Metallo-tallysomycin (an anticancer drug metal complex) recognizes specific tumor cell, and noncovalently binds to DNA base pair to cleave sequence. Anticancer drug metal complexes, zinc- and cobalt-binding tallysomycins, were synthesized and purified in order to understand the functions of metal complexes. Complete exchangeable $^1H-NMR$ signal assignment was accomplished by optimal pH- and temperature-dependent $^1H-NMR$ studies. In addition, a recently developed NERD (2D NOESY-1-1 echo) experiment gave a detail structural feature which is useful for NMR-based solution state structure determinatin of complex. Results exhibit that nitrogen atoms of $eta$-aminoalanine, $eta$-hydroxyhistidine, imidazole, and pyrimidine ring are the metal binding sites with a Zn(Ⅱ) ion, whereas Co(Ⅲ) ion can bind to one and two equivalent of tallysomycin, respectively.