The reaction of Ln(acac)(3).3H(2)O (Ln = Sm, Eu, Gd, Dy, Yb) with K[Cr(2)(CO)(10)(micro-H)] at different molar ratios and solvents leads to the formation of nonanuclear lanthanide hydroxo acetylacetonate complexes of general formula [Ln(9)(OH)(10)(acac)(16)][HCr(2)(CO)(10)]. The compounds are isomorphous, and the common cationic cluster core consists of a novel square antiprismatic arrangement of nine Ln atoms connected by micro(3), micro(4) hydroxo bridges and/or by acetylacetonate ligands as it results from the single-crystal X-ray analysis of the Sm derivative for which the most suitable crystals were obtained.
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