Synthetic routes and structures of [Rh(Hdmg){ClZn(C2H5OH)dmg}(PPh3)Cl], [Rh(Hdmg)2(PPh)2]+[Rh(Hdmg)2(Cl)2]−·2CH3OH, and [Rh(Hdmg)2(PPh3)I]·0.5C2H5OH complexes
摘要:
Treatment of [Rh(Hdmg)(2)(PPh3)Cl] with zinc amalgam afforded a heterobimetallic compound [Rh(Hdmg)(ClZndmg)(PPh3)Cl] (1a) (Hdmg=monoanion of dimethylglyoxime). Crystallization of (la) from a CHCl3/C2H5OH mixture led to the formation of [Rh(Hdmg){ClZn(C2H5OH)dmg)(PPh3)Cl] (1). The X-ray crystal structure of 1 revealed that the ethanol molecule was built into the complex molecule through the oxygen atom coordinated to the zinc cation and a hydrogen bond involving one of the chloride ligands. Reduction of [Rh(Hdmg)(2)(PPh3)Cl] with Zn/Hg, followed by treatment with a CHCl3/CH3OH mixture, gave the complex salt [Rh(Hdmg)(2)(PPh3)(2)](+)[Rh(Hdmg)(2)(Cl)(2)](-) . 2CH(3)OH (2). The X-ray structure of 2 showed crystals formed by cations [Rh(Hdmg)(2)(PPh3)(2)](+) and anions [Rh(Hdmg)(2)Cl-2](-). The anion binds one CH3OH molecule through a hydrogen bond involving the adjacent oxime atom. Reduction of [Rh(Hdmg)(2)(PPh3)Cl] with zinc amalgam in the presence of CH3I led to the compound [Rh(Hdmg)(2)(PPh3)I] . 0.5C(2)H(5)OH (3), which was characterized by X-ray crystallography. (C) 2003 Elsevier Ltd. All rights reserved.
Synthetic routes and structures of [Rh(Hdmg){ClZn(C2H5OH)dmg}(PPh3)Cl], [Rh(Hdmg)2(PPh)2]+[Rh(Hdmg)2(Cl)2]−·2CH3OH, and [Rh(Hdmg)2(PPh3)I]·0.5C2H5OH complexes
摘要:
Treatment of [Rh(Hdmg)(2)(PPh3)Cl] with zinc amalgam afforded a heterobimetallic compound [Rh(Hdmg)(ClZndmg)(PPh3)Cl] (1a) (Hdmg=monoanion of dimethylglyoxime). Crystallization of (la) from a CHCl3/C2H5OH mixture led to the formation of [Rh(Hdmg){ClZn(C2H5OH)dmg)(PPh3)Cl] (1). The X-ray crystal structure of 1 revealed that the ethanol molecule was built into the complex molecule through the oxygen atom coordinated to the zinc cation and a hydrogen bond involving one of the chloride ligands. Reduction of [Rh(Hdmg)(2)(PPh3)Cl] with Zn/Hg, followed by treatment with a CHCl3/CH3OH mixture, gave the complex salt [Rh(Hdmg)(2)(PPh3)(2)](+)[Rh(Hdmg)(2)(Cl)(2)](-) . 2CH(3)OH (2). The X-ray structure of 2 showed crystals formed by cations [Rh(Hdmg)(2)(PPh3)(2)](+) and anions [Rh(Hdmg)(2)Cl-2](-). The anion binds one CH3OH molecule through a hydrogen bond involving the adjacent oxime atom. Reduction of [Rh(Hdmg)(2)(PPh3)Cl] with zinc amalgam in the presence of CH3I led to the compound [Rh(Hdmg)(2)(PPh3)I] . 0.5C(2)H(5)OH (3), which was characterized by X-ray crystallography. (C) 2003 Elsevier Ltd. All rights reserved.