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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Polynuclear platinum phosphanido/phosphinito complexes: formation of P-O and P-O-P bonds through reductive coupling processes
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Polynuclear platinum phosphanido/phosphinito complexes: formation of P-O and P-O-P bonds through reductive coupling processes

机译：多核铂膦酸酯基/膦膦酸酯络合物：通过还原偶联过程形成P-O和P-O-P键

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摘要

A mixture of the asymmetric complexes of formula [(R-F)(2)Pt(mu-Ph2PO)(mu-PPh2)Pt(mu-PPh2)(2)Pt(solv)(solv')] [(1-(solv)(solv')] (solv, solv' = acetone, H2O, CH3CN) has been prepared by reaction of [(R-F)(2)Pt-II(mu-PPh2)(2)Pt-II(mu-PPh2)(2)Pt-II(NCCH3)(2)] with AgClO4 in CH3CN/acetone. The lability of the Pt-solvent bonds allows the displacement of the coordinated solvent molecules by dppm or Cl-and the isolation of the tri-or hexanuclear phosphanido/phosphinito Pt(II) complexes [(C6F5)(2)Pt(mu-PPh2)(mu-PPh2O)Pt(mu-PPh2)(2)Pt(dppm)] (2) or [NBu4](2)[(C6F5)(2)Pt(mu-PPh2)(mu-PPh2O)mu Pt(-PPh2)(2)Pt(mu-Cl)(2)Pt(mu-PPh2)(2)Pt(mu-PPh2)(mu-PPh2O)Pt(C6F5)(2)] (as a mixture of the two possible isomers 4a and 4b). Complex 2 reacts with AgClO4 to form the tetranuclear derivative [(C6F5)(2)Pt(mu-PPh2)(mu-PPh2O)Pt(mu-PPh2)(2)Pt(dppm)Ag(OClO3)] (3), which displays two Pt-Ag donor-acceptor bonds. The mixture of the hexanuclear isomers 4a-4b reacts with Tl(acac) producing the acetylacetonato complex [NBu4][(C6F5)(2)Pt(mu-PPh2)(mu-PPh2O)Pt(mu-PPh2)(2)Pt(acac)] (5) which, upon reaction with HCl, yields back the mixture of 4a-4b. The reaction of 4a-4b with PPh3 produces [NBu4][(C6F5)(2)Pt(mu-PPh2)(mu-PPh2O)Pt(mu-PPh2)(2)Pt(Cl)(PPh3)] (6) as a mixture of isomers with the chloro ligand located syn (6a) or anti (6b) to the PPh(2)O(-)group. Either the reaction of 6 with AgClO4 or the treatment of 5 with HPPh3ClO4 results in the formation of the species [(C6F5)(2)Pt-II(mu-PPh2)(2)Pt-I(mu-PPh2OPPh2) Pt-I(PPh3)] (7) (44 VEC), which can be explained as the consequence of a PPh2O/PPh2 reductive coupling and a rearrangement of ligands in the molecule generating a Pt(II), Pt(I), Pt(I) compound. All complexes were characterised in the solid state by XRD (only one of the isomers, in the cases of 4 and 6) and in solution by NMR spectroscopy.
机译：式[（RF）（2）Pt（mu-Ph2PO）（mu-PPh2）Pt（mu-PPh2）（2）Pt（solv）（solv'）] [[1-（solv ）（solv'）]（solv，solv'=丙酮，H2O，CH3CN）是通过[（RF）（2）Pt-II（mu-PPh2）（2）Pt-II（mu-PPh2）反应制备的（2）Pt-II（NCCH3）（2）]与AgClO4混合在CH3CN /丙酮中。Pt-溶剂键的不稳定性允许配位溶剂分子被dppm或Cl置换并分离出三核或六核phosphanido / phosphinito Pt（II）络合物[（C6F5）（2）Pt（mu-PPh2）（mu-PPh2O）Pt（mu-PPh2）（2）Pt（dppm）]（2）或[NBu4]（2） [（C6F5）（2）Pt（mu-PPh2）（mu-PPh2O）mu Pt（-PPh2）（2）Pt（mu-Cl）（2）Pt（mu-PPh2）（2）Pt（mu-PPh2 ）（mu-PPh2O）Pt（C6F5）（2）]（作为两种可能的异构体4a和4b的混合物），配合物2与AgClO4反应形成四核衍生物[（C6F5）（2）Pt（mu-PPh2 ）（mu-PPh2O）Pt（mu-PPh2）（2）Pt（dppm）Ag（OClO3）]（3），具有两个Pt-Ag供体-受体键。六核异构体4a-4b的混合物与Tl（acac）生成乙酰丙酮络合物[NBu4] [（C6F5）（2）Pt（mu-PPh2）（mu-PPh2O）Pt（mu-PPh2）（2）Pt（acac）]（5），在与HCl反应后，得到4a-4b。 4a-4b与PPh3反应生成[NBu4] [（C6F5）（2）Pt（mu-PPh2）（mu-PPh2O）Pt（mu-PPh2）（2）Pt（Cl）（PPh3）]（6）异构体与氯配体的混合物，位于PPh（2）O（-）基的syn（6a）或anti（6b）。 6与AgClO4的反应或HPPh3ClO4的5处理导致形成[[C6F5）（2）Pt-II（mu-PPh2）（2）Pt-I（mu-PPh2OPPh2）Pt-I （PPh3）]（7）（44 VEC），可以解释为PPh2O / PPh2还原偶联和分子中配体重排产生Pt（II），Pt（I），Pt（I）的结果复合。所有配合物均通过XRD（在4和6的情况下只有一种异构体）为固态，在溶液中通过NMR表征。

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