[Rh(P(4-biphenyl)3)2(CO)Cl] (1)
1H NMR (600 MHz, CD2Cl2) δ 7.90-7.95 (m, 12H), 7.72 (d, JHH = 8.0, 12H), 7.67 (d, JHH = 7.3, 12H), 7.47 (t, JHH = 7.3, 12H), 7.39 (t, JHH = 7.3, 6H). 13C{1H} NMR (151 MHz, CD2Cl2) δ 187.4 (dt, JRhC = 75, JPC = 16) 143.5 (s), 140.6 (s), 135.7 (t, JPC = 7), 132.3 (t, JPC = 23), 129.4 (s), 128.5 (s), 127.7 (s), 127.4 (t, JPC = 5). 31P{1H} NMR (243 MHz, CD2Cl2) δ 27.8 (JRhP = 126). Anal. Calcd for C73H54ClOP2Rh (1147.51 gmol-1): C, 76.41; H, 4.74. Found: C, 76.37; H, 4.82. IR (CH2Cl2, cm-1): ν(CO) 1978. The solid-state structure of this compound has been deposited with the Cambridge Crystallographic Data Centre under CCDC 1498191.
[Ir(P(4-biphenyl)3)2(CO)Cl] (2)
1H NMR (400 MHz, CD2Cl2) δ 7.94 (br d, JHH = 7.8, 12H), 7.67-7.82 (m, 24H), 7.37-7.55 (m, 18H). 13C{1H} NMR (101 MHz, CD2Cl2) δ 172.2 (t, JPC = 11), 143.7 (s), 140.5 (s), 135.9 (t, JPC = 6), 131.6 (t, JPC = 27), 129.5 (s), 128.5 (s), 127.8 (s), 127.4 (t, JPC = 5). 31P{1H} NMR (122 MHz, CD2Cl2) δ 22.8. Anal. Calcd for C73H54ClOP2Ir (1236.82 gmol-1): C, 70.89; H, 4.40. Found: C, 71.01; H, 4.60. IR (CH2Cl2, cm-1): ν(CO) 1965. The solid-state structure of this compound has been deposited with the Cambridge Crystallographic Data Centre under CCDC 1498192.