Inorganic Synthesis, Vol. 23 by Stanley Kirschner

By Stanley Kirschner

The volumes during this carrying on with sequence supply a compilation of present options and concepts in inorganic man made chemistry. comprises inorganic polymer syntheses and training of significant inorganic solids, syntheses utilized in the advance of pharmacologically energetic inorganic compounds, small-molecule coordination complexes, and similar compounds. additionally comprises useful details on transition organometallic compounds together with species with metal-metal cluster molecules. All syntheses awarded the following were demonstrated.

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10. Grillone and B. B. Kedzia, Trunsirion Mer. , 4, 256 (1979). 8. -N. CHAU and A. 1) + 2 CO *Institute of General Chemistry, University of Pisa, 56100 Pisa, Italy. tDepartment of Chemistry, The Ohio State University, Columbus, OH 43210. (1) Bis[halotetracarbonylmanganese(I)] 33 For reaction (l), the authors used an inert solvent, namely a mixture of saturated hydrocarbons boiling in the 100-120" range. The reported yields are about 40% due to partial decompositon. The bromo- and iodo-derivatives, which are more frequently used due to their higher thermal stability with respect to the chloro analog, can be conveniently prepared in a poorly coordinating solvent such as diisopropyl ether, which boils at 68-69'.

The reaction flask is then connected to a gas buret containing carbon monoxide over mercury, and the reaction mixture is vigorously stirred magnetically. The temperature is maintained at 16" by an external water bath operated by a thermostat. Reduction of NbCISoccurs rapidly, as denoted by the change in color of the reaction mixture from yellow-orange to violet and then blue. § After that, a considerable decrease in the gas absorption rate is noted. The reaction mixture is vigorously stirred for about 30 hours when the molar CO/Nb ratio reaches approximately six.

45. Properties Carbonyldiiodo(q5-pentamethylcyclopentadienyl)cobalt(III)is a black, crystalline, air-stable solid. It dissolves readily in polar solvents forming deep purple solutions but is virtually insoluble in diethyl ether, alkanes, and aromatic solvents. 20 ppm. The IR spectrum exhibits a single metal-carbonyl stretchingband at 2053 cm-’ (CH,Cl,). ’ C. 6 An analogous dichloro(q-ethyltetramethylcyclopentadieny1) derivative, [{CoClZ(q’-C,Me4Et)}~] has been prepared’ by the extraction of CoCl, from [Co~Clb(q5-CSMe4Et),] in turn made from [Sn(n-Bu),(a-C5Me4Et)]and CoC12.

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