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Single crystals of the high-temperature modification of RhSn 4  were obtained from a tin flux (1:20 molar ratio; final annealing at 920 K; dissolution of the tin matrix in 2N HCl). The structure was refined from single-crystal X-ray diffractometer data:  I 4 1 / acd ,  a =629.73(5),  c =2288.36(18) pm,  wR 2=0.0382, 447  F  2  values and 14 variables.  β -RhSn 4  is isotypic with  β -IrSn 4 . The rhodium atoms have slightly distorted square-antiprismatic tin coordination with Rh–Sn distances of 4×273.4 and 4×274.1 pm. The RhSn 8  units are condensed via common edges to layers that are staggered with respect to each other and stacked in ABCD sequence. A  119 Sn Mössbauer spectroscopic characterization of  ß -RhSn 4  and the stannides RhSn 3  and  α -RhSn 4  shows the typical isomer shifts for transition metal stannides. Only for  α -RhSn 4  the three crystallographically independent tin sites could be resolved, a consequence of the different  s -electron density. Treatment of  α -RhSn 4  under high-pressure (up to 10 GPa)/high-temperature (up to  T =1370 K) conditions leads to decomposition into Rh 1.5 Sn, RhSn 2  and  β -Sn.

RhSn 3 and the Modifications of RhSn 4 – Structure and 119 Sn Mössbauer spectroscopic characterization