Research output: Contribution to journal › Article › peer-review
Complex Salts Containing [Pd(NH3)4]2+ Cations and WO42− and W7O246− Anions : The Precursors of Pd–W Metal Alloys. / Khranenko, S. P.; Sukhikh, A. S.; Komarov, V. Yu et al.
In: Journal of Structural Chemistry, Vol. 61, No. 3, 01.03.2020, p. 449-455.Research output: Contribution to journal › Article › peer-review
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TY - JOUR
T1 - Complex Salts Containing [Pd(NH3)4]2+ Cations and WO42− and W7O246− Anions
T2 - The Precursors of Pd–W Metal Alloys
AU - Khranenko, S. P.
AU - Sukhikh, A. S.
AU - Komarov, V. Yu
AU - Gromilov, S. A.
PY - 2020/3/1
Y1 - 2020/3/1
N2 - Two crystal structures containing [Pd(NH3)4]2+ cations and WO42− and W7O246− 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.
AB - Two crystal structures containing [Pd(NH3)4]2+ cations and WO42− and W7O246− 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.
KW - crystal chemistry
KW - heptatungstate anion
KW - palladium tetrammine
KW - single crystal X-ray diffraction analysis
KW - thermal decomposition
KW - tungstate anion
KW - CRYSTAL-STRUCTURES
UR - http://www.scopus.com/inward/record.url?scp=85088665808&partnerID=8YFLogxK
U2 - 10.1134/S0022476620030117
DO - 10.1134/S0022476620030117
M3 - Article
AN - SCOPUS:85088665808
VL - 61
SP - 449
EP - 455
JO - Journal of Structural Chemistry
JF - Journal of Structural Chemistry
SN - 0022-4766
IS - 3
ER -
ID: 24868446