P. Sobota et al., THE CRYSTAL-STRUCTURE AND PROPERTIES OF [TICL4(CH(CO(2)ET)(3))] AND [AL2CL6(MU-C2H4(CO(2)ET)(2))], Journal of organometallic chemistry, 526(2), 1996, pp. 329-333
The reactions of TiCl4 with CH(CO(2)Et)(3) and AlCl3 with C2H4(CO(2)Et
)(2) in CH2Cl2 gave [TiCl4{CH(CO(2)Et)(3)}] (1) and [Al2Cl6{mu-C2H4(CO
(2)Et)(2)}] (2) respectively. The crystal structures of 1 and 2 have b
een determined by a single crystal X-ray diffraction studies and refin
ed by full-matrix least squares techniques to R(1) = 0.0272 and 0.0282
(for 2654 and 1274 unique non-zero reflections) for 1 and 2 respectiv
ely. The crystals of 1 belong to the space group C2/c with Z = 8 and a
= 17.131(8), b = 10.715(3), c = 18.512(5)Angstrom and beta = 92.97(3)
degrees. The titanium atom in 1 is octahedrally coordinated by four te
rminal chlorine atoms and two oxygen atoms in cis position from the co
ordinated triester molecule. Crystals of 2 are monoclinic, space group
P2(1)/c, Z = 4, a = 14.109(2), b = 10.049(2), c = 15.644(3)Angstrom a
nd beta = 116.65(2)degrees. In the molecular dimeric compound, each al
uminium atom is tetrahedrally coordinated by three terminal chlorine a
toms and one oxygen atom from the bridging diethyl succinate molecule.