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

Figure S33. 11 B NMR.
Synthesis of mer,trans-(Ph 2PCH 2CHCH 2) 2Re(<strong>CO</strong>) 3Br.
A 60 mL Teflon-stoppered pressure tube was charged with 741 mg (1.82 mmol) Re(<strong>CO</strong>) 5Br, 825
mg (3.64 mmol, 2 equiv) Ph 2PCH 2CHCH 2, 15 mL toluene, and a stirbar. The tube was sealed,
removed from the glovebox, and heated to 120 °C. After 5 days, the reaction was cooled to
ambient temperature, degassed to remove liberated <strong>CO</strong>, and brought into a glovebox. All
solvents were removed under vacuum, the solids were washed with 25 mL pentane, and collected
on a frit. The white powder was dried, giving 1.28 g (1.59 mmol, 88%) pure mer,trans-
(Ph 2PCH 2CHCH 2) 2Re(<strong>CO</strong>) 3Br. 1 H NMR (CD 2Cl 2, 300 MHz): δ 3.62 (m, 4H, Ph 2PCH 2CHCH 2),
4.85 (dd, 4 J PH=1.8 Hz, J HH=17.3 Hz, 2H, Ph 2PCH 2CHCH 2), 4.98 (dd, 4 J PH=1.7 Hz, J HH=10.3 Hz,
2H, Ph 2PCH 2CHCH 2), 5.63 (m, 2H, Ph 2PCH 2CHCH 2), 7.40-7.48 (m, 12H, Ph 2PCH 2CHCH 2),
7.56-7.65 (m, 8H, Ph 2PCH 2CHCH 2). 31 P{ 1 H} NMR (CD 2Cl 2, 121 MHz): δ -0.9 (s). 13 C{ 1 H}
S32