含Schiff碱水杨醛缩氨基硫脲钯(Ⅱ)配合物的晶体结构及荧光性质  

Crystal Structure and Fluorescence Character of Palladium(Ⅱ) Complex Containing Salicylidene Thiosemicarbazone

作　　者：吴文士[1] 戴劲草[1] 郑玉婴[2] 黄婷婷[1] 蓝心仁[1] 林岩心[1] 

机构地区：[1]华侨大学材料学院,泉州362021 [2]福州大学化学化工学院,福州350002

出　　处：《化学学报》2004年第18期1801-1806,共6页Acta Chimica Sinica

基　　金：福建省自然科学基金 (No.E0 2 1 0 0 2 6);福建省重大科技基金 (No.2 0 0 3F0 0 6)资助项目

摘　　要：以Schiff碱水杨醛缩氨基硫脲 (简写为HL)和二氯化钯合成了配合物 [PdL2 ] + ·Cl-.X射线单晶衍射表明 ,配合物晶体属于单斜晶系 ,空间群为P2 1/c,分子式C16H18ClN6O2 PdS2 ,Mr=5 3 2 .3 3 ,晶体学参数 :a =0 .70 0 0 5 ( 2 )nm ,b =1.0 5 813 ( 3 )nm ,c =2 .70 614 ( 9)nm ,β =93 .0 3 6( 1)° ,V =2 .0 0 17( 1)nm3 ,Z =4,Dc=1.766Mg/m3 ,F( 0 0 0 ) =10 68,μ(MoKα) =1.2 95mm-1,R =0 .0 2 5 2 ,wR =0 .0 5 93 ,GOF =1.0 2 0 .在配合物 [PdL2 ] + 离子中 ,钯 (Ⅱ )原子呈扭曲的NOS2 平面四边形配位构型 ,晶体通过分子间氢键作用形成一维的无限链状结构 .红外光谱表明 ,配体在形成配合物后 ,ν(SO) ,ν(CO)和ν(CN)红移 .电子光谱表明存在π π 和d π 的跃迁 .荧光光谱表明 ,配合物金属对配体n π 激发引起的荧光发射峰有较大的影响 .The title complex [PdL 2]+·Cl- ( C 16H 18ClN 6O 2PdS 2, M r=532.33), where HL is salicylidene thiosemicarbazone, has been synthesized from HL and palladium(Ⅱ) chloride in a mixture of dichloromethane and methanol. Crystal data: space group P2 1/c, a=0.70005(2) nm, b=1.05813(3) nm, c=2.70614(9) nm, β=93.036(1)°, V=2.0017(1) nm3, Z=4, D c=1.766 Mg/m3, F(000)=1068, μ(Mo Kα)=1.295 mm -1, R=0.0252, for 3457 observed reflections [I≥2σ(I)], wR=0.0593, GOF=1.020. The palladium(Ⅱ) atom in the complex [PdL 2]+ ion is coordinated with NOS 2, forming a distorted square arrangement. There are several intermolecular hydrogen bonds in the crystal. The one-dimensional chain structure was formed through the intermolecular hydrogen bonds N—H…Cl. The ν(CO) and ν(CN) bands display a shift to low frequencies in IR spectra of the complex. π-π* charge transitions and d-π* charge transitions were observed in their electronic spectra. The emission lines (λ ex=310 nm, n-π* charge transitions) are influenced by the metal of the complex in fluorescence spectra.

关 键 词：SCHIFF碱 水杨醛缩氨基硫脲 钯配合物 晶体结构 荧光性质 芳香醛腙配合物 

分 类 号：O641.4[理学—物理化学]