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A Convenient Route to Lanthanide Triiodide THF Solvates. Crystal Structures of Lnl3(THF)4 [Ln = Pr] and Lnl 3(THF)3.5 [Ln = Nd, Gd, Y]

Lookup NU author(s): Dr Keith Izod, Dr Stephen Liddle, Professor William Clegg

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Abstract

The reaction between 1.5 equiv of elemental iodine and rare earth metals in powder form in THF at room temperature gives the rare earth triiodides Lnl3(THF)n in good yields. Purification by Soxhlet extraction of the crude solids with THF reliably gives the THF adducts Lnl 3(THF)4 [Ln = La, Pr] and Lnl3(THF) 3.5 [Ln = Nd, Sm, Gd, Dy, Er, Tm, Y] as microcrystalline solids. X-ray crystallography reveals that the early, larger lanthanide iodide Prl 3(THF)4 crystallizes as discrete molecules having a pentagonal bipyramidal structure, whereas the later, smaller lanthanide iodides Lnl3(THF)3.5 [Ln = Nd, Gd, Y] crystallize as solvent-separated ion pairs [Lnl2(THF)5][Lnl 4(THF)2] in which the cations adopt a pentagonal bipyramidal geometry and the anions adopt an octahedral geometry in the solid state.


Publication metadata

Author(s): Izod K, Liddle ST, Clegg W

Publication type: Article

Publication status: Published

Journal: Inorganic Chemistry

Year: 2004

Volume: 43

Issue: 1

Pages: 214-218

Print publication date: 12/01/2004

ISSN (print): 0020-1669

ISSN (electronic): 1520-510X

Publisher: American Chemical Society

URL: http://dx.doi.org/10.1021/ic034851u

DOI: 10.1021/ic034851u


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