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Udovenko, A. A.; Земнухова, Л. А.; Gorbunova, Yu. E.; Mikhaǐlov, Yu. N.; Давидович, Р. Л.

doi:10.1023/a:1013703518486

Cited by 4 publications

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“…Their composition did not change after a triple recrystallization. The Sb 2 O 3 admixture was detected in the solids obtained after repeated Table 4 shows that change in the 19 …”

Section: Resultsmentioning

confidence: 96%

“…The structures of the most of the AFC synthesized from the MF-SbF 3 -H 2 O systems (M = Na, K, Rb, Cs, NH 4 , and Tl) are known [11][12][13][14][15][16][17][18][19][20].…”

Section: Resultsmentioning

confidence: 99%

“…The chemical, IR, and X-ray powder diffraction analysis of the obtained crystal phases was performed by the standard procedures [1]. The study of complex formation in an aqueous solution by the 19 …”

Section: Methodsmentioning

confidence: 99%

“…, SCN -, , ) by the preparative chemistry, 19 F NMR, pH-metry, IR, and X-ray powder diffraction methods.…”

mentioning

confidence: 99%

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Conditions for the synthesis of Sb(III) fluoride complexes

et al. 2004

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Complexation of Sb(III) fluorides with alkali metal, ammonium, and thallium cations in the MF-Sb F 3 -H 2 O systems at the molar ratios MF : SbF 3 = (0.01-2) : 1 is studied by preparative chemistry, pH-metry, 19 F NMR, IR and X-ray powder diffraction methods. The crystals of Sb are synthesized and the factors influencing their formation are discussed. Some types of Sb(III) fluoride complexes are shown to be formed in the MX-SbF 3 -H 2 O systems (X = Cl -, , , SCN -, ).

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“…Their composition did not change after a triple recrystallization. The Sb 2 O 3 admixture was detected in the solids obtained after repeated Table 4 shows that change in the 19 …”

Section: Resultsmentioning

confidence: 96%

“…The structures of the most of the AFC synthesized from the MF-SbF 3 -H 2 O systems (M = Na, K, Rb, Cs, NH 4 , and Tl) are known [11][12][13][14][15][16][17][18][19][20].…”

Section: Resultsmentioning

confidence: 99%

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Conditions for the synthesis of Sb(III) fluoride complexes

et al. 2004

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“…At low molar ratios (Val : SbF 3 = (0.25-0.5) : 1), Sb 3 O 2 F 5 (the product of SbF 3 hydrolysis) is formed; its ZEMNUKHOVA et al . synthesis and crystal structure were previously described in [4,5]. At the ratio of 1 : 1 and pH 2-3, The compounds obtained are stable in air and readily soluble in water.…”

Section: Resultsmentioning

confidence: 99%

Sb(III) fluoride complexes with DL-valine. crystal structure of molecular complex SbF3{(CH3)2CHCH(+NH3)COO?}

et al. 2005

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Amino acids playing an important role in biological processes form complexes with many metals. Four complexes, namely, 2 SbF 3 ( + NH 3 CH 2 COO -) ( III ), SbF 3 ( + NH 3 CH 2 COO -) ( IV ), SbFO ( + NH 3 CH 2 COO -) ( V ) , and (NH 3 CH 2 COOH ) SbF 4 ( VI ) were synthesized in aqueous solutions via reaction of SbF 3 with the simplest amino acid, i.e., glycine + NH 3 CH 2 COO -( Gly ) [1]. Crystal structures of complexes IV and VI were also determined in [1].To continue our studies on synthesis of new Sb(III) fluoride complexes with amino acids, we investigated interaction of SbF 3 with aliphatic amino acids in an aqueous solution. The publication concerns the composition and structure of complexes formed in reaction of SbF 3 with α -aminoisovaleric acid (DL-valine, Val) in an aqueous solution.Synthesis. The starting reagents used in synthesis were Sb(III) fluoride (reagent grade), DL-valine (pure grade), and hydrofluoric acid. DL-valine (hereinafter valine), containing insignificant amount of impurity, was preliminarily purified before recrystallization from an aqueous solution. Synthesis of SbF 3 complexes with valine was performed by preparative method via reaction of SbF 3 with valine in an aqueous solution at the molar ratio of components (0.25-2) : 1 in the presence of hydrofluoric acid. The samples of reagents taken in a definite molar ratio were dissolved in water, the solutions were heated to 50-60°ë and poured together. The required pH of the solution (1-3) was monitored by the addition of HF acid. The reaction mixture was evaporated to 1/3 of its initial volume and allowed to stand for crystallization at room temperature. The obtained crystals were filtered in vacuum, washed with acetone on a funnel, and dried in air to a constant weight. The complexes thus formed were identified using chemical X-ray diffraction, and IR analyses. X-ray diffraction analysis of a faceted single crystal of complex I was performed on a SMART-1000 CCD Bruker diffractometer. The experimental data were collected at room temperature in sets of 906, 580, and 360 frames at ϕ = 0°, 90° , and 180° , respectively, using ω scan mode at a step of 0.3° and with 30 s per frame. The absorption was corrected by the crystal faces.The structure was solved by the direct methods and refined by the least-squares method in a full-matrix anisotropic approximation for all non-hydrogen atoms. Hydrogen atoms were located geometrically and refined in isotropic variant with fixed thermal parameters ( U H = 0.0 65 Å) for a limited set of reflections at the initial stage (sin θ / λ = 0.55) and for all reflections at the final stage.The data collection, processing, and refinement of unit cell parameters were carried out with the SMART and SAINT-Plus programs [2]. All calculations for determination and refinement of the structure were performed with the SHELXTL/PC program packages [3].Selected crystallographic data and results of refinement of the structure are given in Table 1, the atomic coordinates and their thermal parameters are presented in Tabl...

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Complexation processes in KF-SbF3-H2O system studied by calorimetric titration

et al. 2005

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Complexation in a KF-SbF 3 -H 2 O system is studied in a range of molar ratios of fluorides KF : SbF 3 = (0.1-2) : 1 by calorimetric titration. The equilibrium formation constants of complexes KSb 2 F 7 , KSbF 4 , and K 2 SbF 5 (5.8 × 10 5 ± 800, 3.3 × 10 4 ± 500, and 1.9 × 10 6 ± 950, respectively) and the changes in enthalpy (-31.75 ± 0.74, -28.15 ± 0.44, and -25.5 ± 0.64 J mol -1 , respectively) and entropy (4 ± 7, -8 ± 5, and -35 ± 9 J mol -1 K -1 , respectively) are determined. The thermodynamic stability of the antimony(III) fluoride complexes is found to increase on going from KSb 2 F 7 to K 2 SbF 5 . Table 2. Characteristics of the formation of potassium fluoroantimonates(III) in water at 298.15 K Compound K c ∆H, J mol -1 ∆S, J mol -1 K -1 KSb 2 F 7 5.8 × 10 5 ± 800 -31.75 ± 0.74 4 ± 7KSbF 4 3.3 × 10 4 ± 500 -28.15 ± 0.44 -8 ± 5 K 2 SbF 5 1.9 × 10 6 ± 950 -25.5 ± 0.64 -35 ± 9

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Cited by 4 publications

References 1 publication

Conditions for the synthesis of Sb(III) fluoride complexes

Conditions for the synthesis of Sb(III) fluoride complexes

Sb(III) fluoride complexes with DL-valine. crystal structure of molecular complex SbF3{(CH3)2CHCH(+NH3)COO?}

Complexation processes in KF-SbF3-H2O system studied by calorimetric titration

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