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  • 1
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Silyl-Komplexe, 18 Hydrido-Silyl- und Bissilyl-Komplexe des Eisens mit verbrückenden oder chelatisierenden Diphosphinoethan-Liganden (1987)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 120 (1987), S. 879-887 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complexes [mer-(CO)3Fe(H)SiR3]2(dppe) (1) (dppe=Ph2PCH2-CH2PPh2), [mer-(CO)3Fe(SiR3)2]2(dppe) (2), (CO)2(dppe)Fe(H)-Sir3 (3), and (CO)2(dppe)Fe(SiR3)2 (6) are synthetized by several routes: by photochemical reaction of dppe-substituted iron carbonyls with HSiR3, by thermal reaction of (CO)4Fe(H)SiR3 or (CO)4Fe(SiR3)2 with dppe, or by exchange of the silyl groups. The dinuclear complexes 1 and 2 can be converted to the mononuclear complexes 3 and 6. The choice of the most suitable method of preparation depends essentially on the nature of the silyl ligand. Bissilyl complexes (2 or 6) are only obtained if SiR3=SiCl3 or SiMeCl2. In solution the complexes 3 are fluxional. In the crystalline state 3d (SiR3=SiMe3) shows a distorted octahedral geometry. The silyl group has trans orientation to one of the phosphorus atoms and cis to the hydride ligand, which in turn is trans to one of the carbonyls.
    Notes: Komplexe [mer-(CO)3Fe(H)SiR3]2(dppe) (1) (dppe=Ph2PCH2CH2PPh2), [mer-(CO)3Fe(SiR3)2]2(dppe) (2), (CO)2(dppe)Fe(H)-SiR3 (3) und (CO)2(dppe)Fe(SiR3)2 (6) können nach mehreren Methoden synthetisiert werden: durch photochemische Umsetzung von dppe-substituierten Eisencarbonylen mit HSiR3, durch thermische Umsetzung von (CO)4Fe(H)SiR3 oder (CO)4Fe(SiR3)2 mit dppe oder durch Silylgruppenaustausch. Die zweikernigen Komplexe 1 und 2 lassen sich in die einkernigen Komplexe 3 und 6 umwandeln. Die Wahl der jeweils günstigsten Darstellungsmethode hängt entscheidend von der Art des Silylrestes ab. Bissilyl-Komplexe (2 oder 6) werden nur mit SiR3=SiCl3 oder SiMeCl2 erhalten. Die Komplexe 3 sind in Lösung fluktuierend. Im kristallinen Zustand ist 3d (SiR3=SiMe3) verzerrt oktaedrisch koordiniert, der SiMe3-Rest steht trans zu einem der Phosphoratome und cis zum Hydrid-Liganden, welcher seinerseits trans zu einem der Carbonyle angeordnet ist.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19871200603
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  • 2
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Silyl-Komplexe, 44. Darstellung der zweikernigen Silyl-Komplexe (CO)3(R3Si)Fe(μ-PR′R′′)Pt(PPh3)2 durch oxidative Addition von (CO)3(R′R′′HP)Fe(H)SiR3 an (C2H4)Pt(PPh3)2 (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 17-21 
    Details
    ISSN: 0009-2940
