K. Brandt et Ws. Sheldrick, SYNTHESIS, STRUCTURE AND REACTIVITY OF THE THIOETHER HALF-SANDWICH RHODIUM(III) COMPLEX )][CF3SO3](2)([9]ANES(3)=1,4,7-TRITHIACYCLONONANE), Journal of the Chemical Society. Dalton transactions, (7), 1996, pp. 1237-1243
The complex [RhCl(MeCN)(2)([9]aneS(3))][CF3SO3](2) 1 ([9]aneS(3) = 1,4
,7-trithiacyclononane) was prepared by reaction of RhCl3 . 3H(2)O with
[9]aneS(3) in the presence of an excess of Ag(O3SCF3) in acetonitrile
. It has been employed as a starting material for the synthesis of the
mixed-ligand sandwich complex [Rh{HB(pz)(3)}([9]aneS(3))][CF3SO3](2)
2 (pz = pyrazol-1-yl) and the half-sandwich complexes [RhCl(pymt)([9]a
neS(3))][CF3SO3] 3 (Hpymt = pyrimidine-2-thiolate), [Rh(pymt)(2)([9]an
eS(3))][CF3SO3] 4 and [RhCl(S(2)CNEt(2))([9]aneS(3))][CF3SO3] 5. Treat
ment of 1 with 2 molar equivalents of Na[S(2)CNEt(2)] in methanol led
to a base-induced ring opening of the thioether [9]aneS(3) and formati
on of the mu-S bridged dinuclear complex )CNEt(2))(2)}(2){mu-S(CH2)(2)
S(CH2)(2)SCH=CH2}(2)] 6 The structures of 1-3 and 6 have been determin
ed by X-ray crystallography.