Titanium(IV) neopentoxides. X-ray structures of Ti-3(mu(3)-Cl)(mu-OCH2CMe3)(3)(OCH2CMe3)(6) and [Ti(mu-OCH2CMe3)(OCH2CMe3)(3)](2)

被引:86
作者
Boyle, TJ
Alam, TM
Mechenbier, ER
Scott, BL
Ziller, JW
机构
[1] LOS ALAMOS NATL LAB,CST 18,CHEM SCI & TECHNOL DIV,XRAY DIFFRACT LAB,LOS ALAMOS,NM 87545
[2] UNIV CALIF IRVINE,DEPT CHEM,XRAY DIFFRACT LAB,IRVINE,CA 92717
关键词
D O I
10.1021/ic960924g
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Attempts to synthesize titanium(IV) neopentoxide led to two unique products which were crystallographically characterized. A metathesis reaction between TiCl4 and NaOCH2CMe3 (NaONp) yielded Ti-3(O)(Cl)(ONp)(9) . C7H8, 1, which adopts a standard M-3(mu(3)-X)(2)(mu-X)(3)X-6 structure. The mu(3) ligands are a Cl and an O atom, with the lest of ligands represented by bridging and terminal ONp ligands. [Ti(ONp)(4)](2), 2, was isolated in high yield by an alcoholysis exchange between Ti(OPri)(4) and HONp. 2 adopts a typical M-2(mu-X)(2)(X)(6) fused axial-equatorial edge-shared geometry, wherein each metal center is 5 coordinated. On the basis of molecular weight solution studies and H-1, C-13, O-17 (natural abundance), and Ti-47,Ti-49 solution and solid-state NMR investigations, 2 was determined to be a monomer in solution.
引用
收藏
页码:3293 / 3300
页数:8
相关论文
共 73 条
[1]  
ABIS L, 1991, MAKROMOL CHEM, V192, P981
[2]   SYNTHESIS AND PROPERTIES OF POLYACETYLENE FILMS PREPARED BY TI(OET)4-ALME3 CATALYST SYSTEM [J].
AKAGI, K ;
MOCHIZUKI, K ;
AOKI, Y ;
SHIRAKAWA, H .
BULLETIN OF THE CHEMICAL SOCIETY OF JAPAN, 1993, 66 (11) :3444-3450
[3]   SYNTHESIS OF NEW TITANIUM OXO CLUSTER COMPOUNDS - X-RAY STRUCTURE OF THE TETRANUCLEAR OXIDE [TI4CL6(MU-2-O2CPH)6(MU-3-O)2] [J].
ALCOCK, NW ;
BROWN, DA ;
ROE, SM ;
WALLBRIDGE, MGH .
JOURNAL OF THE CHEMICAL SOCIETY-CHEMICAL COMMUNICATIONS, 1992, (11) :846-848
[4]   PREPARATION AND PROPERTIES OF SOME CHLOROTITANIUM CARBOXYLATES - X-RAY CRYSTAL AND MOLECULAR-STRUCTURES OF [(TICL3(O2CCME3))3] AND [TI2CL7(O2CR)(RCO2H)] (R = P-CLC6H4 OR CH = CHME) [J].
ALCOCK, NW ;
BROWN, DA ;
ILLSON, TF ;
ROE, SM ;
WALLBRIDGE, MGH .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1991, :873-881
[5]  
[Anonymous], 1992, INT TABLES XRAY CRYS, VC
[6]   UNEXPECTED FORMATION AND STRUCTURE OF NEW TRINUCLEAR TITANIUM(IV)-ORGANYL CATIONS IN BISCYCLOPENTADIENYL-HEXAQUA-TITANIUM(IV) CATIONS AND METHANOL [J].
ASLAN, H ;
SIELISCH, T ;
FISCHER, RD .
JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1986, 315 (03) :C69-C72
[7]   XANES AND EXAFS STUDY OF TITANIUM ALKOXIDES [J].
BABONNEAU, F ;
DOEUFF, S ;
LEAUSTIC, A ;
SANCHEZ, C ;
CARTIER, C ;
VERDAGUER, M .
INORGANIC CHEMISTRY, 1988, 27 (18) :3166-3172
[8]   SOLUTION STUDY OF THE AMBIENT-TEMPERATURE MONOMER-DIMER EQUILIBRIUM TH-2(OR)(8)REVERSIBLE-ARROW-2TH(OR)(4) (R=CH-I-PR-2) AND X-RAY CRYSTAL-STRUCTURES OF TH-2(OCH-I-PR-2)(8), TH(OCH-I-PR-2)(4)(QUIN), AND THI(OCH-I-PR-2)(3)(PY)(2) [J].
BARNHART, DM ;
CLARK, DL ;
GORDON, JC ;
HUFFMAN, JC ;
WATKIN, JG ;
ZWICK, BD .
INORGANIC CHEMISTRY, 1995, 34 (22) :5416-5423
[9]   TITANIUM OXO CARBOXYLATE COMPOUNDS - CRYSTAL AND MOLECULAR-STRUCTURES OF [(TICL2(O(2)CET)(ETCO2H)2O] AND [TI3CL3O2(O(2)CET)(5)] AND AN UNUSUAL QUANTITATIVE CONVERSION OF A TI2O TO A TI3O2 OXO DERIVATIVE [J].
BARROW, H ;
BROWN, DA ;
ALCOCK, NW ;
ERRINGTON, W ;
WALLBRIDGE, MGH .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1994, (24) :3533-3538
[10]   A CONVENIENT HIGH-YIELD SYNTHESIS OF SOME TITANIUM(IV) OXO CLUSTER COMPOUNDS - CRYSTAL-STRUCTURE OF [TI3CL3(MU-O2CC6H4ME-P)5(MU-O)(MU-3-O)] [J].
BASHALL, A ;
BROWN, DA ;
MCPARTLIN, M ;
WALLBRIDGE, MGH .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1992, (16) :2529-2530