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The complexation of RhCl 3 ·3H 2 O and [RH 2 (CH 3 COO) 4 ·2H 2 O] with trans-4,4'-bis (diethoxyphosphoryl)biphenyl-18-crown-6 in various media was studied. In the synthesized compounds the rhodium(III) or dirodium(II) ions form supramolecular ensembles with ligand environment. The compounds were characterized by NMR, IR, Raman, ESR, X-ray electron spectroscopy, conductivity, and the data of elemental and X-ray fluorescence analyses. The predominant role of diethoxyphosphoryl groups at the macrocycle in binding rhodium(III) and dirhodium(II) ions was demonstrated.There is a great interest nowadays in a modified type of macrocyclic polyethers containing a variety of additional groups that supply the polyester cycle with a number of useful properties, such as changing the hydrophilic and surfactant properties of polyesters [1], improve the complexing properties towards transition metal cations [2].In this work, continuing a series of research on the interaction of transition elements with macrocyclic compounds, we studied the complexing ability of RhCl 3 ·3H 2 O (I) and [RH 2 (CH 3 COO) 4 ·2H 2 O] (II) with a derivative of dibenzo-18-crown-6 (DB-18-CR-6) containing two diethoxyphosphoryl groups as substituents in the benzene rings in the trans position, the trans-4,4'-bis(diethoxyphosphoryl)biphenyl-18-crown-6 (L) [3][4][5].The main characteristics of the non-coordinated ligand have been described in [5]. In a number of works [6, 7] the reactivity has been studied of certain types of crown ethers with compounds of platinum group metals, however, in the literature we have not found any information on the conditions of complexation of the ligand L with the compounds of rhodium(III) or dirodium(II).To select the optimal conditions for the synthesis of these complexes we varied solvents and the ratio of the reactants. These parameters play a decisive role in the synthesis. The interaction of compounds I and L in a molar ratio of I:L = 2:1 in a mixture of ethanol and chloroform produced stable in air crystalline dark brown product III, mp 226°C. Te interaction of compounds I and L in ethanol or chloroform medium does not lead to the formation of solid products. The interaction of compounds I and L in a mixture of ethanol and chloroform in molar ratios of I:L = 2:2 and 1:2 leads to complex mixtures of difficultly separable reaction products.

Compounds of the compositions [2(

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