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Layered heterometallic 5f–3d uranyl phosphonates can exhibit unique luminescent and/or magnetic properties, but the fabrication and properties of their 2D counterparts have not been investigated. Herein we report three heterobimetallic uranyl phosphonates, namely, [(UO2)3M(2‐pmbH)4(H2O)4] ⋅ 2H2O [MU, M=Co(II), CoU; Mn(II), MnU; Zn(II), ZnU; 2‐pmbH3=2‐(phosphonomethyl)benzoic acid]. They are isostructural...