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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...

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Autores principales: Tian, Chong, Nie, Wanli, Borzov, Maxim V.
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
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author Tian, Chong
Nie, Wanli
Borzov, Maxim V.
author_facet Tian, Chong
Nie, Wanli
Borzov, Maxim V.
author_sort Tian, Chong
collection PubMed
description 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.
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spelling pubmed-37937242013-10-09 Bis(1,3-dimethyl-1H-imidazolium) hexa­fluoro­silicate methanol 0.33-solvate Tian, Chong Nie, Wanli Borzov, Maxim V. Acta Crystallogr Sect E Struct Rep Online Organic Papers 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. International Union of Crystallography 2013-07-06 /pmc/articles/PMC3793724/ /pubmed/24109311 http://dx.doi.org/10.1107/S1600536813018230 Text en © Tian et al. 2013 http://creativecommons.org/licenses/by/2.0/uk/ This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
spellingShingle Organic Papers
Tian, Chong
Nie, Wanli
Borzov, Maxim V.
Bis(1,3-dimethyl-1H-imidazolium) hexa­fluoro­silicate methanol 0.33-solvate
title Bis(1,3-dimethyl-1H-imidazolium) hexa­fluoro­silicate methanol 0.33-solvate
title_full Bis(1,3-dimethyl-1H-imidazolium) hexa­fluoro­silicate methanol 0.33-solvate
title_fullStr Bis(1,3-dimethyl-1H-imidazolium) hexa­fluoro­silicate methanol 0.33-solvate
title_full_unstemmed Bis(1,3-dimethyl-1H-imidazolium) hexa­fluoro­silicate methanol 0.33-solvate
title_short Bis(1,3-dimethyl-1H-imidazolium) hexa­fluoro­silicate methanol 0.33-solvate
title_sort bis(1,3-dimethyl-1h-imidazolium) hexa­fluoro­silicate methanol 0.33-solvate
topic Organic Papers
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3793724/
https://www.ncbi.nlm.nih.gov/pubmed/24109311
http://dx.doi.org/10.1107/S1600536813018230
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