Abstract
Synthesis of the phase-pure mixed-valent europium chlorides, Eu 4Cl 9, Eu 5Cl 11, and Eu 14Cl 33, is reported. X-ray powder diffraction data are presented for NdBr 3 · (THF) 4. The structures of metastable dihalides synthesized by solvolytic decomposition, fluorite-type LnCl 2, Ln = Sm, Eu, and anti-Fe 2P-type Ba X 2, X = Cl, Br, and that of the cluster-type mixed-valent halide precursor, are described in terms of close-packed layers and a solvolytic decomposition mechanism is proposed. In this mechanism the Ln 3+ ions at the solvent-solid interface are removed as LnX 3 (solvate) from atomic planes perpendicular to the three-fold inversion axis of the precursor and remaining LnX 2 ions relax immediately; primarily in-layer cation rearrangements lead to the fluorite-type structure upon subsequent layer collapse, whereas both in-layer and out-of-layer cation displacements yield the anti-Fe 2P-type structure.
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