Coexistence of pressure-induced structural phases in bulk black phosphorus: a combined x-ray diffraction and Raman study up to 18 GPa.

We report a study of the structural phase transitions induced by pressure in bulk black phosphorus by using both synchrotron x-ray diffraction for pressures up to 12.2 GPa and Raman spectroscopy up to 18.2 GPa. Very recently black phosphorus attracted large attention because of the unique properties of few-layers samples (phosphorene), but some basic questions are still open in the case of the bulk system. As concerning the presence of a Raman spectrum above 10 GPa, which should not be observed in an elemental simple cubic system, we propose a new explanation by attributing a key role to the non-hydrostatic conditions occurring in Raman experiments. Finally, a combined analysis of Raman and XRD data allowed us to obtain quantitative information on presence and extent of coexistences between different structural phases from ~5 up to ~15 GPa. This information can have an important role in theoretical studies on pressure-induced structural and electronic phase transitions in black phosphorus.

Multienergy anomalous diffuse scattering.

A new approach to local structure determination is presented. A three-dimensional region of the reciprocal space of a SrTiO(3) single crystal was mapped by measuring x-ray diffuse scattering patterns at different sample orientations in order to reconstruct the local atomic structure. The phase problem was solved by means of anomalous scattering from strontium atoms at photon energies near their K absorption edge. Real-space reconstruction provides the average short-range order atomic arrangement in the vicinity of anomalous scatterers up to a distance of several unit cells.

Erythromycin-resistant Streptococcus pyogenes in Argentina

Erythromycin (ERY) resistance in Streptococcus pyogenes has recently emerged as a problem of growing concern all through the world. We are presenting the comparison of results of the continuous surveillance of erythromycin resistance in S. pyogenes performed since 1989 in the Hospital de Pediatría J.P.Garrahan of Buenos Aires City, with independently observed rates in other five centers of Buenos Aires and seven centers of six other Argentinian cities, obtained between 1999 and 2001. A significant increase of erythromycin resistance was observed among S. pyogenes isolated in the Hospital Garrahan (6.6% in 1998-1999 to 9.9% in 2000). Similar trends were also detected in other centers of other Argentinian cities when recent data were compared to results of a multicenter study performed in 1995. However, lower rates of resistance were recorded in Mendoza, Cipolletti and Neuquén in comparison with data of 1995, 1998 and 1998 respectively. The reason of such decreasing resistance rates deserves to be investigated. The average of ERY-resistance rates obtained in the surveyed centers was 6.7% (range 0.5-14.1%). Control of antimicrobial use should be performed to warrant the future effectiveness of macrolide antibiotics regarding the positive association between use and resistance. These results also suggest that susceptibility tests for macrolides should be performed whenever S. pyogenes is isolated in Argentina.

La resistencia a la eritromicina en Streptococcus pyogenes ha emergido en los últimos tiempos como un problema creciente en todo el mundo. En este trabajo se presenta la comparación de los resultados de la vigilancia continua de la resistencia a la eritromicina que se viene realizando en el Hospital de Pediatría J.P.Garrahan de Buenos Aires desde 1989, con resultados independientes de otros cinco centros de la ciudad de Buenos Aires y siete de otras seis ciudades argentinas, obtenidos entre 1999 y 2001. Se observó un aumento significativo en el Hospital Garrahan (6.6% en1998-1999 a 9.9% en el año 2000) y una tendencia similar en otros centros de diversas ciudades argentinas si secomparan estos datos con los de un estudio multicéntrico realizado en 1995. No obstante, se registraron menoresporcentajes de resistencia en Mendoza, Neuquén y Cipolletti, en relación a lo hallado en 1995, 1998 y 1998respectivamente. La razón de esta disminución merece ser investigada. El porcentaje promedio de resistencia aeritromicina obtenido en los distintos centros participantes de este estudio fue de 6.7% (rango 0.5-14.1%). Debeefectuarse un control en el uso de estos antibióticos para garantizar la efectividad futura de los macrólidos, teniendo en cuenta la asociación estrecha entre uso y resistencia. Estos resultados sugieren que deberían realizarse pruebas de sensibilidad a los macrólidos para todos los aislamientos de S. pyogenes en la Argentina.

Erythromycin-resistant Streptococcus pyogenes in Argentina

Erythromycin (ERY) resistance in Streptococcus pyogenes has recently emerged as a problem of growing concern all through the world. We are presenting the comparison of results of the continuous surveillance of erythromycin resistance in S. pyogenes performed since 1989 in the Hospital de Pediatría J.P.Garrahan of Buenos Aires City, with independently observed rates in other five centers of Buenos Aires and seven centers of six other Argentinian cities, obtained between 1999 and 2001. A significant increase of erythromycin resistance was observed among S. pyogenes isolated in the Hospital Garrahan (6.6% in 1998-1999 to 9.9% in 2000). Similar trends were also detected in other centers of other Argentinian cities when recent data were compared to results of a multicenter study performed in 1995. However, lower rates of resistance were recorded in Mendoza, Cipolletti and Neuquén in comparison with data of 1995, 1998 and 1998 respectively. The reason of such decreasing resistance rates deserves to be investigated. The average of ERY-resistance rates obtained in the surveyed centers was 6.7% (range 0.5-14.1%). Control of antimicrobial use should be performed to warrant the future effectiveness of macrolide antibiotics regarding the positive association between use and resistance. These results also suggest that susceptibility tests for macrolides should be performed whenever S. pyogenes is isolated in Argentina.(AU)

