Antimony Trichloride Research Articles

Mild, Efficient, and Selective Cleavage of Trityl Ethers with Antimony Trichloride.

AbstractChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 200 leading journals. To access a ChemInform Abstract, please click on HTML or PDF.

Mild, Efficient and Highly Selective Hydrolysis of Acetonides with Antimony Trichloride.

AbstractChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 200 leading journals. To access a ChemInform Abstract, please click on HTML or PDF.

Efficient and Selective Cleavage of Silyl Ethers with Antimony Trichloride.

AbstractChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 200 leading journals. To access a ChemInform Abstract, please click on HTML or PDF.

Phase Transitions Mechanism and Distortion of SbCl6 3– Octahedra in Bis(n-butylammonium) Pentachloroantimonate(III) (C4H9NH3)2[SbCl5

Abstract Bis(n-butylammonium) pentachloroantimonate(III) was obtained in a reaction of n-butylammonium chloride and antimony trichloride (molar ratio 2 : 1; cation : Sb) in acidic aqueous solution. To obtain further information about the mechanism of the earlier reported phase transitions at 229 and 315 K the structure was determined at 100, 260 and 340 K. The orthorhombic system was found in all phases, space groups Ibam at 340 K and Pccn at 260 and 100 K. In all phases the anionic sublattice consists of [SbCl6]3− octahedra, connected via cis chlorine atoms, forming onedimensional zig-zag {[SbCl5]2−}n chains extended along the c direction. The n-butylammonium cations are located between the inorganic chains, with -NH3 + groups facing the oppositely charged polyanions. The phase transitions are of the order-disorder type. They are related to changes in molecular dynamics of the n-butylammonium cations. At high temperature the cations reorient, on decreasing temperature the reorientations are successfully frozen. This leads to the formation on N-H. . .Cl hydrogen bonds, which significantly deform the octahedral coordination of the Sb atoms.

EFFECT OF ANTIMONY AND FLUORINE DOPING ON ELECTRICAL, OPTICAL AND STRUCTURAL PROPERTIES OF TIN OXIDE FILMS PREPARED BY SPRAY PYROLYSIS METHOD

Undoped, antimony doped and fluorine doped tin oxide films have been prepared by spray pyrolysis technique. The films were deposited on glass substrates at temperatures ranging between 300°C and 370°C by spraying an alcoholic solution of tin tetra chloride ( SnCl 4). Dopants used were antimony tri chloride ( SbCl 3) for antimony doped tin oxide (ATO) films, and ammonium fluoride ( NH 4 F ) for fluorine doped tin oxide (FTO) films. Among undoped tin oxide films, the least resistivity was found to be 3.1 × 10-3 Ω-cm for a molar concentration of 0.75 M. In case of antimony doped films minimum resistivity value was found to be 7.7 × 10-4 Ω-cm for a film with ( Sb / Sn ) = 0.065, deposited at 370°C and in case of fluorine doped films it was found to be 1.67 × 10-3 Ω-cm for a doping percentage of 3 at% of fluorine in 0.1 M solution. The corresponding values of the carrier concentrations were found to be 1.8 × 1020/cm3 and 9.98 × 1020/cm3, respectively. The electrical and optical properties of these films were studied as a function of both doping concentration and substrate temperature. Doping percentage of antimony and fluorine in the spray solution has been optimized for achieving a minimum electrical resistivity. The dependence of electrical properties such as resistivity, carrier concentration and mobility of doped films were analyzed. Influence of antimony dopant on the optical band gap of the films has been reported on the basis of electron conduction mechanism. Air and argon annealing effects on the electrical properties of antimony doped tin oxide films were also studied.

Imino Diels–Alder reactions: an efficient one-pot synthesis of pyrano and furanoquinoline derivatives catalyzed by SbCl 3

Antimony trichloride (SbCl 3) was found to be an efficient catalyst for the inverse electron demand imino Diels–Alder reactions of in situ generated N-benzylidenes with 3,4-dihydro-2 H-pyran and 2,3-dihydrofuran to afford pyrano and furano[3,2- c]quinolines in excellent yields.

