Synthesis and crystal structures of bulky guanidinato zirconium(IV) and hafnium(IV) chloride complexes

Cameron Jones, Christian Schulten, Sharanappa Nembenna, Andreas Stasch

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Abstract

Reactions of in situ generated [Li(Giso)] (Giso = [(DipN)(2)CN(C6H11)(2)](-); Dip = C6H3Pr (2) (i) -2,6) with either ZrCl4 or HfCl4 led to the complexes [(Giso)MCl3] (M = Zr 1 or Hf 2). Reduction of [(Giso)ZrCl3] with an excess of magnesium metal in THF afforded a small isolated yield of the THF insertion product, [ (Giso)ZrCl(mu-OC4H8) (2)]. The crystal structures of all complexes have been determined. The cell parameters of the compounds are 1 (toluene)(0.5): P-1, a = 10.961(2), b = 11.046(2), c = 19.668(4), alpha = 75.31(3), beta = 76.69(3), gamma = 61.93(3); 2 (toluene)(0.5): P-1, a = 10.949(2), b = 11.037(2), c = 19.621(4), alpha = 75.29(3), beta = 76.80(3), gamma = 61.90(3); 3 (hexane)(2): P2(1)/c, a = 14.424(3), b = 16.950(3), c = 20.330(4), beta = 109.09(3). The crystal structures of 1 and 2 are the first for five-coordinate, monomeric guanidinato group 4 metal trihalide complexes.
Original languageEnglish
Pages (from-to)866 - 870
Number of pages5
JournalJournal of Chemical Crystallography
Volume42
Issue number8
DOIs
Publication statusPublished - 2012

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