Sains Malaysiana 39(1)(2010): 45–50

Kompleks Praseodimium Ditiokarbamat 1,10 Fenantrolin

(Praseodymium Dithiocarbamate 1,10 Phenantroline Complexes)

IbrahimBaba* & Indah Raya

Pusat Pengajian Sains Kimia dan Teknologi Makanan

Fakulti Sains dan Teknologi, Universiti Kebangsaan Malaysia

43600 Bangi, Selangor D.E., Malaysia

Received: 30 March 2009 / Accepted: 22 June 2009

ABSTRAK

Tujuh kompleks praseodimium (Pr) ditiokarbamat 1,10-fenantrolin baru telah berjaya disintesis menggunakan kaedah in-situ hasil daripada tindak balas lapan jenis amina dengan garam praseodimium(III) bersama dengan karbon disulfida. Kaedah metatesis dan kondensasi merupakan kaedah yang paling berjaya telah menghasilkan praseodimium ditiokarbamat 1,10 fenantrolin dengan formula umum Pr[S2CNR1R2]3phen (R1 = etil dan metil; R2 = butil, heptil, isopropil, isobutil, benzil dan sikloheksil; phen= 1,10-fenantrolin). Kesemua kompleks telah dicirikan menggunakan kaedah analisis unsur, inframerah, termogravimetri dan konduktiviti. Analisis unsur telah menunjukkan kesemua kompleks bersetuju dengan formula umum yang dicadangkan. Spektrum inframerah (FTIR) menunjukkan jalur tioureda v(C-N) terletak dalam kawasan julat 1454 – 1484 cm-1 dan jalur ν(C-H) pula terletak dalam kawasan 2853-2973 cm-1. Jalur v(C-S) yang wujud secara tunggal dalam kawasan 959 – 999 cm-1 mengesahkan ia berikatan secara bidentat. Data spektroskopi NMR 13C moeti NCS2 untuk kesemua kompleks terletak dalam julat 192 – 212 ppm. Struktur hablur tunggal Pr[S2CN(CH3)(C7H7)]3phen mempunyai sistem hablur triklinik (kumpulan ruang Pī) dan geometri dodekahedron dengan a = 10.7165(16) A , b = 12.2897(19) A, c = 16.586(2) A, α = 73.887(2)o; β = 74.879(2)o dan γ = 71.837(2)o and Z = 2. Tiga ditiokarbamat dan satu ligan fenantrolin telah berkoordinat kepada atom Pr di pusat secara bidentat.

Kata kunci: 1,10-fenantrolin; ditiokarbamat; praseodymium

ABSTRACT

Seven promethium (Pr) complexes with 1,10-phenantroline were successfully synthesized using in situ methods from the reactions of eight amines with praseodymium(III) salts together with carbon disulphide. Methatesis and condensation were the most successful methods to prepare praseodymium dithiocarbamate 1,10-phenantroline complexes with general formula Pr[S2CNR1R2]3phen (R1 = ethyl, methyl; R2 = butyl, heptyl, isopropyl, isobutyl, benzyl and cyclohexyl; phen= 1,10-phenantroline). These complexes were characterized using elemental analysis, infrared, thermogravimetric analysis and conductivity. Microelemental analysis data were in agreement with the general formula. Infrared spectra of complexes showed the thioureide ν(C-N) bands were in the region of 1454 - 1484 cm-1 and ν(C-H) bands in the region of 2853-2973 cm-1. The single ν(C-S) bands appeared in the region of 959 – 999 cm-1 has proved to be bidentate bonding. The 13C NMR spectroscopic data for these complexes showed that the carbon signal from NCS2 moiety were in the range of 192 – 212 ppm. The crystal structure of Pr[S2CN(CH3)(C7H7)]3phen adopts triclinic system (space group Pī) with a distorted dodecahedron geometry with a = 10.7165(16) A , b = 12.2897(19) A, c = 16.586(2) A, α = 73.887(2)o, β = 74.879(2)o and γ = 71.837(2)o and Z = 2. Three dithiocarbamates and one phenanthroline ligands were coordinated to the central Pr atom in bidentate manner.

Keywords: 1,10-phenantroline; dithiocarbamate; praseodymium

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*Corresponding author; email: aibi@ukm.my