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  • 1985-1989  (8)
  • Inorganic Chemistry  (8)
  • 1
    Electronic Resource
    Electronic Resource
    Olefin- und Cyclopropan-Aktivierung durch geminale Phosphonium-Zentren (1985)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 118 (1985), S. 3105-3113 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Olefin and Cyclopropane Activation Through Geminal Phosphonium CentresComplete quaternization of vinylidenebis(diphenylphosphane) (1) with CH3I or CH3OSO2F yields the diquaternary salts 2a,b, whose olefinic double bond is strongly electrophilic through the activation by two geminal phosphonium centres. Accordingly, addition of methanol or ethanol to 2a,b leads to β-alkoxy-substituted double phosphonium salts 9a-i. The structure of one of these products (9a: X=I, R=CH3) was elucidated by single crystal X-ray diffraction analysis. Spectroscopic data are provided for the remaining compounds. - Treatment of triphenylphosphonium cyclopropylide (5) with chlorodiphenylphosphane gives the gem-phosphinosubstituted salt 6, which can be quaternized with CH3OSO2F to yield a bis-phosphonium salt (7a,b). A symmetrical homologue 7c is formed from cyclopropylidenebis(diphenylphosphane) (8) and CH3OSO2F. In 7a-i the cyclopropane cycle is also clearly activated. Ring cleavage occurs with alcohols leading to γ-alkoxylated salts 10a,b.
    Notes: Die erschöpfende Quartärisierung von Vinylidenbis(diphenylphosphan) (1) mit CH3I oder CH3OSO2F liefert Diquartärsalze 2a,b, deren olefinische Doppelbindung durch die beiden Phosphonium-Zentren stark elektrophil aktiviert ist. Die Addition von Methanol oder Ethanol an 2a,b liefert entsprechend die β-alkoxysubstituierten Doppelphosphonium-Salze 9a-i. Die Struktur eines dieser Produkte (9a: X=I, R=CH3) wurde durch eine Einkristall-Röntgenbeugungsanalyse gesichert, für die übrigen liegen spektroskopische Daten vor. - Triphenylphosphoniumcyclopropylid (5) ergibt mit (C6H5)2PCl das geminal phosphinosubstituierte Salz 6, das durch CH3OSO2F zum Bisphosphonium-Salz quartärisiert werden kann (7a,b). Ein symmetrisches Homologes 7 c entsteht aus Cyclopropylidenbis(diphenylphosphan) (8) und CH3OSO2F. In 7a-i ist der Cyclopropan-Cyclus ebenfalls deutlich elektrophil aktiviert. Mit Alkoholen tritt Ringspaltung ein, die hier zu γ-alkoxylierten Salzen 10a,b führt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19851180809
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  • 2
    Electronic Resource
    Electronic Resource
    Synthese und Struktur des Zink(l-aspartat)chlorids, Zn(L-AspH)Cl (1987)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 120 (1987), S. 867-869 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of ZnO or ZnCO3 with L-aspartic acid yields zinc di(L-aspartate), wherein aspartic acid (L-AspH2) functions as a monobasic acid: Zn(L-AspH)2. This precursor reacts with one equivalent of ZnCl2 in aqueous solution at pH=4.25 to give the title compound Zn(L-AspH)Cl, which contains no water of crystallisation (solubility: 12.8% [w/w] at 22°C). The X-ray structure analysis shows the zinc atoms to be tetrahedrally surrounded by a chloride ion and three oxygen atoms of carboxylate groups originating from three different L-AspH anions. This constitution is fundamentally different from that of the magnesium analogue, but also of the corresponding halide-free aspartates and glutamates of zinc and cadmium. The results may be of some significance for pharmacological cooperativity phenomena (chloride/aspartate) in metal complexation.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19871200531
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  • 3
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Carben-Komplexe, CXXXVI. Reaktionen kationischer Carbin-Komplexe des Mangans mit Carbonylmetallaten (1985)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 118 (1985), S. 3311-3319 
    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 Carbene Complexes, CXXXVI. Reactions of Cationic Carbyne Complexes of Manganese with Carbonyl MetalatesThe first carbene complexes (5, 6), with a transition metal α-bonded to the carbene carbon atom, are obtained by reaction of dicarbonyl(phenyl, ferrocenylcarbyne)(methylcyclopentadienyl)manganese tetrachloroborate (1, 2) with Na[Co(CO)4]. Analogous reaction with K[Mn(CO)5] leads to the isomeric ketenyl complexes (3, 4) via rearrangement of the carbene to the ketenyl complex. Properties and spectra are reported. An X-ray structure analysis of MeCp(CO)2Mn[μ-C(CpFeCp)CO]Mn(CO)4(Mn - Mn) (4) confirms the presence of a bridging ketenyl ligand.
