Bis{[μ‐N,N′‐bis­(salicyl­idene)‐1,4‐butane­di­amine‐N,N′,O,O′‐copper(II)]‐μ‐chloro‐chloromercury(II)}

A new tetranuclear Cu^II–Hg^II–Hg^II–Cu^II complex, [Cu₂Hg₂Cl₄(C₁₈H₁₈N₂O₂)₂], has been prepared by means of a copper complex found in the literature. The molecular structure of this complex was determined by X‐ray diffraction and the Cu–Hg–Hg–Cu chain was seen to be non‐linear. The change in magnetic susceptibility with temperature was recorded for this complex and observed to abide by the Curie–Weiss law. The coordination around the Hg^II ions is square pyramidal. The Cu?Hg bridging distance is 3.5269 (7) Å.     

Determination of bismuth and lead in geological samples by electrothermal AAS Part 1. Comparative study of tungsten containing chemical modifiers

A comparative study on the efficiency of some tungsten containing chemical modifiers such as W, W+Pd, W+Rh, W+Pt and W+Ru for thermal stabilization of Bi, In, Pb and Sb has been performed systematically by a Zeeman electrothermal atomization atomic absorption spectrometer (ETAAS). The addition of tartaric acid (TA) as a reducing agent additionally to the mixed modifiers was studied. A mixture of W+Pd+TA was found to be a powerful mixed modifier for the determination of Bi, In, Pb and Sb. Pretreatment temperatures could be increased up to 1250–1500° C using this mixed modifier. The use of the mixed modifier results in an enhanced accuracy and precision of the method and recovery rates above 97% for all samples. The W+Pd+TA mixed modifier was applied to the determination of Bi and Pb in dissolved geological reference samples. Received: 14 March 1996 / Revised: 3 June 1996 / Accepted: 30 June 1996     

4‐Amino‐3,5‐diethyl‐4H‐1,2,4‐triazole at 100 K: chains of edge‐fused R44(10) and R44(20) rings

The title compound, C₆H₁₂N₄, has four crystallographically independent molecules in the asymmetric unit. Intermolecular N—H...N hydrogen bonds involving amino groups and triazole N atoms form a three‐dimensional framework involving R₄⁴(10) and R₄⁴(20) rings. The hydrogen bonding is supported by weak C—H...π interactions.     

Determination of bismuth and lead in geological samples by electrothermal AAS Part 1. Comparative study of tungsten containing chemical modifiers

A comparative study on the efficiency of some tungsten containing chemical modifiers such as W, W+Pd, W+Rh, W+Pt and W+Ru for thermal stabilization of Bi, In, Pb and Sb has been performed systematically by a Zeeman electrothermal atomization atomic absorption spectrometer (ETAAS). The addition of tartaric acid (TA) as a reducing agent additionally to the mixed modifiers was studied. A mixture of W+Pd+TA was found to be a powerful mixed modifier for the determination of Bi, In, Pb and Sb. Pretreatment temperatures could be increased up to 1250–1500° C using this mixed modifier. The use of the mixed modifier results in an enhanced accuracy and precision of the method and recovery rates above 97% for all samples. The W+Pd+TA mixed modifier was applied to the determination of Bi and Pb in dissolved geological reference samples. Received: 14 March 1996 / Revised: 3 June 1996 / Accepted: 30 June 1996     

Electrical transport mechanism in boron nitride thin film

Both dc and ac transport characteristics of plasma enhanced chemical vapor deposited (PECVD) boron nitride (BN) thin film was investigated by dc current vs. dc voltage measurement at different temperatures and admittance vs. gate voltage at various frequencies/temperatures, respectively. MIM ≡ metal (Al)-insulator (BN)-metal (Al) or MIS ≡ metal (Al)-BN-semiconductor (p-Silicon) test devices were conventionally produced. Both conductivity anisotropy and dc/ac detailed transport mechanism were analyzed within the frame of a turbostratic structure (t-BN), interfacing the substrate by a thin amorphous layer (a-BN). This defective BN film has been justified by both infrared (IR) analysis and indirectly by the resulting electrical transport behavior. Transport and its variations as a function of temperature/frequency are in agreement with a hopping mechanism across Gauss-like energy distributed localized deep traps.     

