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In the current paper, we have successfully synthesized three new mercury coordination polymers with fascinating structures and properties via a flexible sulfur donor ligand, namely, {[Hg(μ2-Cl)(μ2-Ls)]} n [BF4] n (1), {[Hg(μ2-Cl)(μ2-Ls)]} n [ClO4] n (2), and [Hg(SCN)2(μ2-Ls)] n (3) [Ls = 1,1-bis(3-methyl-4-imidazoline-2-thione)methane]. These complexes have been characterized by means of different techniques such as single crystal X-ray crystallography, FT-IR, elemental analysis (CHNS), UV-Vis, PXRD, BET, and TGA. Suitable single crystals of all complexes were obtained using the branch tube method with a very high yield and good stability due to the high affinity of mercury to bind to the thione groups. The cationic moieties of polymers 1 and 2 were isostructural, with a HgCl2S2 coordination core structure. The voids of the quasi-hexagonal packing of the columnar chains were occupied by unbonded tetrahedral BF4− ions in 1 and perchlorate anions in polymer 2. Polymer 3 has a less distorted tetrahedral geometry than 1 and 2, with a HgS4 core structure. By considering the thiophilicity of mercury, a thioamide-based Ls ligand was used to detoxify Hg(II) into insoluble polymers 1–3. The results of an MTT assay for (HepG2) liver cells confirmed the excellent cytoprotective effect of this ligand against mercury. Based on IC50 calculations, their toxicity was in order of polymer 1 > polymer 2 > polymer 3. These polymers were also considered as adsorbents for the reversible removal of iodine from solution and the kinetics of the process has been studied in detail. Interestingly, all of them showed an excellent stability and high capacity, in order of 763.53 mg g−1, 877.10 mg g−1, and 905.31 mg g−1 for polymers 1–3, respectively. [ABSTRACT FROM AUTHOR]