Abstract
The rhenium complex fac-[ReOCl 3L] [ 1; L = 1,3-bis(diphenylphosphanyloxy)propane] was prepared by reacting L with [ReOCl 3(AsPh 3) 2]. Refluxing complex 1 in ethanol gave [ReOCl 2(OEt)L] ( 2), which X-ray crystallography showed to have an octahedral rhenium environment and an Re–O–Et fragment of unusual linearity. The paramagnetic chlorocomplexes mer-[ReCl 3LL′] [ 3; L′ = P(OEt) 3 in 3a, PPh(OEt) 2 in 3b, PPh 2(OEt) in 3c] were obtained by treating compound 1 with L′. Reaction of complexes 1 and 3a– c with excess NaBH 4 gave the polyhydrides [ReH 7L] ( 4) and [ReH 5LL′] ( 5a– c), respectively, all of which were characterized by variable-temperature (VT) NMR spectroscopy as highly fluxional classical hydrides. Complete protonation of these polyhydrides with HBF 4 · OMe 2 required 3 equiv. of acid, and the cationic polyhydride complexes so obtained were characterized as non-classical species by VT NMR spectroscopy and T 1 measurements.
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