TY - JOUR
T1 - “Anti-Crown” Chemistry
T2 - Synthesis of [9]Mercuracarborand-3 and the Crystal Structure of Its Acetonitrile Complexes
AU - Yang, Xiaoguang
AU - Zheng, Zhiping
AU - Knobler, Carolyn B.
AU - Hawthorne, M. Frederick
PY - 1993/1/1
Y1 - 1993/1/1
N2 - The reaction of mercuric acetate with closo-1,2-Li2-l,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·Cl−, 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, Å = 109.694 (5)°, V = 7909 Å3, and Z = 4. Data were collected on a Picker FACS-1 diffractometer, using Mo Kβ radiation, to a maximum 28 = 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·ClLi, was formed upon treatment of 1 with LiCl. The complexation behavior of 1 in acetone was studied by 199Hg NMR spectroscopy.
AB - The reaction of mercuric acetate with closo-1,2-Li2-l,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·Cl−, 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, Å = 109.694 (5)°, V = 7909 Å3, and Z = 4. Data were collected on a Picker FACS-1 diffractometer, using Mo Kβ radiation, to a maximum 28 = 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·ClLi, 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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U2 - 10.1021/ja00054a026
DO - 10.1021/ja00054a026
M3 - Article
AN - SCOPUS:0000282709
SN - 0002-7863
VL - 115
SP - 193
EP - 195
JO - Journal of the American Chemical Society
JF - Journal of the American Chemical Society
IS - 1
ER -