"Anti-crown" chemistry: Synthesis of [9]mercuracarborand-3 and the crystal structure of its acetonitrile complexes

Xiaoguang Yang, Zhiping Zheng, Carolyn B. Knobler, M. Frederick Hawthorne

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Abstract

The reaction of mercuric acetate with closo-1,2-Li2-1,2-C2B10H10 yielded [9]mercuracarborand-3, (C2B10H10Hg)3 (1), in 60% yield. Compound 1 was characterized by multinuclear NMR spectroscopy and its chloride ion complex, 1-C1-1, by negative ion FAB mass spectroscopy. The structure of 1 was determined by X-ray crystallography. 1 crystallized from acetonitrile in the monoclinic space group P21/c with a = 13.358 (2), b = 26.846 (4), and c = 20.375 Å, β = 109.694 (5)°, V = 7909 Å3, and Z = 4. Data were collected on a Picker FACS-1 diffractometer, using Mo Kα radiation, to a maximum 2θ = 45°, giving 10 348 unique reflections, and the structure was solved by heavy atom methods. The final discrepancy index was R = 0.044, Rw = 0.049 for 5193 independent reflections with I > 3σ(I). The chloride ion complex of 1,1·C1Li, was formed upon treatment of 1 with LiCl. The complexation behavior of 1 in acetone was studied by 199Hg NMR spectroscopy.

Original languageEnglish (US)
Pages (from-to)193-195
Number of pages3
JournalJournal of the American Chemical Society
Volume115
Issue number1
StatePublished - 1993
Externally publishedYes

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Acetonitrile
Crowns
Nuclear magnetic resonance spectroscopy
Chlorides
Crystal structure
Ions
X ray crystallography
Diffractometers
Magnetic Resonance Spectroscopy
Acetone
Complexation
Biomolecular Nuclear Magnetic Resonance
Negative ions
X Ray Crystallography
Spectroscopy
Radiation
Atoms
Mass Spectrometry
mercuracarborand-3
acetonitrile

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

"Anti-crown" chemistry : Synthesis of [9]mercuracarborand-3 and the crystal structure of its acetonitrile complexes. / Yang, Xiaoguang; Zheng, Zhiping; Knobler, Carolyn B.; Hawthorne, M. Frederick.

In: Journal of the American Chemical Society, Vol. 115, No. 1, 1993, p. 193-195.

Research output: Contribution to journalArticle

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abstract = "The reaction of mercuric acetate with closo-1,2-Li2-1,2-C2B10H10 yielded [9]mercuracarborand-3, (C2B10H10Hg)3 (1), in 60{\%} yield. Compound 1 was characterized by multinuclear NMR spectroscopy and its chloride ion complex, 1-C1-1, by negative ion FAB mass spectroscopy. The structure of 1 was determined by X-ray crystallography. 1 crystallized from acetonitrile in the monoclinic space group P21/c with a = 13.358 (2), b = 26.846 (4), and c = 20.375 {\AA}, β = 109.694 (5)°, V = 7909 {\AA}3, and Z = 4. Data were collected on a Picker FACS-1 diffractometer, using Mo Kα radiation, to a maximum 2θ = 45°, giving 10 348 unique reflections, and the structure was solved by heavy atom methods. The final discrepancy index was R = 0.044, Rw = 0.049 for 5193 independent reflections with I > 3σ(I). The chloride ion complex of 1,1·C1Li, was formed upon treatment of 1 with LiCl. The complexation behavior of 1 in acetone was studied by 199Hg NMR spectroscopy.",
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AU - Hawthorne, M. Frederick

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