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• W2171236011 abstract "Abstract The lithium salt of 3,5‐dimethyl‐1‐phenyl‐1 H ‐pyrazole (PyrC 6 H 4 Li) reacts with (Et 2 N) 2 PCl to give the precursor [PyrC 6 H 4 P(NEt 2 ) 2 ] ( 2 ), which, after reaction with PCl 3 , affords PyrC 6 H 4 PCl 2 ( 3 ) in 79 % yield. The phosphorus atom in 3 has four‐coordinate disphenoidal geometry with an axial arrangement of Cl atoms. The length of the hypervalent N–P bond in this compound [1.775(1) Å] is comparable to that of common single bonds. The structure of 3 is better described by canonical formulae containing charges on the N, P, and Cl atoms. The 1 H NMR spectrum of 3 in CDCl 3 shows five pairs of nonequivalent Me groups, which correspond to the positional isomers that exist in the equilibrium mixture. Compound 3 easily exchanges chlorine with methyl iodide to form the diiodo derivative 4 (PyrC 6 H 4 PI 2 ) with nonequivalent P–I bonds. The reduction of 3 with aluminium foil or [GeCl 2 (diox)] gave cationic diphosphines [(PyrC 6 H 4 P) 2 (μ‐Cl)][AlCl 4 ] ( 8 ) and [(PyrC 6 H 4 P) 2 (μ‐Cl)][GeCl 3 ] ( 9 ), respectively, with a chloride bridge between the phosphorus atoms. Compounds 4 , 8 and 9 show a disphenoidal arrangement around the hypervalent phosphorus atoms. The dichloro and diiodo derivatives 3 and 4 are destroyed on heating in pyridine to give diphosphines [(PyrC 6 H 4 PCl) 2 ] ( 10 ) and [(PyrC 6 H 4 P) 2 (μ‐I)] + [I] ( 12 ), respectively, containing hypervalent (trivalent four‐coordinate) phosphorus. The crystal structure of 10 shows multiple C ··· C, C ··· Cl, H ··· H, and C ··· H short contacts between the adjacent molecules. Compound 3 exchanges chlorine for oxygen atoms on heating in dimethylformamide to give the dioxide PyrC 6 H 4 PO 2 ( 13 ) with an N–P V distance [1.808(1) Å] even longer than that in 3 ." @default.
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• W2171236011 date "2015-03-24" @default.
• W2171236011 modified "2023-10-10" @default.
• W2171236011 title "Phenylpyrazole‐Based Hypervalent Phosphorus Compounds: From Positional Isomerism to Stacking Interactions" @default.
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• W2171236011 doi "https://doi.org/10.1002/ejic.201500102" @default.
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