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{Bis [2-(2-pyridyl)ethyl] disulfide)copper(I) perchlorate, alternatively named [2,2'-(dithiodiethylene)dipyridine]copper(I) perchlorate, Cu(CsH4NCH2CH2SSCH2CH2CsH4N)C104, has been synthesized by disulfide ligand reaction with Cu(II) and subsequent Cu(I) coordination with excess disulfide. Its crystal structure has been determined by single-crystal X-ray diffraction techniques. After large-block-diagonal least-squares refinement using anisotropic thermal parameters for nonhydrogen atoms and isotropic ones for hydrogens, the conventional R index converged at 0.043. The yellow crystals form in the monoclinic space group Pljc with a = 10.408 (3) A, b = 8.249 (2) A, c = 20.662 (7) ,ß = 108.99 (3)°, and Z = 4.Half (CsH4NCH2CH2S-) of two different ligands is coordinated to each Cu(I) ion. This results in two six-membered chelate rings and a somewhat distorted tetrahedral coordination environment of two sulfur and two nitrogen atoms about each Cutí). The remaining halves of each disulfide ligand associate with different Cu(I) ions, forming a cationic polymeric chain. The average Cu(I) bond distances to the sulfur and nitrogen donor atoms are 2.322 (1) and 2.029 (1) A, respectively. The Raman shift of the S-S stretch is 484 cm"1, significantly less than the expected value for the uncoordinated disulfide ligand.. This correlates qualitatively with the observed coordination of the disulfide moiety, the closing of the CSSC dihedral angle to 59.7 (1)°, and the lengthening of the S-S bond to 2.081 (1) A. A uv band associated with the complexed disulfide appears at 293 mg, as compared to 248 µ in the uncoordinated ligand. A similar band at approximately 330 mg is observed in the oxidized form of ceruloplasmin, in which the complexation of Cu(I) by disulfide has been reported.

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