Abstract
The first crystal structure of a 10.10.10 cryptand has been determined, during which an unusual single crystal phase transition was observed; at room temperature, crystals of macrobicycle 1d are monoclinic (α) but undergo a first-order topotactic phase change at 207 K to a triclinic (β) lattice; full structure determinations at 150 and 210 K were carried out and show that both phases adopt the in–in cryptand conformation.
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