Preparation, Crystal Structure and Thermal Decomposition Mechanisms of [Ni(CHZ)3] (TNR)·5H2O

Abstract

Abstract: The compound [Ni(CHZ)₃] (TNR)·5H₂Owas prepared by using nickel carbonate, the aqueous solution of styphnic acid and carbohydrazide as reagents. The crystal structure of [Ni(CHZ)₃] (TNR)·5H₂Owas determined by using single crystal diffraction analysis. Thermal decomposition mechanisms of the compound were studied by using TG DTG, DSCand IRtechniques. The crystalline was in triclinic system with space group P1 The unit cell parameters are as follows: a =1.04540(10) nm, b =1.1671(2) nm , c =1.2278(2) nm, α =109.190(10)°, β =121.168(12)°, γ =99.700(10)°, {V =}1.2613(3) nm³, Z =2, Dc=1.744 g/cm³, μ(Mo, Kα)=0.873 mm^-1 , F (000)=688, R =0.0419, R_w=0.1053. 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 Ni₂O₃ at 500 ℃, finally.

Key words: Carbohydrazide, Nickel styphnate, Crystal structure, Thermal decomposition mechanism

CLC Number:

O614.81

TrendMD:

LU Chun-Hua, ZHANG Tong-Lai, ZHANG Jian-Guo, CAI Rui-Jiao . Preparation, Crystal Structure and Thermal Decomposition Mechanisms of [Ni(CHZ)₃] (TNR)·5H₂O[J]. Chem. J. Chinese Universities, 2000, 21(7): 1005.

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Preparation, Crystal Structure and Thermal Decomposition Mechanisms of [Ni(CHZ)₃] (TNR)·5H₂O

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