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Synthesis, Structure and Thermal Decomposition of (H9O4)2[Re6S6Br8]

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Abstract

The condensation of trinuclear rhenium bromide with lead sulfide yields the (H9O4)2Re6S6Br8 octahedral cluster complex isolated from the HBr/EtOH mixture in the form of the acid. (H9O4)2[Re6S6Br8] crystallizes in the P21/c space group, a = 9.2010(2) Å, b = 9.1508(2) Å, c = 17.3759(3) Å, γ = 101.817(1)°. Thermal decomposition of the complex at a moderate temperature (350 °C) results in a metastable Re6S6Br6 compound, which is not formed in the ternary Re–S–Br system at high temperatures. This compound is X-ray amorphous; its structure is determined based on the X-ray photoelectron and Raman spectroscopy data.

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REFERENCES

  1. A. Perrin, C. Perrin, and M. Sergent. Octahedral clusters in molybdenum(II) and rhenium(III) chalcohalide chemistry. J. Less Common Met., 1988, 137(1/2), 241-265. https://doi.org/10.1016/0022-5088(88)90091-4

    Article  CAS  Google Scholar 

  2. J.-C. P. Gabriel, K. Boubekeur, S. Uriel, and P. Batail. Chemistry of hexanuclear rhenium chalcohalide clusters. Chem. Rev., 2001, 101(7), 2037-2066. https://doi.org/10.1021/cr980058k

    Article  CAS  PubMed  Google Scholar 

  3. V. E. Fedorov, Y. V Mironov, N. G. Naumov, M. N. Sokolov, and V. P. Fedin. Chalcogenide clusters of group 5-7 metals. Russ. Chem. Rev., 2007, 76(6), 529-552. https://doi.org/10.1070/rc2007v076n06abeh003707

    Article  ADS  CAS  Google Scholar 

  4. M. N. Sokolov, N. G. Naumov, P. P. Samoylov, and V. P. Fedin. Clusters and cluster assemblies. In: Comprehensive Inorganic Chemistry II / Eds. J. Reedijk and K. Poeppelmeier. Oxford: Elsevier, 2013, Vol. 2, 271-310. https://doi.org/10.1016/B978-0-08-097774-4.00212-6

    Chapter  Google Scholar 

  5. L. Leduc, A. Perrin, M. Sergent, F. Le Traon, J. C. Pilet, and A. Le Traon. Rhenium octahedral clusters: Characterization of Re6Se4Cl10 and the parent compound Re6Br10. Mater. Lett., 1985, 3(5/6), 209-215. https://doi.org/10.1016/0167-577x(85)90057-6

    Article  CAS  Google Scholar 

  6. A. Perricone, A. Slougui, and A. Perrin. Rhenium octahedral clusters: The systems Re–S–Br and M–Re–S–Br (M = Na, K, Rb, Cs). Solid State Sci., 1999, 1(7/8), 657-666. https://doi.org/10.1016/s1293-2558(00)80116-8

    Article  ADS  CAS  Google Scholar 

  7. A. Perrin, L. Leduc, and M. Sergent. Halogen bridged Re6L8 units in octahedral cluster rhenium chalcohalides. Eur. J. Solid State Inorg. Chem., 1991, 28, 919.

    Article  Google Scholar 

  8. C. Fischer, N. Alonso-Vante, S. Fiechter, H. Tributsch, G. Reck, and W. Schulz. Structure and photoelectrochemical properties of semiconducting rhenium cluster chalcogenides: Re6X8Br2 (X = S, Se). J. Alloys Compd., 1992, 178(1/2), 305-314. https://doi.org/10.1016/0925-8388(92)90272-b

    Article  CAS  Google Scholar 

  9. A. Slougui, S. Ferron, A. Perrin, and M. Sergent. Anionic charge effects on the crystal structures of Re6 octahedral cluster based compounds: The structure of the cubic bromide K2Re6S6Br8. J. Clust. Sci., 1997, 8(3), 349-359. https://doi.org/10.1007/bf02764113

    Article  CAS  Google Scholar 

  10. N. I. Kolbin and K. V. Ovchinnikov. Poluchenie i nekotorye svoistva tribromida reniya (Obtaining and some properties of rhenium tribromide). Zh. Neorg. Khim., 1968, 13, 2306. [In Russian]

  11. NETZSCH Proteus Thermal Analysis, v. 4.8.1. Selb, Germany: NETZSCH-Gerätebau.

  12. 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

    Article  ADS  Google Scholar 

  13. 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

    Article  ADS  Google Scholar 

  14. O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard, and H. Puschmann. OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Crystallogr., 2009, 42(2), 339-341. https://doi.org/10.1107/s0021889808042726

    Article  CAS  Google Scholar 

  15. S. S. Yarovoi, Y. I. Mironov, Y. V. Mironov, A. V. Virovets, V. E. Fedorov, U.-H. Pack, S. C. Shin, and M.-L. Seo. Synthesis of octahedral rhenium cluster chalcobromides Re6X4Br10 and Re6X8Br2 (X = S, Se, Te) by condensation from triangular rhenium bromide Re3Br9. Mater. Res. Bull., 1997, 32(9), 1271-1277. https://doi.org/10.1016/s0025-5408(97)00102-5

    Article  CAS  Google Scholar 

  16. A. Slougui, A. Perrin, and M. Sergent. Structure of potassium hexarhenium nonabromide pentasulfide: KRe6S5Br9. Acta Crystallogr., Sect. C: Cryst. Struct. Commun., 1992, 48(11), 1917-1920. https://doi.org/10.1107/s0108270192002919

    Article  ADS  Google Scholar 

  17. A. Y. Ledneva, M. N. Ivanova, P. A. Poltarak, S. S. Yarovoy, B. A. Kolesov, V. E. Fedorov, and N. G. Naumov. Systematic study of vibrational spectra of octahedral rhenium clusters {Re6S8–xBrx}Bry (x = 0, 1, 2, 3, 4) with mixed sulfur/bromine inner ligands. Symmetry, 2023, 15(9), 1791. https://doi.org/10.3390/sym15091791

    Article  ADS  CAS  Google Scholar 

  18. H. Schäfer and H. G. Schnering. Metall–Metall–Bindungen bei niederen Halogeniden, Oxyden und Oxydhalogeniden schwerer Übergangsmetalle Thermochemische und strukturelle Prinzipien. Angew. Chem., 1964, 76(20), 833-849. https://doi.org/10.1002/ange.19640762002

    Article  ADS  Google Scholar 

  19. J. Okal, W. Tylus, and L. Kȩpiński. XPS study of oxidation of rhenium metal on γ-Al2O3 support. J. Catal., 2004, 225(2), 498-509. https://doi.org/10.1016/j.jcat.2004.05.004

    Article  CAS  Google Scholar 

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Funding

This work was funded by the Russian Science Foundation (project No. 22-23-00626). The study was also supported by the Ministry of Science and Higher Education of the Russian Federation.

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Correspondence to S. S. Yarovoy.

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Russian Text © The Author(s), 2024, published in Zhurnal Strukturnoi Khimii, 2024, Vol. 65, No. 2, 122898.https://doi.org/10.26902/JSC_id122898

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Yarovoy, S.S., Sukhikh, T.S. & Naumov, N.G. Synthesis, Structure and Thermal Decomposition of (H9O4)2[Re6S6Br8]. J Struct Chem 65, 381–389 (2024). https://doi.org/10.1134/S002247662402015X

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