Nanometric Antimony Powder Synthesis by Activated Alkaline Hydride Reduction of Antimony Pentachloride

A novel chemical reduction method using an activated alkaline hydride (LiH or NaH-t-BuONa) in tetrahydrofuran solvent has been applied to antimony salt reduction. X-ray diffraction and transmission electron microscopy studies have been carried out to characterize the morphology and structure of the materials. Alkali hydride nature influence has been proved. In both cases the process allows to prepare antimony particles in nanometer range from few nanometers to about 20nm which could be used as anodic materials for lithium–ion batteries. With lithium hydride well-crystallized particles inclined to agglomeration were observed whereas finely dispersed amorphous particles were pointing out after activated sodium hydride reduction.     

Kinetic studies of antimony and selenium atomization processes including a chemical modifier during their determination by electrothermal atomic absorption spectrometry

We have studied antimony and selenium atomization processes including a chemical matrix modifier (palladium-containing activated carbon) during their determination by electrothermal atomic absorption spectrometry. We have developed and fine-tuned an experimental setup for determining the kinetic characteristics (activation energy and frequency factor) for element atomization processes from measurements in the initial section of the analytical signal. We provide a rationale for the most likely mechanism for the interactions that occur. The results of the kinetic studies of the atomization processes showed that the modifier we developed was highly effective, as a result of formation of a thermally stable condensed system C-Pd-A (where A is the analyte). __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 73, No. 4, pp. 530–534, July–August, 2006.     

超高灵敏显色反应测定痕量锑──锑（Ⅲ）─罗丹明B─碘化钾体系

本文研究结果表明，水溶性大分子化合物阿拉伯胶和非离子表面活性剂ＴｒｉｔｏｎＸ－１００共同存在下，锑碘配阴离子和罗丹明Ｂ的显色反应具有很高的灵敏度。缔合物的最大吸收在５ｇ０ｎｍ，摩尔吸光系数ε＝６．１×１０￣５Ｌ·ｍｏｌ－１·ｃｍ－１。用巯基棉富集锑，分离干扰离子。本法可应用于有色金属中痕量锑的测定。     

锑－槲皮素络合物极谱吸附波的研究

在１×１０~（－２）ｍｏｌ／Ｌ。Ｈ＿２ＳＯ＿４，１×１０~（－５）ｍｏｌ／Ｌ。槲皮素，５％乙醇底液中得到了锑－槲皮素络合物还原峰，这是一个明显的络合物吸附极谱波。用其导数波可测定纯Ａｓ＿２Ｏ＿３中微量Ｓｂ。     

Shape-persistent cyclyne-type azamacrocycles: synthesis, unusual light-emitting characteristics, and specific recognition of the Sb(V) ion

Simple members of arene-azaarenecyclynes as a novel family of geometrically-controlled and shape-persistent azamacrocycles have been synthesized. Noteworthy is the specific recognition function for Sb(V). The synthesized azamacrocycles, in particular the Sb(V) complex, have unusually strong light-emitting property.     

Synthesis and characterisation of bis(pentafluorophenyl)antimony(V) cations, [(C6F5)2SbL3]

Pentacoordinate complex cations of the general formula [(C₆F₅)₂SbL₃]³⁺ stabilized as solid salts in combination with tetraphenylborate (BPh₄), tetrafluorobroate (BF₄) anions, where L=DMSO, Ph₃AsO, PyO, DMF, α-, β- and γ-picoline have been isolated. The newly formed complexes were characterized by elemental analysis, molar conductance measurements, solid-state IR and and NMR. From these results, a five-fold coordination around antimony was required.     

