Abstract
A series of new rhenium phosphine heptahydride complexes ReH{sub 7}L{sub 2} (L{sub 2} = a chelating bidentate phosphine) have been synthesized and characterized by IR and {sup 1}H, and {sup 31}P, and {sup 13}C NMR spectroscopy. The hydride resonances of ReH{sub 7}(dppf) (1, dppf = 1,1{prime}-bis(diphenylphosphino)ferrocene), ReH{sub 7}(dppb) (2, dppb = 1,4-bis(diphenylphosphino)butane), and ReH{sub 7}((+)-diop) (3, (+)-diop = (4S,5S)-4,5-bis((diphenylphosphino)methyl)-2,2-dimethyl-1,3-dioxolane) undergo decoalescence upon cooling. The low-temperature hydride patterns suggest classical 9-coordinate tricapped trigonal prismatic structures. Consistent with the classical structures, {sup 1}H NMR spectra of deuterated ReH{sub 7}L{sub 2} complexes show very small and temperature-independent upfield isotope shifts in the hydride region and no change in {sup 2}J{sub HP}.
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