A Fe(Ⅲ) compex with OPPh3,[Fe(OPPh3)4Cl2][FeCl4],has been synthesized and characterized by elemental analysis and IRspectrum.The crystal structure of the title complex has been determined by simgle crystal X-ray diffraction techmiques.The crystal belongs to monoclinic,space group P21/c.The cell parameters are :a=13.9323(13),b=27.5290(2),c=18.2095(17),β= 104.460(2)o,V=6762.9(11)3,Z=4,DC=1.412 g/cm3,μ=0.809 mm-1,F(000)=2952,R1=0.0796 and ωR2=0.1752for 10419 observed reflections(I>2σ(I)) out of 12343 unique data.In the cations[Fe(OPPh3)4Cl2]+,the Fe(Ⅲ) center adopts a slight distoned octahedral geometry comprised oftwo OPPh3 oxygen atoms and two Cl-ions at the equatorial positions,and two OPPh3 oxygenatoms at the axial positions.In the anions[FeCl4]-,The Fe(Ⅲ) ion has a sIightly distortedtetrahedI.al coordination geometry and is bonded to four Cl-ions.