Abstract
The reaction of the bis(triflates) [Y-(CH 2) m -Y][Y = F 3CSO 3, m = 4, 6–9, 12, 14, 16 ( 1a–h)] with the carbonyl metalates M′[M(CO) 5] (M′ = Na, K; M = Mn, Re) affords the alkanediyl bridged metal complexes [(OC) 5M-(CH 2) m -M(CO) 5] [ m = 6–9, 12, 14, 16; M = Mn ( 2b–h) and m = 4, 6–9, 12, 14, 16; M = Re ( 3a–h)]. Starting with K[Mn(CO) 5] and the bis(triflates) 1d and 1e the diesters [H 3CO(O)C(CH 2) m C(O)OCH 3] [ m = 8, 9 ( 4d,e)] are obtained in a one-pot reaction. The unsaturated hydrocarbon bridged rhenium complexes trans-[Re]-(CH 2) 2-CH=CH-(CH 2) 2-[Re]( 6), cis-[Re]-(CH 2) 3-CH=CH-(CH 2) 3-[Re]( 8), and [Re]-(CH 2) p -CH 2-C≡C-CH 2-(CH 2) p -[Re] {[Re] = Re(CO) 5 p = 1, 3 ( 11, 12)} are formed by reaction of the bis(triflates) trans-Y-(CH 2) 2-CH=CH-(CH 2) 2-Y ( 5), cis-Y-(CH 2) 3-CH=CH-(CH 2) 3-Y ( 7), and Y-(CH 2) p -CH 2-C≡C-CH 2-(CH 2) p -Y [Y = F 3CSO 3, p = 1, 3 ( 9, 10)] with Na[Re(CO) 5] in THF. The structure of 8 was determined by an X-ray structural analysis. Crystal data for 8: space group P2 1/ n with a = 12.501(2), b = 6.592(2), c = 26.875(5)Å, β = 93.28(2)°, V = 2211.0(9) Å 3, Z = 4. The structure was refined to R = 0.039. wR = 0.090.
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