Ligand-coupling assembly of Re(i)-thiolate complexes†
By taking advantage of solvothermal reactions of Re2(CO)10 with 2-mercaptobenzothiazol (HNS2) or 2-mercaptobenzoxazol (HNOS), a series of Re(I) complexes (1–4) with in situ ligands were synthesized and structurally characterized by X-ray diffraction. In this study, we examined the effects of reaction conditions (i.e., reaction solvents and temperatures) on the HNS2 system to give complexes 1–3, and also compared the reaction products of the HNS2 (2) and HNOS (4) systems under similar reaction conditions. For the HNS2 system, the reaction temperatures at 140 and 120 °C in mesitylene led to different ligands in complexes 1 and 2, respectively. However, at the same temperature of 140 °C, different solvents (mesitylene or benzene) caused the formation of complexes 1 and 3 containing different ligands, respectively. Although the same temperature and solvent were used, HNS2 and HNOS underwent a similar in situ ligand reaction in dinuclear complexes 2 and 4, which surprisingly show both anti and syn conformations, respectively.