NDLI: Spectroscopy and structures of two complete families, one mononuclear, the other binuclear, of 1 : 2 CuX : dptu stoichiometry (X = Cl, Br, I; ‘dptu’ = <i>N</i>,<i>N</i>′-diphenylthiourea)

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Spectroscopy and structures of two complete families, one mononuclear, the other binuclear, of 1 : 2 CuX : dptu stoichiometry (X = Cl, Br, I; ‘dptu’ = N,N′-diphenylthiourea)

Content Provider	Royal Society of Chemistry (RSC)
Author	White, Allan H. Chaichit, Narongsak Pakawatchai, Chaveng Skelton, Brian W. Hanna, John V. Bowmaker, Graham A.
Copyright Year	2009
Abstract	Crystallization of the copper(I) halides (CuX; X = Cl, Br, I) with N,N′-diphenylthiourea (‘dptu’ = (PhNH)2CS) in 1 : 2 ratio from acetonitrile solution in ambient conditions yields a mononuclear isomorphous series of complexes of the form [XCu(dptu)2]·H2O, an unusually complete array, with the central copper atoms in quasi-trigonal planar environments, as shown by single crystal X-ray studies, in turn providing a platform for comparative spectroscopic studies. Under anhydrous conditions, anhydrous compounds may be obtained, a full series again being accessible, but now of the binuclear form [(dptu)XCu(μ-S-dptu)2CuX(dptu)], the chloride being a bis(acetonitrile) solvate, the isomorphous bromide and iodide pair being unsolvated. A (solvated) sulfate salt is found to be of the form [Cu(dptu)2]2(SO4), providing a novel example of a copper(I) atom being (quasi-)linearly coordinated by the pair of unidentate (dptu) sulfur ligands, Cu–S 2.1770(5), 2.1811(5) Å, S–Cu–S 162.18(2)°. The ν(CuX) vibrational frequencies are assigned in the far-IR spectra of [XCu(dptu)2]·H2O (X = Cl, Br, I) at 274, 207, and 190 cm−1 respectively. The broadline static 65Cu NMR spectra of [Cl2Cu2(dptu)4]·2CH3CN and [X2Cu2(dptu)4] (X = Br, I) have been recorded at 9.4 and 7.05 T, and the spectra have been analysed to yield the 65Cu nuclear quadrupole coupling and chemical shift parameters. The 63,65Cu nuclear quadrupole resonance frequencies of [XCu(dptu)2]·H2O (X = Cl, Br, I) have also been measured, and the resulting 65Cu quadrupole coupling constants are ca. 4× those of the dimeric [X2Cu2(dptu)4] compounds.
Starting Page	8308
Ending Page	8316
Page Count	9
File Format	HTM / HTML PDF
ISSN	14779226
Volume Number	0
Issue Number	39
Journal	Dalton Transactions
DOI	10.1039/b909167j
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Open
Subject Keyword	Cu Copper Acetonitrile Water of crystallization X-ray crystallography Chloride Bromide Iodide Sulfate Denticity Sulfur Nuclear magnetic resonance Quadrupole Chemical shift Nuclear quadrupole resonance
Content Type	Text
Resource Type	Article
Subject	Inorganic Chemistry

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