Crystal and Molecular Structure of Tetrabutylammonium Bis(1,4-dithiin-2,3-dithiolato)nickelate(III), (Bu<i>n</i>4N)[Ni(ddt)2]

Abstract

Abstract The crystal structure of tetrabutylammonium salt of a new multi-sulfur 1,3-dithiolene complex, (Bun4N)[Ni(ddt)2] (ddt=1,4-dithiin-2,3-dithiolato) has been determined by the single-crystal X-ray diffraction technique. Crystals are monoclinic, space group C2⁄c, a=66.107(40), b=9.182(5), c=19.119(12) Å, β=147.29(3)°, V=6271(1) Å3, and Z=8. The structure was solved by the heavy atom method, and refined by a block-diagonal least-squares method to R=0.070. There are two crystallographically independent molecules of Ni(ddt)2, molecule-A and molecule-B. Molecule-B forms segregated uniform stacks along the b-axis. The (Bun4N)+ cations are located between two molecular planes of molecule-A. The Ni(ddt)2 molecules are almost planar except two terminal vinylene moieties, which are folded to opposite side each other and the folding angles of molecule-A and molecule-B are 28° and 39°, respectively.