Structure, synthesis, and thermal properties of trans-[Ru(NO)(NH3)4(SO4)]NO3•H2O

In treatment of trans-[Ru(NO)(NH3)(4)(OH)]Cl-2 with concentrated sulfuric acid on heating trans-[Ru(NO)(NH3)(4)(SO4)](HSO4)center dot 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 center dot H2O (II) precipitate forms whose structure is determined by single crystal XRD: space group P2(1)2(1)2(1), a = 6.8406(3) , b = 12.6581(5) , c = 13.3291(5) . 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 120A degrees C (Delta H = 58.9 +/- 1.5 kJ/mol) is estimated. The final product of the thermolysis of II is a mixture of Ru and RuO2.