SYNTHESIS AND CHARACTERIZATION OF TRIMETHYLSILYL PHOSPHIDE DERIVATIVES OF DINEOPENTYLINDIUM CHLORIDE - X-RAY CRYSTAL-STRUCTURES OF [ME(ME3CCH2)INP(SIME3)2]2, (ME3CCH2)2INP(SIME3)2IN(CH2CME3)2CL, AND (ME3CCH2)2INP(SIME3)2IN(CH2CME3)2PH(SIME3)

被引:13
|
作者
WELLS, RL
MCPHAIL, AT
SELF, MF
机构
关键词
D O I
10.1021/om00032a069
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Three new neopentylindium compounds, [Me(Me3;CCH2)InP(SiMe3)2]2 (1), (Me3CCH2)2-InP(SiMe3)2In(CH2CMe3)2Cl (2), and (Me3CCH2)2-InP(SiMe3)2In(CH2CMe3)2PH(SiMe3) (3), are reported. Dimer 1 contains two different exocyclic alkyl ligands on the group 13 center and is the only product isolated from the reaction of (Me3CCH2)2InCl and LiP(SiMe3)2 in either a 1:1 or 2:1 mole ratio. Compound 1 crystallizes in a trans configuration in the monoclinic space group P2(1)/c, with unit cell parameters a = 11.581(1) angstrom, b = 10.284(1) angstrom, c = 18.221(2) angstrom, beta = 111.51(1)-degrees, and V = 1225.6(7) angstrom3 for Z = 2. Compound 2 is the major product isolated from the reaction of (Me3CCH2)2InCl and P(SiMe3)3 in either a 1:1 or 2:1 mole ratio and is an example of an In-P-In-Cl-ring-containing compound. Crystals of 2 belong to the monoclinic system, space group C2/c, with unit cell parameters a = 20.242(2) angstrom, b = 9.883(1) angstrom, c = 19.709(2) angstrom, beta = 99.71(1)-degrees, and V = 3886(1) angstrom3 for Z = 4. Compound 3, isolated as a minor component (ca. approximately 2%) from the reaction of (Me3CCH2)2InCl and P(SiMe3)3 in a 1:1 mole ratio, is the first example of an indium compound containing an In-P-In-P core wherein the phosphorus centers are not symmetrically substituted. This compound crystallizes in the triclinic space group P1BAR, with unit cell parameters a = 12.426(1) angstrom, b = 18.497(2) angstrom, c = 10.156(1) angstrom, alpha = 94.49(1)-degrees, beta = 104.62(1)-degrees, gamma 81.22(1)-degrees, and V = 2230.3(7) angstrom3 for Z = 2.
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页码:3363 / 3367
页数:5
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