Structure and internal dynamics of N,N-diethylethylendiammonium pentachloroantimoniate(III)–N,N-diethylethylendiammonium dichloride

N,N-Diethylethylendiammonium pentachloroantimoniate(III)–N,N-diethylethylendiammonium dichloride (DEDA), chemical formula [(C2H5)2NH(CH2)2NH3][SbCl5][(C2H5)2NH(CH2)2NH3]Cl2, has been synthesized and characterized by the X-ray diffraction method at 293 K. It crystallizes in the orthorhombic space group Pnam with the following unit-cell dimensions: a = 9.9700(0), b = 10.8400(1), c = 23.6360(6) Å and Z = 4. The crystal structure consists of two N,N-diethylethylendiammonium cations, [SbCl5]2− anions and two isolated chloride ions. The anions, in which distorted [SbCl5]2− square pyramids share a common Cl− ion, are held together in infinite chains parallel to the a axis. These chains are themselves interconnected by N–H⋯Cl hydrogen bridge bonds. The dynamics of the proton and the molecular motion revealed dynamical phase transitions in the vicinity of 208 and 255 K.

Graphical abstractLayered crystal structure of N,N-diethylethylendiammonium pentachloroantimoniate(III)–N,N-diethylethylendiammonium dichloride.Calculated temperature dependence of the correlation times of: C3 fold reorientation of two methyl groups from subunit A (red line a) as well as from subunit B (blue line c), the C3 fold reorientation of the ammonia group from subunit B (dashed blue, line d), the [C6H18N2] cation reorientation around the pseudo C3 fold symmetry axis from subunit A (dashed red, line b) and subunit B (point blue, line e) of the studied sample.Figure optionsDownload full-size imageDownload as PowerPoint slide