Abstract

Abstract Red-orange, transparent single crystals of Yb2[CN2]3 [trigonal, R3̄c (no. 167), a = 630.02(3) and c = 2947.4(2) pm, Z = 6] are obtained by the reaction of Yb, Sn, Zn[CN2] and NaN3 in arc-welded Nb ampoules at 1100 K. The title compound exhibits characteristic C-N bond lengths and angles [d(C-N) = 122.7(3) pm and ∡(N-C-N) = 178.4(5)°, respectively] within the [N=C=N]2− unit as well as the expected fundamental frequencies in its optical spectra (Raman: νs = 1338; δ = 643 / 683 / 695 cm−1; IR: νas = 2005 / 2037; δ = 640 / 679 cm−1). Since Yb2[CN2]3 adopts a corundum-type structure, Yb3+ is octahedrally coordinated by six N atoms of different [CN2]2− anions [d(Yb-N) = 228.6(3) and 233.4(3) pm, 3× each] and every [CN2]2− group has four Yb3+ as next neighbours which form a distorted tetrahedron.

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