Cargando…
Bis(1,3-dimethyl-1H-imidazolium) hexafluorosilicate methanol 0.33-solvate
The title compound, 6C(5)H(9)N(2) (+)·3SiF(6) (2−)·CH(3)OH, (I), was prepared by recrystallization of the crude salt from methanol along with solvent-free 2C(5)H(9)N(2) (+)·SiF(6) (2−) (II). Crystals of these solvatomorphs can be separated manually. The solvate (I) crystallizes in a rare hexagonal...
Autores principales: | , , |
---|---|
Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2013
|
Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3793724/ https://www.ncbi.nlm.nih.gov/pubmed/24109311 http://dx.doi.org/10.1107/S1600536813018230 |
Sumario: | The title compound, 6C(5)H(9)N(2) (+)·3SiF(6) (2−)·CH(3)OH, (I), was prepared by recrystallization of the crude salt from methanol along with solvent-free 2C(5)H(9)N(2) (+)·SiF(6) (2−) (II). Crystals of these solvatomorphs can be separated manually. The solvate (I) crystallizes in a rare hexagonal space group P6/mcc. Its asymmetric unit comprises one half of an imidazolium cation bisected by the crystallographic m-plane, one-sixth and one-twelfth of two crystallographically independent SiF(6) (2–) dianions (Si atoms are located on the 3.2 and 6/m inversion centres), and one-twelfth of a methanol molecule (C atoms are situated on the 622 inversion centres, other atoms are disordered between general positions). In (I), all F atoms of 3.2-located SiF(6) (2–) dianions participate in the formation of symmetry-equivalent contacts to the H atoms of imidazolium fragments, thus forming rod-type ensembles positioned on the -6 axes. These ‘pillar’ rods are, in turn, F⋯H interlinked through SiF(6) (2–) dianions disordered around the 6/m centres. The twelvefold disordered methanol molecules are appended to this array by O—H⋯F hydrogen bonds to the 6/m located SiF(6) (2–) dianions. In terms of graph-set notation, the first and second level networks in (I) are N (1) = C (2) (2)(7)[3R (4) (4)(14)]D (2) (2)(4) and N (2) = D (2) (2)(5) (C—H⋯O hydrogen bonds are not considered). After locating all symmetrically independent atoms in the cation and anions, there remained a strong (> 3 e Å(−3)) residual electron density peak located at the 622 inversion centre. Treatment of this pre-refined model with the SQUEEZE procedure in PLATON [Spek (2009). Acta Cryst. D65, 148–155] revealed two voids per unit cell, indicative of the presence of the solvent methanol molecule disordered about the 622 inversion centre. |
---|