- Zinc Tin Chalcogenide Complexes and Their Evaluation as Molecular Precursors for Cu2ZnSnS4 (CZTS) and Cu2ZnSnSe4 (CZTSe)
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A series of five heteronuclear zinc tin chalcogenide complexes with the general formula [(tmeda)Zn(SnR2)2E3] (1-R, E = S; R = Me, Ph, tBu; 2-R, E = Se; R = Ph, tBu) have been synthesized and characterized by X-ray crystal structure analysis. In all cases, the six-membered ZnSn2E3 rings exhibit twist boat conformation. The presence of the molecular structures in solution is confirmed by 119Sn and 77Se NMR spectroscopy. Cothermolysis experiments using a mixture of complexes 1-R or 2-R and [(iPr3PCu)2(EC2H4E)]2 as a copper source were monitored by thermogravimetry and temperature dependent X-ray powder diffraction to examine the thermolysis reaction. According to Rietveld refinement, the solid residue consists of Cu2ZnSnS4 (up to 78 wt %) or Cu2ZnSnSe4 (up to 43 wt %) as the main product, respectively.
- Fuhrmann, Daniel,Dietrich, Stefan,Krautscheid, Harald
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p. 13123 - 13131
(2017/11/15)
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- Bis(trimethylsilyl)selenide in the selective synthesis of ?2-hydroxy, ?2-mercapto, and ?2-amino diorganyl diselenides and selenides through ring opening of strained heterocycles
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A novel approach to the synthesis of ?2-substituted dialkyl diselenides and selenides is described through reaction of bis(trimethylsilyl)selenide with epoxides, thiiranes, and aziridines catalyzed by tetrabutylammonium fluoride. Selective formation of a wide variety of ?2-hydroxy, ?2-mercapto, and ?2-amino diselenides and selenides is achieved by controlling the reaction conditions in the regioselective attack of the silyl selenide onto the ring-strained heterocycles. All reactions occur in a highly regioselective and enantioconservative manner, affording the title compounds with good to high yields. Selenium-77 NMR chemical shifts were measured to verify the selective formation of the ?2-substituted diselenides and selenides.
- Tanini, Damiano,Degl'Innocenti, Alessandro,Capperucci, Antonella
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p. 357 - 369
(2015/03/04)
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- Synthesis and crystal structures of [(iPr3P)2Cu(μ- ESiMe3)(InMe3)] (E = S, Se): Lewis acid-base adducts with chalcogen atoms in planar coordination
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The structures of [(iPr3P)2Cu(μ-SSiMe 3)(InMe3)] and [(iPr3P)2Cu(μ- SeSiMe3)(InMe3)] were determined by single-crystal X-ray diffraction. Both complexes are Lewis acid-base adducts of the InMe3 acceptor and the chalcogen donor atom linking a Me3Si group and a (iPr3P)2Cu moiety. They are very unstable under atmospheric conditions and decompose at ambient temperatures. Results of DFT calculations for these complexes and the related hypothetical [(Me 3P)2Cu(μ-SSiMe3)(InMe3)] compound show that the unusual planar coordination of the chalcogen atoms is due to steric crowding. Lewis acid-base adducts of trimethylindium and phosphane-stabilized copper(I) (trimethylsilyl)chalcogenolates were synthesized and characterized by X-ray crystal structure determination. They are very unstable under atmospheric conditions and decompose at ambient temperatures. DFT calculations reveal that the unusual planar coordination of the chalcogen atoms is due to steric crowding. Copyright
- Biedermann, Ralf,Kluge, Oliver,Fuhrmann, Daniel,Krautscheid, Harald
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p. 4727 - 4731
(2013/09/24)
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- Bis(oligosilanyl)chalcogenides [Me3Si)xMe3-xSi]2E, alkalimetal oligosilanylchalcogenolates (Me3Si)xMe3-xSi-EMI and oligosilanylchalcogenols (Me3Si)xMe3-xSi-EH (E = S, Se, Te) syntheses and NMR study
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Bis(oligosilanyl)chalcogenides [(Me3Si)x Me3-x Si]2E, alkalimetal oligosilanylchalcogenolates (Me3Si)x Me3-x Si-EMI and oligosilanylchalcogenols (Me3Si)x Me3-x Si-EH (x=1-3; E=S, Se, Te) were synthesized and characterized by 1H-, 13C-, 29Si-, 77Se- and 125Te-NMR spectroscopy. Trends of NMR parameters (chemical shifts, coupling constants) are discussed.
- Lange, Heike,Herzog, Uwe
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- Synthesis and NMR investigation of selenobutyl substituted silanes and oligosilanes
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The reaction of BuSeLi, made from BuLi and elemental selenium, with chlorosilanes MexPhySiCl4-x-y led to selenobutyl substituted derivatives. In the cases of polychlorosilanes formation of the completely substituted products MexPhySi(SeBu)4-x-y are favoured. Higher yields of partially substituted products could be obtained by reaction of chlorosilanes with BuSeH/NEt3. Besides monosilanes the reactions of several methylchlorodi-, tri- and isotetrasilanes with BuSeLi and BuSeH/NEt3 were also investigated. In SiClMe(SiClMe2)2 the chlorine substituent at the middle silicon atom is substituted by BuSeH/NEt3 at first selectively. All products were characterized by 1H, 13C, 29Si and 77Se NMR and trends of chemical shifts and coupling constants (1JSiSi, 1JSiSe, 2JSiSe) with the substitution pattern were investigated. Wiley-VCH Verlag GmbH, 2000.
