高等学校化学学报 ›› 2000, Vol. 21 ›› Issue (4): 509.

• 论文 • 上一篇    下一篇

具有十二元环开放结构磷酸锌的非水合成与表征

徐家宁1, 袁宏明1, 毛友钢2, 史苏华1, 李永佶3, 张泰善3, 宋天佑1, 冯守华1, 徐如人1   

  1. 1. 吉林大学化学系, 无机合成与制备化学开放实验室;
    2. 吉林大学超分子结构与谱学开放实验室, 长春 130023;
    3. 韩国化学研究所化学技术团, 大田 韩国, 305-600
  • 收稿日期:1999-06-23 出版日期:2000-04-24 发布日期:2000-04-24
  • 通讯作者: 宋天佑(1948年出生),男,博士,教授,从事无机合成研究.
  • 基金资助:

    国家自然科学基金(批准号:29731010);吉林大学无机合成与制备化学开放实验室基金

Nonaqueous Synthesis and Characterization of a Zincophosphate with 12-Membered Ring Channel Open Framework

XU Jia-Ning1, YUAN Hong-Ming1, MAO You-Gang2, SHI Su-Hua1, LEE Young-K.3, CHANG Tae-Sun3, SONG Tian-You1, FENG Shou-Hua1, XU Ru-Ren1   

  1. 1. Departmentof Chemistry, Key Laboratory of Inorganic Synthesisand Preparative Chemistry;
    2. Key Laboratoryof Supermolecular Structureand Spectra, Jilin University, Changchun, China, 130023;
    3. Chemical Technology Division, Korea Research Instituteof Chemical Technology, Taejon 305-600, Korea
  • Received:1999-06-23 Online:2000-04-24 Published:2000-04-24

摘要: 从非水体系中制备了Zn2(HPO4)3·H3NCH2CH2NH3单晶,用X射线测定了晶体结构,用红外光谱,DTA-TG等方法对化合物进行了表征.晶体属三斜晶系,P1 空间群.晶胞参数a=0.8215(3)nm,b=0.8557(3)nm,c=0.9760(3)nm,α=93.8(3)°,β=95.38(3)°,γ=109.75(3)°,V=0.6394nm3,Z=2,Dc=2.50g·cm-3.结构中的锌和磷均与氧形成四面体配位,ZnO4和HPO4四面体严格交替排列,骨架中的氧分为二桥氧和端氧,端氧只向P原子配位.三维开放式骨架结构中沿a轴和b轴方向有十二元环直孔道,质子化的有机胺在a轴方向的十二元环孔道中.

关键词: 磷酸锌, 非水体系, 晶体结构

Abstract: Single crystal of Zn2(HPO4)3·H3NCH2CH2NH3 was synthesized from nonaqueous system and its crystal structure was determined using single crystal X-ray diffraction. The crystal structure was solved by direct method and refined by full-matrix least-square method and the crystal is triclinic, space group P1 with a =0.8215(3) nm, b =0.8557(3) nm, c =0.9760(3) nm, α =93.8(3)°, β =95.38(3)°, γ =109.75(3)°, V =0.6394 nm3, Z =2, Dc=2.50 g·cm-3 , μ =43.0 cm-1 , R =0.031, Rw=0.040. The framework is built up from ZnO4 and HPO4 tetrahedra, forming a three dimensional network, and the linkage of Zn and Ptetrahedra displays a strict alternation of zinc and phosphorus. The open framework contains 8-membered ring channels and 12-membered ring channels. The results of XRD, IRand DTA-TGfor the compound are given.

Key words: Zincophosphate, Nonaqueous system, Crystal structure

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