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  • 1
    Electronic Resource
    Electronic Resource
    A long silicon-hydrogen bond or a short silicon-hydrogen nonbond? Neutron-diffraction study of (η5CH3C5H4)(CO)2(H)MnSiF(C6H5)2 (1982)
    s.l. : American Chemical Society
    Journal of the American Chemical Society 104 (1982), S. 7378-7380 
    Details
    ISSN: 1520-5126
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1021/ja00389a107
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  • 2
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    Transition-metal ketenes. 21. Conversion of .eta.2-ketenyl complexes into novel cations with a tungstaphosphabicyclo[1.1.0]butanone unit. Synthesis and structure (1984)
    s.l. : American Chemical Society
    Organometallics 3 (1984), S. 777-782 
    Details
    ISSN: 1520-6041
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1021/om00083a023
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  • 3
    Electronic Resource
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    Kinetic and mechanistic investigations of transition metal complex reactions. 19. Spontaneous rearrangement of amino(chloro)carbene into chloro aminocarbyne complexes. Synthesis of aminocarbene and aminocarbyne complexes and kinetics and mechanism of the rearrangement reaction (1985)
    s.l. : American Chemical Society
    Organometallics 4 (1985), S. 726-735 
    Details
    ISSN: 1520-6041
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1021/om00123a020
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  • 4
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    Übergangsmetall-Carbin-Komplexe, LXVIII. Synthese und Struktur neuartiger zweikerniger Biscarbin-Komplexe des Chroms, Molybdäns und Wolframs mit verbrückenden Phenylthio-, Arylseleno-, Halogeno- und Pseudohalogeno-Liganden (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3152-3166 
    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 Carbyne Complexes, LXVIII. Synthesis and Structure of Novel Binuclear Biscarbyne Complexes of Chromium, Molybdenum, and Tungsten with Bridging Phenylthio-, Arylseleno-, Halogeno-, and Pseudohalogeno LigandsPentacarbonyl[(diethylamino)(ethoxy)carbene]molybdenum (1) reacts with boron trifluoride to give a very unstable product which is supposed to be pentacarbonyl[(diethylamino)carbyne]-molybdenum tetrafluoroborate (2). Low temperature reaction of 2 with bromide, iodide, and thiocyanate yields the neutral trans-substituted carbyne complexes trans-X(CO)4MoCNEt2 (4a-c) [X = Br (a), I (b), SCN (c)] cyanate and 4-(trifluoromethyl)phenylselenolate afford the compounds (μ-X)2[(CO)3MoCNEt2]2 (5d, f) [X = OCN (d), 4-CF3C6H4Se (f)] which are members of a new class of binuclear biscarbyne complexes. Analogues 5a-c, g-l are prepared from the carbyne complexes trans-X(CO)4MCNR2 (4a-c, g-l) on warming in solution. The corresponding complex 5e (X = N3, M = W, R = C2H5) is obtained by the reaction of pentacarbonyl[(diethylamino)carbyne]tungsten tetrafluoroborate (6) with azide. The structures of 5b, d, e, g are ensured by X-ray analyses.
