212784-29-7Relevant academic research and scientific papers
Synthesis of rhenium complexes that contain the [(C6F5NCH2CH2)3N] 3- ligand
Reid, Steven M.,Neuner, Brigitte,Schrock, Richard R.,Davis, William M.
, p. 4077 - 4089 (1998)
The reaction between [Et4N]2[ReOCl5] and (C6F5NHCH2CH2)3N (H3[N3NF]) in CH3CN at room temperature in the presence of NEt3 yielded air stable, emerald green, diamagnetic [(C6F5NCH2CH2)2NCH 2CH2NHC6F5]Re(O)Cl (1). The reaction between 1 and Ta(CH-t-Bu)(THF)2Br3 gave paramagnetic [N3NF]ReBr (2). An X-ray structure of a sample of 2 showed it to be analogous to that of [N3NF]MoCl. Reduction of 2 by methyllithium (or more conveniently by Mg) in the presence of a variety of two-electron ligands gave complexes of the type [N3NF]Re(L) (L = H2, ethylene, propylene, CO, N2, phosphines, pyridine, tetrahydrothiophene, acetonitrile, or silanes). An X-ray structure of [N3NF]Re(ethylene) showed η2-ethylene to be bound in the apical "pocket" with its C-C axis lying in one of the Nax- Re-Neq planes. Protonation of the PMe3 complex gave an authentic hydrido phosphine complex, {[N3NF]Re(H)(PMe3)}+, but protonation of other phosphine complexes gave species in which coupling between H and P is relatively large (～60 Hz) and therefore that are believed to have some {[N3NF]Re(η2-HPRxH 3-x)}+ character. An X-ray study of {[N3NF]Re(H)-(PHPh2)}+ confirmed that one proton is terminally bound to phosphorus and that the phosphorus is "off-axis" in order to accommodate the "hydride" in the same plane.
