32660-96-1Relevant articles and documents
Freeman, Mark J.,Miles, Anthony D.,Murray, Martin,Gui Orpen, A.,Stone, F. Gordon A.
, p. 1093 - 1098 (1984)
Synthesis, structure, and fluxional properties of (η5-C5Me5)(OC)2IrW(CO) 5. A compound with an Ir-W dative bond
Einstein, Frederick W. B.,Pomeroy, Roland K.,Rushman, Paul,Willis, Anthony C.
, p. 250 - 255 (2008/10/08)
The compound (η5-C5Me5)(OC)2IrW(CO) 5 (1) has been synthesized by the reaction of (η5-C5Me5)Ir(CO)2 and W(CO)5(THF) in hexane. The structure of 1 has been solved by conventional crystallographic techniques: space group P1 with a = 9.057 (2) A?, b = 9.560 (3) A?, c = 12.695 (2) A?, α = 71.83 (2)°, β = 83.07 (2)°, γ = 68.62 (2)°, Z = 2; RF = 0.027, RwF = 0.032 for 3426 reflections with I > 3σ(I) having 2θ 5-C5Me5)Ir(CO)2 acts as a donor ligand toward the W(CO)5 fragment via an unbridged Ir-W dative bond of length 3.0539 (11) A?. The 13C NMR spectrum of the compound in CD2Cl2/CH2Cl2 at -97°C was that expected from the solid-state structure. However, on warming the solution all the carbonyl resonances coalesced such that a single broad signal was observed at ambient temperature. A mechanism that involves an intermediate with bridging carbonyls is proposed to account for the carbonyl exchange. The donor-acceptor, metal-metal bond in (η5-C5Me5)(OC)2IrW(CO) 5 was weak since the compound reacted with the donor ligand L (L = CO, PPh3, or Os(CO)4(PMe3)) to yield (η5-C5Me5)Ir(CO)2 and W(CO)5L (in solution at room temperature over a period of ca. 90 min).