Abstract
Rhenium(V) para-tolylimido complexes TpRe(NTol)X 2 (X = Cl ( 2a); I ( 2b)) are formed on refluxing the oxo derivatives TpRe(O)X 2 (X = Cl ( 1a); I ( 1b)) with para-toluidine (Tp = hydrotris(pyrazalyl)borate; Tol = para-tolyl). Reaction of 2a with ZnEt 2 in benzene gives the imido-ethyl complex TpRe(NTol)(Et)Cl (( 3) Et = CH 2CH 3), which was characterized by an X-ray crystal structure. Photolysis of 2a and 3 apparently lead to ReI and ReC bond homolysis, as in their oxo congeners, but the analogous photoproducts are not observed. Reaction of 1a with amines at ambient temperatures leads to the oxo-amido compounds TpReO(NRR′)Cl. Complexes with primary amido ligands, TpReO(NHR)Cl (R = Et ( 4); nPr ( 5); iPr ( 6)) exist as two isomers by 1H NMR. Similarly, NMR spectra of compounds with symmetrical amido ligands, TpReO(NR 2)Cl (R = H ( 7); Et ( 8); NR 2 = piperidyl ( 9)), show inequivalent substituents. These data indicate restricted rotation about the ReN amido bond. Based on the X-ray crystal structure of 8, the barrier to rotation is electronic as well as steric in origin.
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