SYNTHESIS, SOLUTION, MOLECULAR AND CRYSTAL-STRUCTURE OF BIS[5-(COPROPORPHYRINATO-I TETRAETHYLESTER)NICKEL(II)]1,2-ETHANE

Vilsmeier formylation of the oporphyrin-1 tetraethyl ester Ni-complex (III) followed by reduction of the intermediary imine salt (IV) with N aBH4 give the o-dimethylaminomethyl-coproporphyrin-I Ni-complex (V). H eating the latter in methyl iodide gave 65% of the ethane-bis-porphyri n (1), which has been characterized by NMR-spectroscopy and a molecula r 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) Angstrom, b = 13.297(3) Angstrom, c = 14.444(3) Angstrom , alpha = 105.56(2)Angstrom, beta = 100.82(2)degrees, gamma = 112.98(2 )degrees, V = 1981.0(7) A(3), Cu K alpha radiation lambda = 1.54178 An gstrom, space group <P(1)over bar>, Z = 1, R = 0.07.