By reaction of 1,2,4-triazole (Htrz) and 1,3,5-benzenetricarboxylic acid (H(3)btc) ligands with copper salts under hydrothermal or solvothermal conditions, two new mixed-lig and Cu(II)-coordination polymers [Cu-5(btc)(2)(ipa)(2)(trz)(2)4(H2O4] (H2O)(2)) (1, H(2)ipa = isophthalic acid) and {[Cu-5(mu(3)-OH)(2)(trz)(2)(btc)(2)(DMF)(2)]} (2, DMF = N,N-dimethylformamide) with interesting structural diversity have been successfully prepared. The structures of compounds 1 and 2 have been fully analyzed via the powder X-ray diffraction (PXRD) measurements, elemental analyses and X-ray single crystal diffraction technology. With the aid of a reflux treatment, both polymers 1 and 2 could be prepared in nanoscale region. Moreover, we studied the anticancer activity of the two nanostructures on three human spinal tumor cells (OPM-2, MM1S and RPMI-8226) via the standard MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] assay.