Skip to main content
Log in

Study on the thermal behavior of the complexes of the type [PdX2(tdmPz)] (X = Cl, Br, I, SCN)

  • Published:
Journal of Thermal Analysis and Calorimetry Aims and scope Submit manuscript

Abstract

Four new mononuclear Pd(II) complexes of the type [PdX2(tdmPz)] {X = Cl (1); Br (2); I (3); SCN (4); tdmPz = 1-thiocarbamoyl-3,5-dimethylpyrazole} have been synthesized and characterized by elemental analysis, IR spectroscopy, 1H and 13C{1H}-NMR experiments. The thermal behavior of the complexes 14 has been investigated by means of thermogravimetry (TG) and differential thermal analysis (DTA). From the initial decomposition temperatures, the thermal stability of the complexes can be ordered in the sequence: 3 < 4  2 < 1. The final products of the thermal decompositions were characterized as metallic palladium by X-ray powder diffraction.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Scheme 1
Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

References

  1. Kovács A, Nemcsok D, Pokol G, Szécsényi KM, Leovac VM, Jacimovic ZK, Evans IR, Howard JAK, Tomic ZD, Giester G. Structural, spectroscopic and computational studies of the HgL2Cl2 complex (L = 3, 5-dimethyl-1-thiocarboxamide pyrazole) and the crystal structure of L. New J Chem. 2005;29:833–40.

    Article  Google Scholar 

  2. Evans IR, Howard JAK, Howard LEM, Evans JSO. Jaimovic′ ZK, Jevtovicc VS, Leovac VM. Transition metal complexes with pyrazole based ligands, part 18: new binuclear Cu(I), Cu(II) and Co(II) complexes with 3,5-dimethyl-1-thiocarboxamide pyrazole: synthesis, structural and magnetic studies. Inorg Chim Acta. 2004;357:4528–36.

    Article  CAS  Google Scholar 

  3. Barik AK, Bandyopadhyayb P, Kar SK. Copper(II) and nickel(II) complexes of pyrazole derived ligands: synthesis, characterization and coordinating properties of two substituted thiocarbamyl pyrazoles, 3,5-dimethyl-1-N-methyl/ethyl thiocarbamyl pyrazole (HL1, HL2), potential ligands for biological interest. X-ray crystallographic studies of Ni(L2)21. Polyhedron. 1999;18:1–6.

    Article  CAS  Google Scholar 

  4. Barik AK, Paul S, Butcher RJ, Kar SK. Synthesis and characterization of two tris-chelate complexes of cobalt(III) with 3,5-dimethyl-1-(N-methyl/ethyl)thiocarbamyl-pyrazole (HL1, HL2)—biologically important bidentate ligands with one ambidentate donor site. Polyhedron. 2000;19:2651–5.

    Article  CAS  Google Scholar 

  5. Casas JS, Castellano EE, Ellena J, García-Tasende MS, Pérez-Parellé ML, Sánchez A, Sánchez-Gonzalez A, Sordo J, Touceda A. New Pd(II) and Pt(II) complexes with N, S-chelated pyrazolonate ligands: molecular and supramolecular structure and preliminary study of their in vitro antitumoral activity. J Inorg Biochem. 2008;102:33–45.

    Article  CAS  Google Scholar 

  6. Budakoti A, Abid M, Azam A. Synthesis and antiamoebic activity of new 1-N-substituted thiocarbamoyl-3,5-diphenyl-2-pyrazoline derivatives and their Pd(II) complexes. Eur J Med Chem. 2006;42:63–70.

    Article  Google Scholar 

  7. Budakoti A, Abid M, Azam A. Syntheses, characterization and in vitro antiamoebic activity of new Pd(II) complexes with 1-N-substituted thiocarbamoyl- 3,5-diphenyl-2-pyrazoline derivatives. Eur J Med Chem. 2007;42:544–51.

    Article  CAS  Google Scholar 

  8. Husain k, Abid M, Azam A. Novel Pd(II) complexes of 1-N-substituted 3-phenyl-2-pyrazoline derivatives and evaluation of antiamoebic activity. Eur J Med Chem. 2008;43:393–403.

    Article  CAS  Google Scholar 

  9. Rocha FV, Barra CV, Netto AVG, Mauro AE, Carlos IZ, Frem RCG, Ananias SR, Quilles MB, Stevanato A, da Rocha MC. 3,5-Dimethyl-1-thiocarbamoylpyrazole and its Pd(II) complexes: synthesis, spectral studies and antitumor activity. Eur J Med Chem. 2010;45:1698–702.

    Article  CAS  Google Scholar 

  10. Treu-Filho O, Rocha FV, Netto AVG, Pinheiro JC, Utuni VHS, Kondo RT, Mauro AE. Molecular structures and vibrational frequencies for [PdX2(tdmPz)] (X = Cl, SCN): A DFT study. J Mol Struct. 2009;921:239–43.

    Article  CAS  Google Scholar 

  11. Netto AVG, Takahashi PM, Frem RCG, Mauro AE, Zorel Júnior HE. Thermal decomposition of palladium(II) pyrazolyl complexes. Part I. J Anal Appl Pyrolysis. 2004;72:183–9.

