Kg. Parker et al., SYNTHESES OF TANTALUM(V) COMPLEXES CONTAINING TETRAMETHYLPYRROLYL, PYRROLYL, AND INDOLYL LIGANDS, Inorganic chemistry, 35(11), 1996, pp. 3228-3234
The reaction of TaMe(3)Cl(2) with the lithium salt of tetramethylpyrro
le (Li-TMP) led to the formation of (eta(5)-TMP)TaMe(3)Cl (1). Reactio
ns of 1 with a series of anionic ligands have been carried out to form
products of the formula (eta(5)-TMP)TaMe(3)X, where X = SR, Me, pyrro
lyl, or indolyl. Crystals of (eta(5)-TEMP)TaMe(3)(indolyl) (5), were i
solated in space group P2(1)/c with a = 8.957(2) Angstrom, b = 28.540(
6) Angstrom, c = 14.695(3) Angstrom, beta = 99.40(3)degrees, V = 3706.
1(14) Angstrom(3), and Z = 8. The structure confirmed the eta(5)-bondi
ng mode of the tetramethylpyrrolyl ligand and the eta(1)-N-coordinatio
n mode of the indolyl ligand. The derivatives (eta(5)-TMP)TaMe(3)X sho
wed limited stability, and decomposition products which formed in tolu
ene solutions at room temperature have been identified in some cases.
The reaction of (eta(5)-TMP)TaMe(3)(pyrrolyl) with hydrogen (2-3 atm)
in benzene-d(6) solution at room temperature was studied. The stoichio
metric formation of cyclohexane-d(6) by hydrogenation of an equivalent
of solvent was confirmed by H-1 and C-13 NMR and gas chromatographic/
mass spectroscopic data. The characteristics and scope of the room tem
perature arene hydrogenation process are discussed.