Metal derivatives of heterocyclic-2-thiones: Crystal structures of [bis(diphenylphosphanyl)propane][bis(pyrimidine-2-thiolato)]ruthenium(II) and [bis(diphenylphosphanyl)methane][bis(pyridine-2-thiolato)]ruthenium(II)

Lobana T.S.; Kaur P.; Kaur A.; Butcher R.J.

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Metal derivatives of heterocyclic-2-thiones: Crystal structures of [bis(diphenylphosphanyl)propane][bis(pyrimidine-2-thiolato)]ruthenium(II) and [bis(diphenylphosphanyl)methane][bis(pyridine-2-thiolato)]ruthenium(II)

机译：杂环-2-硫酮的金属衍生物：[双（二苯基膦基）丙烷] [双（嘧啶-2-硫代）]钌（II）和[双（二苯基膦基）甲烷] [双（吡啶-2-硫代）]的晶体结构钌（II）

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Ruthenium(II) Complexes containing pyrimidine-2-thiolate (pymS~-) and bis(diphenylphosphanyl)alkanes [Ph_2P-(CH _2)_m-PPh_2, m = 1, dppm; m = 2, dppe; m = 3, dppp; m = 4, dppb] are described. Reactions of [RuCl_2L_2] (L = dppm, dppp) and [Ru_2Cl_4L_3] (L = dppb) with pyrimidine-2-thione (pymSH) in 1:2 molar ratio in dry benzene in the presence of Et _3N base yielded the [Ru(pymS)_2L] complexes (pymS ~- = pyrimidine-2-thiolate; L = dppm (1); dppp (3); dppb (4)). The complex [Ru(pymS)_2(dppe)] (2) was indirectly prepared by the reaction of [Ru(pymS)_2(PPh_3)_2] with dppe. These complexes were characterized using analytical data, IR,~1H, ~(13)C, ~(31)P NMR spectroscopy, and X-ray crystallography (complex 3). The crystal structure of the analogous complex [Ru(pyS)_2(dppm)] (5) with the ligand pyridine-2-thiolate (pyS~-) was also described. X-ray crystallographic investigation of complex 3 has shown two four-membered chelate rings (N, S donors) and one six-membered ring (P, P donors) around the metal atom. Compound 5 provides the first example in which Ru~(II) has three four-membered chelate rings: two made up by N, S donor ligands and one made up by P, P donor ligand. The arrangement around the metal atoms in each complex is distorted octahedral with cis:cis:trans:P, P:N, N:S, S dispositions of the donor atoms. The ~(31)P NMR spectroscopic data revealed that the complexes are static in solution, except 2, which showed the presence of more than one species.

机译：含有嘧啶-2-硫醇盐（pymS--）和双（二苯基膦基）烷烃[Ph_2P-（CH _2）_m-PPh_2，m = 1，dppm; m = 2，dppe; m = 3，dppp; m ＝ 4，dppb]。在干燥的苯中，在Et _3N碱存在下，[RuCl_2L_2]（L = dppm，dppp）和[Ru_2Cl_4L_3]（L = dppb）与嘧啶-2-硫酮（pymSH）的摩尔比为1：2。（pymS）_2L]络合物（pymS〜-=嘧啶-2-硫醇盐; L = dppm（1）; dppp（3）; dppb（4））。通过[Ru（pymS）_2（PPh_3）_2]与dppe的反应间接制备[Ru（pymS）_2（dppe）]（2）。使用分析数据，IR，〜1H，〜（13）C，〜（31）P NMR光谱和X射线晶体学（配合物3）对这些配合物进行表征。还描述了与配体吡啶-2-硫醇吡啶盐（pyS〜-）的类似络合物[Ru（pyS）_2（dppm）]（5）的晶体结构。配合物3的X射线晶体学研究表明，金属原子周围有两个四元螯合环（N，S供体）和一个六元环（P，P供体）。化合物5提供了第一个实例，其中Ru（II）具有三个四元螯合环：两个由N，S供体配体组成，一个由P，P供体配体组成。每个络合物中金属原子周围的排列都以给体原子的cis：cis：trans：P，P：N，N：S，S排列为八面体形。〜（31）P NMR光谱数据表明，该配合物在溶液中是静态的，除2外，这表明存在一种以上。

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |2012年第1期|共6页
作者
Lobana T.S.; Kaur P.; Kaur A.; Butcher R.J.;
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正文语种 eng
中图分类化学;
关键词
Pyridine-2-thione; Pyrimidine-2-thione; Ruthenium;

机译：吡啶-2-硫酮;嘧啶-2-硫酮;钌;

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1. Metal derivatives of heterocyclic-2-thiones: Crystal structures of [bis(diphenylphosphanyl)propane][bis(pyrimidine-2-thiolato)]ruthenium(II) and [bis(diphenylphosphanyl)methane][bis(pyridine-2-thiolato)]ruthenium(II) [J] . Lobana T.S., Kaur P., Kaur A., Zeitschrift fur Anorganische und Allgemeine Chemie . 2012,第1期

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Metal derivatives of heterocyclic-2-thiones: Crystal structures of [bis(diphenylphosphanyl)propane][bis(pyrimidine-2-thiolato)]ruthenium(II) and [bis(diphenylphosphanyl)methane][bis(pyridine-2-thiolato)]ruthenium(II)

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