Multifunctional phosphane and phosphane oxide ligands derived from p-tert-butylcalix[4]arene. Synthesis of a large diphosphane with C2 symmetry and behaving as a cis or trans binding ligand
作者： Cyrille Loeber , Dominique Matt , André De Cian , Jean Fischer
DOI: 10.1016/0022-328X(94)84035-0
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摘要: Abstract The calix[4]arene derived di(phosphane oxide) 2 (cone conformation) was obtained in 78% yield by treatment of 1 with equiv NaO t Bu followed reaction Ph P(O)CH OTs. When KO used instead Bu, the partial cone isomer 2′ formed. Reaction PhSiH 3 refluxing toluene afforded quantitatively mixed di(ester)-di(phosphane) ligand ; crystal data : monoclinic, C 2/ c a = 24.091(7), b 14.416(4), 25.270(8) A, β 128.07(2)°, V 6909.1(5) A , Z 4 and R F 5.8%. molecule which lies on axis adopts distorted conformation; angle formed between ester substituted phenolic rings is 105(2)° that phosphane 95.0(1)°. phosphorus lone pairs point towards exterior space defined four calixarene substituents, whereas two groups are directed to interior this cavity. Ligand reacts [PtCl (PhCN) ] THF cis -PtCl · ( ) 91% yield. sequential [RhCl(1,5-cyclooetadiene)] AgBF gave cationic complex -[Rh(1,5- cyclooctadiene) ](BF 5 ). carbon monoxide commercial RuCl boiling 2-ethoxyethanol subsequent addition cis-cis-trans-P,P -[RuCl (CO) 6 Complexes 4-6 display fluxional behaviour solution. All compounds were characterized elemental analysis IR H, 31 P, 13 NMR spectroscopy.
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