Malaysian
Journal of Analytical Sciences Vol 19 No 5 (2015): 935 - 941
SYNTHESIS,
STRUCTURAL, AND CHEMICAL PROPERTIES OF Nd(III) ISATIN
2-METHYL-3-THIOSEMICARBAZONE
(Sintesis,
Pengstrukturan dan Sifat Kimia Nd(III) Isatin 2-Metil-3-Tiosemikarbazon)
Nur Nadia
Dzulkifli, Yang Farina*, Bohari M Yamin
School
of Chemical Sciences and Food Technology,
Faculty
of Science and Technology,
Universiti
Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia
*Corresponding author: farina@ukm.edu.my
Received:
30 April 2015; Accepted: 28 August 2015
Abstract
Rare earth complexes can exhibit higher coordination numbers. The rare earth metal has the ability to form
a multitude of geometries and stereochemistries. Studies on rare earth
complexes with organic ligands have received considerable attention. Nd(Is2MeTSC)3 [Is2MeTSC= isatin
2-methyl-3-thiosemicarbazone] was synthesized by condensation method. The
compounds were structurally characterized by elemental analysis CHNS, FT-IR,
NMR and thermo-gravimetric analyses. The
elemental analyses for the compounds were in good agreement with the
theoretical values. The melting point of
the complex was higher than the ligand, as expected. The X-ray crystallographic structures for
Is2MTSC showed that in the solid state, the compound existed in the thione form
where the C=S bond length was shorter than a single bond C-S, which was 1.82
Å. Is2MTSC adopted an orthorhombic
system, a = 14.3434(9), b = 8.4242(5), c = 17.8518(11) Å and Z =
8. The FT-IR spectral data impled a
bidentate bonding of Is2MeTSC to Nd(III) ion through carbonyl oxygen and
azomethine nitrogen. Thermal analyses
(TGA) of the complex was carried out to confirm the final molecular structure
of the complex and to study its thermal stability. This study proves that the complex was formed
by the coordination of ligand to metal ion and that there was no coordinated
water.
Keywords: Nd(II),
thiosemicarbazone, isatin, thermogravimetric analysis
Abstrak
Sebatian kompleks nadir bumi boleh mempunyai nombor koordinatan yang
lebih tinggi. Logam nadir bumi berkeupayaan untuk membentuk pelbagai geometri,
stereokimia. Kajian terhadap sebatian kompleks nadir bumi dengan ligan organik
telah mendapat perhatian. Nd(Is2MeTSC)3 [Is2MeTSC= isatin
2-metil-3-tiosemiarbazon] telah disintesis dengan kaedah kondensasi. Kesemua sebatian telah dicirikan dengan
analisis unsur CHNS, FT-IT, NMR dan analisis termogravimetrik. Data analisis
unsur bagi sebatian adalah hampir sama dengan nilai teori. Takat lebur sebatian kompleks adalah lebih
tinggi daripada ligan seperti yang dijangkakan.
Struktur kristalografi sinar-X bagi Is2MTSC menunjukkan bahawa dalam
keadaan pepejal ligan wujud dalam bentuk tion di mana panjang ikatan C=S adalah
lebih pendek daripada ikatan tunggal C-S iaitu 1.82 Å. Is2MTSC menghablur dalam sistem ortorombik, a = 14.3434(9), b = 8.4242(5), c =
17.8518(11) Å dan Z = 8. Data
inframerah menunjukkan Is2MTSC bertindak sebagai ikatan bidentat dengan ion
Nd(III) melalui oksigen karbonil dan nitrogen azometin. Analisis terma (TGA) bagi kompleks telah
dilakukan untuk mengesahkan struktur akhir kompleks dan mengkaji kestabilan
haba. Kajian membuktikan bahawa
terdapatnya pengkoordinatan sebatian ligan dengan ion logam dan mengesahkan
bahawa tiada air yang terkoordinat.
Kata kunci: Nd(III),
tiosemikarbazon, isatin, termogravimetrik analisis
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