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The design and synthesis of new metal–organic frameworks (MOFs) is important from both a fundamental and application standpoint. In this work, a novel, highly‐connected rare‐earth (RE) MOF with shp topology is reported, named RE‐CU‐10 (RE = rare‐earth, CU = Concordia University), comprised of nonanuclear RE(III)‐cluster nodes and tetratopic pyrene‐based linkers. This represents the first time that the 1,3,6,8‐tetrakis(p‐benzoic acid)pyrene (H4TBAPy) linker is integrated in the shp topology. Y‐CU‐10 was explored as a heterogeneous photocatalyst for the selective oxidation and detoxification of a sulfur mustard simulant, 2‐chloroethyl ethyl sulfide (2‐CEES), showing a halflife for conversion to the less toxic 2‐chloroethyl ethyl sulfoxide (2‐CEESO) of 6.0 min.