D. Fenske et al., CRYSTAL-STRUCTURE OF (PH(3)PNH(2))(4)[SB6 O10CL14]CENTER-DOT-2CH(3)CN, Zeitschrift fur Naturforschung. B, A journal of chemical sciences, 49(7), 1994, pp. 983-986
The title compound has been obtained by the reaction of the phosphoran
eiminato complex Cl2Sb(NPPh(3)) with chlorine, followed by partial hyd
rolysis in acetonitrile. The colourless crystals were characterized by
a crystal structure determination. Space group P ($) over bar 1, Z =
2, structure refinement with 8320 observed unique reflections, R = 0.0
63 with I > 2 sigma(I). Lattice dimensions at -70 degrees C: a=1245.0(
6); b=1277.7(8), c=1623.8(9) pm, alpha = 77.97(2)degrees, beta = 86.52
(2)degrees, gamma = 67.07(2)degrees. The compound consists of Ph(3)PNH
(2)(+) ions, [Sb6O10Cl14](4-) ions, in which the central unit is a Sb4
O6 Skeleton with a double heterocubane-like arrangement with two missi
ng corners, and of included acetonitrile molecules without bonding int
eractions.