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  • 1
    Electronic Resource
    Electronic Resource
    Chlorides of antimony and tin as reagents for syntheses of cyclic and linear Chloropermethylpolysilanes (1990)
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 332 (1990), S. 229-232 
    Details
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of c-Si6Me12 with SbCl5 proceeds with cleavage of the methyl groups from silicon and gives c-ClSi6Me11 and c-Cl2Si6Me10 as main products. The molar ratio of those compounds depends on solvent. The same chlorodemethylation reaction takes place if c-Si6Me12 reacts with GaCl3.The reaction with SnCl4 proceeds with cleavage of the Si—Si bonds of polysilane and α,ω-dichloropermethylpolysilanes, with the 1,6-Cl2Si6Me12 as the main product, are formed.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prac.19903320214
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  • 2
    Electronic Resource
    Electronic Resource
    Die Struktur des 1,3-Dimethyl-1,1,3,3-tetraphenyldisiloxans (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 17-22 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of 1,3-Dimethyl-1,1,3,3-tetraphenyldisiloxane1,3-Dimethyl-1,1,3,3-tetraphenyldisiloxane 1 crystallizes monoclinically (P21/n; a = 2237.5; b = 801.4; c = 1396.6 pm, β = 106.29°; Z = 4). The X-ray structural analysis shows a bent configuration of the molecule with Si—O—Si angle = 140°, d(Si—O) = 163.8 pm. The staggered conformation of the six Si—C bonds is distorted. The methyl groups are in gauche position.The results are discussed with respect to an intramolecular H…O interaction in the structure of 1,1,3,3-tetraphenyldisiloxane.
    Notes: 1,3-Dimethyl-1,1,3,3-tetraphenyldisiloxan 1 kristallisiert monoklin (P21/n; a = 2237,5; b = 801,4; c = 1396,6 pm; β = 106,29°; Z = 4). Die Kristallstrukturanalyse ergab eine gewinkelte Konfiguration des Moleküls mit Si—O—Si = 140° und d(Si—O) = 163,8 pm. Die Substituenten an dem Silicium-Atom zeigen eine Abweichung von einer gestaffelten Anordnung der sechs Si—C-Bindungen. Die Methylgruppen sind in gauche-Position.Die Ergebnisse werden im Zusammenhang mit der Struktur des 1,1,3,3-Tetraphenyldisiloxans hinsichtlich einer intramolekularen H…O-Wechselwirkung diskutiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885620103
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  • 3
    Electronic Resource
    Electronic Resource
    Beiträge zur Chemie der Silicium-Schwefel-Verbindungen. 52 [1]. Reaktion von Trialkoxysilanthiolen mit Carbonsäuren. Darstellung und Hydrolyse der Trialkoxyacyloxysilane (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 153-159 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon-Sulphur Compounds. 52. Reaction of Trialkoxysilanethiols with Carboxylic Acids. Preparation and Hydrolysis of TrialkoxyacyloxysilanesThe series of trialkoxyacyloxysilanes have been prepared almost quantitatively from trialkoxysilanethiols (RO)3SiSH (R = i-Pr, s-Bu, s-n-Am, s-i-Am) by the reaction with carboxylic acids R′COOH (R′ = Alkyl or Ph). Kinetics of the acidolysis of (RO)3SiSH as well as hydrolysis of (RO)3SiOCOR′ were investigated and consequently the reaction mechanisms are proposed.
    Notes: Durch Umsetzung von Trialkoxysilanthiolen (RO)3SiSH (R = i-Pr, s-Bu, s-n-Am, s-i-Am) und Carbonsäuren R′COOH (R′ = Alkyl bzw. Ph) wurden fast quantitativ mehrere Trialkoxyacyloxysilane (RO)3SiOCOR′ erhalten. Die Kinetik dieser Acidolysereaktion von (RO)3SiSH wie auch der Hydrolysereaktion von (RO)3SiOCOR′ wurde untersucht und in der Folge die Reaktionsmechanismen formuliert.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885620119
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  • 4
    Electronic Resource
    Electronic Resource
    Darstellung und Struktur von tert-Butyl(tert-butylamino)-[tris(tert-butyloxy)silylthio]boran (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 556 (1988), S. 92-96 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Structure of tert-Butyl(tert-butylamino) [tris(tert-butyloxy)silylthio]-boraneThe smooth addition of the SH bond of (tBuO)3SiSH to the BN bond of tBuB≡NtBu gives the title compound, which crystallizes in the triclinic system, space group P1, with an unexpectedly short BN bond, d(BN) = 137 pm, in a Z configuration.
