Synthesis and characterization of lanthanide complexes containing a bulky tridentate [N,N,O] Schiff base ligand
来源期刊：JOURNAL OF RARE EARTHS2008年第4期
论文作者：ZHANG Yong WANG Yaorong SHEN Qi YAO Yingming LI Bangyu
Key words：Schiff base lanthanide complex; crystal structure; synthesis; rare earths;
Abstract: The lanthanide complexes containing a bulky tridentate [N,N,O] Schiff base ligand 3,5-But2-2-(OH)C6H2CH=N-8-C9H6N (HL) were synthesized and characterized. The reaction of anhydrous LnCl3 with NaL formed in situ in a 1:1 molar ratio in THF at room temperature afforded the lanthanide Schiff base dichloride complexes LnLCl2(DME) (Ln=Eu (1);Sm (2)). Complexes 1 and 2 can be used as precursors for the synthesis of the lanthanide cyclopentadienyl Schiff base derivatives. The reactions of complexes 1 and 2 with one equiv of NaCH3C5H4 in THF provided the desired products LnL(CH3C5H4)Cl(THF)·THF (Ln=Eu (3);Sm (4)) in good isolated yields. These complexes were characterized by elemental analysis, IR spectra, and X-ray structural determination, in the case of complexes 3 and 4. The crystal data of complex 3 are monoclinic, P21/c space group, a=1.3370(2) nm, b=1.5190(2) nm, c=1.8910(3) nm, β=109.846(4)°, V=3.6125(8) nm3, Z=4, Dc=1.416 mg/m3, μ=1.847 mm-1, F(000)=1584, R=0.0707, wR=0.1350. The crystal data of complex 4 are monoclinic, P21/c space group, a=1.3383(1) nm, b=1.5210(2) nm, c=1.8960(2) nm, β =109.878(3)°, V=3.6293(7) nm3, Z=4, Dc=1.407 mg/m3, μ=1.728 mm-1, F(000)=1580, R=0.0670, wR=0.1385.
ZHANG Yong1，WANG Yaorong2，SHEN Qi1，YAO Yingming1，LI Bangyu1
(1.Key Laboratory of Organic Synthesis of Jiangsu Province, Department of Chemistry and Chemical Engineering, Suzhou University, Suzhou 215123, China;
2.College of Material Engineering, Suzhou University, Suzhou 215123, China)
Abstract:The lanthanide complexes containing a bulky tridentate [N,N,O] Schiff base ligand 3,5-But2-2-(OH)C6H2CH=N-8-C9H6N (HL) were synthesized and characterized. The reaction of anhydrous LnCl3 with NaL formed in situ in a 1:1 molar ratio in THF at room temperature afforded the lanthanide Schiff base dichloride complexes LnLCl2(DME) (Ln=Eu (1);Sm (2)). Complexes 1 and 2 can be used as precursors for the synthesis of the lanthanide cyclopentadienyl Schiff base derivatives. The reactions of complexes 1 and 2 with one equiv of NaCH3C5H4 in THF provided the desired products LnL(CH3C5H4)Cl(THF)·THF (Ln=Eu (3);Sm (4)) in good isolated yields. These complexes were characterized by elemental analysis, IR spectra, and X-ray structural determination, in the case of complexes 3 and 4. The crystal data of complex 3 are monoclinic, P21/c space group, a=1.3370(2) nm, b=1.5190(2) nm, c=1.8910(3) nm, β=109.846(4)°, V=3.6125(8) nm3, Z=4, Dc=1.416 mg/m3, μ=1.847 mm-1, F(000)=1584, R=0.0707, wR=0.1350. The crystal data of complex 4 are monoclinic, P21/c space group, a=1.3383(1) nm, b=1.5210(2) nm, c=1.8960(2) nm, β =109.878(3)°, V=3.6293(7) nm3, Z=4, Dc=1.407 mg/m3, μ=1.728 mm-1, F(000)=1580, R=0.0670, wR=0.1385.
Key words:Schiff base lanthanide complex; crystal structure; synthesis; rare earths;
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