Sains Malaysiana 38(2): 185-190(2009)

Synthesis And Structural Studies Of Lanthanum(Iii)

Dialkyldithiocarbamates 1,10-Phenantroline

(Sintesis Dan Kajian Struktur Lantanum(Iii) Dialkilditiokarbamat

1,10 Fenantrolin)

Ibrahim Baba, Indah Raya & Bohari Mohd Yamin

School of Chemical Sciences & Food Technology

Faculty of Science and Technology, Universiti Kebangsaan Malaysia

43600 Bangi, Selangor, Malaysia

Received:  4 April 2008 / Accapted:  4 April 2008

ABSTRACT

A new series of lanthanum dialkyldithiocarbamate complexes with 1,10-phenantroline were successfully synthesized using in situ methods. These complexes were characterized using elemental analysis, infrared, thermogravimetric analysis and conductivity. Microelemental analysis data were in agreement with the general formula La(S₂CNR’R”)₃phen (R’ = ethyl, methyl; R” = butyl, heptyl, isopropyl, isobutyl, benzyl and cyclohexyl; phen = 1,10-phenantroline). Infrared spectra of complexes showed the thioureide n(C-N) bands were in the region of 1450 - 1482 cm^-1. The single n(C-S) bands appeared in the region of 959 – 997 cm^-1 and n(C-H) bands in the region of 2918-2955 cm^-1. The crystal structure of tris(N,N-ethylbenzyldithiocarbamate)(1,10-phenantroline)lantanum(III) adopts an orthorombic system (space group Pccn) with a distorted dodecahedron geometry with a = 19.865(5) Å ,  b = 42.803(10) Å, c = 10.657(3) Å, a = b = g = 90^o and Z = 9. Three dithiocarbamates and one phenanthroline ligands were coordinated to the central La atom in bidentate manner.

Keywords: Crystal structure; dithiocarbamate; lanthanum

ABSTRAK

Satu siri baru kompleks lantanum dialkilditiokarbamat dan 1,10-fenantrolin telah berjaya disintesis secara in-situ. Kompleks telah diciri dengan analisis unsur, spektroskopi inframerah, analisis termogravimetri dan pengukuran konduktiviti. Hasil analisis  unsur menunjukkan formula umum adalah La(S₂CNR’R”)₃phen (R’ = metil, etil; R” = butil, heptil, isopropil, isobutil, benzil dan sikloheksil; phen = fenantrolina). Spektrum inframerah kompleks menunjukkan jalur tioureida n(C-N) berada di sekitar 1450-1482 cm^-1. Manakala jalur tunggal n(C-S) pula berada di kawasan 959-997 cm^-1 dan jalur n(C-H) berada di kawasan 2918-2957 cm^-1. Struktur hablur tris(N,N-etilbenzilditiokarbamat)(1,10-fenantrolin)lantanum(III) dengan sistem hablur ortorombik (kumpulan ruang Pccn) dengan geometri dodekahedron terherot dengan a = 19.865(5) Å,  b = 42.803(10) Å, c = 10.657(3) Å, a = b = g = 90^o dan Z = 9. Tiga molekul ditiokarbamat dan satu molekul fenantrolina membentuk ikatan kelat kepada atom La secara bidentat.

Kata kunci: Ditiokarbamat; lantanum; struktur hablur

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