Acta Crystallographica Section B

Structural Science

Volume 63, Part 1 (February 2007)

short communications

Acta Cryst. (2007). B63, 151-156 [ doi:10.1107/S0108768106047306 ]

Structural study of four complexes of the M-N₂S₂ type derived from diethylphenylazothioformamide and the metals palladium, platinum, copper and nickel

K. T. Nielsen, P. Harris, K. Bechgaard and F. C. Krebs

Abstract: The four electron-transfer complexes trans-(di(N,N-diethyl-(2-phenyldiazenyl)thioformamide- [kappa] S, [kappa] N²))nickel, trans-(di(N,N-diethyl-(2-phenyldiazenyl)thioformamide- [kappa] S, [kappa] N²))copper, trans-(di(N,N-diethyl-(2-phenyldiazenyl)thioformamide- [kappa] S, [kappa] N²))palladium and trans-(di(N,N-diethyl-(2-phenyldiazenyl)thioformamide- [kappa] S, [kappa] N²))platinum have been crystallized, and their structures have been determined at low temperature. All the complexes are of the M-N₂S₂ type. The crystals of both the nickel and the copper complex belong to the tetragonal P4₁2₁2 system, in which the central metal ion lies on a twofold axis. The tetrahedral molecular symmetry around the central metal ion is unusual for the M-N₂S₂ electron-transfer complexes. The crystals of the palladium and platinum complexes on the other hand belong to the monoclinic C2/c system in which the metal ion lies on an inversion centre. The molecular symmetry around these metal ions is square planar. It is demonstrated that the [pi] electron density in the ligand planes has a high degree of delocalization. Furthermore, unusually large line broadening of the ¹H NMR spectra was observed and investigated as a function of temperature for the palladium complex.

Keywords: N,N-diethylphenylazothioformamide; electron-transfer complex; low-temperature determination.


	Structure factor file (CIF format) (178.1 kbytes) [ doi:10.1107/S0108768106047306/bk5045NiL20sup2.hkl ] Contains datablock NiL2O

	Structure factor file (CIF format) (139.1 kbytes) [ doi:10.1107/S0108768106047306/bk5045CuL20sup3.hkl ] Contains datablock CuL2O

	Structure factor file (CIF format) (139.9 kbytes) [ doi:10.1107/S0108768106047306/bk5045PdL20sup4.hkl ] Contains datablock PdL2O

	Structure factor file (CIF format) (144.3 kbytes) [ doi:10.1107/S0108768106047306/bk5045PtL20sup5.hkl ] Contains datablock PtL2O

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