2.10 X-ray crystallographic studies

2.10 X-ray crystallographic studies Single crystals of 1-6, 7a, 7b and 8a suitable for X-ray diffraction analysis were grown by slow diffusion of CH2Cl2 solution into a hexane solution at room temperature. The X-ray diffraction data were collected on a Bruker SMART-1000 CCD diffractometer with graphite-monochromated Mo Kα (λ = 0.71073 Å) radiation at room temperature. The structures were solved by direct methods [47] and refined by the full-matrix least-squares methods on F2 using the SHELX-2018 program [48]. PLATON/SQUEEZE was used to correct the data for the presence of disordered solvent [49]. All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were generated geometrically and refined using riding mode. Crystal data and experimental details of the structure determinations are listed in Tables S1 and S2. For complex 7b and 8a, although every effort was made to grow the best possible crystals, a thin platelet was chosen in order to obtain a single crystal, and this did not diffract well to higher angles, and thus corresponding diffraction data were poor. 2.11 Electrochemical Test Electrochemical measurements were carried out under nitrogen using a CHI 620 Electrochemical Work station. As the electrolyte, n-Bu4NPF6 was recrystallized multiple times from a CH2Cl2 solution by the addition of hexane. CV scans were obtained in a three-electrode cell with a glassy carbon electrode (3 mm diameter) as the working electrode, a platinum wire as the counter electrode, and a nonaqueous Ag/Ag+ electrode as the reference electrode. The potential scale was calibrated against the Fc/Fc+ couple and reported versus this reference system.3. RESULTS and DISCUSSION 3.1 Synthesis and characterization of parent complexes 1-3 Scheme 1Page 9 of 39John Wiley & Sons