Pyrazole-Tethered Heteroditopic Ligands and Their Transition Metal Complexes
FULL PAPER
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anhydrous CuCl2 (0.27 g, 2 mmol) in acetonitrile (10 mL) at room
temperature. Immediately, the solution was change color, to light
yellow. It was then refluxed for 6 h; the solution turned greenish
yellow. After removal of solvent, greenish compound 7 (0.42 g,
41%) was formed, which was purified by recrystallization from ace-
tonitrile. When the reaction was performed under air the yield was
improved (0.95 g, 94%). M.p. Ͼ240 °C. IR (Nujol) 1132, 1554,
1589 cm–1. Microanalysis C23H21Cl2CuN2OP (506.86): calcd. C
54.50, H 4.17, N 5.52; found C 54.42, H 4.32, N 5.51.
Preparation of CuI Complex 8: An acetonitrile solution (10 mL) of
2a (0.356 g, 1 mmol) was added to a suspension of CuCl (0.093 g,
1 mmol) in acetonitrile (12 mL). The reaction mixture was refluxed
for 12 h. The reaction slurry was filtered and the filtrate was con-
centrated under vacuum to give yellow solid 8 (0.40 g, 44%). Crys-
tals suitable for X-ray analysis were obtained from an acetonitrile
solution of CuI complex 8. M.p. Ͼ240 °C. IR (Nujol):
1552, 1587 cm–1. 1H NMR (CDCl3, 200 MHz): δ = 1.81 (s, 3 H,
CH3), 2.40 (br. s, 3 H, CH3), 5.69 (s, 1 H, pzH), 7.24–7.54 (m, 14
H, PhH) ppm. 13C NMR (CDCl3, 50.32 MHz): δ = 11.90,
14.00, 107.77, 128.13, 128.76, 129.20, 130.15, 131.22, 133.68,
142.02, 150.92 ppm. 31P (CDCl3, 80.02 MHz): δ –16.37 ppm.
C46H42Cl2Cu2N4P2·CH3CN (951.87): calcd. C 60.57, H 4.76, N
7.36; found C 60.46, H 4.69, N 7.02.
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Financial support from Reliance Industries Ltd., India, is gratefully
acknowledged; A. M. thanks CSIR, India, for a research fellow-
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Received: September 30, 2004
Eur. J. Inorg. Chem. 2005, 1254–1263
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