Trinuclear NiCoMo and MoRuCo clusters

The reactivity of organometallic clusters has been studied to a point where systematization becomes possible, and details of mechanisms and stereo- 

All materials are handled under an inert gas atmosphere in Schlenk type vessels and in well-ventilated hoods. All solvents must be dried by Na-K alloy, degassed, and distilled. The silica gel for chromatography (Macherey-Nagel 0.06-0.2 mm) is dried for 12 h at 160 °C in high vacuum. For thin layer chromatography (TLC) tests, silica gel on aluminum (Merck-60 F2S4) is used. The term hexane is used for the petroleum ether fraction boiling between 60 and 70 C. 

The syntheses of the starting clusters ( 3-MeC)C03(CO)9 (ref. 6) and RuCo2(CO)i 1 (ref. 7) are well documented. The reagents Na[M C5H5KCX))3] (ref. 8) and [C5H3Ni(CO)]2 (ref. 9) can be prepared according to published procedures. 2-Butyne is commercially available. All intermediate and product clusters have been fully characterized including elemental analyses.  

CFCL04Ij-ETHYLIDYNE-1 2 3-k C-PENTACARBONYL-1k C, 2k C-BIS[1,3(h )-CYCLOPENTADIENYL]COBALT-MOLYBDENUMNlCKEL(Co—Afo)(Co—A KA/o—Ni), (U3-CH3C)N1CoMo(CsH5)2(CO)5 

This chiral cluster is obtained in a two-step metal-exchange sequence with an average yield of 25% based on ( /3-CH3C)Co3(CO)9  

The molecular structure of this compound consists of a trigonal bipyramid of the metal atoms as determined by X-ray analysis. Solutions of the compound instantly dissociate upon addition of phosphines producing [Ph3PAuPR3] cations and [FeCo3(CO)]2] anions. Similar chemistry has been observed by Braunstein et al. for Ph3PAuRuCo3(CO)i2-  

Peraldo, Gazz. Chim. Ital., 90, 1005 (I960). 

Sherlock, Synthesis and Characterization of Some Novel Group IB and Mercury Mixed Metal Clusters, Ph.D. thesis. State University of New York, Stony Brook, New York, Chapter 2, 1985. 

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Chiral Trinuclear NiCoMo and MoRuCo Clusters 193 (Ai3-CH3C)Co3(CO)9 + Na[Mo(C5H5)(CO)3]... 

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