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The description of synthesis, characterization, spectral properties and solid state molecular structures of some new unsymmetrical alpha-aryltellurated ketonyl derivatives is the theme of this book. Electrophilic substitution of methylketones with aryltellurium trichlorides afforded aryl(acylmethyl)tellurium dichlorides, Ar(RCOCH2)TeCl2. The chosen aryl ligands viz. mesityl (2,4,6-Me3C6H2; Mes), 1-naphthyl (1-C10H7; Np) and anisyl (4-MeOC6H4; Anisyl) and methylketones with R = mesityl, t-butyl, i-propyl, ethyl possess varying steric and electronic effects and are known for their ability to cause various conformations and cell packing. These tellurium(IV) derivatives after reduction afforded unsymmetrical -aryl tellurated ketones, RCOCH2TeAr (R = Mes, t-Bu and i-Pr) in situ and were characterized by isolating their halogenated Te(IV) products. Attempts to isolate these arylalkyltellurium(II) compounds were successful for MesCOCH2TeMes, MesCOCH2TeNp and i-PrCOCH2TeMes, while in other cases decomposition resulted in Ar2Te2 and the parent ketones Shon. In Last Chapter we also deals with our efforts to explore Complexes of Mercury(II) Halides with ortho Aryltellurated Schiff Bases.