6) have been prepared and characterized by elemental analysis, IR, 1 H, 13 C NMR, HSQC, HMBC and UV-Vis absorption spectra. For the heteroleptic complexes, the thiocyanide n C-N values were shifted to higher wavenumbers and NCS 2 carbon signals were shifted downfield compared to that of homoleptic complexes, suggesting the increased strength of the thioureide bond due to the presence of p-accepting phosphine. Electronic spectral studies suggest square-planar geometry for the complexes. Complex 5 was also characterized by X-ray diffraction techniques and presents a distorted NiS 2 PN square planar configuration around the Ni atom. Rare C-HÁ Á ÁNi intramolecular short contact interactions were observed in the complex 5.The ability of representative complexes 1 and 2 to sense anions (F À , Cl À , Br À and I À ) was examined by UV-Vis absorption spectra and cyclic voltametric titration studies. These studies show that both the complexes prefer to bind with I À . Complex 2 has been used as a single source precursor for the preparation of nickel sulfide and nickel oxide nanoparticles. The as-prepared nickel sulfide and nickel oxide nanoparticles have been characterized by PXRD, SEM, EDAX, TEM, HRTEM, UV-Vis and Photoluminescence spectroscopy. X-ray diffraction analysis showed the presence of three phases (cubic-NiS 2 , cubic-Ni 3 S 4 and rhombohedral-Ni 3 S 2 ). TEM images of nickel oxide revealed that the particles are spherical in shape with diameter B30 nm.