Ulrich FLÖRKE, Esra KAYHAN, Nevzat KÜLCÜ, Hakan ARSLAN

Synthesis, characterization, crystal structure and thermal behavior of N'-(4-chlorobenzoyl)_N,N-di N-di-n-butylthiourea and its nickel complex

We report the synthesis, structural characterization and thermal behavior of N'-(4-chlorobenzoyl)-N, N-di-n-butylthiourea (HL) and its nickel complex (NiL2). Some physical properties of the prepared compounds were investigated using elemental analyses, IR, $^1H-NMR$, and magnetic susceptibility. The molecular structures of HL and NiL2 were determined by single crystal X-ray diffraction. HL is a mono-clinic, space group $P2_1/c$ with a = 10.7457(5) Â, b = 15.5909(8) Â, c = 10.4536(5) Â, $beta$ = 104.398(1)°, and V = 1696.34(14) $A^3$ with Z = 4 for $d_{calc}$ = 1.280 g/cm3. NiL2 is a triclinic, space group P-1 with a = 8.561(3) Â, b = 16.643(6) Â, c = 25.723(9) Â, $alpha$ = 77.448(6)°, $beta$ = 84.077(7)°, 7 $gamma$= 88.684(6)°, and V = 3558(2) $A^3$ with Z = 4 for $d_{calc}$ = 1.326 g/cm3. The ligands coordinate to the metal atom in a bidentate manner, yielding an essentially neutral complex of the type $ML_2$. Thermal decomposition of related compounds was investigated by TG and DTA. The pyrolytic end product was identified by X-ray powder diffraction.

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1. K.H. König, M. Schuster, G. Schneeweis and B. Steinbrech, Fresenius Z. Anal. Chem. 319, 66-69 (1984).
2. R. Campo, J.J. Criado, R. Gheorghe, F.J. Gonzalez, M.R. Hermosa, F. Sanz, J.L. Manzano, E. Monte and E.R. Fernandez, J. Inorg. Biochem. 98, 1307-1314 (2004).
3. X. Shen, X. Shi, B. Kang, Y. Liu, Y. Tong, H. Jiang and K. Chen, Polyhedron 17, 4049-4058 (1988).
4. F.A. Frech, E.J. Blanz, J.R D. Amaral and D.A. French, J. Med. Chem. 13, 1117-1124 (1970).
5. B.B. Mohapatra, S. Guru and K.B. Mohapatra, J. Inorg. Nul. Chem. 39, 2291-2292 (1977).
6. W. Antholine and F. Taketa, J. Inorg. Biochem. 16, 145-154 (1982).
7. H. Arslan, U. Flörke and N. Külcü, Trans. Metal Chem. 28(7), 816-819 (2003).
8. N. Ozpozan, H. Arslan, T. Ozpozan, M. Merdivan and N. Külcü, J. Thermal Anal. 61, 955-965 (2000).
9. G. Avsar, N. Külcü and H. Arslan, Turk. J. Chem. 26, 607-615 (2002).
10. H. Arslan, U. Flörke and N. Külcü, Acta Crystallogr. E59, o641-o642 (2003).
11. H. Arslan, U. Flörke and N. Külcü, J. Chem. Crystallog. 33, 919-924 (2003).
12. N. Ozpozan, H. Arslan, T. Ozpozan, N. Ozdes and N. Külcü, Thermochimica Acta 343, 127-133 (2000).
13. H. Arslan, D. Vanderveer, F. Emen and N. Külcü, Z. Kristallogr. NCS. 218, 479-480 (2003).
14. E. Kayhan, U. Flörke, N. Külcü and H. Arslan, Acta Crystallog. E59, o1237- o1238 (2003).
15. Bruker (2002). SMART (Ver. 5.62), SAINT (Ver. 6.02), SHELXTL (Ver. 6.10) and SADABS (Version 2.03). Bruker AXS Inc., Madison, Wisconsin, USA.
16. I.B. Dauglass and F.B. Dains, J. Am. Chem. Soc. 56, 719-721 (1934).
17. R.A. Bailey, K.L. Rothaupt and R.K. Kullnig, Inorg. Chem. Acta 147, 233-236 (1988).
18. P. Knuuttila, H. Knuuttila, H. Hennig and L. Beyer, Acta Chemica Scandinavica A36, 541-545 (1982).
19. N. Ozpozan, T. Ozpozan, H. Arslan, F. Karipcin and N. Külcü, Thermochimica Acta 336, 97-103 (1999).