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By reaction of closo-[B 6 H 5 F] 2-  in alkaline solution with excess iodine the monofluoropentaiodo- closo-hexaborate anion [B 6 FI 5 ] 2-  is formed in good yield. The crystal structure of (CH 2 Py 2 )[B 6 FI 5 ] has been determined by single crystal X-ray diffraction analysis (orthorhombic, space group Pnma, a = 13.803(2), b = 11.759(2), c = 13.936(2) Å, Z = 4). The B-F-bond length is 1.41 Å, the B-I distances range from 2.13 to 2.17 Å, the B-B distances from 1.69 to 1.76 A. According to the C 4v  point symmetry the  11 B NMR spectrum of the anion exhibits three singlets at +3.8,-30.1 and-33.3 ppm with the intensity ratio 1:4:1, the  19 F NMR spectrum one quartet at -247.6 ppm with the coupling constant  1 J ( 19 F,  11 B) = 54 Hz.

zeitschrift für naturforschung b

Darstellung,  11 B-und  19 F-NMR-Spektren des Monofluoropentaiodo- closo-hexaboratanions sowie Kristallstruktur von (CH 2 Py 2 )[B 6 FI 5 ]/ Synthesis,  11 B and  19 F NMR Spectra of the Monofluoropentaiodo-closo-hexaborate Anion and the Crystal Structure of (CH 2 Py 2 )[B 6 FI 5 ]