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Axially substituted tin phthalocyanines, namely dichloride-tetra-(α-pentyloxy) tin (IV) phthalocyanine 2, dihydroxy-tetra-(α-pentyloxy) tin (IV) phthalocyanine 3 and its dimmer di-μ-oxo-tetra-(α-pentyloxy) tin(IV) phthalocyanine 4 were synthesized. The catalytic effect of H2O-free CaCl2 in quinoline was used for condensation of dihydroxy tin phthalocyanine 3 to the cofacially array dimmer 4. Their structures were characterized by UV-vis, IR, elemental analysis, MS, as well as 1HNMR spectroscopy.