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  • 1
    Electronic Resource
    Electronic Resource
    Neopentane-Based Tripodal CpL2 Ligands: Synthesis and Reactions of CH3C(CH2-η5-C5H4)(CH2-η1-PPh2)2RuCl; Hindered Rotation of Vinylidene Ligands (2000)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 33-50 
    Details
    ISSN: 1434-1948
    Keywords: Tripod ligands ; Hindered rotation of vinylidene ligands ; CpML2 chelate ligands ; Ruthenium ; Carbenes ; Carbene-type ligands ; Cyclic voltammetry ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tripodal ligand [CH3C(CH2C5H4)(CH2PPh2)2]- reacts with RuCl2(PPh3)3 to produce CH3C(CH2-η5-C5H4)(CH2-η1-PPh2)2RuCl, [tripodCpL2RuCl], 1. Complex 1 undergoes substitution of the chlorine function with various nucleophiles L′ to produce [tripodCpL2RuL′]+. The carbonyl derivative (L′ = CO) 2, isonitrile (L′ = RNC) 3, nitrile compounds (L′ = RCN) 4, and a tolane adduct (L′ = η2-PhC≡CPh) 5 are obtained when 1 is treated with the appropriate ligands in polar solvents. Halide acceptors (e.g. TlPF6) are generally needed to promote these reactions. The cyanide derivative tripodCpL2RuCN (3a) is alkylated by F3CSO3CH3 to give the isonitrile derivative [tripodCpL2RuCNMe]+3b. Terminal alkynes HC≡CR produce vinylidene compounds [tripodCpL2RuL′]+, where L′ = C=CHR (R = tBu, 7b; R = Ph, 7c), or allenylidene derivatives, L′ = C=C=CPh2 (6), depending on the nature of R (R = CPh2OH for synthesis of 6). Trimethylsilylacetylene gives the parent vinylidene species, L′ = C=CH2 (7a), which is transformed to the Fischer-type carbene compound, L′ = C(OMe)Me (8), upon treatment with methanol. The vinylidene species 7 are deprotonated by NaOMe to produce the alkynyl compounds tripodCpL2RuC≡CR (9). Methylation of 9 with F3CSO3CH3 results in the vinylidene derivatives L′ = C=C(Me)R (R = tBu, 7d; R = Ph, 7e), having two organic substituents at the terminal carbon centre. For all vinylidene compounds with two different substituents at their terminal carbon atom, hindered rotation of the single-faced vinylidene π-ligand about its Ru-C bond is observed. Analysis by 31P-NMR spectroscopic coalescence measurements as well as line-shape analyses reveals activation enthalpies of around 40 kJmol-1 for this rotation, with small activation entropies of around ±10 Jmol-1K-1. Solid-state structures of nine compounds of the type [tripodCpL2RuL′]+n (n = 0, 1) demonstrate the remarkable conformational rigidity of the tripodCpL2Ru template. They also show that the possible strain imposed by linking the Cp ligand and the two donor groups L in one and the same chelate scaffolding does not appear to impose a serious steric strain on these templates.
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  • 2
    Electronic Resource
    Electronic Resource
    Electron Transfer in Dinuclear Cobalt Complexes with “Non-innocent” Bridging LigandsPart of this work was presented at the 31st International Conference on Coordination Chemistry, Vancouver (Canada), August 1996. (1997)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 3 (1997), S. 732-743 
    Details
    ISSN: 0947-6539
    Keywords: bridging ligands ; charge transfer ; cobalt ; quinones ; tripodal ligands ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of tripod cobalt(II) templates [{CH3C(CH2PAr2)3}CoII] with potentially bridging ligands L generates the dinuclear compounds [(tripod)-Co-L-Co(tripod)]2+. With L = oxalate (C2O2-4) a biscobalt(II) complex (1) is formed, while with L = C6H2O2-4, the dianion derived from 2,5-dihydroxy-1,4=benzoquinone (anilic acid), two-electron transfer within the dimetallic unit occurs and a biscobalt(III) charge distribution results (2a), as shown by X-ray structural analyses of 1 and 2a, NMR spectroscopy, and theoretical investigations by the INDO method. Complex 2a exhibits an unusually intense, low-energy absorption in its electronic spectrum; this is explained with a simple MO model. One-electron reduction of 2a generates the corresponding mixed-valence complex, which is highly stabilised through extensive electron delocalisation. Substituents at the 3,6 positions of the bridging ligand (Cl, Br, I, NO2, Me, iPr, Ph; 2b-h) as well as alkyl substitution at the aromatic rings of the tripod ligands (3, 4) influence the optical and electrochemical properties consistent with the proposed model of charge distribution. Formal replacement of one [(tripod)CoIII]3+ moiety by [CH2]2+ leads to the mononuclear complex 6, which is shown to be a typical [(tripod)CoIII=(catecholato)]+ complex. Therefore the substantially different optical and electrochemical properties of the dinuclear complexes with respect to those of 6 result from strong metal-metal interactions mediated by the bridging ligand.