    Notes: Die SH-Bindung von (tBuO)3SiSH addiert sich glatt an die BN-Bindung von tBuB≡NtBu unter Bildung der Titelverbindung. Diese kristallisiert triklin, Raumgruppe P1, mit einer unerwartet kurzen, Z-konfigurierten BN-Bindung, d(BN) = 137 pm.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885560109
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  • 5
    Electronic Resource
    Electronic Resource
    Darstellung und Strukturen einiger N-(Tri-t-butoxysilyl)anilin-Derivate (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 377-384 
    Details
    ISSN: 0044-2313
    Keywords: One-pot reactions of tri-t-butoxychlorosilane, K-t-butanolate and substituted anilines. Crystal structure analyses of N-(tri-t-butoxysilyl)-aniline, C18H33NO3Si ; N-(tri-t-butoxysilyl)-p-nitroaniline, C18H32N2O5Si ; N-Methyl-(N-tri-t-butoxysilyl)-p-nitroaniline C19H34N2O5Si ; N-(tri-t-butoxysilyl)-p-cyanoaniline, C19H32N2O3Si ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Structures of N-(tri-t-butoxysilyl)aniline CompoundsPara-substituted N-(tri-t-butoxysilyl)anilines (t-BuO)3SiNRC4H4X-p, R = H, CH3, with substituents of high electron affinity (X = CN, NO2) were prepared by a one-pot reaction of tri-t-butoxychlorsilane, potassium t-butanolate and substituted anilines. Corresponding compounds with substituents of low electron affinity (X = OMe, H) preferably were prepared by metalation of anilines with sodium amide. Four crystal structures were determined. N-(tri-t-butoxysilyl)-p-nitro-aniline, N-methyl-(N-tri-t-butoxysilyl)-p-nitroaniline and N-(tri-t-butoxysilyl)-p-cyanoaniline crystallize at 298 K monoclinically, N-(tri-t-butoxysilyl)aniline crystallizes orthorhombically.
    Notes: Derivate des para-substituierten N-(Tri-t-butoxysilyl)anilins (t-BuO)3SiNRC6H4X-p, R = H, CH3 mit Substituenten hoher Elektronenaffinität (X = CN, NO2) wurden nach einem neuen Eintopfverfahren aus Tri-t-butoxychlorsilan, Kalium-t-butanolat und dem entsprechend substituierten Anilin dargestellt. Für Substituenten niederer Elektronenaffinität (X = OMe, H) wird die Methode der Metallierung von Anilinen mit Natriumamid bevorzugt. Vier Kristallstrukturen wurden bestimmt. N-(Tri-t-butoxysilyl)-p-nitroanilin, N-Methyl-(N-tri-t-butoxysilyl)-p-nitroanilin und N-(Tri-t-butoxysilyl)-p-cyanoanilin kristallisieren bei 298 K monoklin, N-(Tri-t-butoxysilyl)anilin kristallisiert orthorhombisch.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200230
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  • 6
    Electronic Resource
    Electronic Resource
    Contributions to the Chemistry of Silicon-Sulfur Compounds. 65 synthesis, crystal and molecular structure of cyclo-tetrakis[tri-tert-butoxysilanethiolatogold(I)], [(t-C4H9O)3SiSAu]4, the first example of an Au4S4 ring System (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1417-1421 
    Details
    ISSN: 0044-2313
    Keywords: Gold ; thiolate complex ; synthesis ; structure ; X-ray ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Beiträge zur Chemie der Silicium-Schwefel-Verbindungen. 65. Darstellung, Kristall- und Molekülstruktur von cyclo-Tetrakis[tri-tert-butoxysilanthiolatogold(I)], [(t-C4H9O)3SiSAu]4, dem ersten Komplex mit einem Au4S4-Ring-SystemDie Darstellung des ersten Silanthiolato-Goldkomplexes - cyclo-Tetrakis[tri-tert-butoxysilanthiolatogold(I)] - ist beschrieben. Die Kristallstruktur wurde bei 200 K an einem farblosen, orthorhombischen Prisma bestimmt. Bei 187 K wurde eine reversible Phasenumwandlung beobachtet. Das Zentrum des Moleküls ist ein gefalteter Au4S4-Achtring mit alternierender Abfolge aus dreifach koordinierten Schwefel- und zweifach koordinierten Goldatomen. Charakteristische Abstände und Winkel: Au—S 228,4 und 229,6 pm, Si—S 216,9 pm, S—Au—S 178,8° und 178,3°, Au—S—Au 90,3°, Si—S—Au 103,7° und 101,9°. Der kürzeste Abstand zwischen zwei Goldatomen beträgt 324,8 pm.
