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Bis(p-mercapto)bis(tricarbonyliron), (p-HS)2Fe2(CO)6, reacts with a,@-unsaturatsd ketones, esters, and nitriles which contain terminal CH2= or RCH-groups in the presence of piperidine to give 2:l adducts in which each HS unit has added to a molecule of the activated olefin. In the case of disubstituted ketones of type RR'C==CHC(0)CH3, b-HS)2Fe&O)6 reads with only one molecule of the substrate, one HS adding to the C = C bond and the other to the C=O bond, to give a product with a three-carbon bridge between the sulfur atoms. In reactions with a,P-unsaturated acetylenes, the two HS units add to the C=C bond of one molecule of the substrate to give products with a one-carbon bridge between the sulfur atoms. An exception is dimethyl acetylenedicarboxylate, in which case a product with a two-carbon bridge is formed.The structure of one such adduct, p-(CHBC(0)CH2CHS2)Fe2(C0)6, was determined by X-ra diffraction.This compound crystallizes in the space group C2/c with a = 15.378 (2) A, b = 9.6620 (9) 1, c = 21.768(3) A, @ = 108.23 ( 1 ) O , V = 3072.0 A3, and 2 = 8. On the basis of 1593 unique observed reflections and 190 variables, the structure was refined to R = 0.040 and R, = 0.047.

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