Tb. Gunnoe et al., STEPWISE OXIDATION OF BENZYLAMINE COORDINATED TO THE [TP'W(CO)(PHC(2)ME)](+) MOIETY, Journal of the American Chemical Society, 118(29), 1996, pp. 6916-6923
Coordination of benzylamine to the [Tp'W(CO)(PhC(2)Me)](+) moiety acti
vates the amine for stepwise oxidation by sequential hydride/proton re
moval steps. Each metal complex along the stepwise reaction path (amin
e, amido, imine, azavinylidene, and nitrile) has been isolated and cha
racterized. The structure of the imine complex [Tp'W(CO)(PhC(2)Me)(NH
double bond CHPh)][BF4] (4) has been confirmed by an X-ray diffraction
study. Complex 4 crystallizes in the space group P2(1)/c (Z = 4, a =
13.790(3) Angstrom, b = 13.225(3) Angstrom, c = 19.150(4) Angstrom, be
ta = 108.769(1)degrees, R = 3.5%, R(w) = 4.4%), and key geometric feat
ures include a W-N dative bond length of 2.135(6) Angstrom to the imin
e nitrogen and a W-N-C angle of 129.7(5).