The semisepulchrate type complexes Ni2+bisperchlorate tris(((aminoethyl)amino)methyl)amine and Ni2+perchloratechloride tris(((aminoisopropyl)amino)methyl)amine have been obtained and characterized by means of IR, Raman, UV-VIS and proton NMR study. Vibrational spectra have been interpreted on the basis of the deuteration and metal isotope shift data. The capping group vibrations were found near 890 cm−1, 630 cm−1and 470 cm−1. Crystal field parameters were estimated from the UV-VIS spectra. The Dq parameter equals 1232 cm−1for the first complex and 1224 cm−1for the second, Racah'a parameter B equals 767 cm−1and 787 cm−1respectively. The position of N(CH2)3capping group proton resonances were found to be in the region 161–159 ppm.