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Crystal structure of 1,4-diazoniabicyclo[2.2.2]octane diiodide monohydrate
Maderlehner, Sebastian und Pfitzner, Arno
(2012)
Crystal structure of 1,4-diazoniabicyclo[2.2.2]octane diiodide monohydrate.
Zeitschrift für Kristallographie 227, S. 569-574.
Veröffentlichungsdatum dieses Volltextes: 14 Sep 2012 06:45
Artikel
DOI zum Zitieren dieses Dokuments: 10.5283/epub.25880
Zusammenfassung
1,4-diazoniabicyclo [2.2.2]octane diiodide monohydrate was synthesized by protonation of 1,4-diazabicyclo[2.2.2]octane (DABCO) with an excess of concentrated hydroiodic acid in water. It forms colourless rodlike crystals. At room temperature an orthorhombic unit cell, space group Cmc2(1), a = 7.781(2) angstrom, b = 13.010(3) angstrom, c = 11.610(2) angstrom, V = 1175.3(4) angstrom(3), Z = 4, is ...
1,4-diazoniabicyclo [2.2.2]octane diiodide monohydrate was synthesized by protonation of 1,4-diazabicyclo[2.2.2]octane (DABCO) with an excess of concentrated hydroiodic acid in water. It forms colourless rodlike crystals. At room temperature an orthorhombic unit cell, space group Cmc2(1), a = 7.781(2) angstrom, b = 13.010(3) angstrom, c = 11.610(2) angstrom, V = 1175.3(4) angstrom(3), Z = 4, is observed. Both nitrogen atoms bear a proton. The hydrate water molecule within the compound is statistically disordered on a site besides a crystallographic mirror plane at room temperature. DSC measurements indicate a phase transition at about -10 degrees C. A single crystal X-ray diffraction measurement at 123 K reveals a primitive unit cell, space group Pca2(1), a = 12.8835(2) angstrom, b = 7.6819(1) angstrom, c = 11.4392(2) angstrom, v = 1132.16(3) angstrom(3), Z = 4. The water molecule with its hydrogen atoms is well ordered at this temperature. Two almost linear hydrogen bonds O-H center dot center dot center dot I are formed. The formation of hydrogen bonds is also detected by IR-spectroscopy with O-H stretching frequencies at (nu) over bar = 3403 cm(-1) and (nu) over bar = 3354 cm(-1), respectively.
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| Dokumentenart | Artikel | ||||
| Titel eines Journals oder einer Zeitschrift | Zeitschrift für Kristallographie | ||||
| Verlag: | WALTER DE GRUYTER GMBH | ||||
|---|---|---|---|---|---|
| Ort der Veröffentlichung: | BERLIN | ||||
| Band: | 227 | ||||
| Seitenbereich: | S. 569-574 | ||||
| Datum | 2012 | ||||
| Institutionen | Chemie und Pharmazie > Institut für Anorganische Chemie > Lehrstuhl Prof. Dr. Arno Pfitzner | ||||
| Identifikationsnummer |
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| Stichwörter / Keywords | DABCO; ACID; Alkylammonium halide; Hydrogen bonding; Phase transition; Solid hydrate | ||||
| Dewey-Dezimal-Klassifikation | 500 Naturwissenschaften und Mathematik > 540 Chemie | ||||
| Status | Veröffentlicht | ||||
| Begutachtet | Ja, diese Version wurde begutachtet | ||||
| An der Universität Regensburg entstanden | Ja | ||||
| URN der UB Regensburg | urn:nbn:de:bvb:355-epub-258808 | ||||
| Dokumenten-ID | 25880 |
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