苯并15冠5钯配合物:[K(B15C5)_2]_2[Pd(SCN)_4]的合成与结构研究  

Synthesis and Structure of Benzo-15-Crown-5 Complex with Palladium(Ⅱ):[K(B15C5)_2]_2[Pd(SCN)_4]

作　　者：张文圣[1] 朱德中[2] 窦建民[2] 刘颖[2] 王大奇[2] 雍伟[3] 郑培菊[3] 

机构地区：[1]德州学院化学系,山东省德州市253023 [2]聊城师范学院化学系,山东省聊城市文化路34号252000 [3]复旦大学分析测试中心,上海市200433

出　　处：《光谱实验室》2001年第3期281-285,共5页Chinese Journal of Spectroscopy Laboratory

摘　　要：合成了苯并 15冠 5与钯生成的配合物 :[K( B15C5) 2 ]2 [Pd( SCN) 4],并通过元素分析、红外光谱及 X射线单晶结构分析进行了表征。配合物为单斜晶系、空间群 P2 1/ n。晶体学数据 :a=1.2 0 4 30 ( 7) ,b=1.932 99( 10 ) ,c=1.56680 ( 9) nm,β=10 8.1190 ( 10 )°,V=3.4 665( 3) nm3,Z=2 ,F( 0 0 0 ) =142 4 ,R1=0 .0 50 0 ,w R2 =0 .1549。配合物由两个 [K( B15C5) ]+2 配阳离子和一个 [Pd( SCN) 4]2 -配阴离子组成。四个硫氰酸根的硫原子与钯原子配位 ,[Pd( SCN) 4]2 -为平面方形构型。 K+与 2个冠醚环的 10个氧原子成键而形成夹心型结构。两个苯并 15冠The title compound:bis[bis(2,3,5,6,8,9,11,12\|octahydro\|benzopentaoxacyclopentadecin)\|potassium]tetrathiocyanatopalladate,[K(B15C5) 2] 2[Pd(SCN) 4],has been isolated and characterized by element analysis,IR and X\|ray diffraction analysis.The complex belongs to monoclinic, space group P2 1/n with cell dimensions: a =1.20430(7), b =1.93299(10), c =1.56680(9)nm, β =108.1190(10)°, V =3.4665(3)nm 3, Z =2, F (000)=1424, R 1 =0.0500, wR 2 =0.1549.Pd atom is coordinated by four S atoms and [Pd(SCN) 4] 2- is square planar configuration.K + is coordinated by ten oxygen atoms to form a sandwich structure with two crown ether rings.Two benzene rings from two B15C5 molecules are trans\|orientation with respect to potassium ion.

关 键 词：冠醚 苯并15冠 钯配合物 合成 结构 红外光谱 X射线分析 

分 类 号：O614.823[理学—无机化学]