Remarkable reactivity enhancement with Sb?N inter-coordination of ethynyl-1,5-azastibocines in Pd-catalyzed cross-coupling reactions with organic halides

The reaction of 12-arylethynyl-6-methyl-5,6,7,12-tetrahydrodibenzo[c,f][1,5]-azastibocines with organic halides such as acyl halides and aryl halides in the presence of PdCl₂(PPh₃)₂ as a catalyst led to the formation of cross-coupling products, alkynyl ketones and diaryl acetylenes, in good yields. The reactivity of the ethynyl group on the 1,5-azastibocines was far superior to that on diphenyl(phenylethynyl)stibane, which brought about marked improvement in the reaction conditions (lower temperature and shorter reaction time) and in the yields of the cross-coupling products. Single-crystal X-ray analysis of the ethynyl-1,5-azastibocine showed the presence of intramolecular Sb?N interaction which should be responsible for the remarkable reactivity enhancement of the 1,5-azastibocines for this type of reaction.     

d,h-m̈-Alkoxoalkylphosphonato-e-m̈-alkoxo-f-m̈-oxo-bis[trichloroantimon(V)]-Verbindungen

d,h-m?-Alkoxoalkylphosphonato-e-m?-alkoxo-f-m?-oxo-bis[trichloroantimony(V)] Compounds The binuclear antimony(V) complexes Cl₃Sb(O)[R³(R¹O)PO₂](OR²)SbCl₃ 1 to 7 with R¹, R² and R³ = Me or Et in solution slowly exchanges the R² groups between the equatorial oxygen atoms of the Sb₂O₂ ring. The SbO(3)PO(3)Sb ringsystem makes rapid pseudorotation. The resulting isomeres are detected by nmr spectroscopy.     

Einfache Trithio- und Perthiocarbonatokomplexe mit interessanter Koordinationschemie: [E(CS3)2]2− (E = Sn,Zn, Cd), [E(CS3)3]3− (E = As,Sb, Bi,Co), {Cu(CS3)−}∞ und [Zn(CS4)2]2−

Simple Trithio- and Perthiocarbonato Complexes with Interesting Bond Properties: [E(CS₃)₂]^2? (E = Sn, Zn, Cd), [E(CS₃)₃]^3? (E = As, Sb, Bi, Co), {Cu(CS₃)^?}_∞ and [Zn(CS₄)₂]^2? By reactions of potassium trithiocarbonate ( 1 ) with solutions of zinc(II)- acetylacetonate, cadmium(II)-chloride, tin(II)-chloride, arsenic(III)-sulfide (suspension), antimony(III)-chloride, bismuth(III)-chloride and copper(II)-chloride in dimethyl sulfoxide, as well as of trisodium hexanitrito cobaltate(III) in water, and the precipitation of the complexes with an aqueous solution of tetraphenylphosphonium chloride the compounds (PPh₄)₂[Zn(CS₃)₂] ( 2 ), (PPh₄)₂[Cd(CS₃)₂] ( 3 ), (PPh₄)₂[Sn(CS₃)₂] ( 4 ), (PPh₄)₃[As(CS₃)₃] ( 5 ), (PPh₄)₃[Sb(CS₃)₃] ( 6 ), (PPh₄)₃[Bi(CS₃)₃] ( 7 ), (PPh₄)₃[Co(CS₃)₃] ( 8 ) and (PPh₄)Cu(CS₃) ( 9 ) have been isolated. (PPh₄)₂[Zn(CS₄)₂] · CH₃NO₂ ( 10 ) has been prepared by heating a solution of 2 in nitromethane to 60--70°C in presence of air. The reaction of 1 in dimethyl sulfoxide with an aqueous tetraphenylphosphonium chloride solution in presence of oxygen leads to (PPh₄)₂[C₂S₆] ( 11 ). The compounds have been characterized by spectroscopical studies (IR, Raman, UV/Vis, ¹¹³Cd/⁵⁹Co-NMR), magnetic susceptibility measurements, powder diffractometry, elemental analyses and single crystal X-ray structure analysis ( 4 – 7 , 10 and 11 ). The difficult growing of single crystals has been reported in detail. For crystal data see Inhaltsübersicht.