Mild, Efficient, and Selective Cleavage of Trityl Ethers with Antimony Trichloride

Selective detritylation is quite crucial in synthetic chemistry. A mild and efficient procedure for selective hydrolysis of trityl ethers in the presence of other frequently used hydroxy protecting groups: TBDPS, Bz, Bn, Ac and Ts with antimony trichloride was described and 5′‐trityl uridine was detritylated smoothly too.

Mild, Efficient and Highly Selective Hydrolysis of Acetonides with Antimony Trichloride(SUPPORTING INFORMATION)

Mild, Efficient and Highly Selective Hydrolysis of Acetonides with Antimony Trichloride(SUPPORTING INFORMATION)

Efficient and Selective Cleavage of Silyl Ethers with Antimony Trichloride

An efficient method for selective cleavage of silyl ethers mediated by SbCl3 in the presence of a number of function groups was described and the primary silyl ethers were hydrolized in the presence of the secondary ethers. The desilyl reaction took much longer time in dry solution than in wet. Keywords: desilylation, protecting groups, antimony, silyl ethers, catalysis, Hydrolyses

Thermally activated intramolecular motion in the crystalline complex SbCl3 · C6H4(NO2)2-m

Temperature dependences of the 35Cl and 121Sb NQR frequencies and the spin-lattice relaxation times in the molecular complex of antimony trichloride with meta-dinitrobenzene were investigated. These dependences for 35Cl nuclei suggest a thermoactivated motion of chlorine atoms with the activation energy Ea = 50 kJ/mol in the crystal. The data obtained were used for determination of the molecular structure of the complex. Some features of the intramolecular motion in SbCl3 complexes of the vπ and vn types were discussed. The 121Sb NQR data revealed no thermoactivated motion of the ligands bound to the Sb atom.

Solvent‐Free Knoevenagel Condensation Reaction under Microwave Irradiation Exploiting a New Reagent: Antimony Trichloride.

AbstractFor Abstract see ChemInform Abstract in Full Text.

Microstructure and electrical properties of antimony-doped tin oxide thin film deposited by sol–gel process

Antimony-doped tin oxide thin films have a range of technical applications as conductive coatings, and sol–gel processing seems to offer some advantages over other coating techniques. In this study, undoped and antimony-doped tin oxide (ATO) thin films were prepared by sol–gel process in the solution of metal salts of tin (II) chloride dehydrate and antimony tri-chloride. It has been found that the heat-treatment temperature and doping level had strong influences on the microstructure and composition of Sb:SnO 2 films. The microstructure of the thin films was analyzed by scanning electron microscope (SEM) and X-ray diffraction (XRD). The SnO 2 crystals existed mainly as tetragonal rutile structure in the present work. The optimum heat-treatment temperature was about 450–500 °C, and the film was composed with nano-crystals and nano-pores. Compared with undoped tin oxide, doped antimony tin oxide films coated glass substrate were homogenenous in composition and morphology after being sintered at different temperatures. Electrical behavior of the doped films was discussed in terms of sheet resistance measured by four point probe. From the experimental data, the sheet resistance of the films could be as low as 100 Ω/□.

Synthesis and Crystal Structure of (Sb2Te2)[AlCl4], a Compound Containing a Heteroatomic Polymeric Cation (Sb2Te2+)n

AbstractThe reaction of tellurium, antimony, antimony trichloride, sodium chloride, and an excess of aluminium trichloride in a closed evacuated glass ampoule yields dark red crystals of (Sb2Te2)[AlCl4]. During the reaction a melt is formed from which needle shaped crystals of the title compound grow on sublimating off the volatile AlCl3 at 130 °C. Energy dispersive X‐ray emission analysis showed the 1:1 ratio of Sb:Te. The crystal structure analysis (triclinic, P1¯, a = 949.30(2), b = 1348.24(3), c = 1804.97(5) pm, α = 78.983(2), β = 88.060(1), γ = 88.444(1)°, V = 2239.65(9)·106 pm3, Z = 8) shows that the structure is built of almost regular tetrahedral [AlCl4]‐ anions and of one‐dimensional polymeric (Sb2Te2+)ncations. The assignment of Sb and Te atoms to the respective atom positions of the cations was performed by an analysis of the occupation factors, a reasonable electron and charge distribution, and by the analysis of the cation‐anion interactions. The unit cell contains two symmetrically independent but almost isostructural cations which form strands made up of four‐membered stacked Sb2Te2 rings. These rings are connected with their neighboured rings alternatingly via two, three, and four covalent bonds. Predominantly Sb‐Te bonds are present, in smaller degree Sb‐Sb bonds, while Te‐Te bonds are not observed. The cationic strands can be interpreted by the Zintl concept in the connectivity of the different atom types and the resulting charges.

