[Ni(H_2O)(tptz)(C_2O_4)]·4H_2O的合成、结构与表征

Synthesis,Complex and Characterization of[Ni(H_2O)(tptz)(C_2O_4)]·4H_2O

在CH3OH/H2O混合溶剂中,经2,4,6–三(2–吡啶基)–1,3,5–三嗪(tptz)、草酸和新制Ni(OH)2/NiCO3反应合成得到配合物[Ni(H2O)(tptz)(C2O4)]·4H2O.单晶X–射线衍射分析表明:它与已报道的[M(H2O)(tptz)(C2O4)]·4H2O(M=Co(2)、Cu(3)、Zn(4))配合物同晶形,属三斜晶系,P–1空间群,晶胞参数a=7.760(2),b=12.116(2),c=13.031(3),α=78.76(4)°,β=83.84(3)°,γ=78.69(3)°,V=1175.3(5)3,Z=2,Dc=1.543,F(000)=562,R1=0.0472,wR2=0.1350,GOF=1.088.在配合物的结构基础上与同晶形结构进行比较分析,并研究了它们的IR及TG/DTA测试表征.

Reaction of 2,4,6-tris（2-pyridyl）-1,3,5-triazine（tptz）, oxalic acid and freshly prepared Ni（OH）2/ Ni2CO3 in CH3OH/H2O solution yields the ti,tle complex [Ni（H2O）（tptz）（C2O4）]·4H2O. Single crystal X-ray diffraction indicates that it crystallizes isostructurally with Co, Cu, Zn analogues, in the triclinic space group Pi with the cell dimensions a=7.760（2）A, b=12.116（2）A, c=13.03 1（3）A, α=78.76（4）°, β=83.84（3）°, γ= 78.69（3）°, V=1175.3（5） A^3, Z=2, Dc=1.543, F（000）=562, R1=0.0472, wR2=0.1350, GOF=1.088. IR and thermal behaviors of the four isostructural complexs are discussed.