高等学校化学学报

高等学校化学学报 ›› 2009, Vol. 30 ›› Issue (5): 845.

• 研究论文 • 上一篇    下一篇

(C6H8N3)+I3-和[(Cu3I4)(C8H17N2)]配体原位合成与结构表征

宁德宽, 毕明辉, 李光华, 刘国宗, 施展, 冯守华   

  1. 无机合成与制备化学国家重点实验室, 吉林大学化学学院, 长春 130012
  • 收稿日期:2009-01-22 出版日期:2009-05-10 发布日期:2009-05-10
  • 通讯作者: 施展, 男, 博士, 教授, 博士生导师, 主要从事无机合成化学研究, E-mail: zshi@mail.jlu.edu.cn
  • 基金资助:

    国家自然科学基金(批准号: 20631010, 20671040和20601010)资助.

Synthesis and Structure Characterization of (C6H8N3)+I3- and [(Cu3I4)(C8H17N2)] Based on in situ Ligand Reaction

NING De-Kuan, BI Ming-Hui, LI Guang-Hua, LIU Guo-Zong, SHI Zhan*, FENG Shou-Hua   

  1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, China
  • Received:2009-01-22 Online:2009-05-10 Published:2009-05-10
  • Contact: SHI Zhan, E-mail: zshi@mail.jlu.edu.cn

PDF (PC)

摘要：

在溶剂热条件下, 以原位反应为基础合成了两个碘化物(C6H8N3)+I3-(1, C6H8N3=2,3-dihydroimi-dazo[1,2-a]pyrimidin-1-ium, 2,3-二氢咪唑[1,2-α]-嘧啶鎓阳离子)和[(Cu3I4)(C8H17N2)](2, C8H17N2=N-ethyl-4-aza-1-azonia-bicyclo[2.2.2]octane, N-乙基三乙烯二铵阳离子). 用元素分析、粉末X射线衍射及单晶X射线衍射等对化合物进行了表征. 结果表明, 化合物1属于三斜晶系, P1空间群, a=0.74281(15) nm, b=0.84241(17) nm, c=0.9993(2) nm, α=82.02(3)°, β=83.30(3)°, γ=82.92(3)°, V=0.6114(2) nm3. 化合物2属于单斜晶系, P21/c空间群, a=0.68924(14) nm, b=1.0786(2) nm, c=2.2779(5) nm, β=94.84(3)°, V=1.6874(6) nm3. 在两个化合物合成中存在两种不同类型的配体原位合成反应, 即化合物1的2-氨基嘧啶和乙醇的成环反应与化合物2的三乙烯二胺和乙醇的烷基化反应.

关键词: 晶体结构, 溶剂热, 原位合成, 碘化亚铜

Abstract:

Two I-containing compounds, (C6H8N3)+I3-(1, C6H7N3=2,3-dihydroimidazo[1,2-a]pyrimidine-1-ium) and [(Cu3I4)(C8H17N2)](2, C8H17N2=N-ethyl-1,4-diazabicyclo[2.2.2]octane), were synthesized under solvothermal conditions based on in situ ligand reaction and characterized via elemental analysis, XRD and single crystal X-ray diffraction analysis. Complex 1 crystallizes in the triclinic system, space group P1 with a=0.74281(15) nm, b=0.84241(17) nm, c=0.9993(2) nm, α=82.02(3)°, β=83.30(3)°, γ=82.92(3)°, V=0.6114(2) nm3. Complex 2 crystallizes in the monoclinic system, space group P21/c with a=0.68924(14) nm, b=1.0786(2) nm, c=2.2779(5) nm, β=94.84(3)°, V=1.6874(6) nm3. Two kinds of in situ ligand reaction were found in the synthesis of these complexes. (C6H8N3)+ ligand was synthesized from 2-aminopyrimidine and ethanol in complex 1, whereas(C8H17N2)+ ligand was synthesized from 1,4-diazabicyclo[2.2.2]octane and ethanol in complex 2.

Key words: Crystal structure, Solvothermal reaction, In situ reaction, Copper iodide

TrendMD: