D. Zhang, G.-X. Jin / Inorganic Chemistry Communications 9 (2006) 1322–1325
1325
75.17; H, 6.31; N, 2.34%. IR (KBr): 1592 cmꢀ1 (vs, C@N). H NMR
(CDCl3): d = 7.82 ꢀ 5.77(m, 47H, H–Ar + CH@N), 2.52 (s, 6H,
CH3), 2.20 (s, 6H, CH3), 1.59 (s, 3H, CH3), 0.59 ppm (s, 18H,
C(CH3)3). 2a: Yield 88%. Anal. Calcd for C35H30N2O2: C, 82.33; H,
5.92; N, 5.49. Found: C, 82.02; H, 5.81; N, 5.11. IR (KBr): 1618 cmꢀ1
(vs, C@N). 1H NMR (CDCl3): d 13.59 (s, 2H, OH), 8.39 (s, 2H,
N@CH), 7.67 (d, J = 7.4 Hz, 4H, phenyl-oH), 7.44–7.51 (m, 6H,
phenyl-mH + phenyl-pH), 7.35 (m, 4H, phenol-mH), 6.99–7.25 (m,
3H, phenol-pH + mestyl-H), 2.19 (s, 6H, CH3-mestyl), 2.05 ppm (s,
3H, CH3-mestyl). 2b: Yield 91%. Anal. Calcd for C83H68N2Ni2O2P2:
C, 76.40; H, 5.25; N, 2.15. Found: C, 76.51; H, 5.31; N, 2.14. IR
(KBr): 1593 cmꢀ1 (vs, C@N). 1H NMR (CDCl3): d = 7.67 ꢀ 5.85 (m,
59H, H–Ar + CH@N), 2.49 (s, 6H, CH3–Ar), 1.59 ppm (s, 3H, CH3–
Ar).
1
References
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[15] X.F. Li, Y.-S. Li, J. Polym. Sci. Part A: Polym. Chem. 40 (2002) 2680.
[16] Crystal data for 2b: C83H68N2Ni2O2P2, Mr = 1304.75, Monoclinic,
˚
˚
Space group, C2/c, a = 13.491(5) A
,
b = 13.742(5) A
,
c =
3
˚
˚
36.379(13) A , b = 93.307(7)ꢁ, V = 3728(3) (A ), Z = 4, Dc = 1.287
(mg/m3), F(000) = 2728, reflections measured (1.12–25.01), R(wR) =
0.0437(0.0452) for 13,987 reflections with I > 2r(I). The diffraction
data were collected on a Siemens SMART CCD diffractometer. The
structures are solved using direct methods and refined on F2 by full-
matrix least-squares methods using the SHELX 97 program package.
Crystallographic data for the structure of 2b reported in this paper
has been deposited in the Cambridge Crystallographic Data Centre
No. CCDC-612132. Copies of the data can be obtained free of charge
on application to CCDC, 12, Union Road, Cambridge CB2 1EZ,
UK, fax: (internat.) +44 1233 336 033; e-mail: deposit@ccdc.
cam.ac.uk.
(b) F.M. Bauers, R. Thomann, S. Mecking, J. Am. Chem. Soc. 125
(2003) 8838;
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[14] 1a: Yield 77%. Anal. Calcd for C33H42N2O2: C, 79.48; H, 8.49; N,
5.62. Found: C, 79.45; H, 8.52; N, 5.84. IR (KBr): 1619 cmꢀ1 (vs,
1
[17] J. Feldman, S.J. McLain, A. Parthasarathy, W.J. Marshall, J.C.
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163.
C@N). H NMR (CDCl3): d13.37 (s, 2H, OH), 8.28 (s, 2H, N@CH),
7.22 (s, 2H, phenol-mH), 7.00 (s, 1H, H-mestyl), 6.98 (s, 2H, phenol-
mH), 2.32 (s, 6H, pCH3-phenol), 2.18 (s, 6H, CH3-mestyl), 2.05 (s,
3H, CH3-mestyl), 1.47 ppm (s, 18H, tert-Bu). 1b: Yield 84%. Anal.
Calcd for C81H80N2Ni2O2P2: C, 75.25; H, 6.24; N, 2.17. Found: C,