    Notes: The preparation of the first silanethiolate complex of gold, cyclo-tetrakis[tri-tert-butoxysilanethiolatogold(I)] from tri-tert-butoxysilanethiol and tetrachloroauric acid is described. The compound forms colorless orthorhombic crystals, and the molecular structure was determined at 200 K by single crystal X-ray diffraction. At 187 K, a possible, reversible phase transition is observed. The center of the molecule is a distinctly folded eight-membered Au4S4 ring of alternating three-fold coordinated sulfur and two-fold coordinated gold atoms. The relevant bond lengths and angles are: Au—S 228.4 and 229.6 pm, Si—S 216.9 pm, S—Au—S 178.8° and 178.3°, Au—S—Au 90.3°, Si—S—Au 103.7° and 101.9°. The gold atoms are separated by 324.8 pm.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200816
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  • 7
    Electronic Resource
    Electronic Resource
    Beiträge zur Chemie der Silicium-Schwefel-Verbindungen. 53. Die Struktur des 1,3-Dimethyl-1,1,3,3-Tetraphenyldisilthians (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 48-52 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon-Sulphur Compounds. 53. Structure of 1,3-Dimethyl-1,1,3,3-tetraphenyldisilthiane1,3-Dimethyl-1,1,3,3-tetraphenyldisilthiane was obtained by an insertion reaction of sulphur with Ph2 MeSiH. The compound crystallizes triclinically (P1; a = 1166.7; b = 1231.1; c = 988.6 pm; α = 113.23; β = 90.34; γ = 112.43°; Z = 2). The X-ray structure analysis shows a bent configuration of the molecule with Si—S—Si = 108.7°. The results are discussed together with the structures of hexaphenyldisilthiane and dimethyltetraphenyldisiloxane.
    Notes: 1,3-Dimethyl-1,1,3,3-tetraphenyldisilthian entsteht aus Schwefel und Ph2MeSiH in einer Einschub-Reaktion. Die Verbindung kristallisiert triklin (P1; a = 1166,7; b = 1231,1; c = 988,6 pm; α = 113,23; β = 90,34; γ = 112,43°; Z = 2). Die Kristallstruktur-analyse ergab eine gewinkelte Konfiguration des Moleküls mit Si—S—Si = 180,7°. Die Ergebnisse werden im Zusammenhang mit der Struktur des Hexaphenyldisilthians und Dimethyltetraphenyl disiloxans diskutiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885630107
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  • 8
    Electronic Resource
    Electronic Resource
    Beiträge zur Chemie der Silicium-Schwefel-Verbindungen. XL .Struktur α,ω-substituierter Permethylpolysilane (SiMe2)nR2 mit R = (t-BuO)3SiS und n = 2, 3, 6Professor Paul Hagenmuller zum 65. Geburtstage am 3. August 1986 gewidmet (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 540 (1986), S. 271-280 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon-Sulfur Compounds. XL. Structure of α,ω-substituted Permethylpolysilanes (SiMe2)nR2, with R = (t-BuO)3SiS and n = 2, 3, 6The α,ω-substituted permethylpolysilanes (SiMe2)nR2 with R = (t-BuO)3SiS and n = 2, 3, 6, were obtained by reaction of α,ω-dichloropermethylpolysilanes with (t-BuO)3SiSH and Et3N. The crystal Structures were Determined. The mean value of the Si—Si bond distances in the polysilane chains is d(Si—Si) = 233.8(7) pm within small variations. However, in the hexasilane a tendency to Stretch the central bond (234.9 pm) may be observed. The mean value of the Si—S bond length is 213.5 pm. A special feature of the conformation of the disilane and hexasilane derivatives, is the almost in a plane arranged zigzag chain of six or ten atoms, respectively. However, the chain of seven atoms in trisilane derivative is different due to a 120° torsion around the third bond in this chain. Some Structural Details are discussed.