    Additional Material: 15 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chem.19970030513
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  • 3
    Electronic Resource
    Electronic Resource
    Eisenkomplexe als Modellverbindungen zur homogenen Hydrierung von Kohlenmonoxid (1981)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 114 (1981), S. 2754-2768 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Iron Complexes as Model Compounds for the Homogeneous Hydrogenation of Carbon MonoxideThe μ-dinitrogen complex {Fe(CO)2[P(OCH3)3]2N2 (2) is prepared. Its reaction with H2, CH2O and C2H4 leads to dihydrido-, formaldehyde-, and ethylene-dicarbonylbis(trimethylphosphite)-iron complexes (4,5, and 6, respectively). The structures of 2 and of the dicarbonyltris(trimethylphosphite)iron complex 3 were determined by X-ray analyses.
    Notes: Der μ-Distickstoffkomplex {Fe(CO)2[P(OCH3)3]2N2 (2) wird dargestellt und mit H2, CH2O und C2H4 zu Dihydrido-, Formaldehyd- und Ethylen-dicarbonylbis(trimethylphosphit)eisen-Komplexen 4,5 bzw. 6 umgesetzt. Die Strukturen von 2 und dem Dicarbonyltris(trimethylphosphit)-eisen-Komplex 3 wurden röntgenographisch bestimmt.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19811140809
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  • 4
    Electronic Resource
    Electronic Resource
    Substituierte einkernige Carbonyleisendihydride (1981)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 114 (1981), S. 3549-3557 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Substituted Mononucleus Carbonyliron HydridesSubstitution of H2Fe(CO)4 by ligands like L = As(C6H5)3, Sb(C6H5)3 and P(OC6H5)3 in 1:1 ratio leads to fac monosubstituted compounds H2Fe(CO)3L. A 1:2 ratio results in the isolation of disubstituted complexes H2Fe(CO)2L2, L = P(OCH2)3CC2H5, P(OC6H5)3. The structure of H2Fe(CO)3As(C6H5)3 Was elucidated by X-ray analysis.
