Synthesis And Crystal Structure Of An Azide Bridged Binuclear Zinc(Ii) Complex Including The Reduced Derivative Of Nitronyl Nitroxide, [Zn(Him2py)(N-3)(2)](2)

msra(2004)

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摘要
The title compound [Zn(Him2Py)(N-3)(2)](2) (Zn2C26H38N18O2, M-r = 765.48) has been prepared and structurally characterized by X-ray diffraction methods. It crystallizes in monoclinic, space group P2(1)/n with a = 10.989(3), b = 11.519(3), c = 13.812(4) Angstrom, beta = 101.700(5)degrees, V = 1711.9(9) Angstrom(3), Z = 2, D-c = 1.485 g/cm(3), mu(MoKalpha) = 1.456 mm(-1), F(000) = 792, the final R = 0.0401 and wR = 0.0861 for 2054 observed reflections with I>2sigma(I). The imino nitroxide 2-(3'-methyl-2'-pyridyl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazolyl-1-oxyl (im2Py) was reduced to obtain 2-(3'-methyl-2'-pyridyl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazole-1-ydroxy(Him2Py) coordinating to the zinc (11) ion, around which the coordination geometry is a square-based pyramid with a terminal nitrogen atom located at the apical position. The four basal sites are occupied by two mu(1,1) nitrogen atoms from two different bridging azide ions and two nitrogen atoms from Him2Py. The units of [Zn(Him2Py)(N-3)(2)](2) were connected as two dimension planes by intermolecular hydrogen bonds.
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关键词
crystal structure, nitronyl nitroxide radical, Zn(II) complex
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