镝(III)与酰腙及1,10菲啰啉多元配合物的晶体结构及荧光性质  

Crystal Structure, Fluorescence Characterization of Dysprosium(III) Multicomponent Complex with Acylhydrazone and 1,10-Phenanthroline

作　　者：杨锐[1] 何水样[1] 武望婷[1] 文振翼[1] 史启祯[1] 王大奇[2] 

机构地区：[1]西北大学化学系陕西省物理无机化学重点实验室 [2]聊城大学化学系,聊城252059

出　　处：《化学学报》2004年第20期2040-2044,F008,共6页Acta Chimica Sinica

基　　金：陕西省自然科学基金 (No.2 0 0 2B0 5);陕西省教育厅专项基金 (No.0 3JK0 85)资助项目

摘　　要：在水乙醇混合体系中 ,首次得到 2 羰基丙酸水杨酰腙 (C10 H10 N2 O4) ,1,10 菲啉 (C12 H8N2 ,简写作phen)与Dy(NO3 ) 3 ·3H2 O的配合物 [Dy(C10 H8N2 O4) (phen) (NO3 ) (H2 O) 2 ]·H2 O .该配合物属单斜晶系 ,空间群为P2 1/c,晶胞参数a =1 5 2 4( 3 )nm ,b =1 10 18( 19)nm ,c =1 468( 3 )nm ,β =92 2 8( 2 )° ,V =2 4 63 ( 7)nm3 ,Z =4,μ =3 10 0mm-1,Dc=1 83 1g/cm3 ,F( 0 0 0 ) =13 40 ,R =0 0 3 14 ,wR =0 0 660 ,GOF =0 966.测试结果表明 ,该单晶结构为镝的 9配位配合物 ,其中一个 2 羰基丙酸水杨酰腙分子以羧基氧、酰胺基中的羰基氧和CN中的氮与Dy3 + 三齿配位 ,形成两个稳定的共边五元环 ,一个 1,10 菲啉分子以二齿方式配位、一个硝酸根和两个水分子也同时参与配位 ,在空间呈扭曲的单帽四方反棱柱 ,而在配合物周围还有一个游离的水分子 .Dysprosium(III) complex with 2-oxo-propionic acid salicyloyl hydrazone (C_(10)H_(10)N_2O_4) and 1,10-phenanthroline (C_(12)H_8N_2, phen) has been synthesized. The yellow prismatic crystal complex crystallizes in the monoclinic system with space group P2_1/c and parameters a=1.524(3) nm, b=1.1018(19) nm, c=1.468(3) nm, β=92.28(2)°, V=24.63(7) nm^3, Z=4, μ=3.100 mm^(-1), D_c=1.831 g/cm^3, F(000)=1340, R=0.0314, (wR=)0.0660, GOF=0.966. Dysprosium atom is 9-coordinated by carboxyl and carbonyl O atoms and N atom of one tridentate C_(10)H_(10)N_2O_4 ligand to form two stable five-membered rings with the same edge, and the other coordinated atoms coming from one bidentate phen, one bidentate nitrate and two water molecules. The coordination polyhedron around Dy^(3+) was described as a monocapped square antiprism. There is a lattice water molecule in the crystal cell. Luminescence measurement shows that the complex emits fluorescence.

关 键 词：1 10-菲哕啉 镝配合物 晶体结构 荧光性质 2-羰基丙酸水杨酰腙 

分 类 号：O641.4[理学—物理化学]