| Summary: | Coordination-driven self-assembly is an effective synthetic tool for the construction of spatially and electronically tunable supramolecular coordination complexes (SCCs), which are useful in various applications. Herein, we report the synthesis of a two-dimensional discrete metalla-rectangle [(<i>η</i><sup>6</sup>-<i>p</i>-cymene)<sub>4</sub>Ru<sub>4</sub>(C<sub>6</sub>H<sub>2</sub>O<sub>4</sub>)<sub>2</sub>(<b>2</b>)<sub>2</sub>](CF<sub>3</sub>SO<sub>3</sub>)<sub>4</sub> (<b>3</b>) by the reaction of a dinuclear half-sandwich ruthenium (II) complex [Ru<sub>2</sub>(<i>η</i><sup>6</sup>-<i>p</i>-cymene)<sub>2</sub>(C<sub>6</sub>H<sub>2</sub>O<sub>4</sub>)Cl<sub>2</sub>] (<b>1</b>) and bis-pyridyl amide linker (<b>2</b>) in the presence of AgO<sub>3</sub>SCF<sub>3</sub>. This cationic ruthenium metalla-rectangle (<b>3</b>) has been isolated as its triflate salt and characterized by analytical techniques including elemental analysis, Fourier-transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance spectroscopy (<sup>1</sup>H-NMR), carbon nuclear magnetic resonance spectroscopy (<sup>13</sup>C-NMR), <sup>1</sup>H-<sup>1</sup>H correlation spectroscopy (COSY), <sup>1</sup>H-<sup>1</sup>H nuclear Overhauser effect spectroscopy (NOESY), diffusion ordered spectroscopy (DOSY), and high-resolution electrospray ionization mass spectrometry (HR-ESI-MS). Significantly, the 2D cationic ruthenium metalla-rectangle showed better anticancer activity towards three different cell lines (A549, Caki-1 and Lovo) as compared with the parent ruthenium complex (<b>1</b>) and the commercially used drug, cisplatin.
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