
TY  - JOUR
A1  - Deacon, GB 
A1  - Feng, TC 
A1  - Skelton, BW 
A1  - White, AH 
T1  - Organoamido- and Aryloxo-Lanthanoids. XI. Syntheses and Crystal Structures of Nd(Odpp)<sub>3</sub>, Nd(Odpp)<sub>3</sub>(thf) and [Nd(Odpp)<sub>3</sub>(thf)<sub>2</sub>].2(thf) (Odpp<sup>-</sup>=2,6-Diphenylphenolate): Variations in Intramolecular &#960;-Ph-Nd Interactions
JF  - Australian Journal of Chemistry
JO  - Aust. J. Chem.
Y1  - 1995
VL  - 48
IS  - 4
SP  - 741
EP  - 756
KW  - 
UR  - https://doi.org/10.1071/CH9950741 
N2  - The X-ray crystal structure of Nd (Odpp)3 ( Odpp- = 2,6-diphenylphenolate), obtained by sublimation of Nd ( Odpp )3( thf )2 ( thf = tetrahydrofuran ) [triclinic, P&#299; , a 15.835(5), b 13.499(10), c 10.955(11) &#506;, &#945; 116.25(7), &#946; 92.87(7), &#947; 101.66(6)&#176;, V 2031 &#506;3, Z2, No 5726 'observed' data (I > 3&#963;(I)) refined to conventional R 0.047 shows a near triangular array of oxygens surrounding neodymium { Nd -O} 2.169 &#506;, &#8721; O- Nd -O 353.2&#176; with additional, intramolecular Nd-&#951;6-Ph chelate interactions { Nd -C} 3.046 &#506; and Nd-&#951;1-Ph ( Nd -C 2.964(7)&#506;). There is a pseudotrigonal bipyramidal arrangement of the oxygens, the centroid of the &#951;6-Ph, and the &#951;1-carbon. The complex Nd ( Odpp )3( thf ), obtained by crystallization of Nd ( Odpp )3( thf )2 from toluene (monoclinic, P21/c, a 12.213(4), b 21.447(4), c 17.744&#506;, &#946; 104.25(2)&#176;, V 4505 &#506;3, Z 4, R 0.042 for No 8014) also has pseudotrigonal  bipyramidal stereochemistry, with a triangular equatorial array of aryl oxide oxygens { Nd -O} 2.193 &#506;; &#8721; O- Nd -O 358.7&#176;, an apical thf oxygen (Nd -O 2.446(3)&#506;), and an apical intramolecular chelating phenyl group. As the last has three Nd -C contacts (3.094(5), 3.144(5), 3.010(5)&#506;) significantly shorter than the other three (3.300(5), 3.427(5), 3.377(5)&#506;), an &#951;3-Ph-Nd interaction seems likely. For [ Nd ( Odpp )3( thf )2].2( thf ), obtained by crystallization from tetrahydrofuran without drying of the crystals, the X-ray structure (monoclinic, P21, a 10.230(2), b 21.919(5), c 13.411(4) &#506;, &#946; 101.15(2)&#176;, V 2950 A3, Z2, R 0.058 for No 3237) reveals a distorted trigonal bipyramidal arrangement of three aryl oxide oxygens (two equatorial 2.208(9), 2.16(1) &#506;; one axial 2.203(9) &#506;) and two thf oxygens (one equatorial 2.44(1) &#506;; one axial (significantly distant) 2.62(1) &#506;). The X-ray structure of [La( Odpp )3( thf )2].2( thf ) shows it to be isostructural with the neodymium analogue. 
ER  -

