All three isomers (ortho, meta, and para) of [8.8] cyclophane bearing 1, 6-dioxahexa-2, 4- diyne bridges have been synthesized and structually characterized by single-crystal X-ray crystallography to determine the conformation of the cyclophanes and their cavity dimensions. The three isomeric [6.6] cyclophanes bearing 1, 4-dioxabut-2-yne bridges have also been synthesized from but-2-yne-1, 4-diol ditosylate and the isomeric ...