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Synthesis of Platinum Complexes Containing Bidentate N,O-donor Ligands

机译:含双齿N,O供体配体的铂配合物的合成

摘要

The reaction of N,O-donor ligands hippuric acid and N-phenylanthranilic acid with [PtCl₂(COD)] (COD = 1,5-cyclooctadiene) in dichloromethane and in the presence of silver(I) oxide yields the complexes [Pt{OC(O)CH₂N(COPh)}(COD)] and [Pt{OC(O)(C₆H₄)N(Ph)}(COD)]. Several ligand-substitution reactions were performed using complex [Pt{OC(O)CH₂N(COPh)}(COD)] and a variety of phosphines, to produce [Pt{OC(O)CH₂N(COPh)}(PPh₃)₂].1.5.CH₂Cl₂, [Pt{OC(O)CH₂N(COPh)}(dppe)][dppe = 1,2-bis(diphenylphosphino)ethane], [Pt{OC(O)CH₂N(COPh)}(PTA)₂] (PTA = 1,3,5-triaza-7-phosphaadamantane) and [Pt{OC(O)CH₂N(COPh)}(dppf)] [1,1’-bis(diphenylphosphino)ferrocene]. The X-ray crystal structure of [Pt{OC(O)CH₂N(COPh)}(COD)] was obtained which showed the hippurate ligand coordinated to platinum via the nitrogen and oxygen atoms. Attempts were made to synthesise two N,O-coordinated gold(III) complexes, however characterisation showed the resulting products to be a mixture of compounds.All new complexes were characterised by elemental analysis, melting point, electrospray ionisation mass spectrometry (ESI-MS), nuclear magnetic resonance (NMR) and infra-red (IR) spectroscopy. In particular, a range of various 1D (¹H, ¹³C, ³¹P, DEPT and selective NOESY) and 2D (COSY, NOESY, HSQC, HMBC and H2BC) NMR experiments were used to provide full spectral assignment of each complex.
机译:N,O-供体配体马尿酸和N-苯基邻氨基苯甲酸与[PtCl 2(COD)](COD = 1,5-环辛二烯)在二氯甲烷中,在氧化银(I)存在下反应,生成配合物[Pt { OC(O)CH 2 N(COPh)}(COD)]和[Pt {OC(O)(C₆H3)N(Ph)}(COD)]。使用配合物[Pt {OC(O)CH 2 N(COPh)}(COD)]和多种膦进行了几次配体取代反应,生成了[Pt {OC(O)CH 2 N(COPh)}(PPh 3)2]。 .1.5.CH 2 Cl 2,[Pt {OC(O)CH 2 N(COPh)}(dppe)] [dppe = 1,2-双(二苯基膦基)乙烷],[Pt {OC(O)CH 2 N(COPh)}(PTA) 22](PTA = 1,3,5-三氮杂-7-膦金刚烷)和[Pt {OC(O)CH 2 N(COPh)}(dppf)] [1,1′-双(二苯基膦基)二茂铁]。得到了[Pt {OC(O)CH 2 N(COPh)}(COD)]的X射线晶体结构,该结构表明马来酸酯配体通过氮和氧原子与铂配位。尝试合成了两种N,O配位的金(III)配合物,但表征表明所得产物为化合物的混合物。所有新配合物均通过元素分析,熔点,电喷雾电离质谱(ESI-MS)进行了表征),核磁共振(NMR)和红外(IR)光谱。尤其是,使用各种1D(1 H,13 C,31 P,DEPT和选择性NOESY)和2D(COSY,NOESY,HSQC,HMBC和H2BC)NMR实验来提供每种配合物的全光谱归属。

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    Sim Sophie Anne;

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