Reactivity of 2-ethoxy-5-alkyl-3,4-dihydro-2H-pyrans towards aluminum alkyls : a facile synthesis of cyclobutylmethanols

2-Ethoxy-5-alkyl-3,4-dihydro-2H-pyrans react with Albuⁱ₃ and through a regioselective hydride addition provide substituted cyclobutylmethanols in very good yields.     

Studies on comblike polymers. X. Characterization of comblike polyesters by 13C NMR spectroscopy

The ¹³C NMR spectra of aromatic comblike polyesters obtained from 1,2-icosanediol and isomeric phthalic acids are reported and discussed. The analysis shows that the most informative spectral regions are those of the carbonyl and quaternary carbon resonances, whose peak multiplicities have been interpreted in terms of dyad and triad sequences. The results indicate that the extent of structural characterization possible for the polymers examined is dependent on the type of isomerism of the aromatic acid involved.     

Mechanochemical preparation of hydrogen-bonded adducts between the diamine 1,4-diazabicyclo[2.2.2]octane and dicarboxylic acids of variable chain length: an X-ray diffraction and solid-state NMR study

Mechanical mixing of solid dicarboxylic acids of variable chain length HOOC(CH(2))(n)COOH (n = 1-7) with solid 1,4-diazabicyclo[2.2.2]octane generates the corresponding salts or co-crystals of the formula [N(CH(2)CH(2))(3)N]-H-[OOC(CH(2))(n)COOH] (n=1-7). Preparation of the same systems from solution has been instrumental for a full characterization of the mechanochemical products by means of single-crystal and powder-diffraction X-ray analyses, as well as by solid-state NMR. The acid-base adducts, whether involving proton transfer from the COOH group to the N-acceptor, that is having ((-))O...H-N((+)) interactions, or the formation of neutral O-H...N hydrogen bonds, show a melting point alternation phenomenon analogous to that shown by the neutral carboxylic acids. The carbon chemical shift tensors of the COOH group obtained from the sideband intensity of low speed spinning NMR spectra provide a reliable criterion for assigning the protonation state of the adducts.     

Transverse asymmetry AT' from the quasielastic 3He(e,e') process and the neutron magnetic form factor

We have measured the transverse asymmetry A(T') in 3He(e,e(')) quasielastic scattering in Hall A at Jefferson Laboratory with high precision for Q2 values from 0.1 to 0.6 (GeV/c)(2). The neutron magnetic form factor G(n)(M) was extracted based on Faddeev calculations for Q2 = 0.1 and 0.2 (GeV/c)(2) with an experimental uncertainty of less than 2%.     

Nickel nanostructured materials from liquid phase photodeposition

Liquid Phase Photo-Deposition (LPPD) technique has been used to obtain both colloidal particles and thin films of metallic and chloride nickel from solutions of only precursor Ni(acac)₂ (acac=2,4-pentandionato). Metallic nickel was obtained from ethanol solutions by direct nickel(II) photoreduction at 254 nm and by acetone sensitised reaction at 300 nm. In this latter process the rate was higher than in the first one. NiCl₂ was formed from CCl₄ solution by a solvent-initiated reaction. TEM analysis, performed on colloidal particles of nickel, showed that their dimensions are in the range 2–4 nm. The films did not present carbon contamination and were characterized by AFM, XPS and GIXRD. Metallic films consisted of particles of 20–40 nm that are the result of the aggregation of smaller crystallites (4–5 nm). Larger agglomerations (around 200 nm) have been observed for NiCl₂ films.     

Wave propagation in stereo-lithographical (STL) bone replicas at oblique incidence

Comparisons between predictions of a Biot-Allard model allowing for angle-dependent elasticity and angle-and-porosity dependent tortuosity and transmission data obtained at normal incidence on water-saturated replica bones are extended to oblique incidence. The model includes two parameters which are adjusted for best fit at normal incidence. Using the same parameter values, it is found that predictions of the variation of transmitted waveforms with angle through two types of bone replica are in reasonable agreement with data despite the fact that scattering is not included in the theory.     

A comparative study of the structures, NMR properties and magnetic behaviour of complexes of cobalt(II) with octamethylpyrophosphoramide and nonamethylimidodiphosphoramide

The structure of the complex Co(NIPA)₃(ClO₄)₂ has been determined by X-ray diffraction analysis and found to be very close to that of the corresponding OMPA complex. The magnetic susceptibilities of the OMPA and NIPA complexes have been measured by a thermomagnetic method and have allowed the calculation of χ_| and χ, the susceptibilities along the principal axes of the complex. The magnetic properties of the isomorphous nickel compounds have been studied for comparison. Results give evidence for the greater magnetic anisotropy of the NIPA complexes.     

Metal complexes of C2-symmetric chiral bipyridine ligands. X-ray structure of [bis(nitrato)(4S,5S)-2,2-dimethyl-4,5-bis(2-pyridyl)-1,3-dioxolane cobalt(II)]

Chelating properties of C₂-symmetric chiral bipyridine ligands are discussed. In particular we report the syntheses of the cobalt(II), nickel(II), zinc(II) and copper(II) complexes of (4S,5S)-2,2-dimethyl-4,5-bis(2-pyridyl)-1,3-dioxolane. All compounds have been characterized by IR spectroscopy, and an X-ray diffraction analysis has been carried out on one of them: Co(L)(NO₃)₂. The ligand coordinates the cobalt atom by the two nitrogen donors N(1) and N(2). A seven-membered chelation ring is formed, presenting a remarkable non-crystallographic twofold pseudosymmetry around the axis connecting Co and the midpoint of the C(6)–C(7) bond. The metal also binds two monodentate nitrates, thus completing a distorted coordination tetrahedron.