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A Novel Mixed-valence and Capped-keggin Structural Polyoxometal Complex: {[Co(dien)]4- [(PO4)MoVs(WVI0.56 noVI0.44)4033(OH)3]}.nH2O (n ≈ 1)
作者姓名:HU Zhi-Biao  CHEN Wu-Hua  MI Jin-Xiao
作者单位:[1]College of Chemistry and Material Science,Longyan University, Longyan, Fujian 364000, China [2]College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China [3]Department of Materials Science and Engineering,College of Materials, Xiamen University, Xiamen 361005, China
基金项目:This work was supported by the Foundation of Education Department of Fujia Province (Nos. JA 11245 and JB 12199), and the National Natural Science Foundation of China (No. 40972035)
摘    要:A novel inorganic-organic hybrid compound, {Co(dien)]40aO4)MoV8(wV10.56MoV10.44)4- O33(OH)3]}'nH20 (1, n = 1, dien = diethylenetriamine), has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the triclinic system with a = 11.927(2), b = 13.328(3), c = 19.306(4)A, a = 93.76(3), β = 94.14(3), γ = 109.99(3)°, V= 2863.2(12) A3, space group P1 and Z = 2 at 173 K. The final full-matrix least-squares refinement converged to R = 0.049 for 9621 observed reflections with 1 〉 2σ(I) and wR = 0.139 for all data (9871) and S = 1.073. Crystal structure analysis shows that 1 contains a kind of the first reported mixed-valence and molybdenum-tungsten mixed-distributed e-Keggin structural polyanion capped by four Co(dien) fragments with the main group element P occupying the center site. These results were further confirmed by energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Thermogravimetry (TG) and X-ray photoelectron spectroscopy (XPS) analyses.

关 键 词:Keggin型结构  混合价  二烯  MOVS  X射线光电子能谱  傅里叶变换红外光谱  单晶X-射线衍射  X-射线粉末衍射

A Novel Mixed-valence and Capped-keggin Structural Polyoxometal Complex: {[Co(dien)]4- [(PO4)MoVs(WVI0.56 noVI0.44)4033(OH)3]}.nH2O (n ≈ 1)
HU Zhi-Biao,CHEN Wu-Hua,MI Jin-Xiao.A Novel Mixed-valence and Capped-keggin Structural Polyoxometal Complex: {[Co(dien)]4- [(PO4)MoVs(WVI0.56 noVI0.44)4033(OH)3]}.nH2O (n ≈ 1)[J].Chinese Journal of Structural Chemistry,2013(11):1653-1662.
Abstract:inorganic-organic hybrid compound, e-Keggin-structure,hydrothermal synthesis, mixed-valence, mixed-distribution
Keywords:inorganic-organic hybrid compound  e-Keggin-structure  hydrothermal synthesis  mixed-valence  mixed-distribution
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