SYNTHESIS AND STRUCTURES OF N-ALKYLATED AZATITANATRANES

被引:36
作者
SCHUBART, M
ODWYER, L
GADE, LH
LI, WS
MCPARTLIN, M
机构
[1] UNIV WURZBURG,INST ANORGAN CHEM,AM HUBLAND,D-97074 WURZBURG,GERMANY
[2] UNIV N LONDON,SCH CHEM,LONDON N7 8DB,ENGLAND
关键词
D O I
10.1021/ic00096a012
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The N-alkylated azatitanatranes N(CH2CH2NR)3TiCl [R = Me (1), Et (2), i-Pr (3)] have been prepared and 1 and 3 structurally characterized by X-ray crystallography: 1, orthorhombic, Pmna, a = 11.293(3) angstrom, b = 11.977(3) angstrom, c = 9.722(3) angstrom, V = 1314.96 angstrom3, Z = 4, R = 0.0629; 3, cubic, Pa3, a = 15.928(4) angstrom, V = 4040.95 angstrom3, Z = 8, R = 0.0792. The halide ligand in 2 and 3 could be replaced by more labile ligands by chloride abstraction using the appropriate silver salts. A single-crystal X-ray structure analysis of N(CH2CH2NEt)3TiOSO2CF3 (4), the first azatrane-triflate to be reported, was carried out. Crystal data for 4: triclinic, P1BAR (No. 2), a = 16.039(4) angstrom, b = 16.473(4) angstrom, c = 8.954(3) angstrom, alpha = 105.75-degrees, beta = 106.17(2)-degrees, gamma = 107.54(2)-degrees, V = 1996.33 angstrom3, Z = 4, R = 0.0842. The titanium amido complexes reported here may find use as building blocks in more complex structural arrays.
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页码:3893 / 3898
页数:6
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