Pd[B(S 2 O 7 ) 2 ] 2 and Pd[B(SO 4 ) (S 2 O 7 )] 2 : Two Borosulfates with Pd 2+ in Octahedral and One with Pd 2+ in Square Planar Oxygen Coordination

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Abstract
The reaction of elemental palladium with B 2 O 3 and SO 3 at elevated temperature results in the formation of blue crystals of Pd[B(S 2 O 7 ) 2 ] 2 . Dependent on the reaction conditions, the compound crystallizes in two different polymorphs obtained as bulk samples. In both structures the Pd 2+ cations are coordinated by six oxygen atoms in form of an almost perfect octahedron. All oxygen atoms belong to the borosulfate anions [B(S 2 O 7 ) 2 ] − and link via Pd 2+ cations to an extended network structure. Within the uncommon octahedral oxygen coordination, the Pd 2+ cations reveal a d 8 high‐spin configuration, which leads to paramagnetism. Occasionally, red crystals are formed during the reaction next to the major fraction of blue crystals of Pd[B(S 2 O 7 ) 2 ] 2 . Single crystal X‐ray structure analysis on the red crystals reveals the sum formula Pd[B(SO 4 )(S 2 O 7 )] 2 with Pd 2+ in square‐planar coordination.
Funding Information
  • Deutsche Forschungsgemeinschaft (528508733, INST 211/1034–1)

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