High-Throughput Small-Molecule Crystallography at the ‘Belok’ Beamline of the Kurchatov Synchrotron Radiation Source: Transition Metal Complexes with Azomethine Ligands as a Case Study

Abstract

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.

Heptanuclear Cage CuII‐Silsesquioxanes: Synthesis, Structure and Catalytic Activity

“…X‐ray diffraction data for 1 were collected with a Bruker APEX II CCD diffractometer using graphite monochromated Mo‐ K α radiation at the center for molecular composition studies of INEOS RAS. X‐ray diffraction data for 2 and 2a were collected at the “Belok” beamline ( λ = 0.96990 Å) of the Kurchatov Synchrotron Radiation Source. In total, 480–720 frames were collected with an oscillation range of 1.0° in the φ ‐scanning mode using two different orientations for each crystal.…”

Dichloro‐Substituted 1,2‐Diazabuta‐1,3‐dienes as Highly Reactive Electrophiles in the Reaction with Amines and Diamines: Efficient Synthesis of α‐Hydrazo Amidinium Salts

“…The single‐crystal X‐ray diffraction data for 2a , 6b′ , 6b , 6d′ and 8c were collected with the “Belok” beamline of the National Research Center “Kurchatov Institute” (Moscow, Russian Federation) using a Rayonix SX165 CCD detector . In total, 720 frames were collected with an oscillation range of 1.0° in the φ scanning mode, using two different orientations for each crystal.…”

Belok/XSA Diffraction Beamline for Studying Crystalline Samples at Kurchatov Synchrotron Radiation Source

“…More detailed description of diffractometer parameters can be found elsewhere. [ 2 ] New beamline is located on a bending magnet of the Siberia‐2 storage ring. The average current is 100 mA, 24 bending magnets with an electron rotation radius of 4.9054 m and a magnetic field of 1.7 T are used as sources of synchrotron radiation.…”

“…That makes possible to use direct geometry ( θ = 0°), eliminating probable errors that appear during work with oblique geometry ( θ = 15°), allows to collect complete diffraction set from one crystal orientation with symmetry above triclinic and provides apparent resolution as it was at “Belok” beamline in oblique geometry. [ 2 ]…”