Synthesis and Crystal Structure of Two iso-closo 11-Vertex ρ-Bromobenzoate Ruthenoborane Clusters: [(PPh3)(ρ-BrC6H4CO2)2RuB10H8] and [(PPh3)2Ru(ρ-BrC6H4CO2)-(PPh3)RuB10H9]

• 来源期刊: 中国化学（英文版）
• 年，卷（期）: 2006,（12）
• 页码范围: 1741-1746
• 页数: 6页
• 语种: 英文

摘要

The title clusters [(PPh3)(p-BrC6H4CO2)2RuB10H8] (1) and [(PPh3)2Ru(PPh3)(p-BrC6H4CO2)RuB10H9] (2) have been prepared and characterized by elemental analysis, FT-IR, 1H, 13C NMR spectra and single-crystal X-ray diffraction analysis. The clusters crystallize in monoclinic system, space group C2/c, with a=2.569(4) nm, b= 1.546(2)nm, c= 1.927(3) nm,β=95.11(2)°, Z=8, V=7.622(21) nm3, Dc=1.533 Mg/m3, F(000)=3472, S= 1.009, R=0.0418, wR=0.0775 and triclinic system, space group P-l, with a= 1.3142(3) nm, b= 1.3761(3) nm, c= 1.8503(4)nm, α =90.445(4)°,β= 105.950(4)°, γ= 108.980(4)°, Z=2, V= 3.0251 (12) nm3, Dc= 1.434 Mg/m3, F(000)= 1316,S= 1.007, R=0.0464, wR=0.1175, respectively for 1 and 2. In the structures, both of the clusters are based on a closo-type C2v 1: 2: 4: 2: 2 RuB10 stack with the metal occupying the unique six-connected apical position. In cluster 1, the metal center has three exo-polyhedral ligands: one triphenylphosphine and two dative oxygen atoms of p-bromobenzoates. The other oxygen atoms of two p-bromobenzoate are additionally bonded to B(2) and B(3) atoms respectively, resulting in two exo-cyclic five-membered Ru-O-C-O-B rings and engendering a symmetrical conformation. The cluster 2 is a bimetallic species in which the second ruthenium is bound to the {RuB10} center via one Ru-Ru bond and two {RuHμB} bridges resulting in one closo distorted exo-polyhedral Ru(1)-Ru(2)-B(3)-B(6) tetrahedron.