We report the syntheses of the dimeric homonuclear Pcs 9a and 9b and of the dimeric heteronuclear Pc 9c, starting from the unsymmetrical phthalocyanines 7a and 7b, each containing a phenolic OH group in one of its substituents. Compounds 9a and 9b were obtained by single-step alkylations of 7a and 7b with 1,6-dibromohexane or, in better yields, by coupling of Pcs 7a and 7b with the bromoalkyl-derivatized Pcs 8a and 8b, while 9c was prepared by treatment of 8a with Pc-Ni complex 7b. The dimeric Pcs 9a-9c show strong cofacial intramolecular association in solution. ((C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007).