An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

A novel series of amido-functionalized amine reagents has been developed, which are designed for the extraction of anionic metal chloride complexes according to the following equationnL((org)) + nH(+) + MClxn- (sic) [(LH)(n)MClx]((org)).The new reagents were investigated for Zn(II), Co(II), and Fe(III) recovery in order to establish conditions under which the selectivity for base metals over Fe(III) could be achieved. They were found to be much stronger than the aliphatic amine benchmark extractant tris(2-ethylhexyl) amine (TEHA), giving good Zn(II) and Co(II) recovery from solutions with high enough pH to precipitate Fe(III). The new reagents also gave improved Zn(II) extraction from solutions with moderate to low chloride concentration so that the selectivity for Zn(II) over Fe(III) might be achieved at [Cl] < 1 M.

The use of "double-headed" phenolic oximes produces a trigonal antiprismatic [Fe(III)(3)](2) cluster with an "internal cavity" filled with an additional Fe(3+) ion. Magnetic measurements reveal that the competition between different exchange interactions leads to a low-spin ground multiplet weakly separated in energy from a complex pattern of low-lying excited levels.

The synthesis and study of a systematic series of phenolic oximes have shown that substitution in the 3-position can greatly affect extractive efficacy. Solid state, solution and gas phase analytical techniques including X-ray crystallography, Electron Paramagnetic Resonance (EPR) and IR spectroscopy and collision induced dissociation mass spectrometry have been assessed for their applicability in interpreting the origins of differences in extractant strength. The dominant substituent effect on pH0.5 is the change in ligand pKa , with the more acidic ligands being stronger extractants. The influence of the 3-substituent on the stabilizing intracomplex H-bonding of their copper(II) complexes also affects extractant strength. The 3-NO2 substituted ligand shows the lowest pH0.5 value due to a combination of its low pKa and a stabilising bifurcated H-bond assembly around the copper(II) centre. Appending an aminomethyl group to the 3-position gives a ligand capable of binding a metal and its attendant anion(s). These metal salt reagents show potential to open up new flowsheets for the processing of high tenor copper feeds.La synthese et l’etude d’une serie systematique d’oximes phenoliques ont montre que la substitution en position-3 pouvait grandement affecter l’efficacite d’extraction. On a evalue des techniques analytiques a l’etat solide, en solution et en phase gazeuse, incluant la cristallographie aux rayons X, la resonance paramagnetique electronique (EPR), la spectroscopie IR et la spectrometrie de masse a dissociation induite par collision pour leur applicabilite dans l’interpretation de l’origine des differences de la force de l’agent d’extraction. L’effet dominant du substituant sur le pH0.5 est le changement de pKa du ligand, les ligands les plus acides etant les agents d’extraction les plus forts. L’influence du substituant-3 sur la liaison-H de l’intracomplexe stabilisant de leurs complexes de cuivre(II) affecte egalement la force de l’agent d’extraction. Le ligand au NO2-3 substitue montre la plus basse valeur de pH0.5 en raison d’une combinaison de son faible pKa et de l’assemblee stabilisante d’un lien H bifurque autour du centre du cuivre(II). Adjoindre un groupe aminomethyle a la position-3 donne un ligand capable de lier un metal et son anion(s) auxiliaire. Ces reactifs metal-sel montrent la possibilite d’ouvrir de nouveaux schemas de procede pour le traitement de charges a haute teneur en cuivre.

Molecular dynamics simulations were performed under conditions of constant volume and temperature and of constant pressure and temperature to elucidate the structure activity relationships of a series of non-ionic surfactant molecules derived from vegetable fat and employed as friction modifiers in commercial engine oils. The simulations show the extent to which intermolecular hydrogen bonding is important in determining the stability of the monolayer formed by the surfactant molecules and show that mono-alkanoyl glyceride molecules are able to pack more efficiently, forming significantly more intermolecular hydrogen bonds and occupying approximately half the volume needed by di-alkanoyl glyceride molecules. Density profiles are presented which show significant mixing of the hydrophobic tail groups and a non-polar solvent. The distribution of torsion angles in the tail groups shows that the conformation is consistent with a liquid at finite temperature rather than a crystal structure. The measured friction coefficients of equimolar solutions of the glycerides show that the efficacy as friction modifiers varies in the order mono-, di- and the tri-oleyl glyceride, which is consistent with the efficacy of film formation predicted by the molecular dynamics calculations.