La resistencia a la eritromicina en Streptococcus pyogenes ha emergido en los últimos tiempos como un problema creciente en todo el mundo. En este trabajo se presenta la comparación de los resultados de la vigilancia continua de la resistencia a la eritromicina que se viene realizando en el Hospital de Pediatría J.P.Garrahan de Buenos Aires desde 1989, con resultados independientes de otros cinco centros de la ciudad de Buenos Aires y siete de otras seis ciudades argentinas, obtenidos entre 1999 y 2001. Se observó un aumento significativo en el Hospital Garrahan (6.6% en1998-1999 a 9.9% en el año 2000) y una tendencia similar en otros centros de diversas ciudades argentinas si secomparan estos datos con los de un estudio multicéntrico realizado en 1995. No obstante, se registraron menoresporcentajes de resistencia en Mendoza, Neuquén y Cipolletti, en relación a lo hallado en 1995, 1998 y 1998respectivamente. La razón de esta disminución merece ser investigada. El porcentaje promedio de resistencia aeritromicina obtenido en los distintos centros participantes de este estudio fue de 6.7% (rango 0.5-14.1%). Debeefectuarse un control en el uso de estos antibióticos para garantizar la efectividad futura de los macrólidos, teniendo en cuenta la asociación estrecha entre uso y resistencia. Estos resultados sugieren que deberían realizarse pruebas de sensibilidad a los macrólidos para todos los aislamientos de S. pyogenes en la Argentina.(AU)

X-ray absorption holography.

The transmission of monochromatic x rays through a CoO single crystal was measured for different orientations of the sample. The small variations in the linear absorption coefficient were considered as a hologram and the real-space image of the local atomic environment was successfully reconstructed. The holographic signal constituted about 1% of the detected intensity. Besides other benefits, the use of the absorption holography can increase the signal-to-background ratio by more than 1 order compared with the fluorescence holography.

Determination by MAD-DM of the structure of the DNA duplex d[ACGTACG(5-BrU)]2 at 1.46 A and 100 K.

A four-wavelength MAD experiment on a new brominated octanucleotide is reported here. d[ACGTACG(5-BrU)], C77H81BrN30O32P7, Mr (DNA) = 2235, tetragonal, P43212 (No. 96), a = 43.597, c = 26.268 A, V = 49927.5 A3, Z = 8, T = 100 K, R = 10.91% for 4312 reflections between 15.0 and 1.46 A resolution. The self-complementary brominated octanucleotide d[ACGTACG(5-BrU)]2 has been crystallized and data measured to 1.45 A at both 293 K and a second crystal flash frozen at 100 K. The latter data collection was carried out to the same resolution at the four wavelengths 0.9344, 0.9216, 0.9208 and 0.9003 A, around the Br K edge at 0.92 A and the structure determined from a map derived from a MAD data analysis using pseudo-MIR methodology, as implemented in the program MLPHARE. This is one of the first successful MAD phasing experiments carried out at Sincrotrone Elettra in Trieste, Italy. The structure was refined using the data measured at 0.9003 A, anisotropic temperature factors and the restrained least-squares refinement implemented in the program SHELX96, and the helical parameters are compared with those previously determined for the isomorphous d(ACGTACGT)2 analogue. The asymmetric unit consists of a single strand of octamer with 96 water molecules. No countercations were located. The A-DNA helix geometry obtained has been analysed using the CURVES program.

Determination of the site of incorporation of cobalt in CoZnPO-CZP by multiple-wavelength anomalous-dispersion crystallography.

Data were collected from a crystal of CoZnPO-CZP {sodium cobalt-zinc phosphate hydrate, Na(6)[Co(0.2)Zn(0.8)PO(4)](6).6H(2)O} using synchrotron radiation at ELETTRA at the inflection point and 'white line' for both the cobalt and zinc K edges, and at 1.45 Å, a wavelength remote from the K edges of both metals. The data were processed using the programs DENZO and SCALEPACK. The CCP4 program suite was used for the scaling of data sets and the subsequent calculation of dispersive difference Fourier maps. Optimal scaling was achieved by using a subset of reflections with little or no contribution from the metal atoms (i.e. which were essentially wavelength independent in their intensities) and using weights based on the sigma's to obtain an overall scale factor in each case. Phases were calculated with SHELXL97 based on the refined structure using a much higher resolution and complete Cu Kalpha data set. An occupancy of 100% by zinc at the two metal-atom sites was assumed. The dispersive difference Fourier map calculated for zinc gave two peaks above the background of similar heights at the expected metal-atom sites. The peak height at the Zn1 site was a little higher than at the Zn2 site. The dispersive difference Fourier map calculated for cobalt gave just one peak above the background, at the Zn1 site, and only a small peak at the Zn2 site, thus indicating that incorporation of cobalt takes place mainly at one site. Refinement of the zinc occupancies using MLPHARE reinforces this conclusion. The chemical environment of each site is discussed.

