FIELD: chemistry.
SUBSTANCE: present invention relates to the crystalline form of the compound (I) 6,6'-[[3,3',5,5'tetrakis(1,1-dimethylethyl)-[1,1'-biphenyl]-2,2'-diyl]bis(oxy)]bis-dibenzo[d,f][1,3,2]-dioxaphosphphepin, which can be used in the chemical industry. Crystalline form is proposed, selected from: crystalline toluene mono-solvate, which on an X-ray powder diffractogram at 25°C with Cu-Kα radiation demonstrates 2θ values: 5.15°±0.20°, 7.59±0.20°, 8.56±0.20°, 8.80±0.20°, 8.97±0.20°, 9.65±0.20°, 10.55±0.20°, 11.47±0.20°, 14.76±0.20° and 15.35±0.20° or an unsolvated crystalline form, which on an X-ray powder diffractogram at 25°C with Cu-Kα radiation demonstrates 2θ values: 5.39±0.20°, 7.04±0.20°, 8.44±0.20°, 8.65±0.20°, 9.08±0.20°, 9.66±0.20°, 10.66±0.20°, 12.60±0.20°, 16.25±0.20° and 17.36±0.20°. Compositions based on said form, methods for preparing said crystalline form and its use for the preparation of catalysts are proposed. Said crystalline form is obtained by crystallization from a supersaturated solution of compound I in toluene at a temperature of not more than 30°C or by agitating the suspension of compound I in a solvent containing toluene at a temperature above the boiling point of toluene.
EFFECT: new crystalline forms of a valuable substance with low stickiness, reduced tendency to caking, low dust formation, as well as an efficient method for their preparation, compositions based on them and their use for the production of valuable transition metal catalysts.
13 cl, 8 ex, 6 dwg, 10 tbl
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Authors
Dates
2018-07-11—Published
2012-12-28—Filed