G. Westin et al., Synthesis and properties of erbium isopropoxides: Structural characterization of Er5O(OPri)(13), J SOL ST CH, 141(1), 1998, pp. 168-176
We have investigated the synthesis of erbium isopropoxides by dissolution o
f Er metal in 2-propanol-containing solvents or by metathesis of ErCl3 and
KOPri in solution, with or without addition of water. Two different erbium
isopropoxides could be isolated in pure form: one with a structure that has
not been solved (I), which,ve believe to be a solvated non-ore isopropoxid
e, and one oxo isopropoxide, Er5O(OPri)(13). The latter structure was deter
mined by single-crystal X-ray diffraction; it has orthorhombic space group
symmetry Pbca, a = 20.917(6) Angstrom, b = 21.575(6) Angstrom, c = 25.638(6
) Angstrom, with Z = 8. The final R value was 0.0748 (R-w, = 0.1158). The o
xo isopropoxide molecules contain the well-known M5O fragment, which has th
e configuration of a square pyramid with the oxo-oxygen atom slightly above
the basal plane. The compounds have been characterized by FT-IR and UV-vis
spectroscopy, differential scanning calorimetry, and their solubilities an
d chemical reactivities. FTIR studies revealed that both alkoxides largely
retained the molecular structure when dissolved in toluene-2-propanol (2 :1
) or hexane, The stability of Er5O(OPri)(13) in the absence of water is rat
her high, whereas I is more labile. (C) 1998 Academic Press.