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An unreported inorganic-organic hybrid compound [Cu(phen)(H 2 O) 2 (Mo 3 O 10 )] ( 1 ) was hydrothermally synthesized and characterized with elemental analysis, IR spectroscopy, thermal analysis, luminescent spectroscopy, magnetic measurement. The crystal structure was determined with X-ray single-crystal diffraction. Compound 1 has a 1-D chain structure constructed by {Mo 3 O 10 } 2 − units via edge-sharing and [Cu(phen)(H 2 O) 2 ] 2 + fragments grafting the chain from two sides via the coordination of the terminal oxygen atom of the MoO 6 octahedra to Cu 2 + ion. The coordination of phen to Cu 2 + ion increases the molecular rigidity so that an emission peak at 500 nm was observed and assigned to the phosphorescent n–π* and π–π* transition from ligand-centered triple state. In compound 1 Cu(II) exhibits an antiferromagnetic exchange. [ABSTRACT FROM AUTHOR]