摘要
用 2 ,4,6 三硝基间苯二酚 (斯蒂芬酸 ,TNR)镍的水溶液和碳酰肼 (CHZ ,NH2 NHCONHNH2 )水溶液反应 ,制备出配合物 [Ni(CHZ) 3](TNR)·5H2 O ,测定了其晶体结构 ,并用TG DTG ,DSC和IR技术研究了其热分解机理 .该晶体属三斜晶系 ,P1空间群 ,晶胞参数a =1 0 45 40 (1 0 )nm ,b =1 1 6 71 (2 )nm ,c =1 2 2 78(2 )nm ,α=1 0 9 1 90 (1 0 )°,β=1 2 1 1 6 8(1 2 )°,γ =99 70 0 (1 0 )°,V =1 2 6 1 3(3)nm3,Z =2 ,Dc=1 744 g/cm3,μ(Mo ,Kα) =0 873mm-1,F(0 0 0 ) =6 88,R =0 0 41 9,Rw=0 1 0 5 3.在该配合物分子中 ,碳酰肼为双齿配体 ,由羰基O原子和 1位N原子与Ni2 + 离子配位 ,分子中共形成 3个五元平面螯合环 ,中心离子为六配位八面体结构 .该配合物在程序升温条件下 ,分两步脱去所含结晶水 ,第一步失去 4个结晶水 ,第二步失去 1个结晶水 ,在 5 0 0℃时的最终分解产物为Ni2 O3.
The compound [Ni(CHZ) 3] (TNR)·5H 2O was prepared by using nickel carbonate, the aqueous solution of styphnic acid and carbohydrazide as reagents. The crystal structure of [Ni(CHZ) 3] (TNR)·5H 2O was determined by using single crystal diffraction analysis. Thermal decomposition mechanisms of the compound were studied by using TG DTG, DSC and IR techniques. The crystalline was in triclinic system with space group P 1. The unit cell parameters are as follows: a =1.045 40(10) nm, b =1.167 1(2) nm , c =1.227 8(2) nm, α =109.190(10)°, β =121.168(12)°, γ =99.700(10)°, \{ V =\}1.261 3(3) nm 3, Z =2, D c=1.744 g/cm 3, μ (Mo, Kα )=0.873 mm -1 , F (000)=688, R =0.041 9, R w=0.105 3. Carbohydrazide served as a bidentate, coordinating to nickel cation with its carbonyl oxygen atom and the first nitrogen atom so that a five membered chelating ring is formed. There are three such rings in the molecule. The coordination number is six and its configuration is deformed octahedral. The decomposition mechanisms confirm that the first dehydration process lost four water molecules, and the second step dehydrate one molecule. The residue is Ni 2O 3 at 500 ℃, finally. [WT5HZ]
出处
《高等学校化学学报》
SCIE
EI
CAS
CSCD
北大核心
2000年第7期1005-1009,共5页
Chemical Journal of Chinese Universities
关键词
碳酰肼
斯蒂芬酸镍
晶体结构
热分解机理
Carbohydrazide
Nickel styphnate
Crystal structure
Thermal decomposition mechanism
