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Journal of Structural Chemistry

2011 year, number 5

STRUCTURE OF THE FIRST NITROSOAMMINE COMPLEXES OF RUTHENIUM WITH A COORDINATED SULFATE ION: [Ru(NO)(NH3)4(SO4)](HSO4)·H2O AND [Ru(NO)(NH3)3Cl(SO4)]·2H2O

A. N. Makhinya, E. A. Shusharina, I. A. Baidina, M. A. Il'in
Keywords: ruthenium, nitroso complexes, ammine complexes, sulfate complexes, chlorine complexes, single crystal X-ray diffraction, thermogravimetry, IR spectroscopy
Pages: 973-980

Abstract

We present a thermogravimetric study of the thermolysis of trans-[Ru(NO)(NH3)4(H2O)](HSO4)SO4 in a helium atmosphere. The intermediate product of thermolysis (at 186°C) is treated with a 2 M H2SO4 solution to obtain the first example of a sulfate ammine complex of nitrosoruthenium [Ru(NO)(NH3)4(SO4)](HSO4)·H2O (I) with a ~70% yield. The product of higher temperature thermolysis (220°C) is treated with acids (H2SO4 and HCl) to obtain a triammine complex [Ru(NO)(NH3)3Cl(SO4)]·2H2O (II). The structure of the compounds is found by single crystal XRD: Pna21 space group, a = 10.8005(2) Å, b = 14.9032(3) Å, c = 7.7603(1) Å) (I) and P21/n space group, a = 8.9397(1) Å, b = 8.3276(1) Å, c = 13.8993(2) Å; β = 97.358(1)° (II).