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PubMed2001

Crystal structure and functional analysis of the SurE protein identify a novel phosphatase family.

Homologs of the Escherichia coli surE gene are present in many eubacteria and archaea. Despite the evolutionary conservation, little information is available on the structure and function of their gene products. We have determined the crystal structure of the SurE protein from Thermotoga maritima. The structure reveals the dimeric arrangement of the subunits and an active site around a bound metal ion. We also demonstrate that the SurE protein exhibits a divalent metal ion-dependent phosphatase activity that is inhibited by vanadate or tungstate. In the vanadate- and tungstate-complexed structures, the inhibitors bind adjacent to the divalent metal ion. Our structural and functional analyses identify the SurE proteins as a novel family of metal ion-dependent phosphatases.

Acid Phosphatase↗
PubMed1992

Looking back and looking forward.

'Forty years back and forty years on' was the title of the address given by Francis Manfield at the annual meeting of the RCS of England in December 1970. Francis, twice president of the Middx & Herts Branch, which this year celebrates its first 40 years, started in practice in 1930, so he was well qualified to look back over those 40 years. The aspects of change in dentistry, 1930-1970, make arresting reading more than 20 years later. His predictions for the future are equally interesting.

Dental Instruments↗
PubMed1989

Indirect determination of tungstate in rat tissues by atomic absorption spectrometry.

An indirect method is described for the determination of tungsten as tungstate in tissue samples by atomic absorption spectrometry (AAS). Tungstate forms a stable ion-association complex [Fe(dipy)3]2+WO4(2-) (dipy = 2,2'-dipyridyl) in acidic solution, which can be extracted into chloroform with an efficiency of higher than 98%. The extract can be analysed for iron (and hence indirectly for WO4(2-] by flame AAS after stripping back into 60% perchloric acid. The calibration graph is linear up to 19 p.p.m. of WO4(2-) and the limit of detection is 0.17 p.p.m. Many foreign ions do not interfere and the method has been applied successfully to the determination of tungstate in rattus norvegicus tissue samples.

Animals↗
PubMed1990

Comparative study of various polyols as complexing agents for the acidimetric titration of tungstate.

Most polyols (L = alditol or carbohydrate) form dinuclear tungstate complexes according to the over-all equilibrium 2WO4(2-) + 2H+ + L equal equilibrium [W2O7L]2- + H2O. When the reaction is fast and complete, it allows the acidimetric titration of tungstate. The formation constants of the complexes of a series of polyols were determined by potentiometry. Their values were higher at low ionic strengths. Opposite structural factors govern the stabilities and the formation rates of complexes: alditols of threo configuration react with tungstate faster than those of erythro configuration, but the stability order is erythro greater than threo. Of the polyols investigated, only xylitol and D-glucitol (sorbitol) allowed a fast and accurate potentiometric titration. Using 0.02 M HCl as titrand, 0.04 mmol of tungstate was determined in a volume of 100 cm3. The interference of molybdate is discussed in detail.

Alcohols↗
PubMed2004

9,10-Anthracene dicarboxylate bridged complexes with M2 quadruply bonded dimetal units: [[M2(O2CtBu)3]2(mu-9,10-An(CO2)2)], where M = Mo or W.

From the reactions between [M2(O2CtBu)4] and 9,10-anthracenedicarboxylic acid in toluene, the dicarboxylate bridged complexes [[M2(O2CtBu)3]2(mu-9,10An(CO2)2)], have been obtained as microcrystalline yellow (M = Mo) and red (M = W) powders. The powders are soluble in THF forming intense red (M = Mo) and green (M = W) solutions. The electronic absorption spectra in 2-MeTHF have been recorded as a function of temperature (2-298 K) and show a small bathochromic shift on cooling. The electronic structures have been investigated by molecular orbital calculations employing density functional theory on the model compounds [(HCO2)3M2]2(mu-9,10-An(CO2)2) where the M4 unit is constrained to lie in a plane. These reveal a minimum energy, gas-phase structure wherein the plane of the anthracene is twisted by ca. 54 degrees with respect to its 9,10-carboxylate units for both Mo and W. The results of these calculations are correlated with the electronic absorption spectral data and the electrochemical measurements (CV and DPV) of the first and second oxidation waves. The EPR spectra of the radical cations formed by single-electron oxidation with [Cp2Fe](+)[PF6]- in a THF-CH2Cl2 solvent mixture show that the complexes are valence trapped at ambient temperature on the EPR timescale. These results are discussed in the light of recent studies of dicarboxylate-linked MM quadruple bonds.

