Fixation modes of gold(III) from solutions using cadmium(II) dithiocarbamates. Preparation, supramolecular structure and thermal behaviour of polynuclear and heteropolynuclear gold(III) complexes: Bis(N,N-dialkyldithiocarbamato-S,S′)gold(III) polychlorometallates, [Au(S2CNR2)2]nX (n=1: X=[AuCl4]−; n=2: X=[CdCl4]2−, [Cd2Cl6]2−)

Four novel heteropolynuclear and polynuclear complexes of the general formulae [Au(S2CNR2)2]2X (X = [CdCl4]2−, R = CH3 (1); X = [Cd2Cl6]2−, R = C3H7 (2)) and [Au(S2CNR2)2][AuCl4] (R = iso-C3H7 (3); R = iso-C4H9 (4)) were prepared using heterogeneous reactions between appropriate freshly precipitated binuclear cadmium(II) dialkyldithiocarbamates and AuCl3 in 2 M hydrochloric acid. The isolated complexes were studied by 13C CP/MAS NMR spectroscopy, single-crystal X-ray diffraction and simultaneous thermal analysis (STA) under an argon atmosphere. In all molecular structures (1–4), one of the gold atoms coordinates two dialkyldithiocarbamate ligands in the S,S′-bidentate mode, forming a square-planar coordination polygon [AuS4], while the other gold atom (in 3 and 4) has four neighbouring chlorine atoms [AuCl4]. At the supramolecular level, compounds 1 and 2 comprise binuclear cations, [Au2{S2CN(CH3)2}4]2+ and polynuclear chains, ([Au{S2CN(C3H7)2}2]+)n in a combination with [CdCl4]2− and [Cd2Cl6]2− anions, respectively. Unexpected structural distinctions at the supramolecular level were discovered for the chemically related compounds 3 and 4. In these ionic complexes, there are either cationic trinuclear formations, {[Au{S2CN(iso-C3H7)2}2]2[AuCl4]}+, or polynuclear chains, ([Au{S2CN(iso-C4H9)2}2]+)n, both combined with [AuCl4]− anions, in the structural basis of compounds 3 and 4, respectively

A fixation mode of gold from solutions using heterogeneous reaction of cadmium dicyclohexyl dithiophosphate with H[AuCl4]. Structural and (13C, 31P) CP/MAS NMR studies and thermal behaviour of crystalline polymeric gold(I) dicyclohexyl dithiophosphate and bis(dicyclohexylthiophosphoryl) disulphide

Two novel compounds: polynuclear catena-poly[bis(μ3-O, O′-di-cyclo-hexyldithiophosphato-S,S,S′)digold(I)] (AuAu) (1) and crystalline bis(O,O′-di-cyclo-hexylthiophosphoryl)disulphide, (cyclo-C6H11O)2P(S)SS(S)P(O-cyclo-C 6H11)2 (2) were prepared using heterogeneous reaction between freshly precipitated binuclear cadmium(II) dithiophosphate (Dtph), [Cd2{S2P(O-cyclo-C6H11} 4] and H[AuCl4] in 2 M hydrochloric acid. The isolated compounds 1 and 2 (the fixation mode of gold from the solution and the oxidised form of Dtph groups, respectively) have been studied by means of single-crystal X-ray diffraction, 13C and 31P cross-polarisation/magic- angle-spinning (CP/MAS) NMR spectroscopy and simultaneous thermal analysis (STA). Centrosymmetric binuclear molecule of 1, [Au2{S 2P(O-cyclo-C6H11)2}2] comprises a pair of μ-bridging di-cyclo-hexyl Dtph ligands, linking two neighbouring gold atoms, and displays additional intramolecular aurophilic bond Au⋯Au. At the supramolecular level of structural self-organisation of complex 1, infinite polymeric zigzag chains arise due to pairs of the secondary bonds Au···S between neighbouring binuclear molecules. Centrosymmetric molecule of 2 displays two O,O′-di-cyclo- hexythiophosphoryl fragments, which are connected by the chemical bond S(1)S(1)a, and a planar zigzag array [SPSSPS] passing through the central part of the molecule. To characterise additionally the Dtph groups in both compounds 1 and 2, chemical shift anisotropy (CSA) parameters (δaniso and η) were calculated from spinning sideband manifolds in experimental 31P MAS NMR spectra. The thermal behaviour of complex 1 was studied using simultaneous thermal analysis (a combination of TG and DSC) under an argon atmosphere. The thermal behaviour displays stepwise mass loss, comprising thermal decompositions of the organic and inorganic parts of 1 with gold(I) dithio-meta-phosphate and reduced metallic gold as the intermediate and the final products, respectively

