Iridium chloride hydrate

Thin-film surfaces were prepared by using the solution deposition technique on a polycrystalline Ir pellet (ACI alloy, 6 mm diameter, 6 mm thickness, 99.99% purity). Iridium chloride hydrate (Alfa aesar, 99.9%) 0.03 μmol, osmium chloride hydrate (Alfa aesar, 99.99%) 0.09 μmol and ruthenium chloride hydrate (Sigma-Aldrich, 99.98%) 0.09 μmol were employed as the metal sources. The final metal deposition process was carried out in the RF furnace in Ar-3%H₂ for 70 s at 1100 °C. Nanocrystals of IrOs alloy were prepared using metal carbonyl precursors. 52 mg of dodecacarbonyltriosmium (Os₃(CO)₁₂, Alfa aesar, 99%) and 47.6 mg of dodecacarbonyltetrairidium (Ir₄(CO)₁₂, Alfa aesar, 98%), and 76.7 μL trioctylphosphine (Sigma-Aldrich, 97%) were introduced into 10 mL oleylamine (Sigma-Aldrich, 70%) in a three neck round bottom flask. The solution was homogenized by stirring for 1 h at 80 °C. Then, the temperature was elevated to 220 °C with N₂ flow. After stirring for an additional 2 h, the reaction was quenched by cooling abruptly to room temperature. The resulting nanoparticles were washed with n-hexane and ethyl alcohol.

All solvents were of analytical grade (>95% purity). All buffer components were of biological grade and used without further purification. Iridium chloride hydrate, ppy, dfppy, H₂dcbpy and NH₄PF₆ were purchased from Alfa Aesar. Cisplatin, rapamycin, DMSO, PLE, PI, NAC, MTT, H₂DCFDA, JC-1, 3-MA, CCCP, CQ, AO and Annexin V-FITC apoptosis detection kit were purchased from Sigma-Aldrich. MTDR was purchased from Invitrogen. Lipofectamine^® 3000 was purchased from Thermo Fisher Scientific. Hoechst 33342 and z-VAD-fmk were purchased from Beyotime. Caspase-Glo^® 3/7 assay kit and CellTiter-Glo^® luminescence cell viability assay kit were purchased from Promega.
Ligands L₁ (dimethyl 2,2′-bipyridine-4,4′-dicarboxylate), L₂ (diethyl 2,2′-bipyridine-4,4′-dicarboxylate), L₃ (dibutyl 2,2′-bipyridine-4,4′-dicarboxylate) and L₄ (diisobutyl 2,2′-bipyridine-4,4′-dicarboxylate) were synthesized according to reported procedures24 . The cyclometalated Ir(III) chloro-bridged dimers [Ir(ppy)₂Cl]₂ and [Ir(dfppy)₂Cl]₂ were prepared according to literature methods57 58 (link). The purity of synthesized complexes was analysed via combustion analysis and was found to be ≥ 95% pure. All the tested complexes were dissolved in DMSO just before the experiments, and the final concentration of DMSO was 1% (v/v).