A1 Refereed original research article in a scientific journal
Preparation and reactions of rhenium(VII) trioxo hydrogendiolato complexes and rheninm(VI) oxo bis(diolato) complexes
Authors: Edwards PG, Jokela J, Lehtonen A, Sillanpaa R
Publisher: ROYAL SOC CHEMISTRY
Publication year: 1998
Journal:: Dalton Transactions
Journal name in source: JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS
Journal acronym: J CHEM SOC DALTON
Issue: 19
First page : 3287
Last page: 3293
Number of pages: 7
ISSN: 0300-9246
DOI: https://doi.org/10.1039/a803301c
Abstract
The compound Re2O7, Re2O7. 2H(2)O or [ReO3(OSiMe3)] reacted with H(2)diol to form complexes having the general formula [ReO3(Hdiol)] where H(2)diol = 2,3-dimethylbutane-2,3-diol (H(2)pin) or 1,1'-bicyclohexane-1,1'-diol (H(2)bicy). In the case of H(2)pin the complex [ReO3(Hpin)]. H(2)pin is formed initially in the reaction of rhenium(VII) oxides with an excess of pinacol. The hydrogen bonded free pinacol molecule can be removed by sublimation. The monomethyl derivative of pinacol, HMepin, reacts in a similar way to form the complex [ReO3(Mepin)]. In the rhenium(VII) compounds the Re atom has a distorted trigonal bipyramidal co-ordination geometry. Pale yellow solutions of [ReO3(Hdiol)] in CH2Cl2 slowly become orange and red crystals having the formula [ReO(diol)(2)] may be isolated. The reaction of rhenium(VII) oxides with H(2)diol and PPh3 in the presence of drying agents in CH2Cl2 produced the same compounds in high yield. The crystal structures of the rhenium(VI) complexes reveal that the rhenium(VI) cations have square pyramidal co-ordination geometries. The rhenium(VI) oxo bis(diolato) complexes are thermally stable and do not readily undergo oxidation in dry air.
The compound Re2O7, Re2O7. 2H(2)O or [ReO3(OSiMe3)] reacted with H(2)diol to form complexes having the general formula [ReO3(Hdiol)] where H(2)diol = 2,3-dimethylbutane-2,3-diol (H(2)pin) or 1,1'-bicyclohexane-1,1'-diol (H(2)bicy). In the case of H(2)pin the complex [ReO3(Hpin)]. H(2)pin is formed initially in the reaction of rhenium(VII) oxides with an excess of pinacol. The hydrogen bonded free pinacol molecule can be removed by sublimation. The monomethyl derivative of pinacol, HMepin, reacts in a similar way to form the complex [ReO3(Mepin)]. In the rhenium(VII) compounds the Re atom has a distorted trigonal bipyramidal co-ordination geometry. Pale yellow solutions of [ReO3(Hdiol)] in CH2Cl2 slowly become orange and red crystals having the formula [ReO(diol)(2)] may be isolated. The reaction of rhenium(VII) oxides with H(2)diol and PPh3 in the presence of drying agents in CH2Cl2 produced the same compounds in high yield. The crystal structures of the rhenium(VI) complexes reveal that the rhenium(VI) cations have square pyramidal co-ordination geometries. The rhenium(VI) oxo bis(diolato) complexes are thermally stable and do not readily undergo oxidation in dry air.
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