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At least 19 recordsLinked to original sources
PubMed2006

Synthesis, structural characterization, and theoretical studies of gold(I) and gold(I)-gold(III) thiolate complexes: quenching of gold(I) thiolate luminescence.

The gold(I) thiolate complexes [Au(2-SC6H4NH2)(PPh3)] (1), [PPN][Au(2-SC6H4NH2)2] (2) (PPN = PPh3=N=PPh3), and [{Au(2-SC6H4NH2)}2(mu-dppm)] (3) (dppm = PPh2CH2PPh2) have been prepared by reaction of acetylacetonato gold(I) precursors with 2-aminobenzenethiol in the appropriate molar ratio. All products are intensely photoluminescent at 77 K. The molecular structure of the dinuclear derivative 3 displays a gold-gold intramolecular contact of 3.1346(4) A. Further reaction with the organometallic gold(III) complex [Au(C6F5)3(tht)] affords dinuclear or tetranuclear mixed gold(I)-gold(III) derivatives with a thiolate bridge, namely, [(AuPPh3){Au(C6F5)3}(mu2-2-SC6H4NH2)] (4) and [(C6F5)3Au(mu2-2-SC6H4NH2)(AudppmAu)(mu2-2-SC(6)H4NH2)Au(C6F5)3] (5). X-ray diffraction studies of the latter show a shortening of the intramolecular gold(I)-gold(I) contact [2.9353(7) or 2.9332(7) A for a second independent molecule], and short gold(I)-gold(III) distances of 3.2812(7) and 3.3822(7) A [or 3.2923(7) and 3.4052(7) A] are also displayed. Despite the gold-gold interactions, the mixed derivatives are nonemissive compounds. Therefore, the complexes were studied by DFT methods. The HOMOs and LUMOs for gold(I) derivatives 1 and 3 are mainly centered on the thiolate and phosphine (or the second thiolate for complex 2), respectively, with some gold contributions, whereas the LUMO for derivative 4 is more centered on the gold(III) fragment. TD-DFT results show a good agreement with the experimental UV-vis absorption and excitation spectra. The excitations can be assigned as a S --> Au-P charge transfer with some mixture of LLCT for derivative 1, an LLCT mixed with ILCT for derivative 2, and a S --> Au...Au-P charge transfer with LLCT and MC for derivative 3. An LMCT (thiolate --> Au(III) mixed with thiolate --> Au-P) excitation was found for derivative 4. The differing nature of the excited states [participation of the gold(III) fragment and the small contribution of sulfur] is proposed to be responsible for quenching the luminescence.

Crystallography, X-Ray↗
PubMed2002

In vivo liberation of gold ions from gold implants. Autometallographic tracing of gold in cells adjacent to metallic gold.

For some years, the implantation of small pieces of gold has been used as an unauthorised remedy for osteoarthritis and pain. The aim of the present study was to evaluate whether gold ions are released from gold implants. Pieces of pure gold were placed in the connective tissue of skin, bone and brains of anaesthetised animals. Ten days to several months later the animals were anaesthetised and killed by transcardial perfusion. Tissue blocks containing the gold pieces were cut, and the sections were silver-enhanced by autometallography. It was found that gold ions are released from the implanted gold and diffuse out into the surrounding tissue. The gold-containing cells in connective tissues were macrophages, mast cells and fibroblasts. In the brain, gold accumulated in astrocytes and neurons. Proton-induced X-ray emission spectroscopy analysis of the tissue surrounding gold implants confirmed that gold ions are liberated. The findings suggest that the gold implant technique, on a local scale, mimics systemic treatment with a gold-containing drug.

Animals↗
PubMed2002

Gold concentration in blood in relation to the number of gold restorations and contact allergy to gold.

