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  • 1
    Electronic Resource
    Electronic Resource
    Reaktionen an Silicium-Silicium-Bindungen, 2[1] Trichlorsilylierung von tert-Butyldichlorphosphan und tert-Butylbis(trimethylsilyl)phosphan mit Hexachlordisilan: Ein Weg zu neuen bifunktionellen (Trichlorsilyl)phosphanen (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 657-658 
    Details
    ISSN: 0009-2940
    Keywords: Trichlorosilylation ; Chlorophosphanes ; Silylphosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of Silicon-Silicon Bonds, 2[1]. - Trichlorosilylations of tert-Butyldichlorophosphane and tert-Butylbis(trimethylsilyl)phosphane with Hexachlorodisilane: Synthesis of New Bifunctional (Trichlorosilyl)phosphanesDi-tert-butyl(trimethylsilyl)phosphane (1) and tert-butylbis(trimethylsilyl)phosphane (3) react with one equivalent of hexachlorodisilane with exchange of one trimethylsilyl group by a trichlorosilyl group under mild conditions to give di-tert-butyl(trichlorosilyl)phosphane (2) and tert-butyl(trichlorosilyl)(trimethylsilyl)phosphane (4) in fair yields. tert-Butylbis(trichlorosilyl)phosphane (5) is available from tert-butyldichlorophosphane without organometallic reagents and solvents by simple reductive trichlorosilylation with the help of two equivalents of hexachlorodisilane. 5 is a useful precursor for phosphaalkane synthesis: with pivaloyl chloride, 5 leads to tert-butyl-[tert-butyl(trichlorosilyloxy)methylene]phosphane (6). From 4 with pivaloyl chloride mainly 6 and some known tert-butyl[tert-butyl(trimethylsilyloxy)methylene]phosphane (7) are formed.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250318
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  • 2
    Electronic Resource
    Electronic Resource
    Reactions at Silicon-Silicon Bonds, V. Selective Trichlorosilylation of Alkyl(diorganylamino)chlorophosphanes with Hexachlorodisilane or with Trichlorosilane/Triethylamine. - Two Routes to New Functional Trichlorosilylphosphanes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 615-619 
    Details
    ISSN: 0009-2940
    Keywords: Reductive silylation ; Aminochlorophosphanes ; Silylphosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of alkyl(diorganylamino)chlorophosphanes R(R2′N)PCl 1 (1a: R = tBu, R′ = Et, 1b: R = iPr, R′ = iPr; 1c: R = iPr, R′ = Ph) with hexachlorodisilane, afforded alkyl(diorganylamino)trichlorosilylphosphanes R(R2′N)PSiCl3 2 (2a: R = tBu, R′ = Et; 2b: R = iPr, R′ = iPr; 2c: R = iPr, R′ = Ph) and silicon tetrachloride. An intermediate formed in the reaction of 1b with hexachlorodisilane, the adduct iPr(iPr2N)(Cl)P-Si(Cl)3-SiCl3 (3b = 1b · Si2Cl6), was detected by 31P- and 29Si-NMR spectra that indicate pentacoordinated silicon bound to tetracoordinated phosphorus and tetracoordinated silicon. Trichlorosilylphosphanes 2 are also available from 1 under very mild conditions by reductive trichlorosilylation with trichlorosilane in the presence of triethylamine. Compounds 2 were identified analytically, by mass spectroscopy, multinuclear NMR, and an X-ray structure determination of 2c.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280614
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  • 3
    Electronic Resource
    Electronic Resource
    Reversible Rearrangements of Chlorophosphane-Dichlorogermylene Ylides to Trichlorogermylphosphanes  -  Structure Determination of a Tetranuclear Bis(chlorophosphane)bis(trichlorogermylphosphane) Silver Bromide Complex (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1619-1623 
    Details
    ISSN: 0009-2940
