Paper
RSC Advances
1
Changjiang Scholars and Innovative Research Team in
University (IRT-13R06) and Program for DUT Innovative
Research Team (DUT2013TB07), and the Fundamental
Research Funds for the Central Universities (DUT15YQ101
and DUT13LK06) for nancial support of this work.
L-Np. Yield 81%. H NMR (400 MHz, CDCl3) d (ppm) 8.16–
8.14 (m, 2H), 8.12 (d, J ¼ 8.8 Hz, 1H), 8.05 (d, J ¼ 8.0 Hz, 1H),
7.98 (d, J ¼ 8.2 Hz, 1H), 7.89 (d, J ¼ 9.0 Hz, 1H), 7.62–7.59 (t, 1H),
7.57 (d, J ¼ 6.8 Hz, 1H), 7.53–7.49 (m, 3H). TOF-EI-MS (m/z):
261.0620 ([C17H11NS]+).
General procedure for the synthesis of complexes Ir-Cz, Ir-
DBF, Ir-Np. A mixture of IrCl3$3H2O (141 mg, 0.4 mmol), the
corresponding ligand (L-Cz, L-DBF, or L-Np, 1 mmol), 2-ethox-
yethanol (12 mL) and water (4 mL) was reuxed under nitrogen
for 24 h. Upon cooling to room temperature, water (30 mL) was
added into the reaction mixture. The precipitate was collected
by ltration and washed with water. The wet solid was
completely dried to give the yellow crude dichloro-bridged
dimer complex. Without further purication, this dimer was
added to a mixture of K2CO3 (1.06 g, 10 mmol), acetyl acetone
(excessive), and 2-ethoxyethanol (15 mL). Aer reuxing under
nitrogen for 24 h, the solution was cooled to room temperature
and water (100 mL) was added. The precipitate was ltered off
and washed with water. The crude product was puried by
column chromatography over silica using petroleum ether/ethyl
acetate (1 : 4) as eluent to yield the pure product of the desired
iridium complex.
References
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Ir-Cz. Yield 35%. MALDI-TOF-MS (m/z): 946.2756 ([C47H37
-
IrN4O2S2]+). 1H NMR (400 MHz, CDCl3) d (ppm) 8.31 (d, J ¼ 9.0
Hz, 2H), 8.24 (d, J ¼ 7.6 Hz, 2H), 7.75 (d, J ¼ 8.0 Hz, 2H), 7.60–
7.57 (m, 4H), 7.52 (d, J ¼ 9.0 Hz, 2H), 7.45–7.42 (t, 2H), 6.90–6.86
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C
47H37IrN4O2S2: C, 59.66; H, 3.94; N, 5.92; S, 6.78. Found: C,
59.61; H, 3.96; N, 5.89; S, 6.74.
Ir-DBF. Yield 45%. MALDI-TOF-MS (m/z): 892.0980 ([C43H27
-
IrN4O2S2]+). 1H NMR (400 MHz, CDCl3) d (ppm) 8.29 (d, J ¼ 9.0
Hz, 2H), 8.11 (d, J ¼ 6.8 Hz, 2H), 7.77 (d, J ¼ 7.0 Hz, 2H), 7.72–
7.66 (m, 4H), 7.60 (d, J ¼ 8.2 Hz, 2H), 7.56–7.52 (t, 2H), 6.93–6.89
(t, 2H), 6.66–6.62 (t, 2H), 6.48 (d, J ¼ 8.0 Hz, 2H), 5.16 (s, 1H),
1.80 (s, 6H). Anal. calcd for C43H27IrN4O2S2: C, 58.16; H, 3.06; N,
6.31; S, 7.22. Found: C, 58.12; H, 3.09; N, 6.28; S, 7.20.
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Ir-Np. Yield 70%. MALDI-TOF-MS (m/z): 812.1436 ([C39H27
-
IrN2O2S2]+). 1H NMR (400 MHz, CDCl3) d (ppm) 8.20 (d, J ¼ 9.0
Hz, 2H), 8.12 (d, J ¼ 7.8 Hz, 2H), 7.99 (d, J ¼ 8.2 Hz, 2H), 7.85 (d,
J ¼ 9.0 Hz, 2H), 7.74 (d, J ¼ 9.0 Hz, 2H), 7.70–7.66 (t, 2H), 7.61–
7.57 (t, 2H), 6.89–6.85 (t, 2H), 6.48 (d, J ¼ 7.8 Hz, 2H), 5.13 (s,
1H), 1.78 (s, 6H). Anal. calcd for C39H27IrN2O2S2: C, 57.69; H,
3.35; N, 3.45; S, 7.90. Found: C, 57.63; H, 3.33; N, 3.42; S, 7.88.
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Acknowledgements
We thank the National Natural Science Foundation of China 15 R. Wang, L. Deng, T. Zhang and J. Li, Dalton Trans., 2012, 41,
(21274016, 21374013, and 21421005), the Program for
6833.
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