Tiyo-fosfor grubu komplekslerinin sentezi ve yapılarının aydınlatılması

Abstract

Bu çalışmada ditiyofosfonik asitlerin (CH3O-C6H4-(RO)P(S)S-NH4+; R = -C5H11 ve -(CH2)3-C6H5) amonyum tuzları sentezlendi ve bu tuzlardan yeni kompleksler sentezlendi ([M(CH3O-C6H4-(RO)P(S)S)2]n, n= 1, M= Ni2+; n= 2, Cd2+, Hg2+, R= -C5H11, -(CH2)3-C6H5). Ditiyofosfonik asitler, Lawesson reaktifinin (2,4–bis-(p-metoksifenil)–1,3,2,4–ditiyodifosfetan–2,4–disülfür) ile alkollerle reaksiyonundan elde edildi. Oluşan asitler amonyum tuzuna dönüştürüldü. Ayrıca sentezlenen yeni kare düzlem nikel komplekslerinin piridin (Py) ligandıyla yeni oktahedral kompleksleri elde edildi ({Ni(CH3-O-C6H4-(RO)P(S)S)2Py2} R= -C5H11, -(CH2)3-C6H5). Ditiyofosfonik asit esterlerinin ve komplekslerinin yapıları element analizi, erime noktası, 1H-, 13C-, 31P-NMR, MS, FTIR, X-ışınları yapı tayini (AE2-NiPy, AE2-Ni ve AE2-Cd kompleksleri) ve manyetik susseptibilite ölçümleri ile (AE1-NiPy ve AE2-NiPy kompleksleri) aydınlatıldı.

In this study, some dithiophosphinic acids were synthesised (CH3O-C6H4-(RO)P(S)S-NH4+; R = -C5H11 ve –(CH2)3-C6H5) as a ammonium salts, and some novel complexes were synthesised by the reaction of metal cations with ammonium salts ([M(CH3O-C6H4-(RO)P(S)S)2]n, n= 1, M= Ni2+; n= 2, Cd2+, Hg2+, R= -C5H11, –(CH2)3-C6H5). In the first step the dithiophosphinic acids were obtained by means of reaction of between Lawesson reagent (2,4-bis(4-methoxyphenyl)-1,2,3,4-dithiaphosphetane-2,4-disulfide) and some alcohols. Then these acids were converted their ammonium salts. Some novel octahedral nickel complexes were also synthesized by the reaction of some novel square planar which is obtained in this work with pyridine ({Ni(CH3-O-C6H4-(RO)P(S)S)2Py2} R= -C5H11, -(CH2)3-C6H5). The complexes and ligands were characterized by elemental analysis, melting point and 1H-, 13C-, 31P-NMR, MS, FTIR. The magnetic susceptibilities of the complexes which are {Ni(CH3-O-C6H4-(RO)P(S)S)2Py2} (R= -C5H11, –(CH2)3-C6H5) were measured to confirm the hybridization patterns and the geometries. The novel some complexes which are AE2-NiPy, AE2-Ni and AE2-Cd were elucidated by X-ray crystallograph