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Synthesis and Crystal Structure of O-Methyldithiophosphato Nickel Complex [Ni(S2P{O}OCH3)(dppe)]
Corresponding Author(s) : Yu-Long Li
Asian Journal of Chemistry,
Vol. 25 No. 15 (2013): Vol 25 Issue 15
Abstract
O-Methyldithiophosphato nickel complex [Ni(S2P{O}OCH3)(dppe)] (I) (dppe = Ph2PCH2CH2PPh2) has been synthesized by treatment of (dppe)NiCl2 with (CH2O)2P{S}SH·Et2NH in THF solution. The new complex (I) was fully characterized by elemental analysis, TGA, IR, 1H, 13C, 31P NMR spectroscopies. In addition the molecular structure of the complex was established by X-ray crystallography. The crystal of [Ni(S2P{O}OCH3)(dppe)] crystallizes in monoclinic, spacegroup P21/n with a = 9.2762(3), b = 17.1214(5), c = 18.8627(6) Å, a = 90.00, b = 96.813(3), g =90.00º, V = 2974.66(15) Å3, Z = 4, C27H27O2P3S2Ni, Mr = 599.23, Dc = 1.338 g/cm3, F(000) = 1240 and μ(MoKa) = 0.976 mm-1. The final R = 0.0521 and wR = 0.1303 for 6073 observed reflections [I > 2s(I)].
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References
S. Saito, M. Sakai and N. Miyaura, Tetrahedron Lett., 37, 2993 (1996).
S. Saito, S. Oh-tani and N. Miyaura, J. Org. Chem., 62, 8024 (1997).
V. Percec, J.Y. Bae and D.H. Hill, J. Org. Chem., 60, 1060 (1995).
M. Ueda, S. Saito, S. Oh-tani and N. Miyaura, Tetrahedron, 54, 13079 (1998).
A. Sofia, E. Karlström, K. Itami and J.E. Bäckvall, J. Org. Chem., 64, 1745 (1999).
W. Gao, K. Li and X.-L. Wang, Asian J. Chem., 25, 7876 (2013).
L.-L. Duan, M. Wang, P. Li, N. Wang, F.-J. Wang and L.-C. Sun, Inorg. Chim. Acta, 362, 372 (2009).
J.-F. Jiang, M. Maruani, J. Solaimanzadeh, W.-F. Lo, S.A. Koch and M. Millar, Inorg. Chem., 48, 6359 (2009).
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).
W.H. Watson,A. Nagl, M.J. Don and M.J. Richmond, J. Chem. Crystallogr., 29, 871 (1999).
M. Schmidt and G.G. Hoffmann, Chem. Ber., 112, 2190 (1979).
M. Schmidt and G.G. Hoffmann, J. Organomet. Chem., 124, C5 (1977).
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).
J.A.S. Bomfim, F.P. de Souza, C.A.L. Filgueiras, A.G. de Sousa and M.T.P. Gambardella, Polyhedron, 22, 1567 (2003).
Crystal Clear and Crystal Structure, 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, SHELXL97, A Program for Crystal Structure Solution, University of Göttingen, Germany (1997).
L. Szucová, Z. Trávnícek and J. Marek, Polyhedron, 22, 1341 (2003).