Previous studies have demonstrated an association between gold allergy and the presence of dental gold restorations. The aim of the present study was to investigate the relationship between the concentration of gold in blood (B-Au) and the number of tooth surfaces with gold alloys in subjects with and without contact allergy to gold. In 80 patients referred for patch testing because of eczematous disease, blood samples were taken and analyzed for B-Au using inductively coupled plasma mass spectrometry. The detection limit for the Au determination was 0.04 microg/L. In addition, a dentist made a clinical and radiological examination of the patients and registered the number of dental gold surfaces. Patients with dental gold restorations had a statistically significantly higher B-Au in Mann-Whitney U test (P = 0.025), (range < 0.04-1.07 microg/L) than patients without (range < 0.04-0.15 microg/L). Furthermore, a positive correlation was found between B-Au and the number of dental gold surfaces (P < 0.01). There was no statistically significant difference in B-Au between persons with and without contact allergy to gold. The study thus indicates that gold is released from dental restorations and taken tip into the circulation.

Acrylic Resins↗
PubMed1998

Action of gold chloride ("gold toning") on silver-enhanced 1 nm gold markers.

In conventional immunoelectron microscopy (IEM), very small colloidal gold particles (0.8-3 nm), or the gold compound Nanogold (1.4 nm) are silver-enhanced for easy detection. However, silver enhancement has drawbacks. First, the silver layer is dissolved during fixation with osmium tetroxide, even if the concentration and incubation time are strongly reduced during pre-embedding labeling experiments in transmission electron microscopic (TEM) and scanning electron microscopic (SEM) studies. Second, after exposure to the electron beam the silver layer may migrate on the section or the whole particles may disappear. Sometimes silver migration can be observed even without irradiation. This effect strongly hampers reinvestigation of previously inspected areas, after some time of storage. In both cases, gold chloride treatment after silver enhancement is sufficient to completely protect the silver-enhanced 1 nm gold markers. Gold chloride treatment is part of the so-called "gold toning" procedure, which is a method used to substitute and/or cover the silver by a layer of gold. It can be applied in TEM and SEM experiments. As a serious drawback, gold chloride treatment slightly reduces the size of both unenhanced and silver-enhanced gold particles and can lead to disintegrated silver/gold particles. Therefore, this technique is useful for pre-embedding IEM, on-(resin)section, and ultrathin cryosection labeling experiments. However, it appears to be unsuitable for double-labeling studies using different gold sizes, for quantitation experiments, and in SEM.

Cryoultramicrotomy↗
PubMed2005

Gold trichloride and gold sodium thiosulfate as markers of contact allergy to gold.

The usefulness of a trivalent gold salt, gold trichloride (GTC), was evaluated as a marker of contact allergy to gold. Patients patch test-positive or patch test-negative to gold sodium thiosulfate (GSTS), 13 subjects of each, were patch tested with dilution series of GTC and equimolar concentrations of GSTS. In order to avoid false-positive and false-negative test reactions, the salts were buffered and placed on polypropene chambers. Allergic reactions were registered in 9/13 gold-allergic patients with GSTS and in 2/13 with GTC. The sum of positive reactions was 18 with GSTS and 5 with GTC. Irritant reactions were none with GSTS and 2 with GTC in the gold-allergic patients. It is concluded that GTC can elicit positive patch test reactions in patients with gold allergy but to a lesser degree when compared with GSTS. Thus, GTC cannot be recommended in patch testing, and GSTS is still the test agent of choice.

Aged↗
PubMed1991

Gold enhancement of gold-labeled probes: gold-intensified staining technique (GIST).

In this report we present a staining method in which gold chloride is used to enhance the size of gold colloids. We show the utility of this technique when used in conjunction with small gold colloids, i.e., 5 nm, 4 nm, and 2.6 nm. Post-embedding staining of epoxy-embedded, gold-labeled mouse LM fibroblasts showed that staining with 0.1% gold chloride facilitated the visualization of the smallest gold colloids.

Animals↗
PubMed2001

Structural variations and bonding in gold halides: a quantum chemical study of monomeric and dimeric gold monohalide and gold trihalide molecules, AuX, Au2X2, AuX3, and Au2X6 (X = F, Cl, Br, I).

