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Synthesis, Characterization, and Crystal Structures of [N(CH 3 ) 4 ] 2 [B 12 H 12 ] and [N(CH 3 ) 4 ] 2 [B 12 H 12 ] · CH 3 CN
Author(s) -
Hofmann Kathrin,
Albert Barbara
Publication year - 2001
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/1521-3749(200105)627:5<1055::aid-zaac1055>3.0.co;2-t
Subject(s) - characterization (materials science) , chemistry , crystallography , materials science , nanotechnology
Bis(tetramethylammonium) dodecahydrododecaborate, [(CH 3 ) 4 N] 2 [B 12 H 12 ], and bis(tetramethylammonium) dodecahydrododecaborate acetonitrile, [(CH 3 ) 4 N] 2 [B 12 H 12 ] · CH 3 CN, were synthesized and characterized via Infrared, 1 H and 11 B NMR spectroscopy. [(CH 3 ) 4 N] 2 [B 12 H 12 ] crystallizes isopunctual to the alkali metal dodecaborates. The crystal structure of [(CH 3 ) 4 N] 2 [B 12 H 12 ] · CH 3 CN was determined from single crystal data and refined in the orthorhombic crystal system ( Pcmn , no. 62, a = 898.68(8), b = 1312.85(9) c = 1994.5(1) pm, R(|F| , 4σ) = 5.9%, wR(F 2 ) = 18.3%). Here, the geometry of the dodecaborate anion is that of an almost ideal icosahedron, less distorted than most other dodecaborates known. By low‐temperature Guinier‐Simon diffractometry phase transitions were detected for [(CH 3 ) 4 N] 2 [B 12 H 12 ] and [(CH 3 ) 4 N] 2 [B 12 H 12 ] · CH 3 CN at –70 and –15 °C, respectively.