Zirconium alkyls with ancillary cyclooctatetraenyl ligands. X-ray crystal structures of [Li(tmed)][(C8H8)Zr(p-C6H4Me)Cl2] and (C8H8)Zr[CH(SiMe3)2]2

被引:1
作者
Nelsen, Melissa J. [1 ]
Girolami, Gregory S. [1 ]
机构
[1] Univ Illinois, Sch Chem Sci, 600 South Mathews Ave, Urbana, IL 61801 USA
基金
美国国家科学基金会;
关键词
Zirconium; Hafnium; Alkyls; Aryls; Cyclooctatetraene; MOLECULAR-STRUCTURE; IMIDO COMPLEXES; METAL; DERIVATIVES; TITANIUM; BOND; CYCLOPENTADIENYL; STEREOCHEMISTRY; CONFORMATION; HAFNIUM;
D O I
10.1016/j.poly.2020.114581
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Several new group 4 alkyl and aryl compounds have been synthesized that possess ancillary cyclooctatetraene ligands. Most of the complexes isolated are anionic and have stoichiometries of [Li(tmed)(2)][(C8H8)-MRCl2], [Li(tmed)(x)][(C8H8)-MR2Cl], or [Li(tmed)(x)][(C8H8)MR3], where M = Zr or Hf, and R = Me, Ph, p-Tol, or CH(SiMe3)(2). Two neutral 14-electron compounds have also been prepared, (C8H8)M[CH(SiMe3)(2)](2 ), where R = Zr or Hf. The compound (C8H8)Zr[CH(SiMe3)(2)](2) appears to react reversibly with 7 atm of carbon monoxide but does not react with dihydrogen even at 70 atm. IR, H-1 and C-13 NMR data are reported, along with the crystal structures of two of the new compounds. (C) 2020 Published by Elsevier Ltd.
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页数:8
相关论文
共 35 条
[1]   IMPROVED SYNTHESIS AND STRUCTURE OF SOLVATED AND UNSOLVATED FORMS OF CYCLOOCTATETRAENE-ZIRCONIUM AND CYCLOOCTATETRANE-HAFNIUM DICHLORIDE [J].
BERNO, P ;
FLORIANI, C ;
CHIESIVILLA, A ;
RIZZOLI, C .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1991, (11) :3093-3095
[2]   CARBON HYDROGEN AND METAL-CARBON BOND FORMATION AND BREAKAGE IN THERMAL-REACTIONS OF BIS(MESITYL)(CYCLO-OCTATETRAENE)ZIRCONIUM(IV) DERIVATIVES - CRYSTAL-STRUCTURES OF [ZR(ETA-8-C8H8)(MES)2], [(ZR(ETA-8-C8H8)[ETA-OC(MES)2])2], [(ZR(ETA-8-C8H8)-(MU-2,4-ME2-6-CH2C6H2))2], AND [(ZR(ETA-8-C8H8))2(MU-MES)(MU-2,4-ME2-6-CHC6H2)] (MES = 2,4,6-ME3C6H2) [J].
BERNO, P ;
STELLA, S ;
FLORIANI, C ;
CHIESIVILLA, A ;
GUASTINI, C .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1990, (09) :2669-2677
[3]   BIS(CYCLOOCTATETRAENE) DERIVATIVES OF ZIRCONIUM(IV) AND HAFNIUM(IV) - SYNTHESES AND LEWIS BASE ADDUCTS - CRYSTAL-STRUCTURES OF [ZR(ETA-8-C8H8)(ETA-4-C8H8)], [HF(ETA-8-C8H6(SIME3)2)-(ETA-4-C8H6(SIME3)2)], [ZR(ETA-8-C8H8)(ETA-4-C8H8)(NH3)] AND [ZR(ETA-8-C8H8)(ETA-4-C8H8)(CNBUT)] [J].
BERNO, P ;
FLORIANI, C ;
CHIESIVILLA, A ;
RIZZOLI, C .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1991, (11) :3085-3091
[4]   Synthesis and molecular and electronic structure of monomeric [Ti(η8-C8H8)(NBut)] [J].
Blake, AJ ;
Dunn, SC ;
Green, JC ;
Jones, NM ;
Moody, AG ;
Mountford, P .
CHEMICAL COMMUNICATIONS, 1998, (11) :1235-1236
[5]   STEREOCHEMISTRY OF TRANSITION-METAL CYCLOOCTATETRAENYL COMPLEXES - TRIS(CYCLOOCTATETRAENE)DICHROMIUM, A NOVEL STEREOCHEMISTRY FOR A COMPOUND CONTAINING A QUADRUPLE METAL-METAL BOND [J].
BRAUER, DJ ;
KRUGER, C .
INORGANIC CHEMISTRY, 1976, 15 (10) :2511-2514
[6]   STEREOCHEMISTRY OF TRANSITION-METAL CYCLOOCTATETRAENYL COMPLEXES - MOLECULAR-STRUCTURE OF (ETA-CYCLOOCTATETRAENYL) (ETA-ALLYL)-TERT-BUTOXYZIRCONIUM [J].
BRAUER, DJ ;
KRUGER, C .
ORGANOMETALLICS, 1982, 1 (01) :204-207
[7]   MOLECULAR AND ELECTRONIC-STRUCTURES OF BIS[1,4-BIS(TRIMETHYL-SILYL)CYCLOOCTATETRAENE] SANDWICH COMPLEXES OF TITANIUM AND ZIRCONIUM [J].
CLOKE, FGN ;
GREEN, JC ;
HITCHCOCK, PB ;
JOSEPH, SCP ;
MOUNTFORD, P ;
KALTSOYANNIS, N ;
MCCAMLEY, A .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1994, (19) :2867-2874
[8]   FACILE FORMATION OF A BRIDGING CYCLOOCTATRIENEYNE LIGAND - SYNTHESIS AND MOLECULAR-STRUCTURE OF [(ETA-C8H6(SIME(3))(2))ZR(CH(SIME(3))(2))(MU-ETA(8)ETA(2)-C8H4(SIME(3))(2))ZR(CH(SIIME(3))(2))] [J].
CLOKE, FGN ;
HITCHCOCK, PB ;
JOSEPH, SCP .
JOURNAL OF THE CHEMICAL SOCIETY-CHEMICAL COMMUNICATIONS, 1994, (10) :1207-1208
[9]  
COPPENS P, 1974, J APPL CRYSTALLOGR, V7, P315, DOI 10.1107/S0021889874010259
[10]   PREPARATION AND STRUCTURES OF HOMOLOGOUS QUADRUPLY BONDED "TRIS(CYCLOOCTATETRAENE)DIMOLYBDENUM AND TRIS(CYCLOOCTATETRAENE)DITUNGSTEN [J].
COTTON, FA ;
KOCH, SA ;
SCHULTZ, AJ ;
WILLIAMS, JM .
INORGANIC CHEMISTRY, 1978, 17 (08) :2093-2098