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Synthesis, Characterization and X-Ray Crystal Structure of Dizinc(II) Complex of Pseudo Calixarene Macrocycle Based on 2,2-Methylene-bis[(6-formyl)-4-tert-butylphenol] and 1,3-Diamino-2-propanol
Corresponding Author(s) : Imdad Hussain
Asian Journal of Chemistry,
Vol. 27 No. 7 (2015): Vol 27 Issue 7, 2015
Abstract
[(2+2)Zn2·CH3COO] complex was prepared by refluxing 2,2-methylene-bis[(6-formyl)-4-tert-butylphenol] (H2mftbp) and 1,3-diamino-2-propanol in a round-bottomed flask containing Ca(ClO4)2 in ethanol in the presence of a base. Sample was taken from the refluxing solution and submitted for MS. ESI-MS showed the peak to confirm the formation of calcium complex [(2+2)Ca] but when Zn(CH3COO)2·2H2O was added and refluxed for further 6 h. Zinc replaced calcium metal and a new complex of Zn was formed as [Zn2(2+2)] complex. A yellow powder was filtered after cooling at room temperature. The powder was crystallized by vapour diffusion method. The complex crystallizes in the monoclinic crystal system with space group P2(1)/n. Unit cell parameters are; a = 13.6595(7) Å, b = 18.5216(9) Å, c = 25.0723(12) Å, a = 90°, b = 95.7020(10)°, g = 90°, Z = 8 and V= 6311.8(5) Å3. The complex was characterized by using single crystal X-ray spectroscopy, IR-spectroscopy and ESI-mass spectrophotometery.
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- (a) R.C. Long and D.N. Hendrickson, J. Am. Chem. Soc., 105, 1513 (1983); doi:10.1021/ja00344a018; (b) H. Okawa, J. Nishio, M. Ohba, M. Tadokoro, N. Matsumoto, M. Koikawa, S. Kida and D.E. Fenton, Inorg. Chem., 32, 2949 (1993); doi:10.1021/ic00065a025; (c) M. Yonemura, N. Usuki, Y. Nakamura, M. Ohba and H. Okawa, J. Chem. Soc., Dalton Trans., 3624 (2000); doi:10.1039/b006605m; (d) A. Atkins, D. Black, A.J. Blake, A. Marin-Becerra, S. Parsons, L. Ruiz-Ramirez and M. Schroder, Chem. Commun., 457 (1996); doi:10.1039/cc9960000457.
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- O. Jiménez-Sandoval, D. Ramírez-Rosales, M.J. Rosales-Hoz, M.E. Sosa-Torres and R. Zamorano-Ulloa, J. Chem. Soc., Dalton Trans., 1551 (1998); doi:10.1039/a801292j.
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References
(a) R.C. Long and D.N. Hendrickson, J. Am. Chem. Soc., 105, 1513 (1983); doi:10.1021/ja00344a018; (b) H. Okawa, J. Nishio, M. Ohba, M. Tadokoro, N. Matsumoto, M. Koikawa, S. Kida and D.E. Fenton, Inorg. Chem., 32, 2949 (1993); doi:10.1021/ic00065a025; (c) M. Yonemura, N. Usuki, Y. Nakamura, M. Ohba and H. Okawa, J. Chem. Soc., Dalton Trans., 3624 (2000); doi:10.1039/b006605m; (d) A. Atkins, D. Black, A.J. Blake, A. Marin-Becerra, S. Parsons, L. Ruiz-Ramirez and M. Schroder, Chem. Commun., 457 (1996); doi:10.1039/cc9960000457.
(a) A. Hori, M. Yonemura, M. Ohba and H. Okawa, Bull. Chem. Soc. Jpn., 74, 495 (2001); doi:10.1246/bcsj.74.495; (b) M.J. Grannas, B.F. Hoskins and R. Robson, Inorg. Chem., 33, 1071 (1994); doi:10.1021/ic00084a017; (c) K.K. Nanda, S. Mohanta, U. Florke, S.K. Dutta and K. Nag, J. Chem. Soc., Dalton Trans., 3831 (1995); doi:10.1039/dt9950003831; (d) J. McCrea, V. McKee, T. Metcalfe, S.S. Tandon and J. Wikaira, Inorg. Chim. Acta, 297, 220 (2000); doi:10.1016/S0020-1693(99)00361-8.
(a) V. McKee and S.S. Tandon, J. Chem. Soc., Dalton Trans., 221 (1991); doi:10.1039/dt9910000221; (b) P.E. Kruger and V. McKee, Chem. Commun., 1341 (1997); doi:10.1039/a702788e; (c) S. Cromie, V. McKee and F. Launay, Chem. Commun., 1918 (2001); doi:10.1039/b106340p.
S.M. Nelson, Pure Appl. Chem., 52, 2461 (1980); doi:10.1351/pac198052112461.
D.E. Fenton, Pure Appl. Chem., 58, 1437 (1986); doi:10.1351/pac198658111437.
V. McKee, W.T. Robinson, D. McDowell and J. Nelson, Tetrahedron Lett., 30, 7453 (1989); doi:10.1016/S0040-4039(00)70723-4.
Y. Nishida, N. Tanaka, A. Yamazaki, T. Tokii, N. Hashimoto, K. Ide and K. Iwasawa, Inorg. Chem., 34, 3616 (1995); doi:10.1021/ic00118a008.
O. Jiménez-Sandoval, D. Ramírez-Rosales, M.J. Rosales-Hoz, M.E. Sosa-Torres and R. Zamorano-Ulloa, J. Chem. Soc., Dalton Trans., 1551 (1998); doi:10.1039/a801292j.
D. Zhang, H. Wang, L. Tian, J. Jiang and Z. Ni, CrystEngComm, 11, 2447 (2009); doi:10.1039/b903174j.
V. Yu Kukushkin, D. Tudela, Y.A. Izotova, V.K. Belsky and A.I. Stash, Polyhedron, 17, 2455 (1998); doi:10.1016/S0277-5387(98)00041-2.
A.X.S. Bruker, APEX2-Software Suite for Crystallographic Programs, Bruker AXS Inc., Madison (2009).
G.M. Sheldrick, Acta Crystallogr. A, 64, 112 (2008); doi:10.1107/S0108767307043930.
L.J. Farrugia, J. Appl. Cryst., 32, 837 (1999); doi:10.1107/S0021889899006020.
G.M. Sheldrick, SADABS-Bruker AXS Scaling and Absorption Correction, Bruker AXS Inc., Madison (2008).
K. Brandenburg, Diamond-Crystal and Molecular Structure Visualization, v. 3.2g. Crystal Impact GbR, Bonn (2011).
J.D. Dunitz, P. Seiler and R.P. Phizackerley, Acta Crystallogr. B, 30, 2739 (1974); doi:10.1107/S0567740874007928.