Synthesis, Characterization and Properties of a Novel Cationic Hexanuclear Cyclic Guanidinate Copper(I) Cluster of High Solubility in Non-polar Solvents

The reaction of copper(I) tetra-acetonitrile hexaflourophosphate with LiTEhpp (the lithium salt of 3,3,7,7-tetraethyl-1,3,4,6,7,8-hexahydro-2 H -pyrimido[1,2-α)pyrimidine) at low temperature (−80 °C) in THF under Schlenk conditions, produces a cluster salt tetrakis(3,3,9,9-tetraethyl-1,5,7-triazabic...

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Bibliographic Details
Published in:Journal of cluster science 2012-09, Vol.23 (3), p.823-838
Main Authors: Chiarella, Gina M., Melgarejo, Doris Y., Fackler, John P.
Format: Article
Language:English
Subjects:
Acetonitrile
Catalysis
Cations
Chemistry
Chemistry and Materials Science
Clusters
Copper
Copper chloride
Crystal structure
Crystals
Hexanes
Inorganic Chemistry
Ligands
Liquid nitrogen
Lithium
Low temperature
Nanochemistry
Nitrogen
Optical properties
Original Paper
Physical Chemistry
Software packages
Solubility
Solvents
Spectrum analysis
Synthesis
Toluene
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Summary:The reaction of copper(I) tetra-acetonitrile hexaflourophosphate with LiTEhpp (the lithium salt of 3,3,7,7-tetraethyl-1,3,4,6,7,8-hexahydro-2 H -pyrimido[1,2-α)pyrimidine) at low temperature (−80 °C) in THF under Schlenk conditions, produces a cluster salt tetrakis(3,3,9,9-tetraethyl-1,5,7-triazabicyclo[4.4.0]dec-4ene)bis(hexafluorophosphate)-hexa-copper(I), [Cu 6 (TEhpp) 4 )](PF 6 ) 2 ( 1 ). The cation is composed of an octahedral core of six copper(I) with four TEhpp ligands, each in a tri-coordinating fashion through two N atoms. This compound shows strong luminescent properties at liquid nitrogen temperature and is soluble in non-polar solvents such as toluene and hexane. The synthesis, spectroscopic properties and crystal structure are presented and discussed. The use of CuCl for the reaction with LiTEhpp yields a solution from which, in the presence of water, two mononuclear copper structures are produced in low yield, [Cu(II){(μ-O-(HTEhpp) 2 } 2 Cl][Cu(I)Cl 2 ], 2 , and Cu (TEhpp) 2 Cl, 3 .
ISSN:1040-7278
1572-8862
DOI:10.1007/s10876-012-0498-3