Synthesis, structure and cation-binding properties of some [4 + 4] metallocyclic MO₂²⁺ (M = Mo or W) derivatives of 9-phenyl-2,3,7-trihydroxyfluor-6-one

McCormick, Laura J., Abrahams, Brendan F., Boughton, Berin A., Grannas, Martin J., Hudson, Timothy A. and Robson, Richard (2014) Synthesis, structure and cation-binding properties of some [4 + 4] metallocyclic MO₂²⁺ (M = Mo or W) derivatives of 9-phenyl-2,3,7-trihydroxyfluor-6-one. Inorganic Chemistry, 53 (3), 1721-1728. (doi:10.1021/ic402860r).

Abstract

The trianion Z^3- obtained from 9-phenyl 2,3,7-trihydroxyfluor-6- one, ZH₃, affords dioxomolybdenum and dioxotungsten derivatives which contain [4 + 4] metallocycles of composition [(MO₂) ₄Z₄]^4- (M = Mo, W) in combination with a variety of counter cations. The syntheses, structures and ESMS of the following compounds are presented: compound 1, (MePPh₃)₃(NBu ₄)[(MoO₂)₄Z₄]; compound 2, (MePPh₃)₃(NBu₄)[(WO₂) ₄Z₄]; compound 3, (MePPh₃)₄[(WO ₂)₄Z₄]; compound 4, (PPh₄) ₂(NBu₄)₂[(MoO₂)₄Z ₄]; compound 5, (AsPh₄)₃(NBu ₄)[(MoO₂)₄Z₄]; compound 6, (AsPh₄)₂(NBu₄)₂[(WO ₂)₄Z₄]; compound 7, (Ph₃PNPPh ₃)(NBu₄)₃[(MoO₂)₄Z ₄]; compound 8, (Ph₃PNPPh₃)(NBu ₄)₃[(WO₂)₄Z₄]; compound 9, (NEt₄)(NBu₄)₃[(MoO₂) ₄Z₄]. The metallocycles in all of these compounds have similar structures, with the four metal centers located at the corners of a square slightly distorted, to varying degrees, toward a rhombus and also toward a tetrahedron. Various cations are bound inside the anionic metallocycles. ESI mass spectrometry shows that the metallocycles remain intact in the gas phase, forming [(MO₂)₄Z₄]^4-, {X-[(MO ₂)₄Z₄]}^3- and in some cases {X ₂-[(MO₂)₄Z₄]}^2- where X⁺ is an organic cation.

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Contributors

Author: Laura J. McCormick

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