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NMR, X-Ray Crystal Structure Studies and Mechanism for Formation of a Novel Di-gallium Complex and 5-Methoxy-4,5,6-triphenyl-4,5-dihydro-1,2,4-triazene-3(2H)-thione

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Abstract

Gallium complexes of bis-thiosemicarbazones were prepared and characterized using NMR and X-ray crystallography. Formation of a gallium nitrate complex was proven by NMR spectroscopy. Surprisingly, this complex was found to convert on standing to a new hydroxido-bridged di-gallium complex. The X-ray crystal structure of the digallium complex is described. Similarly, a triazene compound was formed during the preparation of the gallium complex comprising a tetraphenyl unit in the bis-thiosemicarbazone structure. We propose a mechanism for the formation of both the di-gallium species as well as triazene compound in solution. The lattice parameters for the digallium complex is as follows: a: 17.6854(13) Å, b:16.6492(7) Å, c: 21.4659(14) Å, β = 112.383(8)°.

Graphical Abstract

Gallium complexes of bis-thiosemicarbazones were prepared and were found to convert to a new hydroxido-bridged di-gallium complex

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References

  1. Abram S, Maichle-Mössmer C, Abram U (1998) Polyhedron 17(1):131–143

    Article  CAS  Google Scholar 

  2. Chan J, Thompson AL, Jones MW, Peach JM (2010) Inorg Chim Acta 363(6):1140–1149

    Article  CAS  Google Scholar 

  3. Molter A, Mohr F (2011) Dalton Trans 40(14):3754–3758

    CAS  PubMed  Google Scholar 

  4. Bermejo E, Carballo R, Castiñeiras A, Domínguez R, Liberta AE, Maichle-Mössmer C, Salberg MM, West DX (1999) Eur J Inorg Chem 1999(6):965–973

    Article  Google Scholar 

  5. Bermejo E, Carballo R, Castiñeiras A, Domínguez R, Maichle-Mössmer C, Strähle J, West DX (1999) Polyhedron 18(27):3695–3702

    Article  CAS  Google Scholar 

  6. Bermejo E, Castiñeiras A, García-Santos I, West DX (2005) Z Anorg Allg Chem 631(11):2011–2019

    Article  CAS  Google Scholar 

  7. Bermejo E, Castiñeiras A, West DX (2003) J Mol Struct 650(1):93–97

    Article  CAS  Google Scholar 

  8. Brown CA, Kaminsky W, Claborn KA, Goldberg KI, West DX (2002) J Braz Chem Soc 13(1):10–18

    Article  CAS  Google Scholar 

  9. Castiñeiras A, Garcia I, Bermejo E, West DX (2000) Polyhedron 19(15):1873–1880

    Article  Google Scholar 

  10. Klayman DL, Lin AJ, Hoch JM, Scovill JP, Lambros C, Dobek AS (1984) J Pharm Sci 73(12):1763–1767

    Article  CAS  PubMed  Google Scholar 

  11. Kovala-Demertzi D, Domopoulou A, Demertzis MA, Papageorgiou A, West DX (1997) Polyhedron 16(20):3625–3633

    Article  CAS  Google Scholar 

  12. Kovala-Demertzi D, Miller JR, Kourkoumelis N, Hadjikakou SK, Demertzis MA (1999) Polyhedron 18(7):1005–1013

    Article  CAS  Google Scholar 

  13. West DX, Bain GA, Butcher RJ, Jasinski JP, Li Y, Pozdniakiv RY, Valdés-Martínez J, Toscano RA, Hernández-Ortega S (1996) Polyhedron 15(4):665–674

    Article  CAS  Google Scholar 

  14. West DX, Carlson CS, Bouck KJ, Liberta AE (1991) Transit Met Chem 16(2):271–275

    Article  CAS  Google Scholar 

  15. Diaz A, García I, Cao R, Beraldo H, Salberg MM, West DX, González L, Ochoa E (1997) Polyhedron 16(20):3549–3555

    Article  CAS  Google Scholar 

  16. West DX, El-Sawaf AK, Bain GA (1997) Transit Met Chem 23(1):1–6

    Article  Google Scholar 

  17. West DX, Ives JS, Krejci J, Salberg MM, Zumbahlen TL, Bain GA, Liberta AE, Valdes-Martinez J, Hernandez-Ortiz S, Toscano RA (1995) Polyhedron 14(15–16):2189–2200

