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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

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
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

The trianion Z3- 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.

0020-1669
1721-1728
McCormick, Laura J.
f1c2f8cd-adcc-4bbf-9289-0b33a006d2bb
Abrahams, Brendan F.
9d8972b1-63c7-4ee8-b5b6-5ccfbcf3f798
Boughton, Berin A.
a760d741-36c3-4102-8e66-940124fcb12c
Grannas, Martin J.
ea453983-cca0-4004-9449-52024b69cf7c
Hudson, Timothy A.
69f051ea-681a-4d09-80a9-caf625a78488
Robson, Richard
2c74c03e-58f1-4fc3-9b11-ff00e28d09c8
McCormick, Laura J.
f1c2f8cd-adcc-4bbf-9289-0b33a006d2bb
Abrahams, Brendan F.
9d8972b1-63c7-4ee8-b5b6-5ccfbcf3f798
Boughton, Berin A.
a760d741-36c3-4102-8e66-940124fcb12c
Grannas, Martin J.
ea453983-cca0-4004-9449-52024b69cf7c
Hudson, Timothy A.
69f051ea-681a-4d09-80a9-caf625a78488
Robson, Richard
2c74c03e-58f1-4fc3-9b11-ff00e28d09c8

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).

Record type: Article

Abstract

The trianion Z3- 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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e-pub ahead of print date: 22 January 2014
Published date: 3 February 2014

Identifiers

Local EPrints ID: 437897
URI: http://eprints.soton.ac.uk/id/eprint/437897
ISSN: 0020-1669
PURE UUID: 693fbbb3-50b6-46aa-81f4-a9755ed8ce6f
ORCID for Laura J. McCormick: ORCID iD orcid.org/0000-0002-6634-4717

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Date deposited: 24 Feb 2020 17:30
Last modified: 07 Oct 2020 02:27

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Contributors

Author: Brendan F. Abrahams
Author: Berin A. Boughton
Author: Martin J. Grannas
Author: Timothy A. Hudson
Author: Richard Robson

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