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

producing an orange oil with yellow solution above it. The solvent was decanted from the oil,
and the oil was washed with 3 x 5 mL pentane, and then dried under vacuum, giving 700 mg
(80%) crude [1-E 2-Mn][BF 4], ~90% pure by NMR spectroscopy. Further purification was
achieved by dissolving the solids in 7 mL toluene, and letting the solution stand overnight, which
yielded analytically pure yellow polycrystalline [1-E 2-Mn][BF 4] (460 mg, 53%). 1 H NMR
(THF-d 8, 300 MHz): δ 0.54 (m, 4H), 0.70 (4H), 1.23 (m, 4H), 1.48 (16H), 1.68 (m, 4H), 2.74 (m,
4H), 7.52 (m, 12H), 7.71 (m, 8H). 31 P{ 1 H} NMR (THF-d 8, 121 MHz): δ 51.5. 13 C{ 1 H} NMR
(CD 2Cl 2, 126 MHz): δ 20.83 (br, Ph 2PCH 2CH 2B(C 8H 14)), 23.51 (Ph 2PCH 2CH 2B(C 8H 14)), 28.14
(dd, J PC = 2.8, 28.6 Hz, Ph 2PCH 2CH 2B(C 8H 14)), 31.91 (br, Ph 2PCH 2CH 2B(C 8H 14)), 33.71
(Ph 2PCH 2CH 2B(C 8H 14)), 130.30 (m, m-Ph), 131.91 (dd, J PC 1.7, 47.6 Hz, ipso-Ph), 132.25 (m, o-
Ph), 132.54 (p-Ph), 212.18 (br, <strong>CO</strong>). 11 B NMR (CD 2Cl 2, 160 MHz): δ -1.2 (BF 4), 86.9 (br, -
B(C 8H 14)). 19 F NMR (CD 2Cl 2, 282 MHz): δ -152.5 (br). IR (THF): ν <strong>CO</strong> 1995 cm -1 .
Figure S30. 1 H NMR.
S30