ISSN:
0044-2313
Keywords:
Halogeno-undecahydro-closo-dodecaborates(2-)
;
Crystal Structures
;
Chemistry
;
Inorganic Chemistry
Source:
Wiley InterScience Backfile Collection 1832-2000
Topics:
Chemistry and Pharmacology
Description / Table of Contents:
Preparation and Crystal Structures of Dipyridiniomethane Monohalogenohydro-closo-Dodecaborates(2-), [(C5H5N)2CH2][B12H11X]; X = Cl, Br, I[B12H12]2- reacts with dihalogenomethanes CH2X2 in presence of trifluoro acetic acid, yielding the monohalogenododecaborates [B12H11X]2- (X = Cl, Br, I), which are separated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose from the starting compound and higher halogenated products. The X-ray structure determinations of [(C5H5N)2CH2][B12H11Cl] · 2(CH3)2SO (orthorhombic, space group Pnma, a = 17.351(6), b = 16.034(5), c = 9.659(2) Å, Z = 4) and of the isotypic bromo and iodo compounds [(C5H5N)2CH2][B12H11X] (monoclinic, space group P21/n, Z = 4; for X = Br: a = 7.339(2), b = 15.275(3), c = 16.761(4) Å, β = 96.80(2)°; for X = I: a = 7.4436(8), b = 15.3510(8), c = 16.9213(16) Å, ß = 97.326(7)°) exhibit crystal lattices build up by columns of substituted boron clusters and angular dications [(C5H5N)2CH2]2+ orientated along the shortest axis which are assembled to alternating layers.
Notes:
[B12H12]2- reagiert mit den Dihalogenmethanen CH2X2 in Gegenwart von Trifluoressigsäure zu den entsprechenden Monohalogenododecaboraten [B12H11X]2- (X = Cl, Br, I). Die Verbindungen werden durch Ionenaustauschchromatographie an Diethylaminoethyl(DEAE)-Cellulose von der Ausgangssubstanz und höherhalogenierten Produkten getrennt. Die Röntgenstrukturanalysen von [(C5H5N)2CH2][B12H11Cl] · 2 (CH3)2SO (orthorhombisch, Raumgruppe Pnma, a = 17,351(6), b = 16,034(5), c = 9,659(2) Å, Z = 4) und der isotypen Bromo-und Iodoverbindungen [(C5H5N)2CH2][B12H11X] (monoklin, Raumgruppe P21/n, Z = 4; für X = Br: a = 7,339(2), b = 15,275(3), c = 16,761(4) Å, β = 96,80(2)°; für X = I: a = 7,4436(8), b = 15,3510(8), c = 16,9213(16) Å, β = 97,326(7)°) zeigen, daß im Kristallgitter Stränge der substituierten Clusteranionen und gewinkelten Dikationen [(C5H5N)2CH2]2+ in Richtung der kürzesten Achse vorliegen, die zu alternierenden Schichten zusammengefügt sind.
Additional Material:
3 Ill.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1002/zaac.19956210903
