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（1,6,7,12-四氮杂苝-κ(2) N,N'）双（4,4',5,5'-四甲基-2,2'-联吡啶-κ(2) N,N'）钌（II）双（六氟磷酸根）乙腈三溶剂合物

(1,6,7,12-Tetra-aza-perylene-κ(2) N,N')bis-(4,4',5,5'-tetra-methyl-2,2'-bipyridyl-κ(2) N,N')ruthenium(II) bis-(hexa-fluorido-phosphate) aceto-nitrile tris-olvate.

作者信息

Brietzke Thomas, Kässler Daniel, Kelling Alexandra, Schilde Uwe, Holdt Hans-Jürgen

机构信息

Universität Potsdam, Institut für Chemie, Anorganische Chemie, Karl-Liebknecht-Strasse 24-25, D-14476 Potsdam, Germany.

出版信息

Acta Crystallogr Sect E Struct Rep Online. 2014 May 31;70(Pt 6):m238-9. doi: 10.1107/S1600536814011969. eCollection 2014 Jun 1.

DOI:10.1107/S1600536814011969
PMID:24940217
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC4051039/
Abstract

In the title compound, rac-Ru(C14H16N2)2(C16H8N4)2·3C2H3N, discrete dimers of complex cations, Ru(tmbpy)2-tape, of opposite chirality are formed (tmbpy = tetra-methyl-bipyridine; tape = tetraazaperylene), held together by π-π stacking inter-actions between the tetra-aza-perylene moieties with centroid-centroid distances in the range 3.563 (3)-3.837 (3) Å. These inter-actions exhibit a parallel displaced π-π stacking mode. Additional weak C-H⋯π-ring and C-H⋯N and C-H⋯F inter-actions are found, leading to a three-dimensional architecture. The Ru(II) atom is coordinated in a distorted octa-hedral geometry. The counter-charge is provided by two hexa-fluorido-phosphate anions and the asymmetric unit is completed by three aceto-nitrile solvent mol-ecules of crystallization. Four F atoms of one PF6 (-) anion are disordered over three sets of sites with occupancies of 0.517 (3):0.244 (3):0.239 (3). Two aceto-nitrile solvent mol-ecules are highly disordered and their estimated scattering contribution was subtracted from the observed diffraction data using the SQUEEZE option in PLATON [Spek (2009 ▶). Acta Cryst. D65, 148-155].

摘要

在标题化合物rac-Ru(C₁₄H₁₆N₂)₂(C₁₆H₈N₄)₂·3C₂H₃N中，形成了具有相反手性的复杂阳离子Ru(tmbpy)₂-tape的离散二聚体（tmbpy = 四甲基联吡啶；tape = 四氮杂苝），通过四氮杂苝部分之间的π-π堆积相互作用结合在一起，质心-质心距离在3.563(3)-3.837(3) Å范围内。这些相互作用呈现出平行错位的π-π堆积模式。还发现了额外的弱C-H⋯π环、C-H⋯N和C-H⋯F相互作用，从而形成了三维结构。Ru(II)原子以扭曲的八面体几何构型配位。抗衡电荷由两个六氟磷酸根阴离子提供，不对称单元由三个乙腈溶剂结晶分子完成。一个PF₆ (-)阴离子的四个F原子在三组位置上无序分布，占有率为0.517(3):0.244(3):0.239(3)。两个乙腈溶剂分子高度无序，使用PLATON中的SQUEEZE选项[Spek (2009 ▶). Acta Cryst. D65, 148 - 155]从观察到的衍射数据中减去了它们估计的散射贡献。

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引用本文的文献

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