- Herzog
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p. 379 - 388
(2007/10/03)
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- New routes to heterocyclic selenium sulfides
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New synthetic routes for heterocyclic selenium sulfides are described and the identification of the molecular species by 77Se NMR spectroscopy is discussed. The reaction of [Ti(Me5C5)2S3] and Se2Cl2 produces initially a mixture of 1,2-Se2S6, 1,5-Se2S6 and 1,2,3,4,5-Se5S3 that can be inferred to be formed as a consequence of a rapid decomposition of 1,2-Se2S3. The product distribution is consistent with a series of selenium-atom transfer reactions as well as a dimerization of a four-atomic species that can be thought to be formed in the early stages of the reaction. The treatment of (Me3Si)2Se with Se2S5Cl2 produces initially 1,2,3-Se3S5 and the reaction of (Me3Si)2S and Se2S5Cl2 a mixture of 1,2-Se2S6, 1,5-Se2S6, and SeS7. These products imply that the reactant chloride is a mixture of Cl-Se-S5-Se-Cl and Cl-Se-Se-S4-S-Cl. Upon prolonged standing of all reaction mixtures described above, an equilibrium of several heterocyclic selenium sulfides is formed with the product distribution governed by the molar ratio of sulfur and selenium. The abundance of 77Sc chemical shift data has enabled the quantitative discussion on the trends and has facilitated a more reliable assignment of resonances to different molecular species. Acta Chemica Scandinavica 1998.
- Pekonen, Pentti,Taavitsainen, Jari,Laitinen, Risto S.
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p. 1188 - 1193
(2007/10/03)
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- ORGANOSELENIUM COMPOUNDS VII. METHODS OF CONTROLLING THE REACTION OF ORGANIC HALIDES WITH MAGNESIUM AND SELENIUM
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The action of aryl bromides on a mixture of magnesium and selenium in ether in ratios of 1.5-2:1:1 leads to diaryl selenides and bis(bromomagnesium) selenide, which gives organic selenides with electrophiles.The reaction of Grignard reagents with an excess of selenium (ArBr:Mg:Se ratios of 1:1:1.5) in ether leads to diaryl diselenides, while the reaction in THF leads to a mixture of polyselenides and diaryl diselenides.
- Nedugov, A. N.,Pavlova, N. N.,Lapkin, I. I.
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p. 1829 - 1832
(2007/10/02)
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- LITHIUM DISELENIDE IN APROTIC MEDIUM - A CONVENIENT REAGENT FOR SYNTHESIS OF ORGANIC DISELENIDES
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The reduction of selenium with lithium in THF in the presence of diphenylacetylene as a catalyst afforded lithium diselenide, which reacted with electrophiles giving alkyl or aryl diselenides 1 - 3 and selenides 4, as by-products.The useful method for preparation of diselenides based on this reaction was elaborated.
- Syper, Ludwik,Mlochowski, Jacek
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p. 6119 - 6130
(2007/10/02)
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- NOVEL REACTIONS WITH TELLURIUM AND ORGANOTELLURIUM REAGENTS
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Novel reactions with elemental tellurium, organic ditellurides and diselenides and or reagents with Te-Li, Se-Li and Te-Si bonds are reviewed.These reagents have been used to prepare new molecules with Te-P, Se-P, Te-C, Te=C, Te-I and Se-I bonds.
- Du Mont, W. -W.,Hensel, R.,Kubiniok, S.,Lange, L.,Severengiz, T.
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- BEITRAG ZUR SYNTHESE VON ORGANYL-TRIMETHYLSILYL-SELENIDEN, R-Se-Si(CH3)3
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Phenyl-trimethyl-selenide and 2,4,6-trimethylphenyl-selenide have been synthesized and characterized from the organobromide, magnesium, selenium and trimethylchlorosilane.A better method has been found for the synthesis of organyl-trimethylsilyl-selenides.It starts from sodium-trimethylsilylselanolate, the synthesis of which is described.Its reactions with methylbromide, benzylbromide and n-pentylbromide result in the formation of the compounds R-Se-Si(CH3)3 with the corresponding groups R.Secundary as well as tertiary bromides do not react in the expected manner.
- Schmidt, Max,Kiewert, Eva,Lux, Horst,Sametschek, Cordula
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p. 163 - 168
(2007/10/02)
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- Studies of silyl and germyl Group VI species. Part IV. Dimethyl- and tetramethyl-disilyl chalcogenides and related species
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The symmetrically substituted disilyl chalcogenides (MenH3-nSi)2E where E = O, S, Se, Te; n = 0 -> 3, have been prepared and characterized spectroscopically and by cleavage reactions.The synthetic routes include reactions of halogenosilanes with water, mercury(II) sulfide, lithium telluride, and complex thio- and seleno-aluminates.The spectroscopic properties of the (MeH2Si)2E and (Me2HSi)2E species, which have not been reported previously, are discussed in some detail.
- Drake, John E.,Glavincevski, Boris M.,Hemmings, Raymond T.
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p. 2161 - 2166
(2007/10/02)
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