[(CH3)2SnTe]3, C6HI8Sn3Te3, Mr = 8291, Mo Ka radiation, h. = 0.71069 A, T = 293 K: (1) monoclinic, P21/c, a = 14-681 (2), b = 10.2775 (8), c =13.561(3) A, fl=112-087(12) ° , V =1896-0A 3, Z = 4, Dx = 2.905 Mg m-3, /.1, = 8.45 mm-1, F(000) = 1439.9, R=0.034 for 1968 observed data; (2) tetragonal, 141/a, a = 12-710 (3), c = 22.757 (4) A, V=3676.3A 3, Z = 8 , Dx=2996Mgm-3 , /z= 8-72 ram-l , F(000) = 2879.8, R = 0-024 for 1507 observed data. In each form the molecule adopts a twist-boat conformation which, in the case of the tetragonal modification, displays crystallographic twofold symmetry. Experimental. [(CH3)2SnTe]3 was obtained in petroleum solution by Soxhlet extraction of the crude reaction product (Blecher & Drfiger, 1979; Gay, Jones & Sharma, 1989). Evaporation of the solvent at room temperature yielded a sample consisting mainly of thin yellow-green sheets and a few thicker plates of amber colour. The solid state l l9Sn and lZSTe NMR spectra (Gay et al., 1989) displayed multiple resonances suggesting that more than one crystalline form was present. A plate selected from this sample for X-ray analysis was found to have crystallized in the space group P2~/c. A different yellow crystal modification was formed exclusively when a saturated petroleum solution of [(CH3)2SnTe]3 was cooled to 255 K, as confirmed by its solid state !19Sn and ~25Te NMR spectra (Gay et al., 1989). X-ray analysis showed these crystals to be tetragonal, space group I4~/a. Attempts to convert this phase to the monoclinic form by heating were unsuccessful. At 343 K the solid material appeared to fuse to give an apparently polymeric material of negligible solubility in petroleum ether. In either case the crystals became black upon exposure to air for several mintues. Crystals were mounted on Pyrex filaments with five-minute epoxy resin and were protected from air exposure by a thin coating of resin. Cell-parameter determination (25 reflections 15.1 _< 0_< 19.1 °, P21/c; 24 reflections 20.3 _ 0_ 25-7 °, I41/a) and data acquisition were performed using an Enraf-Nonius CAD-4F diffractometer with Mo Ka radiation and a graphite monochromator. The symmetry of the intensity-weighted reciprocal lattices and the systematic absences were determined using the diffractometer. Two standard intensities were measured every hour of acquisition time and showed no systematic variations. An empirical absorption correction (North, Phillips & Mathews, 1968) was applied to the data in the case of the I4~/a modification because the irregular shape of the crystal made measurement of crystal faces impracticable. The correction factors applied to the intensities ranged from 1.0 to 0.813. In the P2~/c case, an analytical absorption correction (de Meulenaer & Tompa, 1965) was made (transmission coefficients ranging from 0.614 to 0.248). Data reduction, including Lorentz and polarization corrections, was performed. In both cases the coordinates for the Te and Sn atoms were determined by direct methods (Main, Woolfson & Germain, 1971). The C-atom positions were revealed by electron density difference Fourier syntheses. H atoms were fixed at calculated positions with assigned isotropic temperature factors, basing the rotational conformation of each CH3 group upon the positions of the strongest peaks near the C atoms from a difference Fourier map. The final, full-matrix least-squares refinement, minimizing 0108-2701/89/111813-03503.00 © 1989 International Union of Crystallography 1814 HEXAMETHYLCYCLOTRISTANNATELLURANE Table 1. Data-acquisition and refinement details for two modifications of [(CH3)2SnTe]3