Synthesis and Structures of 1D and 2D ZnGd Coordination Polymers: [ ZnGd (L)( NO 3 ) 2 (4‐ppa)( EtOH )] and [ ZnGd (L)( NO 3 ) 2 (4‐pca)] ( H 2 L = 1,3‐bis((3‐methoxysalicylidene)amino)propane); 4‐Hppa = 4‐pyridinepropionic acid; 4‐Hpca = 4‐pyridinecarboxylic acid

This paper reports the synthesis, crystal structures, and thermal behavior of two zinc–gadolinium (3d–4f) coordination polymers by adjusting the connectivity of a secondary building unit ( SBU ) with two pyridyl–carboxylic acids as linkers. As a SBU , the Zn–Gd compartment compound, [ ZnGd (L)( NO 3 )( CH 3 CN )( H 2 O ) 4 ]( NO 3 ) 2 ( H 2 O ) ( H 2 L  = 1,3‐bis((3‐methoxysalicylidene)amino)propane), was used. Under microwave heating conditions, the SBU reacted with 4‐pyridinepropionic acid (4‐Hppa) and 4‐pyridinecarboxylate (4‐Hpca) to create a 1D polymer, [ ZnGd (L)( NO 3 ) 2 (4‐ppa)( EtOH )], and a 2D polymer, [ ZnGd (L)( NO 3 ) 2 (4‐pca)], respectively. Dimensionality of the products appeared to depend on the continuity of π conjugation of the external linking ligand.