Abstract
Treatment of the pentamethylcyclopentadienyl (Cp*) compound Cp*Os(NO)Br2 (1) with NaBH4 yields the dihydride Cp*Os(NO)H2. The dihydride loses H2 over several days in solution to form [Cp*Os(μ-NO)]2; this dinuclear compound can also be formed directly by reduction of 1 with zinc powder. The X-ray crystal structure of [Cp*Os(μ-NO)]2 shows that nitrosyl ligands are bridging and that the Os−Os distance is 2.539(1) Å. Compound 1 reacts with MgR2 to form the monoalkylated products Cp*Os(NO)RBr, where R = Me, CH2SiMe3, Ph, or o-Tol. The slow ligand substitution kinetics of this reaction prevent the formation of dialkyls of stoichiometry Cp*Os(NO)R2, even after long reaction times or when a large excess of alkylating agent is used. Dialkyls such as Cp*Os(NO)Me2 can, however, be obtained by treatment of Cp*Os(NO)MeBr with silver trifluoromethanesulfonate followed by addition of dimethylmagnesium.
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