Tetracyanamidoaluminates of the type LiM(2)[Al(CN(2))(4)] with M = Eu and Sr were prepared by solid-state metathesis reactions departing from EuF(2) (or SrF(2)), AlF(3), and Li(2)(CN(2)) in a 2 : 1 : 4 molar ratio. The ignition temperature of the exothermic formation of LiSr(2)[Al(CN(2))(4)] was obtained near 420 °C. An X-ray single-crystal structure refinement performed for LiEu(2)[Al(CN(2))(4)] revealed the presence of the novel homoleptic [Al(CN(2))(4)](5-) ion in the structure. The X-ray powder diffraction pattern of LiSr(2)[Al(CN(2))(4)] was indexed isotypically.
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