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

被引:51
作者
Zinn, AA [1 ]
Zheng, ZP [1 ]
Knobler, CB [1 ]
Hawthorne, MF [1 ]
机构
[1] UNIV CALIF LOS ANGELES,DEPT CHEM & BIOCHEM,LOS ANGELES,CA 90095
关键词
D O I
10.1021/ja952474h
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
Hexamethyl[9]mercuracarborand-3, [(CH3)(2)C2B10H8Hg](3) (3), was isolated in 60% yield from the reaction of closo-1,2-Li-2-9,12-(CH3)(2)-1,2-C2B10H8 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 P (1) over bar with a = 13.362(6) Angstrom, b = 14.071(6) Angstrom, and c = 14.303(6) Angstrom, alpha = 105.15(1)degrees, beta = 95.77(1)degrees, and gamma = 110.14(1)degrees, V = 2383 Angstrom(3), and Z = 2. The final discrepancy indexes were R = 0.059, R(w) = 0.064 for 5987 independent reflections with (I > 3 sigma(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 Hg-199 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.
引用
收藏
页码:70 / 74
页数:5
相关论文
共 24 条
  • [1] [Anonymous], 1995, CONTEMP ORG SYNTH
  • [2] [Anonymous], 1974, INT TABLES XRAY CRYS, VIV
  • [3] BACH T, 1992, J CHEM SOC CHEM COMM, P1632
  • [4] THE VANDERWAALS RADIUS OF MERCURY
    CANTY, AJ
    DEACON, GB
    [J]. INORGANICA CHIMICA ACTA-LETTERS, 1980, 45 (06): : L225 - L227
  • [5] 1ST APPLICATION OF ATTRACTIVE INTRAMOLECULAR INTERACTIONS TO THE DESIGN OF CHIRAL CATALYSTS FOR HIGHLY ENANTIOSELECTIVE DIELS-ALDER REACTIONS
    COREY, EJ
    LOH, TP
    [J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1991, 113 (23) : 8966 - 8967
  • [6] GRIMES RN, 1993, ANGEW CHEM INT EDIT, V32, P1289, DOI 10.1002/anie.199312891
  • [7] GRIMES RN, 1970, CARBORANES, P66
  • [8] HOST-GUEST CHEMISTRY OF ANION-COMPLEXATION BY MACROCYCLIC MULTIDENTATE LEWIS-ACIDS
    HAWTHORNE, MF
    YANG, XG
    ZHENG, ZP
    [J]. PURE AND APPLIED CHEMISTRY, 1994, 66 (02) : 245 - 254
  • [9] SCANDIUM TRIFLUOROMETHANESULFONATE AS AN EXTREMELY ACTIVE ACYLATION CATALYST
    ISHIHARA, K
    KUBOTA, M
    KURIHARA, H
    YAMAMOTO, H
    [J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1995, 117 (15) : 4413 - 4414
  • [10] KIDD RG, 1978, NMR PERIOD TABLE, P195