Rhenium(V) Tris(pyrazolyl)borate Thiolate Complex with the Disulfide Bridging Ligand: Synthesis and Structure

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Abstract

The reaction of TpReOCl(StBu) (Tp = tris(pyrazolyl)borate anion) with sodium disulfide in dimethoxyethane affords the new binuclear rhenium complex [TpReO(μ-StBu)]2(μ-S2) (I). Complex I can also be synthesized by the reaction of TpReO(StBu)2 with a suspension of manganese(II) bromide in toluene accompanied by the dealkylation of one of the ligands to form one more new complex [TpReO]2(μ-S2)(μ-S) (II) containing the bridging sulfide and disulfide ligands. The structures of two crystalline solvates of complex I with dichloromethane containing the molecules with different conformations of the Re2S2 fragment (Ia and Ib) and complex II are studied by X-ray diffraction (XRD) (CIF files ССDC nos. 2262677, 2262678, and 2267423 for Ia, Ib, and II, respectively).

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About the authors

I. V. Skabitskii

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Author for correspondence.
Email: skabitskiy@gmail.com
Russian Federation, Moscow

S. S. Shapovalov

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Email: skabitskiy@gmail.com
Russian Federation, Moscow

References

  1. Trofimenko S. // Chem. Rev. 1993. V. 93. P. 943.
  2. Lail M., Pittard K. A., Gunnoe T. B. // Adv. Organomet. Chem. 2008. V. 56. P. 95.
  3. Tisato F., Bolzati C., Duatti A. et al. // Inorg. Chem. 1993. V. 32. № 10. P. 2042.
  4. Doonan C. J., Nielsen D. J., Smith P. D. et al. // J. Am. Chem. Soc. 2006. V. 128. Р. 305.
  5. McWhinnie S.L.W., Jones C. J., McCleverty J.A. et al. // Polyhedron. 1993. V. 12. P. 3743.
  6. Wei L.-P., Ren Z.-G., Zhu L.-W.et al.// Inorg. Chem. 2011. V. 50. P. 4493.
  7. Y. Arikawa, Y. Otsubo, T. Nakayama et al. // Inorg. Chim. Acta. 2019. V. 490. P. 45.
  8. Skabitskii I. V., Sakharov S. G., Pasynskii A. A. et al. // Russ. J. Coord. Chem. 2019. V. 45. P. 539. https://doi.org/10.1134/S1070328419080086
  9. SADABS (version 2008/1). Madison (WI, USA): Bruker AXS Inc., 2008.
  10. Sheldrick G. M. TWINABS (version 2012/1). Madison (WI, USA): Bruker AXS Inc., 2012.
  11. Sheldrick G. M. // Acta Crystallogr. A. 2008. V. 64. P. 112.
  12. Dolomanov O. V., Bourhis L. J., Gildea R. J. et al. // J. Appl. Cryst. 2009. V. 42. P. 339.
  13. Neese F. The ORCA Program System. Wiley Interdisciplinary Reviews – Computational Molecular Science. 2012. V. 2. P. 73.
  14. Perdew J. P., Burke K., Ernzerhof M. // Phys. Rev. Lett. 1996. V. 77. P. 3865.
  15. Perdew J. P., Burke K., Ernzerhof M. // Phys. Rev. Lett. 1997. V. 78. P. 1396 (Errata).
  16. Weigend F., Ahlrichs R. // Phys. Chem. Chem. Phys. 2005. V. 7. P. 3297.
  17. Grimme S., Ehrlich S., Goerigk L. // J. Comput. Chem. 2011. V. 32. P. 1456.
  18. Grimme S., Antony J., Ehrlich S. et al. // J. Chem. Phys. 2010. V. 132. P. 154104.
  19. Adamo C., Barone V. // J. Chem. Phys. 1999. V. 110. P. 6158.
  20. van Lenthe E., Baerend E. J., Snijders J. B. // J. Chem. Phys. 1993. V. 99. P. 4597.
  21. van Wüllen C. // J. Chem. Phys. 1998. V. 109. P. 392.
  22. Rolfes J. D., Neese F., Pantazis D. A. // J. Comput. Chem. 2020. V. 41. P. 1842.
  23. Pantazis D. A., Chen X. Y., Landis C. R. et al. // J. Chem. Theory Comput. 2008. V. 4. P. 908.
  24. Diemann E., Muller A. // Z. Naturforsch. B. 1976. V. 31. P. 1287.
  25. Cordero B., Gómez V., Platero-Prats A.E. // Dalton Trans. 2008. V. 21. P. 2832.
  26. Goodman J. T., Rauchfuss T. B. // Inorg.Chem. 1998. V. 37. P. 5040.
  27. Gourlay C., Taylor M. K., Smith P. D. et al. // Inorg. Chim. Acta. 2010. V. 363. P. 1126.

Supplementary files

Supplementary Files
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1. JATS XML
2. Fig. 1. Molecular structure of Ia (a), Ib molecule 1 (b) and Ib molecule 2 (c) (independent molecules for Ib are shown in separate projections).

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3. Fig. 2. Molecular structure II (the solvate molecule of methylene chloride is not shown). Selected bond lengths: Re(1)—O(1) 1.702(4), Re(2)—O(2) 1.687(4), Re(1)—S(1) 2.320(1), Re(2)—S(1) 2.335(1), Re(1)—S(2) 2.237(2), Re(2)—S(3) 2.251(2), Re(1)—N(1) 2.251(5), Re(1)—N(3) 2.138(5), Re(1)—N(5) 2.165(5), Re(2)—N(7) 2.270(5), Re(2)—N(9) 2.106(5), Re(2)—N(11) 2.176(5), S(2)—S(3) 2.122(2) Å and valence angles: Re(1) S(1) Re(2) 119.84(6)oh, S(3) S(2) Re(1) 113.75(7)oh, S(2) S(3) Re(2) 113.74(8) fr.

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4. Scheme 1.

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5. Scheme 2.

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