    Notes: Durch Umsetzung von Dicarbonyl(phenyl, ferrocenylcarbin)(methylcyclopentadienyl)mangan-tetrachloroborat (1, 2) mit Na[Co(CO)4] erhält man erstmals Carben-Komplexe mit einem Übergangsmetall in α-Stellung zum Carben-Kohlenstoffatom (5, 6). Die analoge Reaktion mit K[Mn(CO)5] führt zu isomeren Ketenyl-Komplexen (3, 4), die durch Umlagerung von Carben- zu Ketenyl-Komplex entstehen. Eigenschaften und Spektren werden beschrieben. Die Röntgenstrukturanalyse von MeCp(CO)2Mn[μ-C(CpFeCp)CO]Mn(CO)4-(Mn - Mn) beweist das Vorliegen eines verbrückenden Ketenyl-Liganden.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19851180830
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  • 4
    Electronic Resource
    Electronic Resource
    Übergangsmetall-koordinierte Heteroolefine als Synthesebausteine: Thio- und Selenoacrylamide aus 1-(Diethylamino)-1-propin und Heteroaldehyd- und -keton-Komplexen (1988)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 121 (1988), S. 2095-2102 
    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-Coordinated Heteroolefins as Synthetic Building Blocks: Thio- and Selenoacrylamides from 1-(Diethylamino)-1-propyne and Heteroaldehyde- and -ketone ComplexesPentacarbonyl(thioaldehyde), -(selenoaldehyde), and -(selenoketone) complexes, (CO)5M[X=C(Ph)R] (1), react with 1-(diethylamino)-1-propyne, Et2N—C≡C—Me (2), by regiospecific addition of the alkyne to the X=C bond and electrocyclic ring opening to give pentacarbonyl(thioacrylamide) and -(selenoacrylamide) complexes, (CO)5M[X=C(NEt2)C(Me)=C(Ph)R] (3) [M = Cr: R = H, X = S (a), Se (e); R = Ph, X = Se (d). - M = W:X = Se, R = H (b), Ph (c)]. If R = H, the reaction is stereospecific. According to the NMR spectra and to an X-ray structure analysis of 3b, the E isomer (with respect to the C=C double bond) is formed. By applying CO pressure (105 bar) at elevated temperatures, the thio- and selenoacrylamide ligands can be cleaved off the metal unchanged. The compound Se=C(NEt2)C(Me)=CPh2 (4c) was investigated by X-ray analysis.
    Notes: Pentacarbonyl(thioaldehyd)-, -(selenoaldehyd)- und -(selenoketon)-Komplexe, (CO)5M[X=C(Ph)R] (1) (M = Cr, W; X = S, Se; R = H, Ph), reagieren mit 1-(Diethylamino)-1-propin, Et2N—C≡C—Me (2) unter regiospezifischer Addition des Alkins an die X=C-Bindung und elektrocyclischer Ringöffnung zu Pentacarbonyl(thioacrylamid)- bzw. -(selenoacrylamid)-Komplexen, (CO)5M[X=C(NEt2)C(Me)=C(Ph)R] (3) [M = Cr: R = H, X = S (a), se (e); R = Ph, X = Se (d). - M = W:X = Se, R= H (b), Ph (c)]. Die Reaktion ist für R = H stereospezifisch. Aufgrund der NMR-Spektren und einer an 3b durchgeführten Röntgenstrukturanalyse wird das E-Isomere (bezüglich der C=C-Bindung) gebildet. Mit CO (105 bar) lassen sich die Thio- und Selenoacrylamid-Liganden bei erhöhten Temperaturen intakt vom Metall ablösen. Die Verbindung Se=C(NEt2)C(Me)=CPh2 (4c) wurde durch eine Röntgenstrukturanalyse gesichert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19881211204
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  • 5
    Electronic Resource
    Electronic Resource
    CH2=PPh und CH2=AsPh als Liganden an Rhodium Kristall- und Molekülstruktur von C5Me5Rh(η2-CH2PPh)(CO) und C5Me5(CO)Rh(AsPh)3 (1989)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 1061-1066 
    Details
    ISSN: 0009-2940
    Keywords: Phospha- and arsaalkene rhodium complexes ; Metalla heterocycle containing RhAs3 ; Rhodium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: CH2=PPH and CH2=AsPh as Ligands Coordinated to Rhodium. Crystal and Molecular Structure of C5Me5Rh(η2-CH2PPh)(CO) and C5Me5(CO)Rh(AsPh)3C5Me5RhCH2I(CO)I (1) reacts with excess LiPHPh or LiAsHPh to give the complexes C5Me5Rh(η2-CH2EPh)(CO) (2: E = P; 3: E = As). The C—P bond length of the coordinated phosphaalkene in 2 is 174.0(4) pm and thus ca. 10 pm shorter than that of a C—P single bond. On standing in solution, the new heterocycle C5Me5(CO)Rh(AsPh)3 (4) is formed from 3. The X-ray analysis of 4 shows that the bonding distances and angles in the central nonplanar RhAs3 four-membered ring are very similar to thos in cyclo-(AsCF3)4.
