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Solvothermal Synthesis and Crystal Structure of A Supramolecular Compound Tris(tert-butylamino)chlorophosphonium Chloride
Corresponding Author(s) : Kangying Shu
Asian Journal of Chemistry,
Vol. 25 No. 4 (2013): Vol 25 Issue 4
Abstract
During the research of the reaction of OP(NHt-Bu)3 and ZnCl2 with hydrochloric acid in toluene, the crystal of the tris(tert-butylamino)chlorophosphonium chloride [ClP(NHt-Bu)3](Cl) (1) was obtained under solvothermal reaction condition. The single-crystal X-ray diffraction reveals the title compound crystallizes in space group P21/c (No. 14) with a = 15.280(3) Å, b = 9.2100(18) Å, c = 12.790(3) Å, a = 90 º, b = 93.19(3) º, g = 90º, V = 1797.1(6) Å3, Z = 4, Dc = 1.176 g cm-3, F(000) = 688, μ = 0.44 mm-1. The phosphorus atom of cation is located in the center of a tetrahedron constructed of a chloride atom and three N atoms of three NHt-Bu groups. The anion of Cl– is connected with a cation and adjacent cation through three N-H···Cl hydrogen bonds. And through these hydrogen bonds, a zig-zag supramolecular chain is formed, which array all along the c axis.
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- G.M. Aspinall, M.C. Copsey, A.P. Leedham and C.A. Russell,Coord. Chem. Rev., 227, 217 (2002).
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- W. Chai, L. Song, H. Shen and K. Shu, Phosphorus, Sulfur, Silicon Rel. Elem., 184, 3212 (2009).
- Y. Yang, W. Chai, L. Song and K. Shu, Acta Crystallogr. E, 66, M1486 (2010).
- J. Chen, W. Chai, L. Song, Y. Yang and F. Niu, Acta Crystallogr. E, 67, M1284 (2011).
- C. Song, W. Chai, L. Song, Y. Yang and J. Lin, Acta Crystallogr. E, 67, M109 (2011).
- Y. Yang, W. Chai, L. Song and J. Lin, Acta Crystallogr. C, 67, M293 (2011).
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- P. Vandersluis and A.L. Spek, Acta Crystallogr. A, 46, 194 (1990).
- A.L. Spek, PLATON A Multipurpose Crystallographic Tool, Utrecht University: Utrecht, The Netherlands (2001).
References
G.M. Aspinall, M.C. Copsey, A.P. Leedham and C.A. Russell,Coord. Chem. Rev., 227, 217 (2002).
T. Chivers, M. Krahn, G. Schatte and M. Parvez, Inorg. Chem., 42, 3994 (2003).
Z. Fu and T. Chivers, Can. J. Chem., 85, 358 (2007).
Z.Y. Fu and T. Chivers, Inorg. Chem., 44, 7292 (2005).
T. Chivers, Z.Y. Fu and L.K. Thompson, Chem. Commun., 2339 (2005).
A.F. Armstrong, T. Chivers, M. Krahn and M. Parvez, Can. J. Chem., 83, 1768 (2005).
W. Chai, J. Lin, L. Song, K. Shu, L. Qin, H. Shi and J. Guo, Solid State Sci., 12, 2100 (2010).
W.-X. Chai, L. Song, K.-Y. Shu, H.-S. Shi and L.-S. Qin, J. Chem. Crystallogr., 40, 448 (2010).
W. Chai, L. Song, H. Shen and K. Shu, Phosphorus, Sulfur, Silicon Rel. Elem., 184, 3212 (2009).
Y. Yang, W. Chai, L. Song and K. Shu, Acta Crystallogr. E, 66, M1486 (2010).
J. Chen, W. Chai, L. Song, Y. Yang and F. Niu, Acta Crystallogr. E, 67, M1284 (2011).
C. Song, W. Chai, L. Song, Y. Yang and J. Lin, Acta Crystallogr. E, 67, M109 (2011).
Y. Yang, W. Chai, L. Song and J. Lin, Acta Crystallogr. C, 67, M293 (2011).
G.M. Sheldrick, Acta Crystallogr. A, 64, 112 (2008).
P. Vandersluis and A.L. Spek, Acta Crystallogr. A, 46, 194 (1990).
A.L. Spek, PLATON A Multipurpose Crystallographic Tool, Utrecht University: Utrecht, The Netherlands (2001).