Thallium triacetate monohydrate

Tl[C2HaO213.H20 , monoclinic, P2j/c, a = 9.311 (4), b = 14.341 (6), c = 9.198 (2)A, f l= 119.69 (2) °, V = 1067.0/k 3, M r = 399.5, Z = 4, D x = 2 . 4 9 M g m -3, g = 1 5 . 1 1 m m -1. The structure was refined by X-ray diffraction to R = 0 . 0 4 for 577 observed reflections. The T1 atom is irregularly coordinated by eight O atoms (T1-O = 2.17-2.78/~). The angles between adjacent bonds correlate with the strengths of the bonds. The molecules are linked by a bridging acetate O atom and a hydrogen bond into columns running along e. There is a simple relation between the structure of the monohydrate and the anhydrous triacetate. * catena-g-Acetato-O, g-O'-aquadiacetatothallium(III). 0567-7408/82/092473-03501.00 Introduction. Thallium triacetate monohydrate was prepared by dissolving 0.2 g of TI[CH3CO2] 3 (Alfa Products) in 10ml distilled water and leaving it uncovered at room temperature. Large colourless plates of the title compound appeared after several days. Since the crystals decomposed in a few hours when removed from the solution, the crystal used was ground to a cylinder and sealed in a Lindemann-glass capillary. The structure was determined by X-ray diffraction, experimental details being given in Table 1. When the structure had been fully refined with anisotropic temperature factors for T1 the largest positive and negative peaks in the residual electron density map were found in the neighbourhood of the T1 atom and were identified as arising from anisotropic extinction. Consequently the 15 strongest reflections were omitted © 1982 International Union of Crystallography Table 1. Summary of structure determination Crystal shape and size Diffractometer Radiation and wavelength Reflections used for measuring lattice parameters Absorption correction applied (max. and min.) Temperature Max. 20 measured Standard reflections Number of intensity measurements Number of unique reflections nl = (ZI IFol -Fcl I /ZIFol ) R 2 = [~,w(IFol IVcl)2/YwF~ol 'n R ~ for 15 strongest reflections with w = 0 Weighting scheme Error in an observation of unit weight Average, maximum (shift/error) Final difference synthesis: maximum minimum Isotropic secondary-extinction correction (Larson, 1967) F(000) Scattering factors 0.4, 2.0 [z(H41)l + 1 e A -3 in neighbourhood 2 e ./k -3 of Tl atom g = 2.8 x 10 -s 736 International Tables f o r X-ray Crystallography (1962) Table 3.3.1A (O,C,H) and Table 3.3.1B (T1) corrected for anomolous dispersion (Table 3.3.2C) Cylinder of radius 0.10 mm and length 0.3 mm along [ 112] Nicolet P21 Graphite-monochromatized Mo Kct, 2 = 0.71069 A 15 10.7 (20 = 0°), 9.6 (20 = 35 o) 293K 35 ° 233, 114, e.s.d. 1.2% 836 655 0.038 for 655 reflections 0.043 0.048 w = (o a ..... ,ns + 0.03 Fo2) -I w = 0 for 63 unobserved reflections with F c < F o and for the 15 strongest reflections. 1.18 Table 2. A tomic parameters for TI[ C H3C 0 2 ] 3.H 2 ° (x 10 4 except H x 10 3)