The beamlines of ELETTRA and their application to structural biology.

Protein crystallographers are nowadays regular users of synchrotron radiation (SR) facilities for several applications. The goal of majority of users is simply to extract more accurate, higher resolution data from existing crystals; they use monochromatic radiation and the rotation method, in order to get a complete survey of the reciprocal space in a short time. In fact the brilliance of SR is essential, due to the weak scattering power of the samples, and because of their sensibility to radiation damage. Over the last few years, however, a general increase of interest for measurements at multiple wavelengths, which exploit the anomalous dispersion for the phase problem (multiwavelength anomalous diffraction--MAD), has generated the need of intense tuneable sources. For these applications, the emphasis is on accurate measurements of the small differences between the intensities of Bragg reflections at various energies across the absorption edge of an element present in the sample. The macromolecular diffraction beamline at ELETTRA, which is now running routinely since spring 1995, has been designed to provide a high flux--highly collimated tuneable X-rays source in the spectral range between 4 and 25 keV. The radiation source is the 57-pole wiggler, which delivers a very intense radiation up to 25 keV, and is shared and used simultaneously with the small angle X-ray scattering (SAXS) beamline. The front-end filter system has a cut-off energy at about 4 keV. The beamline optics consists of a pseudo-channel-cut double-crystal monochromator followed by a double focusing toroidal mirror. The tunability and the stability of the monochromator allows the user to perform MAD experiments, and for this purpose, a fluorescence probe for the exact calibration of the absorption edge is available on-line. The experimental station is based on an imaging plate area detector from MarResearch, with a sensible area of 345 mm in diameter. A cooled N2-stream is available to cool the sample crystal in order to reduce the radiation damage. SAXS is an experimental technique used to derive structural information about supra-molecular assemblies, amorphous materials and partly ordered systems (e.g. size and shape of large molecules). The high-flux SAXS beamline at ELETTRA is mainly intended for time-resolved studies on fast structural transitions in the sub-millisecond time region in solutions and in partly ordered systems, triggered by external or process parameters, with a SAXS resolution between 10 and 1400 A in real space. The source is the already mentioned 57-pole and the SAXS beamline accepts three discrete energies of its spectrum, namely 5.4, 8 and 16 keV. The beamline optics consists of a flat double-crystal monochromator and a double focusing toroidal mirror. A multi-purpose sample stage, movable along an optical table in order to optimise the sample to detect distance, allows to perform fast time-resolved relaxation studies based on temperature- or pressure-jumps as well as stopped flow experiments. Moreover, the users have option to install their own specialised sample surrounding equipment. The optimisation of the beamline with respect to high-flux and consequently high-flux density, allows to perform the following experiments: low contrast solution scattering, grazing incidence surface diffraction, micro-spot scanning, X-ray fluorescence analysis, time-resolved studies > or = 11 microseconds, simultaneous small- and wide-angle measurements on gels, liquid crystals, biopolymers, amorphous materials, muscles.

[Errors of the agar diffusion method to predict Escherichia coli's susceptibility to ampicillin-sulbactam and amoxicillin-clavulanic acid]. / Errores del método de difusión en agar para predecir la susceptibilidad de Escherichia coli frente a ampicilina-sulbactam y amoxicilina-ácido clavulánico.

BACKGROUND: To evaluate the in vitro activity of the ampicillin-sulbactam and amoxicillin-clavulanic acid against Escherichia coli isolations resistant to ampicillin and amoxicillin and the efficacy of the disks of ampicillin sulbactam 10/10 microgram and amoxicillin-clavulanic acid 20/10 micrograms to differentiate the susceptible (S) and resistant (R) isolates. METHODS: We evaluated the in vitro susceptibility of 100 consecutive clinical isolates of ampicillin and amoxicillin resistant E. coli by the broth macrodilution method and disk diffusion test against ampicillin-sulbactam and amoxicillin-clavulanic acid. RESULTS: For amoxicillin-clavulanic acid the 64% of the isolates were susceptible, 34% were moderately susceptible and 2% were resistant. In contrast, the in vitro activity of ampicillin-sulbactam was inferior since 13% of the isolates were susceptible, 24% moderately susceptible and 63% were resistant. By using the disk of ampicillin-sulbactam 10/10 microgram we found a 13% of very major errors and a 44% of minor errors when we consider the actual rules of NCCLS (R < or = 11 mm and S > or = 15 mm). The best results were achieved when we took into account zone size < or = 15 mm as R and > or = 20 mm as S; however, the level of errors was high too (25% minor errors). For the disk of amoxicillin-clavulanic acid 20/10 micrograms we found a 31% of minor errors when using the advised break points (R < or = 13 mm and S > or = 18 mm). CONCLUSIONS: We consider that the disk diffusion tests are not applicable to these combinations when E. coli isolates resistant to aminopenicillin are evaluated. We advise not to extrapolate the results of sensibility or resistance from one combination to the other because it presents a different in vitro activity.