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Unexpected formation and crystal structure of tetra-kis-(1H-pyrazole-κN (2))-palladium(II) dichloride.

Wagner T, Christiansen N, Hrib CG, Kaufmann DE, Edelmann FT - Acta Crystallogr Sect E Struct Rep Online (2014)

Bottom Line: The two chloride anions are not coordinating to Pd(2+).They are connected to the complex cations through N-H⋯Cl hydrogen bonds.In addition, C-H⋯Cl hydrogen bonds are observed, leading to a three-dimensional linkage of cations and anions.

View Article: PubMed Central - HTML - PubMed

Affiliation: Chemisches Institut, Otto-von-Guericke-Universität Magdeburg, Universitätsplatz 2, D-39106 Magdeburg, Germany.

ABSTRACT
The title salt, [Pd(C3H4N2)4]Cl2, was obtained unexpectedly by the reaction of palladium(II) dichloride with equimolar amounts of 1-chloro-1-nitro-2,2,2-tris-(pyrazol-yl)ethane in methanol solution. The Pd(2+) cation is located on an inversion centre and has a square-planar coordination sphere defined by four N atoms of four neutral pyrazole ligands. The average Pd-N distance is 2.000 (2) Å. The two chloride anions are not coordinating to Pd(2+). They are connected to the complex cations through N-H⋯Cl hydrogen bonds. In addition, C-H⋯Cl hydrogen bonds are observed, leading to a three-dimensional linkage of cations and anions.

No MeSH data available.


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Structure diagram of the starting material 1-chloro-1-nitro-2,2,2-tris(pyrazol­yl)ethane.
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fig1: Structure diagram of the starting material 1-chloro-1-nitro-2,2,2-tris(pyrazol­yl)ethane.

Mentions: Transition metal complexes containing pyrazole or substituted pyrazoles as ligands are of current inter­est due to their supra­molecular arrangements (Lumme et al., 1988 ▶; Takahashi et al., 2006 ▶; Casarin et al., 2007 ▶; Alsalme et al., 2013 ▶). In the course of an investigation on the coordination chemistry of various azolyl-nitro­chloro­alkanes (Zapol’skii & Kaufmann, 2008 ▶), we have previously studied the reaction of copper(II) perchlorate hexa­hydrate with equimolar amounts of 1-chloro-1-nitro-2,2,2-tris­(pyrazol­yl)ethane, Cl(NO2)CH—C(C3H3N2)3 (Fig. 1 ▶) in methanol solution (Edelmann et al., 2008 ▶). Quite unexpectedly, a complete degradation of the starting material took place during the course of this reaction. As a result, the dark-blue compound trans-bis­(perchlorato)-tetra­kis(pyrazole)copper(II), [Cu(C3H4N2)4(ClO4)2], was isolated. The formation of free pyrazole could only be explained by a solvolytic degradation of the starting material. This degradation must have taken place to a large extent as the isolated yield was 64% (Edelmann et al., 2008 ▶).


Unexpected formation and crystal structure of tetra-kis-(1H-pyrazole-κN (2))-palladium(II) dichloride.

Wagner T, Christiansen N, Hrib CG, Kaufmann DE, Edelmann FT - Acta Crystallogr Sect E Struct Rep Online (2014)

Structure diagram of the starting material 1-chloro-1-nitro-2,2,2-tris(pyrazol­yl)ethane.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4257448&req=5

fig1: Structure diagram of the starting material 1-chloro-1-nitro-2,2,2-tris(pyrazol­yl)ethane.
Mentions: Transition metal complexes containing pyrazole or substituted pyrazoles as ligands are of current inter­est due to their supra­molecular arrangements (Lumme et al., 1988 ▶; Takahashi et al., 2006 ▶; Casarin et al., 2007 ▶; Alsalme et al., 2013 ▶). In the course of an investigation on the coordination chemistry of various azolyl-nitro­chloro­alkanes (Zapol’skii & Kaufmann, 2008 ▶), we have previously studied the reaction of copper(II) perchlorate hexa­hydrate with equimolar amounts of 1-chloro-1-nitro-2,2,2-tris­(pyrazol­yl)ethane, Cl(NO2)CH—C(C3H3N2)3 (Fig. 1 ▶) in methanol solution (Edelmann et al., 2008 ▶). Quite unexpectedly, a complete degradation of the starting material took place during the course of this reaction. As a result, the dark-blue compound trans-bis­(perchlorato)-tetra­kis(pyrazole)copper(II), [Cu(C3H4N2)4(ClO4)2], was isolated. The formation of free pyrazole could only be explained by a solvolytic degradation of the starting material. This degradation must have taken place to a large extent as the isolated yield was 64% (Edelmann et al., 2008 ▶).

Bottom Line: The two chloride anions are not coordinating to Pd(2+).They are connected to the complex cations through N-H⋯Cl hydrogen bonds.In addition, C-H⋯Cl hydrogen bonds are observed, leading to a three-dimensional linkage of cations and anions.

View Article: PubMed Central - HTML - PubMed

Affiliation: Chemisches Institut, Otto-von-Guericke-Universität Magdeburg, Universitätsplatz 2, D-39106 Magdeburg, Germany.

ABSTRACT
The title salt, [Pd(C3H4N2)4]Cl2, was obtained unexpectedly by the reaction of palladium(II) dichloride with equimolar amounts of 1-chloro-1-nitro-2,2,2-tris-(pyrazol-yl)ethane in methanol solution. The Pd(2+) cation is located on an inversion centre and has a square-planar coordination sphere defined by four N atoms of four neutral pyrazole ligands. The average Pd-N distance is 2.000 (2) Å. The two chloride anions are not coordinating to Pd(2+). They are connected to the complex cations through N-H⋯Cl hydrogen bonds. In addition, C-H⋯Cl hydrogen bonds are observed, leading to a three-dimensional linkage of cations and anions.

No MeSH data available.


Related in: MedlinePlus