    Article  CAS  Google Scholar 

  12. de Almeida ET, Santana AM, Netto AVG, Torres C, Mauro AE. Thermal study of cyclopalladated complexes of the type [Pd2(dmba)2X2(bpe)]. J Therm Anal Calorim. 2005;82:361–4.

    Article  Google Scholar 

  13. Netto AVG, Santana AM, Mauro AE, Frem RCG, de Almeida ET, Crespi MS, Zorel Júnior HE. Thermal decomposition of palladium(II) pyrazolyl complexes. Part II. J Therm Anal Calorim. 2005;79:339–42.

    Article  CAS  Google Scholar 

  14. Netto AVG, Frem RCG, Mauro AE, Crespi MS, Zorel Júnior HE. Synthesis, spectral and thermal studies on pyrazolate-bridged palladium(II) cocordination polymers. J Therm Anal Calorim. 2007;87:789–92.

    Article  CAS  Google Scholar 

  15. Fernandes RL, Takahashi PM, Frem RCG, Netto AVG, Mauro AE, Matos JR. Synthesis, spectral and thermal studies on dicarboxylate-bridged palladium(II) coordination polymers. Part I. J Therm Anal Calorim. 2009;97:123–6.

    Article  CAS  Google Scholar 

  16. Fernandes RL, Takahashi PM, Frem RCG, Netto AVG, Mauro AE, Matos JR. Synthesis, spectral and thermal studies on dicarboxylate-bridged palladium(II) coordination polymers. Part II. J Therm Anal Calorim. 2009;97:153–6.

    Article  CAS  Google Scholar 

  17. Moro AC, Watanabe FW, Ananias SR, Mauro AE, Netto AVG, Lima APR, Ferreira JG, Santos RHA. Supramolecular assemblies of cis-palladium complexes dominated by C–HCl interactions. Inorg Chem Commun. 2006;9:493–6.

    Article  CAS  Google Scholar 

  18. Netto AVG, Frem RCG, Mauro AE. Low-weight coordination polymers derived from the self-assembly reactions of Pd(II) pyrazolyl compounds and azide ion. Polyhedron. 2005;24:1086–92.

    Article  CAS  Google Scholar 

  19. Netto AVG, Mauro AE, Frem RCG, Santana AM, Santos RHA, Zoia JR. Synthesis and structural characterization of dichlorobis(1-phenyl-3-methylpyrazole)palladium(II) and diazidobis(1-phenyl-3-methylpyrazole)palladium(II). J Coord Chem. 2001;54:129–41.

    Article  Google Scholar 

  20. Moro AC, Mauro AE, Netto AVG, Ananias SR, Quilles MB, Carlos IZ, Pavan FR, Leite CQF, Hörner M. Antitumor and antimycobacterial activities of cyclopalladated complexes: X-ray structure of [Pd(C2,N-dmba)(Br)(tu)] (dmba = N, N-dimethylbenzylamine, tu = thiourea). Eur J Med Chem. 2009;44:4611–5.

    Article  CAS  Google Scholar 

  21. de Almeida ET, Mauro AE, Santana AM, Netto AVG, Carlos IZ. Emprego de compostos organometálicos mononucleares de paládio(II) na ativação de macrófagos peritoneais de camundongos. Quím Nova. 2005;28:405–8.

    Article  Google Scholar 

  22. de Souza RA, Stevanato A, Treu-Filho O, Netto AVG, Mauro AE, Castellano EE, Carlos IZ, Pavan FR, Leite CQF. Antimycobacterial and antitumor activities of Palladium(II) complexes containing isonicotinamide (isn): X-ray structure of trans-[Pd(N3)2(isn)2]. Eur J Med Chem. 2010;45:4863–8.

    Article  Google Scholar 

  23. Powder Diffraction File of the Joint Committee on Powder Diffraction Standards. Sets 1–32, published by the International Center of Diffraction Data: Swarthmore, PA 19081, 1982.

  24. Netto AVG, Frem RCG, Mauro AE, Santos RHA, Zoia JR. Crystallographic and spectroscopic studies on palladium(II) complexes containing pyrazole and thiocyanate ligands. Transit Met Chem. 2002;27:279–83.

    Article  Google Scholar 

  25. Mauro AE, Pulcinelli SH, Santos RHA, Gambardella MTP. Synthesis and structural studies of bis(1, 10-phenanthrolinethiocyanatemercury) tetracarbonyliron. Polyhedron. 1992;11:799–803.

    Article  CAS  Google Scholar 

Download references

Acknowledgements

The authors wish to acknowledge CNPq, FAPESP, and CAPES for the financial support.

Author information

Authors and Affiliations

Authors

Corresponding authors

Correspondence to Adelino V. G. Netto or Antonio E. Mauro.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Rocha, F.V., Barra, C.V., Franchi, S.J.S. et al. Study on the thermal behavior of the complexes of the type [PdX2(tdmPz)] (X = Cl, Br, I, SCN). J Therm Anal Calorim 106, 385–389 (2011). https://doi.org/10.1007/s10973-010-1239-1

Download citation

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10973-010-1239-1

Keywords

Navigation