Chromyl Complexes with Aryloxy and Siloxy Ligands

Abstract

Interaction of CrO 3 and 1 equiv of Ph 3CCl in dichloromethane yields a mixture of CrO 2Cl 2, CrO 2Cl(OCPh 3) (1), and CrO 2-(OCPh 3) 2 (2). Fractional crystallization gives pure samples of red 1 and orange 2, which have been characterized by X-ray diffraction. Crystal data for 1: space group P1; a = 9.913 (3), b = 10.173 (3), c = 9.019 (3) Å; α = 92.93 (2), β = 92.74 (2), γ = 110.84 (3)°; Z = 2; R 1 = 0.044, R 2 = 0.059. Crystal data for 2: space group C2/c; a = 23.857 (6), b = 8.759 (3), c = 15.105 (5) Å; β = 110.48 (3)°; Z = 4; R 1 = 0.036, R 2 = 0.057. A similar result was obtained on reaction of CrO 3 and 1 equiv of Ph 3SiCl, giving CrO 2Cl 2, CrO 2Cl(OSiPh 3) (3), and CrO 2(OSiPh 3) 2 (4). These results are compared with the in situ systems CrO 3/Me 3SiCl and CrO 3/Me 3SiOSiMe 3, which have been studied by 1H NMR spectroscopy and EI mass spectrometry.

Department(s)

Chemistry

International Standard Serial Number (ISSN)

0020-1669

Document Type

Article - Journal

Document Version

Citation

File Type

text

Language(s)

English

Rights

© 1990 American Chemical Society (ACS), All rights reserved.

Publication Date

01 May 1990

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