Synthesis, crystal structure and properties of [Cu2(O2CC6H4Me-p)3(Me2NCH2CH2NMe2)2]PF6: an unprecedented [Cu2(μ-O2CR)4] into [Cu2(μ-O2CR)3]+ core conversion

Geetha, Kannappan ; Chakravarty, Akhil R. (1999) Synthesis, crystal structure and properties of [Cu2(O2CC6H4Me-p)3(Me2NCH2CH2NMe2)2]PF6: an unprecedented [Cu2(μ-O2CR)4] into [Cu2(μ-O2CR)3]+ core conversion Journal of the Chemical Society, Dalton Transactions, 1999 (10). pp. 1623-1628. ISSN 0300-9246

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Tris(μ-p-methylbenzoato-O,O')bis(N,N,N',N'-tetramethyl-1,2-diaminoethane)dicopper(II) hexafluorophosphate, [Cu2(O2CC6H4Me-p)3(tmen)2]PF61, was prepared from a reaction of [Cu2(O2CC6H4Me-p)4(H2O)2] with tmen in ethanol at 0°C and characterized by spectral, electrochemical, magnetic and X-ray crystallographic studies. The cationic complex consists of a dicopper(II) unit having three bridging carboxylates and two bidentate chelating tmen ligands. The co-ordination geometry of the copper centres is distorted square pyramidal (CuO3N2). The Cu···Cu distance in the core is unusually long, 3.419(2) Å. The Cu-O-C angles at two copper centres are drastically different. Magnetic studies in the temperature range 20-296 K show the presence of an antiferromagnetically coupled dicopper(II) unit giving -2J = 81.4 cm-1 and g = 2.081. Cyclic voltammetric studies have shown a cathodic peak at -0.92 V with an anodic response at 0.10 V vs. SCE at 100 mV s-1. The visible electronic spectrum of the complex shows a d-d band at 665 nm (ε=263 M-1 cm-1) in MeCN. The magnetostructural data among the syn, syn-carboxylato bridged dicopper(II) systems with a [Cu2(μ-O2CR)m]n+ (m=4−1; n=0−3) core show that while 1 structurally has a tricarboxylato bridged dicopper(II) unit, magnetically it behaves like a dibridged one.

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