Nonahalogenodiantimon( III )ates; their preparation and the crystal structures of [Hpy] 3 [Sb 2 Cl 9 ], [NMe 4 ] 3 [Sb 2 Br 9 ], and [NMe 4 ] 3 [Sb 2 Br 3 Cl 6 ] Academic Article uri icon

abstract

  • Compounds of the type Y3[Sb2BrnCl9-n] {Y = Hpy [pyridinium(1+)], n = 0-9; Y = NMe4+, n = 0,3,6, and 9; and Y = Cs+, n = 0,3,6, and 9} have been prepared by a variety of methods and investigated by i.r. and Raman spectroscopy, mass spectrometry, and X-ray single crystal and powder diffraction. Two further mixed halides [Hpy][SbCl2X2] (X = Br or I) have also been isolated. Crystals of [Hpy]3[Sb2Cl9] are monoclinic, space group C2/c, with a = 29.168(8), b = 10.178(5), c = 9.425(5), β = 106.70(1)°, and Z = 4. Crystals of [NMe4]3[Sb2Br9] and [NMe4]3[Sb2Br3Cl6] are hexagonal, space group P63/mmc, Z = 2, with a = 9.499(4), c = 22.225(8) Å, and a = 9.341 (4), c = 22.038(9) Å respectively. The structure of [Hpy]3[Sb2Cl9] has been refined to R = 0.037 for 1 975 observed reflections and shows a polymeric structure with three terminal and three bridging chlorine atoms similar to that of β-Cs3[Sb2Cl9]. Refinement for the two tetramethylammonium salts (R = 0.140 for 385 and R = 0.115 for 408 observed reflections for the nona- and tri-bromides respectively) was very poor, probably as a consequence of disorder in the necessarily high symmetry of the space group but both show clearly confacial bioctahedral structures. In the mixed halide, the bridging positions are occupied by the bromine atoms.

altmetric score

  • 3

author list (cited authors)

  • Hall, M., Nunn, M., Begley, M. J., & Sowerby, D. B.

citation count

  • 41

publication date

  • January 1986