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Published on: January 26, 2014
Isolation and structural characterization of tetra-n-propyl zirconate in hydrocarbon solution and the solid state
V W Day1, W G Klemperer, M M Pafford
1Department of Chemistry, University of Nebraska, Lincoln, Nebraska 68588, USA.
Abstract:
Tetra-n-propyl zirconate has been purified by vacuum distillation and isolated as an extremely moisture sensitive, crystalline solid. According to a single-crystal X-ray diffraction study, crystalline tetra-n-propyl zirconate is composed of tetrameric Zr(4)(OPr(n))(16) (1) molecules whose Zr(4)O(16) metal-oxygen core structure has virtual C(2)(h) symmetry, the same structure observed previously for n-alkyl orthotitanates. Carbon-13 NMR spectroscopic data indicate that this core structure is retained in hydrocarbon solution. Molecule 1 has the same M(4)O(16) metal-oxygen core structure as [CH(3)C(CH(2)O)(3)](2)M(4)(OPr(i))(10), M = Ti, where the metal centers have octahedral coordination geometry, but a metal-oxygen core structure different from that of the M = Zr case, where trigonal metaprismatic coordination geometry is observed.
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