Synthesis and structural studies of (3,5-dinitrobenzoate)bis(triphenylphosphine)copper(I)

The compound (3,5-dinitrobenzoate)bis(triphenylphosphine)copper(I) was synthesized and studied by IR spectroscopy and X-ray diffraction techniques. It is monomeric with the carboxylato acting as a monodentate ligand. The copper atom shows a trigonal planar coordination geometry. © 1993.

Crystallization and X-ray diffraction data analysis of oxyhemoglobin-I from the catfish Liposarcus anisitsi (pisces)

Hemoglobin remains, despite the enormous amount of research involving this molecule, as a prototype for allosteric models and new conformations. Functional studies carried out on Hemoglobin-I from the South-American Catfish Liposarcus anisitsi [1] suggest the existence of conformational states beyond those already described for human hemoglobin, which could be confirmed crystallographically. The present work represents the initial steps towards that goal.

Crystallization and preliminary X-ray analysis of SIII-SPIII, a ahospholipase A2 isolated from the venom of Bothrops jararacussu

Large single crystals have been obtained of SIII-SPIII, a phospholipase A2 from the venom of Bothrops jararacussu. The crystals belong to the orthorhombic system space group C222, and diffract X-rays to a resolution of 1.9 Å. Preliminary analysis reveals the presence of one molecule in the crystallographic asymmetric unit. The crystal structure is currently being determined using molecular replacement techniques.

Caracterização textural e estrutural de V 2O 5/TiO 2 obtidos via sol-gel: Comparação entre secagem convencional e supercrítica

This work describes a modified sol-gel method for the preparation of V 2O 5/TiO 2 catalysts. The samples have been characterized by N 2 adsorption at 77K, x-ray diffractometry (XRD) and Fourier Transform Infrared (FT-IR). The surface area increases with the vanadia loading from 24 m 2 g -1, for pure TiO 2, to 87 m 2 g -1 for 9wt.% of V 2O 5. The rutile form is predominant for pure TiO 2 but became enriched with anatase phase when vanadia loading is increased. No crystalline V 2O 5 phase was observed in the catalysts diffractograms. Two species of surface vanadium observed by FT-IR spectroscopy a monomeric vanadyl and polymeric vanadates, the vanadyl/vanadate ratio remains practically constant.

Comparative study using small-angle x-ray scattering and nitrogen adsorption in the characterization of silica xerogels and aerogels

A comparative study using small-angle x-ray scattering (SAXS) and nitrogen adsorption has been carried out in the structural characterization of silica xerogels and aerogels, obtained from tetraethoxysilane sonohydrolysis. The specific surface and the mean pore size as measured by both the techniques were found to be in notable agreement in all cases for aerogels and xerogels. According to the SAXS data, aerogels at 500 °C exhibit a mass fractal structure with fractal dimension D∼2.4 in the range between the correlation length ξ∼5.3 nm and a∼0.75 nm. An experimental method to probe the mass fractal structure of aerogels from exclusively nitrogen adsorption isotherms has been presented. For aerogels at 500 °C, we have found D∼2.4 in the range between the pore width 2rξ∼33 nm and 2ra∼4.5 nm, which is in notable agreement with the SAXS results (D ∼2.4, ξ∼5.3 nm, a∼0.75 nm) if we assign the pore width 2r probed by the Kelvin equation in the adsorption method to the Bragg distance 2π/q associated to the correlation length 1/q probed by SAXS.

Performance of the CMS Level-1 trigger during commissioning with cosmic ray muons and LHC beams

The CMS Level-1 trigger was used to select cosmic ray muons and LHC beam events during data-taking runs in 2008, and to estimate the level of detector noise. This paper describes the trigger components used, the algorithms that were executed, and the trigger synchronisation. Using data from extended cosmic ray runs, the muon, electron/photon, and jet triggers have been validated, and their performance evaluated. Efficiencies were found to be high, resolutions were found to be good, and rates as expected. © 2010 IOP Publishing Ltd and SISSA.

CMS data processing workflows during an extended cosmic ray run

The CMS Collaboration conducted a month-long data taking exercise, the Cosmic Run At Four Tesla, during October-November 2008, with the goal of commissioning the experiment for extended operation. With all installed detector systems participating, CMS recorded 270 million cosmic ray events with the solenoid at a magnetic field strength of 3.8 T. This paper describes the data flow from the detector through the various online and offline computing systems, as well as the workflows used for recording the data, for aligning and calibrating the detector, and for analysis of the data. © 2010 IOP Publishing Ltd and SISSA.

Commissioning and performance of the CMS pixel tracker with cosmic ray muons

The pixel detector of the Compact Muon Solenoid experiment consists of three barrel layers and two disks for each endcap. The detector was installed in summer 2008, commissioned with charge injections, and operated in the 3.8 T magnetic field during cosmic ray data taking. This paper reports on the first running experience and presents results on the pixel tracker performance, which are found to be in line with the design specifications of this detector. The transverse impact parameter resolution measured in a sample of high momentum muons is 18 microns. © 2010 IOP Publishing Ltd and SISSA.

Performance of the CMS hadron calorimeter with cosmic ray muons and LHC beam data

The CMS Hadron Calorimeter in the barrel, endcap and forward regions is fully commissioned. Cosmic ray data were taken with and without magnetic field at the surface hall and after installation in the experimental hall, hundred meters underground. Various measurements were also performed during the few days of beam in the LHC in September 2008. Calibration parameters were extracted, and the energy response of the HCAL determined from test beam data has been checked. © 2010 IOP Publishing Ltd and SISSA.

