Homogeneous CO Hydrogenation: Ligand Effects on the Lewis Acid ...

Figure S59. 13 C{ 1 H} NMR.
Synthesis of [(Ph 2P(CH 2) 3B(C 8H 14))Re(<strong>CO</strong>) 5][OTf] ([1-P 1][OTf]).
A 20 mL glass pressure vessel fitted with a Teflon valve was charged with 0.710 g (1.01 mmol)
[Ph 2PCH 2CHCH 2Re(<strong>CO</strong>) 5][OTf], 0.124 g (1.01 mmol) 9-BBN, 5 mL CH 2Cl 2, and a magnetic
stirbar. The vessel was sealed, removed from the box and heated to 60 °C for 12 hours. After this
time the clear colorless solution was cooled to ambient temperature, brought back into the
glovebox, and filtered. Removal of solvents from the filtrate yielded 0.747 g (0.91 mmol, 90%)
of a white powder, which was ~95% pure by 1 H NMR, with the other 5% being unreacted
starting material. Treatment under the same conditions with slightly more 9-BBN gave
spectroscopically pure [1-P 1][OTf] after washing with pentane. Analytically pure material was
obtained by crystallization from a THF solution layered (1:1) with pentane at -35 °C. 1 H NMR
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