Two coordination polymers of Zn(II) and Cu(II) with n-butylmalonic acid have been achieved in this work. The crystallographic structural descriptions along with the sedimentary rock-type microstructural morphology of these two coordination polymers (CPs) have been explored. The reactivity of beta-hydroxy ketones with these two CPs has also been investigated. The Zn(II)-CP shows a specific reactivity with beta-hydroxy ketone at room temperature and in open air conditions. Through a microcolumn-based filtration technique, the Zn(II)-CP shows the capability to break the C-sp(3)-C-sp(3) sigma bonds of beta-hydroxy ketone and simultaneously reduce the associated ketone to alcohol. Such conversion has been progressed without the use of any additional external reducing agent and any chemical workup or column chromatographic purification protocol. Other similar type CPs of Cu(II) and Mn(II) with n-butylmalonic acid completely failed to show similar reactivity with beta-hydroxy ketone. On the basis of much experimental evidence, the most possible mechanistic pathway of the reactivity between beta-hydroxy ketone and Zn(II)-CP has also been proposed through this work.