Preparation and Powder XRD Analysis of Tris(2,2’-bipyridine)nickel(II) Trifluoroacetate

https://doi.org/10.22146/ijc.46483

Kristian Handoyo Sugiyarto(1*), Isana Supiah Yosephine Louise(2), Shinta Setya Wilujeng(3)

(1) Department of Chemistry Education, Universitas Negeri Yogyakarta, Jl. Colombo No. 1, Yogyakarta 55281, Indonesia
(2) Department of Chemistry Education, Universitas Negeri Yogyakarta, Jl. Colombo No. 1, Yogyakarta 55281, Indonesia
(3) Department of Chemistry Education, Universitas Negeri Yogyakarta, Jl. Colombo No. 1, Yogyakarta 55281, Indonesia
(*) Corresponding Author

Abstract


The complex containing Ni(II)-2,2’-bipyridin (bipy)-trifluoroacetate (TFA) was prepared by direct interaction of the corresponding precursors in an aqueous solution. AAS measurement for metal content, TGA-DTA analysis and electrical conductance suggest the ionic complex of [Ni(bipy)3](CF3COO)2·6H2O. The magnetic moment of 3.13–3.17 BM indicates the paramagnetism corresponding to two unpaired electrons which is clearly higher than that of the spin only value (2.87 BM), and commonly observed due to the spin-orbit coupling in Ni(II). UV-Vis spectral property revealed the first two main ligand field bands centered at about 14200 and 18650 cm–1, which are attributed to the spin-allowed transition, 3A2g→3T2g and 3A2g→3T1g(F), respectively. The expected third band at higher energy seems to appear as a shoulder at 26500 cm–1 (378 nm), as it is masked by a strong intensity of charge transfer band centered at 31050 cm–1. The infrared spectrum exhibits mode of vibrations of the functional groups of ligand and TFA. The powder diffractogram was refined by Le Bail method and found fit as monoclinic system of space group of P21/M, with figures of merit: Rp = 3.62, Rwp = 5.76, Rexp = 3.48, goodness of fitting (GOF) 2.745 and the derived Bragg R-Factor = 0.05.


Keywords


Rietica; Le Bail; bipy; trifluoroacetate; nickel(II)

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References

[1] Palmer, R.A., and Piper, T.S., 1966, 2,2’-Bipyridine complexes. I. Polarized crystal spectra of tris(2,2’-bipyridine)copper(II), -nickel(II), -cobalt(II), -iron(II), and -ruthenium(II), Inorg. Chem., 5 (5), 864–878.

[2] Prijamboedi, Z.B., Nugroho, A.A., and Ismunandar, 2009, Synthesis and structure analysis of aurivillius phases Pb1-xBi4+xTi4-xMnxO15, J. Chin. Chem. Soc., 56 (6), 1108–1111.

[3] Wallwork, K.S., Pring A., Taylor M.R., and Hunter B.A., 2003, A model for the structure of the hydrated aluminum phosphate, kingite determined by ab initio powder diffraction methods, Am. Mineral., 88 (1), 235–239.

[4] Wallwork, K.S., James, M., and Carter, M.L., 2006, The crystal chemistry, structure and properties of a synthetic carnotite-type compound, Ba2[UO2)2Ti2O8], Can. Mineral., 44 (2), 433–442.

[5] Zhu, J.H., Wu, H.X., and Le Bail, A., 1999, Structure of [Co(NH3)5CO3]NO3·H2O, Solid State Sci., 1 (1), 55–62.

[6] Sugiyarto, K.H., Saputra, H.W., Permanasari, L., and Kusumawardani, C., 2017, Structural analysis of powder complex of [Mn(phen)3](CF3SO3)2·6.5H2O, AIP Conf. Proc., 1847 (1), 040006.

[7] Kusumawardani, C., Permanasari, L., Fatonah S.D., and Sugiyarto, K.H., 2017, Structural analysis of powder complex of tris(1,10-phenanthroline) copper(II) trifluoromethane sulfonate dihydrate, Orient. J. Chem., 33 (6), 2841–2847.

[8] Kusumawardani, C., Kainastiti, F., and Sugiyarto, K.H., 2018, Structural analysis of powder complex of Cu(bipy)3(CF3SO3)2(H2O)x (x = 0.5, 1), Chiang Mai J. Sci., 45 (4),1944–1952.

[9] Sutrisno, H., Kusumawardani, C., Rananggana, R.Y., and Sugiyarto, K.H., 2018, Structural analysis of powder tris(phenanthroline)nickel(II) trifluoro acetate, Chiang Mai J. Sci., 45 (7), 2768–2778.