    Notes: C5Me5RhCH2I(CO)I (1) reagiert mit überschüssigem LiPHPh oder LiAsHPh zu den Komplexen C5Me5Rh(η2-CH2EPh)(CO) (2: E = P; 3: E = As). Der C—P-Abstand des koordinierten Phosphaalkens in 2 ist mit 174.0(4) pm um ca. 10 pm kürzer als der einer C—P-Einfachbindung. Beim Stehenlassen in Lösung entsteht aus 3 teilweise der Heterocyclus C5Me5(CO)Rh(AsPh)3 (4), von dem die Struktur bestimmt wurde. Die Bindungsabstände und -winkel in dem zentralen, nicht planaren RhAs3-Vierring sind denen in cyclo-(AsCF3)4 sehr ähnlich.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19891220608
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  • 6
    Electronic Resource
    Electronic Resource
    Mehrfachbindungen zwischen Hauptgruppenelementen und Übergangsmetallen, XXVII. Redox-Reaktionen an Chrom  -  Selen-Dreifachbindungen (1986)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 119 (1986), S. 3544-3557 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Multiple Bonds Between Main Group Elements and Transition Metals, XXVII. Redox Reactions of Chromium-Selenium Triple BondsThe title complex μ-selenido-bis[dicarbonyl(η5-cyclopentadienyl)chromium] (1) reacts with reducing agents such as potassium superoxide and cobaltocene to yield novel mono- and multinuclear ionic complexes. Thus, compound 5 results from treatment of 1 with KO2 in the presence of [2.2.2]-cryptand in a solution of acetone; 5 contains the mononuclear complex anion [(η5-C5H5)Cr(CO)2(η2-Se2)]- (X-ray structure). In the reaction with cobaltocene, conducted in tetrahydrofuran/diethyl ether solution at -30°C, 1 is converted into the extremely oxygen-sensitive ionic compound 2 which, for the first time, reveals an organometallic species containing a planar Cr3Se-multiple bond system (X-Ray structure); 2 decomposes at room temperature to give both the tetrameric selenium complex 3 of composition [(C5H5)CrSe]4 (Cr4Se4 cubane-type structure) and the ionic compound [Co-(η5-C5H5)2]+ [(η5-C5H5)Cr(CO)3]- (4; X-Ray structure).
    Notes: Der Titelkomplex μ-Selenido-bis[dicarbonyl(η5-cyclopentadienyl)chrom] (1) reagiert mit Reduktionsmitteln wie Kaliumsuperoxid oder Cobaltocen zu neuartigen ein- und mehrkernigen Komplexsalzen. So ergibt KO2 in Gegenwart von [2.2.2]-Kryptand in Aceton-Lösung bei Raumtemperatur das Komplexsalz 5, welches das einkernige Komplexanion [(η5-C5H5)Cr(CO)2(η2-Se2)]- enthält (Röntgenstrukturanalyse). Mit Cobaltocen ergibt 1 bei -30°C in Tetrahydrofuran/Diethylether-Lösung das extrem sauerstoffempfindliche Komplexsalz 2, in dem erstmals eine Organometall-Spezies mit planarem Cr3Se-Mehrfachbindungssystem vorliegt (Röntgenstrukturanalyse). 2 zerfällt bei Raumtemperatur unter Bildung des tetrameren Selen-Komplexes 3 der Zusammensetzung [(C5H5)CrSe]4 (Cr4Se4-Cubanstruktur) und in den salzartigen Komplex [Co(η5-C5H5)2]+[(η5-C5H5)Cr(CO)3]- (4; Röntgenstrukturanalyse).