    Notes: Pentacarbonyl[(diethylamino)(ethoxy)carben]molybdän (1) reagiert mit Bortrifluorid zu einem sehr instabilen Produkt, bei dem es sich vermutlich um Pentacarbonyl[(diethylamino)carbin]-molybdän-tetrafluroborat (2) handelt. Wird 2 bei tiefer Temperatur mit Bromid, Iodid und Thiocyanat umgesetzt, erhält man die neutralen trans-substituierten Carbinkomplexe trans-X(CO)4MoCNEt2 (4a-c) [X = Br (a), I (b), SCN (c)] demgegenüber ergeben Cyanat und 4-(Trifluormethyl)phenylselenolat die Verbindungen (μ-X)2[(CO)3MoCNEt2]2 (5d, f) [X = OCN (d), 4-CF3C6H4Se (f)] als Vertreter einer neuen Klasse von zweikernigen Biscarbin-Komplexen. Die dazu analogen Verbindungen 5a-c, g--l werden dargestellt, indem man die Carbinkomplexe trans-X(CO)4MCNR2 (4a-c, g-l) in Lösung aufwärmt. Der entsprechende Komplex 5e (X = N3, M = W, R = C2H5) wird bei der Umsetzung von Pentacarbonyl[(diethylamino)carbin]-wolfram-tetrafluoroborat (6) mit Azid erhalten. Der Aufbau von 5b, d, e, g ist durch Röntgenstrukturanalysen gesichert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150920
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  • 5
    Electronic Resource
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    Reaktionen von Komplexliganden, XXIII. Bis(phosphino)inden-Derivate durch C—C-Verknüpfung von Arylcarben-Liganden und Bis(diphenylphosphino)acetylen (1983)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 116 (1983), S. 2337-2343 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Complex Ligands, XXIII. Bis(phosphino)indene Derivatives from Carbon Carbon Bond Formation between Arylcarbene Ligands and Bis(diphenylphosphino)acetylenePentacarbonyl(methoxyphenylcarbene) complexes of chromium and tungsten (1a, 2a) react with bis(diphenylphosphino)acetylene (3) via CO substitution to give binuclear alkyne bridged bis(carbene) complexes (CO)4[CH3O(C6H5) C]M-[(C6H5)2P-C ≡ C-P(C6H5)2]-M(CO)4[C(OCH3)C6H5](4a, 5a). The chromium compound 4a is cleaved on warming to yield the tetracarbonyl-[1,2-bis(phosphino)indene]chromium complex 6a and la. In a one-pot reaction the bis(phosphino)indene derivatives 6a-c are formed directly from arylcarbene chromium complexes (CO)5Cr[C(p-RC6H4)OCH3] (R=;H, CH3, CF3) (1a-c) and 3. The structure of 6c is established by X-ray analysis.
    Notes: Pentacarbonyl(methoxyphenylcarben)-Komplexe des Chroms und Wolframs (1a, 2a) reagieren mit Bis(diphenylphosphino)acetylen (3) unter CO-Substitution zu den zweikernigen alkin-verbrückten Bis(carben)-Komplexen (CO)4[CH3O(C6H5) C]M-[(C6H5)2P-C ≡ C-P(C6H5)2]-M(CO)4[C(OCH3)C65](4a, 5a). Die Chrom-Verbindung 4a wird beim Erwärmen in den Tetracarbonyl [1,2-bis(phosphino)inden]chrom-Komplex 6a und 1a gespalten. Aus den Arylcarben-Chrom-Komplexen (CO)5Cr[Cp-RC6H4)OCH3] (R=;H, CH3, CF3) (1a-c) und 3 entstehen direkt die 1,2-Bis(phosphino)inden-Derivate 6a-c. Der Molekülbau von 6c wird durch eine Röntgenstrukturanalyse belegt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19831160622
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  • 6
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Carben-Komplexe, CXVIII1) Kinetische und mechanistische Untersuchungen von Übergangsmetall-Komplex-Reaktionen, VIII2) C, Cr-Wanderung von SeR in (CO)5Cr[C(SeR)NEt2]: Kinetische, mechanistische und präparative Untersuchungen (1981)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 114 (1981), S. 3220-3232 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Carbene Complexes, CXVIII1) Kinetic and Mechanistic Investigations of Transition Metal Complex Reactions, VIII2) C, Cr-Migration of SeR in (CO)5Cr[C(SeR)NEt2]: Kinetic, Mechanistic and Preparative InvestigationsOn heating in solution, [(arylseleno)(diethylamino)carbene]pentacarbonylchromium complexes, (CO)5Cr[C(SeR)NEt2], (2) [R = 4-C6H4CF3 (a), 4-C6H4Br (b), 4-C6H4F (c), C6H5 (d), 4-C6H4CH3 (e), 4-C6H4OCH3 (f), 1-C10H7 (g)] rearrange with CO-elimination and C, Cr-migration of SeR to form the corresponding trans-(arylseleno)tetracarbonyl(diethylaminocarbyne) chromium complexes, trans-RSe(CO)4CrCNEt2, (3a-g). The rearrangement follows a first-order rate law. Free carbon monoxide does not influence the reaction rate whereas the Polarity of the solvent and the type of the substituent R only influence the rate of the reaction to a very small extent. The activation enthalpies are ΔH≠ = 101-104 kj mol-1, the activation entropies ΔS = 27-33 j mol-1 K-1. Addition of PPh3 to solutions of 2d does not influence the rate of the rearrangement but leads to a different reaction product, mer-(CO)3(PPh)3(SePh)CrCNEt2 (4d). Complex (4d). is also formed by photolysis of 2d in the presence of PPh3, The compounds 3a - d and 4d are characterized by analytical and spectroscopic means, 3c, additionally by an X-ray analysis.
