M. Touboul et G. Nowogrocki, DEHYDRATION PROCESS OF TLB5O6(OH)(4)CENTER-DOT-2H(2)O AND CRYSTAL-STRUCTURE OF TLB5O8, Journal of solid state chemistry, 136(2), 1998, pp. 216-220
The dehydration of TIB5O6(OH)(4) . 2H(2)O leads to a loss of water in
one step, forming anhydrous TIB5O8, which is amorphous to X-ray diffra
ction, This can be explained by structural considerations; a decrease
in oxygenated coordination of thallium ions occurs during the heating.
TIB5O8 crystallizes at about 450 degrees C and melts at 660 degrees C
, By slow cooling from the melt, single crystals were obtained. TIB5O8
is orthorhombic, space group Pbca, with unit cell parameters a = 7.55
7(3) Angstrom, b = 11.925(6) Angstrom, c = 14.734(19) Angstrom; Z = 8,
The structure was solved from 1113 reflections until R = 0.023 and R-
w = 0.026, The structure consists of two separate interlocking three-d
imensional networks of pentaborate groups, which form large empty tunn
els, Nine oxygen atoms belonging to four different pentaborate groups
surround each thallium ion. Except for the presence of pentaborate gro
ups with almost the same geometry, there is no relation between the st
ructure of TIB5O8 and that of its hydrated precursor, TIB5O6(OH)(4) .
2H(2)O; the shorthand notation of polyborate anions in these compounds
is 5:infinity(3)(4 Delta+T) and 5:4 Delta+T, respectively. (C) 1998 A
cademic Press.