Trimethylamine-N-oxide induced disproportionation of Re2(CO)10: Synthesis and X-ray crystal structure of [fac-Re(CO)3(ONMe3)3] [ReO4] |
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Authors: | Sean D Christie Michael D Clerk Michael J Zaworotko |
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Institution: | (1) Department of Chemistry, Saint Mary's University, Halifax, B3H 3C3 Nova Scotia, Canada |
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Abstract: | An attempted synthesis of Re(CO3) ( -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)Å, =109.92(2), =106.89(3), =93.15(4)°,D
calc=2.22 g–3 andZ=2. Least-squares refinement based on 1606 observed (I>3 (I)) reflections gave final values ofR=0.040 andR
w=0.047. The cation is a distorted octahedron that exhibits several structural manifestations of steric crowding among the bulky NMe3O ligands. |
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