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Reactions of methylbismuth(III) dichloride with thiosemicarbazones (TSC) in 1:1 and 1:2 molar ratios in anhydrous methanol yield [MeBiCl 2 .n{RR’CNNHCSNH 2 }] [where, R=R’=CH 3  and n=1  (1)  or n=2  (2) ; R=C 6 H 4 OH, R’=H and n=1  (3)  or n=2  (4) ; R=C 5 H 4 N, R’=CH 3  and n=1  (5)  or n=2  (6) ]. These monomeric adducts have been characterized by elemental analyses, Fourier transform infrared, nuclear magnetic resonance [ 1 H,  13 C{ 1 H}] and fast atom bombardment mass spectrometry. The ligand appears to bind bismuth through sulfur and azomethine nitrogen atoms rendering penta- and hepta- coordination geometries, in  (1, 3  and  5)  and  (2, 4  and 6 ) , respectively, in the solution state. Low temperature (143–145°C) solvothermal transformation of  (3)  or  (4)  in refluxing xylene yields nano-structured flowers of amorphous bismuthinite (Bi 2 S 3 ). Prolonged (~10 h) sintering at 150°C of the powder obtained from  (4)  yielded one-dimensional micro/nanorods of orthorhombic Bi 2 S 3 . All the materials were characterized by X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray analyses.

main group metal chemistry

Synthesis and characterization of thiosemicarbazone derivatives of methylbismuth(III) dichloride: generation of one dimensional micro-rods of bismuthinite from [MeBiCl 2 ·n{(C 6 H 4 OH)CHNNHCSNH 2 }] by a solvothermal process