Crystal structure and catalytic activity of tetra-kis-(μ2-ethyl 2,6-di- tert-butyl-4-methyl-phenyl phos-phato-κ2O: O')bis-(ethyl 2,6-di- tert-butyl-4-methyl-phenyl phosphato-κ2O, O')dilutetium n-heptane disolvate

Mikhail E Minyaev; Alexander N Tavtorkin; Sof'ya A Korchagina; Ilya E Nifant'ev; Andrei V Churakov

doi:10.1107/S2056989018004565

Crystal structure and catalytic activity of tetra-kis-(μ₂-ethyl 2,6-di- tert-butyl-4-methyl-phenyl phos-phato-κ²O: O')bis-(ethyl 2,6-di- tert-butyl-4-methyl-phenyl phosphato-κ²O, O')dilutetium n-heptane disolvate

Acta Crystallogr E Crystallogr Commun. 2018 Mar 23;74(Pt 4):543-547. doi: 10.1107/S2056989018004565. eCollection 2018 Apr 1.

Authors

Mikhail E Minyaev¹, Alexander N Tavtorkin^{1

2}, Sof'ya A Korchagina^{1

2}, Ilya E Nifant'ev^{1

2}, Andrei V Churakov³

Affiliations

¹ A.V. Topchiev Institute of Petrochemical Synthesis, Russian Academy of Sciences, 29 Leninsky prospect, 119991, Moscow, Russian Federation.
² Chemistry Department, M.V. Lomonosov Moscow State University, 1 Leninskie Gory Str., Building 3, Moscow 119991, Russian Federation.
³ N.S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, 31 Leninsky Prospect, Moscow 119991, Russian Federation.

Abstract

The title complex, [Lu₂(C₁₇H₂₈O₄P)₆]·2C₇H₁₆, was formed in the reaction between potassium 2,6-di-tert-butyl-4-methyl-phenyl ethyl phosphate, [K(2,6- ^t Bu₂-4-MeC₆H₂-O)(EtO)PO₂], and LuCl₃(H₂O)₆ in water, followed by vacuum drying and recrystallization from heptane. Its crystal structure has triclinic (P [Formula: see text]) symmetry at 120 K. The lutetium tris-(phosphate) complex has a binuclear [Lu₂(μ-OPO)₄] core and the organophosphate ligand exhibits κ²O,O' terminal and μ₂-κ¹O:κ¹O' bridging coordination modes with the Lu^III ion being sixfold coordinated. The complex is of inter-est as a precatalyst in the acrylo-nitrile polymerization process and displays good catalytic activity under mild conditions.

Keywords: acrylonitrile polymerization; binuclear complex; coordination compound; crystal structure; lutetium; organophosphate.

Grants and funding

This work was funded by the State Program of TIPS RAS supported by FASO Russia grant .