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Structural Analysis of Powder Tris(phenanthroline) nickel(II) Trifluoroacetate


Paper Type 
Contributed Paper
Title 
Structural Analysis of Powder Tris(phenanthroline) nickel(II) Trifluoroacetate
Author 
Hari Sutrisno, Cahyorini Kusumawardani, Rifai Yusuf Rananggana and Kristian Handoyo Sugiyarto
Email 
sugiyarto@uny.ac.id
Abstract:
The powder complex of tris(phenanthroline)nickel(II) trifluoroacetate has been synthesized by interaction of the corresponding nitrate salt in an aqueous solution and slightly excess of 1,10-phenanthroline in water/ethanol, whereupon the precipitate was produced on addition of an excess of saturated sodium trifluoroacetate solution while reducing the solvent. AAS measurement showed the content of metal to be 6.43 % being relatively close to the corresponding theoretical value of 6.60 % masss in [Ni(phen)3](CF3COO)2.3.5H2O. Moreover, the TGA confirmed the lost of 6.943% mass of complex corresponding to 3.43 H2O. The analysis of conductance producing the charge ratio of cation by anion to be 2:1, clearly fonfirms the formula. The magnetic moment, meff, of this complex which was to be 3.19-3.31 BM, indicates that the complex is paramagnetic corresponding to two unpaired electrons which is clearly higher than the spin only value (2.87 BM) due to the spin-orbit coupling. UV-Vis spectrum of the complex revealed the first two main ligand field bands observed at about 12700 and 19250 cm-1, which are associated with the spin-allowed transition, 3A2g ® 3T2g and 3A2g ® 3T1g(F), respectively. The expected third band at higher energy was not well resolved due to the masked strong intensity of charge transfer band. The infrared spectrum shows absorptions of functional group of ligand which is influenced by the metal-ligand interaction in this complex. The powder XRD analysis of this complex was refined using Rietica-Le Bail method (within cycle number of 75) and found to be fit as monoclinic crystal system with space group of P21/M, and cell parameters of a = 12.8182 , b = 30.8076 , c = 16.7725 , a = 90°, b = 88.7349°, g = 90°, V = 6621.8145 3, Z=4, with figure of merit: Rp = 1.7, Rwp = 4.08 and Rexp = 0.32. The goodness of the fitting (GOF = 167.4) was also reflected by the derived Bragg R-Factor of 0.06. 
Start & End Page 
2768 - 2778
Received Date 
2018-01-15
Revised Date 
Accepted Date 
2018-02-12
Full Text 
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Keyword 
Rietica, Le Bail, phen, trifluoroacetate, nickel(II)
Volume 
Vol.45 NO.7 (November 2018)
DOI 
Citation 
Sutrisno H., Kusumawardani C., Rananggana R.Y. and Sugiyarto K.H., Structural Analysis of Powder Tris(phenanthroline) nickel(II) Trifluoroacetate , Chiang Mai J. Sci., 2018; 45(7): 2768-2778.
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Vol.37 No.2 (MAY 2010) View: 632 Download:211
In vitro Antioxidant Activity of Vitex negundo L. Leaf Extracts
page: 489 - 497
Author:Raghavendra H. Lakshmanashetty, Vijayananda B. Nagaraj, Madhumathi G. Hiremath and Vadlapudi Kumar
Vol.37 No.3 (SEPTEMBER 2010) View: 630 Download:368
Partial Characterization of a New Peptide from Ivorian Red Onion that Inhibits Polyphenol Oxidase and Enzymatic Browning of Edible Yam (Dioscorea cayenensis-rotundata cv LongbÔ )
page: 464 - 475
Author:Sophie N. Gnangui , Sebastien L. Niamke and Lucien P. Kouame
Vol.37 No.3 (SEPTEMBER 2010) View: 558 Download:211
Dioxouranium(VI) Complexes of Some Bivalent Tridentate Schiff-base Ligands Containing ONS Donor Set
page: 443 - 450
Author:Didarul A. Chowdhury, Mohammad N. Uddin, and Farhana Hoque
Vol.37 No.3 (SEPTEMBER 2010) View: 572 Download:257



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