N-Acylamidophosphinates RC(X)NHP(Y)R' 2 (NAAP) and their thioanalogues (X,Y= O, S; R = Alk, Ar, CCl 3 , Het, NR 2 2 , NR 2 R 3 ; R ' = Ar, OAlk, OAr, SAlk, NAlk 2 , NHAr) contain X, Y donor atoms and amide nitrogen, which are capable of taking in complexation with metal cations. An application of NAAP complexes in supramolecular chemistry has been investigated in the last decades. Developed synthetic methods allow us to obtain N-acylamidophosphinate ligands contained multiple chelating groups or a combination of several essentially various coordinating fragments in the molecule: chelating moiety C(X)NHP(Y) and a macrocycle. The latter ligands are capable of connecting ions simultaneously by the chelating sites, and by the "guest-host" mechanism using the macrocycle. The bibliography includes 104 references.Investigation of complexing properties of conjugated organophosphorous anions is an important issue of modern coordination and organoelement chemistry [1,2]. The application of NMR, IR and UV spectroscopic methods to study the structure and dynamic processes in solutions of such compounds allows to investigate the nature of the chemical bonds in the conjugated organophosphorous anions and opens the way for the creation of new types of selective complexing agents.N-Acylamidophosphates, N-acylamidophosphinates and their thioanalogues with common formula RC(X)NHP(Y)R`2 (NAAP) contain X, Y donor atoms and an amido nitrogen atom which can be involved in complexation (Scheme 1). In terms of reactivity NAAP are quite different from each other depending on the nature and combination of atoms X and Y in the molecule, as well as the nature of substituents of (thio)carbonyl and (thio)phosphoryl moieties. Scheme 1.
Reaction of the potassium salts of N-thiophosphorylated thioureas of common formula RC(S)NHP(S)(OiPr)(2) [R = morpholin-N-yl (HL(a)), piperidin-N-yl (HL(b)), NH(2) (HL(c)), PhCH(2)NH (HL(d))] with Cu(PPh(3))(3)I in aqueous EtOH/CH(2)Cl(2) leads to mononuclear [Cu(PPh(3))(2)L-S,S'] complexes. Using copper(i) iodide instead of Cu(PPh(3))(3)I, polynuclear complexes [Cu(n)(L-S,S')(n)] were obtained. The structures of these compounds were investigated by ES-MS, elemental analyses, 1H and 31P NMR in solution, IR and 31P solid-state MAS NMR spectroscopy. The crystal structures of [Cu(3)L(3)(a)] and [Cu(PPh(3))(2)L(b)] were determined by single-crystal X-ray diffraction.
Reaction of the potassium salt of N-thiophosphorylthiourea tBuNHC(S)NHP(S)(OiPr) 2 (HL) with Zn II , Cd II , Ni II and Co II in aqueous EtOH leads to complexes of common formula M(L-S,SЈ) 2 (ML 2 ). Complexes were investigated by IR, UV-Vis, 1 H and 31 P{ 1 H} NMR spectroscopy and microanalysis The structure of complex NiL 2 was investigated by single crystal X-ray diffraction * Dr. Damir A. Safin Kremlevskaya str. 18 Kazan, 420008/Russian Federation 967 analysis. The nickel(II) ion has a squre-planar environment, S 4 , with two anionic ligands involving 1,5-S,SЈ-coordination mode. The ligands are bound in a trans configuration.
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