Two new polyoxomolybdate compounds,namely CuII2（HL）3]2[Mo8O26]·（H2O）4（1） and [NiII（HL）3]2（Mo8O26）·（H2O）3（2）（HL = 3-（2-pyridyl）pyrazole）,were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one β-Mo8O264-cluster and a Cu2 dimer which is built from two Cu（II） ions linked by three 3-（2-pyridyl）pyrazole ligands.Compound 2 is generated by two kinds of polyoxomolybdate clusters of α-[Mo8O26]4-and β-[Mo8O26]4-.In complexes 1 and 2,the multi-dimensional frameworks are con-structed with the help of hydrogen-bonding links between the terminaloxygen atoms of [Mo8O26]4-,water molecules,and 3-（2-pyridyl）pyrazole ligands.Crystal data of 1：C24H25Cu2Mo4N9O15,Mr = 1190.37,monoclinic,space group P21/c,a = 10.850（2）,b = 18.510（4）,c = 17.230（3） ,β = 100.57（3）°,V = 3401.6（12） 3,Z = 4,Dc = 2.324 g/cm3,F（000） = 2312,μ = 2.742 mm-1,R = 0.0302 and wR = 0.0775（Ⅰ 〉 2σ（Ⅰ））;Crystal data for 2：C48H48Mo8N18Ni2O29,Mr = 2225.98,monoclinic,space group P21/n,a = 20.799（2）,b = 14.7970（13）,c = 23.141（2） ,β = 91.6180（10）°,V = 7119.0（11） 3,Z = 4,Dc = 2.077 g/cm3,F（000） = 4344,μ = 1.968 mm-1,R = 0.0309 and wR = 0.0696（Ⅰ〉 2σ（Ⅰ））.
