Metal imido complexes (M=Ti, W) containing 2-(dimethylaminomethyl)pyrrote:Synthesis and the crystal structures of Bu(t)N=TiClPy2[2-Me2NCH2(C4H3N)] and PhN=WCl3[2-Me2NCH2(C4H3N)]
Jh. Huang et al., Metal imido complexes (M=Ti, W) containing 2-(dimethylaminomethyl)pyrrote:Synthesis and the crystal structures of Bu(t)N=TiClPy2[2-Me2NCH2(C4H3N)] and PhN=WCl3[2-Me2NCH2(C4H3N)], J CHIN CHEM, 47(4B), 2000, pp. 895-900
A titanium imido complex, (BuN)-N-t=TiClPy2[2-Me2NCH2-(C4H3N)] 1, was synth
esized through metathesis by reacting (BuN)-N-t=TiCl2Py3 with lithium 2-(di
methylaminomethyl) pyrrolate (LLi) in diethyl ether at room temperature. Th
e dark brown red crystals were obtained from a concentrated diethyl ether s
olution of compound 1 at -20 degreesC and the monoclinic crystal shows a di
storted octahedral structure with two pyridines taking trans positions. Hyd
rolysis (BuN)-N-t=TiCl2Py3 with 2,2'-methylene-bis(6-t-butyl-4-methylphenol
) (HO similar to similar to CH(2)similar to similar to OH) generates a bis
phenoxide titanium complex, (O similar to similar to CH(2)similar to simila
r toO)TiCl2Py 2, by eliminating one equivalent of (BuNH2)-N-t. Similarly, t
he reaction of LH with PhN=WCl4(OEt2) in diethyl ether at room temperature
generates PhN=WCl3(L) 3, in moderate yield. 3 has been characterized by NMR
spectroscopies and X-ray crystallography.