Abstract Triphenylarsenic(V) mixed ligand derivatives; [(R 1 )(R 2 )C=NO] 2 [Ph] 3 As[S 2 CN(CH 2 CH 2 ) 2 O] (1 A‐1F) were synthesized [Where R 1 =−C 6 H 5 , R 2 =−CH 3 ( 1 A ); R 1 =−C 6 H 4 CH 3 , R 2 =−CH 3 ( 1 B ); R 1 =−C 6 H 4 Cl, R 2 =−CH 3 ( 1 C ); R 1 =−C 6 H 4 Br, R 2 =−CH 3 ( 1 D ); R 1 =−C 6 H 4 OH, R 2 =−H( 1 E ); R 1 (R 2 )C=C−CH 2 −(CH 2 ) 3 −CH 2 ( 1 F )] by consecutive substitution of Ph 3 AsBr 2 with sodium salt of substituted oximes and morpholinedithiocarbamate in equimolar proportion. Distorted octahedral geometry was proposed around the arsenic atom, for these derivatives. Nano ranged particle size ∼35 nm with crystalline nature was obtained by powder XRD study for these derivatives. The derivatives were examined for bacteria and fungi which exhibited higher antifungal capability than antibacterial. Cytotoxic and antioxidant activities were performed through MTT test in 3T 3 fibroblast cell lines and by FRAP assay, respectively for these derivatives. Amongst six triphenylarsenic(V) mixed ligand derivatives, 1 A , 1 B and 1 C were observed non‐noxious (cell viability >50 % even at 500 μg/mL) in nature and 1 D , 1 E and 1 F were poisonous to 3T 3 fibroblast cell lines. Structural‐Activity relationship for antimicrobial and antioxidant activity amongst six derivatives 1 A – 1 F was explored.