The molecular structures of all gold mono- and trihalides and of their dimers have been calculated at the B3LYP, MP2, and CCSD(T) levels of theory by using relativistic pseudopotentials for all atoms except fluorine. Our computations support the experimental observation that the relative stability of the monohalides increases from the fluoride toward the iodide, while the stability trend of the trihalides is the opposite. The potential energy surface (PES) of all gold trihalides has been investigated. These molecules are typical Jahn-Teller systems; the trigonal planar D3h-symmetry geometry does not correspond to the minimum energy structure for any of them. At the same time, the amount and character of their Jahn-Teller distortion changes gradually from AuF3 to AuI3. The minimum energy geometry is a T-shaped structure for AuF3 and AuCl3, with a Y-shaped transition-state structure. For AuI3, the Y-shaped structure lies lower than the T-shaped structure on the PES. For AuBr3 and AuI3, neither of them is the global minimum but instead an L-shaped structure, which lies outside the Jahn-Teller PES. This structure can be considered to be a donor-acceptor system, or a closed-shell interaction, with I2 acting as donor and AuI as acceptor. The dimers of gold monohalides have very short gold-gold distances and demonstrate the aurophilic interaction. The dimers of the trihalides are planar molecules with two bridging halogen atoms.

Journal Article↗
PubMed2004

Molecular design of luminescence ion probes for various cations based on weak gold(I)...gold(I) interactions in dinuclear gold(I) complexes.

A series of luminescent dinuclear gold(I) complexes with different crown ether pendants, [Au(2)(PwedgeP)(S-B15C5)(2)] [S-B15C5 = 4'-mercaptobenzo-15-crown-5, P(wedge)P = bis(dicyclohexylphosphino)methane (dcpm) (1), bis(diphenylphosphino)methane (dppm) (2)] and [Au(2)(P(wedge)P)(S-B18C6)(2)] [S-B18C6 = 4'-mercaptobenzo-18-crown-6, P(wedge)P = dcpm (3), dppm (4)], and their related crown-free complexes, [Au(2)(P(wedge)P)(SC(6)H(3)(OMe)(2)-3,4)(2)] [P(wedge)P = dcpm (5), dppm (6)], were synthesized. The low-energy emission of the mercaptocrown ether-containing gold(I) complexes are tentatively assigned as originated from states derived from a S --> Au ligand-to-metal charge transfer (LMCT) transition. The crown ether-containing gold(I) complexes showed specific binding abilities toward various metal cations according to the ring size of the crown pendants. Spectroscopic evidence was provided for the metal-ion-induced switching on of the gold...gold interactions upon the binding of particular metal ions in a sandwich binding mode.

Journal Article↗
PubMed2002

Advanced mercury removal from gold leachate solutions prior to gold and silver extraction: a field study from an active gold mine in Peru.

Mercury contamination in the Gold-Cyanide Process (GCP) is a serious health and environmental problem. Following the heap leaching of gold and silver ores with NaCN solutions, portions of the mercury-cyano complexes often adhere to the activated carbon (AC) used to extract the gold. During the electrowinning and retorting steps, mercury can be (and often is) emitted to the air as a vapor. This poses a severe health hazard to plant workers and the local environment. Additional concerns relate to the safety of workers when handling the mercury-laden AC. Currently, mercury treatment from the heap leach solution is nonexistent. This is due to the fact that chelating ligands which can effectively work under the adverse pH conditions (as present in the heap leachate solutions) do not exist. In an effort to economically and effectively treat the leachate solution prior to passing over the AC, a dipotassium salt of 1,3-benzenediamidoethanethiol (BDET2-) has been developed to irreversibly bind and precipitate the mercury. The ligand has proven to be highly effective by selectively reducing mercury levels from average initial concentrations of 34.5 ppm (parts per million) to 0.014 ppm within 10 min and to 0.008 ppm within 15 min. X-ray powder diffraction (XRD), proton nuclear magnetic resonance (1H NMR), Raman, and infrared (IR) spectroscopy demonstrate the formation of a mercury-ligand compound, which remains insoluble over pH ranges of 0.0-14.0. Leachate samples from an active gold mine in Peru have been analyzed using cold vapor atomic fluorescence (CVAF) and inductively coupled plasma optical emission spectroscopy (ICP-OES) for metal concentrations before and after treatment with the BDET2- ligand.

