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 P212121, 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.
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L. A. Kusch, S. Golhen, O. Cador, et al., J. Cluster Sci., 17, 303 (2007).
D. Schaniel, T. Woike, L. Kusch, and E. Yagubskii, Chem. Phys., 340,Nos. 1–3, 211 (2007).
M. J. Clarke, Coord. Chem. Rev., 232, 69 (2002).
A. S. Torsoni, B. F. Barros, J. C. Toledo, et al., Nitric Oxide Biol. Chem., 6, No. 3, 247 (2002).
B. F. Barros, J. C. Toledo, D. W. Franco, et al., Nitric Oxide Biol. Chem., 7, No. 1, 50 (2002).
P. G. Zanichelli, H. F. G. Estrela, R. C. Spadari-Bratfisch, et al., Nitric Oxide Biol. Chem., 16, No. 2, 189 (2007).
O. A. Plyusnina, V. A. Emel’yanov, I. A. Baidina, I. V. Korol’kov, and S. A. Gromilov, J. Struct. Chem., 48, No. 1, 114–121 (2007).
M. A. Il’in, N. V. Kuratieva, O. A. Kirichenko, et al., Acta Crystallogr., E61,Part 06, i126 (2005).
A. Pozio, R. F. Silva, M. D. Franchesco, et al., Electrochim. Acta, 48, 255 (2002).
D. Chu and S. Gilman, J. Electrochem. Soc., 143, No. 5, 1685 (1996).
M. A. Il’in, V. A. Emel’yanov, A. V. Belyaev, et al., Zh. Neorg. Khim., 53, No. 7, 1152 (2008).
P. Kubelka and F. Z. Munk, Tech. Phys., 12, 593 (1931).
J. Tauc, Mater. Res. Bull., 5, 721 (1970).
NETZSCH Proteus Thermal Analysis v.4.8.1, NETZSCH-Gerätebau-Bayern, Germany (2005).
OriginPro 7,5. SR0 v.7.5714 B(714), OriginLab Corporation-Northampton, USA (2003).
G. M. Sheldrick, SHELX-97, Release 97-1, Univ. Göttingen (1997).
A. N. Makhinya, E. A. Shusharina, I. A. Baidina, and M. A. Il’in, J. Struct. Chem., 52, No. 5, 946 (2011).
M. A. Il’in, V. A. Emel’yanov, I. A. Baidina, et al., Zh. Neorg. Khim., 52, No. 1, 71 (2007).
M. A. Il’in, V. A. Emel’yanov, and I. A. Baidina, J. Struct. Chem., 49, No. 6, 1090 (2008).
K. Nakamoto, Infrared and Raman Spectra of Inorganic and Coordination Compounds, 5th Edition. Part B, Wiley-Interscience, New York-Chichester-Weinheim etc. (1997), p. 13.
A. F. Schreiner, S. W. Lin, P. J. Hauser, et al., Inorg. Chem., 11, 880 (1972).
M. G. Gomes, C. U. Davanzo, S. C. Silva, et al., J. Chem. Soc., Dalton Trans., 601 (1998).
L. G. F. Lopes, E. E. Castellano, A. G. Ferreira, et al., Inorg. Chim. Acta, 358, 2883 (2005).
S. I. Gorelsky, S. C. Silva, A. B. P. Lever, and D. W. Franco, Inorg. Chim. Acta, 300–302, 698 (2000).
V. A. Emel’yanov, I. A. Baidina, M. A. Il’in, and S. A. Gromilov, J. Struct. Chem., 47, No. 2, 380 (2006).
V. A. Emel’yanov, I. A. Baidina, S. A. Gromilov, et al., J. Struct. Chem., 41, No. 6, 1030 (2000).
M. A. Il’in, E. V. Kabin, V. A. Emel’yanov, et al., J. Struct. Chem., 50, No. 2, 328 (2009).
E. V. Kabin, V. A. Emel’yanov, I. A. Baidina, et al., J. Struct. Chem., 51,Suppl., S73 (2010).
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Original Russian Text © 2014 A. N. Makhinya, M. A. Il’in, I. A. Baidina, P. E. Plyusnin, N. I. Alferova, D. P. Pishchur.
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Translated from Zhurnal Strukturnoi Khimii, Vol. 55, No. 2, pp. 331–338, March–April, 2014.
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Makhinya, A.N., Il’in, M.A., Baidina, I.A. et al. Structure, synthesis, and thermal properties of trans-[Ru(NO)(NH3)4(SO4)]NO3·H2O. J Struct Chem 55, 311–318 (2014). https://doi.org/10.1134/S0022476614020188
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DOI: https://doi.org/10.1134/S0022476614020188