    Notes: Substitution von H2Fe(CO)4 mit Liganden L = As(C6H5)3, Sb(C6H5)3 und P(OC6H5)3 im Molverhältnis 1:1 Führt zu fac-Monosubstitutionsverbindungen H2Fe(CO)3L. Im Verhältnis 1:2 können trans-Disubstitutionskomplexe H2Fe(CO)2L2, L = P(OCH2)3CC2H5, P(OC6H5)3, erhalten werden. Von H2Fe(CO)3As(C6H5)3 wurde eine Röntgenstrukturanalyse ausgeführt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19811141108
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  • 5
    Electronic Resource
    Electronic Resource
    Darstellung und Struktur homo- und heterometallischer dreikerniger μ3-RP-verbrückter Cluster μ3-RPM2(CO)6M′Ln (M = Fe, Ru; M′Ln = η5-C5H5(CO)2Mn, Ru(CO)3H2) (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 989-1003 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Homo- and Heterometallic Trinuclear μ3-RP Bridged Clusters μ3-RPM2(CO)6M′Ln (M = Fe, Ru; M′Ln = η5-C5H5(CO)2Mn, Ru(CO)3H2)Synthesis of heterometallic clusters η5-C5H5(CO)2MnFe2(CO)6μ3-PR (2) with various organic groups is accomplished on two different routes: Either by reaction of η5-C5H5(CO)2MnP(R)Cl2 (1) with Fe2(CO)9 or from η5-C5H5(CO)2MnP(R)H2 (3) and Fe3(CO)12. Analogously manganese-ruthenium clusters 4 are available from 3 and Ru3(CO)12. The structure of these clusters is exemplified for two compounds η5-C5H5(CO)2MnM2(CO)6μ3-PC6H11 (M = Fe, 2d; Ru, 4a) by single crystal X-ray analyses. Homometallic μ3-RP bridged ruthenium clusters Ru3(CO)9(μ2-H)2μ3-PR (5) are obtained as byproducts of the synthesis of 4. The structure of 5a (R = c-C6H11), including the position of the μ2-hydrogen ligands, is determined by X-ray methods.
    Notes: Die Darstellung der heterometallischen Cluster η5-C5H5(CO)2MnFe2(CO)6μ3-PR (2) aus η5-C5H5(CO)2MnP(R)Cl2 (1) und Fe2(CO)9 sowie aus η5-C5H5(CO)2MnP(R)H2 (3) und Fe3(CO)12 wird für verschiedene organische Reste R beschrieben. Analoge Mangan-Ruthenium-Cluster 4 sind durch Umsetzung von 3 mit Ru3(CO)12 zugänglich. Der Bau dieser Cluster wird an zwei Beispielen η5-C5H5(CO)2MnM2(CO)6μ3-PC6H11 (M = Fe, 2d; Ru, 4a) durch Röntgenstrukturanalyse belegt. Homometallische μ3-RP-verbrückte Rutheniumcluster Ru3(CO)9(μ2-H)2μ3-PR (5) entstehen bei der Darstellung der heterometallischen Cluster 4 als Nebenprodukte. Für 5a (R = c-C6H11) wird die Atomanordnung einschließlich der Lage der μ2-Wasserstoff-Liganden röntgenstrukturanalytisch bestimmt.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19821150315
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  • 6
    Electronic Resource
    Electronic Resource
    Deprotonierung und Substitutionsreaktionen dreikerniger Eisencluster Fe3(CO)9(H)(SR) (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1286-1304 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Deprotonation and Substitution Reactions of Trinuclear Iron Clusters Fe3(CO)9(H)(SR)The trinuclear clusters Fe3(CO)9(H)(SR) (A), first described by Haines et al., are proton acids with pKs values between 3 and 4, thus giving stable salts containing [Fe3(CO)9(SR)]- anions (2-4). The influence of the hydrido bridge present in A on the geometry of the cluster framework is studied by comparison of X-ray results on A and on the anion [Fe3(CO)9(S—t-C4H9)]-. Up to three carbonyl groups of A are substituted by donor ligands E(C6H5)3 (E = P, As, Sb) under thermal or photochemical conditions (5-9). The geometry of the substitution products is inferred from spectroscopic data and from two X-ray analyses.
    Notes: Die von Haines et al. erstmals beschriebenen dreikernigen Eisencluster Fe3(CO)9(H)(SR) (A) erweisen sich als Säuren mit pKs-Werten zwischen 3 und 4, so daß stabile Salze mit [Fe3(CO)9(SR)]-- Anionen (2-4) dargestellt werden können. Ein Vergleich der röntgenographisch ermittelten Struktur von Neutralverbindungen A und des Anions [Fe3(CO)9(S—t-C4H9)]- zeigt den Einfluß der Wasserstoffbrücke auf die Geometrie des Clustergerüstes. Bis zu drei CO-Gruppen der Cluster A können thermisch oder photochemisch durch Donorliganden E(C6H5)3 (E = P, As, Sb) substituiert werden (5-9). Die Geometrie der Substitutionsprodukte wird aus spektroskopischen Daten und aus zwei Röntgenstrukturbestimmungen (5a, b) abgeleitet.
