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  • Articles: DFG German National Licenses  (60)
  • Inorganic Chemistry  (57)
  • Organic Chemistry  (3)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 104 (1971), S. 220-227 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: cis- and trans-3.3′-Dimethoxy-5.5′-di-tert-butyldiphenoquinone-(4.4′)The two geometric isomers of 3.3′-dimethoxy-5.5′-di-tert-butyldiphenoquinone-(4.4′) (1) were isolated. The configurational assignment was made on the basis of n.m.r. spectra and the X-ray diffraction pattern from single crystals. The free enthalpy of activation for the cis/trans-isomerisation was determined. -p-Diphenoquinones with different substituents in both rings, which were needed as model compounds, could be prepared for the first time.
    Notes: Die beiden geometrischen Isomeren des 3.3′-Dimethoxy-5.5′-di-tert.-butyl-diphenochinons-(4.4′) (1) wurden isoliert. Die Konfigurationszuordnung gelang anhand der NMR-Spektren sowie von Einkristall-Röntgenaufnahmen. Die Freie Aktivierungsenthalpie der cis/trans-Isomerisierung wurde bestimmt. -p-Diphenochinone mit verschiedenen Substituenten in beiden Ringen, als Vergleichssubstanzen benötigt, konnten erstmals dargestellt werden.
    Additional Material: 2 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 106 (1973), S. 1069-1075 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal and Molecular Structure of N3S3F3The crystal structure of N3S3F3 has been determined from single crystal X-ray data. The molecule forms a slightly puckered six-membered (S—N)3 ring with axial fluorine atoms. In contrast to N4S4F4 it has no alternating single and double bonds in the ring. The S—N bond lengths were found to be 1.587 (3) and 1.598 (3) Å, the S—F bond lengths to be 1.610 (3) Å. N3S3F3 crystallizes in the rhombohedral space group R3-C3i2.
    Notes: Die Struktur von N3S3F3 wurde röntgenographisch aus Diffraktometer-Einkristalldaten bestimmt. Das Molekül bildet einen leicht gewellten (S—N)3-Sechsring mit axialer Stellung der Fluoratome. Es hat im Gegensatz zum N4S4F4 keine alternierenden Doppel- und Einfach-bindungen im Ring. Die S—N-Bindungslängen betragen 1.587 (3) und 1.598 (3) Å, die S—F-Abstände 1.610 (3) Å. N3S3F3 kristallisiert rhomboedrisch in der Raumgruppe R3-C3i2 mit den (hexagonalen) Gitterkonstanten a = 10.238 (8) Å und c = 9.535 (7) Å.
    Additional Material: 2 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 2934-2940 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal and Molecular Structure of 2-Amino 2,4,4,6,6,-pentafluoro-1,3,5,2λ5, 4λ5, 6λ5- triazatriphosphorineThe crystal structure of the title compound 1 has been determined by direct methods from single crystal X-ray data and has been refined to R = 0.038 for 1465 reflections. The compound crystallizes in the monoclinic space group P21/c. The molecule forms a slightly puckered six-membered (P—N)3 ring. The endocyclic P—N bond lengths are significantly different (mean: 1.565 Å). The mean P—F bond length is 1.521 Å, the P—Namine bond length is 1.601 Å. The molecules are connected as layers through N—H⃛N hydrogen bonds.
    Notes: Die Struktur der Titelverbindung 1 wurde aus Diffraktometer-Einkristalldaten nach direkten Methoden bestimmt und für 1465 Reflexe zu einem R-Wert von 3.8% verfeinert. Die Verbindung kristallisiert monoklin in der Raumgruppe P21/c mit den Gitterkonstanten a = 7.958 Å, b = 5.222 Å, c = 19.297 Å, β = 101.24° Z = 4. Der P—N-Sechsring ist schwach gewellt. Die endocyclischen P—N-Abstände weisen signifikante Unterschiede auf (Einzelwerte: 1.551⃛1.586 Å, Mittelwert: 1.565 Å). Der Mittelwert der P—F-Bindungslängen beträgt 1.521 Å, die Länge der P—NAmin-Bindung ist 1.601 Å. Die Moleküle sind schichtartig über N—H⃛N-Wasserstoffbrücken verknüpft.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 2622-2627 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal and Molecular Structure of 4,4,6,6-Tetrafluoro-1,3,5,2λ5,4λ5,6λ5-triazatriphosphorine-2,2-diamineThe crystal structure of the geminal isomer of N3P3F4(NH2)2 (3) was determined by X-ray analysis and was refined to R = 0.035. Crystals of the compound are orthorhombic, space group Pnma. The six-membered (P—N)3 ring is planar within the limits of error. In the (NH2)2 P—N—P(F2) segment the P—N bond lengths are 1.597 and 1.524Å with the shorter one on the side of the PF2 group. In the (F2)P—N—P(F2) segment the P—N bond length is 1.564 Å. The mean bond lengths in each P—N—P segment are nearly equal. The mean values for the P—F and P—Namine bond lengths were found to be 1.532 and 1.602 Å, respectively. The endocyclic angles are: N—P—N 110.4°, 120.5°; P—N—P 125.7°, 117.2°.
