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At ambient conditions, PdSe 2  dichalcogenides crystallize in the layered PdS 2 -type structure. If pressure is applied, the coordination number of palladium atoms increases and the three-dimensional pyrite-type structure with octahedral (PdSe 6 ) 4−  coordination geometry is observed. For the first time, single crystals of a pyrite-type PdSe 2  modification could be obtained and characterized, which were grown by multianvil high-pressure/high-temperature synthesis at 7.5 GPa and 1023 K. The crystals show the expected pyrite-type space group  Pa 3̅ (no. 205) and refinement results of  a =613.26(3) pm,  R 1=0.0233, and  wR 2=0.0247 (all data) were received for HP-Pd 0.84(1) Se 2 . The single-crystal data revealed significant defect formation on the palladium site with 16% vacancies, which is in line with the orthorhombic Pd X  2 -type high-pressure polymorphs HP-Pd 0.94(1) S 2  and HP-Pd 0.88(1) Se 2 . The tendency of vacancy formation on the palladium site could also be verified by EDX measurements.

Single-crystal structure of pyrite-type HP-Pd 0.84(1) Se 2 prepared by high-pressure/ high-temperature synthesis