Eighteen new mono-organotin dithiocarbamate compounds derived each nine from methyltin(IV) and phenyltin(IV) reacted using in-situ method with various type of N-dialkylamine together with carbon disulphide with the ratio of 1:3:3. Elemental and gravimetric analysis showed that the general formula of these compounds were RSnCl[S2CNR′R″]2 (R= Ph, CH3, R′ = CH3, C2H5, C7H7 and R″ = C2H5, C6H11, iC3H7, C7H7). These compounds had been characterized by infrared spectroscopy, ultraviolet spectroscopy, 1H, 13C NMR spectroscopy and single crystal X-ray crystallography. The infrared spectra of these compounds showed three important peaks indicating the formation of dithiocarbamate compounds, ν(C N), ν(C S) and ν(Sn-S) band which present in the region of 1444–1519, 954–1098 and 318–349 cm−1 respectively. The ultraviolet-visible spectra showed an absorption band...