Moisture-sensitive Compounds Research Articles

First synthesis and structures of aryltellurium(IV) diazides.

Into the small family of chalcogen azides come the first two aryl-substituted tellurium(IV) diazides R2Te(N3)2 (R = Ph or C6F5) by a surprisingly easy synthesis. Structural and spectroscopic investigations of these moisture-sensitive compounds exhibit interesting differences in the sterical arrangement between phenyl and pentafluorophenyl substituents.

Magnesiation of Isodicyclopentadiene. Formation of Sandwich and Monomeric Complexes and the Stereoselectivity of Their Reactions with Transition Metal Halides

The exo,exo-bis(isodicyclopentadienyl)magnesium sandwich and the monomeric exo-(isodicyclopentadienyl)butylmagnesium TMEDA complex have been synthesized and characterized by 1H and 13C NMR spectroscopy in C6D6 solution. The solid-state structures were determined by X-ray crystallography. The stereoselectivity with which both moisture-sensitive compounds react with TiCl3·3THF and ZrCl4 was assessed and suitably compared to related observations recorded for alkali metal (Li+, Na+, and K+) complexes of isodicyclopentadiene.

Dynamic 7Li NMR investigation of dianionic dibenzotetraaza[14]annulene derivatives in solution

Deprotonation of the two dibenzotetraaza[14]annulenes ( 1, H 2L, 6, 8, 15, 17-tetramethyldibenzotetraaza[14]annulene and 6, 15-dimethyl-8, 17-diphenyldibenzotetraaza[14]annulene) by LiCH 3 in ether yielded the corresponding dilithium dibenzotetraaza[14]annulene complexes 2 (Li 2L × n ether) as solvates. These extremely moisture-sensitive compounds have been isolated as deep red solids and characterized by 1H, 13C, variable-temperature 7Li NMR and UV spectroscopies. Based on solution NMR investigations both complexes contain two different Li + environments: one Li + ion is coordinated to the nitrogen centres of the dianionic annulene ([LiL] −), while the second Li + ion is coordinated by ether oxygen atoms and weakly to nitrogen centres of the dianionic annulene. Variable-temperature 7Li NMR spectroscopy between 213 and 300 K indicates a rapid exchange process ( E A ca 47±3 kJ mol −1) between the two types of Li + environments. In the presence of TMEDA (N,N′-tetramethylethylenediamine), the exchange process is slowed ( E A ca 59±5 kJ mol −1) due to stronger coordination of the TMEDA-solvated Li +. These results are discussed with respect to the known coordination behaviour of the Li + ion towards macrocyclic nitrogen donors.

Photomicrocalorimetry: Photosubstitution of carbonyl by phosphites in [Mn(η 5-C 5H 4CH 3)(CO) 3

A photomicrocalorimeter is described for studies of reactions involving oxygen and moisture-sensitive compounds in organic solvents. This calorimeter was used to investigate the thermochemistry of photochemical substitutions of a carbonyl in [Mn(η 5C 5H 4CH 3)(CO) 3] by P(OR) 3 (R  Ph or 1Pr). The measured reaction enthalpies in heptane (λ = 400 nm), ΔH r = −15.7 ± 0.5 and −18.6 ± 0.9 kJ mol −1, respectively, were identified with the bond dissociation enthalpy differences D(MnCO)  D[MnP(OPh) 3] and D(MnCO)  D[Mn-P(O iPr) 3] in solution. These results are discussed in terms of the basicity of the phosphates, spectroscopic data of the complexes (CO stretching frequencies), and the available thermochemical data for other transition metal-phosphorus(III) ligand interactions.

Amido complexes of (cyclopentadienyl)dichlorotitanium(IV): titanium-nitrogen multiple-bond character

Reaction of (RC 5 H 4 )TiCl 3 (1a, R=H; 1b, R=CH 3 ) with Li{NH(t-Bu)} in THF affords (RC 5 H 5 )TiCl 2 {NH(t-Bu)) (2a, R=H; 2b, R=CH3) in 80-90% isolated yields. The moisture-sensitive red-orange compounds can becrystallized from CH 2 Cl 2 /hexane mixtures. The X-ray structures for the two compounds were determined and found to be similar.

Compact Fourier transform infrared spectrometer inside a glove box: Fourier transform spectroelectrochemistry and other applications

Use of a compact Fourier transform infrared (FT-IR) spectrometer inside a glove box to investigate air and moisture sensitive compounds is reported. The FT-IR spectrometer, manufactured by Midac Co., measures 18 cm × 28 cm × 61 cm and can be conveniently placed inside a standard glove box (Vacuum Atmospheres). This match of a low cost, compact FT-IR spectrometer with widely available glove box technology affords researchers a simple, routine method for acquiring FT-IR data for air and moisture sensitive compounds. Several applications are illustrated, including reaction kinetics and FT-IR spectroelectrochemistry. A design for an FT-IR spectroelectrochemical cell is also described.

