Malaysian Journal of Analytical Sciences Vol 21 No 3 (2017): 560 - 570

DOI: https://doi.org/10.17576/mjas-2017-2103-06

 

 

 

SYNTHESIS, STRUCTURAL, CHEMICAL PROPERTIES, AND ANTI-BACTERIAL SCREENING OF Sm(III) THIOSEMICARBAZONE COMPLEXES

 

(Sintesis, Struktur, Sifat-Sifat Kimia, dan Penyaringan Antibakteria bagi Kompleks Sm(III) Tiosemikarbazon)

 

Nur Nadia Dzulkifli1, 2*, Yang Farina1, Bohari M.Yamin1, Nazlina Ibrahim3

 

1School of Chemical Science and Food Technology, Faculty of Science and Technology

Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

2Department of Chemistry, Faculty of Applied Sciences,

Universiti Teknologi MARA, 72000 Kuala Pilah, Negeri Sembilan, Malaysia

3School of Biosciences and Biotechnology, Faculty of Science and Technology

Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

 

*Corresponding author: nurnadia@ns.uitm.edu.my

 

 

Received: 16 August 2016; Accepted: 12 March 2017

 

 

Abstract

Rare earth complexes can exhibit higher coordination numbers while rare earth metals have the ability to form a multitude of geometries with organic ligands. The ligands, [Sm(III) (4Acpy4MTSC)2(4H2O)Cl]Cl2 and [Sm(III) (4Acpy4ETSC)(5H2O)Cl2]Cl [4Acpy4MTSC = 4-acetylpyridine 4-methyl-3-thiosemicarbazone; 4Acpy4ETSC = 4-acetylpyridine 4-ethyl-3-thiosemicarbazone] have been synthesised by condensation method. The compounds were structurally characterised by elemental analysis (CHNS), molar conductivity, Fourier Transform Infrared (FT-IR), Nuclear Magnetic Resonance (NMR), Ultraviolet-Visible (UV-Vis), and Thermo-Gravimetric Analysis (TGA). The elemental analysis for the compounds were in a good agreement with the theoretical values. The molar conductivity of the complexes showed electrolyte behaviour and confirmed the presence of counter ions in the structures. The proposed structures of the compounds have been confirmed by NMR, UV-Vis, and TGA. Based on the analysis, the ligands were coordinated to the metal ions through azomethine N and thione S thus, producing bidentate complexes. From the TGA, it is confirmed that a few water molecules have coordinated with metal ions. The X-ray crystallographic structures for the 4Acpy4ETSC, the C=S bond length is shorter than the single bond C-S which is 1.82 Å. It shows that in the solid state, the ligand exists in the thione form. The 4Acpy4ETSC adopted a monoclinic system, a = 10.5922(7), b = 8.9597(6), c = 13.0407, Z = 4. In vitro antibacterial tests showed that the complexes have an effective inhibitory effect compared to the ligands because the presence of chloride ions, Cl- which caused the complexes to be more acidic, can inhibit bacterial growth.

 

Keywords:  thiosemicarbazone, samarium(III), antibacterial screening

 

Abstrak

Sebatian kompleks nadir bumi boleh wujud dengan nombor koordinatan yang lebih tinggi dan logam nadir bumi berkeupayaan membentuk pelbagai geometri dengan ligan organik.  Sebatian ligan, [Sm(III) (4Acpy4MTSC)2(4H2O)Cl]Cl2 dan [Sm(III) (4Acpy4ETSC)(5H2O)Cl2]Cl [4Acpy4MTSC = 4-asetilpiridin 4-metil-3-tiosemikarbazon; 4Acpy4ETSC = 4-asetilpiridin 4-etil-3-tiosemikarbazon] telah disintesiskan melalui kaedah kondensasi. Kesemua struktur sebatian telah dicirikan dengan analisis unsur (CHNS), kekonduksian molar, spektoskopi Inframerah Transformasi Fourier (FTIR), Resonans Magnet Nukleus (NMR), Ultralembayung-Sinar Nampak (UV-Vis), dan analisis termogravimetrik (TGA). Data analisis unsur bagi semua sebatian adalah hampir sama dengan nilai-nilai teori. Kekonduksian molar bagi sebatian kompleks menunjukkan sifat elektrolit dan membuktikan kehadiran ion pembilang dalam struktur sebatian. Struktur jangkaan bagi sebatian telah dibuktikan dengan NMR, UV-Vis, dan TGA. Berdasarkan kepada analisis, ligan berkoordinat dengan ion logam melalui N azometina dan S tion dengan menghasilkan sebatian kompleks bersifat bidentat.  Analisis TGA membuktikan kehadiran beberapa molekul air yang berkoordinat dengan ion logam.  Struktur kristalografi sinar-X bagi 4Acpy4ETSC, panjang ikatan C=S adalah lebih pendek daripada ikatan tunggal C-S iaitu 1.82 Å.  Ini menunjukkan bahawa dalam keadaan pepejal, ligan wujud dalam bentuk tion. 4Acpy4ETSC menghablur dalam sistem monoklinik, a = 10.5922(7), b = 8.9597(6), c = 13.0407, Z = 4. Ujian antibakteria in-vitro ke atas sebatian kompleks mempamerkan kesan perencatan yang lebih tinggi berbanding dengan ligan kerana kehadiran ion klorida, Cl- yang menyebabkan kompleks bersifat asid, boleh menghalang pertumbuhan bakteria.

 

Kata kunci:  tiosemikarbazon, samarium(III), penyaringan antibakteria

 

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