A new pseudo Keggin-type bicapped compound（Et3N）0.5（en）2[SiMo12O40（VO）2]·4H2O（Et3N=triethylamine,en=ethylenediamine） has been hydrothermally synthesized and characterized by IR,elemental analysis,TG and X-ray crystallography.The title compound crystallizes in monoclinic,space group P21/n with a=17.576（2）,b=13.535（1）,c=21.587（2）,β=103.790（10）°,V=4987.3（8）3,Z=4,Dc=2.925 Mg/m3,Mr=2196.12,F（000）=4148,μ=3.400 mm–1,R=0.0379 and wR=0.1219.The most remarkable structural feature of the compound is that the clusters represent bicapped pseudo-Keggin structure and are linked one by one through V-O-V bonds forming an infinite 1D chain. Furthermore, such chains are interconnected in a cross-like arrangement through multiform hydrogen bonds to yield a 3D supramolecular network.
A new compound has been synthesized under hydrothermal conditions and characterized by IR, elemental analysis, XPS and single-crystal X-ray diffraction analysis. The title compound [Mn（en）3]2en0.5[HV8VV8IVO38（CI）]·4.5H2O crystallizes in monoclinic, space group C2/c, with a = 17.016（4）, b = 18.858（4）, c = 18.872（4） A, β = 93.667（4）°, V = 6043（2）A3, Z = 4, Dc = 2.242 g/cm3, Mr = 2040.12, F（000） = 4020,μ = 2.895 mm-1, Rint = 0.0921, R = 0.0649 and wR = 0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38（CI）]4- cage, two [Mn（en）3]2^2＋ cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H...N, O-H...O, N-H...O and C-H...O hydrogen bonds link the molecules together to form a three-dimensional structure.
