| Due to their interesting topologies and potential applications as catalyst,sorption, molectroics and medication etc, the research on polyoxometalates hasbeen one of the important fields of inorganic chemistry. Because Mo8 andKeggin-structure clusters, which possess steady structure, can be synthesizedexpediently, the research on syntheses novel polyoxometalates containingorganic molecules and/or transition metal coordination ions, namely,inorganic-organic hybrid materials based on the polyoxometalates is necessary.Additionally, porous-solid materials with regular pores can be applied onsorption, catalyst, acting as carrier and ion exchange etc, and are notedextensively.In this paper, five compounds were synthesized by mild-temperaturehydrothermal technique: two Mo8 clusters, two Keggin-structure clusters andone P-V-O micropores material compound. All those compounds werecharacterized by X-ray single crystal diffraction, elemental analyses, IR spectra,X-ray photoelectron spectra and TGA.1. Mo8 clustersTwo Mo8 clusters have been synthesized by hydrothermal techniques.(1) Compound [Cu(phen)2]2[{Cu(phen)}2{Mo8O26}]·H2O 1Compound 1 was characterized by X-ray single crystal diffraction, elementalanalyses, IR spectra, X-ray photoelectron spectra and TGA. Compound 1crystallize as crystal system monoclinic, space group C2/c. The parameters ofunit cell is a = 33.146(7) ?, b = 16.420(3) ?, c = 16.253(3) ?, α = 90.00o, β =119.11(3)o , γ = 90.00o 。 Compound 1 consist of cluster anion[{CuI(phen)}2{β-Mo8O26}]2-, coordination cation [CuI(phen)2]+ and one watermolecule.(2) Compound [Cu(en)2]2[Mo8O26] 2Compound 2 was characterized by X-ray single crystal diffraction,elemental analyses, IR spectra, X-ray photoelectron spectra and TGA.Compound 2 crystallize as crystal system orthorhombic, space group Pbca. Theparameters of unit cell is a = 13.5667(5) ?, b = 15.6149(8) ?, c = 16.7807(7)?, α = 90.00o, β = 90.00o, γ = 90.00o。The cluster unit is γ-[Mo8O26]4-, theterminal oxygen atoms bond to the CuII, which also coordinate with enmolecules, and link the cluster units to form 2-D layer.2. Keggin-structure compounds(1) compound (C2N2H9)2[PMoV5MoVI7SbIII2O40] ·2H2O 3Compound 3 was characterized by X-ray single crystal diffraction, elemental analyses, IRspectra, X-ray photoelectron spectra and TGA. Compound 3 crystallize as crystal systemtriclinic, space group P-1. The parameters of unit cell is a = 9.963(2) ?, b = 10.069(2) ?, c =10.731(2) ?, α = 81.96(3)o, β = 67.18(3)o, γ = 86.81(3)o。Compound 3 is the firstexample of Sb-Mo-O polyoxametalate bicapped by antimony α-Keggin structure.The antimony atoms bond weakly with the terminal oxygen atoms from adjacentcluster units to form 2-D layer. There exsit hydrogen-bonds between water and enmolecules, and link them to form 1-D supramolecular chain, which exsits betweenthe adjacent chains.(2) compound [Cu(en)2]3[VW12O40]·3H2O 4Compound 4 was characterized by X-ray single crystal diffraction, elementalanalyses, IR spectra, X-ray photoelectron spectra and TGA. Compound 4crystallize as crystal system trigonal, space group R-3c. The parameters of unitcell is a = 14.2420(4) ?, b = 14.2420(4) ?, c = 14.2420(4) ?, α =78.2930(10)o, β = 78.2930(10)o, γ =78.2930(10)o。Compound 4 is the firstexample of three-supported W-V-O polyoxometalate. The hydrogen-bondsexisting between the adjacent cluster units link each other to for 3-Dsupramolecular network.3. P-V-O micropore material compound(1) compound H(C2N2H8)2[{(OH)2V}(V2O3)4(PO4)4(HPO4)4]·3H2O 5Compound 5 was characterized by X-ray single crystal diffraction, elementalanalyses, IR spectra, X-ray photoelectron spectra and TGA. Compound 5crystallize as crystal system monoclinic, space group P21/c. The parameters ofunit cell is a = 14.364(5) ?, b = 10.127(7) ?, c = 23.269(9) ?, α = 90.00o, β =128.12o, γ =90.00o。Compound 5 is micropore material compound withcrossed channels.
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