The synthesis of a novel carboxylate-type organic linker-based luminescent MOF (Zn(H₂L) (L₁)) (named PUC2) (H₂L = 2-aminoterephtalic acid, L₁ = 1-(3-aminopropyl) imidazole) is reported by the solvothermal method and comprehensively characterized using single-crystal XRD, PXRD, FTIR, TGA, XPS, FESEM, HRTEM, and BET. PUC2 selectively reacts with nitric oxide (^▪NO) with a detection limit of 0.08 µM, and a quenching constant (0.5 × 10⁴ M⁻¹) indicating a strong interaction with ^▪NO. PUC2 sensitivity remains unaffected by cellular proteins or biologically relevant metals (Cu²⁺/ Fe³⁺/Mg²⁺/ Na⁺/K⁺/Zn²⁺), RNS/ROS, or H₂S to score ^▪NO in living cells. Lastly, we used PUC2 to demonstrate that H₂S inhibition increases ^▪NO production by ~ 14–30% in various living cells while exogenous H₂S suppresses ^▪NO production, indicating that the modulation of cellular ^▪NO production by H₂S is rather generic and not restricted to a particular cell type. In conclusion, PUC2 can successfully detect ^▪NO production in living cells and environmental samples with considerable potential for its application in improving the understanding of the role of ^▪NO in biological samples and study the inter-relationship between ^▪NO and H₂S.

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