Synthesis and Structural Characterization of Butane-1,4-diammonium sulphate

Abstract

The crystal structure of butane-1,4-diammonium sulphate, C4H14N2 2+ · SO4 2−, exhibits a unique packing arrangement where staggered pairs of butane-1,4-diammonium cations form infinite columns surrounded by sulphate anions. The disordered cation straddles the mirror plane and the asymmetric unit contains one half of the butane-1,4-diammonium cation and one half of the sulphate anion. The bond between C2b and C2a′ is twisted into a gauche conformation as a result of the charge-assisted hydrogen bonding between the doubly charged sulphate anion and the two singly charged ends of the cation chain. An intricate and extensive network of hydrogen bonds is formed within the crystal. Thermal analysis by DSC yielded no evidence of a phase change for the compound. Powder X-ray diffraction analysis yielded very good correlation between the observed and calculated powder pattern obtained from the single crystal data. Crystal data: crystal system, orthorhombic, a = 10.0496 (5) A, b = 9.4186 (4) A, c = 8.8987 (4) A, space group, Pnma, V = 842.29 (7) A3, Z = 4. Synthesis and Structural Characterization of Butane-1,4-diammonium sulphate C. van Blerk and G. J. Kruger Department of Chemistry, University of Johannesburg, 524, Auckland Park, Johannesburg, 2006, Republic of South Africa The structural characteristics of the title compound, which include the crystal structure by single crystal X-ray diffraction, description of the packing arrangement and intermolecular forces from the crystal structure, thermal analysis by differential scanning calorimetry and powder X-ray diffraction studies, are described in this work.