Sains Ma1aysiana 27: 127-133 (1998) Sains Fizis dan Gunaan/ Physical and Applied Sciences
Kompleks Feniletanolditiokarbamat Daripada Logam Ni(H), Pb(H), Pd(H) dan Zn(H) (Complexes of phenylethanoldithiocarbamate from metals of Ni(H), Pb(H), Pd(H) and Zn(H))
Ibrahim Baba, Kamariah Muda, Yang Farina & Abdul Hamid Othman Pusat Pengajian Sains Kimia dan Teknologi Makanan Fakulti Sains dan Teknologi Universiti Kebangsaan Malaysia 43600 UKM Bangi Selangor D.E.
ABSTRAK
Kompleks jenis feniletanolditiokarbamat, M(S2CNR1R2)2 (M = Ni, Pb, Pd dan Zn; R1 = C6H5; R2 = C2H4OH) telah berjaya disintesiskan. Kompleks tersebut terbentuk hasil tindak balas N(2-hidroksietil)anilina, karbon disulfida dengan larutan akueus logam klorida dalam pelarut etanol atau metanol. Seperti kompleks metiletanol- dan dietanolditiokarbamat yang telah dilaporkan sebelum ini, kompleks feniletanolditiokarbamat juga tidak larut dalam pelarut organik biasa melainkan dalam DMSO. Analisis gravimetri dan CHNS/O menunjukkan nisbah logam-ligan adalah seperti yang dijangkakan. Kompleks feniletanolditiokarbamat juga telah dicirikan menggunakan spektroskopi inframerah, NMR (1H dan 3C) dan ultralembayung. Spektrum inframerah daripada kompleks tersebut menunjukkan jalur v(C=N+), v(C-S) dan v(C6H5) masing-masing wujud dalam kawasan 1416 - 1476, 1050 - 1063, dan 2955 - 3059 cm-1. Kehadiran kedua-dua jalur tersebut (v(C=N+) dan v(C-S)) mencadangkan bahawa ligan ditiokarbamat membentuk kelat dengan atom logam. Spektrum RMN l3C menunjukkan atom karbon dalam kumpulan NCS2 mempunyai anjakan kimia dalam julat 207.60 - 211.89 ppm. Manakala untuk RMN 1H didapati anjakan kimia proton kumpulan aromatik terletak pada kawasan 7.27 - 7.49 ppm. Serapan maksimum (λmax) yang terdapat dalam spektrum ultralembayung dan boleh nampak untuk keempat-empat kompleks menunjukkan wujudnya geometri segiempat mensatah.
ABSTRACT
Complexes of phenylethanoldithiocarbamate, M(S2CNR1R2)2 (M = Ni, Pb, Pd and Zn; R1 = C6H5; R2 = C2H4OH) have been successfully synthesised. The complexes were synthesised by the reaction of N(2-hydroxyethyl)aniline with carbon disulphide in ethanol or methanol with an aqueous solution of metal chlorides. As reported earlier for methylethanol or diethanoldithiocarbamate complexes, all the phenylethanoldithiocarbamate complexes were not soluble in normal solvents except for DMSO. Elemental (CHNS/O) and gravimetric analysis showed that the metal and ligand ratios conformed to the theoretical values. The complexes were also characterized using infrared, NMR (1H and 3C) and ultraviolet spectroscopy. The infrared spectra of the complexes showed the stretching bands of v(C=N+), v(C-S) and v(C6H5) in the regions of 1402 -1447, 1050 -1063, and 2955 - 3059 cm-1 respectively. The position of both v(C=N+) and v(C-S) bands suggested that the dithiocarbamate complexes form chelates with the metal atom. The 13C NMR spectra showed a peak in the range of 207.60 - 211.89 ppm attributed to the carbon atom in the NCS2 group. The 1H NMR showed the chemical shifts for aromatic group found in the areas of 7.27 - 7.49 ppm. Absorption peaks (λmax) found in ultraviolet and visible spectra of the complexes indicate square planar geometry.
RUJUKAN/REFERENCES
Bookhari, A., Hill, J. O. & Magee, R J. 1974. Nickel(II) and Copper(II) Complexes of Mono- ethanol and Di- ethanol Dithiocarbamaic Acid. J. Inorg. Nucl. Chem. 36: 1253-1257. Campbell, G. L., Ellis, G. D. & Chakrabarty, M. R. 1981. The Synthesis and Characterization of some Titanium(III) Tris N,N,-Dialkyldithiocarbamates. J. Inorg. Nucl. Chem., 43(10): 2265 - 2268. Chatt, J., Duncanson, L. A. & Venanzi, L. M. 1956. Electronic Structures of Dithiocarbamates and Xanthates. Nature 177: 1042-1043. Haas, W. and Schwarz, T. 1963. Diethanodithiocarbamate, a Reagent for the Spectro photometric Determination of Mo and U. Mickrochirn. Ichnoanal. Acta, 253-257. Ibrahim Baba, 1992. Kompleks Ditiokarbamat Logam Rutenium(II), Rhodium(II), Platinum(II) dan Paladium(II). J. Sains Malaysiana 21(2): 59-65. Ibrahim Baba, Yang Farina Abdul Aziz, Normah Awang & Jariah Abdullah. 1994. Kompleks Dietanolditiokarbamat Unsur Kumpulan 12. Laporan Teknik, FSFG. ke-7. 184-191. Ibrahim Baba, Yang Farina Abdul Aziz, Rahmah Mohamad, Normah Awang, Abdul Hamid Othman & Jariah Abdullah. 1995. Penyelidikan Sebatian Ditiokarbamat: Penilaian dan Pencapaian. Prosiding Seminar Kimia Bersama ITB-UKM Kedua. 53-64. Nomura, R, Fuji, S., Takabe, A. & Matsuda, H. 1989. Preparation of Novel Metal Dithiocarbamate Complexes Containing -OH group. Stabilization effect of the OH Group on the HNCS2-Mt Linkage. Polyhedron 8(15): 1891- 1896. Sharma, C. P., Kumar, N., Khandpal, M. c., Sharma, S. & Bhide, V. G. 1981. Studies on The Preparation and Characterization of Bis-Dithiocarbamato Derivatives of Di-n-butyl and Di-n-Hexyl Sn(lV). J. Inorg. Nucl. Chern. 43: 923-930. Thorn, G. D. & Ludwig, R A. 1962. The Dithiocarbarnates and Related Compounds, 7 - 56. Amsterdam: Elsevier.
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