A study on low cost-high conducting fluorine and antimony-doped tin oxide thin films

Thin films of undoped, fluorine- and antimony-doped tin oxide on glass at 400 °C was prepared by spray pyrolysis technique. Tin chloride (SnCl 2), ammonium fluoride (NH 4F), and antimony trichloride (SbCl 3) were used as source for tin (Sn), fluorine (F), and antimony (Sb), respectively. To ensure the control of solution concentration on growth rate, fluorine-doped tin oxide (SnO 2:F) thin films were first prepared with different amount of tin precursor, in the range of 5–12 g, which has resulted in deposition of films with different thickness values. The optimum amount of tin precursor found from this study (11 g) was fixed constant for preparing SnO 2 films with different doping levels of F and Sb. From the X-ray diffraction analyses, it is understood that the preferred orientation of SnO 2:F films is dependent on their thickness and the solution concentration. The variation in the solution concentration and orientation of the films was reflected in their morphology as examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). SEM studies showed that the variation in the solution concentration lead to different grain shapes for different orientations. The AFM study showed that the RMS roughness of undoped films reduced considerably from 86 to 24 nm due to fluorine doping (15 wt.%), whereas the antimony doping (2 wt.%) has no significance effect on RMS roughness (93 nm). The electrical properties of the films were examined by a Hall measurements setup in van der Pauw configuration. A minimum sheet resistance of 1.75 and 2.17 Ω/ ▪ were obtained for F and Sb doped films, respectively. From the optical studies, it is found that the transmittance of undoped films increased from 42% to a maximum 85% on 30 wt.% fluorine doping, whereas that has been decreased to a minimum of 12% on 4 wt.% antimony doping (800 nm). A discussion on the effect of type of dopants and their concentration on the structural, electrical and optical properties of the SnO 2 film have been presented.

Solvent-free Knoevenagel condensation reaction under microwave irradiation exploiting a new reagent : antimony trichloride

A rapid microwave-assisted Knoevenagel condensation exploiting antimony trichloride under solvent-free condition is reported. Several aromatic aldehydes condense with malononitrile and ethyl cyanoacetate within a few minutes in high yields.

Studies on structural and electrical properties of sprayed SnO 2:Sb films

Thin films of antimony-doped tin oxide (SnO 2:Sb) were prepared by spray pyrolysis using stannous chloride (SnCl 2) and antimony trichloride (SbCl 3) as precursors. The antimony doping was varied from 0 to 4 wt%. Scanning electron microscopy (SEM) revealed the surface morphology to be very smooth, yet grainy in nature. X-ray diffraction (XRD) shows films to have preferred orientation, which varies with the extent of antimony doping: undoped films prefer the (2 1 1) orientation, while the (3 0 1) orientation is preferred for doping levels of 0.5 and 1.0 wt%. For higher doping levels, the (2 0 0) orientation is preferred. This difference in preferred orientations is reflected in the SEM of the films. Atomic force microscopy (AFM) reveals that film roughness is not affected by antimony doping. The minimum sheet resistance (2.17 Ω/□) achieved in the present study is lower than values reported to date in SnO 2:Sb films prepared from SnCl 2 precursor. The Hall mobility of undoped SnO 2 films was found to be 109.52 cm 2/V s, which reduces to 2.55 cm 2/V s for the films doped with 4 wt% of Sb. On the other hand, the carrier concentration, which is 1.23×10 19 cm −3 in undoped films, increases to 2.89×10 21 cm −3 for the films doped with 4 wt% of Sb.

