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The simultaneous use of 2-pyridyl oximes (pyridine-2 amidoxime, H₂pyaox; 2-methyl pyridyl ketoxime, Hmpko) and 1,3,5-benzenetricarboxylic acid (H₃btc) provided access to five new compounds, namely [Zn(H₂btc)₂(H₂pyaox)₂]•2H₂O (<b>1</b>•2H₂O), [Zn(Hbtc)(H₂pyaox)₂]_n (<b>2</b>), [Cu(Hbtc)(H₂pyaox)]_n (<b>3</b>), [Cu(Hbtc)(HmpKo)]_n (<b>4</b>) and [Cu₂(Hbtc)₂(Hmpko)₂(H₂O)₂]•4H₂O (<b>5</b>•4H₂O). Among them, <b>3</b> is the first example of a metal-organic framework (MOF) containing H₂pyaox. Its framework can be described as a 3-c uninodal net of <b>hcb</b> topology with the layers being parallel to the (1,0,1) plane. Furthermore, <b>3</b> is the third reported MOF based on a 2-pyridyl oxime in general. <b>2</b> and <b>4</b> are new members of a small family of coordination polymers containing an oximic ligand. <b>1–5</b> form 3D networks through strong intermolecular interactions. Dc magnetic susceptibility studies were carried out in a crystalline sample of <b>3</b> and revealed the presence of weak exchange interactions between the metal centres; the experimental data were fitted to a theoretical model with the fitting parameters being <i>J</i> = −0.16(1) cm⁻¹ and <i>g</i> = 2.085(1). The isotropic <i>g</i> value was also confirmed by electronic paramagnetic resonance (EPR) spectroscopy. Reactivity studies were performed for <b>3</b> in the presence of metal ions; the reaction progress was studied and discussed for Fe(NO₃)₃ by the use of several characterization techniques, including single crystal X-ray crystallography and IR spectroscopy.