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Seven mixed arsenic(III) bis (dimethyldithiocarbamato) derivatives of type [(CH 3) 2 NCS 2 ] 2 AsL where, L = OOCC 6 H 5 , OOCCH 3 , OOCC 6 H 4 (OH), SC 6 H 5 , SCH 2 COOH, SOCCH 3 and S(C 6 H 4)COOH have been synthesized and characterized by various physicochemical [elemental analysis (C, H, N, S & As), molecular weight and melting point determinations], spectral [UV–Vis., FTIR, NMR (1H and 13C)], thermal [TGA and DTG], powder XRD studies. The presence of FT-IR band at 1064–1095 cm−1 due to thiocarbonyl moity and 13C NMR signal in the range 192.56–198.59 ppm due to -NCS 2 carbon resonance have indicated anisobidentate mode of bonding of dithiocarbamate group, alongwith this FT far-IR bands observed due to the υ(As–O) and υ(As–S) vibrations in the region 530–532 cm−1 and 302–333 cm−1 respectively, confirm the bonding of arsenic(III) to oxygen and sulfur. Thus, on the basis of results obtained by above spectral techniques, it may be concluded tentatively that, arsenic(III) derivatives (compound 1–7) adopted a distorted octahedral geometry with lone pair of electrons occupying one of the corner of octahedra. Powder XRD studies revealed that these derivatives have nano ranged particle size (5.72 and 16.29 nm) with lower symmetry (monoclinic) crystal system along with unit cell volume (1731 and 1764 Å3). Thermal studies reveal that arsenic(III) bis (dimethyldithiocarbamato) thiosalicylate (compound 7) gives arsenic sulfide as a final decomposition product, which have various potential applications. Antimicrobial screening test showed enhanced activity than free ligands and standard drugs. Seven type of arsenic(III) bis (dimethyldithiocarbamato) derivatives have been synthesized and structure of the derivatives have been tentetively proposed on the basis of spectral studies. Along with these, Powder XRD, thermal and biological studies have also been performed. These derivatives give arsenic sulfide as a final remaining product which have many potential applications and due to nano particle size of the derivatives, these exhibited enhanced antimicrobial activities (greater zone of inhibition) as compared to the free ligands and standard drugs. Image 1 • Mixed arsenic(III) bis(dimethyldithiocarbamato) derivatives with oxygen and sulfur donor ligands. • These derivatives have distorted octahedral geometry with nano-ranged crystallite size and monoclinic crystal system. • Arsenic(III) bis (dimethyldithiocarbamato) benzoate shows low intensity M+ ion peak at 435.2 m / z with base peak at 315.2 m / z. • These derivatives have shown equal and greater antimicrobial activities than the free ligand and standard drugs. [ABSTRACT FROM AUTHOR]