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首页> 外文期刊>Chemistry: A European journal >The preparation and characterisation of hetero- and homobimetallic complexes containing bridging naphthalene-1,8-dithiolato ligands
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The preparation and characterisation of hetero- and homobimetallic complexes containing bridging naphthalene-1,8-dithiolato ligands

机译：含有桥接萘-1,8-二硫代lato配体的杂双金属和同双金属配合物的制备和表征

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摘要

Homo- and heterobimetallic complexes of the form [(PPh3)(2)(mu(2)-1,8- S-2-nap)[MLn}] (in which (1,8-S-2-nap)= naphth o-1,8-dithiol ate and {MLn} = {PtCl2} (1), {PtClMe} (2), {PtClPh} (3), {Ptme(2)} (4), {PtlMe(3)} (5) and {Mo(CO)(4)} (6)) were obtained by the addition of [PtCl2(NCPh)(2)], [PtClMe-(cod)] (cod = 1,5-cyclooctadiene), (PtClPn(cod)], [PtMe2(cod)], [{PtIMe3}(4)] and [Mo(CO)(4)(nbd)] (nbd=norbornadiene), respectively, to [Pt(PPn(3))(2)(1,8-S-2-nap)]. Synthesis of cationic complexes was achieved by the addition of one or two equivalents of a halide abstractor, Ag[BF4] or Ag[ClO4] to [{Pt(mu-Cl)(mu-eta(2):eta(1)-C3H5)}(4)], [{Pd(mu-Cl)(eta(3)-C3H5)}(2)], [{IrCl(mu-Cl)(eta(5)- C5Me5)}(2)] (in which C5Me5=Cp*=1,2,3,4, 5-pentamethylcyclopentadienyl), [{RhCl(mu-Cl)(eta(5)-C5Me5)}(2)]. [PtCl2-(PMe2Ph)(2)] and [{Rh(mu-Cl)(cod)}(2)] to give the appropriate coordinatively unsaturated species that, upon treatment with [(PPh3)(2)Pt(1,8-S-2-nap)], gave complexes of the form [(PPh3)(2)(mu(2)-1,8-S-2- nap){MLn][X] (in which {MLn}[X]= {Pt(eta(3)-C3H5)}[ClO4] (7), {Pd(eta(3)-C3H5)}- [ClO4] (8), (IrCl(eta(5)-C5Me5)}[ClO4] (9), (RhCl(eta(5)-C5Me5)}[BF4] (10), (Pt-(PMe2Ph)(2)}[ClO4](2) (11), (Rh(cod)-[CIO4] (12); the carbonyl complex jRh(CO)(2))[ClO4] (13) was formed by bubbling gaseous CO through a solution of 12. In all cases the naphtho-1,8-dithiolate ligand acts as a bridge between two metal centres to give a four-membered PtMS2 ring (M=transition metal). All compounds were characterised spectroscopically. The X-ray structures of 5, 6, 7, 8, 10 and 12 reveal a binuclear PtMS2 core with Pt...M distances ranging from 2.9630(8)-3.438(1) angstrom for 8 and 5, respectively. The napS(2) mean plane is tilted with respect to the PtP2S2 coordination plane, with dihedral angles in the range 49.7-76.1 degrees and the degree of tilting being related to the Pt...M distance and the coordination number of M. The sum of the Pt(1) coordination planeapS(2) angle, a, and the Pt(1)coordination plane/ M(2)coordination plane angle, b, a+b, is close to 120 degrees in nearly all cases. This suggests that electronic effects play a significant role in these binuclear systems.
机译：[（PPh3）（2）（mu（2）-1,8-S-2-nap）[MLn}]形式的同金属和异双金属配合物（其中（1,8-S-2-nap）=萘基o-1,8-二硫醇盐，{MLn} = {PtCl2}（1），{PtClMe}（2），{PtClPh}（3），{Ptme（2）}（4），{PtlMe（3） }（5）和{Mo（CO）（4）}（6））是通过添加[PtCl2（NCPh）（2）]，[PtClMe-（cod）]（鳕鱼= 1,5-环辛二烯）获得的，（（PtClPn（cod）]，[PtMe2（cod）]，[{PtIMe3}（4）]和[Mo（CO）（4）（nbd）]（nbd = norbornadiene）分别为[Pt（PPn（ 3））（2）（1,8-S-2-nap）]。阳离子配合物的合成是通过将一或两当量的卤化物抽象剂Ag [BF4]或Ag [ClO4]添加到[{ Pt（mu-Cl）（mu-eta（2）：eta（1）-C3H5）}（4）]，[{Pd（mu-Cl）（eta（3）-C3H5）}（2）]，[ {IrCl（mu-Cl）（eta（5）-C5Me5）}（2）]（其中C5Me5 = Cp * = 1,2,3,4，5-五甲基环戊二烯基），[{RhCl（mu-Cl）（ eta（5）-C5Me5）}（2）]。[PtCl2-（PMe2Ph）（2）]和[{Rh（mu-Cl）（cod）}（2）]得到适当的配位不饱和物质，用[（PPh3）（2）Pt（1,8-S-2-nap）]处理，得到[（PPh3）（2）（mu （2）-1,8-S-2-小睡）{MLn] [X]（其中{MLn} [X] = {Pt（eta（3）-C3H5）} [ClO4]（7），{Pd （eta（3）-C3H5）}-[ClO4]（8），（IrCl（eta（5）-C5Me5）} [ClO4]（9），（RhCl（eta（5）-C5Me5）} [BF4]（ 10），（Pt-（PMe2Ph）（2）} [ClO4]（2）（11），（Rh（cod）-[CIO4]（12）;羰基配合物jRh（CO）（2））[ClO4]（13）是通过将气态CO鼓泡通过12溶液而形成的。在所有情况下，萘-1,8-二硫代配体都充当两个金属中心之间的桥梁给出一个四元的PtMS2环（M =过渡金属）。所有化合物均经光谱表征。 5、6、7、8、10和12的X射线结构揭示了双核PtMS2核，其Pt ... M距离分别为2.9630（8）-3.438（1）埃，分别为8和5。 napS（2）平均平面相对于PtP2S2协调平面倾斜，二面角的范围为49.7-76.1度，并且倾斜程度与Pt ... M距离和M的协调数有关。在几乎所有情况下，Pt（1）协调平面/ napS（2）角度α和Pt（1）协调平面/ M（2）协调平面角度b，a + b的总和接近120度。这表明电子效应在这些双核系统中起着重要作用。

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