| Summary: | The new coordination polymers (CPs) [Zn(tr<sub>2</sub>ad)Cl<sub>2</sub>]<i><sub>n</sub></i>, {[Cu(tr<sub>2</sub>ad)Cl]Cl∙4H<sub>2</sub>O}<i><sub>n</sub></i>, [Cd<sub>2</sub>(tr<sub>2</sub>ad)Cl<sub>4</sub>]<i><sub>n</sub></i>, {[Cu(tr<sub>2</sub>ad)(NO<sub>3</sub>)](NO<sub>3</sub>)}<i><sub>n</sub></i> and {[Cd(tr<sub>2</sub>ad)(NO<sub>3</sub>)](NO<sub>3</sub>)∙H<sub>2</sub>O}<i><sub>n</sub></i> were obtained in the form of air- and moisture-stable microcrystalline powders by the solvothermal reactions of zinc(II), copper(II) and cadmium(II) chlorides or nitrates with the ligand 1,3-bis(1,2,4-triazol-4-yl)adamantane (tr<sub>2</sub>ad). Investigation of the thermal behaviour assessed the thermal stability of these CPs, with [Cd<sub>2</sub>(tr<sub>2</sub>ad)Cl<sub>4</sub>]<i><sub>n</sub></i> starting to decompose only around 365 °C. As retrieved by powder X-ray diffraction, while [Zn(tr<sub>2</sub>ad)Cl<sub>2</sub>]<i><sub>n</sub></i> features 1-D chains along which the metal centre shows a tetrahedral geometry and the spacer is exo-bidentate, the other CPs contain 2-D double-layers in which the metal ions possess an octahedral stereochemistry and the linker is exo-tetradentate. A comparative structural analysis involving known coordination compounds containing the tr<sub>2</sub>ad ligand enabled us to disclose (i) the versatility of the ligand, as far as the coordination modes are concerned; (ii) the variability in crystal structure dimensionality, ranging from 1-D to 3-D; (iii) the fact that, to the best of our knowledge, [Zn(tr<sub>2</sub>ad)Cl<sub>2</sub>]<i><sub>n</sub></i> is the first Zn<sup>II</sup>-based CP containing the tr<sub>2</sub>ad spacer.
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