    Keywords: Dichlorogermylene ; Trichlorogermylphosphanes ; Insertion ; Silver bromide complex ; Carbene homologues ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chlorophosphanes RR'PCl (1a: R,R' = 1b: R = tBu, R' = iPr, 1c: R = iPr, R' = Et2N, 1d: R = Et2N react with the dichlorogermylene dioxane complex 2 furnishing trichlorogermylphosphanes RR'PGeCl3 4a-d. In the cases of 1c/4c and 1d/4d the insertion reaction remain incomplete; similarly, 4a always contains, shortly after isolation in pure state, small amounts of 1a that can be detected by NMR. A provided by the reaction of trichlorosilylphosphane tBu(Et2N)PSiCl3 (5d) with GeCl4. The alkyl(dialkylamino) trichlorogermylphosphane 4d exists only in an equilibrium with chlorophosphane 1d, which coordinates GeCl2 leading to the dichlorogermylene complex 3d. A 1:1 mixture of 4a with 1a is formed by the novel cleavage (“chlorogermylation”) of the P-P bond of tetraisopropyldiphosphane with germanium tetrachloride. Di-tert-butyl(trichlorogermyl)phosphane 4e (R, R' = tBu) reacts with silver bromide providing a crystalline silver complex 7. A structure determination by X-ray diffraction reveals that 7 is [Ag4Br4(tBu2PCl)2(tBu2PGeCl3)2]. 2C7H8. Two of the Ag atoms of the cubane-like (AgBr)4 core of 7 are coordinated by chlorophosphane 1e, the other two by trichlorogermylphosphane 4e.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301110
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  • 4
    Electronic Resource
    Electronic Resource
    Darstellung von cis-Dichloro[tellurobis(di-tert-butyl-phosphan)]platin(II) (1985)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 118 (1985), S. 5016-5017 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparation of cis-Dichloro[tellurobis(di-tert-butylphosphane)]platinum(II)The title complex 2 is obtained in 50-60% yield from heterogeneous reactions between tellurobis(di-tert-butylphosphane) (1) and bis(benzonitrile)dichloroplatinum(II) in methylene chloride or platinum dichloride in toluene suspension. NMR and MS data are consistent with a chelate-type Cl2Pt(tBu2P)2Te structure of the new complex.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19851181233
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  • 5
    Electronic Resource
    Electronic Resource
    Lithium-(2,4,6-tri-tert-butylphenylselenid); Erzeugung, Struktur und Reaktionen unter Knüpfung von Se -P-, Se - C-, Se - Si-, Se - Sn- und Se - Au-Bindungen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1315-1320 
    Details
    ISSN: 0009-2940
    Keywords: Chalcogen-chalcogen bonds ; Selenium ; Selenide (2,4,6-tri-tert-butylphenyl)- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Properties of Chalcogen-Chalcogen Bonds, XV1). - Lithium 2,4,6-Tri-tert-butylphenylselenide: Synthesis, Structure, and Reactions with Formation of Se - P, Se - C, Se - Si, Se - Sn, and Se - Au BondsBis(2,4,6-tri-tert-butylphenyl)diselenide (1) is reduced by lithium triethylhydridoborate to give lithium 2,4,6-tri-tert-butyl-phenylselenide (2) in high yield. 2 crystallizes with three molecules of tetrahydrofuran coordinated to lithium ([2(THF)3] ≡ 2a, space group P&1macr; Z =4). The monomeric compound 2a contains four-coordinate lithium bonded to two-coordinate selenium. 2 (LiSeR) reacts with the nonmetal and metal halides tBu2PCl, CH2Cl2, Me3SiCl, Me3SnCl, and Ph3PAuCl to give tBu2PSeR (3), RSeCH2Cl (4), (RSe)2CH2 (5), Me3SiSeR (6), Me3SnSeR (7), and the novel gold(I) selenophenolate derivative Ph3PAuSeR (8)(R = 2,4,6-tri-tert-butylphenyl).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240602
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  • 6
    Electronic Resource
    Electronic Resource
    Spaltung sperriger Diarylditelluride mit Brom und Iod[1]; Strukturbestimmung an Et4N+ 2,4,6-(i-C3H7)3C6H2TeI-2 (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 761-766 
    Details
    ISSN: 0009-2940
