Bis adducts of phthalocyaninatoiron(II) with Group 6 axial donor atoms. Crystal and molecular structure of sulphur-bonded bis(dimethyl sulphoxide)phthalocyaninatoiron(II)–dimethyl sulphoxide (1/2)

Abstract

The bis adducts of tetrahydrothiophen (tht) and dimethyl sulphoxide (dmso) with phthalocyaninatoiron(II), [Fe(pc)L2], have been obtained by direct combination of the components. The crystal and molecular structure of the dmso adduct, [Fe(pc)(dmso)2]·2dmso, has been solved by Patterson and Fourier methods. The crystals are monoclinic, space group P21/c, with a= 7,993(2), b= 16.175(7), c= 16.086(7)Å, β= 104.53(3)°, U= 2 013 Å3, Dm(flotation)= 1.45 ± 0.01 g cm–3, Z= 2, Dc= 1.454 g cm–3, R= 0.067 for 1 062 independent reflections. The iron is six-co-ordinated to the four inner nitrogens of the macrocycle and to the sulphur atom of the dmso ligands, with Fe–S 2.308(4), S–O 1.474(14), and Fe–N(average) 1.94 Å. The bonding parameters of the lattice dmso present in the bis adduct have also been determined, S–O 1.443(18)Å. Unsuccessful attempts to prepare some bis adducts with oxygen donors are reported.