Acta Chimica Sinica ›› 2005, Vol. 63 ›› Issue (21): 1967-1973. Previous Articles     Next Articles

Original Articles

N-皮考林酰肼及其双核钯配合物的晶体结构和荧光性质

吴文士*,陈静,戴劲草,林建明,蓝心仁,黄婷婷   

  1. (华侨大学材料学院 泉州 362021)
  • 收稿日期:2005-02-24 修回日期:2005-07-20 出版日期:2005-11-14 发布日期:2010-12-10
  • 通讯作者: 吴文士

Crystal Structure and Fluorescence of N-Picoloylhydrazide and Its Binuclear Palladium Complex

WU Wen-Shi*, CHEN Jing, DAI Jing-Cao, LIN Jian-Ming, LAN Xin-Ren, HUANG Ting-Ting   

  1. (College of Material, Huaqiao University, Quanzhou 362021)
  • Received:2005-02-24 Revised:2005-07-20 Online:2005-11-14 Published:2010-12-10
  • Contact: WU Wen-Shi

N-Picoloylhydrazide (Hphz) and its binuclear palladium complex [Pd2(phz)2Cl2] were synthesized and determined by single crystal X-ray diffraction. They belong to monoclinic system. Crystal data: Hphz(C6H7N3O), space group C2/c, a=1.9245(2) nm, b=0.38927(2) nm, c=1.8073(2) nm, b=107.255(2)°, V=1.2931(2) nm3, Z=8, Dc=1.409 Mg/m3, F(000)=576, m(Mo Kα)=0.102 mm-1, 0.0541 for 1257 observed reflections [I≥σ(I)], wR=0.1762, GOF=1.124; [Pd2(phz)2Cl2](C12H12Cl2N6O2Pd2), space group P21/c, a=1.48274(9) nm, b=1.44797(9) nm, c=0.73951(5) nm, β=92.719(3)°, V=1.5860(2) nm3, Z=4, Dc=2.329 Mg/m3, F(000)=1072, μ(Mo Kα)=2.62 mm-1, R=0.0262 for 2937 observed reflections [I≥σ(I)], wR=0.0555, GOF=0.959. The palladium(II) ion of the complex [Pd2(phz)2Cl2] is coordinated with two pyridine nitrogen atom and two diazine nitrogen atom, forming a distorted square geometry. Pd…Pd distance is 0.38111 nm in the complex. There is a one-dimensional chain structure through the intermolecular hydrogen bonds N—H…Cl in complex crystal. There are π-π interactions in the neighboring ligands. The ab initio calculation with Hartree-Fork method showed that there are interactions between Pd and Pd in the complex molecule and the neighboring molecule. ν(C=O) and ν(C=N) were shifted to lower frequencies and ν(C—N) was shifted to higher frequencies in IR spectra. The emission lines (lex=310 nm) were shifted to higher frequencies in fluorescence spectra.

Key words: crystal structure, N-picoloylhydrazide, binuclear palladium complex