Three polyoxomolybdate compounds, namely {[M II (HL) 2 ] 2 (Mo 8 O 26 )} n (M = Co (1), Ni (2), Zn (3)) (HL, 3-(2-pyridyl)pyrazole), were designed and synthesized under the hydrothermal conditions and characterized by elemental analysis, IR spectroscopy, and TGA. Single-crystal X-ray diffraction analysis results reveal that compounds 1-3 own the isostructural chain structure consisting of the -[Mo 8 O 26 ] 4 anions, which are linked by M(HL) 2 2+ units via the terminal oxygen atoms. TGA curves show that the organic ligands separate from the related compounds above ca. 673 K. polyoxomolybdate, 3-(2-pyridyl)pyrazole, polyoxomolybdate, cobalt, nickel, zinc