STRUCTURE, SYNTHESIS, AND THERMAL PROPERTIES OF trans-[Ru(NO)(NH3)4(SO4)]NO3В·H2O
S. A. Adonin1, P. A. Abramov1, S. I. Uskov2
1Novosibirsk State University, 630090 Pr. Lavrentieva 3
2Novosibirsk State University, 630090 st. Pirogova, 2
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)](HSO 4)×H2O (I) is obtained with a yield close to quantitative. In the interaction of the saturated solution of I with a saturated NaNO 3 solution a trans-[Ru(NO)(NH3)4(SO4)]NO3×H2O (II) precipitate forms whose structure is determined by single crystal XRD: space group Р 2 12 12 1, 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 (D H = 58.9 ± 1.5 kJ/mol) is estimated. The final product of the thermolysis of II is a mixture of Ru and RuO2.
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