A new calcium(II) complex was synthesized by one-pot synthesis method from disodium 4-formylbenzene-1,3-disulfonate, isonicotinic acid hydrazide and Ca(ClO4)2•2H2O. The structure of calcium(II) complex was determined by elemental analysis, IR and single crystal X-ray diffraction. The results show that the Ca(II) complex molecules form 3D network structure by the interactions of π-π stacking and hydrogen bonds. The Ca(II) complex catalyst could efficiently catalyse oxidation of benzylic alcohol with good conversion of benzyl alcohol (78 %) and excellent selectivity of benzaldehyde (98 %).Copyright © 2018 BCREC Group. All rights reserved. Received: 13rd December 2017; Revised: 23rd May 2018; Accepted: 23rd May 2018 How to Cite: Tai, X.S., Li, P.F., Liu, L.L. (2018). Synthesis, Crystal Structure, and Catalytic Activity of a Calcium(II) Complex with 4-Formylbenzene-1,3-disulfonate-isonicotinic Acid Hydrazone. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (3): 429-435 (doi:10.9767/bcrec.13.3.1961.429-435) Permalink/DOI: https://doi.org/10.9767/bcrec.13.3.1961.429-435