- The first examples of germanium tetrafluoride and tin tetrafluoride complexes with soft thioether coordination-synthesis, properties and crystal structures
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The first thioether complexes of the hard Lewis acidic GeF4 and SnF4 have been prepared by reaction of [GeF4(MeCN) 2] or [SnF4(MeCN)2] respectively with the thioether ligand in rigorously a
- Davis, Martin F.,Levason, William,Reid, Gillian,Webster, Michael,Zhang, Wenjian
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- Polymorphism of the mixed tin fluoride Sn2F6
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The mixed tin fluoride SnIISnIVF6 undergoes two phase transitions which have been unambiguously characterized by X-ray diffraction and micro-DTA. They occur at 385 ± 15 K and 470 ± 15 K. Evidence of the α ? β transition has also been given from a Mossbauer resonance investigation carried out over the temperature range 77 6-type.
- Grannec, J.,Fournes, L.,Lagassie, P.,Hagenmuller, P.,Cousseins, J. C.
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- Structural investigation and 119Sn Mossbauer study of graphite/SnF4 intercalation compound
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The intercalation of tin tetrafluoride into graphite has been carried out in fluorinated anhydrous HF. For long reaction times, a stage-2 compound has been obtained with an identity period of 11.53 angstrom. The structural characteristics of the intercala
- Fournes,Roisnel,Grannec,Tressaud,Hagenmuller,Imoto,Touhara
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- Synthesis and crystal structure of silver(II) fluorides AgMIVF6 (MIV = Sn, Ti, Pb, Pd, Pt, Rh)
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For the first time single crystals of AgSnF6 (light blue, triclinic with a = 519.93(7) pm, b = 524.96(10) pm, c = 563.13(9) pm, α = 115.66(2)°, β= 89.28(2)°, γ = 118.77(2)°, spcgr. P1-Ci1; (No. 2), Z = 1) and AgPdF6 (brown green, triclinic with a = 501.5(2) pm, b = 508.7(2) pm, c = 996.4(2) pm, α = 89.58(2)°, β = 103.10(2)°, γ = 120.88(2)°, spcgr. P1-Ci1, (No. 2), Z = 2) have been synthesized and investigated. Other compounds of this type, like AgTiF6 and AgPbF6 (isotypic to AgSnF6) or AgPtF6 and AgRhF6 (isotypic to AgPdF6) have been synthesized in form of microcrystalline powders, their lattice parameters have been determined by Guinier data. All compounds are structure variants oft the LiSbF6-type and isotypic with CuMF6 (M = Ti, Sn, Pb and Pd, Pt, respectively). Wiley-VCH Verlag GmbH, 2001.
- Fischer,Mueller
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p. 445 - 452
(2008/10/08)
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- The BaF2-SnF4 System
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The BaF2-SnF4 system is studied up to 55 mol % SnF4 by DTA and X-ray powder diffraction. The compound BaSnF6, which crystallizes congruently at 1120°C and undergoes phase transformations at 755 and 850°C, forms in the system. Another compound, hypothetically, Ba3SnF10, is formed peritectically at 900±5°C. The eutectic coordinates are 810±5°C, 35.5±2 mol % SnF4.
- Lukiyanchuk,Fedorov
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p. 826 - 827
(2008/10/08)
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- On the constitution of PbF4 with structure refinement of SnF4
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Colourless single crystals of SnF4 have been prepared heating powder samples of SnF4 in Pt-tubes (500°C, 20 d). Single crystals of PbF4 could be synthesized by pressure fluorination of 'PbF4-x' and sublimation in autoclaves. The fluorides crystallize isosructural in space group I4/mmm with SnF4: a = 404.42(4) pm; c = 792.41(9) pm; Z = 2 and PbF4: a = 425.36(8) pm; c = 806.4(1) pm; Z = 2 (Guinier-de Wolff data, Cu-Kα1). The parameters zF2 of both fluorides were refined from four-circle diffractometer data (Siemens AED 2) with SnF4: R1 = 1.5%; 1623 Io(Hkl) and PbF4: R1 = 1.0%; 777 Io(hkl) (SHELXL-93). The structures correspond to the supposition by Hoppe and Daehne from 1962. The Madelung Part of Lattice and Molecule Energy, MAPLE and MAPME, Mean Fictive Ionic Radii, MEFIR, and Effective Coordination Numbers, ECoN, are calculated. Johann Ambrosius Barth 1996.
