2560
B.-S. Zhang et al. / Journal of Organometallic Chemistry 694 (2009) 2555–2561
(100 MHz, CDCl3): d 170.1, 170.0, 162.1, 162.0, 153.5, 146.3, 133.1,
factors. The structures were solved by direct methods and ex-
panded using Fourier techniques and refined by full-matrix least-
squares methods [44]. The non-hydrogen atoms were refined
anisotropically, and the hydrogen atoms were included but not re-
fined. Their raw data were corrected and the structures were
solved using the SHELXL-97 program [45].
132.6, 132.1, 131.8, 131.7, 128.9, 128.8, 126.8, 122.0, 114.6, 114.4,
60.0, 22.5. 31P{1H} NMR (162 MHz, CDCl3): d 152.6. IR (KBr):
m
3053, 2969, 2930, 2870, 1596, 1550, 1429, 1319, 1230, 1150,
1109, 814, 745, 691 cmꢂ1. HRMS (positive ESI): [MꢂCl]+ calcd for
C22H21NOPPd: 452.0396, found: 452.0402.
[2-{N-(m-chlorophenyl)imino}-6-(diisopropylphosphinoxy)phenyl]
chloropalladium(II) (2d): 125 mg, 47% yield, pale yellow solids.
M.p. 190–191 °C. 1H NMR (400 MHz, CDCl3): d 8.35 (d, J = 3.9 Hz,
1H, CH@N), 7.55–7.52 (m, 1H, Ar-H), 7.48 (t, J = 2.0 Hz, 1H, Ar-H),
7.37 (app t, J = 8.0 Hz, 1H, Ar-H), 7.30–7.27 (m, 1H, Ar-H), 7.19
(d, J = 7.4 Hz, 1H, Ar-H), 7.11 (dt, J = 0.9, 7.8 Hz, 1H, Ar-H), 6.88
(d, J = 8.0 Hz, 1H, Ar-H), 2.56–2.47 (m, 2H, CH(CH3)2), 1.47 (d,
J = 7.1 Hz, 3H, CH(CH3)2), 1.42 (d, J = 7.1 Hz, 3H, CH(CH3)2), 1.36
(d, J = 7.0 Hz, 3H, CH(CH3)2), 1.32 (d, J = 7.0 Hz, 3H, CH(CH3)2).
13C{1H} NMR (100 MHz, CDCl3): d 173.2, 163.6, 153.3, 148.8,
145.6, 134.4, 129.9, 127.8, 126.8, 123.4, 122.6, 122.4, 115.0,
114.8, 29.7, 29.6, 29.3, 17.4, 17.3, 16.7. 31P{1H} NMR (162 MHz,
4. Supplementary material
CCDC 701329 and 701328 contain the supplementary crystallo-
graphic data for complexes 2a and 2b. These data can be obtained
free of charge from The Cambridge Crystallographic Data Centre
Acknowledgments
We are grateful to the National Natural Science Foundation of
China (Nos. 20572102, 20872133) and the Innovation Fund for
Outstanding Scholar of Henan Province (No. 074200510005) for
financial support of this work.
CDCl3): d 204.4. IR (KBr):
m 3067, 2969, 2926, 2869, 1575, 1544,
1457, 1424, 1351, 1227, 910, 821, 787, 760, 688 cmꢂ1. HRMS
(positive ESI): [MꢂCl] + calcd for C19H22ClNOPPd: 452.0162, found:
452.0166.
[(S)-2-{(N-1-phenylethyl)imino}-6-(diphenylphosphinoxy)phenyl]
chloropalladium(II) (2e): 145 mg, 48% yield, pale yellow solids.
References
M.p. 132–133 °C. ½a D20
ꢃ
ꢂ66 (c 0.23, CH2Cl2). 1H NMR (400 MHz,
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