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Determination of Coupling Signs 1J(119Sn, 15N ) and 2J(119Sn, 117Sn) in Trimethylstannylamines

  • Bernd Wrackmeyer , Jürgen Weidinger , Heinrich Nöth , Wolfgang Storch , Thomas Seifert and Martina Vosteen
Published/Copyright: June 2, 2014
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Zeitschrift für Naturforschung B
From the journal Zeitschrift für Naturforschung B Volume 53 Issue 12

The l5N-labelled trimethylstannylamines 1 - 3 [(Me3Sn)3N, (Me3Sn)2NPh, (Me3Sn)2NBCgHi4 (BCgHi4 = 9-borabicyclo[3.3.0]nonyn and the non-labelled 4, Me3Sn-N(BC8Hi4)2 , were prepared and studied by 1H, 1C, 15N and 119Sn NMR. The 15N ultrahigh resolution NMR spectra of 1 revealed otherwise unobserved parameters such as 2J(15N ,Sn ,13C ) and the isotope induced chemical shift 2Δ12/13C(15N). 119Sn NMR spectra of 1, recorded under similar conditions, also show new parameters such as 3J(119Sn,N,Sn,13C) which are not resolved in the non-labelled derivative. By using various types o f two-dimensional heteronuclear shift correlations, absolute coupling signs of 1J(119Sn,15N) (all < 0) in 1 - 3 were determined. By the same techniques it proved possible to confirm the negative sign o f :7(Sn,Sn) (-195.4 Hz) in 1. In contrast, the coupling constants 2J(Sn,Sn) for 2 (+71.7) and 3 (+62.0) possess a positive sign. This sign inversion, observed here for the first time for apparently similar compounds, demonstrates the enormous influence of substituents on the nature of the lone pair of electrons at the nitrogen atom. It also shows that these experiments for sign determinations of coupling constants are necessary in order to interpret these data correctly.

Keywords: Tin; Amines; NM R Data; Ultrahigh Resolution; Coupling Sign Determination
Received: 1998-7-30
Published Online: 2014-6-2
Published in Print: 1998-12-1

