New di-ferrocenyl-ethynylpyridinyl triphenylphosphine copper halide complexes and related di-ferricenyl electro-crystallized materials

H.H. Shah, R.A. Al-Balushi, M.K. Al-Suti, M.S. Khan, F. Marken, A.L. Sudlow, Gabriele Kociok-Kohn, C.H. Woodall, P.R. Raithby, K.C. Molloy

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Abstract

Three new neutral di-ferrocenyl-ethynylpyridinyl copper complexes, [L (CuCl)(PPh)] (2), [L (CuBr)(PPh)] (3), and [L (CuI)(PPh)] (4) were synthesized from the ferrocenyl-ethynylpyridine ligand (L) (1), the appropriate copper halide CuX (with X = Cl, Br, I) and triphenylphosphine. These neutral complexes were fully characterized by spectroscopic methods and by single crystal X-ray crystallography. Cyclic voltammetry in dichloroethane revealed chemically reversible ferrocenyl oxidation signals followed by characteristic "stripping reduction peaks" showing evidence for oxidation-product electro-crystallization. Scanning electron microscopy confirmed spontaneous formation of crystalline oxidation products with three distinct morphologies for X = Cl, Br, I. Energy dispersive X-ray elemental analysis data show Fe:P ratios of 1:2.0, 1:2.1 and 1:2.1 for electro-crystallization products of complexes 2, 3, and 4, respectively, indicating the presence of two [PF ] anions in the vicinity of the dioxidized complexes, and suggesting product formulae [2][PF] , [3][PF] and [4][PF].
LanguageEnglish
Pages9497-9507
Number of pages11
JournalDalton Transactions
Volume43
Issue number25
DOIs
StatusPublished - 7 Jul 2014

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Copper
Crystallization
Oxidation
Platelet Factor 3
Ethylene Dichlorides
X ray crystallography
Cyclic voltammetry
Anions
Single crystals
Crystalline materials
Ligands
X rays
Scanning electron microscopy
Chemical analysis
triphenylphosphine
ethynylpyridine

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New di-ferrocenyl-ethynylpyridinyl triphenylphosphine copper halide complexes and related di-ferricenyl electro-crystallized materials. / Shah, H.H.; Al-Balushi, R.A.; Al-Suti, M.K.; Khan, M.S.; Marken, F.; Sudlow, A.L.; Kociok-Kohn, Gabriele; Woodall, C.H.; Raithby, P.R.; Molloy, K.C.

In: Dalton Transactions, Vol. 43, No. 25, 07.07.2014, p. 9497-9507.

Research output: Contribution to journalArticle

Shah, H.H. ; Al-Balushi, R.A. ; Al-Suti, M.K. ; Khan, M.S. ; Marken, F. ; Sudlow, A.L. ; Kociok-Kohn, Gabriele ; Woodall, C.H. ; Raithby, P.R. ; Molloy, K.C. / New di-ferrocenyl-ethynylpyridinyl triphenylphosphine copper halide complexes and related di-ferricenyl electro-crystallized materials. In: Dalton Transactions. 2014 ; Vol. 43, No. 25. pp. 9497-9507.
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abstract = "Three new neutral di-ferrocenyl-ethynylpyridinyl copper complexes, [L (CuCl)(PPh)] (2), [L (CuBr)(PPh)] (3), and [L (CuI)(PPh)] (4) were synthesized from the ferrocenyl-ethynylpyridine ligand (L) (1), the appropriate copper halide CuX (with X = Cl, Br, I) and triphenylphosphine. These neutral complexes were fully characterized by spectroscopic methods and by single crystal X-ray crystallography. Cyclic voltammetry in dichloroethane revealed chemically reversible ferrocenyl oxidation signals followed by characteristic {"}stripping reduction peaks{"} showing evidence for oxidation-product electro-crystallization. Scanning electron microscopy confirmed spontaneous formation of crystalline oxidation products with three distinct morphologies for X = Cl, Br, I. Energy dispersive X-ray elemental analysis data show Fe:P ratios of 1:2.0, 1:2.1 and 1:2.1 for electro-crystallization products of complexes 2, 3, and 4, respectively, indicating the presence of two [PF ] anions in the vicinity of the dioxidized complexes, and suggesting product formulae [2][PF] , [3][PF] and [4][PF].",
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AU - Al-Balushi, R.A.

AU - Al-Suti, M.K.

AU - Khan, M.S.

AU - Marken, F.

AU - Sudlow, A.L.

AU - Kociok-Kohn, Gabriele

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AU - Molloy, K.C.

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AB - Three new neutral di-ferrocenyl-ethynylpyridinyl copper complexes, [L (CuCl)(PPh)] (2), [L (CuBr)(PPh)] (3), and [L (CuI)(PPh)] (4) were synthesized from the ferrocenyl-ethynylpyridine ligand (L) (1), the appropriate copper halide CuX (with X = Cl, Br, I) and triphenylphosphine. These neutral complexes were fully characterized by spectroscopic methods and by single crystal X-ray crystallography. Cyclic voltammetry in dichloroethane revealed chemically reversible ferrocenyl oxidation signals followed by characteristic "stripping reduction peaks" showing evidence for oxidation-product electro-crystallization. Scanning electron microscopy confirmed spontaneous formation of crystalline oxidation products with three distinct morphologies for X = Cl, Br, I. Energy dispersive X-ray elemental analysis data show Fe:P ratios of 1:2.0, 1:2.1 and 1:2.1 for electro-crystallization products of complexes 2, 3, and 4, respectively, indicating the presence of two [PF ] anions in the vicinity of the dioxidized complexes, and suggesting product formulae [2][PF] , [3][PF] and [4][PF].

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