865183-16-0Relevant articles and documents
Reaction of hafnium tetrafluoride monohydrate with imidotetraphenyldiphosphinic acid in dmso: The crystal structure of HfF 2[Ph2P(O)NP(O)Ph2]2 · dmso
Il'in,Kovalev,Aleksandrov,Schmidpeter
, p. 210 - 217 (2008/10/09)
19F and 31P NMR spectra are used to demonstrate that the reaction between HfF4 - H2O and Ph2P(O)-N= PPh2OH (HL) in a mixture of equal volumes of dmso and CH 2Cl2 results in the octahedral complexes cis-HfF 2L2, cis-HfF2(dmso)2+, fac-HfF3L(dmso), and cis-HfF4L- with chelating ligand L- and HfF62-. The existence of isomers of dimeric complexes (μ-F2)(HfF3Q)2, where Q = dmso or H2O, with CN = 7 is suggested on the basis of the 19F NMR spectra obtained at temperatures below 203 K. With a twofold excess of HL, HfF2L2(dmso) single crystals are isolated. The crystals are characterized by ER spectroscopy and X-ray crystallography. The monoclinic unit cell parameters are as follows: space group P21/c, a = 11.560(3) A?, b = 23.444(4) A?, c= 18.198(4) A?, β= 101.06(2)°, V=4840(4) A?3, Z=4, μ(MoKα) = 0.44mm-1.In HfF2L2dmso), the central ion has a distorted octahedral surrounding (which is atypical of fluorine compounds of hafnium) with two cis fluorine atoms and two cis-chelating ligands L -. One of the chelate rings has a half-boat conformation; the other is a flattened chair. When HfF2L2(dmso) reacts with SbF3, fluoride ions displace the coordinated L- from the inner sphere of the complex. Copyright
