallium nuclei, A = 2.1 mT (8%). The even number of lines obse
rved in the experimental spectra indicate an odd number of gallium nuclei w
ith at least five bring required to give the number of observed lines. (C)
1999 Elsevier Science S.A. All rights reserved.