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  • Inorganic Chemistry  (4)
  • μ-Isonitrile complexes  (2)
  • Dinuclear complexes  (1)
  • Hydrido complexes  (1)
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  • 1
    Digitale Medien
    Digitale Medien
    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
    Schlagwort(e): Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: 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.
    Notizen: 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.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/cber.19871200603
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  • 2
    Digitale Medien
    Digitale Medien
    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
    Schlagwort(e): Dinuclear complexes ; Iron complexes ; Platinum complexes ; Silyl complexes ; Phosphide bridges ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/cber.19931260104
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  • 3
    Digitale Medien
    Digitale Medien
    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
    Schlagwort(e): Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: 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.
    Notizen: 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.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/cber.19871200703
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  • 4
    Digitale Medien
    Digitale Medien
    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
    Schlagwort(e): Heterobimetallic complexes ; Iron complexes ; Platinum complexes ; Silyl complexes ; Phosphido bridges ; Hydrido complexes ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/cber.19941270204
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  • 5
    Digitale Medien
    Digitale Medien
    Synthesis, Reactivity, and Molecular Structures of Bis(diphenylphosphanyl)amine- and Bis(diphenylphosphanyl)amide-Bridged Heterobimetallic μ-Isonitrile- and μ-Aminocarbyne Complexes (Fe-Pt) (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 495-499 
    Details
    ISSN: 1434-1948
    Schlagwort(e): Heterobimetallics ; μ-Isonitrile complexes ; μ-Aminocarbyne complexes ; Bis(diphenylphosphanyl)amine ; Iron ; Platinum ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Addition of isonitriles to [(OC)3Fe(μ-CO)(μ-Ph2PNHPPh2)Pt(PPh3)] 1 produces the μ-isonitrile complexes [(OC)3Fe(μ-C=NR)(μ-Ph2PNHPPh2)Pt(PPh3)] 2, which are transformed to the μ-aminocarbyne complexes [(OC)3Fe{μ-CN(El)R}(μ-Ph2PNHPPh2)Pt(PPh3)]+;3 and 4 by electrophilic addition of [El][BF4] or [El][OSO2CF3] (El = H, Me). The dppa backbone of 4 is readily deprotonated by KOSiMe3 to yield the very stable zwitterionic aminocarbyne complex [(OC)3Fe{μ-CN(Me)2,6-xylyl}(μ-Ph2PNPPh2)Pt(PPh3)] 5.
    Materialart: Digitale Medien
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  • 6
    Digitale Medien
    Digitale Medien
    Reactivity of Silyl-Substituted Heterobimetallic Iron-Platinum Hydride Complexes towards Unsaturated Molecules, I Alkyne Insertions into the Platinum-Hydride Bond, Phosphane-Induced σ-Alkenyl-μ-Vinylidene Rearrangements and Formation of μ-Isonitrile Complexes (2000)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 241-252 
    Details
    ISSN: 1434-1948
    Schlagwort(e): Heterobimetallics ; Hydride complexes ; Alkenyl complexes ; μ-Isonitrile complexes ; Silicon ; Iron ; Platinum ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The heterobimetallic hydride complexes [(OC)3Fe{Si(OMe)3}(μ-Ph2PXPPh2)Pt(H)(PR3)] (1a: X = CH2, PR3 = PPh3; 1b: X = NH, PR3 = PPh3; 1c: X = CH2, PR3 = PMePh2) have been prepared by the oxidative addition of [(OC)3Fe(H){Si(OMe)3}(η1-Ph2PXPPh2)] to [Pt(H2C=CH2)(PPh3)2] or by reaction of K[(OC)3Fe{Si(OMe)3}(η1-dppm)] with trans-[Pt(Cl)(H)(PPh3)2]. The solid-state structure of compound 1b has been determined by single-crystal X-ray diffraction. 1-Alkynes such as methylpropiolate or phenylacetylene insert in a regiospecific manner into the Pt-H bond of 1 to yield the σ-alkenyl complexes [(OC)3Fe{μ-Si(OMe)2(OMe)}(μ-Ph2PXPPh2)Pt{C(R)=CH2}] (2a: X = CH2, R = CO2Me; 2b: X = NH, R = CO2Me; 3a: X = CH2, R = Ph). Addition of the Pt-H bond of 3a across the triple bond of [D1]phenylacetylene affords [(OC)3Fe{μ-Si(OMe)2(OMe)}(μ-dppm)Pt{C(Ph)=C(D)H}] (3a*) having the deuteron trans to platinum (cis addition). This insertion reaction is accompanied by dissociation of the platinum-bonded PR3 ligand and saturation of the vacant coordination site by a dative μ-η2-Si-O→Pt interaction. When 3 is treated with PR3 again, a subsequent phosphane-induced rearrangement leading to vinylidene-bridged complexes [(OC)3Fe{μ-C=C(H)R′}(μ-Ph2PXPPh2)Pt(PR3)] (4a: X = CH2, R′ = Ph, PR3 = PPh3; 4b: X = NH, R′ = Ph, PR3 = PPh3; 4c: X = CH2, R′ = Ph, PR3 = PMePh2; 4d: X = CH2, R′ = p-tolyl, PR3 = PPh3) occurs. Upon purging a solution of 3a with carbon monoxide, the labile CO adduct [(OC)3Fe{Si(OMe)3}(μ-dppm)-Pt(CO){C(Ph)=CH2}] 5a is formed, addition of 2,6-xylyl isocyanide to 2a and 3a affords the isonitrile adducts [(OC)3Fe{Si(OMe)3}(μ-dppm)Pt(CNxylyl){C(R)=CH2}] (5b: R = CO2Me; 5c: R = Ph), respectively. When hydride complex 1a is allowed to react with stoichiometric amounts of aromatic isonitriles, formal elimination of HSi(OMe)3 occurs, yielding the heterodinuclear isonitrile-bridged complexes [(OC)3Fe(μ-C=N-R)(μ-dppm)Pt(PPh3)] (6a: R = 2,6-xylyl; 6b: R = o-anisyl; 6c: R = p-anisyl; 6d: R = p-C6H4NH2) and the bis(isonitrile) complexes [(OC)2(RN≡C)Fe(μ-C=N-R)(μ-dppm)Pt(PPh3)] (7a: R = 2,6-xylyl; 7b: R = p-anisyl). Single-crystal X-ray diffraction studies perfomed on 6a and 6b reveal that the molecular structures of these μ-isonitrile complexes closely resemble the μ-vinylidene complexes 4. The two metal centers are bridged in a symmetric manner by strongly bent CNR ligands, the aromatic groups R being oriented towards the Fe(CO)3 moiety. Electrophilic addition of HBF4 to the basic nitrogen atom of the μ-CNR ligand transforms 6 to the cationic μ-aminocarbyne complexes [(OC)3Fe{μ-CN(H)R}(μ-dppm)Pt(PPh3)][BF4] (8a: R = 2,6-xylyl; 8b: R = p-anisyl; 8c: R = p-C6H4NH2).
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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