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Journal : Indonesian Journal of Chemistry

Synthesis and Structural Analysis of Powder Complex of Tris(bipyridine)cobalt(II) Trifluoromethanesulfonate Octahydrate Kristian Handoyo Sugiyarto; Cahyorini Kusumawardani; Kristanti Eka Wulandari
Indonesian Journal of Chemistry Vol 18, No 4 (2018)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (539.372 KB) | DOI: 10.22146/ijc.26833

Abstract

The powder complex of tris(bipyridine)cobalt(II) trifluoromethanesulfonate octahydrate has been synthesized by direct interaction of the corresponding aqueous solutions (and drops of ethanol) of cobalt(II) nitrate, bipyridine, and potassium triflate. The yellow-orange powder produced was filtered off and allowed to dry on an aeration for characterization. AAS measurement showed the content of metal to be 6.06%, corresponding to the theoretical value of 6.06% in [Co(bipy)3](CF3SO3)2.8H2O. The analysis of conductance producing the charge ratio of cation to anion to be 2:1, confirms the formula. The magnetic moment, µeff, of this complex which was to be 4.5-4.9 BM, indicates that the complex is paramagnetic corresponding to the three unpaired electrons with a significantly orbital contribution. UV-Vis spectrum of the complex reveals the first band observed at about 11100 cm–1, which is associated with the spin-allowed transition, 4T1g → 4T2g. A distinct shoulder at only about 16100 cm–1 should be associated with the spin-forbidden transition of 4T1g → 2T2g,2T2g (G). The expected second and third bands which are associated with spin-allowed transitions of 4T1g → 4T1g(P) and 4T1g → 4A2g at higher energy were not well resolved. The infrared spectrum shows absorptions of the functional group of ligand which is influenced by the metal-ligand interaction in this complex. The powder XRD of this complex was refined using Le Bail method of Rietica program and found to be fit as monoclinic symmetry with a space group of C2/c.
Preparation and Powder XRD Analysis of Tris(2,2’-bipyridine)nickel(II) Trifluoroacetate Kristian Handoyo Sugiyarto; Isana Supiah Yosephine Louise; Shinta Setya Wilujeng
Indonesian Journal of Chemistry Vol 20, No 4 (2020)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (427.139 KB) | DOI: 10.22146/ijc.46483

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.
Preparation, Electronic Properties, and Powder-XRD Structure Analysis of 3,5-Bis(pyridin-2-yl)-H-1,2,4-triazoledichloridocopper(II) Kristian Handoyo Sugiyarto; Isti Yunita; Harold Andrew Goodwin
Indonesian Journal of Chemistry Vol 20, No 6 (2020)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.22146/ijc.55600

Abstract

Salt of [Cu(bptrzH)Cl2], (bptrzH = 3,5-bis(pyridin-2-yl)-H-1,2,4-triazole) has been prepared and characterized its electronic spectral and magnetic properties. This salt is paramagnetic with magnetic moment, μs, being 1.77–1.78 BM at 293 K, but decreased significantly with decreasing temperature to be 0.60–0.63 BM at 90 K, indicating antiferromagnetic nature. This is associated with Cu–Cu magnetic interactions at low temperatures, and suggests that the salt adopt an octahedrally polymeric structure. The electronic spectrum of this salt reveals a strong ligand field band centered at about 13,000 cm–1 and a very strong charge transfer absorption at about 23,000–24,000 cm–1. The spectrum is better resolved at lower temperature and this is parallel to the slight change in color from yellowish-green at room temperature to bright green at low temperature (90 K). The powder XRD of this complex was refined by Le Bail method of Rietica program and found to be fit as triclinic symmetry of space group PĪ with the figure of merit: Rp = 5.02; Rwp = 7.95; Rexp = 5.40; Bragg R-Factor = 0.05; and GOF = 2.166.
Synthesis of Powdered [Mn(bipy)3](CF3SO3)2·5.5H2O: The Physical Properties and Antibacterial Activity Kristian Handoyo Sugiyarto; Dwi Anggi Marini; Hari Sutrisno; Dyah Purwaningsih; Cahyorini Kusumawardani
Indonesian Journal of Chemistry Vol 23, No 1 (2023)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.22146/ijc.77565

Abstract

The synthesis of the complex containing manganese(II), bipyridine (bipy) as a ligand, and an anionic trifluoromethane sulfonate (triflate) is reported. The corresponding metal content, conductance, and DTG-TGA of the complex lead to the formula of [Mn(bipy)3](triflate)2·5.5H2O. The fully high-spin magnetic moment is observed, corresponding to five unpaired electrons in the metal ion. The electronic spectral bands suggest the three possible spin-forbidden transitions of the sextet to quartet states. The mode of vibrations of the IR spectrum supports the typical ring of bipy, and the triflate. The images of SEM-EDX indicate the presence of the corresponding elemental content and reflect the relatively high crystallinity, as it is evidenced in the profile of the corresponding powdered diffractogram. The refinement of powdered XRD following the Le Bail program suggests being structurally triclinic symmetry of P21/c. This complex shows inhibition of bacterial activity against S. aureus and E. coli.
Synthesis, Characterization, and Magnetic Properties of Iron(II) Complex with 2,6-Bis(pyrazol-3-yl)pyridine Ligand and Tetracyanonickelate Anion Fitriani Fitriani; Irma Mulyani; Djulia Onggo; Kristian Handoyo Sugiyarto; Ashis Bhattacharjee; Hiroki Akutsu; Anas Santria
Indonesian Journal of Chemistry Vol 23, No 4 (2023)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.22146/ijc.81625

Abstract

The complex containing iron(II), 2,6-bis(pyrazol-3-yl)pyridine (3-bpp) as ligand, and tetracyanonickelate as counter anion has been synthesized and characterized. The characterization data suggest the corresponding formula of [Fe(3-bpp)2][Ni(CN)4]·4H2O. Meanwhile, the SEM–EDX analysis image confirms the existence of all elements contained in the complex except the hydrogen atom. The infrared spectra exhibit vibration bands of the functional groups of 3-bpp ligand and [Ni(CN)4]−1 anion. From magnetic property measurement, the complex's molar magnetic susceptibility (XMT) value is 2.65 emu mol−1 K at 300 K, which contains about 75% high-spin state of the Fe(II) complex. Upon lowering the temperature, the XMT value gradually decreases around 1.37 emu mol−1 K at 13 K. It decreases sharply to about 0.73 emu mol−1 K at 2 K. These values reveal that Fe(II) complex is in the low-spin (LS) state. As a result, the complex exhibited spin-crossover characteristics of gradual transition without thermal hysteresis, and the transition temperature occurred below room temperature with a transition temperature (T1/2) close to 140 K. The spin crossover property of the complex is supported by a thermochromic reversible color change from red-brown at room temperature to dark brown on cooling in liquid nitrogen associated with the high-spin to low-spin transition.