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

被引:8
|
作者
Makhinya, A. N. [1 ,2 ]
Il'in, M. A. [1 ,2 ]
Baidina, I. A. [1 ]
Plyusnin, P. E. [1 ,2 ]
Alferova, N. I. [1 ]
Pishchur, D. P. [1 ]
机构
[1] Russian Acad Sci, Siberian Branch, Nikolaev Inst Inorgan Chem, Novosibirsk, Russia
[2] Novosibirsk State Univ, Novosibirsk, Russia
关键词
ruthenium; nitroso complexes; amino complexes; sulfato complexes; synthesis; single crystal X-ray diffraction analysis; thermal analysis; CRYSTAL-STRUCTURE; RUTHENIUM; COMPLEXES;
D O I
10.1134/S0022476614020188
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
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.
引用
收藏
页码:311 / 318
页数:8
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