High‐Yield Syntheses of Sodium, Potassium, and Thallium Hydrotris[3,5‐bis(trifluoromethyl)pyrazolyl]borates and the X‐ray crystal structure of {hydrotris[3,5‐bis(trifluoromethyl)pyrazolyl]borato} thallium(I)
Authors:
- 28 June 1995
- journal article
- research article
- Published by Wiley in Helvetica Chimica Acta
- Vol. 78 (4) , 993-1000
Abstract
An improved synthesis of 3,5‐bis(trifluoromethyl)pyrazole (1) is described. This compound was used for the high‐yield syntheses of the tris(pyrazoly1)borates Nd[HB(3,5‐(CF3),‐pz)3] (2a) and the corresponding potassium salt, 2b, starting from 1 and NaBH4 and KBH4, respectively. A convenient route to the corresponding thallium(I) salt, 2c, using thallium(I) acetate and either 2a or 2b in CHCI3, is also described. The sodium (3a), potassium (3b), and thallium (3c) salts of bis(pyrazolyl)borate [H2B(3,5‐(CF3)2‐pz)2]− were also prepared. The above pyrazolylborates were characterized by 1H‐, 13C‐, 19F‐, and 11B‐NMR spectroscopy. The X‐ray crystal structure of the thallium derivative 2c was determined. The compound crystallizes in the monoclinic space group P21/m with a = 8.248(9) Å, b = 15.034(12) Å c = 9.243(8) Å, β = 100.10(7)°, Z = 2. The Tl‐atom adopts a pyramidal geometry with respect to the three N‐atoms. However, two TI–N distances (2.725(7) Å) are longer than the third (2.675(10) Å).Keywords
This publication has 37 references indexed in Scilit:
- Homoscorpionate (Tris(pyrazolyl)borate) Ligands Containing Tethered 3-Phenyl GroupsInorganic Chemistry, 1994
- The reaction of 1,1,1,5,5,5-hexafluoropentane-2,4-dione with hydrazines: a re-investigationJournal of Fluorine Chemistry, 1993
- Fixation of atmospheric carbon dioxide by a series of hydroxo complexes of divalent metal ions and the implication for the catalytic role of metal ion in carbonic anhydrase. Synthesis, characterization, and molecular structure of [LM(OH)]n (n = 1 or 2) and LM(.mu.-CO3)ML (M(II) = Mn, Fe, Co, Ni, Cu, Zn; L = HB(3,5-iso-Pr2pz)3)Journal of the American Chemical Society, 1993
- A single model displaying all the important centers and processes involved in catalysis by molybdoenzymes containing [MoVIO2]2+ active sitesJournal of the American Chemical Society, 1992
- Synthesis and structural characterization of a mononuclear copper nitrosyl complexJournal of the American Chemical Society, 1992
- 3,5-Bis(trifluoromethyl)pyrazole and some N-substituted derivativesJournal of Fluorine Chemistry, 1991
- Crystal structure of a side-on superoxo complex of cobalt and hydrogen abstraction by a reactive terminal oxo ligandJournal of the American Chemical Society, 1990
- Boron-pyrazole chemistry. IV. Carbon- and boron-substituted poly[(1-pyrazolyl) borates]Journal of the American Chemical Society, 1967
- Boron-pyrazole chemistry. II. Poly(1-pyrazolyl)-boratesJournal of the American Chemical Society, 1967
- Boron-pyrazzole chemistry. I. PrrazabolesJournal of the American Chemical Society, 1967