Distribution by Scientific Domains

Kinds of Analysis.

  • crystal structure analysis.
  • diffraction analysis.
  • structure analysis.
  • x-ray analysis.
  • x-ray crystal structure analysis.
  • x-ray diffraction analysis.

  • Selected Abstracts

    Practitioner assessments of ,good enough' parenting: factorial survey

    Julie Taylor
    Aim., The aim of this study was to measure health visitors' professional judgements on ,good enough' parenting and identify what factors and combinations of these are important when making such judgements. Background., The relationship between parenting and child health is unclear. Whilst agreement exists that ,good enough' parenting requires boundary setting, consistency and putting the child's needs first, attempting to define ,good enough' parenting in precise terms is complex. When faced with a complex situation, practitioners rely on relatively few factors to form judgements. Design., Factorial survey methods were employed using vignette techniques. Methods., Vignettes were constructed using previous research on those variables, which may influence nurses' judgements, for example, accommodation and child dentition. The level of factors was randomly varied. Two thousand vignettes were administered to a sample of 200 health visitors in two Health Boards who then made a judgement about this scenario. Analysis., Data were analysed through multiple regression with dummy variables and one-way analysis of variance. Regression equations for both good enough mothering and good enough parenting are reported. Results., The models used are significant predictors of parenting and mothering. Significant predictors on health visitor judgements' were boundary setting in sleep behaviours, type of housing inhabited and health behaviours. Although parenting and mothering are often conflated, health visitors appear to separate these aspects when making judgements based on type of housing. Conclusions., Most professionals can articulate what makes a ,good' parent, equally they may have strong views regarding what constitutes ,poor' parenting. The difficulty is in determining when parenting is ,good enough' to provide a child with a nurturing environment. Relevance to clinical practice., This study suggests that practitioners move their thresholds of what is ,good enough' depending on a narrow range of factors. Awareness of the factors, which influence individuals' judgements is important in safeguarding children. [source]

    A study of a training scheme for Macmillan nurses in Northern Ireland

    BSocSc, Cert Ed., DipDN, Johnston Gail PhD
    Aim., To evaluate a one year training scheme for Macmillan Nurses. Background., The role of the clinical nurse specialist has evolved and expanded greatly over the past few years so that it now encompasses components far beyond the traditional nursing remit of direct clinical practice. While several studies have looked at the barriers and facilitators to this process for clinical nurse specialists in particular, none has looked at the benefits of a structured training scheme which involves both a theoretical and clinical component. Methods., Tape recorded, semi-structured interviews were undertaken with a purposive sample of trainees who undertook the scheme, their practice-based facilitators and another person(s) involved in the trainee's support Analysis., Tapes were transcribed verbatim and each transcript anonymized to prevent identification of participants. Data were analysed thematically using the main headings of expectations, experience and impact and the structured prompts from the aide-memoir within these headings. Results., Results showed that the majority of respondents felt the scheme had been successful with one of the main achievements being that trainees were perceived to be adequately prepared to take on the role of a CNS on completion of the scheme. While the Role Development Programme was thought to provide a good academic structure for the scheme some participants thought that more theory on symptom control and communication skills and a placement in a specialist palliative care centre should also be included. Conclusion., The Macmillan Trainee Scheme has succeeded in its objectives to facilitate the transition from generalist to specialist nursing. It should be extended to include an induction and consolidation period and more theoretical input on communication skills and symptom control. Relevance to clinical practice., With these improvements, the scheme could be used as a standard model for training specialist practitioners and a means to address the current issues of workforce planning. [source]

    MLJ,Reviews: Working with Texts: A Core Introduction to Language Analysis. by CARTER, RONALD, ANGELA GODDARD, DANUTA REAH, KEITH SANGER, & NIKKI SWIFT

    No abstract is available for this article. [source]

    Frequency of the sit-to-stand task: a pilot study of free-living adults

    Andy Kerr
    Purpose.,To report contemporary data on the daily frequency of the sit-to-stand (STS) movement in a healthy, independently living, adult population.,Relevance.,As a key determinant of functional independence, which has a high mechanical load, the STS movement is a common feature of rehabilitation. Knowledge of STS frequency during daily activities could inform rehabilitation goals and content, but has rarely been examined. To date, only McLeod et al. (1975) have investigated this, reporting an average of 92 daily STS transitions in healthy young participants.,Methods.,Fifteen healthy, free-living, ambulant adults (three males; mean age 40 years) were recruited from the general population. An activity monitor (activPALTM, PALtechnologies, Glasgow, UK) reported free-living activity for each subject for seven consecutive days.,Analysis.,The average number of STS transitions per day was calculated from the whole period. Data were separated into working and non-working days, and compared using a paired t-test.,Results.,On average, participants performed 64 (±19) STS movements each day, with large individual differences [range 35,105]. Participants performed significantly (p = 0.047) more STS movements on a working day [68 (±24)] than on a non-working day [55 (±17)].,Discussion.,Fewer STS movements were recorded than previously reported (McLeod et al., 1975). This may reflect general changes in lifestyle; however, comparisons should consider the small samples involved and methodological differences.,Conclusion.,This study provides contemporary data for STS frequency and demonstrates a significant difference between working and non-working days. This information could guide rehabilitation and future research. Copyright © 2008 John Wiley & Sons, Ltd. [source]

