One-dimensional (1D) coordination polymer, [Zn(4,4´-bpy)(H2O)4](ADC).4H2O (1) (4,4´-bpy = 4,4´-bipyridine and H2ADC = acetylenedicarboxylic acid), and three-dimensional (3D) metal-organic framework (MOF), Zn(ADC)2.(HTEA)2(2) (HTEA = triethylamine) were prepared at room temperature. The compounds were characterized by single-crystal X-ray diffraction and powder X-ray diffraction (PXRD) analyses. The polymers were applied as precursors for the synthesis of ZnO nanocrystals via direct thermal decomposition. The prepared nanocrystals were characterized by PXRD, scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). It was found that the nanocrystals of different morphologies such as rods and particles were formed using 1 and 2, respectively.