Multielement n.m.r. measurements (1H, 1H-{103Rh}, 13C, 13C-{103Rh}, and 103Rh) show that protonation of [Rh6(CO)13C]2- at low temperature gives [Rh6H(CO)13C]- which contains an edge-bridging hydride with the carbonyl distribution being very similar to that found in [Rh6(CO)13C]2- Warming this solution to < -20 °C results in complete CO- and H-migration over the Rh6 octahedron and at ≥ -20 °C there is formation of [Rh6H(CO)15C]- together with loss of hydrogen to give [Rh12(CO)24(C)2]2- which has been spectroscopically characterised. Multielement n.m.r. studies on products resulting from the reaction of [Rh6(CO)13C]2- (1 mol equiv.) with diphosphines Ph2P(CH2)nPPh2 [0.5 mol equiv.; n = 1,2 (dppe), 3, or 4] or Ph2AsCH2CH2AsPh2 suggest that they all have similar structures and an X-ray crystallographic analysis of the dppe derivative shows it to be [Rh6(CO)11C(μ-dppe)]2-.

Derivatives of [Rh6(CO)13C]2-: Solution structure of [Rh6H(CO)13C]- from nuclear magnetic resonance measurements and the X-ray crystal structure of [Rh6(CO)11C(μ-Ph2PCH2CH 2PPh2)]2-

Bordoni S.;
1988

Abstract

Multielement n.m.r. measurements (1H, 1H-{103Rh}, 13C, 13C-{103Rh}, and 103Rh) show that protonation of [Rh6(CO)13C]2- at low temperature gives [Rh6H(CO)13C]- which contains an edge-bridging hydride with the carbonyl distribution being very similar to that found in [Rh6(CO)13C]2- Warming this solution to < -20 °C results in complete CO- and H-migration over the Rh6 octahedron and at ≥ -20 °C there is formation of [Rh6H(CO)15C]- together with loss of hydrogen to give [Rh12(CO)24(C)2]2- which has been spectroscopically characterised. Multielement n.m.r. studies on products resulting from the reaction of [Rh6(CO)13C]2- (1 mol equiv.) with diphosphines Ph2P(CH2)nPPh2 [0.5 mol equiv.; n = 1,2 (dppe), 3, or 4] or Ph2AsCH2CH2AsPh2 suggest that they all have similar structures and an X-ray crystallographic analysis of the dppe derivative shows it to be [Rh6(CO)11C(μ-dppe)]2-.
1988
Bordoni S.; Heaton B.T.; Seregni C.; Strona L.; Goodfellow R.J.; Hursthouse M.B.; Thornton-Pett M.; Martinengo S.
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11585/902124
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