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Pyrrole-based pincer ligands containing iminophosphorane moieties and their coordination chemistry with group 1 metals and magnesium
Zeitschrift für anorganische und allgemeine Chemie ( IF 1.1 ) Pub Date : 2021-05-07 , DOI: 10.1002/zaac.202100080
Nico Ehrlich 1 , Matthias Freytag 1 , Jan Raeder 1 , Peter G. Jones 1 , Marc D. Walter 1
Affiliation  

The Staudinger reaction of 2,5-bis((di-tert-butylphosphaneyl)methyl)-1H-pyrrole (tBuPNP)H; tBuPNP=C4H2N-2,5-CH2PtBu2) with 2 equiv. of Me3SiN3 cleanly furnishes 1,1′-((1H-pyrrole-2,5-diyl)bis(methylene))bis(1,1-di-tert-butyl-N-(trimethylsilyl)-λ5-phosphanimine) (1; (NPNPN)H, NPNPN=C4H2N-2,5-CH2PtBu2NSiMe3) in excellent yield. Pyrrole 1 is easily deprotonated by alkali metal amides, [MN(SiMe3)2] (M=Li, Na, K, Cs) to yield the corresponding alkali metal pyrrolides, 1-M. Compound 1-Li is features a κ-N,N,N coordination whereby both iminophosphorane side-arms are coordinated to the lithium cation (with additional short Li⋅⋅⋅H contacts, whereas the heavier congeners form dimeric structures. This results in κ-N,N coordination within one [(NPNPN)M] (M=Na, Cs) unit, and the dimeric structure is then completed by additional η5-coordination of the pyrrolyl ligand to the neighbouring alkali metal. Furthermore, heteroleptic magnesium alkyl complexes, 1-MgR, are isolated from the reaction of [MgR2] (R= CH2SiMe3, CH2CMe3, CH2CMe2Ph) with (PNP*)H (1 equiv).

中文翻译:

含有亚氨基正膦部分的吡咯基钳状配体及其与第 1 族金属和镁的配位化学

2,5-双((二-丁基膦酰基)甲基) -1H-吡咯( t Bu PNP)H的Staudinger反应;t Bu PNP=C 4 H 2 N-2,5-CH 2 P t Bu 2 ) 与 2 当量。的我3的SiN 3干净配料1,1' - ((1- ħ -吡咯-2,5-二基)二(亚甲基))二(1,1-二-丁基- ñ - (三甲硅烷基)-λ 5 -膦亚胺) ( 1 ; (NPNPN)H, NPNPN=C 4 H 2 N-2,5-CH 2 P t Bu2 NSiMe 3 ) 以优异的产量。吡咯1很容易被碱金属酰胺 [MN(SiMe 3 ) 2 ] (M=Li, Na, K, Cs)去质子化,生成相应的碱金属吡咯化物1-M。化合物1-Li具有 κ- N , N , N配位,其中两个亚氨基膦侧臂与锂阳离子配位(具有额外的短 Li⋅⋅⋅H 接触,而较重的同系物形成二聚体结构。这导致 κ -N,N 在一个 [(NPNPN)M] (M=Na, Cs) 单元内配位,然后通过额外的 η 5完成二聚体结构- 吡咯基配体与相邻碱金属的配位。此外,杂配镁烷基配合物1-MgR是从 [MgR 2 ](R= CH 2 SiMe 3、CH 2 CMe 3、CH 2 CMe 2 Ph)与(PNP*)H(1 当量)的反应中分离出来的.
更新日期:2021-07-14
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