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PubMed2004

Synthesis and characterization of N-heterocyclic carbene complexes of uranium(III).

Reaction of [(((Ad)ArO)(3)tacn)U(III)] (1) or [((Me(3)Si)(2)N)(3)U(III)] (3) with tetramethylimidazol-2-ylidene (Me(4)IMC:) yields novel N-heterocyclic carbene complexes [(((Ad)ArO)(3)tacn)U(III)(Me(4)IMC:)] (2) and [((Me(3)Si)(2)N)(3)U(III)(Me(4)IMC:)] (4). Uranium complexes 2 and 4 represent the first examples of compounds with an N-heterocyclic carbene ligand coordinated to a low-valent uranium center. The paramagnetic complexes 1, 2, and 4 were characterized by (1)H NMR, UV-vis-NIR, and EPR spectroscopy as well as SQUID magnetization measurements and X-ray diffraction analyses. DFT studies indicate a significant degree of pi-bonding in the U(III)-carbene entity.

Journal Article↗
PubMed1984

A comparison of the distributions of the actinides uranium and thorium with the lanthanide gadolinium in the tissues and eggs of Japanese quail: concentrations of uranium in feeds and foods.

Japanese quail were given UCl3 , UO2 (NO3)2, Th(NO3)4, or GdCl3 ( 153Gd -labeled) intravenously in aqueous solution. Distribution of Th among the tissues was as for Gd; distributions of U(III) and U(VI) were markedly different. For example, 18 hr after a 1.5 mumol/100 g dose, accumulations in females were: growing oocytes, U(III) 2.0%, U(VI) 2.4%, Th 27.7%, Gd 44.7%; leg bones, U(III) 12.5%, U(VI) 14.1%, Th 1.2%, Gd 1.4%; liver, U(III) 1.1%, U(VI) 1.1%, Th 44.0%, Gd 40.2%. Whole body losses by 18 hr were: females, U 24%, Th 14%, Gd 4%; males, U 72%, Th 23%, Gd 1%. Cumulative depositions in yolks of eggs laid over 8 days were: U(III) 1.9%, U(VI) 1.7%, Th 57.3%, Gd 46.8%. The distribution of U in quail may be atypical of actinides . Concentrations of U in various feeds, foods, and mineral supplements ranged from 169 micrograms/g in a phosphate fertilizer for farm use to below the lower detectable limit of .01 microgram/g in many foods intended for human use. Two batches of the game bird laying ration supplied to the quail colony contained 3.05 and 4.42 micrograms U/g. Body burdens of 3.5 micrograms U/bird for noninjected quail were attributed to the U content of this feed.

Animal Feed↗
PubMed1984

Differences in the morphology of isometric particles of some plant viruses stained with uranyl acetate as an aid to their identification.

Purified preparations of viruses with small polyhedral particles representing ten distinct taxonomic groups were examined by electron microscopy after negative staining with uranyl acetate. Comparisons of the relative size, shape and surface appearance of the particles established that some of them could be distinguished at the group level. However, the particles of viruses belonging to the bromovirus group could not be distinguished from those of the cucumovirus group, the nepovirus group from those of the comovirus group, and the tombusvirus group from those of the dianthovirus group. Furthermore, the particles of viruses of the sobemovirus, lutoevirus and tobacco necrosis virus groups were indistinguishable. The usefulness of the observed differences in the particle morphologies to virus identification is discussed.

Microscopy, Electron↗
PubMed2006

EXAFS study of U(VI) uptake by calcium silicate hydrates.

Among the different cement minerals, calcium silicate hydrates (C-S-H) are the prime candidates for heavy metal binding because of their abundance and appropriate structure. Immobilization processes of heavy metals by cementitious materials, and in particular C-S-H phases, thus play an important role in multibarrier concepts developed worldwide for the safe disposal of hazardous and radioactive wastes. In this study, the uptake of U(VI) by C-S-H has been investigated using X-ray absorption fine structure (XAFS) spectroscopy. C-S-H phases were synthesized using two different procedures: One is based on the mixing of CaO and SiO2 solids ("direct reaction" method); for the other one starting solutions of Ca and Si are used ("solution reaction" method). XAFS investigations were carried out on samples doped with U(VI). U(VI) was either sorbed onto previously precipitated C-S-H phases (sorption samples) or added during C-S-H synthesis (coprecipitation samples). The coordination environment of U(VI) in the sorption samples was found to be independent of the procedure used for C-S-H synthesis. A split equatorial oxygen shell (Oeq1: R=2.23-2.27 A; Oeq2: R=2.36-2.45 A), neighboring silicon atoms at short (R=3.07-3.11 A) and long (R=3.71-3.77 A) distances, and neighboring Ca atoms (R=3.77-3.81 and 4.15-4.29 A) were observed for all the samples. The structural parameters resemble those reported for uranophane. The coordination environment of U(VI) in the coprecipitation samples depends on the method used for C-S-H synthesis, and further, the spectra differ from those determined for the sorption samples. UU backscattering contributions were observed in the samples prepared using the direct reaction method, whereas no split equatorial shell appeared in the samples prepared using the solution reaction method.

