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Issue 18, 1977
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Crystal structure of, and solution adduct equilibria involving, tetraphenylarsonium tetrachloro-oxochromate(V)

Abstract

Crystals of the title complex are tetragonal, space group P4/n, with a= 12.590(7), c= 7.840(5)Å, and Z= 2. The crystal structure has been solved by the heavy-atom method and refined by full-matrix least-squares calculations to R 0.059 over 860 statistically signrfrcant reflections from diffractometer measurements (Cu-Kα radiation). The square-pyramidal [CrCl4O] anion has crystallographic 4mm(C4v) symmetry with Cr–O 1.519(12) and Cr–Cl 2.240(3)Å, and O–Cr–Cl 104.5(1)°. The [AsPh4]+ cation has crystallographic [4 with combining macron](S4) symmetry [As–C 1.906(6)Å C–As–C 105.3(3) and 111.5(3)°]. E.s r. spectroscopy has been used to estimate the equilibrium constants for the reaction [CrCl4O]+ L [graphic omitted] [CrCl4OL]n in CH2Cl2solution {n= 1 when L = PPh3O (K= 3 ± 2), P(NMe2)3O (K= 463 ± 130), thf (K < 1), or py (K= 160); n= 2 when L = Cl(K= 43 ± 10 with [AsPh4]Cl and 250 ± 33 dm3 mol–1 with [NEt4]Cl)}.

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Article type: Paper
DOI: 10.1039/DT9770001726
Citation: J. Chem. Soc., Dalton Trans., 1977,0, 1726-1729
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    Crystal structure of, and solution adduct equilibria involving, tetraphenylarsonium tetrachloro-oxochromate(V)

    B. Gahan, D. C. Garner, L. H. Hill, F. E. Mabbs, K. D. Hargrave and A. T. McPhail, J. Chem. Soc., Dalton Trans., 1977, 0, 1726
    DOI: 10.1039/DT9770001726

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