    Keywords: Dinuclear complexes ; Iron complexes ; Platinum complexes ; Silyl complexes ; Phosphide bridges ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition Metal Silyl Complexes, 44.  -  Preparation of the Binuclear Silyl Complexes (CO)3(R3Si)Fe(μ-PR′R′′)Pt(PPh3)2 by Oxidative Addition of (CO)3(R′R′′HP)Fe(H)SiR3 to (C2H4)Pt(PPh3)2The complexes (CO)3(R′R′′HP)Fe(H)SiR3 (1) [PHR′R′′ = PHPh2, PH2Ph, PH2Cy; SiR3 = SiPh3, SiPh2Me, SiPhMe2, Si(OMe)3] react with Pt(C2H4)(PPh3)2 to give the dinuclear, silyl-substituted complexes (CO)3(R3Si)Fe(μ-PR′R′′)Pt(PPh3)2 (2) in high yields. Upon reaction of 2 (R = R′ R′′ = Ph) with CO, the PPh3 ligand at Pt being trans to the PPh2 bridge is exchanged, and (CO)3(Ph3Si)Fe(μ-PPh2)Pt(PPh3)CO (3) is formed. Complex 3 is characterized by an X-ray structure analysis. The rather short Fe  -  Si distance [233.9(2) pm] and the infrared spectrum of 3 indicate that the Fe  -  Pt bond is quite polar.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260104
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  • 3
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Silyl-Komplexe, 201) Untersuchungen zur Reaktivität der anionischen Silyl-Komplexe [Fe(CO)3(PR′3)SiR3]- (1987)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 120 (1987), S. 1079-1085 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition-Metal Silyl Complexes, 201). - Investigations on the Reactivity of the Anionic Silyl Complexes [Fe(CO)3(PR3′)SiR3[-Phosphane-substituted anionic silyl complexes [Fe(CO)3(PR′3)SiR3]- (1) are distinctly more reactive than their tetracarbonyl analoga, particularly towards metal or metal-complex halides. Their solution structure depends on the corresponding cation, with which they are able to form contact ion pairs. Reaction of 1 with CH3I, Me2SiHCl or Me3SnCl (R″3EX) yields phosphanesubstituted alkyl silyl, bissilyl or silyl stannyl complexes mer-Fe(CO)3(PR′3)(ER″3)SiR3. By reaction of 1 with (Ph3PAgCl)4, Ph3PAuCl, PhHgBr or HgBr2 (LnMX) stable hetero-binuclear complexes mer-Fe(CO)3(PR′3)SiR3)MLn can be prepared, which contain unsupported Fe-Ag-, Fe-Au-, or Fe-Hg bonds. X-ray structure analysis of Fe(CO)3(PPh3)(SiMePh2)AuPPh3 (6) (Fe-Au 255.1 (1), Fe-Si 235.7 (3) pm) reveals that the SiMePh2 and the PPh3 ligand are cis oriented to the Fe-Au bond.
    Notes: Die phosphansubstituierten anionischen Silyl-Komplexe [Fe(CO)3(PR′3)SiR3]- (1) sind besonders gegenüber Metall- oder Metallkomplex-Halogeniden deutlich reaktiver als ihre Tetracarbonyl-Analoga. Ihre Struktur in Lösung hängt vom jeweiligen Kation ab, mit dem sie Kontaktionenpaare ausbilden können. Reaktion von 1 mit CH3I, Me2SiHCl oder Me3SnCl (R″3EX) ergibt phosphansubstituierte Alkyl-Silyl-, Bissilyl- oder Silyl-Stannyl-Komplexe mer-Fe(CO)3(PR′3)(ER″3)SiR3. Durch Umsetzung von 1 mit (Ph3PAgCl)4, Ph3PAuCl, PhHgBr oder HgBr2 (LnMX) können die stabilen Hetero-Zweikernkomplexe mer-Fe(CO)3(PR′3)-(SiR3)MLn dargestellt werden, die unverbrückte Fe-Ag-, Fe-Au- oder Fe-Hg-Bindungen enthalten. Die Röntgenstrukturanalyse von Fe(CO)3(PPh3)(SiMePh2)AuPPh3 (6) (Fe-Au 255.1 (1), Fe-Si 235.7(3) pm) zeigt, daß der SiMePh2- und der PPh3-Ligand cis zur Fe-Au-Bindung angeordnet sind.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19871200703
