(C5H5)3Ln(THF)reacted with amine bis(phenol) LH2 [ L = Me2NCH2CH2N {CH2-(2-O-C6H2-But^1-3-Me- 5)}2 ] in a 1:1 molar ratio in THF to generate the amine bis(phenolato) cyclopentadienyl lanthanide complexes LL...(C5H5)3Ln(THF)reacted with amine bis(phenol) LH2 [ L = Me2NCH2CH2N {CH2-(2-O-C6H2-But^1-3-Me- 5)}2 ] in a 1:1 molar ratio in THF to generate the amine bis(phenolato) cyclopentadienyl lanthanide complexes LLn(C5H5) (THF)·(THF),(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, P21/c space goup, 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, Dc = 1.338 mg· m^3,μ = 1240 mm^-1, F(000)= 1488, R =0.0249, wR = 0.0568. The crystal data of complex 2 are monoclinic, P21/c sp ace goup, a = 0.9692 (1) nm, b = 1.4583 (2) nm, c = 2.8192 (3) nm, = 96.805 (2)°, V = 3.9584 (7) nm^3, Z=4, Dc =1.340 mg · ma, 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 ε-caprolactone polymerization.展开更多
基金Project supported by the National Natural Science Foundation of China (20472063)the Key Laboratory of Organic Synthesis of Jiangsu Province
文摘(C5H5)3Ln(THF)reacted with amine bis(phenol) LH2 [ L = Me2NCH2CH2N {CH2-(2-O-C6H2-But^1-3-Me- 5)}2 ] in a 1:1 molar ratio in THF to generate the amine bis(phenolato) cyclopentadienyl lanthanide complexes LLn(C5H5) (THF)·(THF),(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, P21/c space goup, 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, Dc = 1.338 mg· m^3,μ = 1240 mm^-1, F(000)= 1488, R =0.0249, wR = 0.0568. The crystal data of complex 2 are monoclinic, P21/c sp ace goup, a = 0.9692 (1) nm, b = 1.4583 (2) nm, c = 2.8192 (3) nm, = 96.805 (2)°, V = 3.9584 (7) nm^3, Z=4, Dc =1.340 mg · ma, 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 ε-caprolactone polymerization.