[N‐(2‐Hydroxy­ethyl)ethyl­enediamine‐κ3N,N′,O]‐cis‐bis(isothio­cyanato‐κN)copper(II)

In the novel transition metal isothio­cyanate complex of N‐(2‐hydroxy­ethyl)ethyl­enediamine (hydet‐en) with copper, [Cu(NCS)₂(C₄H₁₂N₂O)], the Cu atom lies in a distorted square‐pyramidal environment, coordinated by four N atoms in the basal plane and an apical O atom. The hydet‐en ligand is N,N,O‐tridentate, in contrast to the disposition in previously studied complexes, while the isothio­cyanate ions act as N‐atom donor ligands. The monomeric units are linked to one another by hydrogen bonds.     

(2,9‐Dimethyl‐1,10‐phenanthroline‐κ2N,N′)(pyridine‐2,6‐dicarboxylato‐κ3O2,N,O6)copper(II) trihydrate

The copper(II) centre in the mononuclear title complex, [Cu(C₇H₃NO₄)(C₁₄H₁₂N₂)]·3H₂O, is surrounded by one bidentate 2,9‐dimethyl‐1,10‐phenanthroline (dmphen) ligand and one tridentate pyridine‐2,6‐dicarboxylate ligand, and exhibits a distorted square‐pyramidal geometry. The crystal packing involves both hydrogen‐bonding and π–π inter­actions. The solvent water mol­ecules link monomers to one another through hydrogen‐bonding inter­actions, forming ladder‐like chains in the bc plane. Face‐to‐face and slipped π–π inter­actions also occur between dmphen rings of neighboring mol­ecules and are responsible for inter­chain packing.     

Novel dinuclear and polynuclear copper(II)-pyrazine-2,3-dicarboxylate supramolecular complexes with 1,3-propanediamine, N,N,N′,N′-tetramethylethylenediamine and 2,2′-bipyridine

Three novel Cu(II)-pyrazine-2,3-dicarboxylate complexes with 1,3-propanediamine (pen), [Cu₂(μ-pzdc)₂(pen)₂] · 2H₂O (1), N,N,N′,N′-tetramethylethylenediamine (tmen), {[Cu(μ-pzdc)(tmen)] · H₂O}_n(2), and 2,2′-bipyridine (bipy), {[Cu(μ-pzdc)(bipy)]·H₂O}_n(3) have been synthesized and characterized by means of elemental and thermal analyses, magnetic susceptibilities, IR and UV/vis spectroscopic studies. The molecular structures of dinuclear (1) and polynuclear (2 and 3) complexes have been determined by the single crystal X-ray diffraction technique. The pyrazine-2,3-dicarboxylate acts as a bridging ligand through oxygen atom of carboxylate group and N atom of pyrazine ring and one oxygen atom of neighboring carboxylate. It links the Cu(II) ions to generate a distorted square pyramidal geometry forming a one-dimensional (1D) chain. Adjacent chains of 1 and 2 are then mutually linked via hydrogen bonding interactions, which are further assembled to form a two and three-dimensional network, respectively. The chains of complex 3 are further constructed to form three-dimensional framework by hydrogen bonding, C–H?π and ring?ring stacking interactions. In the complexes, Cu(II) ions have distorted square pyramidal geometry. Thermal analyses properties and thermal decomposition mechanism of complexes have been investigated by using thermal analyses techniques (TG, DTG and DTA).     

Synthesis of palladium complexes derived from imidazolidin‐2‐ylidene ligands and used for catalytic amination reactions

N‐Aryl amination and the Buchwald–Hartwig reaction are of great synthetic and industrial interest and scientists accept their usefulness and versatility for obtaining arylamines. In this study Ag–N‐heterocyclic carbene complexes were used as transmetallation reagents for the synthesis of Pd–N‐heterocyclic carbene complexes. The new Pd–N‐heterocyclic carbene complexes were characterized using elemental analysis and ¹H NMR, ¹³C NMR and infrared spectroscopies. The crystal structure of one, namely dichlorobis[1,3‐bis(2‐methylbenzyl)imidazolidin‐2‐yliden]palladium(II), is presented. The activity of the Pd(II) complexes in the coupling reaction of anilines or amines with bromobenzene was investigated. These complexes exhibited high catalytic activities in the direct synthesis of triarylamines and secondary amines in a single step. Copyright © 2016 John Wiley & Sons, Ltd.