X-ray diffraction, PGSE diffusion, and related NMR studies on a series of Cp*-based Ru(IV)(Cp*)(η3-CH2-CH-CHPh) allyl complexes

被引：23
作者：
Fernandez, Ignacio
Pregosin, Paul S. [1 ]
Albinati, Alberto
Rizzato, Silvia
机构：
[1] ETH, HCI, Inorgan Chem Lab, CH-8093 Zurich, Switzerland
[2] Univ Milan, Dept Struct Chem DCSSI, I-20133 Milan, Italy
来源：
ORGANOMETALLICS | 2006年 / 25卷 / 19期
关键词：
D O I：
10.1021/om060448u
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
The new ruthenium (IV) allyl complexes [Ru(Cp*)Cl(DMF)(eta(3)-CH2-CH-CHPh)](PF6) (2b) and [Ru(Cp*) Cl(t-BuCN)(eta(3)-CH2-CH-CHPh)](PF6) (2c) have been prepared and their structures determined. These results are compared with the analogous X-ray data for [Ru(Cp*) Cl(CH3CN)(eta(3)-CH2-CH-CHPh)](PF6), [Ru(Cp*) {OC(O-t-Bu)O}(eta(3)-CH2-CH-CHPh)](PF6), [Ru(Cp*)(CH3CN)(2)(A(3)-CH2-CH-CHPh)](PF6)(2), and [Ru(Cp*)(DMF)(2)(A(3)-CH2-CH-CHPh)](PF6)(2). In all of the structures, the Ru-((eta(3)-CH2CH- CHPh) moiety is markedly distorted such that Ru-CPh(allyl) separation is much longer than the remaining two Ru- C(allyl) distances. The DMF and acetonitrile ligands are shown to exchange on the NMR time scale via both variable-temperature and 2-D exchange spectroscopy. Pulsed gradient spin-echo (PGSE) diffusion and H-1, F-19 HOESY NMR methods show that there is relatively little ion pairing in these salts in DMF and acetonitrile solutions. The PF6 anions take up specific positions with respect to the Ru(IV) cations.
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页码：4520 / 4529
页数：10
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