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New versatile phosphorus ligands containing SPNSO skeleton - synthesis and characterization of (SPPh2)(O2SR)NH acids (R=Me, C6H4Me-4) and their alkaline metal salts. Crystal and molecular structures of (SPPh2)(O2SR)NH
Authors:Mihaela Szabo  Ciprian Rat  John E Drake  Mark E Light
Institution:a Facultatea de Chimie si Inginerie Chimica, Universitatea Babes-Bolyai, RO-400028 Cluj-Napoca, Romania
b Department of Chemistry and Biochemistry, University of Windsor, Windsor, Ont. Canada N9B 3P4
c Department of Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ, UK
Abstract:New phosphorus ligands of the type (SPPh2)(O2SR)NH R=Me (1), C6H4Me-4 (2)] were prepared as white crystalline solids using the reactions between LiHN(S)PPh2] and RSO2Cl. They were easily converted into their alkali metal salts, M(SPPh2)(O2SR)N] (M=Li, Na, K). Both the free acids and their alkali metal salts were characterised by multinuclear (1H, 13C, 31P) NMR spectroscopy. The molecular structures of the free acids were established by single crystal X-ray diffraction. They crystallize in the tetragonal space group I41/a (1) and the triclinic space group P−1 (2), respectively. In both compounds the acidic proton is attached to nitrogen and the molecular units are associated through SO?H-N intermolecular hydrogen bonding H?O 2.216 in 1 and 2.029 Å in 2]. A supramolecular chain-like structure is formed in 1 and dimeric units are built in 2. For both compounds a conformation close to syn-syn can be considered for the SP(C)2-N-SC(O)2 fragment.
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