Abstract: | Two new metal–organic frameworks (MOFs), namely, three‐dimensional polydiaquabis{μ2‐1,4‐bis(2‐methyl‐1H‐imidazol‐1‐yl)methyl]benzene}bis(μ2‐glutarato)dinickel(II)] monohydrate], {Ni2(C5H6O4)2(C16H18N4)2(H2O)2]·H2O}n or {Ni2(Glu)2(1,4‐mbix)2(H2O)2]·H2O}n, ( I ), and two‐dimensional poly{μ2‐1,4‐bis(2‐methyl‐1H‐imidazol‐1‐yl)methyl]benzene}(μ2‐glutarato)zinc(II)] tetrahydrate], {Zn(C5H6O4)(C16H18N4)]·4H2O}n or {Zn(Glu)(1,4‐mbix)]·4H2O}n ( II ), have been synthesized hydrothermally using glutarate (Glu2?) mixed with 1,4‐bis(2‐methyl‐1H‐imidazol‐1‐yl)methyl]benzene (1,4‐mbix), and characterized by single‐crystal X‐ray diffraction, IR and UV–Vis spectroscopy, powder X‐ray diffraction, and thermogravimetric and photoluminescence analyses. NiII MOF ( I ) shows a 4‐connected 3D framework with point symbol 66, but is not a typical dia network. ZnII MOF ( II ) displays a two‐dimensional 44‐ sql network with one‐dimensional water chains penetrating the grids along the c direction. The solid‐state photoluminescence analysis of ( II ) was performed at room temperature and the MOF exhibits highly selective sensing toward Fe3+ and Cr2O72? ions in aqueous solution. |