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DOI: 10.1039/A604434D (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1997, 277-282

Crystal structure of bis(tetraethylammonium) bis[4,5-disulfanyl-1,3-dithiol-2-onato(2-)]nickelate(II) and spectroscopic and electrical properties of related oxidized complexes

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Shuging Q. Sun, Bin Zhang, Peiji J. Wu and Daoben B. Zhu

Abstract

Bis(4,5-disulfanyl-1,3-dithiol-2-onato)nickelate anion complexes [Ni(C3S4O)2]2- were prepared. A single- crystal structure analysis has been performed for the bis(tetraethylammonium) salt 1: orthorhombic, space group I4(1)acd, Z = 8, a = b = 19.605(3), c = 16.217(5) Å. Full-matrix least-squares refinement based on 744 independent reflections with I > 2σ(I) yielded an R factor of 0.0651. The geometry around the nickel atom is greatly distorted from square planar, with a dihedral angle of 17.4° between the dithiolate ligand planes. Although it is essentially an insulator, with an electrical conductivity of 1.4 × 10-8 S cm-1 measured for a single crystal at room temperature, some partially and completely oxidized nickel complexes as well as iodine-doped single crystals exhibit increased conductivities of 10-3–10-2 S cm-1. Electronic, IR, ESR and X-ray photoelectron spectra of these complexes are discussed.

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