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Transition metal complexes of P-rich phosphanes and silylphosphanes. XI. Formation, reactions, and structures of chromium carbonyl complexes from reactions of Li(THF)2[eta2-(tBu2P) 2P] with Cr(CO)5 ¡¤ THF and Cr(CO)4 ¡¤ NBD
Reactions of Li(THF)2[eta2-(tBu2P) 2P] 1 with Cr(CO)5¡¤ THF yield Li(THF)2Et2O[Cr(CO)4{eta2-( tBu2P)2P}eta1-Cr(CO)5] 2 and the compounds [Cr(CO)4{eta2-(tBu2P) 2PH}] 3, [Cr(CO)5{eta1-(tBu2P) 2PH}] 4, (tBu2P)2PH 5 and tBu2PH¡¤Cr(CO)5 6. The formation of 3, 4, 5 and 6 is due to byproducts coming from the synthesis of 1. 2 reacts with CH3COOH under formation of 3. After addition of 12-crown-4 1 with NBD¡¤Cr(CO)4 in THF forms Li(12-crown-4)2[Cr(CO)4-{eta2-( tBu2P)2P}] 7 (yellow crystals). 7 reacts with CH3COOH to 3 – which regenerates 7 with LiBu – with Cr(CO)5THF to compound 2, with NBD¡¤Cr(CO)4 in THF to 2 and 3 (ratio 1:1). With EtBr, 7 forms [Cr(CO)4{eta2-(tBu2P) 2PEt}] 8, and [Cr(CO)4{eta2-(tBu2P) 2PBr}] 9 with BrCH2-CH2Br. The compounds were characterized by means of 1H, 13C, 31P, 7Li NMR spectroscopy, IR spectroscopy, elementary analysis, mass spectra, and 2, 3 and 4 additionally by means of X-ray diffraction analysis. 2 crystallizes in the space group P1 with 2 formula units in the elementary cell; a = 10.137(9), b = 15.295(12), c = 15.897(14) A; alpha = 101.82(7), beta = 91.65(7), gamma = 98.99(7); 3 crystallizes in the space group P21/n with 4 molecules in the elementary unit; a = 11.914(6), b = 15.217(10), c = 14.534(10) A; alpha = 90, beta = 103.56(5), gamma = 90. 4: space group P1 with 2 molecules in the elementary unit; a = 8.844(4), b = 12.291(6), c = 14.411(7) A, alpha = 66.55(2), beta = 89.27(2), gamma = 71.44(2). Johann Ambrosius Barth 1996.
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Chiral Catalysts,
Chiral catalysts – SlideShare