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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Synthesis and characterisation of yttrium complexes supported by the beta-diketiminate ligand {ArNC(CH3)CHC(CH3)NAr}~-(Ar = 2,6-Pr_2~iC_6H_3)
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Synthesis and characterisation of yttrium complexes supported by the beta-diketiminate ligand {ArNC(CH3)CHC(CH3)NAr}~-(Ar = 2,6-Pr_2~iC_6H_3)

机译：β-二酮配体{ArNC（CH3）CHC（CH3）NAr}〜-（Ar = 2,6-Pr_2〜iC_6H_3）负载的钇配合物的合成与表征

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Reaction of YI_3(THF)_(35)with one equivalent of the potassium beta-diketiminate(BDI)complex [HC{C(CH3)NAr}2K](1)(Ar = 2,6-Pi_2~iC6H3)affords the monomeric,mono-substituted yttrium BDI complex [HC{C(CH3)NAr}2YI2(THF)](2)in good yield. Reaction of 2 with DME affords [HC{C(CH3)NAr}2YI2(DME)](3)in quantitative yield,which is monomeric also. Reaction of the primary terphenyl phosphane Ar*PH2(Ar* = 2,6-(2,4,6-Pr_3~iC6H2)2C6H3)with potassium hydride,and recrystallisation from hexane,affords the potassium primary terphenyl phosphanide complex [{Ar*P(H)K(THF)}2](4)in high yield. Compound 4 is dimeric in the solid state,constructed around a centrosymmetric K2P2 four-membered ring,the coordination sphere of potassium is supplemented with an eta~6 K... C_(aryl)interaction. The reaction of 2 with one molar equivalent of 4 in THF affords the THF ring-opened compound [HC{C(CH3)NAr}2Y{O(CH2)4P(H)Ar*}(I)(THF)](5). Compound 5 is formed as a mixture endo_(OR)(5a)and exo_(OR)(5b)isomers(5a:5b = ~2:1)which may be separated by fractional crystallisation from hexane-toluene to give pure 5a. Attempted alkylation of 3 with two equivalents of KCH2Si(CH3)3 affords the potassium yttriate complex [Y{mu-eta~5:eta~1-ArNC(CH3)=CHC(=CH2)NAr}2K(DME)2](6)in moderate yield;6 contains two dianionic dianilide ligands,which are derived from C-H activation of a backbone methyl group,each bonded eta~5 to yttrium in the solid state. The reaction of 3 with one equivalent of KC_8 affords [{HC(C[CH3]NAr)2YI(mu-OCH3)}2](7),derived from C-0 bond activation of DME,as the only isolable product in very low yield. Compounds 2,3,4,5a,6,and 7 have been characterised by single crystal X-ray diffraction,NMR spectroscopy and CHN microanalyses.
机译：YI_3（THF）_（35）与一当量的β-二酮化钾（BDI）络合物[HC {C（CH3）NAr} 2K]（1）（Ar = 2,6-Pi_2〜iC6H3）的反应单体单取代钇BDI络合物[HC {C（CH3）NAr} 2YI2（THF）]（2），收率良好。 2与DME反应可定量获得[HC {C（CH3）NAr} 2YI2（DME）]（3），这也是单体。伯三苯膦膦Ar * PH2（Ar * = 2,6-（2,4,6-Pr_3〜iC6H2）2C6H3）与氢化钾反应，然后从己烷中重结晶，得到伯三苯膦酸钾配合物[{Ar * P（H）K（THF）} 2]（4）的高收率。化合物4为固态二聚体，围绕着一个中心对称的K2P2四元环构筑，钾的配位域补充有η〜6 K ... C_（芳基）相互作用。 2与1摩尔当量的4在THF中的反应得到THF开环的化合物[HC {C（CH3）NAr} 2Y {O（CH2）4P（H）Ar *}（I）（THF）]（5 ）。化合物5是内-（OR）（5a）和外-（OR）（5b）异构体（5a：5b =〜2：1）的混合物，可以通过分步结晶从己烷-甲苯中分离得到纯的5a。尝试用两当量的KCH2Si（CH3）3进行3的烷基化反应可得到钇酸钾络合物[Y {mu-eta〜5：eta〜1-ArNC（CH3）= CHC（= CH2）NAr} 2K（DME）2]（ 6）中等收率; 6含有两个双阴离子二苯胺配体，它们是由骨架甲基的CH活化而衍生的，每个eta〜5键合在固态。 3与一当量KC_8的反应提供[{HC（C [CH3] NAr）2YI（mu-OCH3）} 2]（7），其是DME的C-0键活化作用，是唯一可分离的产物产量低。化合物2、3、4、5a，6和7已通过单晶X射线衍射，NMR光谱和CHN微量分析进行了表征。

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