    Notes: Beim Erwärmen in Lösung lagern sich die [(Arylseleno)(diethylamino)carben]pentacarbonyl-chrom-Komplexe, (CO)5Cr[C(SeR)NEt2], (2) [R = 4-C6H4CF3 (a), 4-C6H4Br (b), 4-C6H4 (c_, C6H4 (d), 4-C6H4OCH3 (e) 4-C6H4OCH3 (f), 1-C10H7 (g)] unter CO-Abspaltung und C, Cr-Wanderung von SeR zu den entsprechenden trans-(Arylseleno)tetracarbonyl(diethylaminocarbin)-chrom-Komplexen, trans-RSe(CO)4CrCNEt2, (3a-g) nach einem Geschwindigkeitsgesetz erster Ordnung um. Freies Kohlenmonoxid ist ohne, die Polarität des Solvens sowie die Art des Substituenten R sind nur von geringem Einfluß auf die Reaktionsgeschwindigkeit. Die Aktivierungsenthalpien betragen ΔH≠ = 101 104 kj mol-1, die Aktivierungsentropien ΔS≠ = 27-33 j mol-1 K-1. Zusatz von PPh3 zu Lösungen von 2d beeinflußt zwar die Umlagerungsgeschwindigkeit nicht, man erhält jedoch mer-(CO)3(PPh)3(SePh)CrCNEt2 (4d) als Reaktionsprodukt. Photolyse von 2d in THF in Anwesenheit von PPh3 liefert ebenfalls 4d. Die Verbindungen 3a-d und 4d wurden analytisch und spektroskopisch gesichert, 3c zusätzlich durch eine Röntgenstrukturanalyse.
    Additional Material: 8 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19811141004
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  • 7
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    Electronic Resource
    Untersuchungen zur Reaktivität von Metall-π-Komplexen, XXXVI. Zweikernige Sandwichkomplexe mit Metall-Metall-Bindung: Synthese und Struktur von (μ-C5H5)2Pd2(PR3)2 (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2905-2913 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on the Reactivity of Metal π-Complexes, XXXVI. Dinuclear Sandwich Complexes Containing a Metal-Metal Bond: Synthesis and Structure of (μ-C5H5)2Pd2(PR3)2The complexes (C5H5)2Pd2(PR3)2 (1-6) are prepared by reduction of C5H5Pd(PR3)OCOCH3 with NaK2.8 or in a one-pot synthesis by reaction of [(PR3)PdCl]2(μ-OCOCH3)2 with 4 equivalents TlC5H5. The triphenyl phosphite complex (C5H5)2Pd2[P(OPh)3]2 (7) is obtained from [P(OPh)3PdCl2]2 and TlC5H5. The X-ray structure analysis of (C5H5)2Pd2(PEt3)2 (5) shows that the two planar cyclopentadienyl ligands are coordinated sandwich-like to the Pd2(PR3)2 unit; according to the bond angle P—Pd—Pd = 175.45° the P—Pd—Pd—P arrangement is nearly linear. The different C—C distances in the five-membered rings point to the presence of an „allyl-ene“ system and thus to a trihapto- (h3) coordination of the C5H5 ligands.
