The reaction of 2-picoline N-Oxide with o-substituled benzoates and lsatoic anhydrides

The reaction of 2-picoline N-Oxide anion with o-substituted henzoates and isatoic anhydrides to give synthetically useful l-(2-methoxyphenyl)-2-(2-pyridinyl)ethanone N-oxides, I-(2-hydroxy-phenyJ)-2-(2-pyridinyl)ethanone N-oxides and I -(2-arninopheny])-2-(2-pyridinyl)ethanone N-oxides is described.     

Analysis of 19-norandrosterone in human urine by gas chromatography–isotope-dilution mass spectrometry: method adopted by LGC for participation in the Comité Consultatif pour la Quantité de Matière (CCQM) Pilot Study P68

The method used at LGC for analysis of “total” 19-norandrosterone (19-norandrosterone glucuronide plus “free” 19-norandrosterone) in urine for the Comité Consultatif pour la Quantité de Matière Pilot Study (CCQM-P68) is described. The analytical method used was a modified version of the method developed at the National Measurement Institute of Australia, which used a hydrolysis and derivatisation procedure first described by the German Sports University. This method is routinely used by World Anti-Doping Agency-accredited laboratories for sports drug testing. The main modifications made to the method were the use of 19-norandrosterone glucuronide as a calibration standard and 19-norandrosterone glucuronide-d4 as an isotopically labelled internal standard, and the use of a bench-top quadrupole gas chromatograph–mass spectrometer. The results produced by LGC (2.14 ± 0.15 ng g⁻¹ expanded uncertainty, coverage factor k = 2) were in excellent agreement with those from other participating national metrology institutes and thus further validates the exact-matching isotope-dilution mass spectrometric procedures used at LGC for a wide range of reference measurement applications, including measurement of ng g⁻¹ levels of steroids in a biological matrix.     

The structure of 1-formyl-3-phenyl-Δ-pyrazoline in the gas phase (DFT calculations), in solution (NMR) and in the solid state (X-ray crystallography)

The molecular structure of 1-formyl-3-phenyl-Δ²-pyrazoline was determined by X-ray crystallography (triclinic, P-1). The geometry thus obtained was compared with that obtained by DFT calculations. The GIAO method was used to calculate absolute shieldings, which agree conveniently with those measured by ¹³C and ¹⁵N NMR. The title compound appears to be an essentially planar molecule.     

Synthesis and X-ray crystal structure determination of first examples of donor-functionalized terphenyl lanthanide complexes

The molecular structures of novel donor-functionalized terphenyl derivatives of trivalent ytterbium, yttrium, and samarium of composition [DanipYb(mu2-Cl)2(mu3-Cl)Li(THF)]2 (1) and [DanipLn(mu2-Cl)2(mu2-Cl)Li(THF)2]2 (Ln = Y, 2; Ln = Sm, 3) are reported [Danip = 2,6-di(o-anisol)phenyl]. The complexes are obtained from the reaction of equimolar amounts of DanipLi and LnCl3 (Ln = Yb, Y, Sm) in tetrahydrofuran at room temperature in 60% yield. 1-2 toluene crystallizes in the monoclinic space group Ponebar. Crystal data for 1-2 toluene at 203 K: a = 9.7281(9) A; b = 12.7989(12) A; c = 13.4870(12) A; alpha = 91.553(2) degrees; beta = 103.957(2) degrees; gamma = 109.916(2) degrees; V = 1521.2(2) A(3); Z' = 1; D(calcd) = 1.615 g cm(-3); R1 = 3.43%. 2-toluene crystallizes in the monoclinic space group Ponebar. Crystal data for 2-toluene at 203 K: a = 10.4152(10) A; b = 12.5783(12) A; c = 14.4640(14) A; alpha = 69.963(2) degrees; beta = 80.900(2) degrees; gamma = 66.603(2) degrees; V = 1633.3(3) A(3); Z' = 1; D(calcd) = 1.386 g cm(-3); R1 = 4.07%. 3-toluene crystallizes in the monoclinic space group Ponebar. Crystal data for 3-toluene at 203 K: a = 10.3457(8) A; b = 12.5658(10) A; c = 14.4365(11) A; alpha = 70.2250(10) degrees; beta = 81.2820(10) degrees; gamma = 66.8330(10) degrees; V = 1623.3(2) A(3); Z' = 1; D(calcd) = 1.521 g cm(-3); R1 = 3.40%. Complexes 1-3 represent first examples of donor-functionalized terphenyl complexes of the elements ytterbium, yttrium, and samarium, respectively. The molecular structures of 1-3 feature a "constraint geometry" type arrangement of the Danip ligand at the lanthanide atom. The complexes reported are dimeric and composed of lithium chloride bridged DanipLnCl(2) moieties (Ln = Yb, Y, Sm), stabilized through additional coordination of two methoxy functions to the lanthanide atom.     

