The crystal structure of a new member of the alkylammonium chloroantimonate
family, namely bis(ethyldimethylammonium) pentachloroantimonate(III), [C2H
2NH(CH3)(2)](2)[SbCl5], was determined at room temperature. The anionic sub
lattice consists of isolated distorted square-pyramidal [SbCl5](2-) units a
nd two crystallographically inequivalent disordered ethyldimethylammonium c
ations connected to anions by N-H ... Cl hydrogen bonds. The disorder is re
alised by the presence of two positions for all C, N and H atoms, and is ex
plained as being a result of the overall reorientation of cations along the
long axis of the molecule. One second-order phase transition was found at
ca 160 K and results in a lowering of the symmetry from orthorhombic to mon
oclinic or triclinic.