A preliminary study of the metabolism of morphine in patients with liver failure

The Renal Hypothesis, which suggests that patients with kidney failure do not metabolise morphine, has been refuted by work carried out in this department and this study is continued in this thesis. Several solid phase extraction methods for preconcentrating morphine from plasma are assessed and a method which is fast, and gives 90-95% extraction efficiency, is used. An improved synthesis of N-trideuteromethylnormorphine, for use as internal standard, is described, and optimum conditions for derivatisation of morphine using pentafluoroproprionic anhydride are established. The metabolism of morphine in patients with chronic liver failure is investigated by GCMS. The GCMS SIM methodology for the determination of morphine, originally carried out using an HP 5982A instrument, is transferred to an HP MSD and to an MS80RFA magnetic sector instrument. The SIM function of the MS80 is shown to be unreliable, and the fault to lie in the proprietary DS90 software. Preliminary results for one patient with chronic liver failure are interpreted as showing that morphine metabolism in such patients is not impaired

Crystal structure of (E)-2-{[(6-meth­oxy-1,3-benzo­thia­zol-2-yl)imino]­meth­yl}phenol

The title compound, C15H12N2O2S, crystallizes in the ortho­rhom­bic space group Pna21, with two mol­ecules in the asymmetric unit (Z′ = 2). Each mol­ecule consists of a 2-hy­droxy Schiff base moiety linked through a spacer to a 2-amino­benzo­thia­zole moiety. Each mol­ecule contains an intra­molecular hydrogen bond between the –OH group and imine N atom, forming a six-membered ring. The two independent molecules are linked by a pair of C—H⋯O hydrogen bonds, forming dimers with an R 2 2(20) ring motif. These dimers are further lined into sheets in the ab plane by weak inter­molecular C—H⋯N inter­actions. The structure was refined as an inversion twinQatar National Research Fund Grant No. NPRP 7–495-1–094

Ranking very young Pinus radiata families for acoustic stiffness and validation by microfibril angle

International audienceAbstractKey messageAcoustic techniques can be utilised to rank a large population of young trees for stiffness and stability for breeding purposes.IntroductionThis study sought to validate new approaches to rapid, very early screening and selection of radiata pine families, using microfibril angle (MFA) as a reference for comparative purposes.MethodA key feature was tilting the trees at an angle of ∼30° after the initial 12 months of growth in order to force production of opposite wood (OW) and compression wood (CW) and prevent the co-mingling of the two distinctive wood types as occurs ‘at random’ within vertical stems. After 34 months, OW and CW materials were characterised independently for acoustic velocity (V), dynamic modulus of elasticity (MOEdynamic), basic density and longitudinal shrinkage. Finally, MFA were determined with X-ray diffraction.ResultNo phenotypic correlation was observed between OW and CW wood properties. The Spearman ranking correlation between V2 and MFA values in OW was 0.81.ConclusionWe show that families or individual trees with superior wood properties can be screened at this young age using acoustics. Further, the same outcomes can be achieved as with X-ray diffraction (MFA) but more cheaply and rapidly

catena-Poly[[silver(I)-μ-4-aminopyridine] perchlorate]: a 1-D staircase coordination polymer

Reaction of 4-amino­pyridine with silver(I) perchlorate leads to a one-dimensional coordination polymer, {[Ag(C5H6N2)]ClO4}n, in which the amino­pyridine binds through both N atoms. The perchlorate anion is hydrogen bonded to the amino H atoms and inter­acts weakly with the silver(I) atoms (Ag—O > 2.70 Å), both located on inversion centres, and some aromatic H atoms (O—H > 2.55 ÅA), thereby extending the dimensionality of the assembly. This is the first silver complex in which this ligand acts in a bridging mode

Ferromagnetice exchange in bichloride bridged Cu(II) chains: magnetostructural correlations between ordered and disordered systems

