Abstract: | The reaction of Mo2(O3CCF3)4 with (CH3)3SiI and PPh3 gave the title complex [Mo3(O2CCF3)2I4]-(HPPh3)2 which was characterized by X-ray crystallography. Crystal data for [Mo2(O2CCF3)2I4](HPPh3)2: space group $ {rm P}bar 1 $, a = 10.953(4) Å, b = 12.784(3) Å, c = 19.829(4) Å, α = 100.68(2)°, β = 91.16(2)°, γ = 112.98(2)°, V = 2498.6(10) Å3, Z = 2, with final residuals R = 0.0887 and Rw = 0.0965. There are two independent molecules in each asymmetric unit. The molybdenum, oxygen, and fluoride atoms in one of the two independent molecules are disordered, such that the primary set is 53% occupied, and the secondary set 47%. |