Alkaline earth complexes of a sterically demanding guanidinate ligand

The synthesis of the guanidine MesN{C(NCy2)}N(H)Mes (LH; Mes = 2,4,6-Me3C6H2, Cy = cyclohexyl), and its use as a proligand for the synthesis of alkaline earth metal complexes are reported. Described herein are (i) an unusual Hauser base cubane, (ii) a homoleptic and a base-stabilized magnesium compl...

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Main Authors: Moxey, Graeme J., Blake, Alexander J., Lewis, William, Kays, Deborah L.
Format: Article
Published: Wiley 2015
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Online Access:https://eprints.nottingham.ac.uk/31238/
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author Moxey, Graeme J.
Blake, Alexander J.
Lewis, William
Kays, Deborah L.
author_facet Moxey, Graeme J.
Blake, Alexander J.
Lewis, William
Kays, Deborah L.
author_sort Moxey, Graeme J.
building Nottingham Research Data Repository
collection Online Access
description The synthesis of the guanidine MesN{C(NCy2)}N(H)Mes (LH; Mes = 2,4,6-Me3C6H2, Cy = cyclohexyl), and its use as a proligand for the synthesis of alkaline earth metal complexes are reported. Described herein are (i) an unusual Hauser base cubane, (ii) a homoleptic and a base-stabilized magnesium complex featuring the same guanidinate ligands, and (iii) the comparison of a series of alkaline earth (Mg, Ca, Sr, Ba) bis(guanidinate) complexes, which allows the opportunity to compare the changing trends in bonding as the Group is descended. The reaction between LH and MeMgI(OEt2)2 yields the Hauser base as a mixture of the tetramer [Mg4L4(μ3-I)4] (1a) and dimer [Mg2L2(μ-I)2(OEt2)2] (1b), and the reaction with two equivalents of MgnBu2 leads to the formation of four-coordinate [MgL2] (2), which features a square-planar geometry for the magnesium cation, or five-coordinate [MgL2(THF)] (3), depending on the solvent used. 1a is the first crystallographically-characterized cubane structure to consist of four LAeX (L = ligand, X = halide) units. The complexes [AeL2(THF)2] (Ae = Ca, 4; Ae = Sr, 5) and [BaL2] (6) were synthesized via redox transmetallation/ligand exchange reactions. Complex 6 is the first example of a homoleptic, monomeric barium complex of the NCN ligand family, with the structure stabilized by a number of barium-arene interactions in the solid state.
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spelling nottingham-312382020-05-04T17:28:22Z https://eprints.nottingham.ac.uk/31238/ Alkaline earth complexes of a sterically demanding guanidinate ligand Moxey, Graeme J. Blake, Alexander J. Lewis, William Kays, Deborah L. The synthesis of the guanidine MesN{C(NCy2)}N(H)Mes (LH; Mes = 2,4,6-Me3C6H2, Cy = cyclohexyl), and its use as a proligand for the synthesis of alkaline earth metal complexes are reported. Described herein are (i) an unusual Hauser base cubane, (ii) a homoleptic and a base-stabilized magnesium complex featuring the same guanidinate ligands, and (iii) the comparison of a series of alkaline earth (Mg, Ca, Sr, Ba) bis(guanidinate) complexes, which allows the opportunity to compare the changing trends in bonding as the Group is descended. The reaction between LH and MeMgI(OEt2)2 yields the Hauser base as a mixture of the tetramer [Mg4L4(μ3-I)4] (1a) and dimer [Mg2L2(μ-I)2(OEt2)2] (1b), and the reaction with two equivalents of MgnBu2 leads to the formation of four-coordinate [MgL2] (2), which features a square-planar geometry for the magnesium cation, or five-coordinate [MgL2(THF)] (3), depending on the solvent used. 1a is the first crystallographically-characterized cubane structure to consist of four LAeX (L = ligand, X = halide) units. The complexes [AeL2(THF)2] (Ae = Ca, 4; Ae = Sr, 5) and [BaL2] (6) were synthesized via redox transmetallation/ligand exchange reactions. Complex 6 is the first example of a homoleptic, monomeric barium complex of the NCN ligand family, with the structure stabilized by a number of barium-arene interactions in the solid state. Wiley 2015-12-02 Article PeerReviewed Moxey, Graeme J., Blake, Alexander J., Lewis, William and Kays, Deborah L. (2015) Alkaline earth complexes of a sterically demanding guanidinate ligand. European Journal of Inorganic Chemistry, 2015 (36). pp. 5892-5902. ISSN 1434-1948 alkaline earth metals N ligands bidentate ligands ligand effects coordiination modes http://onlinelibrary.wiley.com/doi/10.1002/ejic.201501239/abstract doi:10.1002/ejic.201501239 doi:10.1002/ejic.201501239
spellingShingle alkaline
earth metals
N ligands
bidentate ligands
ligand effects
coordiination modes
Moxey, Graeme J.
Blake, Alexander J.
Lewis, William
Kays, Deborah L.
Alkaline earth complexes of a sterically demanding guanidinate ligand
title Alkaline earth complexes of a sterically demanding guanidinate ligand
title_full Alkaline earth complexes of a sterically demanding guanidinate ligand
title_fullStr Alkaline earth complexes of a sterically demanding guanidinate ligand
title_full_unstemmed Alkaline earth complexes of a sterically demanding guanidinate ligand
title_short Alkaline earth complexes of a sterically demanding guanidinate ligand
title_sort alkaline earth complexes of a sterically demanding guanidinate ligand
topic alkaline
earth metals
N ligands
bidentate ligands
ligand effects
coordiination modes
url https://eprints.nottingham.ac.uk/31238/
https://eprints.nottingham.ac.uk/31238/
https://eprints.nottingham.ac.uk/31238/