Add time:09/26/2019         Source:infona.pl

Praseodymium(III), neodymium(III) and gadolinium(III) chloride adducts with tetrahydrofuran (THF) have been prepared and structurally characterized by X-ray crystallography. Removal of water from the corresponding hexahydrate LnCl 3 (H 2 O) 6 using thionyl chloride in the presence of excess THF provides light-green cubic crystals of [PrCl 3 (THF) 2 ] n (1), blue block crystals of [NdCl 3 (H 2 O)(THF)] n (2) and colourless needle crystals of GdCl 3 (THF) 4 (3). In 1 each praseodymium atom is seven-coordinate and is linked to (two) adjacent metal centres by double (μ-Cl) 2 halogen bridging units, resulting in a polymeric chain structure. The metal geometry approximates to distorted pentagonal bipyramidal with Pr--Cl b r i d g e 2.852(6)-2.891(5), Pr--Cl t e r m i n a l 2.668(6), Pr--O T H F 2.51(1) (axial), 2.53(2) 9 (equatorial). In 2 the structure is a two-dimensional cross-linked polymer in which each neodymium atom is connected to (three) others via double (μ-Cl) 2 halogen bridge bonds. The coordination sphere of each metal centre comprises six chlorine atoms [Nd--Cl b r i d g e 2.816(3)- 2.938(3) 9] and a water molecule [Nd--O, 2.490(7) 9], respectively. Hydrogen bonding interactions involving halogen atoms and coordinated water molecules from adjacent metal units (intermolecular) are observed, O--H Cl 3.147-3.350 9. In 3 the molecular structure is based on a seven-coordinate pentagonal bipyramidal metal geometry in which two chlorides occupy the axial positions with the other chloride and the four solvate (THF) molecules making up the equatorial plane. Gd--Cl 2.60(2)-2.66(2), Gd--O 2.40(2)-2.52(3) 9. In addition, general comments concerning structural relationships within the series LnCl 3 (THF) n , where n = 2, 3, 3.5 and 4, are discussed.

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