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  • 1
    ISSN: 1520-510X
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    Inorganic chemistry 34 (1995), S. 5166-5170 
    ISSN: 1520-510X
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 237-245 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organo[chloro(methyl)stannyl]phosphines and -aminesEquimolar amounts of di-tert-butyl(trimethylsily)phosphine (1) and dichlorodimethylstannane or trichloro(methyl)stannane react with formation of di-tert-butyl(chlorodimethylstannyl)phosphine (2) and di-tert-butyl[dichloro(methyl)stannyl]phosphine (3), respectively. The reaction of 1 with trichloro(methyl)stannane in a molar ratio of 2:1 yields chloro(methyl)stannanediylbis(di-tert-butylphosphine)(4). All experiments to synthesize he analogous (chlorodimethylstannyl)diphenyl-phosphine failed. A new method for the synthesis of (chlorodimethylstannyl)diethylamine (6) and (bromodimethylstannyl)diethylamine (7) was found with the reaction of bis(diethylamino)dimethylstannane with chloro- and bromotrimethylsilane, respectively. The i. r. and 1H n.m.r. spectra are discussed.
    Notes: Äquimolare Mengen von Di-tert-butyl(trimethylsilyl)phosphin (1) und Dichlordimethylstannan bzw. Trichlor(methyl)stannan reagieren unter Bildung von Di-tert-butyl(chlordimethylstannyl)-phosphin (2) und Di-tert-butyl[dichlor(methyl)stannyl]phosphin (3). Die Umsetzung von 1 mit Trichlor(methyl)stannan im Molverhältnis 2:1 führt glatt zu Chlor(methyl)stannandiylbis(di-tert-butylphosphin) (4). Die Versuche, ein entsprechendes (Chlordimethylstanny)diphenyl-phosphin zu synthetisieren, schlugen dagegen fehl. Diäthyl(chlordimethylstannyl)amin (6) und Diäthyl(bromdimethylstannyl)amin (7) werden durch Spaltung von Bis(diäthylamino)dimethylstannan mit Chlor- bzw. Bromtrimethylsilan dargestellt. IR- und NMR-Spektren werden diskutiert.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 121 (1988), S. 2109-2110 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Iodo[tris(trimethylsily)methyl]selane: Synthesis of the First Alkylselenenyl IodideBis[tris(trimethylsilyl)methyl]diselane (1) reacts with elemental iodine to provide iodo[tris(trimethylsilyl)methyl]selane (2) in high yield. 2 is the first iodoselane that does not suffer from redismutation equilibria in solution at ambient temperature with iodine and the parent diselane.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 2325-2327 
    ISSN: 0009-2940
    Keywords: Diselenide, torsion angle/NMR, 77Se/Selenenyl halide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis[tris(trimethylsilyl)methyl] Diselenide: An Unusual Diselenide with Sterically Enforced trans-C2h ConformationDeselenation of bis[tris(trimethylsilyl)methyl] triselenide (1) with copper occurs with formation of bis[tris(trimethylsilyl)-methyl] diselenide (2) and minor amounts of 3,3,5,5-tetrakis(trimethylsilyl)-1,2,4-triselenolane (3). The structures of 2 and 3 have been studied by multinuclear NMR spectroscopy and by X-ray crystallography. The C—Se—Se—C moiety of 2 adopts an unusual antiperiplanar conformation. Cleavage of the Se — Se bond by iodine providing iodo[tris(trimethylsilyl)-methyl]selane (5) is complete with 2, but reversible with 1.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 0009-2940
    Keywords: Hexafluoroacetone ; Phosphorus, pentacoordinated ; Diphosphane diselenide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reduction of the isoprene - PCl3 adduct 1 with magnesium powder, or with Si2Cl6, furnished P-chloro-3-methyl-phosphol-2-ene, 2, in satisfactory yield. Further reduction of 2 with Si2Cl6 gave the new trichlorosilyl-3-methylphosphol-2-ene, 3. The reaction of 2 with magnesium powder, with 3, or with 1/2 equivalent of Si2Cl6 provided the new γ3P-γP-diphosphane 1,1′-bi(3-methylphosphol-2-ene) 4. Reduction of 4 with Si2Cl6 led to 3. Oxidation of 4 with selenium gave the 1,2-diphosphane diselenide, 5. The oxidation of 4 with hexafluoroacetone led to a mixture of products, from which a novel tricyclic phosphorane 6 was separated. the structure of 196 was determined by X-ray diffraction; the coordination geometry at phosphorus in distorted trigonal bipyramidal, with a very long equatorial P - C(CF3)2 bond of 193.2(2) pm.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 114 (1981), S. 3572-3580 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complexes of Germanium Dichloride with 1,2-Bis(diphenylphosphino)ethane: A Semi-Chelate and A Double-Ylide1,2-Bis(diphenylphosphino)ethane (dppe) reacts with the germanium dichloride dioxane complex depending on the stoichiometric ratio to give a 1:2 dppe-bridged bis(germylene) complex (1) or a 1:1 complex (2) that shows equilibration of both phosphorus atoms in 31P-NMR. The crystal structure of 2 has been determined from single crystal X-ray data. The compound crystallizes with 8 units dppe-GeCl2· 1/2 C6H6 in a unit cell of symmetry A 2/a-C2h6 in a monoclinic system. The dppe-GeCl2 molecules contain a novel semi-chelating type of coordination of the dppe ligand [distorted Ψ-trigonal bipyramidal coordination at Ge11 with an exceptionally long distance Ge-P(apical)]. 2 thus represents an intermediate structure between chelate complex and phosphorus ylid.
