| Summary: | Three new supramolecular coordination polymers, namely [Zn(1,3-BDC)(HL)]<i><sub>n</sub></i> (Polymer 1), [Zn<sub>3</sub>(1,3,5-BTC)<sub>2</sub>(HL)<sub>2</sub>(H<sub>2</sub>O)<sub>2</sub>]<i><sub>n</sub></i> (Polymer 2), and [Zn<sub>9</sub>(5-SO<sub>3</sub>-1,3-BDC)<sub>2</sub>(L)<sub>8</sub>(OH)<sub>4</sub>]<sub>n</sub> (Polymer 3), were synthesized under solvothermal conditions, based on 1H-pyrazolo[3,4-b]pyridin-3-amine (HL) along with 1,3-benzenedicarboxylate (1,3-BDC) and its derivatives, such as 1,3,5-benzenetricarboxylate (1,3,5-BTC) and 5-sulfo-1,3-benzenedicarboxylate (5-SO<sub>3</sub>-1,3-BDC). Polymers 1–3 were characterized by elemental analysis, IR spectroscopy, powder X-ray diffraction (PXRD), and single crystal X-ray diffraction analysis. Polymer 1 exhibited a two-dimensional (2D) 4-connected sql net. The neighboring 2D nets were further linked into a 3D supramolecular network by hydrogen-bonding interactions. Polymer 2 displayed a 3D (4, 4, 4)-connected network, which was further stabilized by <inline-formula> <math display="inline"> <semantics> <mrow> <msubsup> <mi>R</mi> <mn>2</mn> <mn>2</mn> </msubsup> </mrow> </semantics> </math> </inline-formula>(14) and S(9) hydrogen-bonding rings along with π–π interactions. The 2D sheet structure of Polymer 3 was constructed by novel quasi-linear nonanuclear Zn(II) units, which further extended into a 3D supramolecular structure by hydrogen-bonding interactions. The solid-state photoluminescence properties of Polymers 1–3 were also investigated.
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