The Accounting of Regime and Atmosphere Factors in Calculation of Technical Loss of Electricity in Distributive Network

Выполнен анализ имеющейся исходной информации, обосновывающий эффективность применения метода, базирующегося на средних нагрузках, для расчёта потерь электроэнергии в распределительных электрических сетях. Оценено влияние внутримесячной неравномерности электропотребления и температуры провода на погрешность расчёта потерь электроэнергии. Исследованы погрешности расчёта потерь электроэнергии методом статистических испытаний, и выполнен их учёт при помощи полиномов второй степени.The efficiency of application of the method is based on the analysis of initial information. This method is founded on average loads for calculation of losses of electricity in distributive network. The influence on the error of calculation of electricity losses is appraised taking into consideration the inequality of electricity consumption during the month and the temperature of a wire. The errors of calculation of electricity losses are studied by the method of statistics tests and their account is made on the basis of polynomial of the second degree

The Accounting of Regime and Atmosphere Factors in Calculation of Technical Loss of Electricity in Distributive Network

Выполнен анализ имеющейся исходной информации, обосновывающий эффективность применения метода, базирующегося на средних нагрузках, для расчёта потерь электроэнергии в распределительных электрических сетях. Оценено влияние внутримесячной неравномерности электропотребления и температуры провода на погрешность расчёта потерь электроэнергии. Исследованы погрешности расчёта потерь электроэнергии методом статистических испытаний, и выполнен их учёт при помощи полиномов второй степени.The efficiency of application of the method is based on the analysis of initial information. This method is founded on average loads for calculation of losses of electricity in distributive network. The influence on the error of calculation of electricity losses is appraised taking into consideration the inequality of electricity consumption during the month and the temperature of a wire. The errors of calculation of electricity losses are studied by the method of statistics tests and their account is made on the basis of polynomial of the second degree

A pyridine adduct of bis(di-iso-butyldithiocarbamato-S,S′)cadmium(II) : multinuclear (13C, 15N, 113Cd) CP/MAS NMR spectroscopy, crystal and molecular structure, and thermal behaviour

Crystalline bis(N, N-di-iso-butyldithiocarbamato-S,S')(pyridine)cadmium(II) - adduct 1 was prepared and studied by means of multinuclear (13)C, (15)N, (113)Cd CP/MAS NMR spectroscopy, single-crystal X-ray diffraction and simultaneous thermal analysis (STA). In molecular structure 1, the cadmium atom coordinates with four sulphur atoms and one nitrogen atom of pyridine, forming a coordination polyhedron [CdS(4)N], whose geometry is an almost ideal tetragonal pyramidal (C(4v)). The coordinated py molecule is in the apical position, while two structurally non-equivalent di-iso-butyldithiocarbamate ligands, playing the same terminal S,S'-chelating function, define the basal plane. To characterise additionally the structural state of the cadmium atom in this fivefold coordination, (113)Cd chemical shift anisotropy (CSA) parameters, delta(aniso) and eta, were calculated from experimental MAS NMR spectra that revealed an almost axially symmetric (113)Cd chemical shift tensor. From a combination of TG and DSC measurements taken under an argon atmosphere, we found that the mass of adduct 1 is lost in two steps involving initial desorption of coordinated py molecules with subsequent thermal destruction of liberated cadmium(II) di-iso-butyldithiocarbamate, with yellow-orange, fine-powdered solid CdS as the final product. (C) 2011 Elsevier B.V. All rights reserved