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  • 1
    Electronic Resource
    Electronic Resource
    Reaktive E = C(p - p)π-Systeme, XXXI Erste Vertreter aminosubstituierter 1,2,4-Diazaphosphole (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 411-414 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkyne, amino- ; [3 + 2] Cycloaddition ; 1,2,4-Diazaphospholes ; 1,2,3-Diazaphospholes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactive E = C(p - p)π Systems, XXXII[1].  -  First Representatives of Amino-Substituted 1,2,4-Diazaphospholes(Diisopropylamino)phosphaethyne iPr2N - C≡P reacts at 20° C in a [3 + 2] cycloaddition with (trifluoromethyl)diazomethane (2a) or methyl diazoacetate (2b) to yield a mixture of the corresponding regioisomers 1H-1,2,4-diazaphospholes (5a or 5b) and 1H-1,2,3-diazaphospholes (6a or 6b) in quantitative yields (isomer ratio: 5a/6a = 2:1; 5b/6b = 4:1). X-ray diffraction studies on 5a and 5b indicate a delicate charge balance in the bonding system of 1H-1,2,4,σ2-diazaphospholes under the influence of the exocyclic push/pull substituents iPr2N and CF3 or CO2Me, respectively.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250219
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  • 2
    Electronic Resource
    Electronic Resource
    Reaktive E = C(p-p)π-Systeme, XXXIII. Side-on-Koordination des Phosphaalkins P ≡ C  -  N(iPr)2 im 16e-Nickel(0)-Komplex Ni(CO)PCy3[PCN(iPr)2] (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 63-65 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkyne, amino- ; Nickel carbonyl phosphane complex ; π Coordination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactive E = C(p-p)π Systems, XXXIII.  -  Side-on Coordination of the Phosphaalkyne P ≡ C  -  N(iPr)2 in the 16e Nickel(0) Complex Ni(CO)PCy3[PCN(iPr)2]The reaction of (diisopropylamino)phosphaethyne P ≡ C  -  N(iPr)2 with the nickel complex [Ni(CO)3PCy3] - in contrast to the analogous reactions with Ni(CO)4 or Ni(CO)3PR3 (R = Me, Ph) - leads to the novel 16e nickel(0) system [Ni{η2-P ≡ C  -  N(iPr2)}(CO)PCy3] with a planar geometry of all skeleton atoms besides the methyl and cyclohexyl groups. Side-on coordination of the P ≡ C triple bond results in an increase of the PC distance to 1.665 Ȧ typical for phosphaalkenes.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260111
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  • 3
    Electronic Resource
    Electronic Resource
    Organic Syntheses via Transition Metal Complexes, 74[1] Novel Phosphonium Allenide and 2-Phosphanylethenyl Carbene Chromium and Tungsten Complexes (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 2475-2482 
    Details
    ISSN: 0009-2940
    Keywords: Vinylcarbene complexes ; Chromium complexes ; Tungsten complexes ; Phosphorus ylide complexes ; Alkynylcarbene complexes ; Allene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Alkynylcarbene complexes (CO)5M≡C(OEt)-C≡C—R 1 (M = Cr, W; R = Ph, tBu, SiMe3) readily add tertiary phosphanes PPhR2′ 4 (R′ = Ph, Me) to form stable zwitterionic phosphonium allenide complexes (CO)5M--C(OEt) = C≡C(R)-P+PhR2′ 5. Complex 5a (M = Cr, R = R′ = Ph) was characterized by X-ray diffraction. The addition of secondary phosphanes PHR2 6 to 1 affords red (2-phosphanyl ethenyl)-carbene complexes (CO)5M≡C(OEt)-CH≡C(R)-PR2 (E)-8 (R = tBu, cC6H11, Ph) in 34-89% isolated yields. Dinuclear complexes (CO)5M≡C(OEt)-CH≡C(R)-P(R2)M(CO)5 (E)-9 are obtained as byproducts. Compounds (E)-8b (M = Cr, R = cC6H11) and (E)-9i (M = Cr, R = Ph) were characterized by X-ray analyses.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941271218
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  • 4
    Electronic Resource
    Electronic Resource
    Organische Synthesen mit Übergangsmetallkomplexen, 71. Methylcarben-Komplexe von Chrom und Wolfram mit Cycloheptatrienyl-, Cyclohexadienyl[Fe(CO)3]- und Cycloheptadienyl[Fe(CO)3]-Resten als α-Substituenten (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 731-738 
    Details
    ISSN: 0009-2940
    Keywords: Methylcarbene complexes of chromium and tungsten ; Cyclohexadienyl tricarbonyliron, carbene derivatives of ; Cycloheptadienyl tricarbonyliron, carbene derivatives of ; Cycloheptatrienyl, carbene derivatives of ; Enol ether, elimination from carbene complexes ; Spirocyclopropanes, elimination from carbene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organic Syntheses via Transition Metal Complexes, 71[1].  -  Methylcarbene Complexes of Chromium and Tungsten with Cycloheptatrienyl-, Cyclohexadienyl[Fe(CO)3]- and Cycloheptadienyl[Fe(CO)3] SubstituentsMethylcarbene complexes LnM=C(OEt)CH3 1 [LnM = (CO)5Cr, (CO)5W] react with tropylium tetrafluoroborate (2a) or coordinated olefins of [C6H7Fe(CO)3]BF4 (2c), [C7H9Fe-(CO)3]BF4 (2d), and [C7H7Fe2(CO)6]BF4 (2d) in the presence of Et3N to give complexes LnM=C(OEt)CH2R 3a-e and LnM=C(OEt)CHR2 7a-d by substitution of one or two α-hydrogen atoms. The trimetallic WFe2 carbene complexes 7c, d derived from 1b with 2c, d form three stereoisomers each, which are fully characterized spectroscopically, (R*,R*,S*)-7c additionally also by an X-ray structure analysis, Ligand elimination from 3 and 7 may involve a-and/or β-hydrogen transfer reactions: Thus enol ethers (Z/E)-6 are eliminated from α-monosubstituted methylcarbene complexes 3a, c, d in yields of 62-90% by a pyridine-induced transfer of an α-hydrogen to the carbene carbon atom; with increasing steric demand of R the elimination of the (Z) isomer (Z)-6 from 3 is favoured over the formation of the (E) isomer (E)-6. The enol ether 10 becomes a minor side product in the pyridine-induced ligand elimination from α-disubstituted complexes 7a, b. In these cases the spirocyclopropane 8 is formed as the main product (60-82%) besides the 4,5-homotropylidene 9 by a conformationally directed β-hydrogen transfer reaction.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270424
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  • 5
    Electronic Resource
    Electronic Resource
    1,2-Dihydro-1,3,2λ5,4λ5-diazadiphosphet - Synthese, Struktur und Isomerisierung zum „inneren Salz“ von 1,3,2,4λ5-Diazadiphosphetan-2-iumhydroxid* (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 2631-2634 
    Details
    ISSN: 0009-2940
    Keywords: 1,2-Dihydro-1,3,2λ5,4λ5-diazadiphosphete ; Isomerization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,2-Dihydro-1,3,2λ5,4λ5-diazadiphosphete - Synthesis, Structure and Isomerization to the „Inner Salt“ of 1,3,2,4λ5-Diazadiphosphetan-2-ium HydroxideThe photochemical reaction of the azidophosphane (iPr2N)2PN3 (1) with the tetraazaphospholene (3) and the bis(imino)phosphorane (Me3Si)2NP(=NSiMe3)2 (6) proceeds by elimination of N2 to yield (5) and by 1,3-silyl group shift to furnish (8) the structures of which were determined by means of NMR data and, in the case of 5, additionally by X-ray structure analysis.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921251202
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  • 6
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur einer Neuen hexagonalen Modifikation von Al2S3 mit fünffach koordiniertem AluminiumProfessor Heinrich Nöth zum 65. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 983-988 
    Details
    ISSN: 0044-2313
    Keywords: Aluminum sulfide ; crystal structure ; chemical transport ; five-coordinated aluminum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of a Novel Hexagonal Modification of Al2S3 with Five-coordinated AluminumA new hexagonal high temperature modification of Al2S3 could be prepared by chemical vapour transport with iodine (860 → 750°C) or by annealing of α -Al2S3 at 550°C. According to the single crystal X-ray structure determination the novel form of Al2S3 crystallizes in space group P 61 (No. 169) with a = 6.491(1), c = 17.169(4) Å, V = 626.5 Å3, Z = 6; R = 0.0253. In this modification one half of the aluminum atoms are tetrahedrally coordinated [d(Al—S): 2.226-2.267 Å], whereas the other half are in trigonal bipyramidal coordination of five S atoms with bond lengths of 2.272-2.315 Å (equatorial) and 2.495-2.521 Å (axial).Aluminum in AlS5 coordination is observed for the first time in this compound. The crystal structure is isotypic to In2Se3 and AlInS3. In addition, results of a refinement of the α -Al2S3 crystal structure are reported which were obtained on crystals prepared also by chemical vapour transport with iodine.
    Notes: Eine bisher noch nicht beschriebene hexagonale Hochtemperatur-Modifikation von Al2S3 konnte in reiner Form entweder durch chemischen Transport mit Iod (860 → 750°C) oder durch Tempern von α -Al2S3 oberhalb 550°C erhalten und durch eine Einkristall-Röntgenstrukturanalyse charakterisiert werden.Die neue Form des Al2S3 kristallisiert in der Raumgruppe P 61 (Nr. 169) mit a = 6,491(1), c = 17,169(4) Å, V = 626,5 Å3, Z = 6; R = 0,0253. In dieser Modifikation liegt die eine Hälfte der Aluminiumatome tetraedrisch koordiniert vor [d(Al—S): 2,226-2,267 Å], während die andere Hälfte trigonal-bipyramidal von fünf S-Atomen mit Al—S-Bindungslängen von 2,272 bis 2,315 Å (äquatorial) und 2,495-2,521 Å (axial) umgeben ist.Aluminium in AlS5-Koordination ist bisher unbekannt und wird hier zum ersten Mal beobachtet. Die Struktur ist isotyp zu In2Se3 und AlInS3. Zusätzlich wird über die Verfeinerung der Kristallstruktur α von -Al2S3 an Einkristallen berichtet, die ebenfalls durch chemischen Transport mit Iod hergestellt wurden.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190604
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