2.3.5. [(benzene)Ru(Se=PPh2Py)Cl]PF6 (5). Color: Orange precipitate; Yield: 53 mg (75%); IR (KBr, cm-1):
3431(b), 3133(w), 1637(m), 1587(m), 1479(w), 1436(m), 1400(vs), 1314(w), 1286(m), 1186(w), 1141(m),
1096(s), 1000(w), 836(vs), 771(m), 754(m), 716(m), 688(m), 616(w), 557(vs), 510(s); 1H NMR (400 MHz,
CD3CN): δ = 9.10 (d, 1H, HJJ = 3.25, py ring), 8.20 (t, 1H, py ring), 7.92 (d, 2H, HJJ = 2.00, ph ring), 7.80-
7.75 (m, 5H, ph ring), 7.63-7.57 (m, 4H, ph ring), 7.41 (t, 1H, py ring), 5.60 (s, 6H, benzene ring); 13C NMR
(400 MHz, CD3CN): δ = 162.54, 152.20, 136.26, 135.42, 132.67, 131.87, 130.42, 128.62, 126.71, 85.90; ESI-
MS: 557.89 [M+] peak, 522.90 [M+-Cl] peak, 214.90 [(ben)RuCl+] peak; UV-Vis {CH3CN, λmax nm (ε, M-1
cm-1)}: 228(7300), 324(700); Anal. Calc. for C23H20NSeRuClPF6 (701.83) (%): C, 39.36; H, 2.87; N, 2.00.
Found (%): C, 39.53; H, 2.99; N, 2.17.
2.3.6. [(p-cymene)Ru(Se=PPh2Py)Cl]PF6 (6). Color: Orange precipitate; Yield: 59 mg (78%); IR (KBr, cm-
1): 3434(m), 3129(m), 2970(m), 1631(m), 1584(w), 1456(m), 1439(s), 1400(s), 1320(m), 1280(w), 1186(w),
1133(m), 1100(s), 1054(m), 1028(w), 838(vs), 779(w), 756(w), 693(m), 557(vs), 518(s); 1H NMR (400 MHz,
CD3CN): δ = 9.15 (d, 1H, HJJ = 3.25, py ring), 8.21 (t, 1H, py ring), 7.80 (d, 2H, HJJ = 2.25, ph ring), 7.76-
7.71 (m, 5H, ph ring), 7.61-7.55 (m, 4H, ph ring), 7.42 (t, 1H, py ring), 5.97 (d, 2H, HJJ = 3.75, ph ring), 5.72
(d, 2H, HJJ = 3.75, ph ring), 2.90 (sep, 1H, Ar(p- Cy)), 2.51 (s, 3H, CH3), 2.01 (s, 3H, CH3Ar(p- Cy)), 1.34 (d, 6H,
HJJ = 4.00, CH3Ar(p- Cy)), 1.22 (d, 6H, HJJ = 4.25, CH3Ar(p- Cy)); 13C NMR (400 MHz, CD3CN): δ = 160.26,
153.42, 138.21, 135.71, 132.90, 132.02, 130.65, 129.47, 128.82, 102.73, 90.82, 85.34, 82.51, 31.26, 21.12,
16.54; ESI-MS: 613.93 [M+] peak, 578.98 [M+-Cl] peak, 236.08 [(p-cy)RuCl+] peak; UV-Vis {CH3CN, λmax
nm (ε, M-1 cm-1)}: 227(5800), 330(400); Anal. Calc. for C27H28NSeRuClPF6 (757.94) (%): C, 42.79; H, 3.72;
N, 1.85. Found (%): C, 42.98; H, 3.86; N, 1.96.
2.3.7. [Cp*Rh(Se=PPh2Py)Cl]PF6 (7). Color: Red orange precipitate; Yield: 61 mg (81%); IR (KBr, cm-1):
3436(b), 2926(w), 1636(m), 1439(m), 1400(m), 1385(w), 1163(m), 1131(m), 1096(s), 1024(m), 998(w),
861(s), 841(vs), 781(w), 756(m), 716(w), 697(m), 556(vs), 513(s); 1H NMR (400 MHz, CD3CN): δ = 9.09 (d,
1H, HJJ = 3.25, py ring), 8.10 (t, 1H, py ring), 7.70 (d, 2H, HJJ = 2.00, ph ring), 7.86-7.74 (m, 5H, ph ring),
7.60-7.52 (m, 4H, ph ring), 7.37 (t, 1H, py ring), 1.42 (s, 15H, Cp* ring); 13C NMR (400 MHz, CD3CN): δ =
158.24, 154.63, 138.95, 134.69, 132.98, 132.25, 130.93, 129.54, 127.02, 97.89, 7.65; ESI-MS: 568.02 [M+]
peak, 536.01 [M+-Se] peak, 236.09 [Cp*RhCl+] peak; UV-Vis {CH3CN, λmax nm (ε, M-1 cm-1)}: 249(4500),
414(400); Anal. Calc. for C27H30NSeRhClPF6 (761.79) (%): C, 42.57; H, 3.97; N, 1.84. Found (%): C, 42.76;
H, 4.08; N, 1.93.
2.3.8. [Cp*Ir(Se=PPh2Py)Cl]PF6 (8). Color: Yellow precipitate; Yield: 67 mg (65%); IR (KBr, cm-1):
3436(b), 2924(w), 1624(w), 1455(m), 1439(m), 1384(m), 1133(w), 1099(s), 1033(m), 998(w), 862(s),
841(vs), 782(m), 755(m), 731(w), 715(w), 691(m), 556(s), 512(s); 1H NMR (400 MHz, CD3CN): δ = 9.03 (d,
1H, HJJ = 3.25, py ring), 8.15 (t, 1H, py ring), 7.88 (d, 2H, HJJ = 2.50, ph ring), 7.79-7.60 (m, 5H, ph ring),
7.59-7.55 (m, 4H, ph ring), 7.43 (t, 1H, py ring), 1.43 (s, 15H, Cp* ring); 13C NMR (400 MHz, CD3CN): δ =
158.24, 153.92, 138.86, 135.23, 132.76, 132.89, 131.64, 129.72, 126.61, 97.72, 8.29; ESI-MS: 706.04 [M+]
peak, 626.08 [M+-Se] peak, 363.07 [Cp*IrCl+] peak; UV-Vis {CH3CN, λmax nm (ε, M-1 cm-1)}: 226(7600),
307(1300), 386(400); Anal. Calc. for C27H30NSeIrClPF6 (851.10) (%): C, 38.10; H, 3.55; N, 1.65. Found (%):
C, 38.26; H, 3.62; N, 1.78.
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