Performance of CMS hadron calorimeter timing and synchronization using test beam, cosmic ray, and LHC beam data

This paper discusses the design and performance of the time measurement technique and of the synchronization systems of the CMS hadron calorimeter. Time measurement performance results are presented from test beam data taken in the years 2004 and 2006. For hadronic showers of energy greater than 100 GeV, the timing resolution is measured to be about 1.2 ns. Time synchronization and out-of-time background rejection results are presented from the Cosmic Run At Four Tesla and LHC beam runs taken in the Autumn of 2008. The inter-channel synchronization is measured to be within 2 ns. © 2010 IOP Publishing Ltd and SISSA.

Aligning the CMS muon chambers with the muon alignment system during an extended cosmic ray run

The alignment system for the muon spectrometer of the CMS detector comprises three independent subsystems of optical and analog position sensors. It aligns muon chambers with respect to each other and to the central silicon tracker. System commissioning at full magnetic field began in 2008 during an extended cosmic ray run. The system succeeded in tracking muon detector movements of up to 18 mm and rotations of several milliradians under magnetic forces. Depending on coordinate and subsystem, the system achieved chamber alignment precisions of 140-350 μm and 30-200 μrad, close to the precision requirements of the experiment. Systematic errors on absolute positions are estimated to be 340-590 μm based on comparisons with independent photogrammetry measurements. © 2010 IOP Publishing Ltd and SISSA.

Performance of CMS muon reconstruction in cosmic-ray events

The performance of muon reconstruction in CMS is evaluated using a large data sample of cosmic-ray muons recorded in 2008. Efficiencies of various high-level trigger, identification, and reconstruction algorithms have been measured for a broad range of muon momenta, and were found to be in good agreement with expectations from Monte Carlo simulation. The relative momentum resolution for muons crossing the barrel part of the detector is better than 1% at 10 GeV/c and is about 8% at 500 GeV/c, the latter being only a factor of two worse than expected with ideal alignment conditions. Muon charge misassignment ranges from less than 0.01% at 10GeV/c to about 1% at 500 GeV/c. © 2010 IOP Publishing Ltd and SISSA.

Integrated X-ray crystallography, optical and computational methods in studies of structure and luminescence of new synthesized complexes of lanthanides with ligands derived from 2,6-diformylpyridine

The reaction of 2,6-diformylpyridine-bis(benzoylhydrazone) [dfpbbh] and 2,6-diformylpyridine-bis(4-phenylsemicarbazone) [dfpbpsc] with lanthanides salts yielded the new chelates complexes [Eu(dfpbpsc-H +) 2]NO 3 (1), [Dy(fbhmp) 2][Dy(dfpbbh-2H +) 2]·2EtOH·2H 2O (fbhmp = 2-formylbenzoylhydrazone-6-methoxide-pyridine; Ph = phenyl; Py = pyridine; Et = ethyl) and [Er 2(dfpbbh-2H +) 2(μ-NO 3)(H 2O) 2(OH)]·H 2O. X-ray diffraction analysis was employed for the structural characterization of the three chelate complexes. In the case of complex 1, optical, synthetic and computational methods were also exploited for ground state structure determinations and triplet energy level of the ligand and HOMO-LUMO calculations, as well as for a detailed study of its luminescence properties. © 2010 Elsevier Ltd. All rights reserved.

In vitro assessment of dentin erosion after immersion in acidic beverages: Surface profile analysis and energy-dispersive X-ray fluorescence spectrometry study

The aim of this study was to investigate the effects of some acidic drinks on dentin erosion, using methods of surface profile (SP) analysis and energy-dispersive X-ray fluorescence spectrometry (EDXRF). One hundred standardized dentin slabs obtained from bovine incisor roots were used. Dentin slabs measuring 5x5 mm were ground flat, polished and half of each specimen surface was protected with nail polish. For 60 min, the dentin surfaces were immersed in 50 mL of 5 different drinks (Gatorade®, Del Valle Mais orange juice®, Coca-Cola®, Red Bull® and white wine), 20 blocks in each drink. The pH of each beverage was measured. After the erosive challenge, the nail polish was removed and SP was analyzed. The mineral concentration of dentin surfaces was determined by means of EDXRF. Data were analyzed statistically by ANOVA and Tukey's test (α=0.05). SP analysis showed that Red-Bull had the highest erosive potential (p<0.05). EDXRF results exhibited a decrease in phosphate in the groups immersed in Red-Bull, orange juice and white wine (p<0.05), and no significant difference in calcium content between the reference surface and eroded surface. In conclusion, this study demonstrated that all studied beverages promoted erosion on root dentin and Red Bull had the highest erosive potential. There was no correlation between pH of beverages and their erosive potential and only the P content changed after erosive challenge.

Synthesis, crystal structure and photoluminescence of a binuclear complex of europium(III) containing 3,5-dicarboxypyrazolate and succinate

The new europium binuclear complex [Eu2(dcpz) 2(suc)(H2O)8]·(H2O) 1.5 (dcpz = 3,5-dicarboxypyrazolate and suc = succinate) has been synthesized and structurally characterized by single crystal X-ray diffraction methods. The binuclear complex crystallizes in the triclinic space group P1̄ and consists of two lanthanide ions linked by two different bridging organic ligands. 3D supramolecular framework is constructed by hydrogen bonds. The compound shows strong red emission under UV excitation at room temperature associated to IL transitions indicating a ligand to metal energy transfer mechanism since the triplet energy level lies higher than that of europium 5D0 level. Magnetic susceptibility studies showed weak temperature dependence characteristic of the Van Vleck paramagnetism. © 2013 Elsevier Ltd. All rights reserved.