    Notes: α,ω-substituierte Permethylpolysilane (SiMe2)nR2 mit R = (t-BuO)3SiS und n = 2, 3, 6 wurden durch Reaktion der α,ω-Dichloropermethylsilane mit (t-BuO)3SiSH und Et3N dargestellt. Die Kristallstrukturen wurden bestimmt. In Den Polysilanketten liegen Bindungslängen mit geringen Variationen bei d(Si—Si) = 233,8(7) pm. Lediglich im Hexasilan wird eine Tendenz zur Streckung der zentralen Bindung auf 234,9 pm sichtbar. Der Mittelwert für die Si-S-Bindungslängen beträgt 213,5 pm. Ein besonderes Merkmal der Konformation Von Disilan und Hexasilan ist die nahezu in einer Ebene verlaufende Zick-Zack-Kette aus sechs bzw. zehn Atomen. Im Trisilan ist die Kette aus sieben Atomen dagegen an der dritten Bindung um 120° tordiert. Die Einzelheiten der Strukturen werden im Zusammenhang diskutiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865400930
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  • 9
    Electronic Resource
    Electronic Resource
    Die Struktur des Tetraphenyldisiloxans (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 537 (1986), S. 31-39 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of TetraphenyldisiloxaneTetraphenyldisiloxane 1 crystallizes at 298 K monoclinically (P21/n; a = 1407.6; b = 610.7; c = 1262.7 pm; β = 95.87° Z = 2) and undergoes a second order phase transition at 200 K, in an almost unchanged structure of triclinic symmetry. At 298 K the molecules are already bent (Si—O—Si = 160°) with static or dynamical disorder of the bridging atom. Both Si—O distances are different (156 or 169 pm), because the shift of the bridging O atom is not perpendicular to the Si—to—Si vector. The reason for this remarkable behavior is not yet clear. According to the vibrational spectra, the Si—O—Si bridge is bent in the crystal but, in CCl4 solution a dynamical oscillation through the linear configuration may occur.
    Notes: Tetraphenyldisiloxan 1 kristallisiert bei 298 K monoklin (P21/n; a = 1407,6 pm; b = 610,7 pm; c = 1262,7 pm; β = 95,87° Z = 2) und durchläuft bei 200 K einen Phasenübergang 2. Ordnung in eine kaum veränderte Struktur trikliner Symmetrie. Bereits bei 298 K liegen in der Struktur gewinkelte Moleküle (Si—O—Si = 160°) mit statischer oder dynamischer Fehlordnung des Brückenatoms vor. Die beiden Abstände Si—O sind verschieden (156 bzw. 169 pm), weil die Auslenkung des Brückenatoms aus der zentralen Lage nicht senkrecht zum Vektor Si—Si erfolgt. Der Grund für dieses merkwürdige Verhalten ist unklar. Die Schwingungsspektren beweisen für den kristallinen Zustand ebenfalls die gewinkelte Struktur, während in CCl4-Lösungen ein dynamisches Durchschwingen durch die gestreckte Konfiguration wahrscheinlich ist.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865370604
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  • 10
    Electronic Resource
    Electronic Resource
    Beiträge zur Chemie der Silicium-Schwefel-Verbindungen. XLIX. Reaktion von Silicium-Schwefel-Verbindungen mit Glykolen (1987)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 554 (1987), S. 197-204 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contribtions to the Chemistry of Silicon-Sulphur Compounds. XLIX. Reaction of Silicon-Sulphur Compounds with GlycolsThe reactions of Ph3SiSH, (RO)3SiSH, (RO)2Si(SH)2, cyclo-[(t-BuO)2SiS]2, and SiS2 with aliphatic glycols were investigated. Among other compounds representatives of a new group of silanethiols (t-BuO)2Si(SH)OrOSi(SH)(OBu-t)2 (r = pr; neopent)r = kohlenwasserstoffgerüst des Glykols: pr = —CH2CH2CH2—, bu = —CH2(CH2)2CH2—, hex = —CH2(CH2)4CH2—, neopent = —CH2C(CH3)2CH2—, pin = —C(CH3)2C(CH3)2— were obtained. Informations about the hydrolytic splitting of the Si—S bond of the prepared silanethiols were obtained by thiomercurimetric titration. A pathway of the reaction of SiS 2 with glycols is discussed.
    Notes: Die Reaktionen von Ph3SiSH, (RO)3SiSH, (RO)2Si(SH)2, cyclo-[(t-BuO)2SiS]2 und SiS2 mit aliphatischen Glykolen wurden untersucht. Neben anderen Verbindungen wurden Vertreter einer neuen Gruppe von Silanthiolen (t-BuO)2Si(SH)OrOSi(SH)(OBu-t)2 (r = pr; neopent) erhalten. Informationen über die hydrolytische Spaltung der Si—S-Bindung der erhaltenen Silanthiole wurden mittels thiomercurimetrischer Titration erhalten. Eine Reaktionsfolge der Um-setzung von SiS2 mit Glykolen wird diskutiert.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19875541126
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