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Crystalline materials have been synthesized in reactions of titanium(iv) tetraisobutoxide with branched organic acids (HOOCR', R' = CMe(2)Et, (t)Bu, CH(2)(t)Bu) in the molar ratio 1:1 at room temperature under Ar atmosphere. Particular attention has been paid to the structural and spectral characterization of metastable intermediate complexes of general formula [Ti(7)O(9)(O(i)Bu)(4)(HO(i)Bu)(OOCCMe(2)Et)(6)](2) (1) and [Ti(6)O(5)(O(i)Bu)(6)(OOC(t)Bu)(8)] (3), and their conversion towards more structurally stable compounds [Ti(6)O(6)(O(i)Bu)(6)(OOCC(Me)(2)Et)(6)] (2) and [Ti(6)O(6)(H(2)O)(2)(O(i)Bu)(6)(OOC(t)Bu)(6)] (4). The hexanuclear structure of (5) ([Ti(6)O(6)(O(i)Bu)(6)(OOCCH(2)(t)Bu)(6)]) has been postulated on the basis of IR and (13)C NMR spectroscopic data analysis. The possible reaction pathways which may occur during the formation of the above mentioned compounds are also discussed.

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