REACTIONS OF GALLIUM TRICHLORIDE WITH BIS(DIALKYLAMINO)DIMETHYLSILANES AND BIS(ALKYLAMINO)DIMETHYLSILANES

被引:19
作者
NUTT, WR [1 ]
BLANTON, JS [1 ]
BOCCANFUSO, AM [1 ]
SILKS, LA [1 ]
GARBER, AR [1 ]
ODOM, JD [1 ]
机构
[1] UNIV S CAROLINA,DEPT CHEM,COLUMBIA,SC 29208
关键词
D O I
10.1021/ic00022a011
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The Lewis acid-base adduct Me2Si(NMe2)2.GaCl3 was isolated when GaCl3 was allowed to react with Me2Si(NMe2)2. The reaction of Me2Si(NEt2)2 with GaCl3 proceeded by dehalosilylation to give [Cl2Ga(NEt2)2SiMe2][(Cl3Ga)2NEt2] and ET2NSi(Cl)Me2. The N-alkylated hexamethylcyclotrisilazane (RNSiMe2)3 and RNH2.GaCl3 were obtained from the reaction of GaCl3 with [R(H)N]2SiMe2, where R = Et and n-Bu. The molecular structures of Me2Si(NMe2)2.GaCl3 and [Cl2Ga(NEt2)2SiMe2][(Cl3Ga)2NEt2] were confirmed by X-ray crystallography. Crystal data for Me2Si(NMe2)2.GaCl3: monoclinic space group C2/c (No. 15), a = 26.146 (7) angstrom, b = 8.043 (2) angstrom, c = 16.164 (6) angstrom, beta = 124.97 (2)-degrees, V = 2785 (1) angstrom 3, Z = 8, rho(calcd) = 1.538 g cm-3, and R = 0.0489. Crystal data for [Cl2Ga(NEt2)2SiMe2][Cl3Ga)2NEt2]: orthorhombic space group P2(1)2(1)2(1) (No. 19), a = 14.813 (4) angstrom, b = 15.768 (4) angstrom, c = 13.102 (2) angstrom, V = 3060 (1) angstrom 3, Z = 4, rho(calcd) = 1.665 g cm-3, and R = 0.0556. The four-membered (Ga-N-Si-N) ring in [Cl2Ga(NEt2)2SiMe2]+ is nonplanar with a fold angle of 165.5 (5)-degrees on the Ga...Si diagonal. The H-1, C-13, and Si-29 NMR spectra are reported and discussed.
引用
收藏
页码:4136 / 4140
页数:5
相关论文
共 30 条
[1]   TRIS(N-METHYL) AND TRIS(N-ETHYL)-HEXAMETHYL-CYCLOTRISILAZANES - PREPARATIONS AND SOME PROPERTIES [J].
ABEL, EW ;
BUSH, RP .
JOURNAL OF INORGANIC & NUCLEAR CHEMISTRY, 1964, 26 (10) :1685-1691
[2]  
ANDRIANOV KA, 1963, IZV AKAD NAUK SSSR K, V12, P2227
[3]   CLEAVAGE OF POLY(DIORGANOSILOXANES) BY TRIMETHYLALUMINUM [J].
APBLETT, AW ;
BARRON, AR .
ORGANOMETALLICS, 1990, 9 (07) :2137-2141
[4]  
BOCCANFUSO AM, 1988, THESIS U S CAROLINA
[5]   SYNTHESIS + PROPERTIES OF N-SUBSTITUTED CYCLOTRISILAZANES [J].
BREED, LW ;
ELLIOTT, RL .
INORGANIC CHEMISTRY, 1964, 3 (11) :1622-&
[6]  
BUSING WR, 1985, ORFFE
[7]   NUCLEOPHILIC DISPLACEMENT AT SILICON STEREOCHEMISTRY AND MECHANISTIC IMPLICATIONS [J].
CORRIU, RJP ;
GUERIN, C .
JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1980, 198 (03) :231-320
[8]  
Cromer D.T, 1974, INT TABLES XRAY CRYS, VIV
[9]   NATURE OF SOLUBLE COPPER (I) HYDRIDE [J].
DILTS, JA ;
SHRIVER, DF .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1968, 90 (21) :5769-&
[10]  
DURKIN T, 1971, J CHEM EDUC, V48, P452