173467-73-7Relevant academic research and scientific papers
Synthesis and characterization of arene, mono-and dihydrido-arene, monohydrido-cyclopentadienyl, and phosphite complexes of molybdenum containing the tridentate ligand PhP (CH2CH2PPh2)2
Hammud, Hassan H.,George, T. Adrian,Kurk, David N.,Shoemaker, Richard K.
, p. 153 - 159 (2008/10/08)
The reduction of [MoCl3(TRI)], where TRI = PhP(CH2CH2PPh2)2, with sodium amalgam in benzene, toluene or anisole resulted in the formation of the corresponding [Mo(η6-arene) (TRI)] complex. Each complex displayed a reversible one-electron oxidation in the cyclic voltammogram at ～ - 1.0 V versus the ferrocenium/ferrocene couple at 0.0 V, corresponding to the oxidation of Mo(0) to Mo(1+). A second pseudo-reversible oxidation occurred at ～0.7 V more positive. Monoprotonation of the arene complexes with CF3COOH in THF resulted in the isolation of [Mo(H)(η6-arene)(TRI)][CF3COO] (δ(MoH) ～ - 6 ppm). In neat CF3COOH or HBF4, evidence of diprotonation of the arene complexes was observed in the 1H NMR spectra. Upon work-up, only the monoprotonated product was isolated. [Mo(TRI)(P(OMe)3)] was formed by the reduction of [MoCl3(TRI)] in the presence of a small excess of P(OMe)3. Attempts to prepare [Mo(TRI)(PMe3)3] by a similar method resulted in a product that readily absorbed N2 to form fac-[Mo(N2)(TRI)(PMe3)2]. Yellow [Mo(H)(η5-C5H5)(TRI)] was formed by (i) the reduction of [MoCl3(TRI)] with sodium amalgam in the presence of cyclopentadiene, or (ii) heating fac-[Mo(N2)(TRI)(PMe3)2] with cyclopentadiene in heptane, or (iii) heating trans-[Mo(N2)2(TRI)(PPh3)] with cyclopentadiene in THF.