Anthracenes↗
PubMed2004

Oxygen-17 NMR study of aqueous peroxotungstates.

Aqueous peroxotungstates have been studied from pH 0.5 to 9.0, over a range of peroxide concentrations. Although equilibria are not always established, many anions can be identified by 17O NMR because the ratio of deltaO(W anion)/deltaO(known Mo anion) is consistently 79 +/- 3%. They are [WO3(HO2)]-; [WO(OH)(O2)2]-; [WO(OH2)(O2)2]0; [W2O3(O2)4]2-; [W2O3(OH)(O2)4]3-; [W4O12(O2)2]4-; [W7O23(O2)]6- and [W7O22(O2)2]6-. Their pKa values, where measurable, are about 2 units lower than the corresponding peroxomolybdates, e.g. 0.0 for [WO(OH2)(O2)2]0 and 8.0 for [W2O3(O2)4]2-. Other peroxotungstate species are also present but can only be broadly identified. These include Keggin structures with relatively low peroxo content, and a very unsymmetrical anion appearing at pH ca. 7 that bears no obvious structural relationship to any species previously reported. The main product from the reaction of powdered W metal with 30% aqueous peroxide is provisionally identified as the symmetrical anion [W6O13(OH)2(OH2)2(O2)5]2-, although other minor species are also formed, probably having fewer peroxo substituents.

Hydrogen-Ion Concentration↗
PubMed2004

A low cost instrument based on a solid state sensor for balloon-borne atmospheric O(3) profile sounding.

The design of an instrument based on a solid state tungsten oxide sensor for making profile measurements of atmospheric ozone from balloon platforms is described. The sensor is operated at a constant temperature, typically 530 [degree]C. The importance of a detailed consideration of the electronic design is demonstrated, with particular reference to the circuit to control the sensor heater. Calibration methods which are straightforward to implement are illustrated, and the results of a test flight alongside an electrochemical ozonesonde are shown. Quantitative agreement within 25% for most of the profile demonstrates the potential of this type of sensor for ozone sounding. Future improvements from manufacture to analysis are expected to improve on this.

Calibration↗
PubMed2005

The Ru(II)-supported heptatungstates [HXW7O28Ru(dmso)3]6-(X=P, As).

The ruthenium(II)-supported heteropolyanions [HXW7O28Ru(dmso)3]6-(X=P, 1; As, 2) are composed of a Ru(dmso)3 group attached to an unprecedented heptatungstate fragment via two Ru-O-W bonds and one Ru-O-X bond, which represents a fundamentally novel mode of Ru-coordination to a polyoxoanion framework. Multinuclear 183W, 31P, 13C, and 1H NMR studies indicate high stability of 1 and 2 in solution.

Magnetic Resonance Spectroscopy↗
PubMed1982

Interaction of rat liver glucocorticoid receptor with sodium tungstate.

Effects of sodium tungstate on various properties of rat liver glucocorticoid receptor were examined at pH7 and pH 8. At pH 7, [3H]triamcinolone acetonide binding in rat liver cytosol preparations was completely blocked in the presence of 10--20 mM-sodium tungstate at 4 degrees C, whereas at 37 degrees C a 30 min incubation of cytosol receptor preparation with 1 mM-sodium tungstate reduced the loss of unoccupied receptor by 50%. At pH 8.0, tungstate presence during the 37 degrees C incubation maintained the steroid-binding capacity of unoccupied glucocorticoid receptor at control (4 degrees C) levels. In addition, heat-activation of cytosolic glucocorticoid-receptor complex was blocked by 1 mM- and 10 mM-sodium tungstate at pH 7 and pH 8 respectively. The DNA-cellulose binding by activated receptor was also inhibited completely and irreversibly by 5 mM-tungstate at pH 7, whereas at pH 8 no significant effect was observed with up to 20 mM-tungstate. The entire DNA-cellulose-bound glucocorticoid-receptor complex from control samples could be extracted by incubation with 1 mM- and 20 mM-tungstate at pH 7 and pH 8 respectively, and appeared to sediment as a 4.3--4.6 S molecule, both in 0.01 M- and 0.3 M-KCl-containing sucrose gradients. Tungstate effects are, therefore, pH-dependent and appear to involve an interaction with both the non-activated and the activated forms of the glucocorticoid receptor.

Animals↗