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化学学报
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化学学报 ›› 2002, Vol. 60 ›› Issue (5): 800-809. 上一篇    下一篇

研究论文

零维和一维钒氧簇合物的水热合成及晶体结构

单永奎;戴立益;余淑媛;叶生荣;何鸣元   

  1. 华东师范大学离子液体化学研究中心.上海(200062)
  • 发布日期:2002-05-15

Hydrothermal Synthesis and Crystal Structure of Zero-and One- dimensional Polyoxovanadates

Shan Yongkui;Dai Liyi;Yu Shuyuan;Ye Shengrong;He Mingyuan   

  1. Center for Chemistry of Ionic Liquids, East China Normal University. Shanghai(200062)
  • Published:2002-05-15

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被引次数

3 | 1

利用水热合成方法制备了一个零维钒氧簇合物，一个一维链状钒氧簇合物。并 通过X射线单晶衍射方法进行了结构表征，两个化合物的晶体学数据为：[Na-15-C- 5]_4(H)_2V_(15)O_(36)Cl(H_2O)_2 (1)，空间群为C2/c(No.15)，a = 2.8492(1) nm，b = 1.4842(3) nm，c = 2.3741(1) nm，β= 12.411(1)°，V = 8.3126(7) nm~3，Z = 4，R = 0.0558，R_w = 0.0988；[K-18-C-6]_4(H)_2V_(15)O_(36)Cl (2)，空间群C2/c(No.15)，a = 2.5588(1) nm，v = 1.4921(1) nm，c = 2.7113 (2) nm，β= 117.90(2)°，V = 9.148(1) nm~3，Z = 4，R = 0.0540，R_w 0. 1485。在一维链状化合物中含有阳离子的二聚体[K-18-crown-6]_2~(2+)作为桥连 链结，结构分析说明配位阳离子的几何变形性对结构有较大的影响。

关键词: 水热反应, 冠式化合物, 晶体结构, 钒, 氧, 簇状化合物, X射线衍射分析, 结构表征

A zero-dimension and a one-dimension polyoxovanadates [Na-15-C-5]_4 (H)_2V_(15)O_(36)Cl(H_2O)_2 (1) and [K-18-C-6]_4(H)_2V_(15)O_(36)Cl (2) have been hydrothermally synthesized and characterized by single- crystal X-ray diffraction. Compound 1 is crystallized in monoclinic space group C2/c with a = 2.8492 (1) nm, b = 1.4842 (3) nm, c = 2.3741 (1) nm, β= 12.411 (1)°, V = 8.3126(7) nm~3, Z = 4, R = 0.0558, R_w = 0.0988. Compound 2 is crystallized in monoclinic space group C2/c with a = 2.5588(1) nm, v = 1.4921(1) nm, c = 2.7113(2) nm, β= 117.90(2)°, V = 9.148(1) nm~3, Z = 4, R = 0.0540, R_w 0.1485. There is a dimeric cation [K-18-crown-6]_2~(2+) with double-charge as a bridge-linkage in the one-dimensional polyoxovanadate compound. The structures analysis of 1 and 2 reveals that the geometrical deformability of the coordinated cation has a significant effect on the structure.

Key words: HYDRO-THERMAL REACTION, CROWN ETHER COMPOUNDS, CRYSTAL STRUCTURE, VANADIUM, OXYGEN, CLUSTER COMPOUND, XRD, STRUCTURE CHARACTERISTICS

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