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19861191205
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  • 7
    Electronic Resource
    Electronic Resource
    Synthese und Struktur des Mangan(II)-L-aspartat-trihydrats, Mn(L-Asp) · 3H2O (1988)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 121 (1988), S. 795-797 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Structure of Manganese(II) L-Aspartate Trihydrate, Mn(L-Asp)· 3H2OManganese L-aspartate chloride, Mn(L-AspH)Cl, has been prepared from equimolar quantities of MnCl2 and Mn(L-AspH)2 in water. This material can be converted into the title compound by treatment with aqueous KOH, and crystallized as a trihydrate from solutions kept at pH = 7.85. The compound has been characterized by elemental analysis and by single crystal X-ray structure determination. In the crystal, the aspartate dianion functions as a facially tridentate ligand to the Mn(II) center whose octahedral coordination sphere is completed by two water molecules and a carboxylate oxygen atom from a neighboring complex in trans position to the amino group. The stereochemistry of this coordination mode is different from that in the analogous magnesium compound, but similar to that in the cobalt(II) and zinc(II) analogues. The third water molecule is a hydrogen-bonded crystal water.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19881210427
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  • 8
    Electronic Resource
    Electronic Resource
    Metallaheterocumulene, IV. 2-Azaallyliden-Komplexe  -  neuartige Verbindungen mit einem gewinkelten CNCR2-Fragment als Komplexligand (1986)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 119 (1986), S. 2080-2093 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metallaheterocumulenes, IV. 2-Azaallylidene Complexes  -  Novel Compounds with a Bent CNCR2 Fragment as Complex Ligand(2-Azoniaallenylidene)pentacarbonyltungsten tetrabromoaluminate complexes [(CO)5W(CNCR2)]+AlBr4- (2-AlBr4) (CR2=C(C6H4Br-4)2 (a), CPh2 (b), C(C6H4OMe-4)2 (c), C(C6H4)2O (d), C(2,4,6-C6H2Me3)2 (e)) Which are synthesized by the reaction of (CO)5W[C(OEt)N=CR2] (1) with AlBr3, react with freshly distilled tetrahydrofuran to give neural trans-bromo(2-azaallylidene) complexes trans-Br(CO)4W(CNCR2) (3) and small amounts of (CO)5W—C≡N—[CR2]2—N≡C—W(CO)5 (4). The compounds 4 correspond to the product of a reductive dimerization of two cations 2. If 1b (or the corresponding methoxy compound 5) reacts with BBr3 instead of AlBr3/THF 4b is the main product. The spectroscopic data of 3 and the results of an X-ray analysis of 3b show that the replacement of a CO ligand in the cations 2 by Br- with formation of 3 results in a drastic change of the bonding situation within the CNCR2 ligand. 3a-e are the first compounds in which a strongly bent CNCR2 fragment functions as a complex ligand. The aminocarbyne complex trans-Br(CO)4W≡CNPh2 (7) was synthesized by BBr3-induced fragmentation of (CO)5W[C(NPh2)N=C(Ph)OMe] (6).
    Notes: (2-Azoniaallenyliden)pentacarbonylwolfram-tetrabromoaluminat-Komplexe [(CO)5W(CNCR2)]+AlBr4- (2-AlBr4) (CR2=C(C6H4Br-4)2 (a), CPh2 (b), C(C6H4OMe-4)2 (c), C(C6H4)2O (d), C(2,4,6-C6H2Me3)2 (e))  -  darstellbar durch Umsetzung von (CO)5W[C(OEt)N=CR2] (1) mit Albr3  -  reagieren mit frisch destillierten Tetrahydrofuran zu neutralen trans-Bromo(2-azaallyliden)-Komplexen trans-Br(CO)4W(CNCR2) (3) und wenig (CO)5W—C≡N—[CR2]2—N≡C—W(CO)5 (4). Die Verbindungen 4. entsprechen dem Produkt einer reduktiven Dimerisierung zweier Kationen 2. 4b wird zum Hauptprodukt der Umsetzung, wenn 1b (oder der entsprechende Methoxy-Komplex 5) mit BBr3 anstatt AlBr3/THF umgesetzt wird. Wie die spektroskopischen Daten von 3 sowie die Ergebnisse der an 3b durchgeführten Röntgenstrukturanalyse zeigen, führt der Austausch eines CO-Liganden in den Kationen 2 gegen Br- unter Bildung von 3 zu einer drastischen Veränderung der Bindungsverhältnisse im CNCR2-Liganden. 3a-e sind die ersten Verbindungen, in denen ein stark gewinkeltes CNCR2-Fragment als Komplexligand fungiert. Durch BBr3-induzierte Fragmentierung von (CO)5W[C(NPh2)N=C(Ph)OMe] (6) wurde der Aminocarbin-Komplex trans-Br(CO)4W≡CNPh2 (7) dargestellt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19861190703
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