Deacon, Glen B., Forsyth, Craig M., Junk, Peter C., Hilder, Matthias, Leary, Stuart G., Bromant, Claudia, Pantenburg, Ingo, Meyer, Gerd, Skelton, Brian W., and White, Allan H. (2008) Synthesis and structural properties of anhydrous rare earth cinnamates, [RE(cinn)(3)]. Zeitschrift für Anorganische und Allgemeine Chemie, 634 (1). pp. 91-97.

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Abstract

Anhydrous rare earth tris(cinnamates) [RE(cinn)(3)] (RE= La - Lu, Y and Sc and cinnH = trans-cinnamic acid) were prepared by metathesis in water and by direct reaction of the metal with cinnamic acid in a 1,2,4,5-tetramethylbenzene flux at ca. 200 degrees C. X-ray crystal structure determinations and X-ray powder data show that, in the solid state, the larger lanthanoids (La - Dy) form an isomorphous polymeric series consisting of homoleptic ninecoordinate metal centres bonded to three chelating and bridging tridentate cinnamates. The late REIII cinnamate (RE = Dy, Ho - Lu, Y) complexes also form linear one-dimensional polymeric chains with all RE metal atoms being seven-coordinate. The cinnamates are either bound tridentate bridging in a V-T,2:111 fashion, or mu-eta(1):eta(1) syn-syn bidentate bridging. A structural break occurs at dysprosium which has been characterised in both crystallographic forms, and gives solely the late RE form when precipitated at 80 degrees C. Sc-III cinnamate was also isolated as an analytically pure precipitate which was, again, found to be anhydrous in nature. A structural change was identified by powder XRD between the late REIII cinnamates and Sc-III cinnamate.

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