Nature of acid or basic sites, their amount and distribution of their strength in the zeolitic lattice belong to the most important problem of surface chemistry.The aim of our study was to estimate the location of chemisorbed species in the lattice and to elucidate the role of lattice oxygen types in chemisorption.We have dedicated to carry out our experimental study on well-developed crystals of NaX and NaY with high content of sodium cations and with low content of defects and decationation.Distribution of chemisorbed methyl groups and sodium cations in the structure of NaX and NaY zeolites was studied by neutron diffraction and NMR technique.Chemisorbed methyl groups were prepared in the structure by chemical reaction of methyl iodide with reactive sodium cations available in SII and SIII position of faujasites.The polarized covalent bond of methyl carbon to lattice oxygen resembles methoxy compounds as demonstrated by 13 C NMR signals of chemisorbed surface species at 54 and 56 ppm TMS for NaX and NaY, respectively.Changes in the distribution of structural sodium cations in the lattice after chemisorption of methyl cations has been detected.The location of methyl groups was also estimated.The location at O1 lattice oxygen type was found to be most probable for NaY.Nuclear densities of chemisorbed methyl groups were detected in NaX at O1 and O4 lattice oxygen.

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

A new range of structurally-related macrocyclic ligands have been prepared and their potential as metal-ion discriminating agents examined.

A rapid lutropin assay with a 2-h incubation time and a second antibody/polyethylene glycol separation step is presented. Assay time is shortened by incubating at 37 degrees C and using relatively high concentrations of antibody and radioligand. The interval required for the antigen/antibody reaction varies directly with lutropin concentration, from 1 h for ovulation values to 8 h for low values. After a 2-h incubation, low concentrations have reached 80% of their equilibrium concentration. Separation of the bound fraction by use of combined second antibody/polyethylene glycol (50 g/L) gave one-third the nonspecific binding and as rapid a separation as with polyethylene glycol (180 g/L) alone. Optimal conditions for separating the immune complex were established, and separation was found to be independent of protein concentrations in urine or serum. This tested assay can detect increasing and ovulatory lutropin concentrations in urine or serum, but with some sacrifice in sensitivity.

The title compound, Cu(C10H24N4)(ClO4)2, crystallizes in the triclinic system with unit cell dimensionsa= 8.744,b= 8.022,c= 8.677 Å, α = 118.7, β = 56.9, γ = 113.5 °,Z= 1, space group P¯1. The structure was solved by Fourier methods and refined by least-squares techniques using the 1545 nonzero three-dimensional counter-diffraction intensity data (CuKα) to give a conventionalR factor of 0.056. The coordination sphere of the copper ion is defined by a planar arrangement of the four nitrogen donors in the macrocyclic ligand with oxygen atoms from the perchlorate groups lying above and below this plane. The resulting tetragonally distorted octahedron of donor atoms gives interatomic distances Cu−N = 2.02(4) Å and 2.02(3) Å, and Cu−N = 2.57(4) Å.

AbstractDie Reaktion des Tetraaminobenzols (II) als Hydrochlorid in wasserfreiem Methanol mit dem Dialdehyd (I) bei Rückflußtemperatur liefert den Titelliganden (III), der mit Metallacetaten in Pyridin zu den Komplexen (IV) umgesetzt wird.

AbstractDie Pyridine (I) reagieren mit dem Acetylen (II) in Acetonitril zu den Cyclobutapyridinen (III).

AbstractAus Polyalkoholen (I) werden über die Tosylate (II) und die Azide (III) durch Reduktion mit Lithiumalanat die Polyamine (IV) hergestellt; es werden z.B. in wesentlich verbesserten Ausbeuten die Amine (V)‐(VIII) gewonnen und ihre Konformationen z.Tl. bestimmt.

Several 1,3-disubstituted 1,4-dihydropyridines with dimethyl acetylenedicarboxylate in acetonitrile at room temperature gave 1,4,4a,6a-tetrahydrocyclobuta[b]pyridines and where a 3-carboxy- or a 3-carbamoyl group was present, a novel cycloelimination of this group occurred to give the corresponding 3-(cis-1,2-dimethoxycarbonylvinyl) derivative. 1-Benzyl-1,4-dihydroquinoline-4-carbonitrile gave the 3-(cis-1,2-dimethoxycarbonylvinyl) derivative quantitatively, and 2-benzyl-1,2-dihydroisoquinoline-1-carbonitrile formed a phenanthridine.