Synthesis of (Me3SiCH2Sb)n and reactions with ditellurides: crystal structure of [Cp2Co][Me3SiCH2SbCl3]
摘要:
Substitution of phenyl groups in Ph(2)SbR (1) (R = Me(3)SiCH(2)) with chlorine atoms leads to RSbCl(2) (2). Reduction of 2 with magnesium in tetrahydrofuran gives red crystals of (RSb)(n) (3) and a black solid containing the polymer (RSb)(x). Solutions of 3 in C6D6 are yellow. They consist of an equilibrium mixture of (RSb)(5) and (RSb)(4). The reaction between 2 and cobaltocene in tetrahydrofuran or C6D6 leads to the polymer (RSb)(x) and to the salt [CoCp(2)](+)[RSbCl(3)](-) (4). The structure of 4 has been determined by single-crystal X-ray diffraction. It contains a centrosymmetric double-chlorine-bridged dimeric anion. The ditellurostibane RSb(Te-p-Tol)(2) (5) has been obtained with a quantitative yield through a complete reaction between 3 and (p-TolTe)(2). Compound 5 has been detected in the product mixtures resulting from reactions of polymeric (RSb)(x) with (p-TolTe)(2) or by reducing p-TolTeCl(3) and RSbCl(2) with magnesium in tetrahydrofuran.
Synthesis of (Me3SiCH2Sb)n and reactions with ditellurides: crystal structure of [Cp2Co][Me3SiCH2SbCl3]
摘要:
Substitution of phenyl groups in Ph(2)SbR (1) (R = Me(3)SiCH(2)) with chlorine atoms leads to RSbCl(2) (2). Reduction of 2 with magnesium in tetrahydrofuran gives red crystals of (RSb)(n) (3) and a black solid containing the polymer (RSb)(x). Solutions of 3 in C6D6 are yellow. They consist of an equilibrium mixture of (RSb)(5) and (RSb)(4). The reaction between 2 and cobaltocene in tetrahydrofuran or C6D6 leads to the polymer (RSb)(x) and to the salt [CoCp(2)](+)[RSbCl(3)](-) (4). The structure of 4 has been determined by single-crystal X-ray diffraction. It contains a centrosymmetric double-chlorine-bridged dimeric anion. The ditellurostibane RSb(Te-p-Tol)(2) (5) has been obtained with a quantitative yield through a complete reaction between 3 and (p-TolTe)(2). Compound 5 has been detected in the product mixtures resulting from reactions of polymeric (RSb)(x) with (p-TolTe)(2) or by reducing p-TolTeCl(3) and RSbCl(2) with magnesium in tetrahydrofuran.