[10] Anonymous, Trifluoroacetic acid, http://www.commonorganicchemistry.com/Common_Reagents/Trifluoroacetic_Acid/Trifluoroacetic_Acid.htm, accessed on April 2019.

[11] Table of Acids with Ka and pKa Values, 2013, Compiled from Appendix 5 Chem 1A, B, C Lab Manual and Zumdahl 6th Ed., The pKa values for organic acids can be found in Appendix II of Bruice 5th Ed., https://www.chem.purdue.edu/docs/exams/ 2013/April_20_2013_cume.pdf, accessed on April 2019.

[12] Tokareva, A.O., Tereshchenko, D.S., Boltalin, A.I., and Troyanov, S.I., 2006, Acid Co(II) and Ni(II) trifluoroacetate complexes: Synthesis and crystal structure, Russ. J. Coord. Chem., 32 (9), 663-668.

[13] Reiß, G.J., and Meyer, M.K., 2010, Synthesis and structural characterization of diisopropylammonium trifluoroacetate and diisoproplyammonium penta fluoropropionate, Z. Naturforsch. B, 65 (4), 479–484.

[14] Agambar, C.A., and Orrell, K.G., 1969, Trifluoroacetate complexes of cobalt(II), nickel(II), and copper(II) with pyridine-type ligands. Part I. Metal(II) trifluoroacetates and copper(II) complexes, J. Chem. Soc. A, 0, 897–904.

[15] Angulo, I.M., Bouwman, E., Lok, S.M., Lutz, M., Mul, W.P., and Spek, A.L., 2001, The first low-spin nickel complex with two coordinated water molecules, [Ni(o-MeO-dppp)(H2O)2](PF6)2-synthesis and structural characterization, Eur. J. Inorg. Chem., 2001 (6), 1465–1473.

[16] Figgis, B.N., and Lewis, J., 1960, Modern Coordination Chemistry, Interscience, New York.

[17] Sugiyarto, K.H., Kusumawardani, C., Wigati, H., and Sutrisno, H., 2019, Structural study of the powder complex of Cu(II)-1,10-phenanthroline-trifluoroacetate, Orient. J. Chem., 35 (1), 325–331.

[18] Sugiyarto, K.H., Kusumawardani, C., Sutrisno, H., and Wibowo, M.W.A., 2018, Structural analysis of powdered manganese(II) of 1,10-phenanthroline (phen) as ligand and trifluoroacetate (TFA) as counter anion, Orient. J. Chem., 34 (2), 735–742.

[19] Chandra, S., and Sangeetika, X., 2004, EPR, magnetic and spectral studies of copper(II) and nickel(II) complexes of Schiff base macrocyclic ligand derived from thiosemicarbazide and glyoxal, Spectrochim. Acta, Part A, 60 (1-2), 147–153.

[20] Eloussifi, H., Farjas J., Roura P., Ricart S., Puig T., Obradors X., and Dammak M., 2013, Thermo analytical study of the decomposition of yttrium trifluoroacetate thin films, Thin Solid Films, 545, 200–204

[21] Laishram, N.S., 2012, Synthesis, characterization and thermal studies of copper(II) complexes of 2,2’-bipyridyl and 1,10-phenanthroline, J. Chem. Pharm. Res., 4 (9), 4400–4405.

[22] Singh, V.P., Singh, P., and Singh, A.K., 2011, Synthesis, structural and corrosion inhibition studies on cobalt(II), nickel(II), copper(II) and zinc(II) complexes with 2-acetylthiophene benzoyl hydrazone, Inorg. Chim. Acta, 379 (1), 56–63

[23] Ferenc, W., Walków-Dziewulska, A., Sarzynski, J., and Paszkowska, B., 2006, Magnetic, thermal and spectral properties of Ni(II) 2,3- , 3,5- and 2,6-dimethoxybenzoates, Eclet. Quím., 31 (3), 53–60.

[24] Mabbs, F.E., and Machin, D.J., 1973, Magnetism and Transition Metal Complexes, Chapman and Hall, London.

[25] Abramov, V., 2010, New nickel(II) complexes with N-donor ligands and anions as coligands. Structures and optical properties, Dissertation, Faculty of Mathematics and Natural Sciences, University of Cologne, Deutschland.

[26] Shad, H.A., Thebo, K.H., Ibupoto, Z.H., Malik, M.A., O’Brien, P., and Raftery, J., 2011, Synthesis, characterization, and crystal structure of a copper(II) complex of 1,10-phenanthroline and succinate, J. Coord. Chem., 64 (13), 2353–2360.

[27] Kumar, S.P., Suresh, R., Giribabu, K., Manigandan, R., Munusamy, S., Muthamizh, S., and Narayanan, V., 2014, Microwave synthesis of tris-(1,10-phenanthroline) manganese(II) complex and its electrochemical sensing property of catechol, Int. J. ChemTech Res., 6 (6), 3280–3283.

