Syntheses and Crystal Structures of the closo-Borates M2[B7H7] and M[B7H8] (M = PPh4, PNP, and N(n-Bu4)): the Missing Crystal Structure in the Series [BnHn]2- (n=6-12)

被引:20
|
作者
Schlueter, Florian [1 ]
Bernhardt, Eduard [1 ]
机构
[1] Berg Univ GH Wuppertal, Fachbereich Anorgan Chem C, D-42097 Wuppertal, Germany
关键词
SPIN COUPLING-CONSTANTS; BORANE ANIONS; PERTURBATION-THEORY; BOND-LENGTH; CHEMISTRY; APPROXIMATION; NONRIGIDITY; EXCHANGE;
D O I
10.1021/ic102434t
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Oxidation of [N(n-Bu-4)](2)[B9H9] with oxygen in a mixture of dimethoxyethane and CH2Cl2 leads to salts of the [B7H7](2-) dianion. This is the first convenient synthesis for a seven-vertex hydro-closo-borate anion. Protonation with NEt3 center dot HCl resulted in salts of the [B7H8](-) monoanion. Both closo-borate anions were isolated and characterized by H-1, H-1{B-11}, B-11, and B-11{H-1} NMR spectroscopy. The temperature-dependent H-1{B-11}, B-11, and B-11{H-1} NMR spectra of [B7H8](-) were also measured. The structure of [B7H7](2-) as well as of [B7H8](-) were determined by single-crystal X-ray diffraction.
引用
收藏
页码:2580 / 2589
页数:10
相关论文
共 50 条
  • [1] Syntheses and Crystal Structures of the closo-Borate M[B8H9] (M = [PPh4]+ and [N(n-Bua)4]+)
    Schlueter, Florian
    Bernhardt, Eduard
    INORGANIC CHEMISTRY, 2012, 51 (01) : 511 - 517
  • [2] Selenocyanato derivatives of hydro-closo-borates: Syntheses and crystal structures of (PPh(4))(2)[(SeCN)BnHn-1] (n=6, 10, 12)
    Nachtigal, C
    Steuer, B
    Preetz, W
    CHEMISCHE BERICHTE-RECUEIL, 1996, 129 (12): : 1531 - 1534
  • [3] CRYSTAL STRUCTURE OF [Mn(1,10-C12H8N2)3](B6H7)2
    Polyanskaya, T. M.
    Drozdova, M. K.
    Volkov, V. V.
    Myakishev, K. G.
    JOURNAL OF STRUCTURAL CHEMISTRY, 2009, 50 (02) : 368 - 372
  • [4] Crystal structure of [Mn(1,10-C12H8N2)3](B6H7)2
    T. M. Polyanskaya
    M. K. Drozdova
    V. V. Volkov
    K. G. Myakishev
    Journal of Structural Chemistry, 2009, 50 : 368 - 372
  • [5] CRYSTAL AND MOLECULAR-STRUCTURE OF [N(N-C4H9)4]+[FE(CO)4B7H12]-
    MANGION, M
    CLAYTON, WR
    HOLLANDER, O
    SHORE, SG
    INORGANIC CHEMISTRY, 1977, 16 (08) : 2110 - 2114
  • [6] Crystal structure of 2-(methylthio)thiazolo[4,5-b]pyridine, C7H6N2S2
    Ren, Yun-Lai
    Tian, Xin-Zhe
    Sun, Yan-Pei
    Liu, Gui-Hua
    ZEITSCHRIFT FUR KRISTALLOGRAPHIE-NEW CRYSTAL STRUCTURES, 2014, 229 (03): : 201 - 202
  • [7] Isoselenocyanatoborates - Crystal structures of (n-Bu4N)[BH(NCSe)3] and (Ph4P)[B3H7(NCSe)]
    Steuer, B.
    Preetz, W.
    Zeitschrift fur Naturforschung - Section B Journal of Chemical Sciences, 1998, 53 (03): : 271 - 274
  • [9] Isoselenocyanatoborates -: Crystal structures of (n-Bu4N)[BH(NCSe)3] and (Ph4P)[B3H7(NCSe)]
    Steuer, B
    Preetz, W
    ZEITSCHRIFT FUR NATURFORSCHUNG SECTION B-A JOURNAL OF CHEMICAL SCIENCES, 1998, 53 (03): : 271 - 274
  • [10] THE CRYSTAL-STRUCTURES OF DIAQUATETRA(BETA-PICOLINE)M(II) PERCHLORATE, [CU(H2O)2(C6H7N)4](CLO4)2 [CO(H2O)2(C6H7N)4](CLO4)2
    HU, S
    BARTON, RJ
    JOHNSON, KJ
    ROBERTSON, BE
    CANADIAN JOURNAL OF CHEMISTRY-REVUE CANADIENNE DE CHIMIE, 1983, 61 (02): : 395 - 399