- Bork,Hoppe
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p. 1557 - 1563
(2008/10/09)
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- Synthesis, solution and magic angle spinning tin-119 nuclear magnetic resonance studies and crystal structures of dithioether complexes of tin(IV) halides
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The compounds SnX4 reacted with 1 molar equivalent of dithioether, L-L, in dry CHCl3 solution to give the six-co-ordinate species [SnX4(L-L)] [X = Cl, L-L = MeS(CH2)nSMe, o-C6H4(SMe)2 or PhS(CH2)nSPh (n = 2 or 3); X = Br, L-L = MeS(CH2)nSMe or o-C6H4(SMe)2] in high yield as white or pale yellow powdered solids. Using SnBr4 and PhS(CH2)nSPh or SnI4 with MeS(CH2)nSMe did not produce isolable products, although solution 119Sn-{1H} NMR spectroscopy provided evidence for their existence at low temperatures. X-Ray structural studies on [SnCl4{MeS(CH2)2SMe}], [SnCl4{MeS(CH2)3SMe}], [SnCl4{o-C6H4(SMe)2}], [SnCl4{PhS(CH2)3SPh}] and [SnBr4{MeS(CH2)3SMe}] confirmed an S2X4 donor set with the dithioether acting as a bidentate chelate. Variable-temperature solution 1H and 119Sn-{1H} NMR spectroscopic studies showed that the complexes are extremely labile and ligand dissociation and pyramidal inversion are fast except at low temperatures. Magic angle spinning 119Sn NMR data for [SnCl4(L-L)] are reported. The crystal structure of cis-[SnI4{MeS(O)(CH2)3SMe}2], obtained as a decomposition product from the SnI4-MeS(CH2)3SMe reaction, shows monodentate sulfoxide (O) co-ordination.
- Dann, Sandra E.,Genge, Anthony R. J.,Levason, William,Reid, Gillian
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p. 4471 - 4478
(2007/10/03)
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- Polymorphic and magnetic study of ternary palladium (II) fluorides PdMIVF6 (MIV?Zr, Sn, Hf)
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Palladium(II) fluorides with formula PdMIVF6 (MIV≡Zr, Sn, Hf) exhibiting an ordered LiSbF6 type structure (R3ˉ space group) were synthesized. A structural phase transition was detected using microdifferential thermal analysis, microcalorimetry and X-ray diffraction. The thermal dependence of the spontaneous strain was determined. A cubic Fm3ˉm high-temperature form was characterized for PdZrF6 and PdHfF6. The three phases show antiferromagnetic behavior.
- Ruchaud, N.,Grannec, J.,Tressaud, A.
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- Organotin chemistry. 16. Reactions of stannane with organic functional groups
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The reactions of stannane with a variety of organic substrates have been studied. Benzaldehyde, acetone, nitrobenzene, and 2-nitropropane are reduced to benzyl alcohol, isopropyl alcohol, aniline, and isopropylamine, respectively. With boron trifluoride etherate and benzyl chloride, stannane undergoes halogen-hydrogen exchange, while with isopropylamine and acetic acid, it is decomposed catalytically into its elements. Tetrakis(2-cyanoethyl)tin is formed by the addition of stannane to acrylonitrile. Stannane did not react with the following: (a) ethyl acetate, (b) methyl acrylate, (c) aniline, (d) triethylamine, (e) dimethylacetamide, and (f) N-ethylacetamide. The results obtained with stannane are for the most part analogous to those reported for the corresponding organotin hydrides.
- Reifenberg, Gerald H.,Considine, William J.
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p. 3015 - 3018
(2008/10/08)
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