    Keywords: Tellurium compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cleavage of Bulky Diaryl Ditellurides with Bromine and Iodine; Crystal Structure of Et4N+ 2,4,6-(i-C3H7)3C6H2TeI-2Bis(2,4,6-triisopropylphenyl) ditelluride (1a), obtained from 2,4,6-triisopropylphenylmagnesium bromide with tellurium followed by oxidation with oxygen, and bis(2,4,6-tri-tert-butylphenyl) ditelluride (1b) react with equimolar amounts of bromine and iodine to provide new monomeric arenetellurenyl halides 2,4,6-R3C6H2TeX (2a, b, 3a, b: R = i-C3H7, t-C4H9; X = Br, I). Both tellurenyl iodides are thermally more stable than the corresponding bromides. Green 2,4,6-(i-C3H7)3C6H2TeI (3a) reacts with Et4N+I- to give the stable, red adduct Et4N+ 2,4,6-(i-C3H7)3C6H2TeI-2 (4a). An X-ray crystal structure determination of 4a revealed a T-shaped structure of the hypervalent aryldiiodotellurate(II) anion. Iodide-ion transfer between aryldiiodotellurate(II) and arenetellurenyl iodide is a fast process (1H-NMR time scale). 125Te-NMR data of this anion and of tellurenyl halides are compared with those of the ditellurides and of lithium benzenetellurolates (LiTeR·(THF)x).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250402
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  • 7
    Electronic Resource
    Electronic Resource
    Eigenschaften von Chalkogen-Chalkogen-Bindungen, XVII. Di-und Trisulfane mit sterisch anspruchsvollen Alkyl-Substituenten: Das erste trans1-Dialkyldisulfan (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 1355-1359 
    Details
    ISSN: 0009-2940
    Keywords: Disulfanes ; Trisulfanes ; Bond conformations, S—S ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Properties of Chalcogen-Chalcogen Bonds, XVII[1]. - Di-and Trisulfanes with Sterically Congested Alkyl Substituents: The First trans1-DialkyldisulfaneBis[tris(trimethylsilyl)methyl]trisulfane (1) is obtained from tris(trimethylsilyl)methyllithium and sulfur with subsequent oxidation by oxygen or from tris(trimethylsily)methanethiol with sulfur dichloride. The solid trisulfane contains a transoid (helical) C—S-S—S-C backbone without severe distortion from steric strain. Desulfuration of the byproduct bis[tris(trimethylsilyl)methyl]tetrasulfane (2) with mercury provides 1, but further desulfuration of 1 to bis[tris(trimethylsilyl)1-methyl]disulfane (3) has not been achieved. 3 was isolated after oxidation of lithium tris(trimethylsilyl)methanethiolate with bromine. 3 contains a trans1-C—S-S—C moiety with an unusually long S—S bond (210-211 pm). The less crowded bis(triphenylmethyl)disulfane (4) contains a “normal” C—S-S—C moiety with anticlinal conformation (torsion angle - 110°).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260614
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  • 8
    Electronic Resource
    Electronic Resource
    Halogenation of 1-Ethoxy-1-oxophosphindolin-3-one, a Potential Phosphaindigo Precursor (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1765-1770 
    Details
    ISSN: 0009-2940
    Keywords: Phosphinic acid ; Phosphaindole bromination and chlorination ; Layer structure ; Hydrogen bonds ; Bromine-bromine interaction ; Phosphorus heterocycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The bromination of 1-ethoxy-1-oxophosphindolin-3-one (1) with two equivalents oi bromine occurs with elimination of hydrogen bromide and ethyl bromide, providing 2,2-di- bromo-1-hydroxy-1-oxophosphindolin-3-one (4) in high yield. In the presence of triethylamine this process leads to 2,2-dibromo-1-ethoxy-1-Oxophosphindolin-3-one (3) instead. Triethylamine deprotonates 4, providing the solid triethylammonium salt 5. Silylation of 4 with chlorotrimethylsilane leads to the trimethylsilyl ester 6. Monobromination in a two-phase reaction allows the isolation of a mixture of isomers of 2-bromo-1-ethoxy-1-oxophosphindolin-3-one (2a, b). Chlorination with chlorine furnishes 2,2-dichloro-1-ethoxy-1-oxo-phosphindolin-3-one (7). The new compounds 2-7 were characterized analytically and spectroscopically (EI-MS, 1H, 13C and 31P NMR). The crystal structure of acid 4 was determined by X-ray diffraction. Solid 4 consists of aryl stacks connected by chains of P—OH…O==P hydrogen bonds and secondary Br…Br contacts.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301210