Carbon↗
PubMed2005

Glutathione-protected gold clusters revisited: bridging the gap between gold(I)-thiolate complexes and thiolate-protected gold nanocrystals.

Small gold clusters (approximately 1 nm) protected by molecules of a tripeptide, glutathione (GSH), were prepared by reductive decomposition of Au(I)-SG polymers at a low temperature and separated into a number of fractions by polyacrylamide gel electrophoresis (PAGE). Chemical compositions of the fractionated clusters determined previously by electrospray ionization (ESI) mass spectrometry (Negishi, Y. et al. J.Am. Chem. Soc. 2004, 126, 6518) were reassessed by taking advantage of freshly prepared samples, higher mass resolution, and more accurate mass calibration; the nine smallest components are reassigned to Au10(SG)10, Au15(SG)13, Au18(SG)14, Au22(SG)16, Au22(SG)17, Au25(SG)18, Au29(SG)20, Au33(SG)22, and Au39(SG)24. These assignments were further confirmed by measuring the mass spectra of the isolated Au:S(h-G) clusters, where h-GSH is a homoglutathione. It is proposed that a series of the isolated Au:SG clusters corresponds to kinetically trapped intermediates of the growing Au cores. The relative abundance of the isolated clusters was correlated well with the thermodynamic stabilities against unimolecular decomposition. The electronic structures of the isolated Au:SG clusters were probed by X-ray photoelectron spectroscopy (XPS) and optical spectroscopy. The Au(4f) XPS spectra illustrate substantial electron donation from the gold cores to the GS ligands in the Au:SG clusters. The optical absorption and photoluminescence spectra indicate that the electronic structures of the Au:SG clusters are well quantized; embryos of the sp band of the bulk gold evolve remarkably depending on the number of the gold atoms and GS ligands. The comparison of these spectral data with those of sodium Au(I) thiomalate and 1.8 nm Au:SG nanocrystals (NCs) reveals that the subnanometer-sized Au clusters thiolated constitute a distinct class of binary system which lies between the Au(I)-thiolate complexes and thiolate-protected Au NCs.

Electrophoresis, Polyacrylamide Gel↗
PubMed2005

Genesis of gold clusters from mononuclear gold complexes on TiO2: reduction and aggregation of gold characterized by time-resolved X-ray absorption spectroscopy.

Mononuclear gold complexes bonded to TiO(2) were synthesized from Au(CH(3))(2)(C(5)H(7)O(2)), and their decomposition and conversion into gold nanoclusters on the TiO(2) surface were characterized by time-resolved X-ray absorption and infrared spectroscopies as the temperature of the sample in flowing helium was ramped up. Mass spectra of the evolved gases were also measured during this process. The results show (a) the onset of formation of CH(4) as a decomposition product, (b) the reduction of Au(III) to Au(0), and (c) the formation of Au-Au bonds, all occurring in approximately the same temperature range (about 335-353 K), indicating that the reduction and aggregation of the supported gold are simultaneous processes facilitated by the removal of methyl ligands initially bonded to the gold. IR spectra recorded during the treatment indicate that water on the TiO(2) surface may be involved in the process by reacting with methyl groups bonded to Au(III) to give CH(4).

Journal Article↗
PubMed2006

Morphology of gold nanoparticles synthesized by filamentous cyanobacteria from gold(I)-thiosulfate and gold(III)--chloride complexes.

