Synthesis, Characterization, and Reactivity of Amine Bis(phenolato) Cyclopentadienyl Lanthanide Complexes
来源期刊：JOURNAL OF RARE EARTHS2007年第5期
论文作者：Zhou Lanzhi Zhang Yong Shen Qi Wang Yuming Yao Yingming
Key words：inorganic chemistry; amine bis(phenolate) lanthanide complex; crystal structure; rare earths;
Abstract: (C5H5)3Ln(THF) reacted with amine bis(phenol) LH2[L=Me2NCH2CH2N{CH2-(2-O-C6H2-But-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)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, P21/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) nm3, Z=4, Dc=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, P21/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) nm3, Z=4, Dc=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 ε-caprolactone polymerization.
Zhou Lanzhi1，Zhang Yong1，Shen Qi1，Wang Yuming2，Yao Yingming1
(1.Key Laboratory of Organic Synthesis of Jiangsu Province, Department of Chemistry and Chemical Engineering, Dushu Lake Campus, Suzhou University, Suzhou 215123, China;
2.Changzhou Institute of Mechatronic Technology, Changzhou 213164, China)
Abstract:(C5H5)3Ln(THF) reacted with amine bis(phenol) LH2[L=Me2NCH2CH2N{CH2-(2-O-C6H2-But-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)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, P21/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) nm3, Z=4, Dc=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, P21/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) nm3, Z=4, Dc=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 ε-caprolactone polymerization.
Key words:inorganic chemistry; amine bis(phenolate) lanthanide complex; crystal structure; rare earths;
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