The synthesis, structure, magnetic properties, and theoretical analysis of a new phase of dichloro(2-thlaro-3-methylpyridine)copper(II) (2) and its isomorphous analogue dichloro(2bromo-3-methylpyridine)copper(II) (3) are reported. Both complexes crystallize in the orthorhombic space group Pbca and present square pyramidal Cu(II) ions bridged into chains by chloride ions with each,copper(II)-bearing a single pyridine ligand. Variable temperature magnetic Susceptibility measurements were well fit by a uniform one-dimensional ferromagnetic chain model with,2) J = 69.0(7) K, C = 0.487 emu-K/mol-Oe; 3, J = 73.9(4) K, C = 0.463 emu-K/mol-Oe = Hamiltonian). The experimental J-values were confirmed-via theOretical calculations. Comparison to a known disordered polymorph of dichloro(2-chloro-3-inethylpyridine)copper(II), 1, shows marked differences as there are significant antiferromagnetic next-nearest neighbor interactions, in 1 in addition to randomness induced by the disorder which provide a distinctly different magnetic response. The differences in magnetic behavior are attributed principally to the structural difference in the Cu(II) coordination sphere, 1 being significantly closer to trigonal-bipyramidal, whose difference changes both the nearest and next-nearest neighbor interactions

Polynuclear complexes with macrocyclic ligands

A series of polynuclear macrocyclic complexes has been prepared by the Schiff-base condensation of 1,5-diaminopentan-3-ol with 2,6-diformyl-4-methyl-R-phenol (where R = Me or tBu) in the presence of transition metal template ions. The (2 + 2) macrocyclic complexes, containing two or four metal ions, have been characterised by a variety of methods including microanalysis, infrared spectroscopy, cyclic voltammetry, E.I. and FAB mass spectrometry and X-ray crystallography. When the template ion is copper, tetranuclear complexes are obtained. The structures of [Cu₄(μ₄-OH)L1(CH₃CN)₃(ClO₄)₂]⋅ClO₄⋅H₂O and [Cu₄(H₂LVS)(dfmp) ₂Cl(H₂O)₂]⋅BF₄ have been determined; both complexes contain planar tetracopper cations with an exogenous hydroxo donor in the centre of the cavity, bound to all four copper ions. Under appropriate conditions the tetra copper complexes dimerise to form octacopper assemblies and the structure of one of these [{Cu₄(μ₄-O)LV5(ClO₄)}₂]⋅(ClO₄)₂⋅4H₂O is reported. Ligand binding to the exposed faces of these arrays was investigated. Tetranuclear cobalt complexes have also been prepared. The X-ray structure of [Co₄(μ₄-O)LV5(CH₃COO)₄]Cl⋅3H₂O shows that, in contrast to the copper complexes, the cation is not planar and the central exogenous donor is an oxo rather than a hydroxo ligand. Tetracobalt complexes can be obtained at various oxidation levels between Co(II)₄ and Co(III)₄. A series of dicobalt complexes has been synthesised. In contrast to the familiar Robson dinuclear complexes, the cobalt ions are not bridged by phenolate donors but are diagonally disposed in the cavity and bridged by two chloride ions. X-ray crystal structure determinations have been carried out on five of these complexes, each having a core structure of [Co₂(H₄L)Cl₂]. These complexes offer a potential route to the formation of tetra nuclear complexes containing mixed metal ions. Synthetic organic work directed towards the development of new ligands was also undertaken

Synthesis, structure, and magnetic properties of bis(3-amino-2-chloropyridinium) tetrahalocuprate(II) [halide = Cl or Br]

The reaction of CuX₂(X=Cl or Br) with 3-amino-2-chloropyridine in aqueous acids (HX; X=Cl or Br) yields bis(3-amino-2-chloropyridinium)tetrachlorocuprate(II) and bis(3-amino-2- chloropyridinium)tetrabromocuprate(II). Both compounds have been characterized by IR, powder X-ray diffraction, single-crystal X-ray diffraction and temperature dependent magnetic susceptibility. The compounds are isomorphous and exhibit weak antiferromagnetic interactions