| Summary: | The influence of arene/perfluoroarene ratio on the structure and crystal packing of carboxylate and nitrate-carboxylate complexes of Cd, Cd-Tb and Cu was studied, using the following compounds: pentafluorobenzoate (pfb) and 4-allyl-2,3,5,6-tetrabenzoate (Afb) anions and 1,10-phenanthroline (phen) composition [Cd(pfb)<sub>2</sub>(phen)]<sub>n</sub> (<b>1</b>), [Cd(NO<sub>3</sub>)(pfb)(phen)]<sub>n</sub> (<b>2</b>), [Tb<sub>2</sub>Cd<sub>2</sub>(pfb)<sub>10</sub>(phen)<sub>2</sub>]. 3MeCN]<sub>n</sub> (<b>3</b>), [Tb<sub>2</sub>Cd<sub>2</sub>(NO<sub>3</sub>)<sub>2</sub>(pfb)<sub>8</sub>(phen)<sub>2</sub><sup>.</sup>1.5MeCN]<sub>n</sub> (<b>4</b>), [Cu<sub>2</sub>(Afb)<sub>4</sub>(phen)<sub>2</sub>] (<b>5</b>), [Cu<sub>2</sub>(NO<sub>3</sub>)<sub>2</sub>(Afb)<sub>2</sub>(phen)<sub>2</sub>] (<b>6</b>). It is shown that the main contribution to the stabilization of the crystal packing of coordination polymers <b>1–4</b> and molecular binuclear complexes <b>5</b> and <b>6</b> can be attributed to non-covalent π···π, C-H···F, and C-F···π interactions. It was found that the partial exchange of pfb or Afb anions on compact NO<sub>3</sub><sup>−</sup> anions leads to a decrease in steric hindrance, a more efficient overlap of aromatic fragments, and a significant change in the geometry of complexes. Synthesized compounds were characterized by X-ray diffraction analysis, IR spectroscopy, and CHN analysis. The thermal stability of complexes <b>1</b> and <b>2</b> was studied. Non-covalent interactions were analyzed using the Hirshfeld surface method.
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