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A new Cd(II) coordination polymer, {[Cd 3 (L) 2 (DMF) 2 (H 2 O) 2 ]·H 2 O}n (H 2 L = 1,3-bisbenzyl-2-imidazolidine-4,5-dicarboxylic acid) was synthesized by one-pot synthesis method from 1,3-bisbenzyl-2-imidazolidine-4,5-dicarboxylic acid, NaOH, DMF, and Cd(NO 3 ) 2 ·4H 2 O. Its structure was determined by elemental analysis and single crystal X-ray diffraction. Structural analysis shows that three Cd(II) ions are all six-coordinated with four oxygen atoms of four 1,3-bisbenzyl-2-imidazolidine-4,5-dicarboxylate ligands and two O atoms from two DMF molecules (Cd1) or two oxygen atoms of two coordinated H 2 O molecules (Cd2 and Cd3) to form an octahedral coordination geometry. The Cd(II) coordination polymer displays a 1D chained structure by the bridging carboxylate groups from 1,3-bisbenzyl-2-imidazolidine-4,5-dicarboxylate ligands. The conversion of benzaldehyde is 90.9%, which is 40~50% higher than those of the other three aldehydes (4-methylbenzaldehyde, p-methoxybenzaldehyde and 3-chlorobenzaldehyde), so the Cd(II) coordination polymer catalyst shows better catalytic activity for the coupling reaction of benzaldehyde, phenylacetylene, and piperidine than the other three aldehydes. Copyright © 2018 BCREC Group. All rights reserved Received: 25 th April 2017; Revised: 11 st September 2017; Accepted: 1 st November 2017; Available online: 11 st June 2018; Published regularly: 1 st August 2018 How to Cite : Ji, Z.X., Li, P.F. (2018). Crystal Structure and Catalytic Activity of A Novel Cd(II) Coordination Polymer Formed by Dicarboxylic Ligand. Bulletin of Chemical Reaction Engineering & Catalysis , 13 (2): 220-226 (doi:10.9767/bcrec.13.2.1178.220-226)