Structure and polymorphism of the 10.10.10 Simmons and Park cryptandElectronic supplementary information (ESI) available: experimental details of the crystal structure determinations, orientation and phase transformation matrices and diagram of the unit cells of α- and β-1d. See http://www.rsc.org/suppdata/cc/b0/b008044f/

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.