A tri-thiocyanate molybdenum (Ⅴ) complex containing pyridine has been prepared by one step process; namely, the solvent extraction of molybdenum (Ⅴ)-thiocyanate complex into organic solvents followed by precipitation of the compound by addition of pyridine to the extract. It is concluded that the compound has a definite composition regardless of the various mole ratios of molybdenum to thiocyanate ion employed in the preparation. The use of hydrazine as the reducing agent eliminates the necessity of working under inert atmosphere and of further purification of the product. Molybdenum (Ⅴ)-thiocyanate (1:3) complex can be quantitatively and selectively extracted with slightly polar organic solvents such as ethyl acetate, and the pyridine complex is quantitatively obtained due to the insolubility of the compound in them. The oxidation state of molybdenum in the compound is + 5 and the formula appears to be