Synthesis and characterization of some methylbismuth (III) O , O ‐alkylenedithiophosphates: convenient transformation of and to pure Bi 2 S 3

A series of methylbismuth(III) O , O ‐alkylenedithiophosphates of the type [where G = CH 2 CH(CH 3 ) ( 1 ), (CH 2 ) 4 ( 2 ), CH 2 CH 2 CH(CH 3 ) ( 3 ), CH(CH 3 )CH(CH 3 ) ( 4 ), CH 2 CHCH 2 CH 3 ( 5 ), CH(CH 3 )CH 2 C(CH 3 ) 2 ( 6 ) and C(CH 3 ) 2 C(CH 3 ) 2 ( 7 )] have been isolated by the reaction of methylbismuth(III) dichloride with potassium salt of O , O ‐alkylenedithiophosphoric acids in 1:2 molar ratio in anhydrous benzene. These newly synthesized derivatives were characterized by elemental analyses, FT IR and multinuclear NMR ( 1 H, 13 C and 31 P) spectral studies. Thermogravimetric analysis of 6 has shown a single‐step decomposition of complex to Bi 2 S 3 at 154.3 °C. Transformation of 2 and 6 to pure Bi 2 S 3 was carried out successfully at refluxing xylene temperature (142 °C) as revealed by XRD and SEM analyses. Copyright © 2006 John Wiley & Sons, Ltd.