5-COD)Rh(μ-Cl)]2, respectively. The synthesis of such well-defined second and third row model precursors is key to determining the true nature of commercial Ziegler-type hydrogenation catalysts (i.e., catalysts made from the combination of a non-zerovalent, group 8−10 transition metal precatalyst and a trialkylaluminum cocatalyst), an unsolved, ∼40 year old problem. The characterizations of 1 and 2 were accomplished
的化合物[(1,5-COD)M(μ-O 2 C ^ 8 ħ 15)] 2(COD =
环辛二烯,M =
铱(1)或Rh(2),O 2 Ç 8 ħ 15 = 2-乙基
己酸)通过将Bu 3 NH(2-乙基
己酸)或Na(2-乙基
己酸)加到[(1,5-COD)Ir(μ-Cl)] 2或[(1,5-COD)的
丙酮悬浮液中来合成Rh(μ-Cl)] 2, 分别。此类定义明确的第二排和第三排模型前体的合成对于确定商业齐格勒型加氢催化剂(即由非零价8-10族过渡
金属预催化剂和六价
铬的组合制成的催化剂)的真实性质至关重要。三烷基铝助催化剂),一个尚未解决的问题,已有40多年的历史了。1和2的表征是通过元素分析,熔点,FAB-MS,FT-IR,UV-vis,NMR光谱和单晶X射线衍射完成的。配合物C 32 H 54 Ir 2 O 4和C 32 H 54 O 4 Rh 2是同构:单斜晶系,P 2 1 / Ñ,Ž = 4晶格常数为1是一个=