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  • 4
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Silyl-Komplexe, 48. Synthese neuartiger heteronuklearer Silyl-Zweikernkomplexe (OC)3(R3Si)Fe(μ-PR′R″)Pt(1,5-COD)(Fe-Pt), Phosphan-Austauschreaktionen an (OC)3 (R3Si)Fe(μ-PR′R″)Pt(PPh3)2(Fe - Pt) und Darstellung der Dihydrido-Komplexe [(OC)3Fe(μ-PPh2)(μ-H)2Pt(PR3)2][BF4](Fe - Pt) (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 295-304 
    Details
    ISSN: 0009-2940
    Keywords: Heterobimetallic complexes ; Iron complexes ; Platinum complexes ; Silyl complexes ; Phosphido bridges ; Hydrido complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition Metal Silyl Complexes, 48[1]. - Synthesis of the New Heterobimetallic Dinuclear Silyl Complexes (OC)3(R3Si)-Fe(μ-PR′R″)Pt(1,5-COD)(Fe-Pt), Phosphane Exchange Reactions of (OC)3(R3Si)Fe(μ-PR′R″)Pt(PPh3)2(Fe-Pt), and Preparation of the Dihydrido complexes [(OC)3Fe(μ-PPh2)(μ-H)2Pt(PR3)2][BF4](Fe-Pt)The dinuclear, silyl-substituted complexes (OC)3(R3Si)Fe(μ-PR′r″)Pt(1,5-COD) (1) [μ-PR′R″ = PPh2, PCY2, PHPh; SiR3 = SiPh3, Si(OMe)3] were prepared in high yields by the oxidative addition of the hydrido complexes (OC)3(PHR′R″)Fe(H)-SiR3 to Pt(1,5-COD)2. Upon reaction of (OC)3(R3Si)Fe(μ-PR′R″)Pt(PPh3)2 [μ-PR′R″ = PPh2, PHCy; SiR3 = SiPh3, SiPh2Me, SiPhMeCl, Si(OMe)3] with two equivalents of PR‴3 (PMe3, PBu3, PEt3) or with one equivalent of chelating di-phosphanes (vdpp, dppe, dppm) both PPh3 ligands are displaced, and (OC)3(R3Si)Fe(μ-PR′R″)Pt(PR‴3)2 or (OC)3(R3Si)-Fe(μ-PR′R″)Pt[(PPh2)2X] (X = C=CH2, C2H4, CH2) are formed, respectively. When one equivalent of PMe3 is used, only the PPh3 ligand trans to the μ-PPh2 bridge is substituted, and (OC)3(Ph3Si)Fe(μ-PPh2)Pt(PPh3)(PMe3 is formed. The 1,5-COD ligand in 1 is displaced by P(OR)3 to give (OC)3-(Ph3Si)Fe(μ-PPh2)Pt[P(OR)3]2 (R = Me, Ph). The complexes (OC)3(Ph3Si)Fe(μ-PPh2)Pt(PMe3)2and (OC)3(Ph3Si)Fe(μ-PPh2)Pt[(PPh2)2C=CH2] were characterized by X-ray structure analysis. The short Fe-Si distances [233.0(2) and 235.6(3) pm] and the infrared v(CO) absorptions indicate that the Fe-Pt bonds are quite polar. Protonation of (OC)3(Me2-PhSi)Fe(μPPh2)Pt(PPh3)2 with CF3COOH gives the hydrido-bridged complex [(OC)3(Me2PhSi)Fe(μ-PPh2)(μ-H)Pt-(PPh3)2][O2CCF3]. Upon addition of an excess of HBF4 · Et2O to (OC)3(R3Si)Fe(μ-PPh2)Pt(PPh3)2 (R = Ph, OMe), (OC)3-Si)Fe(μ-PPh2)Pt[Pt[P(OMe)3]2 or (OC)3(Ph2MeSi)Fe(μ-PPh2)-Pt(dppe) R3SiF is split, and the corresponding μ-dihydrido complexes [(OC)3Fe(μ-PPh2)(μ-H)2Pt(PR3)2][BF4] are obtained.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270204
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