Plectonema boryanum UTEX 485, a filamentous cyanobacterium, has been reacted with aqueous Au(S(2)O(3))(2)(3)(-) and AuCl(4)(-) solutions ( approximately 400-550 mg/L Au) at 25-100 degrees C for up to 1 month and at 200 degrees C for 1 day. The interaction of cyanobacteria with aqueous Au(S(2)O(3))(2)(3)(-) promoted the precipitation of cubic (100) gold nanoparticles (<10-25 nm) at membrane vesicles and admixed with gold sulfide within cells and encrusted on the cyanobacteria, whereas reaction with AuCl(4)(-) resulted in the precipitation of octahedral (111) gold platelets ( approximately 1-10 microm) in solutions and nanoparticles of gold (<10 nm) within bacterial cells. Functional groups imaged by negative ion TOF-SIMS on (111) faces of the octahedral platelets were predominantly Cl and CN, with smaller amounts of C(2)H and CNO.

Journal Article↗
PubMed2006

Toward rational construction of gold, gold-silver, and gold-mercury string complexes: syntheses, structures, and properties of [Au(Tab)2]2L2 (L = I and PF6), {[(Tab)2M][Au(CN)2]}2 (M = Au and Ag), and {[Hg(Tab)2][Au(CN)2]2} [Tab = 4-(trimethylammonio)benzenethiolate].

The reaction of AuI with 2 equiv of TabHPF6 [TabH = 4-(trimethylammonio)benzenethiol] in the presence of excess Et3N in dimethylformamide (DMF)/MeOH afforded a binuclear gold(I) complex [Au(Tab)2]2I2.2H2O (1). Anion exchange of 1 with NH4PF6 in DMF gave rise to the more soluble complex [Au(Tab)2]2(PF6)2 (2). Treatment of 2 with K[Au(CN)2] produced a tetranuclear gold(I) complex {[(Tab)2Au][Au(CN)2]}2 (3). Analogous reactions of two known mononuclear complexes [Ag(Tab)2](PF6) (4) and [Hg(Tab)2](PF6)2 (5) with 1 or 2 equiv of K[Au(CN)2] generated one Ag2Au2 complex {[(Tab)2Ag][Au(CN)2]}2 (6) and one Au/Hg complex {[Hg(Tab)2][Au(CN)2]2} (7), respectively. Compounds 1-3, 6, and 7 were fully characterized by elemental analysis, IR spectra, UV-vis spectra, 1H NMR, and single-crystal X-ray crystallography. 1 and 2 have a similar [Au(Tab)2]2(2+) dimeric structure in which the two [Au(Tab)2]+ cations are connected via one Au-Au aurophilic interaction. In the structure of 3 or 6, each of the two pairs of [M(Tab)2]+ cation and [Au(CN)2]- anion is held together via ionic interactions to form a {[(Tab)2M][Au(CN)2]} species (M = Au, 3; Ag, 6). Two such species are further connected by one Au-Au aurophilic bonding interaction to form an uncommon Au(4) or Ag2Au2 linear string structure with three ligand-unsupported metal-metal bonds. For 7, the [Hg(Tab)2]2+ dication and the [Au(CN)2]2(2-) dianion are interconnected by the secondary Hg...N(CN) interactions to form a 1D chain structure. The thermal and luminescent properties of 1-3, 6, and 7 in solid state were also investigated.

Journal Article↗
PubMed2006

Electrogenerated chemiluminescence of luminol on a gold-nanorod-modified gold electrode.

Electrogenerated chemiluminescence (ECL) of luminol on a gold-nanorod-modified gold electrode was studied, and five ECL peaks were obtained under conventional cyclic voltammetry in both neutral and alkaline solutions. Among them, four ECL peaks (ECL-1-4) were also observed on a gold-nanosphere-modified gold electrode, but the intensities of these ECL peaks were enhanced about 2-10-fold on a gold-nanorod-modified gold electrode in neutral solution. One new strong ECL peak (ECL-5) was obtained at -0.28 V (vs SCE) on a gold-nanorod-modified gold electrode in both neutral and alkaline solutions and enhanced with an increase in pH. In strong alkaline solutions, ECL-1 and ECL-2 on a gold-nanosphere-modified electrode were much stronger than those on a gold-nanorod-modified gold electrode, while ECL-3-5 appeared to only happen on a gold-nanorod-modified gold electrode. The emitter of all the ECL peaks was identified as 3-aminophthalate. The ECL peaks were found to depend on the scan direction, the electrolytes, the pH, and the presence of O(2) and N(2). The reaction pathways for ECL-4 have been further elucidated, and the mechanism of the new ECL peak (ECL-5) has been proposed. The results indicate that a gold-nanorod-modified gold electrode has a catalytic effect on luminol ECL different from that of a gold-nanosphere-modified gold electrode, revealing that the shape of the metal nanoparticles has an important effect on the luminol ECL behavior. The strong ECL of luminol in neutral solution obtained on a gold-nanorod-modified electrode may be used for the sensitive detection of biologically important compounds in physiological conditions.

