化学学报 ›› 2004, Vol. 62 ›› Issue (18): 1801-1806. 上一篇    下一篇

研究论文

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

吴文士1, 戴劲草1, 郑玉婴2, 黄婷婷1, 蓝心仁1, 林岩心1   

  1. 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
  • 投稿日期:2004-04-14 修回日期:2004-07-06 发布日期:2014-02-17
  • 通讯作者: 吴文士,E-mail:wuwenshi@sohu.com;Tel:0595-22691376,13159011162. E-mail:wuwenshi@sohu.com
  • 基金资助:
    福建省自然科学基金(No.E0210026)和福建省重大科技基金(No.2003F006)资助项目.

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

WU Wen-Shi1, DAI Jing-Cao1, ZHENG Yu-Ying2, HUAUG Ting-Ting1, LAN Xin-Ren1, LIN Yan-Xin1   

  1. 1. College of Material, Huaqiao University, Quanzhou 362021;
    2. College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350002
  • Received:2004-04-14 Revised:2004-07-06 Published:2014-02-17

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P21/c,分子式C16H18ClN6O2PdS2,Mr=532.33,晶体学参数:a=0.70005(2)nn,b=1.05813(3)nm,c=2.70614(9)nm,β=93.036(1)°,V=2.0017(1)nm3,Z=4,Dc=1.766 Mg/m3,F(000)=1068,μ(MoKa)=1.295mm-1,R=0.0252,wR=0.0593,GOF=1.020.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,v(S=O),v(C=O)和v(C=N)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.

关键词: 晶体结构, 水杨醛缩氨基硫脲, 钯配合物, 荧光性质

The title complex [PdL2]+·Cl- (C16H18ClN6O2PdS 2, Mr=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 P21/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, Dc=1.766 Mg/m3, F(000)=1068, μ(MoKα)=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 [PdL2]+ ion is coordinated with NOS2, 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(C=O) and ν(C=N) 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.

Key words: crystal structure, salicylidene thiosemicarbazone, palladium complex, fluorescence character