Abstract
Metastable palladium deficient high‐pressure phases with the compositions Pd1–xS2 and Pd1–xSe2 could be obtained via high‐pressure/high‐temperature syntheses at 7.5 GPa (Pd0.88(1)Se2) and 11.5 GPa (Pd0.94(1)S2) at 1523 K. Compared to the normal‐pressure modifications they showed a significant decrease in the c‐lattice parameters of Δc/c = 4.4 % (Pd0.94(1)S2) and Δc/c = 10.8 % (Pd0.88(1)Se2) accompanied by under‐occupied palladium sites. Single‐crystal analyses indicated the space group Pbca with lattice parameters and refinement results of a = 552.02(8), b = 555.11(8), c = 720.20(11) pm, R1 = 0.0562, wR2 = 0.0710 (all data) for Pd0.94(1)S2 and a = 587.93(3), b = 593.16(4), c = 685.99(4) pm, R1 = 0.0139, wR2 = 0.0232 (all data) for Pd0.88(1)Se2. XPS investigations revealed a partial oxidation of Pd2+ to Pd4+, which was observed for the first time in palladium chalcogenide chemistry. Magnetic susceptibility measurements confirmed the expected diamagnetic behavior.
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