Homogeneous CO Hydrogenation: Ligand Effects on the Lewis Acid ...
Homogeneous CO Hydrogenation: Ligand Effects on the Lewis Acid ...
Homogeneous CO Hydrogenation: Ligand Effects on the Lewis Acid ...
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NMR studies, but <strong>the</strong> undesired product was not fur<strong>the</strong>r purified. 1 H NMR (C 6D 6, 500 MHz): δ<br />
1.01-1.09 (m, 3H), 1.4-1.6 (m, 12H), 1.6-1.8 (m, 12H), 1.9-2.1 (m, 12H), 2.4-2.6 (m, 3H), 2.94<br />
(m, 1H), 3.09 (m, 1H), 5.85 (br m, 1H), 6.9-7.1 (m, 12H), 7.75 (dt, J = 9.1, 17.9 Hz, 6H), 7.88 (t,<br />
J = 7.9 Hz, 2H). 31 P{ 1 H} NMR (C 6D 6, 202 MHz): δ 12.6 (d, 2 J PP = 124.8 Hz, 1P), 39.9 (d, 2 J PP =<br />
124.8 Hz, 1P). 13 C{ 1 H} NMR (C 6D 6, 125 MHz): δ 22.2 (br, Ph 2PCH 2CH 2B(C 8H 14)), 23.78, 24.33,<br />
24.8 (br), 27.61 (d, 1 J PC = 27.2 Hz, Ph 2PCH 2CH 2B(C 8H 14)), 31.38 (d, 1 J PC = 31.3 Hz,<br />
Ph 2PCH 2CH 2CH(OBR 2)Re), 31.93, 33.78, 33.84, 34.41, 34.64, 45.87 (dd, J PC = 14.4, 5.3 Hz,<br />
Ph 2PCH 2CH 2CH(OBR 2)Re), 76.66 (dd, J PC = 7.0, 2.2 Hz, Ph 2PCH 2CH 2CH(OBR 2)Re), 128.81 (d,<br />
3 JPC = 9.3 Hz, m-Ph), 128.90 (d, 3 J PC = 9.3 Hz, m-Ph), 129.08 (d, 3 J PC = 9.7 Hz, m-Ph), 129.12 (d,<br />
3 JPC = 9.5 Hz, m-Ph), 129.93 (d, 4 J PC = 1.8 Hz, p-Ph), 130.17 (d, 4 J PC = 1.9 Hz, p-Ph), 130.25 (d,<br />
4 JPC = 1.9 Hz, p-Ph), 130.32 (d, 4 J PC = 2 Hz, p-Ph), 132.07 (d, 2 J PC = 10.5 Hz, o-Ph), 132.67 (d,<br />
2 JPC = 11.0 Hz, o-Ph), 132.68 (d, 2 J PC = 10.2 Hz, o-Ph), 133.99 (d, 2 J PC = 9.9 Hz, o-Ph), 137.37 (d,<br />
1 JPC = 43.6 Hz, ipso-Ph), 137.71 (d, 1 J PC = 45.7 Hz, ipso-Ph), 137.90 (d, 1 J PC = 44.5 Hz, ipso-Ph),<br />
139.54 (d, 1 J PC = 42.2 Hz, ipso-Ph), 195.17 (t, 2 J PC = 9.3 Hz, Re-<str<strong>on</strong>g>CO</str<strong>on</strong>g>), 198.65 (t, 2 J PC = 5.7 Hz,<br />
Re-<str<strong>on</strong>g>CO</str<strong>on</strong>g>), 199.12 (t, 2 J PC = 9.4 Hz, Re-<str<strong>on</strong>g>CO</str<strong>on</strong>g>). 11 B{ 1 H} NMR (C 6D 6, 160 MHz): δ 54.9, 88.0.<br />
Assignments were made using 1 H- 31 P gHMBC, 1 H- 13 C gHMQC, 1 H- 13 C gHMBC, and 1 H- 1 H<br />
g<str<strong>on</strong>g>CO</str<strong>on</strong>g>SY 2-D NMR experiments.<br />
S74