SYNTHESIS, CHARACTERIZATION, AND STRUCTURE DETERMINATION OF A NEW HETEROMETALLIC OXOALKOXIDE - ER2TI4O2(OC2H5)(18)(HOC2H5)(2)

Different synthesis routes have been studied for the preparation of a new oxoalkoxide, Er2Ti4O2(OEt)(18)(HOEt)(2) (Et = C2H5). The compound was best prepared by reacting KOEt and Ti(OEt)(4) first with water and then with ErCl3. The structure was determined by single-crystal X-ray diffraction, showing the unit cell to have the monoclinic space group symmetry, P2(1)/n, and the lattice constants a = 15,180(2) Angstrom, b = 12.693(2) Angstrom, c = 16.602(3) Angstrom and beta = 98.91(1)degr ees and to contain two formula units, The final R value was 0.053 (wR = 0.077). The molecule contains three of the most commonly found struc ture fragments of alkoxides, namely the C-2h fragment of Ti-4(OEt)(16) (Er2Ti2O6), the M-4(mu(4)-O) fragment (Er2Ti2O), and the face-sharing MO6 octahedra, with M = Ti4+, IR studies revealed that the molecular s tructure of the alkoxide was retained to a large extent when the alkox ide was dissolved in 4:1 ethanol:toluene and hexane solvents. (C) 1998 Academic Press.