Compact Fourier transform infrared spectrometer inside a glove box: Fourier transform spectroelectrochemistry and other applications

Use of a compact Fourier transform infrared (FT-IR) spectrometer inside a glove box to investigate air and moisture sensitive compounds is reported. The FT-IR spectrometer, manufactured by Midac Co., measures 18 cm × 28 cm × 61 cm and can be conveniently placed inside a standard glove box (Vacuum Atmospheres). This match of a low cost, compact FT-IR spectrometer with widely available glove box technology affords researchers a simple, routine method for acquiring FT-IR data for air and moisture sensitive compounds. Several applications are illustrated, including reaction kinetics and FT-IR spectroelectrochemistry. A design for an FT-IR spectroelectrochemical cell is also described.

Tetrakisisopropoxy tantalum(V)O, O?-alkylene dithiophosphate complexes

Tetrakisisopropoxytantalum(V) alkylene dithiophosphato complexes, (G=−CMe2CMe2−, −CHMeCHMe−, −CH2CMe2CH2− and −CH2CEt2CH2−) have been prepared from equimolar ratios of tantalum(V) isopropoxide and alkylene dithiophosphoric acids in benzene. These moisture-sensitive compounds, which are soluble in common organic solvents and are monomeric, have been characterized by elemental analysis, molecular weight determinations and by their i.r. and n.m.r. spectra. An octahedral geometry is suggested in which the ligand is bidentate.

A reusable apparatus for the convenient determination of the molecular weight of air- or moisture-sensitive compounds

ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTA reusable apparatus for the convenient determination of the molecular weight of air- or moisture-sensitive compoundsRobert W. Zoellner Cite this: J. Chem. Educ. 1990, 67, 8, 714Publication Date (Print):August 1, 1990Publication History Received3 August 2009Published online1 August 1990Published inissue 1 August 1990https://doi.org/10.1021/ed067p714RIGHTS & PERMISSIONSArticle Views249Altmetric-Citations21LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit PDF (1 MB) Get e-Alerts Get e-Alerts

ChemInform Abstract: Dicarbollide Complexes of Samarium and Ytterbium. Synthesis and Structural Characterization of the First closo‐Lanthanacarboranes.

AbstractThe air and moisture sensitive compounds (IV) are obtained by anaerobic addition of a THF solution of (I) to equimolar solutions of (II).

Apparatus for absorption spectroscopy of temperature and moisture sensitive compounds

ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTApparatus for absorption spectroscopy of temperature and moisture sensitive compoundsMark E. Jason Cite this: J. Chem. Educ. 1982, 59, 9, 803Publication Date (Print):September 1, 1982Publication History Received3 August 2009Published online1 September 1982Published inissue 1 September 1982https://doi.org/10.1021/ed059p803RIGHTS & PERMISSIONSArticle Views29Altmetric-Citations-LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit PDF (429 KB) Get e-Alerts Get e-Alerts

Convenient apparatus for determining molecular weights of moisture-sensitive compounds by a modified Rast method

An apparatus easily assembled from readily available components is described for the determination of molecular weights of moisture-(and/or oxygen-) sensitive compounds by a modified Rast method. A procedure for sealing moisture- (and/or oxygen-) sensitive compounds in capillary tubes is also described.

Preparation of nmr samples of air and moisture sensitive compounds

The simple procedure described in this note was developed in a laboratory for the production of contaminant free NMR samples.

An efficient gas chromatographic effluent trap for collecting air- and moisture-sensitive compounds

An efficient gas chromatographic effluent trap for collecting air- and moisture-sensitive compounds

An Improved Fraction Collector for the Distillation and Subsequent Handling of Air and/or Moisture Sensitive Compounds

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Colligative property measurements on oxygen- and moisture-sensitive compounds. I. Organolithium reagents in donor solvents at 25.degree.

Colligative property measurements on oxygen- and moisture-sensitive compounds. I. Organolithium reagents in donor solvents at 25.degree.

Microanalysis of air and moisture sensitive compounds

Complete elemental microanalysis was performed on a series of air and (or) moisture sensitive compounds, utilizing rapid automatic combustion instruments. Techniques are described for protecting these samples from the air and for effecting complete combustion through the use of additives.

Technique for infrared measurements on solutions of moisture-sensitive compounds

Presents a device and method for infrared measurements on solutions of moisture-sensitive compounds.