A Tb(iii)-based coordination polymer (polyTb) was synthesized by complexation of Tb(NO3)3·(6H2O) and 4',4''''-[1,1'-biphenyl]-4,4'-diylbis[6,6''-bis(ethoxycarbonyl)2':6',2''-terpyridine](L). The polymer structure was determined by Job's plots, DFT calculation, and X-ray absorption fine structure (XAFS) measurement. Job's plots indicated that the mole ratio (Tb ion : L) is 1 : 1. The optimized model structures suggested a La model: the LaN6(O[double bond, length as m-dash]C)2 model. The bond distances of La-O and La-N are ∼2.80 Å and 2.60 Å, respectively. The EXAFS fitting indicated that the bond distances of Tb-O and Tb-N are 2.65 Å and 2.95 Å, respectively. polyTb shows field-induced magnetic relaxation in the solid and solution state. The luminescence of polyTb, originating from an f-f transition, was observed (φ = 6.9%). polyTb formed a porous structure on a Si substrate, whereas a fibrous complex structure was formed on glass. polyTb chains are orientated on glass, which were determined by XRD.
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