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The reaction of SbI 3  with Me 4 NI, Me 3 SI. and Me 3 NCH 2 PhI in acetonitrile (molar ratios 2:1) yields (Me 4 N) 4 Sb 8 I 28  (I), (Me 3 S) 4 Sb 8 I 28  (2), and (Me 3 NCH 2 Ph)Sb 2 I 7  (3), respectively. The struc­tures of 1-3 were determined from single crystal X-ray diffraction data. 1-3 crystallize in the monoclinic space group P2 1 /n. 2: a = 1434.2(3). b = 1484.1(4). c = 2102.6(4) pm, β = 105.4(1)°, Z = 2. I: a = 1441.7(1). b = 1545.1(1). c = 2117.3(1) pm. β = 106.4(1)°, Z = 2. 3: a = 1004.4(1). b = 1378.8(1). c = 1899.3(2) pm. β = 94.2(1)°. Z = 4. The structures of I and 2 are very similar and consist of isolated cations and anions. The Sb 8 I 28  4-  ions of 1 and 2 and the anion of the same stoichiometry of (Ph 4 P) 4 Sb 8 I 28  exhibit different struc­tures with a nearly identical Sb 4 I 16  core. The anions of 3 are built up of polymeric cfiains.

zeitschrift für naturforschung b

Iodoantimonate der Zusammensetzung A + Sb 2 I 7  -  : Diskrete Anionen in (Me 4 N) 4 Sb 8 I 28  und (Me 3 S) 4 Sb 8 I 28  , polymere Ketten in (Me 3 NCH 2 Ph)Sb 2 I 7  (Me = CH 3  , Ph = C 6 H 5  )