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Nickel and cadmium complexes of the anionic form of 4,6-dimethylpyrimidine-2-thione (Hdmpymt) and their adducts with neutral ligands (1.1 0-phenanthroline or 2,2'-bipyridine) have been prepared by an electrochemical procedure and characterized by spectroscopic (IR, UV, 'H and 13C NMR) methods, and for the [{Cd(dmpymt),},] complex by X-ray crystallographic techniques. This compound is hexanuclear with an array of six cadmium atoms bridged by twelve sulfur atoms. Each cadmium atom has a distortedoctahedral cis-CdS,N, environment with each ligand acting in a N,S bidentate S-bridging mode. The hexamer has a calixarene-like structure with cavities large enough to accommodate molecules such as acetonitrile, carbon monoxide and molecular iodine.

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Al f onso Cast i iiei ras, Wolf gang H i I ler, and J oac hi m St ra h le lnstitut fur Anorganische Chemie der Universitat Tubingen. Auf der Morgenstelle, 18. D -7400 Tubingen, Federal Republic of Germany The compound [Ni(pyt),] has been prepared in good yield by electrochemical oxidation of the metal in a solution of pyridine-2-thione (Hpyt) in acetonitrile. When pyridine (py), 2,2'-bipyridine (bipy), or 1 ,I O-phenanthroline (phen) is present in the electrochemical cell the corresponding adducts [Ni(pyt),(py),], [Ni(pyt),( bipy)], or [Ni(pyt),(phen)] is obtained. The crystal structure of [Ni(pyt),(bipy)]*0.5 bipy is monoclinic, with a = 10.409(2), b = 12.01 3(3), c = 19.790(3) A, p = 103.95(3)", space group P2,/c, and R = 0.032 for 3 176 reflections with ll0l > 301/,(. The molecule has a distorted octahedral Ni N,S, kernel, with average bond distances of 2.065 A for Ni-N and 2.485 8, for Ni-S. The vibrational and electronic spectra of the compounds are discussed.