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General Experimental Section ## Materials and Physical Techniques [ n Bu4N]2[Cu II (opba)] (opba = o-phenylenebis(oxamato)), bis(pyrazoly)(3-bromopyridinyl)methane [HC(Pz)2(3-BrPy)] and bis(pyrazoly)(3-pyrazolypyridinyl)methane (PyPz3) were synthesized based on the literature. 1 All other chemicals and reagents were commercially available and used without further purification. All synthesis was carried out under Ar atmosphere unless stated otherwise. FT-IR spectra was recorded in the range 600-4000 cm -1 on a Bruker tensor II spectrophotometer. Elemental analyses (C, H, N) were measured using an Elemental vario EL analyser. Powder X-ray Diffraction (PXRD) measurements were recorded on a Rigaku Smartlab X-ray diffractometer. The high resolution mass spectra were obtained using Thermo Scientific Q Exactive mass spectrometer in the positive ion mode. Magnetic measurements were carried out with a SQUID MPMS3 magnetometer. Dc magnetic susceptibility data were collected under 1000 Oe dc field over the temperature range 2-300 K. Dc magnetization data were collected in the temperature range of 2-5 K with dc fields from zero to 7 T. Ac magnetic susceptibility data were collected using a 3 O

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American Chemical Society (ACS)