Synthesis, crystal structure and spectroscopic characterization of new neutral and cationic (η<sup>6sup>-p-cymene)–ruthenium(II) complexes with phosphine–amide ligands

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• 作者：Gregorio S&#xe1 ; nchez ; Joaqu&#xed ; n Garc&#xed ; a ; Juan J. Aylló ; n ; Jos&#xe9 ; L. Serrano ; Luis Garc&#xed ; a ; Jos&#xe9 ; P&#xe9 ; rez ; Gregorio Ló ; pez
• 关键词：Phosphino-amides ; Hemilabile ligands ; Coordination modes ; (η ; <sup>6sup>-p-cymene) complexes ; Crystal structures ; Ruthenium
• 刊名：Polyhedron
• 出版年：2007
• 期刊代码：87_02775387
• 类别：ch
• 出版时间：23 July 2007
• 卷：26
• 期：12
• 页码：2911-2918
• 文件大小：305 K

摘要

The dimeric starting material [Ru(η<sup>6sup>-p-cymene)(μ-Cl)Cl]<sub>2sub> reacts with the phosphino-amides o-Ph<sub>2sub>P–C<sub>6sub>H<sub>4sub>CO–NH–R [R = <sup>isup>Pr (<strong>astrong>), Ph (<strong>bstrong>), 4-MeC<sub>6sub>H<sub>4sub> (<strong>cstrong>), 4-FC<sub>6sub>H<sub>4sub> (<strong>dstrong>)] to give the mononuclear compounds <strong>1astrong>–<strong>dstrong> [RuCl(η<sup>6sup>-p-cymene)(o-Ph<sub>2sub>P–C<sub>6sub>H<sub>4sub>–CO–NH–R)]Cl. The subsequent reaction of these complexes with KPF<sub>6sub> produced the cationic species <strong>2astrong>–<strong>dstrong> [RuCl(η<sup>6sup>-p-cymene)(o-Ph<sub>2sub>P–C<sub>6sub>H<sub>4sub>–CO–NH–R)][PF<sub>6sub>] in which phosphino-amides also act as rigid P,O-chelating ligands. The molecular structures of <strong>2bstrong>–<strong>dstrong> were determined crystallographically. Amide deprotonation is achieved when complexes <strong>2astrong>–<strong>dstrong> were made react with 1 M aqueous solution of KOH, affording the corresponding neutral species <strong>3astrong>–<strong>dstrong> [RuCl(η<sup>6sup>-p-cymene)(o-Ph<sub>2sub>P–C<sub>6sub>H<sub>4sub>–CO–N–R)] in which a P,N-coordination mode is suggested.