A hexamethyl derivative of [9]mercuracarborand-3: Synthesis, characterization, and host-guest chemistry

Alfred A. Zinn; Zhiping Zheng; Carolyn B. Knobler; M. Frederick Hawthorne

doi:10.1021/ja952474h

A hexamethyl derivative of [9]mercuracarborand-3: Synthesis, characterization, and host-guest chemistry

Alfred A. Zinn, Zhiping Zheng, Carolyn B. Knobler, M. Frederick Hawthorne

Research output: Contribution to journal › Article › peer-review

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Abstract

Hexamethyl[9]mercuracarborand-3, [(CH₃)₂C₂B₁₀H₈Hg] ₃ (3), was isolated in 60% yield from the reaction of closo-1,2-Li₂-9,12-(CH₃)₂-1,2-C ₂B₁₀H₈ with mercuric acetate. The title compound was characterized by multinuclear NMR spectroscopy and its halide ion complexes by negative ion FAB mass spectrometry. Both 3 and its complexes are air-stable and soluble in poorly or noncoordinating solvents such as CH₂Cl₂ and toluene. Compound 3 crystallized from acetonitrile in the triclinic space group P1 with a = 13.362(6) Å, b = 14.071(6) Å, and c = 14.303(6) A, α = 105.15(1)°, β= 95.77(1)°, and γ = 110.14(1)°, V = 2383 Å³, and Z = 2. The final discrepancy indexes were R = 0.059, R_w = 0.064 for 5987 independent reflections with (1 > 3σ(I)). Halide ion complexes of 3 were formed upon treatment of 3 with salts of the corresponding halide ions. The complexation behavior of 3 in acetone was studied by ¹⁹⁹Hg NMR spectroscopy, and the guest/host ratio of the resulting complexes has been established to be 1, 2, and 2 for chloride, bromide, and iodide, respectively.

Original language	English (US)
Pages (from-to)	70-74
Number of pages	5
Journal	Journal of the American Chemical Society
Volume	118
Issue number	1
DOIs	https://doi.org/10.1021/ja952474h
State	Published - Jan 10 1996
Externally published	Yes

ASJC Scopus subject areas

Catalysis
General Chemistry
Biochemistry
Colloid and Surface Chemistry

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title = "A hexamethyl derivative of [9]mercuracarborand-3: Synthesis, characterization, and host-guest chemistry",

abstract = "Hexamethyl[9]mercuracarborand-3, [(CH3)2C2B10H8Hg] 3 (3), was isolated in 60% yield from the reaction of closo-1,2-Li2-9,12-(CH3)2-1,2-C 2B10H8 with mercuric acetate. The title compound was characterized by multinuclear NMR spectroscopy and its halide ion complexes by negative ion FAB mass spectrometry. Both 3 and its complexes are air-stable and soluble in poorly or noncoordinating solvents such as CH2Cl2 and toluene. Compound 3 crystallized from acetonitrile in the triclinic space group P1 with a = 13.362(6) {\AA}, b = 14.071(6) {\AA}, and c = 14.303(6) A, α = 105.15(1)°, β= 95.77(1)°, and γ = 110.14(1)°, V = 2383 {\AA}3, and Z = 2. The final discrepancy indexes were R = 0.059, Rw = 0.064 for 5987 independent reflections with (1 > 3σ(I)). Halide ion complexes of 3 were formed upon treatment of 3 with salts of the corresponding halide ions. The complexation behavior of 3 in acetone was studied by 199Hg NMR spectroscopy, and the guest/host ratio of the resulting complexes has been established to be 1, 2, and 2 for chloride, bromide, and iodide, respectively.",

author = "Zinn, {Alfred A.} and Zhiping Zheng and Knobler, {Carolyn B.} and Hawthorne, {M. Frederick}",

year = "1996",

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T1 - A hexamethyl derivative of [9]mercuracarborand-3

T2 - Synthesis, characterization, and host-guest chemistry

AU - Zinn, Alfred A.

AU - Zheng, Zhiping

AU - Knobler, Carolyn B.

AU - Hawthorne, M. Frederick

PY - 1996/1/10

Y1 - 1996/1/10

N2 - Hexamethyl[9]mercuracarborand-3, [(CH3)2C2B10H8Hg] 3 (3), was isolated in 60% yield from the reaction of closo-1,2-Li2-9,12-(CH3)2-1,2-C 2B10H8 with mercuric acetate. The title compound was characterized by multinuclear NMR spectroscopy and its halide ion complexes by negative ion FAB mass spectrometry. Both 3 and its complexes are air-stable and soluble in poorly or noncoordinating solvents such as CH2Cl2 and toluene. Compound 3 crystallized from acetonitrile in the triclinic space group P1 with a = 13.362(6) Å, b = 14.071(6) Å, and c = 14.303(6) A, α = 105.15(1)°, β= 95.77(1)°, and γ = 110.14(1)°, V = 2383 Å3, and Z = 2. The final discrepancy indexes were R = 0.059, Rw = 0.064 for 5987 independent reflections with (1 > 3σ(I)). Halide ion complexes of 3 were formed upon treatment of 3 with salts of the corresponding halide ions. The complexation behavior of 3 in acetone was studied by 199Hg NMR spectroscopy, and the guest/host ratio of the resulting complexes has been established to be 1, 2, and 2 for chloride, bromide, and iodide, respectively.

AB - Hexamethyl[9]mercuracarborand-3, [(CH3)2C2B10H8Hg] 3 (3), was isolated in 60% yield from the reaction of closo-1,2-Li2-9,12-(CH3)2-1,2-C 2B10H8 with mercuric acetate. The title compound was characterized by multinuclear NMR spectroscopy and its halide ion complexes by negative ion FAB mass spectrometry. Both 3 and its complexes are air-stable and soluble in poorly or noncoordinating solvents such as CH2Cl2 and toluene. Compound 3 crystallized from acetonitrile in the triclinic space group P1 with a = 13.362(6) Å, b = 14.071(6) Å, and c = 14.303(6) A, α = 105.15(1)°, β= 95.77(1)°, and γ = 110.14(1)°, V = 2383 Å3, and Z = 2. The final discrepancy indexes were R = 0.059, Rw = 0.064 for 5987 independent reflections with (1 > 3σ(I)). Halide ion complexes of 3 were formed upon treatment of 3 with salts of the corresponding halide ions. The complexation behavior of 3 in acetone was studied by 199Hg NMR spectroscopy, and the guest/host ratio of the resulting complexes has been established to be 1, 2, and 2 for chloride, bromide, and iodide, respectively.

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A hexamethyl derivative of [9]mercuracarborand-3: Synthesis, characterization, and host-guest chemistry

Abstract

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