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Journal of Structural Chemistry

2014 year, number 4

STRUCTURE AND PROPERTIES OF TRIPYRIDINE NITROSOCOMPLEXES OF RUTHENIUM: mer-[Ru(NO)Py 3Cl(OH)]ClГ—1.5H 2O AND mer-[Ru(NO)Py 3Cl(H 2O)]Cl 2Г—2H 2OГ—0.5HCl

A.N. Makhinya1,2, M.A. Il’in1,2, I.A. Baidina1, P.E. Plyusnin1,2, M.R. Gallyamov1
1Nikolaev Institute of Inorganic Chemistry, Russian Academy of Sciences, Siberian Branch, Novosibirsk, Russia
2Novosibirsk state university, Russia
Keywords: нитрозокомплексы, рутений, аминокомплексы, пиридин, рентгеноструктурный анализ, ИК спектроскопия, ЯМР, термогравиметрия, nitrosocomplexes, ruthenium, amine complexes, pyridine, X-ray crystallography, IR spectroscopy, NMR, thermal analysis

Abstract

Reaction of K 2[Ru(NO)Cl 5] with pyridine in aqueous ethanol at pH ~ 7-8 affords a nitrosoruthenium hydroxocomplex mer -[Ru(NO)Py 3Cl(OH)]Cl×1.5H 2O (I), yield ~55 %. The treatment of the hydroxocomplex I with hydrochloric acid at room temperature gives the aqua complex mer -[Ru(NO)Py 3Cl(H 2O)]Cl 2×2H 2O×0.5HCl (II). The structures of the compounds have been determined by X-ray crystallography: I - sp. gr. P 2 1/ n , a = 9.2292(4), b = 11.7781(4), c = 17.4915(7) Å, β = 90.9560(10)°, R = 4.84%; II - sp. gr. P -1, a = 7.3528(9), b = 11.5793(11), c = 13.6961(16) Å, α = 84.558(3), β = 87.668(4), γ = 74.146(4)°, R = 6.22%. Compounds I and II have been characterized by powder XRD, 1Н and 13С NMR, as well as IR spectroscopy. Thermal decomposition of compound II in inert atmosphere has been examined with thermal analysis.