Bis(1,10‐phenanthroline‐N,N′)(thiosulfato‐O,S)­nickel(II)–water–methanol (1/0.92/1.4) and bis(2,2′‐bi­pyridyl‐N,N′)(thiosulfato‐O,S)nickel(II)–water–methanol (1/2/0.55)

The title compounds, [Ni(S₂O₃)­(C₁₂H₈N₂)₂]·­0.92H₂O·­1.4CH₄O and [Ni(S₂O₃)­(C₁₀H₈N₂)₂]·­2H₂O·­0.55CH₄O, are monomeric, containing nickel(II) in a distorted octahedral coordination environment provided by the four N atoms of two bidentate bipy or phen groups and one S and one O atom from a chelating thio­sulfate anion. The crystals are highly unstable outside their mother liquors and are stabilized in solution by a not fully determined number of water and methanol solvate mol­ecules. The phenanthroline structure includes two independent moieties related by a non‐crystallographic inversion center. The thio­sulfate anions display the usual S—O lengthening found when the anion acts in a bidentate mode.     

Multi-use NBD-based tetra-amino macrocycle: fluorescent probe for metals and anions and live cell marker

Ligand L (4-(7-nitrobenzo[1,2,5]oxadiazole-4-yl)-1,7-dimethyl-1,4,7,10-tetra-azacyclododecane) is a versatile fluorescent sensor useful for Cu(II), Zn(II) and Cd(II) metal detection, as a building block of fluorescent metallo-receptor for halide detection, and as an organelle marker inside live cells. Ligand L undergoes a chelation-enhanced fluorescence (CHEF) effect upon metal coordination in acetonitrile solution. In all three complexes investigated the metal cation is coordinatively unsaturated; thus, it can bind secondary ligands as anionic species. The crystal structure of [ZnLCl](ClO(4)) is discussed. Cu(II) and Zn(II) complexes are quenched upon halide interaction, whereas the [CdL](2+) species behaves as an OFF-ON sensor for halide anions in acetonitrile solution. The mechanism of the fluorescence response in the presence of the anion depends on the nature of the metal ion employed and has been studied by spectroscopic methods, such as NMR spectroscopy, UV/Vis and fluorescence techniques and by computational methods. Subcellular localization experiments performed on HeLa cells show that L mainly localizes in spot-like structures in a polarized portion of the cytosol that is occupied by the Golgi apparatus to give a green fluorescence signal.     

A new equation for the thermal conductivity of organic compounds

This work presents a wide literature survey of the available data of the experimental thermal conductivity data of organic liquids. The experimental data were collected for 136 compounds belonging to the following families: refrigerants, alkanes, alkenes, aromatics, cycloalkanes, cycloalkenes, ethers, esters, ketones, carboxylic acids, and alcohols. The experimental data were regressed with the most reliable semi-empirical correlating methods existing in the literature and a reliable set of 4,584 experimental data was finally selected. The influence of several physical parameters on the thermal conductivity calculation is discussed and a new equation to represent the thermal conductivity of organic liquids at atmospheric pressure for temperatures below normal boiling point and at saturation for temperatures above the normal boiling point is presented. To minimize the deviation between the predictions and the experimental data and to find the optimal coefficients for the proposed equation, a statistical analysis was performed. The resulting equation is simple and is able to predict the thermal conductivities with low deviations for the major part of the collected data for the studied families.     

A comparative study of immunoglobulin IgM and rheumatoid factor IgMRF in solution by small-angle X-ray scattering

The shapes of rheumatoid factor molecules calculated from X-ray small-angle solution scattering data suggest that the peripheral Fab regions of rheumatoid factor in solution are more flocculent because of a higher flexibility of Fab domains.     

Aripiprazole salts. I. Aripiprazole nitrate

The crystal structure of aripiprazole nitrate (systematic name: 4‐(2,3‐dichlorophenyl)‐1‐{4‐[(2‐oxo‐1,2,3,4‐tetrahydroquinolin‐7‐yl)oxy]butyl}piperazin‐1‐ium nitrate), C₂₃H₂₈Cl₂N₃O₂⁺·NO₃⁻ or AripH⁺·NO₃⁻, is presented and the molecule compared with the aripiprazole molecules reported so far in the literature. Bond distances and angles appear very similar, except for a slight lengthening of the C—NH distances involving the protonated N atom, and the main differences are to be found in the molecular spatial arrangement (revealed by the sequence of torsion angles) and the intermolecular interactions (resulting from structural elements specific to this structure, viz. the nitrate counter‐ions on one hand and the extra protons on the other hand as hydrogen‐bond acceptors and donors, respectively). The result is the formation of [100] strips, laterally linked by weak π–π and C—Cl...π interactions, leading to a family of undulating sheets parallel to (010).     

REACTION OF (ORGANYLTHIO)CHLOROACETYLENES WITH ALIPHATIC 1,2-DITHIOLS: A ROUTE TO FUNCTIONALIZED 1,3-DITHIOLANES

(Organylthio)chloroacetylenes react with aliphatic 1,2-dithiols in dimethyl sulfoxide at 20–25°C in the presence of a two-fold molar excess of alkali to form 2-[(alkylthio)methyliden]-1,3-dithiolanes in up to 66% yield.     

New tethered ansa‐bridged zirconium catalysts: Insights into the “self‐immobilization” mechanism

New ω‐alkenyl‐substituted ansa‐bridged bisindenyl zirconium complexes are prepared and tested as self‐immobilized catalysts for ethene polymerization. But, even at very high concentration of the tethered complexes and low pressure of ethene, there is no evidence of their insertion into the polyethene chain. A “cross polymerization” test, performed by copolymerizing the tethered complexes with ethene using rac‐Me₂Si(2‐MeBenzInd)₂ZrCl₂ ( MBI ), does not lead to their incorporation into the polyethene chain. However, the corresponding ligand proves to be a suitable comonomer for ethene, and, through copolymerization promoted by MBI, innovative poly(ethene‐co‐2,2′‐bis[(1H‐inden‐3′‐yl)‐hex‐5‐ene) copolymers are prepared and characterized by ¹³C NMR. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2013     

The study of the mural painting in the 12th century monastery of Santa Maria delle Cerrate (Puglia‐Italy): characterization of materials and techniques used

A multidisciplinary research was conducted by the University of Salento in collaboration with the Lecce Provincial Museum, in order to study different forms of art widespread in the Salento peninsula (Southern Italy) very valuable from an artistic point of view and important as driving force for the tourism of the area. In this research, the archaeometrical analysis was used to study the first cycle of paintings of the church of Santa Maria delle Cerrate, an italo‐greek monastery located in the country about 15 km north‐east of Lecce, probably built in the 12th century. Microscopic, chromatographic and spectrometric techniques were used: optical microscopy was used to study samples and the relevant stratigraphy, micro‐Raman Spectroscopy to identify pigments and Gas Chromatography with Mass Spectrometric Detection to investigate the techniques masters used to decorate the monastery church. Further information on organic and inorganic materials present in the samples were obtained from Fourier transform infrared analysis in attenuated total reflectance. Materials and techniques were clearly ascertained, and, interestingly, pigments were applied both by fresco and egg‐based tempera. Among the various pigments detected, the identification of both lapis lazuli and lead white opened new perspectives both from the historical and conservative points of view. Copyright © 2013 John Wiley & Sons, Ltd.