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 ,P2 1/n空间群 .晶体学参数为 :a=0 .6470 0 ( 10 )nm ,b =1.60 74 ( 3)nm ,c=1.4 883( 3)nm ,β =97.4 2 ( 2 )° ,V =1.534 9( 5)n ,Z =2 ,DC=2 .572 g·cm- 3,μ(Mo ,Kα) =11.0 80cm- 1,F( 0 0 0 ) =112 8.最终偏离因子R =0 .0 4 2 2 ,Rw=0 .0 735.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H2
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,M r=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)n,Z=2,D C=2.572g·cm -3 ,μ(Mo,Kα)=11.080cm -1 ,F(000)=1128.R=0.0422,R w=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.
出处
《物理化学学报》
SCIE
CAS
CSCD
北大核心
2000年第5期441-446,共6页
Acta Physico-Chimica Sinica
关键词
碳酰肼
铅配合物
分子结构
热分解机理
Carbohydrazide, Lead coordination compound, Molecular structure, Thermal decomposition Mechanism