    Notes: Die Komplexe (C5H5)2Pd2(PR3)2 (1-6) sind durch Reduktion von C5H5Pd(PR3)OCOCH3 mit NaK2.8 oder in einer Eintopfsynthese durch Umsetzung von [(PR3)PdCl]2(μ-OCOCH3)2 mit 4 äquivalenten TlC5H5 erhältlich. Der Triphenylphosphit-Komplex (C5H5)2Pd2[P(OPh)3]2 (7) entsteht aus [P(OPh)3Pdl2]2 und TlC5H5. Die Röntgenstrukturanalyse von (C5H5)2Pd2(PEt3)2 (5) zeigt, daß die beiden planaren Cyclopentadienylliganden sandwich-artig an die Pd2(PR3)2-Einheit koordiniert sind; die Anordnung P—Pd—Pd—P ist mit einem Bindungswinkel P—Pd—Pd von 175.45° nahezu linear. Die unterschiedlichen C—C-Abstände in den Fünfringen weisen auf das Vorliegen eines „allyl-ene“-Systems und damit auf eine trihapto- (h3)-Koordination der C5H5-Liganden hin.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19821150821
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  • 8
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    Übergangsmetall-substituierte Phosphane, Arsane und Stibane, XXVI. Synthese und Kristallstruktur von Dicarbonyl(cyclopentadienyl)-bis(trimethylphosphan)molybdän-tricarbonyl(cyclopentadienyl)-molybdat (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2003-2008 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition Metal Substituted Phosphanes, Arsanes, and Stibanes, XXVI. Synthesis and Crystal Structure of Dicarbonyl(cyclopentadienyl)bis(trimethylphosphane)-molybdenum-tricarbonyl(cyclopentadienyl)molybdate{[Cp(CO)2(Me3P)M]2AsMe2}M(CO)3Cp (M = Cr, Mo, W) (1a-c) reacts in acetonitrile with Me3P to give [Cp(CO)2(Me3P)2M] M(CO)3Cp (2a-c) and Cp(CO)2(Me3P)M—AsMe2 (3a-c). 2b, c are in addition obtained by treatment of [Cp(CO)3)3M]2 (M = Mo, W) with Me3P in benzene. The structure of 2a-c is established by NMR and IR spectroscopy and in the case of 2b by X-ray analysis.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19821150531
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  • 9
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    Übergangsmetall-Carben-Komplexe, CXXIV. Ein- und zweikernige Biscarbenkomplexe von Chrom, Molybdän und Wolfram und ihre Umsetzung mit Bortrihalogeniden (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2951-2964 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Carbene Complexes, CXXIV. Mono- and Binuclear Biscarbene Complexes of Chromium, Molybdenum, and Tungsten and their Reaction with Boron TrihalidesThe reaction of p-phenylenedilithium with hexacarbonylchromium and -tungsten and subsequent alkylation by triethyloxonium tetrafluoroborate yields μ-[p-phenylenebis[(ethoxy)carbene]]-bis-(pentacarbonylmetal) complexes (CO)5MC(OEt)-p-C6H4-(OEt)CM(CO)5 (M = Cr (3a), W (3b)) as well as the mononuclear carbene complexes 4a and 4b. The analogous reaction of o-phenylenedilithium with metalhexacarbonyls of the VI. subgroup affords the expected mononuclear 1,4-chelated biscarbene complexes (M = Cr (5a), Mo (5b), W (5c)), while 1,2-dilithio-1,2-diphenylethane gives a mixture of mononuclear (M = Cr (6a), W (6b)) and binuclear (CO)5MC(OEt)CH(Ph)CH(Ph)-(OEt)CM(CO)5 (M = Cr (7a), W (7b)) biscarbene complexes. The aminolysis of 5a - c with dimethylamine leads to cis-tetracarbonyl[o-phenylenebis[(dimethylamino)carbene]] compounds of chromium, molybdenum, and tungsten (8a - c). 3a, b and 4a, b react with boron trihalides BX3 to form the corresponding trans-halogenocarbyne complexes 9a, b and 10a - c. Properties, spectra, and the results of an X-ray structure analysis of 9b are reported.
