Source of materialThe mixture of Ce(SO 4 ) 2 × 6H 2 O( 0.086 g, 0.2m mol) and 3,3',5,5'-diazenediyldiphthalic acid (0.074 g, 0.2 mmol) was stirred into 15 ml aqueous solution. Then the pH value was adjusted to approx. 4with 1.0 mol/L diluted nitric acid. After stirring for 10 min in air, the mixture was placed into a25mlTeflon-lined autoclave under autogenous pressure, and then heated at 155°C for 72 h. The autoclave was cooled over aperiod of 12 hat arate of 5°C/h. After the mixture was slowly cooled to room temperature, block-shaped red crystals were obtained, and the product is insoluble in water. The Ce(IV) cations do not present in the final product, which mayb ed ue to the acidic conditions [1]. When as imilar reaction was performed in the absence of Ce(SO 4 ) 2 × 6H 2 Oi nt he reaction mixture, the samec ompound could not be obtained, which indicates that the Ce(IV) ion plays an important role in selective oxidation of the organic compound to form final products. IR data areavailable in theCIF file.
Experimental detailsThes tructureo ft he titlec omplex,i ncluding Hp ositions, have been locatedd irectlyf romd ifferenceF ourier maps.A ll U iso values were restrained on U eq values of the parent atoms. O1 is given with an occupation of position 0.25, while both refined and unrefined Hatomswere included.
Discussion