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Synthesis, Characterization and Crystal Structure of Nickel Complex (dppv)Ni(C7H4NS2)2
Corresponding Author(s) : Yu-Long Li
Asian Journal of Chemistry,
Vol. 26 No. 1 (2014): Vol 26 Issue 1
Abstract
Reaction of 2-mercaptobenzothiazole with (dppv)NiCl2 (dppv: Ph2PCH=CHPPh2) in the presence of Et3N affords the title complex (dppv)Ni(C7H4NS2)2 in 92 % yield. The new complex was fully characterized by elemental analysis, TGA, IR and 1H (13C, 31P) NMR spectroscopies. In addition, the molecular structure of the title complex was established by X-ray crystallography. The crystal of (dppv)Ni(C7H4NS2)2·CH2Cl2 crystallizes in monoclinic, space group P2/n with a = 15.927(9), b = 8.3553(5), c = 16.3728(8) Å, a = 90.00, b = 112.417(4), g = 90.00°, V = 2014.22(19) Å3, Z = 2, C40H30N2NiP2S4·CH2Cl2, Mr = 872.48, Dc = 1.439 g/cm3, F(000) = 896 and μ(MoKa) = 0.934 mm-1. The final R = 0.0920 and wR = 0.2220 for 2572 observed reflections with I > 2s(I) and R = 0.1171 and wR = 0.2434 for all data. The geometry at the Ni centre in the title complex is square-planar with the NiP2S2 chromophore.
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References
S. Saito, M. Sakai and N. Miyaura, Tetrahedron Lett., 37, 2993 (1996); doi:10.1016/0040-4039(96)00482-0.
S. Saito, S. Oh-tani and N. Miyaura, J. Org. Chem., 62, 8024 (1997); doi:10.1021/jo9707848.
V. Percec, J.Y. Bae and D.H. Hill, J. Org. Chem., 60, 1060 (1995); doi:10.1021/jo00109a044.
M. Ueda, A. Saitoh, S. Oh-tani and N. Miyaura, Tetrahedron, 54, 13079 (1998); doi:10.1016/S0040-4020(98)00809-6.
A.S.E. Karlström, K. Itami and J.-E. Bäckvall, J. Org. Chem., 64, 1745 (1999); doi:10.1021/jo982060h.
A. Volbeda, M.H. Charon, C. Piras, E.C. Hatchikian, M. Frey and J.C. Fontecilla-Camps, Nature, 373, 580 (1995); doi:10.1038/373580a0.
M. Cowie, R.L. DeKock, T.R. Wagenmaker, D. Seyferth, R.A. Henderson and M.K. Gallagher, Organometallics, 8, 119 (1989); doi:10.1021/om00103a015.
A.A. Lozano, M.D. Santana, G. Garcia, J.E. Barclay, S.C. Davies and D.J. Evans, Z. Anorg. Allg. Chem., 631, 2062 (2005); doi:10.1002/zaac.200570015.
W.H. Watson, A. Nagl, M.J. Don and M.J. Richmond, J. Chem. Crystallogr., 29, 871 (1999); doi:10.1023/A:1009565726187.
L.-L. Duan, M. Wang, P. Li, N. Wang, F.-J. Wang and L.-C. Sun, Inorg. Chim. Acta, 362, 372 (2009); doi:10.1016/j.ica.2008.04.011.
J.-F. Jiang, M. Maruani, J. Solaimanzadeh, W.-F. Lo, S.A. Koch and M. Millar, Inorg. Chem., 48, 6359 (2009); doi:10.1021/ic900929u.
M. Schmidt and G.G. Hoffmann, Chem. Ber., 112, 2190 (1979); doi:10.1002/cber.19791120626.
M. Schmidt and G.G. Hoffmann, J. Organomet. Chem., 124, C5 (1977); doi:10.1016/S0022-328X(00)90057-3.
W.-F. Zhu, A.C. Marr, Q. Wang, F. Neese, D.J.E. Spencer, A.J. Blake, P.A. Cooke, C. Wilson and M. Schröder, Proc. Natl. Acad. Sci. USA, 102, 102 (2005).
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Crystalclear and Crystalstructure, Rigaku and Rigaku Americas. 9009 New Trails Dr. The Woodlands TX 77381 USA.
G.M. Sheldrick, SHELXS97, A Program for Crystal Structure Solution, University of Göttingen: Germany (1997).
G.M. Sheldrick, SHELXS97, A Program for Crystal Structure Refinement, University of Göttingen: Germany (1997).