Similar to the NMR experiment, the bulk of the complex precipitated but was still soluble enough to be detected by H NMR. Suitable crystals were grown from a solution in DMSO through slow evaporation of the solvent under a high vacuum, allowing the elucidation of the product structure via single-crystal X-ray crystallography. The obtained metallacycle consists of two triazolylquinoxaline ligands, two silver atoms, and four nitrate ligands (see Scheme 2). The N3atom of the triazole and the pyrazine nitrogen each coordinate to a silver atom, linking the dimer in an almost planar configuration. The complex crystallizes in the monoclinic space group P21/n with N-Ag bond lengths of 2.309 and 2.310 Å, only slightly longer than for reported dimeric benzotriazole analogues. 17 between the nitrogen and metal center are analogous to the results obtained for a CH2-spaced complex reported in the literature. For PdCl2 and RuCl3, no suitable single crystals could be grown from the precipitated reaction mixture in the batch experiment. Due to the low solubility of the palladium complex, no conclusion regarding the complexation mode could be drawn from the NMR data. Nevertheless, the obtained mass data indicates the formation of a dimeric complex with two involved triazolylquinoxaline ligands similar to literature-reported benzotriazole palladium complexes. For the ruthenium complex, a trimeric complex with three ligand molecules and one central ruthenium atom is assumed to be present in analogy to the literature. The assumed complexation through the triazole nitrogen is supported by the downfield shift of the proton linked to the triazole in the 1 H NMR spectrum, similar to the other complexes (see also was employed, following previous reports on heteroleptic Cu(I) and Ag(I) complexes. The solutions were shaken for 20-30 min, then a solution of the triazolylquinoxaline ligand was added, and the mixture was shaken for another 20-30 min before the 1 H NMR measurement was conducted. A successful complexation of the triazolylquinoxaline ligand was observed for all the combinations (see Table and Figure ), again indicated by the shift of the aromatic signals of the quinoxaline and, most remarkably, the triazole hydrogen atom. The spectra for experiments with ligands 5a and 5b-e are respectively given in Figure and in the Supporting Information section