Picoline as ligand with antimony trichloride and triiodide adducts

Solid adducts SbX3·L-pic (X=Cl, I and L=α-, β- and γ-picolines) were synthesized and characterized by elemental analysis, 1H and 13C NMR, IR spectroscopy and thermal analysis. The infrared spectroscopy and the magnetic resonance for 1H and 13C nuclei of these compounds suggest that the ligands coordinate through nitrogen atom. Kinetic studies were accomplished by means of thermogravimetric data, through isothermal and non-isothermal techniques. The best adjusting models for adducts thermal decomposition were R1 for isothermal and R1 and R2 for the non-isothermal methods. The energy of activation values obtained by isothermal method indicate the following orders of thermal stability for adducts: i) SbCl3·α-pic>SbCl3·β-pic>SbCl3·γ-pic and ii) SbI3·β-pic>SbI3·γ-pic>SbI3·α-pic. The activation energy values obtained by non-isothermal were higher than those from isothermal methods, showing the order of stability:iii) SbCl3·α-pic SbI3·α-pic=SbI3··γ-pic. These obtained data through R1 model presented the kinetic compensation effect for trichloride adducts, which could be associated to both isothermal and non-isothermal processes.

Morphology-controlled growth of crystalline antimony sulfide via a refluxing polyol process

By refluxing antimony trichloride (SbCl 3) and thiourea in various solvents at suitable reaction conditions, antimony sulfide (Sb 2S 3) crystallites with a diversity of well-defined morphologies were synthesized. Sb 2S 3 rods with the average diameter of 800 nm and the length of 7 μm, as well as microtubes with the average outer diameter of 1.2 μm, the average inner diameter of 800 nm and the length of 8 μm, were obtained in 1,2-propanediol at 180°C for 10 min. In contrast, a series of experiments under different conditions were carried out to investigate the influencing factors on the reaction. The as-synthesized products were characterized by powder X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscope and X-ray photoelectron spectra. The results indicate Sb 2S 3 crystals with different morphologies, including rod-like, tube-like, bowknot-like, flower-like, straw-bundled-like, taken under different experimental conditions. It is found that the reaction temperature, time, solvent and poly(vinyl pyrrolidone) (as a polymer capping reagent) play important roles in the formation of the final Sb 2S 3 crystallites with different morphologies. Also, the possible growth mechanism is discussed.

Sonochemical fabrication and characterization of stibnite nanorods.

Regular stibnite (Sb(2)S(3)) nanorods with diameters of 20-40 nm and lengths of 220-350 nm have been successfully synthesized by a sonochemical method under ambient air from an ethanolic solution containing antimony trichloride and thioacetamide. The as-prepared Sb(2)S(3) nanorods are characterized by employing techniques including X-ray powder diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, energy-dispersive X-ray analysis, transmission electron microscopy, selected area electron diffraction, high-resolution transmission electron microscopy, and optical diffuse reflection spectroscopy. Microstructural analysis reveals that the Sb(2)S(3) nanorods crystallize in an orthorhombic structure and predominantly grow along the (001) crystalline plane. High-intensity ultrasound irradiation plays an important role in the formation of these Sb(2)S(3) nanorods. The experimental results show that the sonochemical formation of stibnite nanorods can be divided into four steps in sequence: (1) ultrasound-induced decomposition of the precursor, which leads to the formation of amorphous Sb(2)S(3) nanospheres; (2) ultrasound-induced crystallization of these amorphous nanospheres and generation of nanocrystalline irregular short rods; (3) a crystal growth process, giving rise to the formation of regular needle-shaped nanowhiskers; (4) surface corrosion and fragmentation of the nanowhiskers by ultrasound irradiation, resulting in the formation of regular nanorods. The optical properties of the Sb(2)S(3) amorphous nanospheres, irregular short nanorods, needle-shaped nanowhiskers, and regular nanorods are investigated by diffuse reflection spectroscopic measurements, and the band gaps are measured to be 2.45, 1.99, 1.85, and 1.94 eV, respectively.

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