A new dinuclear dysprosium (III) complex has been synthesized with the formula [DyIII2(valpico)2(NO3)4].4CH3CN, where (Hvalpico = 2-methoxy-6-((pyridin-2-ylmethylimino)methyl)phenol) in acetonitrile medium. The single crystals started to form from acetonitrile solution after 5 minutes of reaction and completed within 10 minutes at room temperature. The crystals were of good quality for single crystal X-ray diffraction measurement. The structural and magnetic properties of the dinuclear (Dy2) phenoxo-bridged motif are explored. The magnetic property of the Dy-dimer complex show single molecular magnetic (SMM) behaviour.