Abstract
Two crystal structures containing [Pd(NH3)4]2+ cations and \(\text{WO}_4^{2-}\) and \(\text{W}_7\text{O}_{24}^{6-}\) anions are studied. For the [Pd(NH3)4]WO4 structure at 150 K the following crystallographic data are obtained: a = 7.4626(3) Å, c = 15.5718(8) Å, space group I41/amd, V = 867.20 Å3, Z = 4. With increasing temperature to 400 K, the unit cell parameters change in different directions: a increases by 0.032 Å, c decreases by 0.036 Å. The total increase in the unit cell volume is 5 Å3. In a range of 150 K to 400 K, the observed W-O distances decrease by 0.019 Å from 1.778(18) Å to 1.759(3) Å. For the [Pd(NH3)4]3W7O24·4.4H2O structure at 298 K the crystallographic data are as follows: a = 8.3409(2) Å, b = 22.2654(6) Å, c = 10.5450(3) Å, β = 104.449(1)°, space group P21/m, V = 1896.41 Å3, Z = 2. In the heptatungstate anion the shortest are the W—O distances with the terminal O atoms (1.731–1.745 Å). The distances to the bridging O atoms connecting two W atoms are 1.930–2.406 Å; those connecting three W atoms are 1.882–2.234 Å, and those connecting four W atoms are 2.192–2.220 Å. It is shown that the [Pd(NH3)4]3W7O24·4.4H2O structure has a pseudohexagonal motif in the a direction. The thermal decomposition of the salts is performed in the presence of LiH in the He atmosphere at 1273 K. The ex situ powder X-ray diffraction study reveals the formation of Pd–W alloys.
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Russian Text © The Author(s), 2020, published in Zhurnal Strukturnoi Khimii, 2020, Vol. 61, No. 3, pp. 472–478.
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Khranenko, S.P., Sukhikh, A.S., Komarov, V.Y. et al. Complex Salts Containing [Pd(NH3)4]2+ Cations and \(\text{WO}_4^{2-}\) and \(\text{W}_7\text{O}_{24}^{6-}\) Anions: The Precursors of Pd–W Metal Alloys. J Struct Chem 61, 449–455 (2020). https://doi.org/10.1134/S0022476620030117
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DOI: https://doi.org/10.1134/S0022476620030117