    Notes: 1,2-Bis(diphenylphosphino)ethan (dppe) reagiert mit dem Germanium(II)-chlorid-Dioxankomplex je nach Mengenverhältnis zu einem dppe-verbrückten Bis(germylen)-Komplex (1) oder zu einem 1:1-Komplex (2), der sich durch die Äquivalenz der Phosphanfunktionen in Lösung (31PNMR) auszeichnet. 2 kristallisiert mit 1/2 C6H6 monoklin mit acht Einheiten der Formal dppe-GeCl2· 1/2 C6H6 in der Elementarzelle, Raumgruppe A 2/a-C2h6. Die verzerrt Ψ-trigonal-bipyramidale Koordination um Ge11 mit ungewöhnlich langem Abstand Ge-p(apikal) weist 2 als Komplex mit halb-chelierendem dppe-Liganden aus (Zwischenstellung zwischen Chelatkomplex und einfachem \documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\rm P}\limits^{\rm + } - \mathop {{\rm Ge}}\limits^{\rm - } - {\rm Ylid} $\end{document}).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 118 (1985), S. 1045-1049 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimeric Phospha- and Thiastannylenes: Ylide-type Diphospha- and DithiadistannetanesBis(di-tert-butylphosphino)tin(II) (1) is obtained from the reaction of potassium di-tert-butyl-phosphide with stannous chloride or with the stannous chloride-triethylphosphane complex. Bis(tert-butylthio)tin(II) (2) is prepared by reaction of (η5-C5H5)2Sn with 2-methyl-2-propanethiol or from stannous chloride and (tert-butylthio)trimethylsilane. In solution, 1 and 2 are PR2-and SR-bridged dimers, respectively. NMR spectra indicate that rapid scrambling of terminal and bridging substituents occurs in 2 but not in the cyclic \documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\rm P}\limits^ + - \mathop {\rm S}\limits^{\rm - } {\rm n} $\end{document} ylide 1.
    Notes: Bis(di-tert-butylphosphino)zinn(II) (1) entsteht durch Reaktion von Kalium-di-tert-butylphos-phid mit Zinndichlorid oder dem Zinndichlorid-Triethylphosphan-Komplex. Bis(tert-butylthio)-zinn(II) (2) wird hergestellt durch Umsetzung von (η5-C5H5)2Sn mit 2-Methyl-2-propanthiol und entsteht auch bei der Reaktion von Zinndichlorid mit (tert-Butylthio)trimethylsilan. 1 und 2 liegen in Lösung als PR2- bzw. SR-verbrückte Dimere vor. Kernresonanzspektren zeigen, daß bei dem cyclischen \documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\rm P}\limits^ + - \mathop {\rm S}\limits^{\rm - } {\rm n} $\end{document}-Ylid 1 im Gegensatz zu 2 auch in Ethern keine raschen Platzwechselvorgänge (Brücke/terminal) ablaufen.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
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  • 10
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Properties of Tellurium-Tellurium Bonds, VI.  -  Structure and Barrier of Interconversion of Enantiomeric Conformations of Bis(2,4,6-tri-tert-butylphenyl)ditellaneOxidation of lithium (2,4,6-tri-tert-butylphenyl)telluride provides red and strong refractive needles of bis(2,4,6-tri-tert-butylphenyl)-ditellane (1) which crystallize monoclinically in the space group C2/c. The bond distance d(Te-Te), the bond angle at the Te atoms, and the torsion angle at the Te-Te bond were found to be 271.3 pm, 100.6°, and 92.1°, respectively. The C2 symmetry of the molecule gives rise to different chemical surroundings for both tert-butyl groups in ortho position belonging to the aryl groups. This effect can also be observed in solution at low temperatures. For the first time, dynamic NMR spectroscopy succeeded in determination of the barrier of rotation about a Te-Te bond. This barrier was found to be 40.9 kJ · mol-1 and is 20% less than that in the corresponding diselane.
    Notes: Bis(2,4,6-tri-tert-butylphenyl)ditellan (1) wird durch Oxidation von Lithium-(2,4,6-tri-tert-butylphenyl)tellurid in Form roter, stark lichtbrechender Kristalle erhalten. 1 kristallisiert monoklin in der Raumgruppe C2/c. Der Bindungsabstand d(Te-Te) beträgt 271.3 pm, der Bindungswinkel an den Te-Atomen 100.6° und der Torsionswinkel an der Te-Te-Bindung 92.1°. Durch die C2-Symmetrie besitzen die beiden ortho-ständigen tert-Butylgruppen der Substituenten unterschiedliche chemische Umgebung, die auch in Lösung bei tiefen Temperaturen erkennbar wird. Aus NMR-spektroskopischen Daten gelang erstmals die Bestimmung der Rotationsbarriere um eine Te-Te-Bindung; sie beträgt 40.9 kJ · mol-1. Dieser Wert ist um 20% kleiner als für das entsprechende Diselan.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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