Su. Ghazi et al., SYNTHESES AND MOLECULAR-STRUCTURES OF THE DIALKYLALUMINUM AND DIALKYLGALLIUM STANNOXIDES [R(2)M(MU-OSNPH(3))](2), Inorganic chemistry, 33(3), 1994, pp. 411-414
The reaction of trialkylaluminum derivatives, R(3)Al(R = Me, Et, i-Bu)
, and trimethylgallium with the distannoxane (Ph(3)Sn)(2)O yields R(2)
MOSnPh(3) (M = Al, R = Me (1a); Et (1b), i-Bu (1c); M = Ga, R = Me (2)
) and the corresponding organotin compound, RSnPh(3). Attempts to disr
upt the Al-O bridge bonds of [R(2)Al(mu-OSnPh(3))](n) (R Me (1a), Et (
1b) and form stable adducts with diethyl ether failed, but 4-picoline
gives a 1:1 complex. The resulting derivatives have been characterized
by H-1 and C-13:NMR spectroscopy. The structure of la was determined
by single-crystal X-ray diffraction techniques and was found to be in
the triclinic space group P $$($) over bar 1 with cell constants a = 9
.076(1) Angstrom, b = 9.733(2) Angstrom, c 13.084(3) Angstrom, alpha =
71.03(2)degrees, beta = 74.22(1)degrees, gamma = 65.05(1)degrees, and
Z = 1. The structure was refined to a final R = 2.6% (R(w) = 3.9%) ba
sed on 3185 (I > 2.5 sigma(I)) observed reflections. The molecule exis
ts as a dimer, (Me(2)AlOSnPh(3))(2), with Al-O bond distances of 1.84
Angstrom and Sn-O bond distances of 1.98 Angstrom. Both aluminum and t
in centers in the dimer are in a pseudotetrahedral environment.