Absorptiometry, Photon↗
PubMed2004

Synthesis, structure, and catalytic properties of V(IV), Mn(III), Mo(VI), and U(VI) complexes containing bidentate (N, O) oxazine and oxazoline ligands.

Synthesis of seven complexes containing oxazoline ([(L(1))(2)V=O] (4), [(L(1))(2)MoO(2)] (5), [(L(1))(2)UO(2)] (6); HL(1) (1) [HL(1) = 2-(4',4'-dimethyl-3'-4'-dihydroxazol-2'-yl)phenol]), chiral oxazoline ([(L(2))(2)UO(2)] (7); HL(2) (2) [HL(2) = (4'R)-2-(4'-ethyl-3'4'-dihyroxazol-2'-yl)phenol]), and oxazine ([(L(3))(2)V=O] (8), [(L(3))(2)Mn(CH(3)COO(-))] (9), [(L(3))(2)Co] (10); HL(3) (3) [HL(3) = 2-(5,6-dihydro-4H-1,3-oxazolinyl)phenol]) and their characterization by various techniques such as UV-vis, IR, and EPR spectroscopy, mass spectrometry, cyclic voltammetry, and elemental analysis are reported. The novel oxazine (3) and complexes 4, 5, 8 and 9 were also characterized by X-ray crystallography. Oxazine 3 crystallizes in the monoclinic system with the P2(1)/n space group, complexes 4 and 9 crystallize in the monoclinic system with the P2(1)/c space group, and complexes 5 and 8 crystallize in the orthorhombic system with the C222(1) space group and the P2(1)2(1)2(1) chiral space group, respectively. The representative synthetic procedure involves the reaction of metal acetate or acetylacetonate derivatives with corresponding ligand in ethanol. Addition of Mn(OAc)(2).4H(2)O to an ethanol solution of 3 gave the unexpected complex Mn(L(3))(2).(CH(3)COO(-)) (9) where the acetate group is coordinated with the metal center in a bidentate fashion. The catalytic activity of complexes 4-9 for oxidation of styrene with tert-butyl hydroperoxide was tested. In all cases, benzaldehyde formed exclusively as the oxidation product.

Catalysis↗
PubMed2005

Theoretical investigation of uranyl dihydroxide: oxo ligand exchange, water catalysis, and vibrational spectra.

Density functional theory is employed to investigate uranyl dihydroxide, UO2(OH)2, isomerization reaction energy barriers, including those occurring via proton shuttles. The ground-state structure of a uranyl dihydroxide complex containing a uranyl moiety with a near 90 degrees O=U=O bond angle is reported for the first time. Furthermore, we predict the vibrational spectra of these compounds. Scalar-relativistic effects for uranium are treated by employing a relativistic effective core potential.

Journal Article↗
PubMed2005

Structural and zeolitic features of a series of heterometallic supramolecular porous architectures based on tetrahedral {M(C2O4)4}4- primary building units.

The utilization of tetrahedral pre-formed coordination compounds {M(C2O4)4}4- (M = Zr(IV), U(IV); C2O4(2-) = oxalate) permitted the efficient construction of rare examples of heteronuclear supramolecular nano-porous architectures. A series of metal-organic coordination frameworks prepared by association of these building units with either Mn2+, Cd2+, or Mg2+ have been structurally characterized and are described. Their 3-D chemical scaffold is based on the primary tetrahedral building unit but their pore sizes and topologies could be varied through the M2+ metal ion involved in the assembling process, and the anionic tetrahedral moiety. These structures display channels with apertures up to 12 Angstrom x 8 Angstrom which are emptied of solvates at mild temperatures without affecting the chemical scaffold, the integrity of which is maintained up to 250-300 degrees C. A certain degree of flexibility of the coordination polymers upon guest release is suggested by the temperature dependence of the powder X-ray patterns and N2 sorption experiments, but reversible and selective sorption of small molecules has been observed substantiating that these open-frameworks behave like sponges.

Cadmium↗
PubMed1981

Inhibition by metals of a canine renal calcium, magnesium-activated adenosinetriphosphatase.

A number of metals were examined for inhibition of a canine renal calcium, magnesium-activated adenosinetriphosphatase (Ca2+, Mg2+-ATPase). Of the 27 metals investigated, only compounds of mercury, silver, gold, and uranium demonstrated 50% inhibition of the enzyme at concentrations lower than 10(-4) M. The order of inhibitory potency was Hg greater than Ag greater than U greater than Au. Organic mercury (chlormerodrin, mersalyl, p-chloromercuribenzoate) was less potent than inorganic mercuric chloride, but organic gold sodium thiomalate was equipotent with inorganic gold chloride. The inhibition produced by each metal decreased parallel to the decrease in enzyme activity, seen as the source of enzyme moved from the outer cortex inward to the papilla of the kidney. The regions of highest activity showed the greatest inhibition by each metal, and inhibition decreased as the control activity of the tissue decreased. This variability of inhibition was not related to the protein content of the enzyme preparation. As the ATP concentration increased, the inhibition produced by U was reduced; if the Mg (but not the Ca concentration) was increased while the ATP concentration remained constant, the inhibition increased. Changes in the Ca, Mg, and ATP concentrations did not alter the inhibition produced by Hg, Ag, and Au.

