The present invention provides process for preparing crystalline Pemetrexed dipotassium (I) Form-SP9characterized by X-ray powder diffraction pattern comprising at least 5 characteristic 2θ° peaks selected from the XRPD peak set of 5.0, 12.5, 17.2, 20.8, 22.4, 25.7, 26.9 and 27.9±0.2 2θ°. The invention also provides process for preparing its pharmaceutical composition thereof, which may be useful for anti-cancer treatment.