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Single crystals of (n-C 4 H 9 ) 4 NAu(CN) 2  were obtained by crystallization using the temperature decreasing method in a newly developed computer-controlled apparatus. The colourless crystals are monoclinic, space group A2/n, with a = 20.216(2) Å, b = 13.130(1) Å, c = 9.328(1) Å, and β = 109.69(1)°. The measured density is 1.45 g/cm 3 , which agrees with the calculated density of 1.40 g/cm 3  for Ζ = 4. The structure was solved by Direct Methods using 674 independent reflections and refined by least-squares procedures to conventional and weighted R factors of 0.068 and 0.058, respectively. The nearly linear [Au(CN) 2 ] - -anions form pseudohexagonal layers, in which they are arranged parallel to each other. The shortest Au—Au distance is 8.05 A. The stacking of the layers produces pseudo-trigonal channels, occupied by the cations. The tetra-n-butylammonium cation has four ordered trans chains with idealized D 2d  symmetry (4̄2 m).

Tetra-n-butylammoniumdicyanoaurat(I), (n-C 4 H 9 ) 4 NAu(CN) 2 / Tetra-n-butylammonium Dicyanoaurate(I), (n-C 4 H 9 ) 4 NAu(CN) 2