© 1946 – 2014: Verlag der Zeitschrift für Naturforschung

Articles in the same Issue

  1. Die Kristallstruktur von N,N'-Ditosyl-/7-phenylendiamin, Dichtefunktionaltheorie-Berechnungen von Konformationen und Wasserstoffbrücken-Motive von Sulfonamiden / Interactions in M olecular Crystals, 146 [1, 2], The Crystal Structure of N,N'-Ditosyl-p-phenylenediam ine, Density Functional Theory Calculations of Conformations and Hydrogen Bond Motifs in Sulfonamides
  2. Wechselwirkungen in Molekülkristallen, 147 [1, 2]. Isostrukturelle Wirt/Gast-Einschluß-Verbindungen von N,N'-Ditosyl- p-phenylendiamin mit Aceton, Cyclopentanon, Cyclopent-2-en-l-on, 1,3-Dioxolan, Tetrahydrofuran und 2,5-Dihydrofuran / Interactions in Molecular Crystals, 147 [1, 2], Isostructural Host/Guest-Inclusion Compounds of N,N'-Ditosyl-p-phenylenediamine with Acetone, Cyclopentanone, Cyclopent-2-ene-l-one, 1,3-Dioxolane, Tetrahydrofurane, and 2,5-D ihydrofurane
  3. Wechselwirkungen in Molekülkristallen, 148 [1,2 ]. Wirt/Gast-Einschlußverbindungen von N,N'-Ditosyl-p-phenylendiamin mit Furan, Benzol und Dioxan / Interactions in M olecular Crystals, 148 [1, 2]. Host/Guest-Inclusion Compounds of N ,N'-Ditosyl-p-phenylenediamine with Furane, Benzene and Dioxane
  4. Wechselwirkungen in Molekülkristallen, 149 [1 -3]. Wirt/Gast-Einschlußverbindungen von NjN'-Ditosyl-p-phenylendiamin: Die Wasserstoffbrücken-Addukte mit Morpholin; Pyridin, N,N-Dimethylformamid und Dimethylsulfoxid / Interactions in Molecular Crystals, 149 [1 - 3]. Host/Guest-Inclusion Compounds of N,N'-Ditosyl-/?-phenylenediamine: The Hydrogen Bonded Adducts with Morpholine, Pyridine, N ,N -Dimethylform amide, and Dimethylsulfoxide
  5. Oligomere Tetraeder-Anionen in Borophosphaten: Sechserringe mit offenen und cyclischen Phosphat-Verzweigungen in der Kristallstruktur von K6Cu2[B4P8O28(OH)6] / Oligomeric Tetrahedral Anions in Borophosphates: Six-Membered Rings with Open and Cyclic Phosphate Branchings in the Crystal Structure of K6Cu2[B4P8O28(OH)6]
  6. Four Novel N3O4 Donor Macrocycles and their Lanthanide(III) Complexes
  7. Reaktionen des donorfreien (CF3)2Cd mit Phosphor(V)halogeniden: Difluorcarben-Einschiebungen und Direktsynthese von (CF3)3PF2 / Reactions of Donor-Free (CF3)2Cd with Phosphorus(V) Halides: Insertion of Difluorocarbene and Direct Synthesis of (CF3)3PF2
  8. Übergangsmetallkomplexe mit Schwefelliganden, CXXXIII [1]. Synthese, Struktur und Eigenschaften neuer FeII-Komplexe mit [FeN2S2]-Gerüsten / Transition Metal Complexes with Sulfur Ligands, CXXXIII [1]. Synthesis, Structure, and Properties of New FeII Complexes with [Fe2N2S2] Cores
  9. Arsenic(III), Antimony (III) and Bismuth(III) Thiobenzoates: Crystal and Molecular Structures of M(SOCR)3 and PhSb(SOCPh)2
  10. BaCu6Ge2S8 -Ein Thiogermanat als Variante der Li3Bi-Struktur / BaCu6Ge2S8 -A Thiogermanate as a Variant of the Li3Bi Structure
  11. Tetrazinn(II)-und Bariumtrizinn(II)-tetrakis[μ3 -tri-ter/-butyIsilylphosphan- diid]-Verbindungen mit einem Tetrametallatetraphosphacuban-Gerüst / Tetratin(II) and Barium Tritin(II) Tetrakis[μ3-tri-rm-butylsilylphosphandiide] Compounds with a Tetrametallatetraphosphacubane Core
  12. Determination of Coupling Signs 1J(119Sn, 15N ) and 2J(119Sn, 117Sn) in Trimethylstannylamines
  13. Metallkomplexe mit biologisch wichtigen Liganden, CIX [1]. Metallorganische Verbindungen von Platin(II), Ruthenium(II), Rhodium (III) und Iridium (III) mit Oxocarbonyl-N-geschützten a-Am inosäuren und L-Methionylglycinat / Metal Complexes with Biologically Important Ligands, CIX [1]. Organometallic Compounds of Platinum(II), Ruthenium(II), Rhodium(III), and Iridium(III) with Oxocarbonyl-N-protected a-Amino Acids and L-Methionylglycinate
  14. Phosphenium-Komplexe, XXIX [1]. [4+2]-Cycloadditionen von Phospheniumkomplexen des Typs Cp(OC)2W = PR2(R = Alkyl, Aryl) mit 2,3-Dimethylbutadien / Phosphenium Complexes, XXIX [1], [4+2]-Cycloaddition of Phosphenium Complexes of the Type Cp(OC)2W=PR2 (R = Alkyl, Aryl) with 2,3-Dimethylbutadiene
  15. Molecular Recognition Analyzed by Observing Intramolecular Interconversion with EPR Spectroscopy
  16. Synthesis of the Stereoisomers of β-Hydroxyhistidine and their Analytical Identification in Hydrolysates of Bacterial Peptides
  17. The Structure of Lithiumiodide 3-Tetrahydrofuran
  18. Benzo-18-krone-6 -Acetonitril (1/2): Kristallisation und Tieftemperatur- Röntgenstrukturanalyse / Benzo-18 -crown-6 -Acetonitrile (1/2): Crystallization and Low-Temperature X-Ray Analysis
  19. Subject Index
  20. Authors Index
https://doi.org/10.1515/znb-1998-1212
Keywords for this article
Tin; Amines; NM R Data; Ultrahigh Resolution; Coupling Sign Determination

