Synthesis, Solid State NMR and Powder X-Ray Diffraction Studies on Ethane-1,2-Dithiolatobismuth(III) Alkyl Dithiocarbonates

GRAPHICAL ABSTRACT

Abstract

Complexes of the type ethane-1,2-dithiolatobismuth(III) alkyl dithiocarbonate (SCH₂CH₂SBiS₂COR, where R = CH₃, C₂H₅, C₃H₇ⁿ, C₃H₇ⁱ, C₄H₉ⁿ, C₄H₉ⁱ) have been synthesized by the reaction of ethane-1,2-dithiolatobismuth(III) chloride with potassium alkyl dithiocarbonates in equimolar ratios by stirring at room temperature in a methanol/carbon disulfide mixture for ∼6h. All newly synthesized derivatives are dark brown solids and are insoluble in common organic solvents. These derivatives have been characterized by elemental analysis and spectroscopic (IR, Far-IR, solid state ¹³C NMR, and powder X-ray diffraction) studies. X-ray diffraction analysis provides basic material properties as crystal system, particle size, and different lattice parameters. Particle size obtained indicates nano-range features ranges from 4-nm to 88-nm size. Such small particle sizes introduce many peculiar characteristics and unique properties of the synthesized complexes. On the basis of all above studies, tentative structures of the complexes are proposed.

Keywords:

• Bismuth(III)
• dithiocarbonate
• dithiolate
• far-IR
• solid state NMR
• powder XRD

Notes

Benzene is a carcinogenic solvent! It was only used together with CH₂Cl₂ for the recrystallization of the complexes. All precautions were taken to prevent discharge/release of benzene.