Novel double complex salts [M(im) n][RuNOCl5] (M = Ni, Cu): synthesis, structure, thermal properties

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Abstract

Methods for the synthesis of new double complex salts [Cu(im)4][RuNOCl5], [Ni(im)6][RuNOCl5]·H2O and [Ni(im)4(DMF)2][RuNOCl5] have been developed and their crystalline crystalline properties have been determined. structure. The thermal properties of synthesized DCS were studied in inert and reducing atmospheres using synchronous TG–DTA/EGA–MS analysis and ex situ X-ray diffraction of intermediate and final thermolysis products. It has been established that thermal decomposition occurs in three stages. The final products of thermolysis of [Cu(im)4][RuNOCl5] in inert and reducing atmospheres are a mixture of copper and ruthenium, and the product of thermal decomposition of [Ni(im)6][RuNOCl5]·H2O in an inert atmosphere is a mixture of nickel and ruthenium. In the nickel-ruthenium system, upon thermolysis in a reducing atmosphere in the range of up to 400°C, it is possible to obtain a supersaturated solid solution of Ni0.27Ru0.73. Increasing the thermolysis temperature to 800°C leads to partial decomposition of the solid solution.

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About the authors

А. O. Borodin

Nikolaev Institute of Inorganic Chemistry

Author for correspondence.
Email: borodin@niic.nsc.ru
Russian Federation, Novosibirsk, 630090

E. Yu. Filatov

Nikolaev Institute of Inorganic Chemistry

Email: borodin@niic.nsc.ru
Russian Federation, Novosibirsk, 630090

P. E. Plusnin

Nikolaev Institute of Inorganic Chemistry

Email: borodin@niic.nsc.ru
Russian Federation, Novosibirsk, 630090

N. V. Kuratieva

Nikolaev Institute of Inorganic Chemistry

Email: borodin@niic.nsc.ru
Russian Federation, Novosibirsk, 630090

S. V. Korenev

Nikolaev Institute of Inorganic Chemistry

Email: borodin@niic.nsc.ru
Russian Federation, Novosibirsk, 630090

G. A. Kostin

Nikolaev Institute of Inorganic Chemistry

Email: borodin@niic.nsc.ru
Russian Federation, Novosibirsk, 630090

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Supplementary files

Supplementary Files
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2. Fig. 1. Calculated (1) and experimental (2) diffraction patterns for [Cu(im)4][RuNOCl5] (a) and [Ni(im)6][RuNOCl5] · H2O (b)

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3. Fig. 2. Cationic and anionic parts of the [Cu(im)4][RuNOCl5] DCS. Hydrogen atoms are not shown for clarity, thermal ellipsoids are given with a probability of 50% (a). Packing of anionic and cationic fragments in the [Cu(im)4][RuNOCl5] DCS (b)

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4. Fig. 3. Cationic and anionic fragments in the DCS [Ni(im)4(DMF)2][RuNOCl5]

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5. Fig. 4. Thermal analysis curves for [Cu(im)4][RuNOCl5] in inert (red lines) and reducing (black lines) atmospheres

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6. Fig. 5. Thermal analysis curves for [Ni(im)6][RuNOCl5] · H2O in inert (red lines) and reducing (black lines) atmospheres

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7. Fig. 6. Experimental diffraction patterns of the products of thermal decomposition of DCS [Cu(im)4][RuNOCl5] (a) and [Ni(im)6][RuNOCl5] · H2O (b) in a hydrogen atmosphere at different temperatures

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8. Fig. 7. Experimental diffraction patterns of the products of thermal decomposition in a hydrogen atmosphere of DCS [Cu(im)4][RuNOCl5] at 800C (a) and [Ni(im)6][RuNOCl5] H2O at 400C (b), theoretical diffraction patterns corresponding to metallic Cu, Ni, Ru and solid solution Ni0.27Ru0.73, as well as difference curves between the experimental diffraction pattern and the total theoretical

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