This paper concisely describes capabilities of the ‘Belok’ beamline at the Kurchatov synchrotron radiation source, related to high-throughput small-molecule X-ray crystallography. As case examples, a series of four novel transition metal complexes with azomethine ligands were selected. The complexes demonstrate somewhat unexpected changes in the coordination geometry and nuclearity in response to the introduction of substituents in the ligand’s periphery.

Data on luminescent complexes with azomethine ligands are generalized and systematized. The synthesis and luminescent properties of complexes with acyclic and cyclic azomethines are considered.

New NIR emitting materials were found among the lanthanide complexes with 2-(tosylamino)benzylidene-N-benzoylhydrazone. Complexes of Nd³⁺, Er³⁺ and Yb³⁺, as well as Eu³⁺, Gd³⁺ and Lu³⁺, were synthesized for the first time. Owing to the absence of vibration quenching the ytterbium complex was found to exhibit a photoluminescence quantum yield of 1.4%. Since the sensitization efficiency was calculated to be 55%, the losses in the quantum yield are probably due to Yb–Yb resonant energy transfer.