The Ni (I1) complexes of 1, 4, 7, 10, 13, 16-hexathiacyclooctadecane (1 8S6, hexathia-18- crown-6), 2, 5, 8-trithianonane, 1, 5, 9-trithiacyclododecane (1 2S3, trithia-l2-crown-3), and 1, 5, 9, 13, 17, 21-hexathiacyclotetracosane (2496, hexathia-24-crown-6) have been synthesized and characterized by single-crystal X-ray diffraction and electronic spectroscopy. Each of these complexes contains a high-spin [Ni (thi~ ether)~]~+ cation ...