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Two 2D 3d‐4f heterometallic coordination polymers, [Ln2Cu4Br3(IN)6(OH)(H2O)4]n [Ln = Ho (1) and Yb (2), HIN = isonicotinic acid], were synthesized by hydrothermal reaction of Ln2O3, CuBr2, and HIN with HNO3, and characterized by elemental analyses, IR spectroscopy, PXRD, and single‐crystal X‐ray diffraction. Structural analyses revealed that 1 and 2 are isostructural and have a 2D structure, which consists [Cu4Br3]nn+ chains linked by dinuclear [Ln2(IN)6(OH)]– clusters. Additionally, the thermogravimetric analysis and luminescent properties of 1 were investigated and discussed.

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