Trimethylamine-N-oxide induced disproportionation of Re2(Co)10: synthesis and X-ray crystal structure of [fac-Re(CO)3(ONMe3)3] [ReO4]

An attempted synthesis of [Re(CO3) (μ-OH)]4,1, by reacting Re2(CO)10 with an excess of NMe3O in THF resulted instead in isolation of a disproportionation product, [fac-Re(CO)3(ONMe3)3][ReO4],2. The structure of2 was determined via X-ray crystallography: tri-clinic,P1¯,a=9.499(5),b=9.841(2),c=13.448(2)A,α=109.92(2),β=106.89(3), γ=93.15(4)°,Dcalc=2.22 g−3 andZ=2. Least-squares refinement based on 1606 observed (I>3σ(I)) reflections gave final values ofR=0.040 andRw=0.047. The cation is a distorted octahedron that exhibits several structural manifestations of steric crowding among the bulky NMe3O ligands.