Inorganic Chemistry p. 6141 - 6144 (1995)
Update date:2022-08-04
Topics:
Landtiser, Richard
Mague, Joel T.
Fink, Mark J.
Silvestru, Cristian
Haiduc, Ionel
The reaction of Pd2(μ-dcpe)2 (dcpe = 1,2-bis(dicyclohexylphosphino)ethane) with the bis(thiophosphinyl)disulfanes, R2P(S)SSP(S)PR2 (R = Et, Ph), give the ionic complexes [(dcpe)Pd(SPR2S)](1+)[SPR2S](1-) in 60% (1; R = Et) and 72% (2: R = Ph) yields. An unusual dimer, {(Et2PS2)Pd}2(μ-Et2PS2)2, is also isolated in low yield for R = Et. The X-ray structure of a benzene solvate of 1 (C50H68P4S4Pd.1.5C6H6; monoclinic, a = 14.628(1) ?, b = 16.662(3) ?, c = 21.612(4) ?, β = 107.66(1), P21/n, Z = 4, R = 0.047(Fo), Rw = 0.056(Fo)) shows a nearly planar spirocyclic palladium atom in the cation and a free SPR2S(1-) anion. Variable-temperature (31)P NMR spectra of 1 indicate rapid interchange of thecoordinated and free SPR2S(1-) counterion in solution at room temperature.
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Doi:10.1016/0040-4039(95)02221-X
(1996)Doi:10.1016/0022-1139(95)03252-9
(1995)Doi:10.1021/om00011a053
(1995)Doi:10.1021/jm950835y
(1996)Doi:10.1002/hlca.19970800202
(1997)Doi:10.1016/0040-4020(95)00834-U
(1995)