A novel triangle-shaped macrocyclic complex, [(tmeda)Pt(azpy)](3)(PF6)(6)center dot 13H(2)O (tmeda: tetramethylethylenediamine, azpy: 4,4'-azopyridine) has been successfully synthesized via self-assembly of [(tmeda)PtCl2] with a bulky capping ligand, tmeda and flexible organic linker, azpy. (HNMR)-H-1 results show the realization of a triangle-shaped complex as a major component of the self-assembly. The single-crystal X-ray study shows its shape to be an equilateral triangle with ca. 2.1 um sides.