Abstract
The synthesis method for [NiEn3]WO4 complex salt is described. Data of single crystal X-ray diffraction at 115 K are: space group \(p\bar 3\), a = 15.9633(5) Å, c = 9.9446(4) Å, V = 2194.6(1) Å3, Z = 6, dx = 2.210 g/cm3, Ni–N is 2.120(2)-2.149(2) Å, ∠N–Ni–N is 80.69(7)-82.28(7)°. From the differential scanning calorimetry data it is found that a phase transition occurs at 269 K. The crystal structural characteristics at 298 K are as follows: space group \(p\bar 31c\), a = 9.2641(3) Å, c = 9.9817(3) Å, V = 741.89(4) Å3, Z = 2, dx = 2.179 g/cm3, Ni–N is 2.128(2) Å, ∠N–Ni–N is 81.05(12)°. The phase transition is shown to correspond to the disordering of tungstate anions over three positions. The comparative analysis of N–H…O and C–H…O interionic contacts is performed.
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References
A. I. Gubanov. Double Complexes with Tetrammine Cations–Precursors of Metal Powders. Diss. … Cand. of Chem. Sc. [in Russian], Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, 2002.
S. V. Korenev. Synthesis, Structure, and Physicochemical Properties of Double Complex Salts of Platinum Metals with Ammonia and Halide Ions. Diss. … Dr. of Chem. Sc. [in Russian], Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences Novosibirsk, 2003.
K. V. Yusenko. Double Complex Salts of Hexachloro(bromo)metallates(IV) (Ir, Pt, Os, Re) of Rhodium(III) and Iridium(III) Chloropentammines. Diss. … Cand. of Chem. Sc. [in Russian], Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, 2005.
A. V. Zadesenets. Synthesis and Physicochemical Study of Complex Salts–Precursors of Ultrafine Metal Powders Containing Pt, Pd, and Some Base Metals. Diss. … Cand. of Chem. Sc. [in Russian], Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, 2008.
P. E. Plyusnin. Synthesis and Physicochemical Study of Double Complex Salts Pd(II), Pt(II), and Au(III) Tetrafluorometallates. Diss. … Cand. of Chem. Sc. [in Russian], Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, 2009.
E. Yu. Filatov. Preparation and Powder X–ray Diffraction Study of Nanosized Bimetallic Powders Containing Platinum Metals. Diss. … Cand. of Chem. Sc. [in Russian], Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, 2009.
Yu. V. Shubin. Formation and Structural Phase Transformations of Nanoscale Noble–Metal Based Bimetallic Particles. Diss. … Dr. of Chem. Sc. [in Russian], Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, 2009.
S. I. Pechenyuk and D. P. Domonov. J. Struct. Chem., 2011, 52(2), 412.
S. V. Korenev, I. A. Baidina, S. A. Gromilov, and K. V. Yusenko. J. Struct. Chem., 2002, 43(3), 488–494.
S. V. Korenev, A. B. Venediktov, Yu. V. Shubin, K. V. Yusenko, and S. A. Gromilov. J. Struct. Chem., 2003, 44(1), 46–49.
S. V. Korenev, S. A. Gromilov, A. I. Gubanov, and A. B. Venediktov. Rus. J. Coord. Chem., 2003, 29(3), 234–236.
K. V. Yusenko, S. A. Gromilov, I. A. Baidina, I. V. Korolkov, V. V. Zhivonitko, A. B. Venediktov, and S. V. Korenev. J. Struct. Chem., 2003, 44(1), 60–67.
K. V. Yusenko, S. A. Gromilov, I. V. Korolkov, I. A. Baidina, G. V. Romanenko, and S. V. Korenev. Russ. J. Inorg. Chem., 2004, 49(4), 568–573.
K. V. Yusenko, S. Riva, P. Carvalho, S. Arnaboldi, A. S. Sukhikh, M. Hanfland, and S. A. Gromilov. Scripta Materialia, 2017, 138, 22–27.
F. H. Allen. Acta Crystallogr., 2002, B58(3–1), 380–388.
W. Kraus and G. Nolze. J. Appl. Crystallogr., 1996, 29(3), 301.
G. B. Jameson, R. Shneider, E. Dubler, and H. R. Oswald. Acta Crystallogr., 1982, B38, 3016–3020.
Bruker AXS Inc. APEX2 V2013.6–2, SAINT V8.32B and SADABS–2012/1. Bruker Advanced X–ray Solutions, Madison, Wisconsin, USA.
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard, and H. Puschmann. J. Appl. Cryst., 2009, 42, 339–341.
G. M. Sheldrick. Acta Crystallogr., 2015, C71, 3–8.
A. L. Spek. Acta Crystallogr., 2009, D65, 148–155.
M. Lutz. Acta Crystallogr. Sect. C: Cryst. Struct. Commun., 2010, 66, m330–m335.
A. S. Sukhikh, S. P. Khranenko, D. P. Pishchur, and S. A. Gromilov. J. Struct. Chem., 2018, 59(3), 657–663.
S. P. Khranenko, V. Yu. Komarov, E. Yu. Gerasimov, A. V. Zadesenets, E. A. Maksimpvskii, and S. A. Gromilov. J. Struct. Chem., 2017, 58(7), 1448–1452.
S. A. Gromilov, E. Yu. Gerasimov, S. P. Khranenko, V. Yu. Komarov, and A. V. Zadesenets. J. Struct. Chem., 2017, 58(7), 1448–1452.
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Original Russian Text © 2018 S. P. Khranenko, A. S. Sukhikh, D. P. Pishchur, P. S. Buneeva, V. Yu. Komarov, S. A. Gromilov.
Translated from Zhurnal Strukturnoi Khimii, Vol. 59, No. 8, pp. 1960–1966, November-December, 2018.
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Khranenko, S.P., Sukhikh, A.S., Pishchur, D.P. et al. [NiEn3]WO4. Crystal Structural Features Of The Phase Transition At 269 K. J Struct Chem 59, 1897–1902 (2018). https://doi.org/10.1134/S0022476618080188
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DOI: https://doi.org/10.1134/S0022476618080188