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  • 9
    Electronic Resource
    Electronic Resource
    Dichlorogermylene-Alkyldichlorophosphane Reactions Revisited: Characterisation of Bis(trichlorogermyl)phosphanes, Trichlorogermyldiphosphanes, and Ge-P Heterocycles (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1611-1618 
    Details
    ISSN: 0009-2940
    Keywords: Alkyldichlorophosphanes ; Insertions ; Carbene homologues ; Germanium ; Phosphonium germanate(II) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of alkyldichlorophosphanes 1 (RPCl2; R = tert-butyl: 1a, R = isopropyl; 1b, R = 1-adamantyl: 1c) with the germanium dichloride dioxane complex were followed by 31P NMR. Depending on the organic substituents and the reaction conditions, mixtures of trichlorogermylphosphanes RP(GeCl3)2 4a-c, RPHGeCl3 5a-c, diphosphanes R(H)PP(H)GeCl3 6a-c, R(Cl)PP(H)GeCl3 7a, b cyclophosphanes, and Ge-P heterocycles such as triphosphadigermolanes (RP)3(GeCl2)2 8a, b and tetraphosphagermolane (RP)4)GeCl2 10b are formed. As a further unexpected byproduct of the reaction of 1a with GeCl2-dioxane, a small amount of tri-tert-butyl(trichlorogermyl)cyclotetraphosphane 9a was isolated. From the reaction of 1c with two equivalents of GeCl2-dioxane, separation from byproducts 5c and 6c by crystallisation furnished colourless crystals of 4c (R = 1-adamantyl) as the first pure organylbis(trichlorogermyl)phosphane. Surprisingly, the reaction of isoprophylphosphane with germanium tetrachloride, intended to prepare 5a, led to crystalline isopropylphosphonium trichlorogermanate(II) 11. The structures of molecular 4c and 9a and ionic 11 were determined by X-ray crystallography.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301109
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  • 10
    Electronic Resource
    Electronic Resource
    Vierring-Chelatkomplexe von Tellurobis(di-tert-butylphosphan) mit Tetracarbonylmetall (VIA)-Acceptoren (1985)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 118 (1985), S. 1580-1587 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Four-membered Chelate Complexes of Tellurobis(di-tert-butylphosphane) with Tetracarbonylmetal (VI A) AcceptorsTellurobis(di-tert-butylphosphane) (1) reacts with tetracarbonyl(norbornadiene)chromium(0) and -molybdenum(0) with formation of norbornadiene and the new chelate complexes (CO)4M-[P-t-Bu2)2)Te] 2 (M = Cr) and 3 (M = Mo). The corresponding tungsten complex 4 (M = W) is obtained from 1 with the acetonitrile complexes W(CO)6-n(CH3CN)n (n = 2,3). The sulfur ylide complex (CO)4Cr[CH2S(O)(CH3)2]2 reacts with 1 to provide 2 and with methylenebis(di-tert-butylphosphane) (6) to the four-membered chelate complex (CO)4Cr[P-tBu2)2CH2] (8). Spectroscopic data like IR, MS and NMR and the X-ray crystal structure analysis of the chromium complex 2 provide evidence for the function of 1 as rather bulky bidentate ligand in the chelate complexes 2-4.
    Notes: Tellurobis(di-tert-butylphosphan) (1) reagiert mit Tetracarbonyl(norbornadien)chrom(0) und -molybdän(0) unter Verdrängung von Norbornadien zu den Chelatkomplexen (CO)4M[P-t-Bu2)2 Te] 2 (M = Cr) und 3 (M = Mo). Der entsprechende Wolframkomplex 4 (M = W) wird durch Umsetzung von 1 mit dem Acetonitrilkomplexgemisch W (CO)6-n(CH3CN)n (n = 2, 3) erhalten. 2 entsteht auch bei der Umsetzung von 1 mit dem Schwefelylid-Komplex (CO)4Cr[CH2S(O)(CH3)2]2. Methylenbis(di-tert-butylphosphan) (6) gibt unter gleichen Bedingungen den Vierring-Chelatkomplex (CO)4Cr[P-t-Bu2)2CH2] (8). Spektroskopische Daten (IR, MS, NMR) sowie die Kristallstrukturanalyse von 2 belegen die Funktion von 1 als sehr sperrigem zweizähnigem Phosphorliganden.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19851180425
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