Bromides↗
PubMed1999

Prevalence of gold sensitivity in asymptomatic individuals with gold dental restorations.

BACKGROUND: The clinical relevance of positive patch test reactions to gold sodium thiosulfate in asymptomatic individuals with gold dental restorations is often unclear. Knowledge of the prevalence of gold sensitivity in individuals with and without gold dental restorations is required to better understand the relevance of these reactions. OBJECTIVE: To determine the prevalence of positive patch test reactions to gold in asymptomatic individuals with gold dental restorations (gold patients) compared with similar individuals without gold dental appliances (nongold patients). METHODS: One hundred thirty-six healthy, asymptomatic patients were patch tested to gold sodium thiosulfate, nickel sulfate and palladium chloride. Readings occurred after 2 days and 7 days. RESULTS: Of the patients tested, 24 of 71 (33.8%) gold patients had a positive reaction to gold versus 7 of 65 (10.8%) of the nongold patients, P <.001. Of those with a positive gold reaction, 12 of 31 (38.7%) also had a positive nickel reaction. Nickel alone was positive in 18 of 71 (25. 4%) of gold patients versus 11 of 65 (16.9%) of nongold patients. 19 of 29 (65.5%) of those with a positive nickel reaction also reacted to palladium and 19 of 22 (86.4%) of those with a palladium reaction also reacted to nickel. The rate of allergy to gold computed over a 3-year period for patients patch tested in the Oregon Health Sciences University (OHSU) Contact Dermatitis Clinic was 13.5% (46/342). CONCLUSIONS: The prevalence of gold sensitivity in individuals with gold dental restorations is approximately 33.8%. This is significantly greater than the 10.8% prevalence seen in individuals without gold dental appliances, as well as greater than the 3-year rate from the OHSU Contact Dermatitis Clinic. This data should help shed light on issues of clinical relevance.

Adult↗
PubMed1992

Characterization of gold in urine and bile following administration of gold sodium thiomalate with chelating agents to rats.

Gold was characterized in the urine and bile of rats treated with D-penicillamine (D-PEN), 2,3-dimercaptosuccinic acid (DMSA), 2,3-dimercaptopropane sulphonate (DMPS), or N-(2-mercapto-2-methylpropanoyl)-L-cysteine (bucillamine) immediately after gold sodium thiomalate (AuTM) injection by both gel chromatographic and electrophoretic methods. It is suggested that the gold in the urine and bile after AuTM administration was predominantly bound to high molecular weight compounds. The characterization of gold in the urine after administration of AuTM with D-PEN, DMSA, or DMPS showed that most of the gold was bound to the chelating agents. In the treatment with the chelating agents such as D-PEN and DMPS, the gold was mainly excreted as a gold-chelating agent compound in the bile and a minor portion of the gold was present in the form of a gold-L-cysteine compound and high molecular weight compounds. DMSA treatment showed that a major portion of the gold was bound to high molecular weight compounds in the bile and a minor portion of the gold was present in the forms of gold-DMSA and gold-L-cysteine compounds. The administration of AuTM and bucillamine indicated that the gold was mainly present as a gold-Me-bucillamine compound in the urine and a gold-bucillamine compound in the bile.

Animals↗