    Notes: Die Struktur des geminalen N3P3F4(NH2)2 (3) wurde aus Röntgenbeugungsdaten bestimmt und zu einem R-Wert von 3.5% verfeinert. Die Verbindung kristallisiert orthorhombisch in der Raumgruppe Pnma. Der (P—N)3-Ring ist innerhalb der Fehlergrenzen planar. Die P—N-Abstände betragen im (NH2)2 P—N—P(F2)-Segment 1.597 und 1.524 Å mit dem kürzeren Abstand auf der Seite der PF2-Gruppe. Im (F2)P—N—P(F2)-Segment ergibt sich die P—N-Bindungslänge zu 1.564 Å. Damit sind die Mittelwerte der Bindungslängen in jedem P—N—P-Segment nahezu gleich groß. Die Mittelwerte für die P—F- und die P—NAmin-Bindungslängen betragen 1.532 bzw. 1.602 Å. Die N—P—N-Winkel im Ring wurden zu 110.4° und 120.5°, die P—N—P-Winkel zu 125.7° und 117.2° beobachtet.
    Additional Material: 1 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 1358-1361 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: S3N2-Rings with Fluorine Containing SubstituentsFrom the tin compound 1 and SOF2 the five-membered sulfur-nitrogen oxide 2 was prepared. 2 reacts with FSO2N=S=O, CF3SO2N=S=O, as well as with CF3SO2N=C=O and n-C4F9SO2NSO to yield the 1-sulfonylimino-1λ4,2,4λ4,3,5-trithiadiazoles 3,4 and 5 under evolution of SO2 as well as CO2. The X-ray structure analysis of 3 is reported. CH3SO2NSO, CF3S(O)NSO, and (CH3)3SiNSO react with 2 to form only sulfur and S4N4. In 1 the methyl-groups can be exchanged for chlorine atoms to give 7.
    Notes: Aus der Zinnverbindung 1 wurde mit SOF2 ein fünfgliedriges Schwefel-Stickstoff-Oxid 2 hergestellt. 2 reagiert mit FSO2N=S=O, CF3SO2N=S=O bzw. CF3SO2N=C=O und n-C4F9SO2NSO zu den 1-Sulfonylimino 1λ42,4λ4,3,5-trithiadiazolen 3,4 und 5 unter SO2-Abspaltung. Die Röntgenstrukturanalyse von 3 wird mitgeteilt. CH3SO2NSO, CF3S(O)NSO und (CH3)3SiNSO ergeben mit 2 lediglich Schwefel und S4N4. In 1 lassen sich die Methylgruppen mit SnCl4 gegen Chloratome unter Bildung von 7 austauschen.
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  • 6
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Existence of a Silaolefin: Synthesis and Crystal Structures of Wittig and Diels-Alder Products in Reactions of Lithiated (Fluorosilyl)diazasilacyclopentenes with Benzaldehyde and MethacroleinLithium salts of 1,2-diaza-3-sila-5-cyclopentenes react with fluorosilanes and aminofluorosilanes to give 4-(fluorosilyl)-substituted compounds 1 - 4. By reaction with tert-butyllithium 1 - 4 themselves form lithium salts 5 - 8, which react with fluorosilanes in a second substitution giving 9 and 10.5 and 7 undergo a Wittig-type reaction with benzaldehyde to form the benzylidene derivative 11. Spirocyclic Diels-Alder adducts (12, 13) are obtained from the reaction of 5 and 6 with 2-methyl-2-propenal. The propenylidene derivative 14 is formed as a by product. With excess 2-methyl-2-propenal, 12 reacts as a dienophile giving the oligocyclic Diels-Alder adducts 15 and 16. The crystal structures of 11 and 15 are reported.
    Notes: Lithiumsalze der 1,2-Diaza-3-sila-5-cyclopentene reagieren mit Fluorsilanen und Aminofluorsilanen zu den 4-(Fluorsilyl)-substituierten Verbindungen 1 - 4. In Reaktion mit tert-Butyllithium bilden 1 - 4 erneut Lithiumsalze (5 - 8), die mit Fluorsilanen unter Zweitsubstitution zu 9 und 10 reagieren. In Wittig-analoger Reaktion reagieren 5 und 7 mit Benzaldehyd zum Benzyliden-Derivat 11. Spirocyclische Diels-Alder-Addukte (12, 13) werden aus 5 und 6 mit 2-Methyl-2-propenal erhalten. Als Nebenprodukt entsteht das Propenyliden-Derivat 14. Mit überschüssigem Dien (2-Methyl-2-propenal) reagiert 12 als Dienophil zu den oligocyclischen Diels-Alder-Addukten 15 und 16. Kristallstrukturen von 11 und 15 werden mitgeteilt.
