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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 19, Number 1
BKCSDE 19(1)
January 20, 1998 

Synthesis and Characterization of Aluminum and Gallium Complexes of Heterocyclic Thiosemicarbazones. Crystal Structures of Me2M[SC4H3CHNNC(S)SCH3] (M=Al, Ga)
Youngjin Kang, Seungjoo Kang, Byungwoo Yoo, Sang Ook Kang*, Jaejung Ko*
The synthesis and characterization of the monomeric group 13 heterocyclic thiosemicarbazone complexes Me2M[SC4H3CHNNC(S)SCH3] (M=Al (2), Ga (3)) are described. Compounds 2-3 were prepared using MMe3 (M=Al, Ga) in toluene with 2-thiophenecarboxaldehyde-S-methyldithiocarbazat e under anaerobic conditions. These complexes have been characterized by 1H NMR, 13C NMR, elemental analyses, and single-crystal X-ray diffraction. 2 crystallizes in the monoclinic space group P21/c with unit cell parameters a=10.2930(5) Å, b=18.564 (1) Å, c=7.3812(6) Å, V=1347.9(2) Å3, Dcalc=1.342 gcm-3 for Z=4, 9281 reflections with Io o), R1=0.0500 and wR2=0.0526. 3 crystalizes in the orthorhombic space group Pbca with unit cell parameters a=13.340(3) Å, b=19.9070(5) Å, c=11.3690(2) Å, V=2673.88(9) Å 3, Dcalc=1.511 gcm-3 for Z=8, 17004 reflections with Io < 3¥o(Io), R1=0.0480 and wR2=0.0524. Compound 3 is a monomeric gallium compound witha weak interaction between the pendant thiophene and the gallium center.
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