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Coppery-red, transparent single crystals of (Ba 6 N 5/6 ) 2 [NbN 4 ][CN 2 ] 6  (Im¯3, no. 204, a =1125.83(3) pm, Z = 2) are obtained by the reaction of Ba 2 N and ZnCN 2  with the container walls of the arc-welded Nb ampoules at 1100 K. The title compound assumes a stuffed skutterudite-type structure in which edge-sharing (Ba 6 N 5/6 ) octahedra form large voids which are occupied by either [NbN 4 ] tetrahedra or by [N=C=N] 2−  units with symmetric C=N bond lengths of d = 121.8(6) pm but a bond angle deviating significantly from linearity (∡ (N-C-N) = 175.3(9)°). The IR spectra corroborate this crystallographic result by the fact that all fundamental vibrations are visible in the IR spectrum [ν 1  = 1262 (symmetric stretching mode); ν 2  = 1957/2009 (antisymmetric stretching mode); ν 3  = 611/633/653 cm −1  (bending modes)], which is symmetry forbidden for [N=C=N] 2−  units having D ∞h  symmetry but expected for the C 2v  symmetry found in the title compound.

zeitschrift für naturforschung b

A Metal Nitride Carbodiimide with a Stuffed Skutterudite-type Structure: Synthesis, Crystal Structure and IR Spectra of (Ba 6 N 5/6 ) 2 [NbN 4 ][CN 2 ] 6