物理化学学报 >> 2000, Vol. 16 >> Issue (05): 441-446.doi: 10.3866/PKU.WHXB20000513

研究论文 上一篇    下一篇

[Pb2(TNR)2(CHZ)2(H2O)2]4H2O的结构及热分解机理

吕春华, 张同来, 乔小晶, 蔡瑞娇, 郁开北   

  1. 北京理工大学机电工程系,北京 100081|中国科学院成都分院分析测试中心,成都 610041
  • 收稿日期:1999-09-24 修回日期:1999-12-28 发布日期:2000-05-15
  • 通讯作者: 张同来

Structure and Thermal Decomposition Mecharism of [Pb2(TNR)2(CHZ)2(H2O)2]4H2O

Lv Chun-Hua, Zhang Tong-Lai, Qiao Xiao-Jing, Cai Rui-Jiao, Yu Kai-Bei   

  1. The Department of Mechano-electric Engineering,Beijing Institute of Technology,Beijing 100081|Chengdu Branch,Chinese Science Academy,Chengdu 610064
  • Received:1999-09-24 Revised:1999-12-28 Published:2000-05-15
  • Contact: Zhang Tong-Lai

摘要:

用碳酰肼 (CHZ ,NH2 NHCONHNH2 )、硝酸铅和三硝基间苯二酚 (TNR ,斯蒂酚酸 )的水溶液制备 [Pb2 (TNR) 2 (CHZ) 2 (H2 O) 2 ]•4H2 O .采用单晶分析的方法测定它的分子结构 ,并用TG-DTG、DSC和IR相结合的技术研究它的热分解机理 .所得晶体属单斜晶系 ,P21/n空间群 .晶体学参数为 :a=0 .64700(10)nm ,b =1.6074(3)nm ,c=1.4883(3)nm ,β =97.4 2 ( 2 )° ,V =1.5349(5)n ,Z =2 ,DC=2 .572 g•cm- 3,μ(Mo ,Kα) =11.080cm- 1,F(000) =1128. 最终偏离因子R =0.0422, Rw=0.0735. 该配合物分子呈中心对称 ,两个羰基O原子形成两个氧桥 ,TNR2 - ,CHZ和H2O同时参与了与中心离子的配位.

关键词: 碳酰肼, 铅配合物, 分子结构, 热分解机理

Abstract:

The coordination compound of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O was prepared by using the aqueous solution of carbohydrazide, lead nitrate and sodium styphnate. The molecular structure of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O(C 7H 13 N 7O 12 Pb, Mr=594.43) was determined by using a single crystal diffraction analysis .The thermal decomposition mechanism of the title compound was studied by TGDTG, DSC and IR techniques. The crystal belongs to monoclinic with space group P2 1/n.The unit cell parameters are as follows: a=0.64700(10)nm, b=1.6074(3)nm, c=1.4883(3)nm,β=97.42(2)°,V=1.5349(5)nm3, Z=2, DC=2.572g•cm -3 ,μ(Mo, Kα)=11.080cm -1 , F(000)=1128. R=0.0422, Rw=0.0735. The binuclear lead coordination compound is bridged by two carbohydrazide molecules. The molecule has a symmetrical center. TNR 2- ,CHZ and H 2O coordinate with the central ions simultaneously.

Key words: Carbohydrazide, Led coordination compound, Molecular structure, Thermal decomposition Mechanism