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Michael J Clarke J. Received June IAbstract: Kinetically stable, monodentate, pentaammineruthenium II1 complexes of the reductate ligands ascorbate and tetramethylreductate have been synthesized and characterized spectroscopically and electrochemically, and the autoxidation kinetics have been studied.
For all the complexes, axial or rhombic ESR spectra and magnetic susceptibilities in the range 1.
Both TMRA and ascorbate yield two distinct complexes with closely parallel properties, which form in varying amounts and interconvert depending on the pH of the reaction with an apparent pK, around 4. At low pH this isomerization takes place with a specific rate of 8.
At neutral pH the O 2 to O 3 isomerization occurs rapidly, and reductate ligand dissociation proceeds with a half-life of about 6 h. Cyclic voltammetric studies reveal reversible on the CV time scale couples E o values of 0. Both the reductate complexes and a related squarate complex exhibit an irreversible reduction, apparently due to ligand loss from the Ru I1 complex.
The rate of autoxidation of the reductate complexes at pH 7. Ascorbic acid is a relatively complex reductant see Figure lkinetically stable and so have not been well characterized as to whose chemical and biological effects often involve the presence their mode of coordination in solution.
Similarly, the autoxidation of redox-active transition-metal ions. In an effort to delve into the actual of undergoing redox reactions are thought to catalyze the aut- electron transfer to oxygen, in a manner that essentially precludes oxidation of ascorbic acid through the formation of intermediate binding of dioxygen and subsequent inner-sphere electron transfer, metalascorbate-dioxygen complexes.
Tetramethylreductic acid24effectively mimics to result in substantial D N A strand cleavage. Washington, DC, ; pp New York, ; pp Washington, 18 Tauqi Khan, M.
Acta 19 Taqui Khan, M. Critical Stabiliry Constants; Plenum: Abstracfs of Papers, National Crystallogr.
Proton and oxidation-reduction equilibria of ascorbic acid. The solvent was stripped in a rotary vacuum evaporator at OC, and a colorless oil was obtained. The crude oil from the reaction was dissolved in a minimum of acetone and loaded onto a silica gel column.
A, nm emax 9. Purification was effected by ion-exchange chromatography on S P Figure 2. Proton and oxidation-reduction equilibria for tetramethyl- Sephadex eluted with 0. Crystals formed from the eluant on reductic acid. Crystalline samples of this compound redissolved only very slowly.
Asc, ascorbic acid; Asc', ascorbate semiquinone; C, Ascorbato pentaammineruthenium lII trifluoromethanesulfonate TMRA, tetramethylreductic acid 2,3-dihydroxy-4,4,5,5-tetra- was prepared by deaerating two vessels by argon bubbling, one containing methylcyclopentenone ; TMRA', tetramethylreductate semi- 20 mL of 1 M N a O H and the other 25 mL of distilled water.
The methyltetramethylreductate; Sqr, squarate 3,4-dihydroxy- solution was adjusted to pH 9. If 3-cyclobutene-1,2-dione dianion ; TFMS, trifluoromethane- necessary, additional ascorbic acid was added to lower the pH.
The components of the resulting blue solution were separated on an inert- Experimental Section atmosphere SP Sephadex column 2 cm diameter X cm ,'O which Synthesis.
The product band was collected acetone, recrystallized from warm 1 M HCI, and stored in a vacuum in an argon-purged round-bottom flask and the solvent rotary-evaporated desiccator for a few days before use.
Trifluoromethylsulfonic acid off until just dry. Acetonitrile 25 mL was added to the flask NaTFMS was prepared by carefully neutralizing a 6 M solution of and swirled for a few minutes before filtering under vacuum.
The neutralized solution was rotary-evapo- amorphous blue product was washed with 25 mL of acetonitrile to re- rated to dryness and the solid product recrystallized with ethanol.Meanwhile, as a list of services our experts in varioius substance where in less than a deadline or.
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