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2D-NMR: Part VI. 2D-INADEQUATE spectral analysis and crystal structure of tricyclo[7.3.1.02,7]tridecane

2D-NMR, 6. Mitt.: 2D-INADEQUATE Spektrum und Kristallstruktur von einem Tricyclo[7.3.1.02,7]tridecanderivat

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Abstract

2-Hydroxy-13-oxo-tricyclo[7.3.1.02,7]tridecane derivatives can be obtained by reaction of cyclohexanone with alcohols under alkaline conditions. The unambiguous assignment of all signals of the1H-NMR- and13C-NMR-spectrum is possible by 2D-1H-13C-shift correlation and 2D-INADEQUATE. Compound1 crystallizes in space group P21/n witha=8.518 (1),b=14.789 (2),c=19.321 (2) Å, γ=94.91 (1)°,Z=8,D c =1.22 Mg cm−3. The structure refined toR=0.100 andR w =0.097 for 1719 observed reflections. Two independent molecules form centrosymmetric hydrogen-bonded dimers.

Zusammenfassung

Das13C-NMR-Spektrum von 2-Hydroxy-13-oxo-tricyclo[7.3.1.02,7]tridecan kann mit Hilfe eines INADEQUATE Experimentes eindeutig zugeordnet werden. Die Kristallstrukturdaten dieser Verbindung werden beschrieben.

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Authors and Affiliations

  1. Institute of Pharmaceutical Chemistry, University of Vienna, A-1090, Wien, Austria

    Gerhard Buchbauer, Angela Fischlmayr & Carla Wassmann

  2. Institute of Organic Chemistry, University of Vienna, A-1090, Wien, Austria

    Ernst Haslinger, Wolfgang Robien & Carla Wassmann

  3. Institute of Mineralogy, Crystallography and Structural Chemistry, Technical University of Vienna, A-1060, Wien, Austria

    Horst Völlenkle & Carla Wassmann

Authors
  1. Gerhard Buchbauer
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  2. Angela Fischlmayr
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  3. Ernst Haslinger
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  4. Wolfgang Robien
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  5. Horst Völlenkle
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  6. Carla Wassmann
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Additional information

Part V:Haslinger E.,Kalchhau-ser H.,Robien W.,Steindl H., Monatsh. Chem.115, 597 (1984).

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Buchbauer, G., Fischlmayr, A., Haslinger, E. et al. 2D-NMR: Part VI. 2D-INADEQUATE spectral analysis and crystal structure of tricyclo[7.3.1.02,7]tridecane. Monatsh Chem 115, 739–748 (1984). https://doi.org/10.1007/BF01120969

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  • DOI: https://doi.org/10.1007/BF01120969

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