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Coordination compounds and complexes exhibit different colors, geometries, and magnetic behavior, depending on the metal atom/ion and ligands from which they are composed. In an attempt to explain the bonding and structure of coordination complexes, Linus Pauling proposed the valence bond theory, or VBT, using the concepts of hybridization and the overlapping of the atomic orbitals. According to VBT, the central metal atom or ion (Lewis acid) hybridizes to provide empty orbitals of suitable...
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Vicinal or three-bond coupling is commonly observed between protons attached to adjacent carbons. Here, nuclear spin information is primarily transferred via electron spin interactions between adjacent C‑H bond orbitals. This generally favors the antiparallel arrangement of spins, so 3J values are usually positive.
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Coupling interactions are strongest between NMR-active nuclei bonded to each other, where spin information can be transmitted directly through the pair of bonding electrons. While nuclei polarize their electrons to the opposite spins, the bonding electron pair has opposite spins. Configurations with antiparallel nuclear spins are expected to be lower in energy. When coupling makes antiparallel states more favorable, J is considered to have a positive value. The one-bond coupling constant, 1J,...
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Two NMR-active nuclei bonded to a central atom can be involved in geminal or two-bond coupling. Geminal coupling is commonly seen between diastereotopic protons in chiral molecules and unsymmetrical alkenes, among others.
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In bromoethane, the three methyl protons are coupled to the two methylene protons that are three bonds away. In accordance with the n+1 rule, the signal from the methyl protons is split into three peaks with 1:2:1 relative intensities. The methylene protons appear as a quartet, with the relative intensities of 1:3:3:1.
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Intermolecular (119)Sn,(31)P Through-Space Spin-Spin Coupling in a Solid Bivalent Tin Phosphido Complex.

Janet Arras1,2, Klaus Eichele1, Boris Maryasin2

  • 1Institut für Anorganische Chemie, Universität Tübingen , Auf der Morgenstelle 18, 72076 Tübingen, Germany.

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This study details a novel bivalent tin complex, [Sn(NP)2], revealing unexpected through-space spin-spin couplings between tin and phosphorus atoms. These findings challenge conventional understanding of non-bonding interactions in organometallic chemistry.

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Area of Science:

  • Organometallic Chemistry
  • Solid-State Chemistry
  • Computational Chemistry

Background:

  • Bivalent tin complexes are of interest due to their unique electronic properties.
  • Nuclear Magnetic Resonance (NMR) spectroscopy is a powerful tool for characterizing molecular structure and bonding.
  • Spin-spin couplings provide insights into through-bond and through-space interactions.

Purpose of the Study:

  • To synthesize and characterize a novel bivalent tin complex, [Sn(NP)2].
  • To investigate through-bond and through-space spin-spin couplings in the complex using NMR spectroscopy.
  • To computationally validate the observed NMR parameters and coupling mechanisms.

Main Methods:

  • Synthesis and X-ray diffraction of the bivalent tin complex [Sn(NP)2].
  • Solution and solid-state Nuclear Magnetic Resonance (NMR) spectroscopy, including phosphorus-31 ((31)P) and tin-119 ((119)Sn) cross-polarization magic angle spinning (CP/MAS) NMR.
  • Density Functional Theory (DFT) calculations for NMR parameter prediction.
  • Natural Bond Orbital (NBO) analysis to assess bonding interactions.

Main Results:

  • The bivalent tin complex [Sn(NP)2] was successfully prepared and characterized, with X-ray diffraction revealing two polymorphs.
  • (31)P and (119)Sn CP/MAS NMR spectra showed single crystallographic sites for phosphorus and tin.
  • Both through-bond (1)J((117/119)Sn,(31)P) and unexpected through-space (TS)J((117/119)Sn,(31)P) spin-spin couplings were observed.
  • DFT calculations corroborated the experimental NMR data, including the through-space coupling.
  • Intermolecular tin-phosphorus distances (>4.6 Å) exceeded the sum of van der Waals radii, indicating no direct bonding.

Conclusions:

  • The study successfully synthesized and characterized a bivalent tin complex with novel structural and spectroscopic properties.
  • The observation of through-space spin-spin couplings between tin and phosphorus atoms, despite large intermolecular distances, provides new insights into non-covalent interactions.
  • DFT and NBO analyses support the experimental findings, highlighting the importance of considering subtle electronic effects in organometallic systems.