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    URL: http://dx.doi.org/10.1002/cber.19821150405
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  • 7
    Electronic Resource
    Electronic Resource
    Reaktionen von Arsiniden-Komplexen: Arsen als trigonal planar koordiniertes Brückenelement in dreikernigen Metallkomplexen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2035-2043 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Arsinidene Complexes: Arsenic Atoms as Trigonally Planar Coordinated Bridging Elements within Trinuclear Metal ComplexesThe synthesis of compounds in which all five valence electrons of a μ3-bridging arsenic atom are involved in bonding to three metal ligand fragments is achieved for the first time by the reaction of arsinidene complexes ClAs[MLn]2 (MLn = Cr(CO)5, Mn(CO)2(η5-CH3C5H4)) with η5-C5H5(CO)3Ml′- (M′ = Mo, W); chlorine substitution and MM′ bond formation with accompanying loss of one carbonyl group leads to the complexes 3, (3a, M′ = Mo, MLn = Mn(CO)2(η5-CH3C5H4); 3b, M′ = Mo, MLn = Cr(CO)5; 3c, M′ = W, MLn = Cr(CO)5). In compounds 3 there is no lone pair left at the μ3-arsenic atom which therefore shows trigonal planar coordination. The electron deficiency at the arsenic atom is compensated for by metal-arsenic η-bonding in a manner similar to the bonding situation in arsinidene complexes. X-ray analyses for 3a-c confirm this statement.
    Notes: Die erstmalige Synthese von Verbindungen, in denen alle fünf Valenzelektronen eines μ3-verbrückenden Arsenatoms in die Bindung zu drei Metall-Ligand-Fragmenten einbezogen sind, gelingt durch Umsetzung von Arsiniden-Komplexen ClAs[MLn]2 (MLn = Cr(CO)5, Mn(CO)2(η5-CH3C5H4)) mit η5-C5H5(CO)3M′- (M′ = Mo, W). In den unter Substitution der Chlorfunktion und Ausbildung einer M′M-Bindung unter CO-Abspaltung entstandenen Komplexen 3, (3a, M′ = Mo, MLn = Mn(CO)2(η5-CH3C5H4); 3b, M′ = Mo, MLn = Cr(CO)5; 3c, M′ = W, MLn = Cr(CO)5) besitzt das Arsen kein freies Elektronenpaar mehr. Es ist daher trigonal planar koordiniert; sein Elektronendefizit wird, wie in Arsiniden-Komplexen, durch π-Bindungsanteile in den Metall-Arsen-Bindungen ausgeglichen. Röntgenstrukturanalysen für 3a-c belegen dies.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19821150604
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  • 8
    Electronic Resource
    Electronic Resource
    Abfangreaktionen für Arsiniden- und Stibiniden-Komplexe: Addition von Lewisbasen an [(CO)5M]2XR (X=As, Sb; M=Cr, Mo, W) (1985)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 118 (1985), S. 3114-3126 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trapping of Arsinidene and Stibinidene Intermediates: Addition of Lewis Bases to [(CO)5M]2XR (X=As, Sb; M=Cr, Mo, W)The compounds [(CO)5M]2XR (X=As, Sb) which contain the sextett ligand stabilised by π-interaction with the 16 electron fragments (CO)5M (M=Cr, Mo, W) form stable adducts [(CO)5M]2X(R)B with lewis bases |B. The formation of adducts may be used to demonstrate the intermediate existence of non-isolable arsinidene and stibinidene complexes [(CO)5M]2XR. By this method it is shown that Na2M2 (CO)10 reacts with RXCl2 to give arsinidene and stibinidene complexes in any case. These compounds may be isolated as stable adducts by lewis bases such as PR3, P(OMe)3, thiourea, RNH2, and THF. Syntheses and properties of adducts of this type are discussed here. The structure is documented by X-ray analyses of 1i, 3b, and 5a.
