Synthesis of hydride and alkyl compounds containing the CpOs(NO) fragment.: Crystal structure of [CpOs(μ-NO)]2

被引：42

作者：

Brumaghim, JL ^{[1
]}

Priepot, JG ^{[1
]}

Girolami, GS ^{[1
]}

机构：

[1] Univ Illinois, Sch Chem Sci, Urbana, IL 61801 USA

来源：

ORGANOMETALLICS | 1999年 / 18卷 / 11期

关键词：

D O I：

10.1021/om980657h

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

Treatment of the pentamethylcyclopentadienyl (Cp*) compound Cp*Os(NO)Br-2 (1) with NaBH4 yields the dihydride Cp*Os(NO)Hz. The dihydride loses Hz over several days in solution to form [Cp*Os(mu-NO)](2); this dinuclear compound can also be formed directly by reduction of 1 with zinc powder. The X-ray crystal structure of [Cp*Os(mu-NO)](2) shows that nitrosyl ligands are bridging and that the Os-Os distance is 2.539(1) Angstrom. Compound 1 reacts with MgR2 to form the monoalkylated products Cp*Os(NO)RBr, where R = Me, CH2SiMe3, Ph, or o-Tol. The slow ligand substitution kinetics of this reaction prevent the formation of dialkyls of stoichiometry Cp*Os(NO)R-2, even after long reaction times or when a large excess of alkylating agent is used. Dialkyls such as Cp*Os(NO)Me-2 can, however, be obtained by treatment of Cp*Os(NO)MeBr with silver trifluoromethanesulfonate followed by addition of dimethylmagnesium.

引用

页码：2139 / 2144

页数：6

共 50 条

[21] Synthesis and Crystal Structure of [Cp2Ln(OC（SEt）NPh )]2
ZHANG Chun-Meia
Chinese Journal of Structural Chemistry, 2006, (02) : 131 - 134
[22] The reactivity of lanthanide alkyl compounds with phenylacetylene: Synthesis and structure of [(Bu(t)Cp)(2)LnC CPh](2) (Ln=Nd, Gd)
Ren, JS
Hu, JY
Lin, YH
Xing, Y
Shen, Q
POLYHEDRON, 1996, 15 (13) : 2165 - 2169
[23] The synthesis of alkyl niobocene imido complexes and the X-ray crystal structure of [Nb(=O)CP2Me] (CP = η5-C5H5)
Antiñolo, A
López-Solera, I
Otero, A
Prashar, S
JOURNAL OF ORGANOMETALLIC CHEMISTRY, 2001, 631 (1-2) : 151 - 156
[24] PREPARATION AND CRYSTAL-STRUCTURE OF THE ISOTYPIC COMPOUNDS CA2OS3B5 AND EU2OS3B5
SCHWEITZER, K
JUNG, W
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 1986, 533 (02): : 30 - 36
[25] Cluster build-up reactions via the ionic coupling of tetraosmium anions and the [RhCp*(NCMe)3]2+ cation;: the crystal and molecular structures of [Os4Rh(μ-H)3(MeC=NH)(CO)11(η5-Cp*)], [Os4Rh(μ-H)2(CO)13(η5-Cp*)] and [Os4Rh2(μ-H)2(CO)11(η5-Cp*)2] (Cp*=C5Me5)
Clegg, W
Feeder, N
Castro, AMM
Nahar, S
Raithby, PR
Shields, GP
Teat, SJ
JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1999, 573 (1-2) : 237 - 246
[26] CRYSTAL STRUCTURE OF THE RARE-EARTH-RICH OSMIUM COMPOUNDS R3Os AND Y3Os.
Palenzona, A.
Journal of the less-common metals, 1980, 72 (01):
[27] Synthesis and structure of Cp*2TiH, Cp*2TiH2Li(tmed), and [Cp*2TiOLi(THF)]2
Lukens, WW
Matsunaga, PT
Andersen, RA
ORGANOMETALLICS, 1998, 17 (24) : 5240 - 5247
[28] Comparison of the One-Electron Oxidations of CO-Bridged vs Unbridged Bimetallic Complexes: Electron-Transfer Chemistry of Os2Cp2(CO)4 and Os2Cp2*(μ-CO)2(CO)2 (Cp = η5-C5H5, Cp* = η5-C5Me5)
Laws, Derek R.
Bullock, R. Morris
Lee, Richmond
Huang, Kuo-Wei
Geiger, William E.
ORGANOMETALLICS, 2014, 33 (18) : 4716 - 4728
[29] Synthesis and characterization of scandium complexes with reduced ligands:: Crystal structures of Cp*ScI2, [Cp*ScI(bpy)]2, and [Cp*ScCl(bpy)]2
Tupper, KA
Tilley, TD
JOURNAL OF ORGANOMETALLIC CHEMISTRY, 2005, 690 (07) : 1689 - 1698
[30] Synthesis and structure of Cp2*TiH, Cp2*TiH2Li(tmed), and [Cp2*TiOLi(THF)]2
Organometallics, 24 (5240-5247):

← 1 2 3 4 5 →

Synthesis of hydride and alkyl compounds containing the Cp*Os(NO) fragment.: Crystal structure of [Cp*Os(μ-NO)]2

Synthesis of hydride and alkyl compounds containing the CpOs(NO) fragment.: Crystal structure of [CpOs(μ-NO)]2