    Notes: Die Umsetzung von p-Phenylendilithium mit Hexacarbonylchrom und -wolfram und anschließende Alkylierung mit Triethyloxonium-tetrafluoroborat ergibt μ-[p-Phenylenbis[(ethoxy)carben]]-bis(pentacarbonylmetall)-Komplexe (CO)5MC(OEt)-p-C6H4-(OEt)CM(CO)5 (M = Cr (3a), W (3b)), sowie die einkernigen Carbenkomplexe 4a und 4b. Die analoge Reaktion von o-Phenylendilithium mit Metallhexacarbonylen der VI. Nebengruppe ergibt die erwarteten einkernigen, 1,4-chelatisierten Biscarbenkomplexe (M = Cr (5a), Mo (5b), W (5c)), während 1,2-Dilithio-1,2-diphenylethan ein Gemisch von einkernigen (M = Cr (6a), W (6b)) und zweikernigen (CO)5MC(OEt)CH(Ph)CH(Ph)(OEt)CM(CO)5 (M = Cr (7a), W (7b)) Biscarben-Komplexen liefert. Die Aminolyse von 5a-c mit Dimethylamin führt zu cis-Tetracarbonyl[o-phenylenbis[(dimethylamino)carben]]-Verbindungen von Chrom, Molybdän und Wolfram (8a-c-). 3a, b und 4a, b reagieren mit Bortrihalogeniden BX3 unter Bildung der entsprechenden trans-Halogenocarbin-Komplexe 9a, b und 10a-c. Eigenschaften, Spektren und die Ergebnisse einer Röntgenstrukturuntersuchung an 9b werden beschrieben.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19821150903
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  • 10
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    Übergangsmetall-Carbin-Komplexe, LXVII. Kationische Carbin-Komplexe des Wolframs  -  Synthese, Struktur und Reaktionsverhalten gegenüber Nucleophilen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3141-3151 
    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 Carbyne Complexes, LXVII. Cationic Carbyne Complexes of Tungsten - Synthesis, Structure, and Reaction with NucleophilesPentacarbonyl[(diethylamino)(ethoxy)carbene]tungsten (1) reacts with boron trifluoride to give the unstable cationic carbyne complex pentacarbonyl[(diethylamino)carbyne]tungsten tetrafluoroborate (2a). Replacing the BF4- anion by SbX6- yields the more stable compounds [(CO)5WCNEt2]SbX6 [2c (X = F) and 2d (X = Cl)]. The X-ray structure determination of 2d shows that there are at most charge transfer-like anion-cation interactions in the crystal. Complex 2a shows two different types of reaction with nucleophiles X-: rearrangement with CO-elimination gives trans-BF4(CO)4WCNEt2 (3a) even at low temperatures. The neutral carbyne complexes trans-X(CO)4WCNEt2 [4a-e; X = CN (a), NCO (b), NCS (c), NCSe (d), SC6H5 (e)] are then formed by nucleophilic substitution of BF4- by X- on 3a. In case of X- = As(C6H5)2- only nucleophilic addition to the carbyne carbon atom of 2a is observed to afford pentacarbonyl[(diethylamino)(diphenylarsino)carbene]tungsten (5). Complex 2d reacts with X- (X = SC6H5, OC6H5) at low temperature - or without X- on warming - to give trans-Cl(CO)4WCNEt2 (4f).
    Notes: Pentacarbonyl[(diethylamino)(ethoxy)carben]wolfram (1) reagiert mit Bortrifluorid zum instabilen kationischen Carbinkomplex Pentacarbonyl[(diethylamino)carbin]wolfram-tetrafluoroborat (2a). Ersetzt man das BF4--Anion durch SbX6-, erhält man die stabileren Verbindungen [(CO)5WCNEt2]SbX6[2c (X = F) und 2d (X = Cl)]. Eine von 2d durchgeführte Röntgenstrukturanalyse zeigt, daß im Kristall höchstens Charge-Transfer-artige Kation-Anion-Wechselwirkungen vorliegen. Gegenüber Nucleophilen X- zeigt Komplex 2a zwei verschiedene Reaktionsmöglichkeiten: die bereits bei tiefen Temperaturen unter CO-Abspaltung erfolgende teilweise Umlagerung von 2a zu trans-BF4(CO)4WCNEt2 (3a) führt nach nucleophiler Substitution von BF4- durch X- in 3a zu den neutralen Carbinkomplexen trans-X(CO)4WCNEt2 [4a-e; X = CN (a), NCO (b), NCS (c), NCSe (d), SC6H5 (e)]. Im Fall von X- = As(C6H5)2- beobachtet man ausschließlich Addition des Nucleophils an das Carbin-Kohlenstoffatom von 2a und Bildung von Pentacarbonyl[(diethylamino)(diphenylarsino)carben]wolfram (5). Komplex 2d ergibt durch Umsetzung mit X- (X = SC6H5, OC6H5) bei tiefen Temperaturen - beim Erwärmen auch in Abwesenheit von X- - stets trans-Cl(CO)4WCNEt2 (4f).
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19821150919
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