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The compounds of trinitroaryl type with the common formula А_Х_D which according to usual terminology are bridge compounds with intramolecular charge – transfer (ICT), so-colled autocomplexes (AC) were objects of the investigation in this paper [1]. The acceptor fragments (А) are trinitroaryl type, such as picryl and trinitrofluorenyl, donor (D) fragments contains N - and O - heterocyclic substituents and the isolating spacer (Х) was one-membered (-NH-) and two-membered (-NHCHR-, R=H, CH3 ; -CO-NH-). Synthesis and investigation of such structures are actual becouse of they can be used as a model structures for medicines, vitamins, enzymes and other bioactive substances. A series of metallochelates with transition metalls can be synthesized on the base of some of this chemicals with different practical use [2]. Some of such derivatives are chosen as the objects for searching new effective boicide and fungicide preparates upon different contagious diseases of the man and animals. Synthesis of this autocomplexes has been carried out by the reaction between picryl chloride or 4,5,7-trinitro-9-oxo-9H-fluorene-2-carbonyl chloride and corresponding heterocyclic amine in the solution of the appropriate solvent under reflux at about 30 min. The polymorphism phenomena in the series of synthesized compounds has been investigated [3-4]. So, AC I.4 was prepared and completely described by the X-ray analysis (RSA) in a three differently coloured polymorphous forms, which are different in crystalline packs and molecular conformations. It leads to the essential distinctions between their solid state IR- spectra.