| Summary: | Two multi-dentate nitronyl nitroxide radicals, namely, bisNITPhPy ([5-(4-pyridyl)-1,3-bis(1′-oxyl-3′-oxido-4′,4′,5′,5′-tetramethyl-4,5-hydro-1<i>H</i>-imidazol-2-yl)]benzene) and NIT-3Py-5-4Py (2-{3-[5-(4-pyridyl)]pyridyl}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide), were assembled with Cu<sup>II</sup> ions to obtain two-dimensional heterospin 2p–3d coordination polymers [Cu<sub>7</sub>(hfac)<sub>14</sub>(bisNITPhPy)<sub>2</sub>]<sub>n</sub> (<b>1</b>) and [Cu<sub>2</sub>(hfac)<sub>4</sub>(NIT-3Py-5-4Py)]<sub>n</sub> (<b>2</b>) (hfac: hexafluoroacetylacetonate). In both compounds, the bisNITPhPy and NIT-3Py-5-3Py radicals acted as pentadentate and tetradentate ligands, respectively, to connect with Cu<sup>II</sup> ions, generating a 2D layer structure. The analysis of the magnetic behavior indicated that strong antiferromagnetic coupling and ferromagnetic interaction (<i>J</i> = 17.1 cm<sup>−1</sup>) coexisted in <b>1</b>. For <b>2</b>, there were ferromagnetic couplings between the Cu<sup>II</sup> ion and NO group, as well as the Cu<sup>II</sup> ion and radical via the pyridine ring with <i>J</i><sub>1</sub> = 32.8 and <i>J</i><sub>2</sub> = 2.2 cm<sup>−1</sup>, respectively.
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