Animals↗
PubMed1981

The use of a simple method to avoid cell shrinkage during SEM preparation.

In the course of preparing specimens for scanning electron microscopy, both glutaraldehyde and OsO4-fixed cells exhibit a considerable shrinkage with a reduction of the mean cellular diameter of about 45% after critical point drying. However, if cells are successively treated with glutaraldehyde, OsO4, tannic acid and uranyl acetate solutions, cellular shrinkage of only 5% is observed.

Animals↗
PubMed1973

The onset of the effects of zinc and tetraethylammonium ions on action potential duration and twitch amplitude of single muscle fibres.

1. Single dissected muscle fibres were used to examine the rates of onset and reversal of the effects of zinc and tetraethylammonium (TEA) ions on the duration of the action potential and the amplitude of the twitch.2. The increases in fall time (100-50%) of the action potential and in the amplitude of the twitch resulting from the application of zinc or TEA follow exponential time courses.3. The time constants for the onset of the effects of 0.1 mM zinc were 11.03+/-0.71 sec (six fibres) and 9.24+/-0.77 sec (sixteen fibres) on action potential and twitch amplitude respectively. The values are not significantly different from each other.4. The onset of the effect of zinc on action potential duration was speeded up by ;detubulation' by glycerol treatment. The time constant was 3.88+/-0.68 sec (six fibres).5. The time constants for the onset of the effects of 25 mM-TEA were 3.48+/-0.69 sec (six fibres) and 3.81+/-0.26 sec (nine fibres) on action potential and twitch respectively. These values are not significantly different from each other.6. The results are consistent with the idea that zinc and TEA act as twitch potentiators by way of their effect on action potential duration. It seems likely that this effect is, in part at least, on the surface membrane, but an effect within the T-system is not ruled out.

Acetates↗
PubMed1981

Intranuclear crystalloids associated with abnormal granules in eosinophilic leukocytes.

Ultrastructural evaluation of eosinophilic leukocytes from a 2-yr-old asymptomatic girl with chronic benign neutropenia (CBN) revealed a variety of morphological abnormalities. All eosinophils obtained from blood and marrow specimens contained multipole microcrystalloids in most of the mature cytoplasmic granules. An increase in crystalloid-free, immature granules in late (bilobed nuclei) eosinophils suggested a delay in granule maturation. The eosinophil granules appeared to be of normal size and demonstrated normal acid phosphatase reactivity. Eosinophilic myelocytes contained abnormal cisternae of rough endoplasmic reticulum (RER) and lacked abundant elongated RER cisternae seen in normal cells. A few eosinophilic myelocytes in specimens of bone marrow from the child contained large intranuclear crystalloids measuring up to 3 mu in length. The intranuclear crystalloid contained as cubic lattice of dense material with a periodicity similar to that described for cytoplasmic crystalloids. The ultrastructural morphology of marrow neutrophils was normal, as described in other cases of CBN. Ultrastructural examination of blood eosinophils from the father demonstrated microcrystalloids in cytoplasmic granules identical to those seen in the child. The father was asymptomatic and had normal leukocyte counts. Thus, anomalous crystalloid granule genesis occurred in the father and daughter and was not necessarily associated with neutropenia or clinical symptomatology. This anomaly is associated with the accumulation of intranuclear crystalloid material in eosinophilic myelocytes, which do not appear to be released from the marrow compartment.

Acid Phosphatase↗
PubMed1991

Modified biokinetic model for uranium from analysis of acute exposure to UF6.

Urinalysis measurements from 31 workers acutely exposed to uranium hexafluoride (UF6) and its hydrolysis product UO2F2 (during the 1986 Gore, Oklahoma UF6-release accident) were used to develop a modified recycling biokinetic model for soluble U compounds. The model is expressed as a five-compartment exponential equation: yu(t) = 0.086e-2.77t + 0.0048e-0.116t + 0.00069e-0.0267t + 0.00017 e-0.00231t + 2.5 x 10(-6) e-0.000187t, where yu(t) is the fractional daily urinary excretion and t is the time after intake, in days. The excretion constants of the five exponential compartments correspond to residence half-times of 0.25, 6, 26, 300, and 3,700 d in the lungs, kidneys, other soft tissues, and in two bone volume compartments, respectively. The modified recycling model was used to estimate intake amounts, the resulting committed effective dose equivalent, maximum kidney concentrations, and dose equivalent to bone surfaces, kidneys, and lungs.

Accidents, Occupational↗