    Notes: Komplexe [(CO)5M]2XR (X=As, Sb), in denen die Sextettliganden durch π-Wechselwirkung mit den 16-Elektronenfragmenten (CO)5M (M=Cr, Mo, W) stabilisiert sind, bilden mit Lewisbasen |B stabile Addukte [(CO)5M]2X(R)B. Die Adduktbildung kann zum Nachweis des intermediären Auftretens von nicht isolierbaren Arsiniden- und Stibiniden-Komplexen [(CO)5M]2XR eingesetzt werden. Auf diese Weise gelingt es zu zeigen, daß bei Reaktionen von Na2M2(CO)10 mit RXCl2 stets Arsiniden- bzw. Stibiniden-Komplexe gebildet werden, die sich als stabile Addukte mit Lewisbasen wie PR3, P(OMe)3, Thioharnstoff, RNH2 und THF isolieren lassen. Synthese und Eigenschaften solcher Addukte werden besprochen. Ihr Bau wird durch Kristallstrukturen von 1i, 3b und 5a belegt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19851180810
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  • 9
    Electronic Resource
    Electronic Resource
    μ-Allenyliden-dimangan- und -dirhenium-Komplexe (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 3423-3431 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: μ-Allenylidene-dimanganese and -dirhenium ComplexesThe syntheses of a nonacarbonyl-μ-(di-tert-butylallenylidene)-dimanganese compound (1a) and of an isomeric rhenium complex 1b containing a terminal allenylidene residue are described. A (3-tert-butyl-3-hydroxy-4,4-dimethyl-1-pentynyl)pentacarbonylmanganese (2a) and the corresponding rhenium complex (2b) are the main products in these reactions. 2a and 2b can also be obtained in an independent way. The structure of 1a has been determined by an X-ray analysis.
    Notes: Die Synthesen einer Nonacarbonyl-μ-(di-tert-butylallenyliden)-dimangen-Verbindung (1a) und eines isomeren Rheniumkomplexes 1b mit terminal gebundenem Allenyliden-Rest werden beschrieben. Die Hauptprodukte bei diesen Umsetzungen zu 1a bzw. 1b stellen die (3-tert-Butyl-3-hydroxy-4,4-dimethyl-1-pentinyl)pentacarbonylmangan- bzw. -rhenium-Verbindungen 2a bzw. 2b dar, die auch auf einem unabhängigen Wege erhalten werden können. 1a wurde durch eine Röntgenstrukturanalyse charakterisiert.
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    URL: http://dx.doi.org/10.1002/cber.19841171211
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  • 10
    Electronic Resource
    Electronic Resource
    Di-tert-butylallenyliden-Komplexe des Eisens (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 3432-3442 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Di-tert-butylallenylidene Complexes of IronThe synthesis of a tetracarbonyl(di-tert-butylallenylidene)iron(0) complex (1) is reported. It can be transformed to an octacarbonyl-μ-(di-tert-butylallenylidene)-diiron(0) compound 2 and reacts thermally to an allenylidenetriiron derivative Fe3(CO)10C3(tBu)2 3. The synthesis of 1 via a trimethylamine oxide-induced substitution of CO with di-tert-butylpropargylate residues is accompanied by the formation of (CO)4Fe=C=C= complex 4, which has been characterized by an X-ray analysis.
    Notes: Die Synthese eines Tetracarbonyl(di-tert-butylallenyliden)eisen(0)-Komplexes (1) wird beschrieben. Dieser läßt sich in eine Octacarbonyl-μ-(di-tert-butylallenyliden)-dieisen (0)-Verbindung 2, überführen und reagiert thermisch zu einem Allenylidentrieisen-Derivat Fe3(CO)10C3(tBu)2 3. Bei der Darstellung von 1 über eine Trimethylaminoxid-induzierte Substitution von CO durch Di-tert-butylpropargylat-Reste wird die Bildung eines (CO)4Fe=C=C=-Komplexes 4 beobachtet, dessen Aufbau durch eine Röntgenstrukturanalyse bestimmt wurde.
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    URL: http://dx.doi.org/10.1002/cber.19841171212
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