The synthesis and spectroscopic identification of [(η5-C5H5)Re(N2)3] and [(η5-C5H5)Re(CO)(N2)2] in supercritical xenon at room temperature and in N2matrices at 20 K

Howdle, Steven M.; Grebenik, Peter D.; Perutz, Robin N.; Poliakoff, Martyn

doi:10.1039/c39890001517

Cited by 21 publications

(16 citation statements)

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“…The table also shows that SCFs allow the multiple substitution of CO by N2 to occur [4,5,32]. This is perhaps one of the most intriguing features of this chemistry (Scheme 4.2-1).…”

Section: Chemistrymentioning

confidence: 89%

“…Under those conditions, the low temperatures of the liquid gas solvent helped to stabilize complexes [24], such as Ni(C0)3N2, which would have been very short lived at ambient temperatures. In most cases, characterization of the metal carbonyl moiety via v(C-0) IR bands is definitive, particularly if library spectra are available from liquid noble gas [23] or matrix isolation experiments [4]. There are a number of important points which should be made about the compounds listed in the Table. Nearly all of the compounds were synthesized photochemically, which imposes a number of quite strict limitations on larger-scale preparations of these compounds.…”

Section: Chemistrymentioning

confidence: 99%

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Synthesis of Coordination Compounds

King¹,

Poliakoff²

1999

Chemical Synthesis Using Supercritical Fluids

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Historically, interest in supercritical fluids (SCFs) has been cyclical or, perhaps more accurately, sinusoidal. Currently, research into SCFs is undergoing a substantial resurgence, largely driven by possible applications in so-called "green" chemistry, where supercritical C02 (scCO2) offers considerable scope as an environmentally more acceptable replacement for conventional organic solvents. However, the emphasis here is rather different because the synthesis of new organometallic or coordination compounds in SCFs does not have such obviously. green applications as homogeneous catalysis (see chapter 4.7). Nevertheless, these compounds occupy an important place in SCF chemistry because they represent a large number of the new compounds which have been prepared in SCF solution.The use of coordination compounds in SCFs is rather larger than one might initially expect [I]. The major applications can be divided into two broad categories: (1) the transport of metals, which includes selective extraction, deposition of metal and oxide films and impregnation of metals as a route to composite materials; and (2) synthesis and reactions, which covers a wide range of topics from the synthesis of oxides and other solid state materials to the reactions of organometallic compounds. This chapter focuses on the synthesis of organometallic compounds because this is the area where the majority of the new experimental techniques have been developed. The chapter complements chapter 3.1 and 3.2 which cover, respectively, vibrational and NMR spectroscopy, because IR spectroscopy, and to a lesser extent NMR, have been key tools in the exploration of this chemistry.The chapter is divided into four parts: Strategy, which explains the rationale for carrying out these reactions in SCF solution; Chemistry, which outlines what the reactions are; Equipment, which describes some of the key components and introduces a modular approach to high pressure experiments; and Synthesis, which gives details of how to make particular compounds, including the use of flow reactors and semiflow reactors. It concludes with a brief summary and outlook.

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“…The table also shows that SCFs allow the multiple substitution of CO by N2 to occur [4,5,32]. This is perhaps one of the most intriguing features of this chemistry (Scheme 4.2-1).…”

Section: Chemistrymentioning

confidence: 89%

Section: Chemistrymentioning

confidence: 99%

Synthesis of Coordination Compounds

King¹,

Poliakoff²

1999

Chemical Synthesis Using Supercritical Fluids

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“…Reactions in scCO 2 were performed in a stainless-steel high pressure batch reactor specially designed at the University of Nottingham. 14 The batch reactor (autoclave) equipped with a magnetic stirrer had an internal volume of 8.5 mL and was placed on an IKA Labotecknick RCT basic stirring plate. Solid substrates and reactants and stirrer bar were added into the reactor prior to sealing using a clamp.…”

Section: Methodsmentioning

confidence: 99%

Dynamic kinetic resolution of rac-1-phenylethanol in supercritical carbon dioxide

2009

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“…Reactions in scCO 2 were performed in a stainless-steel high pressure batch reactor specially designed at the University of Nottingham. 25 The batch reactor (autoclave) equipped with a magnetic stirrer bar has an internal volume of 8.5 mL and was placed on an IKA Labotecknick RCT basic stirring plate. Solid substrates and reactants and stirrer bar were added into the reactor prior to sealing.…”

Section: Batch Reactionsmentioning

confidence: 99%