Macrocycles containing heteroatom donors have long been used to study the coordination of transition-metal ions, model metallo-protein active sites, and, more recently, develop inorganic co-ordination polymers. Cyclononane macrocycles possessing N, O, or S donors, or some combination of two of these heteroatoms, have been well-studied. We have developed a synthesis of a cyclononane ligand bearing N, O, and S donor atoms in the same macrocycle. The synthesis of this novel [9]aneNOS, and an [18]aneN₂O₂S₂ byproduct, along with evidence of binding to transition metals, will be presented.