Abstract
A comparative crystal chemical analysis of о-[Pd(NH3)4]3Мо7O24·6H2O (а = 17.3472(3) Å, b = 28.9064(4) Å, с = 30.2463(4) Å, space group Ibca, V = 15166.9 Å3, Z = 16) and m-[Pd(NH3)4]3Мо7O24·3H2O (а = 10.6617(2) Å, b = 20.5248(5) Å, с = 16.4676(3) Å, β = 103.0792(10)°, space group P21/n, V = 3510.11(13) Å3, Z = 4) is performed. Thermal decomposition products of o-[Pd(NH3)4]3Мо7O24·6H2O are studied. In the Н2 atmosphere at 900 °C, a mixture of mixed-metal solid solutions based on the Мо bcc lattice and the Pd fcc lattice is formed while in the 90% Не/10% Н2 atmosphere at 910 °C, a mixture of the solid solution based on the Мо bcc lattice and Pd2Mo3N is formed.
REFERENCES
Inorganic Crystal Structure Database, Release 2022. Karlsruhe, Germany: Fashinformationszentrum, 2022.
A. El-Himri, F. Sapiña, R. Ibañez, and A. Beltrán. Pd2Mo3N: a new molybdenum bimetallic interstitial nitride. J. Mater. Chem., 2001, 11(9), 2311-2314. https://doi.org/10.1039/b101616o
A. I. Gubanov, E. Y. Filatov, E. Y. Semitut, A. I. Smolentsev, P. V. Snytnikov, D. I. Potemkin, and S. V. Korenev. [Pd(NH3)4]MoO4 as a precursor for Pd–Mo-containing catalysts: Thermal behavior, X-ray analysis of the thermolysis products and related catalytic studies. Thermochim. Acta, 2013, 566, 100-104. https://doi.org/10.1016/j.tca.2013.03.036
S. P. Khranenko, A. S. Sukhikh, V. Y. Komarov, and S. A. Gromilov. Complex salts containing [Pd(NH3)4]2+ cations and and anions: The precursors of Pd–W metal alloys. J. Struct. Chem., 2020, 61(3), 449-455. https://doi.org/10.1134/s0022476620030117
Powder Diffraction File, PDF-2. Newtown, PA, USA: International Centre for Diffraction Data, 2022.
NETZSCH Thermal Analysis v.4.8.1. Bayern, Germany: NETZSCH-Gerätebau, 2005.
G. M. Sheldrick. SHELXT - Integrated space-group and crystal-structure determination. Acta Crystallogr., Sect. A: Found. Adv., 2015, 71(1), 3-8. https://doi.org/10.1107/s2053273314026370
G. M. Sheldrick. Crystal structure refinement with SHELXL. Acta Crystallogr., Sect. C: Struct. Chem., 2015, 71(1), 3-8. https://doi.org/10.1107/s2053229614024218
F. H. Allen. The Cambridge Structural Database: a quarter of a million crystal structures and rising. Acta Crystallogr., Sect. B: Struct. Sci., 2002, 58(3), 380-388. https://doi.org/10.1107/s0108768102003890
P. R. Spackman, M. J. Turner, J. J. McKinnon, S. K. Wolff, D. J. Grimwood, D. Jayatilaka, and M. A. Spackman. CrystalExplorer: a program for Hirshfeld surface analysis, visualization and quantitative analysis of molecular crystals. J. Appl. Crystallogr., 2021, 54(3), 1006-1011. https://doi.org/10.1107/s1600576721002910
A. S. Sukhikh, S. P. Khranenko, A. V. Zadesenets, and S. A. Gromilov. Structural features of mixed anions (Мо7–хWхO24)6– and their packing in the [Pd(NH3)4]3(Мо7–хWxO24)6H2O crystal structure. Crystallogr. Rep., 2022, 67(2), 143-149. https://doi.org/10.1134/s1063774522020213
S. V. Borisov. Cation sublattices in inorganic compounds. J. Struct. Chem., 1986, 27(3), 486-488. https://doi.org/10.1007/bf00751836
S. A. Gromilov and S. V. Borisov. Using pseudoperiodicity for polycrystal XRD determination of the general structural motif of coordination compounds. J. Struct. Chem., 2003, 44(4), 664-680. https://doi.org/10.1023/b:jory.0000017943.51537.b7
S. A. Gromilov, E. A. Bykova, and S. V. Borisov. Algorithms, software, and examples of pseudotranslational sublattice analysis for crystal structures. Crystallogr. Rep., 2011, 56(6), 947-952. https://doi.org/10.1134/s1063774511060101
H. Kleykamp. Constitution and thermodynamics of the Mo–Ru, Mo–Pd, Ru–Pd and Mo–Ru–Pd systems. J. Nucl. Mater., 1989, 167, 49-63. https://doi.org/10.1016/0022-3115(89)90424-8
J. C. Crowhurst, A. F. Goncharov, B. Sadigh, J. M. Zaug, D. Aberg, Y. Meng, and V. B. Prakapenka. Synthesis and characterization of nitrides of iridium and palladium. J. Mater. Res., 2008, 23(1), 1-5. https://doi.org/10.1557/jmr.2008.0027
Funding
The work was supported by the Ministry of Science and Higher Education of the Russian Federation (project No. 121031700313-8). The HR SEM analysis was performed using the facilities of the National Center for the Study of Catalysts.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
The authors declare that they have no conflicts of interests.
Additional information
Russian Text © The Author(s), 2023, published in Zhurnal Strukturnoi Khimii, 2023, Vol. 64, No. 3, 107726.https://doi.org/10.26902/JSC_id107726
Rights and permissions
About this article
Cite this article
Sukhikh, A.S., Khranenko, S.P., Zadesenets, A.V. et al. Crystal Chemical Analysis of Two Modifications of [Pd(NH3)4]3Мо7O24·nH2O. Thermal Decomposition Products. J Struct Chem 64, 450–461 (2023). https://doi.org/10.1134/S0022476623030101
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0022476623030101