SYNTHESIS OF VANADIUM AND TITANIUM COMPLEXES OF THE TYPE RM[(ME3SINCH2CH2)3N] (R = CL, ALKYL) AND THE STRUCTURE OF CLV[(ME3SINCH2CH2)3N]

被引：130

作者：

CUMMINS, CC ^{[1
]}

SCHROCK, RR ^{[1
]}

DAVIS, WM ^{[1
]}

机构：

[1] MIT,DEPT CHEM,CAMBRIDGE,MA 02139

来源：

ORGANOMETALLICS | 1992年 / 11卷 / 04期

关键词：

D O I：

10.1021/om00040a011

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

Vanadium and titanium complexes of the type CIM[(Me3SiNCH2CH2)3N] have been synthesized by adding Li3[(Me3SiNCH2)3N] to MCl4L2 (M = Ti, L = THF; M = V, L2 = DME). An X-ray study of ClV[(Me3SiNCH2CH2)3N] (P2(1)/a, a = 15.167 (2) angstrom, b = 10.242 (2) angstrom, c = 16.301 (1) angstrom, beta = 93.705 (8)-degrees, V = 2527 (1) angstrom 3, Z = 4, T = -72-degrees-C, R = 5.8%, R(w) = 5.6%) showed it to be a monomer having pseudo-C3 symmetry. Addition of LiR (M = Ti, R = n-Bu, s-Bu; M = V, LiR = [Li.TMED]CH2SPh) to ClM-[(Me3SiNCH2CH2)3N] gave isolable alkyl derivatives, RM-[(MeSiNCH2CH2)3N]. When it is either heated (70-degrees-C) or treated with H-2 (3 atm, 25-degrees-C), s-BuTi-[(Me3SiNCH2CH2)3N] cleanly cyclometalates via an observable Ti(IV) hydride intermediate (Ti-H delta 8.29).

引用

页码：1452 / 1454

页数：3

共 41 条

[1] PREPARATION, PROPERTIES, AND CRYSTAL-STRUCTURES OF THE MONOCHLOROTRIS-[BIS(TRIMETHYLSILYL)AMIDO]-COMPOUNDS OF TITANIUM, ZIRCONIUM, AND HAFNIUM
AIROLDI, C
BRADLEY, DC
CHUDZYNSKA, H
HURSTHOUSE, MB
ABDULMALIK, KM
RAITHBY, PR
[J]. JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1980, (10): : 2010 - 2015
[2] IDENTIFICATION OF SOME INTERMEDIATES IN THE TITANOCENE-CATALYZED DEHYDROGENATIVE COUPLING OF PRIMARY ORGANOSILANES
AITKEN, CT
HARROD, JF
SAMUEL, E
[J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1986, 108 (14) : 4059 - 4066
[3] TRIS((HEXAMETHYLDISILYL)AMIDO)URANIUM(III) - PREPARATION AND COORDINATION CHEMISTRY
ANDERSEN, RA
[J]. INORGANIC CHEMISTRY, 1979, 18 (06) : 1507 - 1509
[4] CONVENIENT PREPARATION OF METAL PSEUDO-HALIDE COMPOUNDS
ANDERSEN, RA
[J]. INORGANIC & NUCLEAR CHEMISTRY LETTERS, 1980, 16 (01): : 31 - 32
[5] CHLORO[(HEXAMETHYLDISILYL)AMIDO]ZIRCONIUM(IV) AND METHYLTRIS[(HEXAMETHYLDISILYL)AMIDO]ZIRCONIUM(IV) AND CHLORO[(HEXAMETHYLDISILYL)AMIDO]HAFNIUM(IV) AND METHYLTRIS[(HEXAMETHYLDISILYL)AMIDO]HAFNIUM(IV)
ANDERSEN, RA
[J]. INORGANIC CHEMISTRY, 1979, 18 (06) : 1724 - 1725
[6] CRYSTAL AND MOLECULAR-STRUCTURE OF HYDRIDOTRIS[BIS(TRIMETHYLSILYL)AMIDO]URANIUM(IV)
ANDERSEN, RA
ZALKIN, A
TEMPLETON, DH
[J]. INORGANIC CHEMISTRY, 1981, 20 (02) : 622 - 623
[7] BIS(PENTAMETHYLCYCLOPENTADIENYL)TITANIUM(II) AND ITS COMPLEXES WITH MOLECULAR NITROGEN
BERCAW, JE
[J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1974, 96 (16) : 5087 - 5095
[8] Bradley D. C., 1978, INORG SYNTH, P112
[9] SYNTHESIS, PHOTOCHEMISTRY AND X-RAY CRYSTAL-STRUCTURES OF THE METHYLTRIS[BIS(TRIMETHYLSILYL)AMIDO] COMPOUNDS METI[N(SIME3)2]3 AND MEZR[N(SIME3)2]3
BRADLEY, DC
CHUDZYNSKA, H
BACKERDIRKS, JDJ
HURSTHOUSE, MB
IBRAHIM, AA
MOTEVALLI, M
SULLIVAN, AC
[J]. POLYHEDRON, 1990, 9 (11) : 1423 - 1427
[10] LOW SPIN 4-CO-ORDINATED CHROMIUM NITROSYL DIALKYLAMIDES AND ALKOXIDES
BRADLEY, DC
NEWING, CW
[J]. JOURNAL OF THE CHEMICAL SOCIETY D-CHEMICAL COMMUNICATIONS, 1970, (04): : 219 - &

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