Abstract
The complexes [(PMe 3) 6Pd 3(μ-S) 2](BPh 4) ( 4) and [(PMePh 2) 6Pd 3(μ-S) 2](BPh 4) 2 ( 6) are formed from [Pd(CH 3CN) 4](BF 4) 2 ( 5), H 2S and the corresponding phosphine in presence of NaBPh 4. Complex 4 is also obtained, although in low yields, as a secondary product in the reaction of [(PMe 3) 3PdH]BPh 4 with COS. 4 crystallizes in the space group P2 1/c (Z = 4) with a = 1551(2), b = 2517(7), b = 2517(7), c = 1830(3) pm and β = 94.74(9)°. The palladium and sulfur atoms of the dication [(PMe 3) 6Pd 3S 2] 2+ form a slightly distorted trigonal bipyramid in which one of the PdPd distances is significantly shorter than the other two. The coordination sphere around each palladium atom is nearly square-planar with angles SPdS = 79.3, PPdP = 97.4 and SPdP = 91.6° (mean values).
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