STRUCTURE, SYNTHESIS, AND THERMAL PROPERTIES OF trans-[Ru(NO)(NH3)4(SO4)]NO3В·H2O
A. N. Makhinya1,2, M. A. Il’in1,2, I. A. Baidina1, P. E. Plyusnin1,2, N. I. Alferova1, D. P. Pishchur1
1Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2Novosibirsk State University, Novosibirsk, Russia
Keywords: ruthenium, nitroso complexes, amino complexes, sulfato complexes, synthesis, single crystal X-ray diffraction analysis, thermal analysis
Abstract
In treatment of trans-[Ru(NO)(NH3)4(OH)]Cl2 with concentrated sulfuric acid on heating trans-[Ru(NO)(NH3)4(SO4)](HSO4)×H2O (I) is obtained with a yield close to quantitative. In the interaction of the saturated solution of I with a saturated NaNO3 solution a trans -[Ru(NO)(NH3)4(SO4)]NO3×H2O (II) precipitate forms whose structure is determined by single crystal XRD: space group Р212121, a = 6.8406(3) Å, b = 12.6581(5) Å, c = 13.3291(5) Å. A monodentately coordinated sulfate ion is in the trans-position to the nitroso group. Compound II is characterized by IR spectroscopy, powder XRD, and diffuse reflectance spectroscopy. The process of its thermolysis is studied; by differential scanning calorimetry the thermal effect of the dehydration reaction occurring on heating to 120°C (ΔH = 58.9 ± 1.5 kJ/mol) is estimated. The final product of the thermolysis of II is a mixture of Ru and RuO2.
|
