SYNTHESIS AND CHARACTERIZATION OF A NOVEL AZATITANATRANE

被引:27
作者
DUAN, ZB [1 ]
VERKADE, JG [1 ]
机构
[1] IOWA STATE UNIV SCI & TECHNOL,DEPT CHEM,AMES,IA 50011
关键词
D O I
10.1021/ic00121a008
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Azatitanatrane [Ti(i-PrNCH2CH2)(2)NCH2CH2N](2) (13) is obtained in 44% yield by the reaction of Ti(NMe(2))(4) with the new ligand (i-PrNHCH2CH2)(2)NCH2CH2NH2. Compound 13, which features a dimeric structure as determined by H-1, C-13{H-1}, and (HH)-H-1-H-1 NOESY NMR techniques and mass spectroscopy, exhibits a rigid configuration in solution on the NMR time scale. The structure of the azatitanatrane Me(2)NTi(MeNCH(2)CH(2))(3)N (1) was determined by single-crystal X-ray crystallography and was shown to exhibit unusually short axial Ti-N bonds. Crystal data: monoclinic, space group P2(1)/c, a = 7.9550(7) Angstrom, b = 10.546(2) Angstrom, c = 18.105(2) Angstrom, beta = 97.365(8)degrees, V = 1506.4(3) Angstrom(3), Z = 4, R = 0.0373.
引用
收藏
页码:4311 / 4316
页数:6
相关论文
共 31 条
[1]   METALLO-ORGANIC COMPOUNDS CONTAINING METAL-NITROGEN BONDS .1. SOME DIALKYLAMINO-DERIVATIVES OF TITANIUM AND ZIRCONIUM [J].
BRADLEY, DC ;
THOMAS, IM .
JOURNAL OF THE CHEMICAL SOCIETY, 1960, (OCT) :3857-3861
[2]   TIN COATINGS ON STEEL [J].
BUHL, R ;
PULKER, HK ;
MOLL, E .
THIN SOLID FILMS, 1981, 80 (1-3) :265-270
[3]   THERMAL-STABILITY OF TITANIUM NITRIDE FOR SHALLOW JUNCTION SOLAR-CELL CONTACTS [J].
CHEUNG, NW ;
VONSEEFELD, H ;
NICOLET, MA ;
HO, F ;
ILES, P .
JOURNAL OF APPLIED PHYSICS, 1981, 52 (06) :4297-4299
[4]   SYNTHESIS OF VANADIUM AND TITANIUM COMPLEXES OF THE TYPE RM[(ME3SINCH2CH2)3N] (R = CL, ALKYL) AND THE STRUCTURE OF CLV[(ME3SINCH2CH2)3N] [J].
CUMMINS, CC ;
SCHROCK, RR ;
DAVIS, WM .
ORGANOMETALLICS, 1992, 11 (04) :1452-1454
[5]   TRIGONAL-MONOPYRAMIDAL M(III) COMPLEXES OF THE TYPE [M(N3N)] (M = TI, V, CR, MN, FE N3N = [(TBUME2SI)NCH2CH2]3N) [J].
CUMMINS, CC ;
LEE, J ;
SCHROCK, RR ;
DAVIS, WD .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION IN ENGLISH, 1992, 31 (11) :1501-1503
[6]  
DUAN Z, IN PRESS INORG CHEM
[7]   LEWIS BASICITY OF SILATRANES AND THE MOLECULAR-STRUCTURES OF ETOSI(OCH2CH2)3N, ME2O+SI(OCH2CH2)3N, AND CF3CO2HETOSI(OCH2CH2)3N [J].
GARANT, RJ ;
DANIELS, LM ;
DAS, SK ;
JANAKIRAMAN, MN ;
JACOBSON, RA ;
VERKADE, JG .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1991, 113 (15) :5728-5735
[9]  
HIROSE M, 1983, Patent No. 68464
[10]  
LENSINK C, 1990, J AM CHEM SOC, V111, P3478