u2212 with ceric 4 ammonium nitrate in acetonitrile to produce closo b 12 ch 3 12 u2212 by starting with closo b n h n u2212 where n 6 12 various different compounds of the formula closo b n ch 3 n u2212 can be produced the anion closo b 12 ch 3 12 u2212 was characterized by high resolution fast atom bombardment mass spectrometry hr fab ms electron paramagnetic resonance epr uv vis spectroscopy and cyclic voltammetry furthermore the crystal structure of ph 3 p u2550 n u2550 pph 3 closo b 12 ch 3 12 was determined by single crystal x ray diffraction negative hr fab ms found mlz 310 4022 calc 310 4014 crystal data for ph 3 p u2550 n u2550 pph 3 closo b 12 ch 3 12 is c 48 h 66 b 12 np 2 m 878 04 monoclinic a 3466 3 b 934 2 8 c 1869 2 pm u 5 120 7 nm 3 t 298 u00b0 k space group c2 cz 4 u03bc mo k u03b1 1 2 cm u2212 1 4900 unique reflections were measured 2489 reflections were considered observed i gt 2 u03b1 i and all data was used in all calculations the final r factor r u03c3 f o u2212 f c u03c3 f o was 0 066 for 2489 independent reflections the structure was solved using statistical methods and refined by full matrix least squares on f 2 ccdc 182 1405 crystallographic files are available in cif format at http www rsc org suppdata cc 1999 2039 blood red single crystals of c 5 h 5 n 2 ch 2 closo b 12 ch 3 12 ch 3 cn orthorhombic pc2 1 n a 971 5 7.