Articles in the same Issue

  1. Die Kristallstruktur von N,N'-Ditosyl-/7-phenylendiamin, Dichtefunktionaltheorie-Berechnungen von Konformationen und Wasserstoffbrücken-Motive von Sulfonamiden / Interactions in M olecular Crystals, 146 [1, 2], The Crystal Structure of N,N'-Ditosyl-p-phenylenediam ine, Density Functional Theory Calculations of Conformations and Hydrogen Bond Motifs in Sulfonamides
  2. Wechselwirkungen in Molekülkristallen, 147 [1, 2]. Isostrukturelle Wirt/Gast-Einschluß-Verbindungen von N,N'-Ditosyl- p-phenylendiamin mit Aceton, Cyclopentanon, Cyclopent-2-en-l-on, 1,3-Dioxolan, Tetrahydrofuran und 2,5-Dihydrofuran / Interactions in Molecular Crystals, 147 [1, 2], Isostructural Host/Guest-Inclusion Compounds of N,N'-Ditosyl-p-phenylenediamine with Acetone, Cyclopentanone, Cyclopent-2-ene-l-one, 1,3-Dioxolane, Tetrahydrofurane, and 2,5-D ihydrofurane
  3. Wechselwirkungen in Molekülkristallen, 148 [1,2 ]. Wirt/Gast-Einschlußverbindungen von N,N'-Ditosyl-p-phenylendiamin mit Furan, Benzol und Dioxan / Interactions in M olecular Crystals, 148 [1, 2]. Host/Guest-Inclusion Compounds of N ,N'-Ditosyl-p-phenylenediamine with Furane, Benzene and Dioxane
  4. Wechselwirkungen in Molekülkristallen, 149 [1 -3]. Wirt/Gast-Einschlußverbindungen von NjN'-Ditosyl-p-phenylendiamin: Die Wasserstoffbrücken-Addukte mit Morpholin; Pyridin, N,N-Dimethylformamid und Dimethylsulfoxid / Interactions in Molecular Crystals, 149 [1 - 3]. Host/Guest-Inclusion Compounds of N,N'-Ditosyl-/?-phenylenediamine: The Hydrogen Bonded Adducts with Morpholine, Pyridine, N ,N -Dimethylform amide, and Dimethylsulfoxide
  5. Oligomere Tetraeder-Anionen in Borophosphaten: Sechserringe mit offenen und cyclischen Phosphat-Verzweigungen in der Kristallstruktur von K6Cu2[B4P8O28(OH)6] / Oligomeric Tetrahedral Anions in Borophosphates: Six-Membered Rings with Open and Cyclic Phosphate Branchings in the Crystal Structure of K6Cu2[B4P8O28(OH)6]
  6. Four Novel N3O4 Donor Macrocycles and their Lanthanide(III) Complexes
  7. Reaktionen des donorfreien (CF3)2Cd mit Phosphor(V)halogeniden: Difluorcarben-Einschiebungen und Direktsynthese von (CF3)3PF2 / Reactions of Donor-Free (CF3)2Cd with Phosphorus(V) Halides: Insertion of Difluorocarbene and Direct Synthesis of (CF3)3PF2
  8. Übergangsmetallkomplexe mit Schwefelliganden, CXXXIII [1]. Synthese, Struktur und Eigenschaften neuer FeII-Komplexe mit [FeN2S2]-Gerüsten / Transition Metal Complexes with Sulfur Ligands, CXXXIII [1]. Synthesis, Structure, and Properties of New FeII Complexes with [Fe2N2S2] Cores
  9. Arsenic(III), Antimony (III) and Bismuth(III) Thiobenzoates: Crystal and Molecular Structures of M(SOCR)3 and PhSb(SOCPh)2
  10. BaCu6Ge2S8 -Ein Thiogermanat als Variante der Li3Bi-Struktur / BaCu6Ge2S8 -A Thiogermanate as a Variant of the Li3Bi Structure
  11. Tetrazinn(II)-und Bariumtrizinn(II)-tetrakis[μ3 -tri-ter/-butyIsilylphosphan- diid]-Verbindungen mit einem Tetrametallatetraphosphacuban-Gerüst / Tetratin(II) and Barium Tritin(II) Tetrakis[μ3-tri-rm-butylsilylphosphandiide] Compounds with a Tetrametallatetraphosphacubane Core
  12. Determination of Coupling Signs 1J(119Sn, 15N ) and 2J(119Sn, 117Sn) in Trimethylstannylamines
  13. Metallkomplexe mit biologisch wichtigen Liganden, CIX [1]. Metallorganische Verbindungen von Platin(II), Ruthenium(II), Rhodium (III) und Iridium (III) mit Oxocarbonyl-N-geschützten a-Am inosäuren und L-Methionylglycinat / Metal Complexes with Biologically Important Ligands, CIX [1]. Organometallic Compounds of Platinum(II), Ruthenium(II), Rhodium(III), and Iridium(III) with Oxocarbonyl-N-protected a-Amino Acids and L-Methionylglycinate
  14. Phosphenium-Komplexe, XXIX [1]. [4+2]-Cycloadditionen von Phospheniumkomplexen des Typs Cp(OC)2W = PR2(R = Alkyl, Aryl) mit 2,3-Dimethylbutadien / Phosphenium Complexes, XXIX [1], [4+2]-Cycloaddition of Phosphenium Complexes of the Type Cp(OC)2W=PR2 (R = Alkyl, Aryl) with 2,3-Dimethylbutadiene
  15. Molecular Recognition Analyzed by Observing Intramolecular Interconversion with EPR Spectroscopy
  16. Synthesis of the Stereoisomers of β-Hydroxyhistidine and their Analytical Identification in Hydrolysates of Bacterial Peptides
  17. The Structure of Lithiumiodide 3-Tetrahydrofuran
  18. Benzo-18-krone-6 -Acetonitril (1/2): Kristallisation und Tieftemperatur- Röntgenstrukturanalyse / Benzo-18 -crown-6 -Acetonitrile (1/2): Crystallization and Low-Temperature X-Ray Analysis
  19. Subject Index
  20. Authors Index
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