TY - JOUR
T1 - New di-ferrocenyl-ethynylpyridinyl triphenylphosphine copper halide complexes and related di-ferricenyl electro-crystallized materials
AU - Shah, Hakikulla H.
AU - Al-Balushi, Rayya A.
AU - Al-Suti, Mohammed K.
AU - Khan, Muhammad S.
AU - Marken, Frank
AU - Sudlow, Anna L.
AU - Kociok-Köhn, Gabriele
AU - Woodall, Christopher H.
AU - Raithby, Paul R.
AU - Molloy, Kieran C.
PY - 2014/7/7
Y1 - 2014/7/7
N2 - Three new neutral di-ferrocenyl-ethynylpyridinyl copper complexes, [L 2(CuCl)2(PPh3)2] (2), [L 2(CuBr)2(PPh3)2] (3), and [L 2(CuI)2(PPh3)2] (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 6]- anions in the vicinity of the dioxidized complexes, and suggesting product formulae [2]2+[PF6] -2, [3]2+[PF6]- 2 and [4]2+[PF6]-2.
AB - Three new neutral di-ferrocenyl-ethynylpyridinyl copper complexes, [L 2(CuCl)2(PPh3)2] (2), [L 2(CuBr)2(PPh3)2] (3), and [L 2(CuI)2(PPh3)2] (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 6]- anions in the vicinity of the dioxidized complexes, and suggesting product formulae [2]2+[PF6] -2, [3]2+[PF6]- 2 and [4]2+[PF6]-2.
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U2 - 10.1039/c3dt52914b
DO - 10.1039/c3dt52914b
M3 - Article
AN - SCOPUS:84902108525
SN - 1477-9226
VL - 43
SP - 9497
EP - 9507
JO - Dalton Transactions
JF - Dalton Transactions
IS - 25
ER -