Carmona Daniel, Lamata Pilar, Sánchez Antonio, Pardo Pilar, Rodríguez Ricardo, Ramírez Paola, Lahoz Fernando J, García-Orduña Pilar, Oro Luis A
Instituto de Síntesis Química y Catálisis Homogénea (ISQCH), CSIC - Universidad de Zaragoza, Departamento de Química Inorgánica, Pedro Cerbuna 12, 50009 Zaragoza, Spain.
Dalton Trans. 2014 Nov 7;43(41):15546-59. doi: 10.1039/c4dt02171a.
Complexes of the formula [(η(n)-ring)M(NOH){(R)-P1}][SbF6]2 ((η(n)-ring)M = (η(5)-C5Me5)Rh, (η(5)-C5Me5)Ir, (η(6)-p-MeC6H4iPr)Ru; NOH = hydroxymethylpyridine ligand; {(R)-P1} = (R)-monophos) have been prepared from the corresponding dimers [{(η(n)-ring)MCl}2(μ-Cl)2] through routes involving [(η(5)-C5Me5)RhCl2{(R)-P1}] or [(η(n)-ring)MCl(NOH)][SbF6] intermediates. The new complexes have been characterized by analytical and spectroscopic means, including the determination of the crystal structures of [(η(5)-C5Me5)IrCl2{(R)-P1}] (1b), [(η(6)-p-MeC6H4iPr)RuCl(NOH-1)][SbF6] (2c), [(η(5)-C5Me5)IrCl{(R)-NOH-2}][SbF6] ((R)-3b), [(η(5)-C5Me5)Rh(NOH-1){(R)-P1}][SbF6]2 (4a) and [(η(6)-p-MeC6H4iPr)Ru{(R)-NOH-2}{(S)-P1}][SbF6]2 ((R)-5c') by X-ray diffractometric methods. From NMR and X-ray data, the absolute configuration of the new chiral compounds was established.
式为[(η(n)-环)M(NOH){(R)-P1}][SbF6]2的配合物（(η(n)-环)M = (η(5)-C5Me5)Rh、(η(5)-C5Me5)Ir、(η(6)-对甲基苯异丙基)Ru；NOH = 羟甲基吡啶配体；{(R)-P1} = (R)-单膦）已通过涉及[(η(5)-C5Me5)RhCl2{(R)-P1}]或[(η(n)-环)MCl(NOH)][SbF6]中间体的路线，由相应的二聚体[{(η(n)-环)MCl}2(μ-Cl)2]制备得到。这些新配合物已通过分析和光谱手段进行了表征，包括通过X射线衍射法测定[(η(5)-C5Me5)IrCl2{(R)-P1}] (1b)、[(η(6)-对甲基苯异丙基)RuCl(NOH-1)][SbF6] (2c)、[(η(5)-C5Me5)IrCl{(R)-NOH-2}][SbF6] ((R)-3b)、[(η(5)-C5Me5)Rh(NOH-1){(R)-P1}][SbF6]2 (4a)和[(η(6)-对甲基苯异丙基)Ru{(R)-NOH-2}{(S)-P1}][SbF6]2 ((R)-5c')的晶体结构。根据核磁共振和X射线数据，确定了新的手性化合物的绝对构型。