[28] Chen, H., Xu, X.Y., Gao, J., Yang, X.J., Lu, L.D., and Wang, X., 2006, Study on crystal structure of [Ni(phen)3](ClO4)2, Acta Phys. Chim. Sin., 22 (7), 856–859.

[29] Tosonian, S., Ruiz, C.J., Rios, A., Frias, E., and Eichler, J.F., 2013, Synthesis, characterization, and stability of iron (III) complex ions possessing phenanthroline-based ligands, Open J. Inorg. Chem., 3 (1), 7–13.

[30] Abdelhak, J., Cherni, S.N., and Zid, M.F., 2014, Synthesis, characterization, and crystal structure of new cobalt(III) complex: [Tris(1,10-phenanthroline-κ2N,N’) cobalt(III)] trinitrate monohydrate [Co(C12H8N2)3](NO3)3·H2O, Mediterr. J. Chem., 3 (1), 738–745.

[31] Zang, J., Wang, L.X., Zang, L., Chen, Y., and Zang, Q.T., 2013, Co-luminescence properties of terbium ions–benzoic acid–phen complexes doped with europium ions, Rare Met., 32 (6), 599–604.

[32] Skyrianou, K.C., Perdih, F., Turel, I., Kessissoglou, D.P., and Psomas, G., 2010, Nickel–quinolones interaction. Part 2 – Interaction of nickel(II) with the antibacterial drug oxolinic acid, J. Inorg. Biochem., 104 (2), 161–170.

[33] Suzuki, H., Takiguchi, T., and Kawasaki, Y., 1978, Synthesis and spectroscopy of acetato and dithiocarbamate complexes of bis(cyclopentadienyl)zirconium(IV), Bull. Chem. Soc. Jpn., 51 (6), 1764–1767.

[34] Osowole, A.A., Kolawole, G.A., and Fagade, O.E., 2008, Synthesis, characterization and biological studies on unsymmetrical Schiff-base complexes of nickel(II), copper(II) and zinc(II) and adducts with 2,2′-dipyridine and 1,10-phenanthroline, J. Coord. Chem., 61 (7), 1046–1055.

[35] Sinha, S.P., 1964, 2,2'-Dipyridyl complexes of rare earths. I: Preparation, infrared and some other spectroscopic data, Spectrochim. Acta, 20, 879–886.

[36] Lawrance, G.A., 1986, Coordinated trifluoro methanesulfonate and fluorosulfate, Chem. Rev., 86 (1), 17–33

[37] Crowder, G.A., and Jackson, D., 1971, Infrared and Raman spectra of methyl trifluoroacetate, Spectrochim. Acta, Part A, 27 (9), 1873–1877.

[38] Crowder, G.A., 1971, Infrared spectra of trifluoroacetate esters, J. Fluorine Chem., 1 (2), 219–225.

[39] Fan, L., Wei, P., Pang, S., and Zhang, X., 2010, Tris(2,2′-bipyridine)nickel(II) hexamolybdate, Acta Crystallogr., Sect. E: Struct. Rep. Online, 66 (9), m1119.

[40] Zhou, Y., Li, X., Xu, Y., Cao, R., and Hong, M., 2003, Tris(2,2′-bipyridine)nickel(II) diperchlorate, Acta Crystallogr., Sect. E: Struct. Rep. Online, 59 (5), m300–m302.

[41] Golovnev, N.N., Molokeev, M.S., Sterkhova, I.V., Lesnikov, M.K., and Samoilo, A.S., 2019, Structure of bis(2-thiobarbiturate)Tris (2,2-bipyridyl)nickel(II) hexahydrate, J. Struct. Chem., 60 (1), 111–116.

[42] Ruiz-Perez, C., Lorenzo Luis, P.A., Lloret, F., and Julve, M., 2002, Dimensionally controlled hydrogen-bonded nanostructures: Synthesis, structure, thermal, and magnetic behaviour of the tris(chelated)nickel(II) complex [Ni(bipy)3]Cl2·5.5H2O (bipy = 2,2’-bipyridyl), Inorg. Chim. Acta, 336, 131–136.

[43] Lin, S.H., Wang, Z.K., Zhang, B.H., Hu, H.M., and Huang, J.S., 2000, Crystal structure of tris(2,2′-bipyridine)nickel(II) tetrachlorozincate, Chin. J. Chem., 19 (2), 95–98.

[44] Toby, B.H., 2006, R factors in Rietveld analysis: How good is good enough?, Powder Diffr., 21 (1), 67–70.



DOI: https://doi.org/10.22146/ijc.46483

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