Synthesis of Complexes of Re(V), Ru(II), Os(II), Rh(I), Ir(I) and Ir(III). Crystal and Molecular Structures of , and

DOI: 10.1039/DT9950003143

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 3143 - 3152 (1995)

Update date:2022-08-03

Topics:

Authors:

Ahmet, Mustafa T.

Lu, Canzhong

Dilworth, Jonathan R.

Miller, John R.

Zheng, Yifan

et al. et al.

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Article abstract of DOI:10.1039/DT9950003143

The rhenium(V) precursors (X = Cl or Br) reacted with 2-triphenylsilylbenzenethiol in methanol in the presence of base to give 1 and 2 respectively.In the presence of NaBH4 and no base the blue thiolate polyhydride 3 was formed in high yield.The crystal structures of 2 and 3 were determined and showed 2 to be monomeric with distorted trigonal-bipyramidal geometry and the oxide and hydroxide ligands in equatorial sites.The thiolate and phosphine ligands of 3 are in a tetrahedral array with the hydride ligands assumed to be in capping sites on the tetrahedral faces.Reaction of the thiol with in methanol in the presence of NEt3 gave 4 in good yield.Its crystal structure revealed the geometry about the Ir to be pseudo-octahedral with mer phosphine ligands and cis thiolates, and the hydride presumed to be in a vacant site trans to a thiolate ligand.The complex reacted under similar conditions to give monomeric 6 whereas gave 5; gave 7 whereas formed 8.The potentially bidentate thiol SiPh2(C6H4SH-2)2 gave a series of products with the same precursors which proved difficult to characterise unequivocally in the absence of X-ray structural data.The geometry adopted by the SC6H4SiPh3-2 ligand was analysed in some detail and contrasted with symmetrically 2,6-disubstituted aromatic thiolates.

Full text of DOI:10.1039/DT9950003143

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