Hydration of fac-tris(2-phenylpyridinato-C²,N)iridium(III) in dichloromethane solution and in solid state

详细信息    查看全文

• 作者：Satoshi Takayasu¹ ; Kazuteru Shinozaki ; ¹ ; ^{shino@yokohama-cu.ac.jp}
• 关键词：fac-Ir(ppy)3 ; Pseudo-polymorphic crystal ; DOSY 1H NMR ; Hydration ; Non-luminescent water-adduct
• 刊名：Polyhedron
• 出版年：2017
• 出版时间：17 February 2017
• 年：2017
• 卷：123
• 期：Complete
• 页码：328-333
• 全文大小：627 K
• 卷排序：123

文摘

We found a pseudo-polymorphic crystal of fac-tris(2-phenyl pyridinato-C2,N)iridium(III) (fac-Ir(ppy)3) and hydration of fac-Ir(ppy)3 in dichloromethane. Slow evaporation of solvent from dichloromethane solution containing fac-Ir(ppy)3 gave a dark yellow crystal having six waters of crystallization, which were confirmed by FTIR and thermogravimetric analysis (TGA). The hydration of fac-Ir(ppy)3 was found to proceed slowly in wet dichloromethane containing ∼1 × 10−2 M. With increasing the water content in dichloromethane, the signal at ∼1.5 ppm in 1H NMR was split into two peaks, which were assigned to water molecules in bulk solvent and that in hydrated fac-Ir(ppy)3, respectively, from the measurement of diffusion coefficient (D) using the DOSY technique. Two water molecules were determined to attach to fac-Ir(ppy)3 in wet CH2Cl2.