Synthesis, Characterization, and Reactivity of Amine Bis(phenolato) Cyclopentadienyl Lanthanide Complexs

Abstract

(C 5H 5), Ln(THF) reacted with amine bis(phenol) LH 2 [L = Me 2NCH 2CH 2N {CH 2-(2-O-C 6H 2-Bu t-3-Me-5)} 2] in a 1:1 molar ratio in THF to generate the amine bis(phenolato) cyclopentadienyl lanthanide complexes LLn(C 5H 5) (THF) · (THF) n (Ln = La ( 1), n = 0; Ln = Sm( 2), n = 1) in high yields. Complexes 1 and 2 were fully characterized by elemental analysis, NMR (for 1) and IR spectra, and X-ray structural determination. The crystal data of complex 1 are monoclinic, P2 1/ c space group, a = 1.1595(1) nm, b = 1.8588(2) nm, c = 1.6647(1) nm, β = 98.490(2)°, V = 3.5486(5) nm 3, Z=4, D c = 1.338 mg · m −3, μ = 1.240 mm −1, F(000) = 1488, R = 0.0249, wR = 0.0568. The crystal data of complex 2 are monoclinic, P2 1/ c space group, a = 0.9692(1) nm, b = 1.4583(2) nm, c = 2.8192(3) nm, β = 96.805(2)°, V = 3.9584(7) nm 3, Z = 4, D c = 1.340 mg · m −3, μ = 1.524 mm −1, F(000) = 1668, R = 0.0346, wR = 0.0756. The attempts failed to synthesize the amine bis (phenolate) lanthanide alkoxides by the reactions of complexes 1 and 2 with alcohols. The preliminary results revealed that complex 1 can initiate ɛ-caprolactone polymerization.