Sains Malaysiana 31: 101-108 (2002)                                                                           Sains Fizis dan Gunaan /

                                                                                                                                                Physical and Applied Sciences

Synthesis and Characterizations of Ethylbutyldithiocarbamate Compounds: Crystal Structure of Bismuth(III)

Ethylbutyldithiocarbamate

Karimah Kassim, Ibrahim Baba, Yang Farina,

Abdul Hamid Othman & H.K. Fun

Pusat Pengajian Sains Kimia dan Teknologi Makanan

Fakulti Sains dan Teknologi

Universiti Kebangsaan Malaysia

43600 UKM Bangi, Selangor Malaysia

 ABSTRACT

A new series of ethylbutyldithiocarbamate compounds have been synthesized. The compounds made of Zn(II), Cu(II), Ni(II), Pb(II), Sb(III) and Bi(III) were prepared by reacting the respective metal salts with ethylbutylamine and carbon disulphide using "in situ" method. Results of elemental analysis showed that the isolated compounds have the general formula, M[S₂CNR₁RZ₂]_n (n = 2; M = Zn(II), Cu(II), Ni(II), Pb(II), and n = 3; M = Sb(III) and Bi(III)). Infrared spectra of the compounds showed the thioureido v(C-N) bands in the regions 1468 – 1497 cm^-1.  The (C-S) bands appeared in the region 956 – 997 cm^-1  while the v(M-S) bands appeared in the region 300 – 400 cm^-1.  The ¹H NMR signals indicated ethyl- and butyl- in the region 0.40 – 3.85 ppm.  The 13C NMR spectra of zinc(II) and lead(II) showed a resonance in the region 202.0 ppm, which attributed to the carbon atom of NCS₂ group.  Tris(N-ethyl-N-butyldithiocarbamato-S) bismuth(III) is pentagonal pyramid distorted with triclinic system with P1, a = 10.5120(1)Å, b = 10.5128(1)Å, b = 10.5128(1)Å, c = 14.5755(1)Å, α = 99.927(1)^o, γ = 103.3383(1) and Z = 2.

ABSTRAK

Kompleks etilbutilditiokarbamat telah berjaya disintesis. Zinke(II), nikel(II), kuprum(II), plumbum(II), stibium(III) dan bismuth(III) etilbutilditiokarbamat disintesis dengan tindak balas secara stoikiometri sebatian garam logam di atas dengan etibutilamina dan karbon disulfida menggunakan kaedah in situ dalam larutan etano1. Analisis unsur dan gravimetri menunjukkan setiap kompleks ditiokarbamat mempunyai formula yang dijangkakan, iaitu M[S₂CNR₁R₂]n (di mana n = 2; M = zink, kuprum, nikel, plumbum dan n = 3; M = stibium, bismuth). Analisis spektroskopi inframerah kompleks etilbutilditiokarbamat menunjukkan serapan pada julat 1468 - 1497 cm^-1 hasil daripada regangan tioureida v(C-N) dan serapan pada julat 956 - 997 cm^-1 adalah hasil daripada regangan ikatan v(C=S). Kompleks ini memberikan julat serapan pada 300 - 400 cm^-1 hasil daripada regangan v(M-S). Analisis ¹H RMN bagi kompleks etilbutilditiokarbamat menunjukkan resonans proton bagi kumpulan etil- dan butil- dalam julat 0.40 - 3.85 ppm. Analisis ¹³C RMN bagi sebatian zink(II) dan plumbum(II) menunjukkan puncak N¹³CS₂ berada dalam kawasan anjakan kimia 202.0 ppm. Kompleks Tris(N-etil-N­butilditiokarbamato-S) bismuth(III) berstruktur piramid pentagon terherot dengan sistem triklinik dengan P(1, a = 10.5120(1)Å., b = 10.5128(1)Å., c = 1'4.5755(1)Å., α = 99.713(1)^o, β = 99.927(1) ⁰, γ = 103.3383(1)° dan Z = 2.

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