Preparation and crystal structure of [Mo{S2P(OMe)2}3] and an improved route to [MoCl3(thf)3]

Abstract

The complex [MoCl₃(thf)₃](thf = tetrahydrofuran) is prepared in high yield by the tin reduction of [MoCl₄(thf)₂] in thf. It reacts with [NH₄][S₂P(OMe)₂] in dry methanol to give [Mo{S₂P(OMe)₂}₃] which crystallizes in the space group C2/c with a= 14.342(5), b= 11.239(5), c= 12.945(4)Å, β= 97.12(1)° and Z= 4. 2 453 Reflections gave R= 0.039. The molybdenum is pseudo-octahedral and the complex has overall C₂ symmetry. The Mo–S average distance is 2.507(2)Å.