Hydrothermal Syntheses and Structural Characterizations of Two ML-Containing Polyoxomolybdates: [CuⅡ

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Two new polyoxomolybdate compotnds, 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- andβ-[Mo8O26]4-. In complexes 1 and 2, the multi-dimensional frameworks are constructed 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) (A), β =100.57(3)°, V= 3401.6(12) (A)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) (A),β = 91.6180(10)°, V= 7119.0(11)(A)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)).
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