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A new dysprosium based Metal-Organic Framework with {[Dy(dhbdc)(DMF)]·DMF} formula has been obtained from solvothermal reaction with 2,5-dihydroxyterephthalic acid ligand and dysprosium chloride. This coordination polymer has been characterized and its crystal structure has been solved by X-ray diffraction methods elucidating a three-dimensional network. Magnetic studies of this compound reveal the existence of weak antiferromagnetic interactions among the metal ions with θ value of −0.26 K. Dynamic ac magnetic susceptibility measurements were carried out under an external dc field of 1 kOe, highlighting that at high frequencies two relaxation processes can be observed. However, when studying the diamagnetically diluted analogue 1, a single relaxation process was detected highlighting the effect of the weak but not negligible exchange interactions. Finally, photoluminescence measurements were performed at different temperatures with the aim of getting a more representative characterization of the emissive performance of the material for potential applications in lighting and thermometry., Financial support was given by Junta de Andalucía (Spain) (project number FQM-394 and FQM-1484), University of the Basque Country (GIU 17/13), Gobierno Vasco/Eusko Jaurlaritza (IT1005-16) and the Spanish Ministry of Economy and Competitiveness (MCIU/AEI/FEDER, UE) (PGC2018-102052-A-C22, PGC2018-102052-B-C21 and CTQ-2015-64049-C3-3R). The authors thank for technical and human support provided by SGIker of UPV/EHU and European funding (ERDF and ESF). A.Z.-L. is grateful to the Government of the Basque Country for the predoctoral fellowship