Crystal structure of di-μ-aqua-μ-(pyrazine N,N'-dioxide)-κ(2) O:O-bis-(di-aqua-sodium) tetra-phenyl-borate dihydrate pyrazine N,N'-dioxide monosolvate.

Elaine P Boron,Kelsey K Carter,Jacqueline M Knaust

doi:10.1107/s205698901502071x

Elaine P Boron, Kelsey K Carter + Show 1 more

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https://doi.org/10.1107/s205698901502071x

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Abstract

The search for novel lanthanide coordination networks using pyrazine N,N'-dioxide (pzdo, C4H4N2O2) as a structure-directing unit, led to the synthesis and the structure determination of the title compound, [Na2(C4H4N2O2)(H2O)6][B(C6H5)4]2·C4H4N2O2·2H2O. The crystal structure is comprised of discrete [{Na(H2O)2}2(μ-H2O)2(μ-pzdo)](2+) cations and tetra-phenyl-borate anions, as well as pzdo and H2O solvent mol-ecules. The dinuclear cation is located about a twofold rotation axis, and the symmetry-related Na(I) atoms display a distorted square-pyramidal coordination sphere defined by two O atoms of terminal water ligands, two O atoms of bridging water ligands and one O atom of a bridging pzdo ligand. In the crystal, O-H⋯O hydrogen bonds link the dinuclear cation and solvent pzdo mol-ecules (point-group symmetry -1) into rectangular grid-like layers parallel to the bc plane. Additional C-H⋯O, O-H⋯O, C-H⋯π and O-H⋯π inter-actions link the anion and solvent water mol-ecules to the layers. The layers are further linked into a three-dimensional network through a combination of C-H⋯π and O-H⋯π hydrogen bonds involving the tetra-phenyl-borate anion.

Highlights

Supporting information: this article has supporting information at journals.iucr.org/e a Chemistry Department, 520 North Main St., Meadville, PA 16335, USA, and bDepartment of Chemistry Mathematics and Physics, Clarion University, 840 Wood Street, Clarion, PA 16214, USA. *Correspondence e-mail: The search for novel lanthanide coordination networks using pyrazine N,N0 dioxide as a structure-directing unit, led to the synthesis and the structure determination of the title compound, [Na2(C4H4N2O2)(H2O)6][B(C6H5)4]2C4H4N2O22H2O
The dinuclear cation is located about a twofold rotation axis, and the symmetry-related NaI atoms display a distorted square-pyramidal coordination sphere defined by two O atoms of terminal water ligands, two O atoms of bridging water ligands and one O atom of a bridging pzdo ligand
The layers are further linked into a three-dimensional network through a combination of C—H and O—H hydrogen bonds involving the tetraphenylborate anion

Summary

Chemical context

N,N0 -dioxide (pzdo) and 4,40 -pyridine-N,N0 -dioxide (bpydo) in the synthesis of transition metal and lanthanide metal compounds with coordination networks has been of recent interest (Hill et al, 2005b; Ma et al, 2001; Mantero et al, 2006; Sun et al, 2004). The coordination modes and hydrogenbonding modes of N,N0 -dioxide ligands are flexible (Ma et al., 2001; Mantero et al, 2006). Structure prediction with these ligands can be difficult, in part due to their flexible bonding, and due to the influences of the anion and solvent (Hill et al, 2005a; Mantero et al, 2006).

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Synthesis and crystallization