Vilsmeier formylation of the oporphyrin-I tetraethyl ester Ni-complex (III) followed by reduction of the intermediary imine salt (IV) with NaBH4 gave the o-dimethylaminomethyl-coproporphyrin-I Ni-complex (V). Heating the latter in methyl iodide gave 65% of the ethane- bis-porphyrin (I), which has been characterized by NMR-spectroscopy and a molecular and crystal structure investigation. The crystal structure shows an extended structure of the bisporphyrin with a parallel arrangement of the porphyrin subunits. Crystal data: I - C90H106N8Ni2O16. Triclinic, a = 12.319(3) Å. b = 13.297(3) Å, c = 14.444(3) Å, α = 105.56(2)°, β = 100.82(2)°, γ = 112.98(2)°, V = 1981.0(7) Å3, Cu Kα radiation, λ = 1.54178 Å, space group P1̄, Z = 1, R = 0.07.
© 1946 – 2014: Verlag der Zeitschrift für Naturforschung
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.