三（3－苯基－4－苯甲酰基异噁唑酮－5）－乙醇－水合铕三元配合物的合成、表征及晶体结构

Synthesis,Characterization and Crystal Structure Studies on a Mixed Ligand Complex of Aquatris(3-phenyl-4-benzoyl-5-isoxazolone)(Ethanol) Europium Monohydrate[Eu(PBI)_3(C_2H_5OH)(H_2O)]·H_2O

合成了三（３－苯基－４－苯甲酰基异唑酮－５）－乙醇－水合铕的配合物。有关鉴定和元素分析结果表明：该配合物的分子式为［Ｅｕ（ＰＢＩ）３（Ｃ２Ｈ５ＯＨ）（Ｈ２Ｏ）］·Ｈ２Ｏ，其中３－苯基－４－苯甲酰基异唑酮－５简记为ＨＰＢＩ，是一种新型高酸度的β－双酮。用Ｘ射线单晶衍射法测定了［Ｅｕ（ＰＢＩ）３（Ｃ２Ｈ５ＯＨ）（Ｈ２Ｏ）］·Ｈ２Ｏ的晶体结构，结果表明，该晶体属单斜晶系，Ｐ２１／ａ空间群，晶胞参数：ａ＝１．５５８６（９）ｎｍ，ｂ＝２．１２９７（７）ｎｍ，ｃ＝１．６０４（１）ｎｍ，β＝１１７．９７（５）°，Ｖ＝４．７０３（９）ｎｍ３，Ｚ＝４．中心离子铕为八配位，其配位多面体为畸变的双帽三棱柱。配位的８个氧原子分别来自３个ＰＢＩ配体中的６个氧、１个溶剂化乙醇分子中的氧和１个水分子中的氧，Ｅｕ—Ｏ配位键平均键长０．２３９１（４）ｎｍ。晶体结构中还存在１个未配位的水分子。该水分子、配位水分子、乙醇分子与配体ＰＢＩ中的Ｎ原子之间均存在强的氢键作用。同一ＰＢＩ基团内配位氧之间的平均距离为０．２８０８ｎｍ。

The[Eu(PBI)3(C2H5OH)(H2O)]·H2O was systhesized by reacting Eu2O3 with highly acidic β-diketone 3-phenyl-4-benzoyl-5-isoxazolone(HPBI) in C2H5OH under heating.The X-ray single crystal structure analysis shows that the crystal is monoclinic with space group P2 1/a and the unit cell parameters are as follows:a=1.5586(9) nm,b=2.1297(7) nm,c=1.604(1) nm,β=117.97(5)°,V=4.703(9) nm3,Z=4.The central ion Eu3+ is eight coordinated by six oxygen atoms from three β-diketone,one from water and one from C2H5OH molecule.The coordination polyhedron takes bicapped triangular prism arrangement.The Eu-O average bond length is 0.2391(4) nm.The average distance of O-Owithin a β-diketone is 0.2808 nm which is larger than those for other β-diketones.