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9 - [双 -(苄基硫烷基)甲基]蒽与 - 十二 - (μ - 苯甲烷硫醇根合 - κ:)六钯(6 -)- 蒽 - 9,10 - 二酮(1/1)的晶体结构

Crystal structures of 9-[bis-(benzyl-sulfan-yl)meth-yl]anthracene and of -dodeca-kis-(μ-phenyl-methane-thiol-ato-κ :)hexa-palladium(6 -)-anthracene-9,10-dione (1/1).

作者信息

Raghuvanshi Abhinav, Krupp Anna, Viau Lydie, Knorr Michael, Strohmann Carsten

机构信息

Institut UTINAM UMR 6213 CNRS, Université Bourgogne Franche-Comté, 16, Route de Gray, 25030 Besançon, France.

Anorganische Chemie, TU Dortmund University, Otto-Hahn-Str. 6, D-44227 Dortmund, Germany.

出版信息

Acta Crystallogr E Crystallogr Commun. 2021 Jun 18;77(Pt 7):718-725. doi: 10.1107/S2056989021006113. eCollection 2021 Jul 1.

Abstract

The first title compound, CHS, , represents an example of an anthracene-based functionalized di-thio-ether, which may be useful as a potential chelating or terminal ligand for coordination chemistry. This di-thio-acetal crystallizes in the monoclinic space group 2/. The phenyl rings of the benzyl groups and that of the anthracene unit form dihedral angles of 49.21 (4) and 58.79 (5)° and the crystal structure displays short C-H⋯π contacts. Surprisingly, when attempting to coordinate to [PdCl(PhCN)], instead of the targeted chelate complex [PdCl(κ-)], a cleavage reaction leads to the formation of the centrosymmetric hexa-nuclear cyclic cluster of composition [Pd(μ-SCHPh)] , or [Pd(CHS)]·CHO. This tiara-shaped hexa-mer crystallizing in the triclinic space group consists of six approximately square planar Pd(II)S centers, which are inter-connected through twelve μ-bridging benzyl thiol-ate groups. The Pd⋯Pd contacts range from 3.0892 (2) to 3.1609 (2) Å and can be considered as weakly bonding. The unit cell of contains also a co-crystallized anthracene-9,10-dione mol-ecule.

摘要

第一个标题化合物CHS,代表了一种基于蒽的功能化二硫醚的实例,它可能作为配位化学中潜在的螯合或末端配体。这种二硫缩醛在单斜空间群2/中结晶。苄基的苯环与蒽单元的苯环形成的二面角分别为49.21 (4)和58.79 (5)°,并且晶体结构显示出短的C-H⋯π接触。令人惊讶的是,当试图使与[PdCl(PhCN)]配位时,不是形成目标螯合配合物[PdCl(κ-)],而是发生裂解反应,导致形成组成为[Pd(μ-SCHPh)]的中心对称六核环状簇,即[Pd(CHS)]·CHO。这种冠状六聚体在三斜空间群中结晶,由六个近似正方形平面的Pd(II)S中心组成,它们通过十二个μ-桥连苄基硫醇盐基团相互连接。Pd⋯Pd接触距离范围为3.0892 (2)至3.1609 (2) Å,可以认为是弱键合。的晶胞中还包含一个共结晶的蒽-9,10-二酮分子。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d01a/8382052/25ac22ed0b3a/e-77-00718-fig1.jpg

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