
%0 Journal Article
%A Cosgriff, JE 
%A Deacon, GB 
%A Gatehouse, BM 
%T Organoamido- and Aryloxo-lanthanoids. IX. Preparations and Structures of Tris(&#951;<sup>2</sup>-3,5-diphenyl-pyrazolato)lanthanoid(III) Complexes With Triphenylphosphine Oxide and Tetrahydrofuran
%J Australian Journal of Chemistry
%D 1993/12/01
%V 46
%N 12
%P 1881-1896
%K 
%R https://doi.org/10.1071/CH9931881
%U https://www.publish.csiro.au/paper/CH9931881 
%X From reaction of lanthanoid metals with bis ( pentafluorophenyl )mercury and 3,5-diphenylpyrazole (HPh2pz) in 1,2-dimethoxyethane ( dme ) and treatment of the products with triphenylphosphine oxide, the complexes [ Ln (&#951;2-Ph2pz)3(OPPh3)2].( dme )n ( Ln = Er or Nd , n = 1; Ln = La, n = 0.6) have been isolated. An X-ray crystal structure shows that the erbium complex [monoclinic, space group C2, a 22.08(3), b 14.30(1), c 13.37(1) &#506;, &#946; 124.09(7)&#176;, Z 2 2730 'observed' data refined to R 0.046] is monomeric , with eight coordination of the metal. There is a trigonal  bipyramidal arrangement of the centre ( Cen ) of the N-N bonds of three &#951;2-3,5-diphenylpyrazolate groups ( &#931;Cen-Er-Cen 360&#176;; ( Er -N) 2.344 &#506;) and the oxygens of two equivalent trans triphenylphosphine oxide ligands [O- Er -O 176(1)&#176;; Er -O 2.207(9)&#506;]. Unit cell data indicate that the neodymium analogue [monoclinic, space group C2, a 23.01(3), b 14.94(2), c 13.82(2) &#506;, &#946; 123.65(8)&#176;] is isostructural with the erbium complex. An analogous reaction of lanthanum or neodymium metal, Hg(C6F5)2, and HPh2pz in tetrahydrofuran ( thf ) gives [ Ln (&#951;2-Ph2pz)3( thf )3]. thf ( Ln = La or Nd ). The X-ray crystal structure of the neodymium complex [orthorhombic, space group P212121, a 14.009(9), b 16.280(8), c 22.640(16)&#506;, Z 4, 2967 'observed' data refined to R 0.046 reveals a nine-coordinate monomer with three &#951;2-Ph2pz ligands [ Nd -N 2.420(10)-2.524(8)&#506;] and three thf ligands [ Nd -O 2.497(8)-2.587(8)&#506;]. There is a trigonal prismatic arrangement of the centres of the N-N bonds and the oxygen donor atoms. 