Temperature and density measurements in a non-axisymmetric,continuously operating fusion experiment using a heavy ion beam probe

Two-dimensional electron temperature and density data have been obtained in the midplane of the non-axisymmetric magnetic confinement device ELMO Bumpy Torus (EBT) through the use of a heavy ion beam probe. This beam probe differs from others operated on toroidal or open magnetic geometries in its combination of complete computer control with the steady-state nature of EBT which allows, under normal operating conditions, for extensive calibration of the system in situ, minimizing both alignment and acquisition errors, along with the use of synchronous detection to dramatically improve the quality of the detected signal over what is typically possible in fast pulse devices. These techniques are important and applicable to long pulse devices where the beam probe may be an ideal diagnostic to measure, for example, parameters of the edge plasma. While the EBT beam probe was implemented to obtain profiles of plasma space potential, we have found that it can also be used effectively to measure the temperature and density profiles in the midplane between magnetic field coils. The data obtained support the contention that the formation of a hollow temperature profile in the T-Mode sufficiently inverts the plasma pressure such that stability of the core plasma would be expected even without diamagnetic effects from the hot electron rings which have previously been considered essential     

Packing two graphs of ordern having total size at most 2n − 2

Two graphsG andH of the same order are packable ifG can be embedded in the complement ofH. In this paper we give a complete characterization of two graphs of ordern having total size at most 2n – 2 which are packable. This result extends an earlier result of B. Bollobás and S.E. Eldridge.     

Associations between Neurocardiovascular Signal Entropy and Physical Frailty

In this cross-sectional study, the relationship between noninvasively measured neurocardiovascular signal entropy and physical frailty was explored in a sample of community-dwelling older adults from The Irish Longitudinal Study on Ageing (TILDA). The hypothesis under investigation was that dysfunction in the neurovascular and cardiovascular systems, as quantified by short-length signal complexity during a lying-to-stand test (active stand), could provide a marker for frailty. Frailty status (i.e., “non-frail”, “pre-frail”, and “frail”) was based on Fried’s criteria (i.e., exhaustion, unexplained weight loss, weakness, slowness, and low physical activity). Approximate entropy (ApEn) and sample entropy (SampEn) were calculated during resting (lying down), active standing, and recovery phases. There was continuously measured blood pressure/heart rate data from 2645 individuals (53.0% female) and frontal lobe tissue oxygenation data from 2225 participants (52.3% female); both samples had a mean (SD) age of 64.3 (7.7) years. Results revealed statistically significant associations between neurocardiovascular signal entropy and frailty status. Entropy differences between non-frail and pre-frail/frail were greater during resting state compared with standing and recovery phases. Compared with ApEn, SampEn seemed to have better discriminating power between non-frail and pre-frail/frail individuals. The quantification of entropy in short length neurocardiovascular signals could provide a clinically useful marker of the multiple physiological dysregulations that underlie physical frailty.