Three Zn(II)/Co(II) coordination compounds with condensed heterocyclic based 1,2,4-triazole 8H-4, 7-diphenyl-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazines (L 1 ), and 8H-4-phenyl-7-(pyridine-2-yl)-1,2,4-triazolo[3,4-b]-1,3, 4-thiadiazines (L 2 ), Co(L 1 ) 2 Cl 2 (1), Zn(L 1 ) 2 Cl 2 (2). and Co(L 2 ) 2 Cl 2 (3) were synthesized and structurally characterized by elemental analyses, IR spectroscopy and single-crystal X-ray diffraction. Complexes 1, 2 and 3 have mononuclear structure, the mononuclear structures of 1 and 2 were further assembled by the C-H_Cl and C-H_N weak interactions into an infinite 2-D supramolecular sheet.