    Additional Material: 4 Tab.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 116 (1983), S. 1107-1117 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Rearrangement with Oxygen-Insertion in Azabicyclic Hydroxylamine DerivativesN-Hydroxy-2-azabicyclo[2.2.1]hept-5-ene (1) is rearranged to the oxaazabicyclic compounds 3, 4, and 8 by the reaction with either tosyl or benzoyl chloride. The structure of 3 was proved by X-ray analysis. Experiments with [18O]tosyl chloride as well as products of the intermediate 12 with methanol are consistent with a heterolysis in the intermediate 11 formed by N-tosylation  -  in contrast to the homolytic1) Meisenheimer rearrangement.
    Notes: N-Hydroxy-2-azabicyclo[2.2.1]hept-5-en (1) wird bei der Umsetzung mit Tosyl- und Benzoylchlorid umgelagert zu den Oxaazabicyclen 3, 4 und 8. Die Struktur von 3 wurde durch Röntgenstrukturanalyse bewiesen. Versuche mit [18O]Tosylchlorid sowie die Abfangprodukte mit Methanol sprechen für eine ionische Spaltung in dem durch N-Tosylierung gebildeten Intermediären 11, im Gegensatz zum radikalischen Ablauf der sonst analogen Meisenheimer-Umlagerung.
    Additional Material: 1 Ill.
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  • 8
    ISSN: 0009-2940
    Keywords: Carbene complexes of chromium and tungsten ; 1-Metalla-1,3,5-trienes ; 1-Metalla-1,3-dien-5-ynes ; Insertion of alkynes into M=C and C=C bonds ; [2 + 2] Cycloaddition reactions of carbene complexes and alkynes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organic Syntheses via Transition Metal Complexes, 51. - 1-Metalla-1,3,5-trienes and 1-Metalla-1,3-dien-5-ynes of Chromium and Tungsten by Insertion of Alkynes into M=C and C=C Bonds of 1-Metalla-1,3-dienes and 1-Metalla-1-en-3-ynes, respectively1-Metalla-1,3,5-trienes LnM=C(NEt2)-C(Me)—C(OEt)-CH=CHPh (3,4) and LnM=C(OEt)- CH=C(NEt2) - C(Me)=CHPh [5, LnM=Cr(CO)5 (a), W(CO)5 (b)] are obtained for the first time from the corresponding 1-metalla-1,3-dienes LnM=C(OEt) - CH=CHPh (1a, b) under very mild conditions by the insertion of the electron-rich alkyne Et2N-C ≡ C - Me (2) into the M=C and the C=C bonds, respectively, of 1. The chelate complex (6b) and the cyclobutenyl carbene complex 7b are isolated as minor side products. 1-Metalla-1,3-dien-5-ynes LnM=C(NEt2) - C(Me)=C(OEt) - C ≡ CPh [9, 10, LnM=Cr(CO)5 (a), W(CO)5 (b)] are formed with high regio- and stereoselectivity on insertion of 2 into the M=C bonds of 1-metalla-1-en-3-ynes 8. X-ray data are given for the tungsten complex 3b.
    Additional Material: 1 Ill.
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  • 9
    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.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 226-232 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structures of the S3N2+ Radical Cation in S3N2+SO3CF3- · 1/2 CH3CN and of S3N2(NSO2F)The molecular and crystal structures of S3N2+SO3CF3- · 1/2 CH3CN (1) and S3N2NSO2F (2) were determined from single crystal X-ray diffraction data. The S3N2+ radical cation in 1 is planar, two cations being connected through weak S—S bonding interactions to form dimers with a chair configuration. The S3N2 ring of 2, in which the NSO2F group is covalently bonded to one of the S atoms of the S — S group, is not planar; the S — S bond is weaker than in 1.
    Notes: Die Röntgenstrukturanalysen von S3N2+SO3CF3- - 1/2 CH3CN (1) und S3N2NSO2F (2) zeigen in 1 ein planares S3N2+-Radikalkation, wobei zwei Kationen über schwache S-S-Wechselwirkungen zu sesselförmigen Dimeren assoziiert sind. Der an einem S-Atom der S — S-Gruppe substituierte S3N2-Ring in 2 ist nicht planar; die S — S-Bindung ist schwächer als in 1.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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