Abstract
Single crystal X-ray diffraction, 35Cl nuclear quadrupole resonance (NQR) and differential scanning calorimetry (DSC) measurements were taken for bis(pyrrolidinium) hexachlorometallates, (C4H8NH2)2MCl6 (M=Sn, Te and Pt). A solid–solid phase transition was observed at 150(1), 159(1) and 134(1)K for stannate, tellurate and platinate, respectively. 35Cl NQR signals were observed in stannate and platinate, both of which showed a two-line spectrum in the high-temperature phase and a three-line spectrum in the low-temperature phase. The high-temperature phases of the three complexes were found to be isostructural with each other belonging to the space group C2/m (#12). The C4H8NH2+ and MCl62− ions are connected by N–H⋯Cl hydrogen bonds forming parallel sheets in the crystals. Disorder of the cation ring appears in these high-temperature phases. Semi-empirical MO calculations were performed to estimate the stable structure of the pyrrolidinium ion.
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