DIMETHYL(TETRAMETHYLCYCLOPENTADIENYL)SILYL-, -GERMYL-, AND -STANNYLPHOSPHANES - X-RAY STRUCTURES OF CHLORO(DIMETHYL)TETRAMETHYLCYCLOPENTADIENYL-STANNANE AND TETRACARBONYL[1-DIMETHYL(TETRAMETHYLCYCLOPENTADIENYL)GERMYL-3,4-DIMETHYL-P HOSPHOLENE]IRON(0)

摘要

Me(2)Cp'SiCl (1) (Cp' = C(5)HMe(4)) reacts with magnesium and R(2)PCl (R = Ph, Bu) as well as PCl3 in tetrahydrofurane yielding Me(2)Cp;SiPPh(2) (4), M3(2)Cp'SiP(t)Bu(2) (5) and (Me(2)Cp'Si)(3)P (6) respectively. The raction of Me(3)SiPPh(2) (7) or Me(3)SiPC(4)H(4)Me(2) (10) with Me(2)Cp'GeCl (2) and Me(2)Cp'SnCl (3) leads to the formation of me(2)Cp'EPPh(2) (E = Ge (8), sn (9)) and Me(2)Cp'EPC(4)H(4)Me(2) (E = Ge (11), Sn (12)). 11 reacts with Fe(CO)(5) with formation of Fe(CO)(4)[PC(4)H(4)Me(2))GeCP'Me(2)] (13). 3 crystallizes in the space group P2(1) with a = 986, 7(1), b = 1247,3(2), c = 1028,2(1) pm, beta = 92,71(1)degrees, Z =4 and V = 1264,1(2) 10(-30)m(3). The final refinement resulted in R(1) = 0,0249 for 2097 observed reflexions with F-0 greater than or equal to 4 sigma(F-0). 13 crystallizes in the space group P2(1) with a = 967,7(3), b = 1298,70(16), c = 1832,7(3) pm, beta = 95,810(19)degrees, Z = 4 and V = 2291,4(8) 10(-30) m(3) (R(1) = 0,0444 for 4043 observed reflexions with F-0 greater than or equal to 4 sigma(F-0). 13 forms a trigonal bipyramide with the phosphane ligand 11 in an axial position. [References: 46]