Preparation of [I3Cl2]+[SbCl6]- and its characterization by x-ray crystallography and Raman spectroscopy
| Autor: | Ronald D. Myers, Thomas Birchall |
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| Rok vydání: | 1982 |
| Předmět: | |
| Zdroj: | Inorganic Chemistry. 21:213-217 |
| ISSN: | 1520-510X 0020-1669 |
| DOI: | 10.1021/ic00131a039 |
| Popis: | The X-ray crystal structure of 13SbC18 !as been determined from diffractometer data by the heavy-atom method. Crystals of 13SbC18 are triclinic, space group P1, with a = 7.090 (1) A, b = 11.591 (2) A, c = 7.126 (1) A, a = 122.29 (l)', 0 = 98.85 (l)', y = 115.86 (I)', V = 383.5 ( 1 ) A3, and ddd = 3.404 g cm-' for Z = 1. The structure was solved by Patterson and Fourier methods and refined by full-matrix least squares to RI = 0.032 and R2 = 0.040 for 1545 observed (I > 3 4 ) reflections. In an ionic approximation, the structure consists of planar centrosymmetric (C2& [IpC12]+ cations and slightly distorted octahedral [SbCI6]anions. A reasonably strong cation-anion interaction does exist however in the form of an iodine-chlorine bridging contact of 2.941 (1) A. The 1-1 and I-CI bond distances in the novel [I3CI2]+ cation are 2.9057 (6) and 2.333 (1) A, respectively. The Raman and visible absorption spectra of [13C12]+[SbC16]are nearly identical with those which have been reported previously for [12C1]+[SbC16]-. The unit cell parameters of crystals obtained from the reaction reported to produce [I2CI]+[SbCl6]have been determined from diffractometer measurements and were found to be the same as those which we report here for [I3CI2]+[SbCl6]-. These findings cast considerable doubt on the existence of the previously reported [IzX]+ (X = C1, Br) cations. |
| Databáze: | OpenAIRE |
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