A screening approach based on NMR spectroscopy for metal complexes with triazolylquinoxaline ligands has been developed to support the systematic investigation of metal complexation for selected examples. The formation of homoleptic complexes with different metals and the triazolylquinoxaline as the lone organic ligand and of heteroleptic complexes with an additional phosphine ligand was successfully investigated using this methodology. Selected complexation reactions were reproduced in batches, and the structures of the obtained complexes were confirmed via single-crystal X-ray diffraction, showing the versatility of the employed ligand in monodentate, chelating, and bridging complexes. Additional computations allowed for an increased understanding of the experimentally observed properties and enabled in-silico predictions for similar compounds prior to their synthesis. In combination with the observed shifts of