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Synthesis and Crystal Structure of Two iso-closo 11-Vertex p-Bromobenzoate Ruthenoborane Clusters: [(PPh3)(p-BrC6H4CO2)2RUB10H8 and [(PPh3)2Ru(p-BrC6H4CO2)-(PPh3)RuB10H9]

Synthesis and Crystal Structure of Two iso-closo 11-Vertex p-Bromobenzoate Ruthenoborane Clusters: [(PPh3)(p-BrC6H4CO2)2RUB10H8 and [(PPh3)2Ru(p-BrC6H4CO2)-(PPh3)RuB10H9]
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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 ,8=95.11(2)°, Z=8, V=7.622(21) nm^3, Dc=1.533 Mg/m^3, 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, a =90.445(4)°,β=105.950(4)°, γ108.980(4)°, Z=2, V=3.0251(12) nm^3, Dc = 1.434 Mg/m^3, F(000)= 1316, S=1.007, R=0.0464, wR=0.1175, respectively for 1 and 2. In the structures, both of the dusters 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. 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 ,8=95.11(2)°, Z=8, V=7.622(21) nm^3, Dc=1.533 Mg/m^3, 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, a =90.445(4)°,β=105.950(4)°, γ108.980(4)°, Z=2, V=3.0251(12) nm^3, Dc = 1.434 Mg/m^3, F(000)= 1316, S=1.007, R=0.0464, wR=0.1175, respectively for 1 and 2. In the structures, both of the dusters 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.
出处 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2006年第12期1741-1746,共6页 中国化学(英文版)
基金 Project supported by the National Natural Science Foundation of China (No. 20371025).
关键词 ruthenoborane cluster crystal structure para-bromobenzoate metalloborane ruthenoborane, cluster, crystal structure, para-bromobenzoate, metalloborane
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