New heteroligand peroxo compounds of titanium(IV): synthesis, characterisation and spectroscopic studies of A2[Ti(O2)2SO4].4H2O (A = NH4 OR K), [Ti(O2)2(L-L)] (L-L = 1,10-phenanthroline, 2,2'-bipyridine) and [Ti(O2)2(thiourea)]. H2O

Chaudhuri, Mihir K. ; Das, Bimalendu ; Lal, Ram A. (1989) New heteroligand peroxo compounds of titanium(IV): synthesis, characterisation and spectroscopic studies of A2[Ti(O2)2SO4].4H2O (A = NH4 OR K), [Ti(O2)2(L-L)] (L-L = 1,10-phenanthroline, 2,2'-bipyridine) and [Ti(O2)2(thiourea)]. H2O Journal of Molecular Catalysis, 51 (1). pp. 59-66. ISSN 0304-5102

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Official URL: http://linkinghub.elsevier.com/retrieve/pii/030451...

Related URL: http://dx.doi.org/10.1016/0304-5102(89)87009-9

Abstract

Alkali diperoxomonosulphatotitanate(IV) tetrahydrates, A2[Ti(O2)2-SO4.4H2O (A = NH4 or K), have been synthesised from the reaction of freshly precipitated TiO2 with 7.65 M H2SO4 and 30% H2O2 at pH 2.5 - 3, adjusted by the addition of aqueous ammonia or potassium hydroxide. Also, three molecular mixed-ligand diperoxo compounds of titanium(IV), viz. [Ti(O2)2(o-phen)], [Ti(O2)2(bipy)] and [Ti(O2)2(thiourea)] . H2O have been obtained by reacting a solution of freshly precipitated TiO2 in 40% HF with an ethanolic solution of 1,10-phenanthroline (o-phen), an ethanolic solution of 2,2'-bipyridine (bipy), and an aqueous solution of thiourea, respectively, and 30% H2O2 maintained at pH 7 by the addition of aqueous ammonia. The compounds are all yellow products and have been characterised from the results of elemental analyses, room temperature magnetic susceptibility measurements, and IR and laser Raman (1R) spectroscopic studies. The IR and laser Raman spectra show that each of the O22- and SO42- ligands in [Ti(O2)2SO4]2- ion, and the O22- and o-phen or bipy in the respective cases occur as bidentate ligands, while thiourea in [Ti(O2)2 (thiourea)] . H2O binds the metal centre in a monodentate manner. The compounds are all diamagnetic and EPR-silent.

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