Organometallics noted when I3C-enriched W(CO),THF was added to the S [ Cr3(C0)12] 2-anion.Acknowledgment. The financial support of the Robert A. Welch Foundation is greatly appreciated. [ Na] [ PPN] [ ((CO),Cr),S], 87039-34-7; (w-CO)& C0)&r3(p4-S)Cr-(CO)52-, 87050-03-1; Cr(CO)STHF, 15038-41-2; W(CO)5THF, Registry NO. 1,91670-43-8; 2% [PPN+]p(CH&CO, 91670-45-0; 36477-75-5. Summary: Mo,(OCMe,), reacts with phenylacetylene in pentane to produce Mo(CPh)(OCMe,), in -60 % yield (by 'H NMR) in -2 h. I t can be isolated by sublimation in -30% yield. In the presence of quinuclidine (quin) Mo,(OCMe,), reacts with phenylacetylene to yield an inseparable 1 : 1 mixture of Mo(CPh)(OCMe,),(quin) and Mo(CH)(OCMe,),(quin) in a combined yield of -60 % .
Analogous reactions between Mo,(OCMe,), and l-pentyne in the presence of quinuclidine yield oily 1-pentyne oligomers containing a mixture of Mo(CPr)(OCMe,),(quin) and Mo(CH)(OCMe,),(quin) in -50% yield (by 'H NMR).In the absence of quinuclidine only Mo(CPr)(OCMe,), is observed by NMR in the oily product mixture. Addition of acetylene to Mo,(OCMe,), yields what we propose to be Mo,(OCMe,),(p-C,H,), which upon attempted recrystallization loses acetylene to reform MO,(OCMe,),.Summary: Acyl chlorides can be selectively and rapidly reduced, under mild conditions, by group 66 anionic hy-(1) On leave from the
