Synthesis, Characterization and Phase Transformation of 3D Open-framework Zinc Phosphate [Zn6(H2O)P5O20][C5N2H14][C6H16N2]0.5·3H2O

Chemical Research in Chinese Universities ›› 2009, Vol. 25 ›› Issue (4): 407-411.

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Synthesis, Characterization and Phase Transformation of 3D Open-framework Zinc Phosphate [Zn₆(H₂O)P₅O₂₀][C₅N₂H₁₄][C₆H₁₆N₂]_0.5·3H₂O

SONG Yu^1,2, DONG Zhao-jun¹, WANG Yong-wei², FU Jun³* and LI Ji-yang¹*

1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changchun 130012, P. R. China;
2. School of Chemistry Engineering & Material, Dalian Institute of Light Industry, Dalian 116034, P. R. China;
3. Geriatric Ward, First Hospital of Jilin University, Changchun 130021, P. R. China

Received:2008-12-12 Revised:2009-03-09 Online:2009-07-25 Published:2009-10-16
Contact: FU Jun. E-mail: fjjilin@yahoo.com.cn; LI Ji-yang. E-mail: lijiyang@jlu.edu.cn
Supported by:
Supported by the National Natural Science Foundation of China(No.20871051) and the Scientific and Technological Planning Project of Jilin Province, China(No.20080504).

Abstract

Abstract:

With N,N'-dimethylpiperazine(DMPIP) as the structure-directing agent, a zinc phosphate [Zn₆(H₂O)·P₅O₂₀][C₅N₂H₁₄][C₆H₁₆N₂]_0.5·3H₂O(1) with a novel three-dimensional(3D) open-framework architecture was hydrothermally synthesized. Its structure was determined by single-crystal X-ray diffraction analysis and further characterized by ICP, NMR, and TG analyses. Compound 1 crystallized in the triclinic space group P1(No.2) with a=0.9984(2) nm, b=1.2354(3) nm, c=1.2384(3) nm, α=88.32(3)°, β=74.57(3)°, γ=75.81(3)° and Z=2. The alternation arrrangement of tetrahedral Zn units[ZnO₄ and ZnO₃(H₂O)] and PO₄ units forms an anionic 3D open framework containing intersecting 16-, 10- and 8-ring channels. Water molecules, diprotonated DMPIP, and diprotonated N-methyl-piperazine(MPIP) decomposed from DMPIP, are located in the channels and interact with the host framework via H-bonds. Compound 1 transforms to another new phase(compound 2) upon calcination at 200―350 °C with the removal of the water coordinated to Zn atoms in the lattice. The phase transformation of compound 2 was further studied.

SONG Yu, DONG Zhao-jun, WANG Yong-wei, FU Jun* and LI Ji-yang*. Synthesis, Characterization and Phase Transformation of 3D Open-framework Zinc Phosphate [Zn₆(H₂O)P₅O₂₀][C₅N₂H₁₄][C₆H₁₆N₂]_0.5·3H₂O[J]. Chemical Research in Chinese Universities, 2009, 25(4): 407-411.

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Synthesis, Characterization and Phase Transformation of 3D Open-framework Zinc Phosphate [Zn₆(H₂O)P₅O₂₀][C₅N₂H₁₄][C₆H₁₆N₂]_0.5·3H₂O

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