Abstract
The crystal structure of Cs2(B12H12) has been determined from X-ray single-crystal data collected at room temperature. Dicesium dodecahydro-closo-dodecaborate crystallizes as colourless, face-rich crystals (cubic, Fm 3; a = 1128.12(7) pm; Z = 4). Its synthesis is based on the reac- tion of Na(BH4) with BF3(O(C2H5)2) via the decomposition of Na(B3H8) in boiling diglyme, followed by subsequent se- parations, precipitations (with aqueous CsOH solution) and recrystallizations. The crystal structure is best described as anti-CaF2-type arrangement with the Cs + cations in all tetra- hedral interstices of the cubic closest-packed host lattice of the icosahedral (B12H12) 2- -cluster dianions. The intramolecu- lar bond lengths are in the range usually found in closo-hy- droborates: 178 pm for the B-B and 112 pm for the B-H dis- tance. Twelve hydrogen atoms belonging to four (B12H12) 2- icosahedra provide an almost perfect cuboctahedral coordi- nation sphere to the Cs + cations, and their distance of 313 pm (12 ·) attests for the salt-like character of Cs2(B12H12) according to 3{(Cs + )2((B12H12) 2- )}. The 11 B{ 1 H}-NMR data in aqueous (D2O) solution are d = -12,70 ppm ( 1 JB-H = 125 Hz), and d = -15,7 ppm (linewidth: Dm1/2 = 295 Hz) for the solid state 11 B-MAS-NMR.
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