    Article  CAS  Google Scholar 

  18. West DX, Liberta AE, Padhye SB, Chikate RC, Sonawane PB, Kumbhar AS, Yerande RG (1993) Coord Chem Rev 123(1–2):49–71

    Article  CAS  Google Scholar 

  19. West DX, Salberg MM, Bain GA, Liberta AE (1997) Transit Met Chem 22(2):180–184

    Article  CAS  Google Scholar 

  20. West DX, Stark AM, Bain GA, Liberta AE (1996) Transit Met Chem 21(4):289–295

    Article  CAS  Google Scholar 

  21. Yadav B, Kumar V, Yadav M (1998) Indian J Pure Appl Phys 36(10):557–566

    CAS  Google Scholar 

  22. Wadas TJ, Wong EH, Weisman GR, Anderson CJ (2010) Chem Rev 110(5):2858–2902

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  23. Pascu SI, Waghorn PA, Conry TD, Betts HM, Dilworth JR, Churchill GC, Pokrovska T, Christlieb M, Aigbirhio FI, Warren JE (2007) Dalton Trans 43:4988–4997

    Article  CAS  Google Scholar 

  24. Pascu SI, Waghorn PA, Conry TD, Lin B, Betts HM, Dilworth JR, Sim RB, Churchill GC, Aigbirhio FI, Warren JE (2008) Dalton Trans 16:2107–2110

    Article  CAS  Google Scholar 

  25. MacroModel, version 2016-3, Schrödinger. LLC, New York (2016)

  26. Sheldrick GM (2008) Acta Crystallogr A 64(1):112–122

    Article  CAS  PubMed  Google Scholar 

  27. Farrugia LJ (1999) J Appl Crystallogr 32(4):837–838

    Article  CAS  Google Scholar 

  28. Farrugia LJ (2012) J Appl Crystallogr 45(4):849–854

    Article  CAS  Google Scholar 

  29. Venkatachalam T, Pierens G, Bernhardt PV, Stimson D, Bhalla R, Lambert L, Reutens D (2016) Aust J Chem 69(9):1033–1048

    Article  CAS  Google Scholar 

  30. Addison AW, Rao TN, Reedijk J, van Rijn J, Verschoor GC (1984) J Chem Soc 7:1349–1356

    Google Scholar 

  31. Calatayud DG, Escolar FJ, López-Torres E, Mendiola MA (2007) Helv Chim Acta 90(11):2201–2216

    Article  CAS  Google Scholar 

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Acknowledgements

This work was partially supported by an ARC Linkage Project Grant LP 130100703 (D.R.). We thank our colleagues at the Centre for Advanced Imaging for their help during the course of this investigation.

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Authors and Affiliations

  1. Center for Advanced Imaging, The University of Queensland, Brisbane, 4072, Australia

    T. K. Venkatachalam, G. K. Pierens & D. C. Reutens

  2. School of Chemistry and Molecular Biosciences, The University of Queensland, Brisbane, 4072, Australia

    Paul V. Bernhardt

Authors
  1. T. K. Venkatachalam
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  2. Paul V. Bernhardt
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  3. G. K. Pierens
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  4. D. C. Reutens
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Correspondence to T. K. Venkatachalam.

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Venkatachalam, T.K., Bernhardt, P.V., Pierens, G.K. et al. NMR, X-Ray Crystal Structure Studies and Mechanism for Formation of a Novel Di-gallium Complex and 5-Methoxy-4,5,6-triphenyl-4,5-dihydro-1,2,4-triazene-3(2H)-thione. J Chem Crystallogr 49, 131–138 (2019). https://doi.org/10.1007/s10870-018-0745-z

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