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

Figure S15. 11 B{ 1 H} NMR (broad underlying signal is borosilicate in probe construction).
Synthesis of Ph 2PCH 2B(C 8H 14):
A 20 mL scintillation vial was charged with 615 mg (1.5 mmol) Ph 2PCH 2B(C 8H 14)pyridine, 18
mL Et 2O, and a stirbar. With stirring, 195 μL BF 3OEt 2 was added dropwise by syringe. As the
BF 3OEt 2 was added, fluffy white precipitates formed, eventually giving a thick white slurry.
After stirring for 20 minutes, the solids were collected on a frit, and washed with 3 x 5 mL Et 2O,
and 4 x 4 mL CH 2Cl 2, yielding 369 mg (1.15 mmol, 77%) Ph 2PCH 2B(C 8H 14). This material was
quite insoluble, precluding full characterization, but yielded clean metallation reactions. Anal.
Calcd. for C 21H 26BP: C, 78.77; H, 8.18. Found: C, 78.52; H, 8.45.
Synthesis of mer,trans-(Ph 2PCH 2B(C 8H 14)) 2Re(<strong>CO</strong>) 3Br.
A pressure vessel equipped with a Teflon valve was charged with 1.33 g (4.16 mmol, 2 equiv)
Ph 2PCH 2B(C 8H 14), 0.85 g (2.08 mmol, 1 equiv) Re(<strong>CO</strong>) 5Br, 30 mL toluene, and a stirbar. The
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