Solid Isolation from the Reaction Mixture of di-t-butylacetylene with Stoichiometric Amounts of Nickel Tetracarbonyl.

Article abstract of DOI:10.1016/0304-5102(85)80016-X

From the reaction mixture of di-t-butylacetylene with stoichiometric amounts of nickel tetracarbonyl and concentrated hydrochloric acid in methanol a cinnabar-red solid could be isolated. Elementary analysis and spectroscopic data (IR, **1H and **1**3C-NMR, MS) favor the assumption of a two-center sigma -alkenyl-complex left bracket trans-( sigma -(E)-(CH//3)//3C minus CH equals C minus C(CH//3)//3)-Ni( mu Cl)(CO) right bracket //2. The crystal structure, on the contrary, unequivocally indicates it to be a Ni( mu -Cl)//2Ni core with two allylic 2,3-di-t-butylacrylyl ligands. Reactions of the complex with methanol/water, oxygen and PPh//3 respectively are reported.