Do sitting-atop metalloporphyrin complexes exist? Observation of N-H- - -pi bonding in arene solvates of a diprotonated porphyrin dication

Inorg Chem. 2007 Mar 5;46(5):1514-6. doi: 10.1021/ic062213g. Epub 2007 Jan 31.

Abstract

The existence of sitting-atop metalloporphyrin complexes, the proposed intermediates in the metalation of free-base porphyrins, has been explored via the microscopic reverse reaction, i.e., protonation of metalloporphyrins with a strong acid. The reaction of M(Tp-TP) (M = Zn, Cu, Ni; Tp-TP = dianion of tetra-p-tolylporphyrin) with mesitylenium carborane salts produced only the demetalated porphyrin in its diprotonated form, [H4Tp-TP][carborane]2 (carborane = CHB11H5Cl6-, CHB11H5Br6-, CHB11Cl11-). In arene solvents, the H4Tp-TP2+ dication shows an unusually upfield shifted 1H NMR resonance at ca. -6 ppm, which X-ray crystallography reveals to arise from N-H- - -pi hydrogen bonding of the acidic protons to arene solvent molecules.

Publication types

  • Research Support, N.I.H., Extramural
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Calixarenes / chemistry*
  • Cations / chemistry
  • Crystallography, X-Ray
  • Magnetic Resonance Spectroscopy / methods
  • Metalloporphyrins / chemistry*
  • Models, Molecular
  • Molecular Structure
  • Porphyrins / chemistry*
  • Protons
  • Sensitivity and Specificity

Substances

  • Cations
  • Metalloporphyrins
  • Porphyrins
  • Protons
  • Calixarenes