The two novel tetraarsaniobates(V) Na5Sr[NbAs4] and K5Ba[NbAs4] have b
een synthesized from the powders of As, Nb and binary arsenides Na3As,
K3As, SrAs or BaAs in sealed niobium ampoules and characterized by si
ngle crystal X-ray crystallography. The compounds crystallize in the h
P22 type of Na-6[ZnO4] (space group P6(3)mc (No. 186); Na5Sr[NbAs4], a
= 955.7(1) pm, c = 751.7(2) pm; K5Ba[NbAs4], a = 1039.6(2) pm, c = 80
9.7(3) pm; Z = 2). The bond lengths d(Nb-As) in the [NbAs4](7-) anions
range from 248.0(4) to 248.8(1) pm and from 249.2(3) to 250.3(1) pm i
n Na5Sr[NbAs4] and K5Ba[NbAs4] respectively.