    A data logger for teaching data capturing and analysis to engineering students

    Dogan IbrahimArticle first published online: 17 FEB 200
    Abstract Data logging is the process of collecting and storing data from an experiment. Traditionally, data from science experiments was collected manually by hand and graphs were produced using pen and paper. By the introduction of cheap and powerful microcontrollers, all data logging operations are currently carried out using microcontroller-based data logging devices. This article describes the design of an educational microcontroller-based data logger device, which can be used to collect and save data for both offline and online analysis. © 2009 Wiley Periodicals, Inc. Comput Appl Eng Educ 18: 397,405, 2010; Published online in Wiley InterScience (; DOI 10.1002/cae.20281 [source]

    A software player for providing hints in problem-based learning according to a new specification

    Pedro J. Muñoz-Merino
    Abstract The provision of hints during problem solving has been a successful strategy in the learning process. There exist several computer systems that provide hints to students during problem solving, covering some specific issues of hinting. This article presents a novel software player module for providing hints in problem-based learning. We have implemented it into the XTutor Intelligent Tutoring System using its XDOC extension mechanism and the Python programming language. This player includes some of the functionalities that are present in different state-of-the-art systems, and also other new relevant functionalities based on our own ideas and teaching experience. The article explains each feature for providing hints and it also gives a pedagogical justification or explanation. We have created an XML binding, so any combination of the model hints functionalities can be expressed as an XML instance, enabling interoperability and reusability. The implemented player tool together with the XTutor server-side XDOC processor can interpret and run XML files according to this newly defined hints specification. Finally, the article presents several running examples of use of the tool, the subjects where it is in use, and results that lead to the conclusion of the positive impact of this hints tool in the learning process based on quantitative and qualitative analysis. © 2009 Wiley Periodicals, Inc. Comput Appl Eng Educ 17: 272,284, 2009; Published online in Wiley InterScience (; DOI 10.1002/cae.20240 [source]

    Virtual laboratory: A distributed collaborative environment

    Tiranee Achalakul
    Abstract This article proposes the design framework of a distributed, real-time collaborative architecture. The architecture concept allows information to be fused, disseminated, and interpreted collaboratively among researchers who live across continents in real-time. The architecture is designed based on the distributed object technology, DCOM. In our framework, every module can be viewed as an object. Each of these objects communicates and passes data with one another via a set of interfaces and connection points. We constructed the virtual laboratory based on the proposed architecture. The laboratory allows multiple analysts to collaboratively work through a standard web-browser using a set of tools, namely, chat, whiteboard, audio/video exchange, file transfer and application sharing. Several existing technologies are integrated to provide collaborative functions, such as NetMeeting. Finally, the virtual laboratory quality evaluation is described with an example application of remote collaboration in satellite image fusion and analysis. © 2004 Wiley Periodicals, Inc. Comput Appl Eng Educ 12: 44,53, 2004; Published online in Wiley InterScience (; DOI 10.1002/cae.20008 [source]


    ECONOMIC INQUIRY, Issue 4 2008
    Dawkins, Srinivasan, and Whalley ("Calibration,"Handbook of Econometrics, 2001) propose that estimation is calibration. We illustrate their point by examining a leading econometric application in the study of international and interregional trade by Anderson and van Wincoop ("Gravity with Gravitas: A Solution to the Border Puzzle,"American Economic Review, 2003). We replicate the econometric process and show it to be a calibration of a general equilibrium model. Our approach offers unique insights into structural estimation, and we highlight the importance of traditional calibration considerations when one uses econometric techniques to calibrate a model for comparative policy analysis. (JEL F10, C13, C60) [source]

    A technique of waveform judgment for harmonic analysis on distribution lines

    Tadao Aizawa
    Abstract Most general-purpose analyzers for harmonic analysis on distribution lines are designed to sample the data of one or two power supply periods. In other words, these analyzers process waveforms and display the results based on the assumption that the analyzed waveforms contain no noninteger components, such as subharmonics and interharmonics. When waveforms containing noninteger components are analyzed with these general-purpose analyzers, the results often indicate components that are not actually present. This paper proposes a technique of waveform judgment and explains its method of application. The technique allows noninteger components to be recognized in analyzed waveforms from the properties of Lissajous figures, and clarifies the types of components and the time windows necessary for appropriate analysis. © 2008 Wiley Periodicals, Inc. Electr Eng Jpn, 166(2): 32, 38, 2009; Published online in Wiley InterScience ( DOI 10.1002/eej.20536 [source]

    Cover Picture: Electrophoresis 10'2010

    ELECTROPHORESIS, Issue 10 2010
    Article first published online: 18 MAY 2010
    Issue no. 10 is a regular issue comprising 19 manuscripts distributed over four distinct parts. Part I is on microfluidics and miniaturized systems and has 5 articles; Part II is on nucleic acids with 4 articles on restriction endonuclease fingerprinting, mutation detection and DNA separation and detection; Part III has 7 articles on monolithic stationary phases for CEC, single walled carbon nanohorns as pseudo-stationary phases for CEC and EKC, MEEKC, cyclodextrin-modified gold nanoparticles for enantioseparations by CEC, use of divalent dipeptides as counter ions in CE and capillary coating for CE of proteins; and Part IV has 3 articles on proteomics methodologies. Featured articles include: Microfluidic preparative free-flow isoelectric focusing in a triangular channel: System development and characterization ((10.1002/elps.200900577)) Separation and recovery of nucleic acids with improved biological activity by acid-degradable polyacrylamide gel electrophoresis ((10.1002/elps.200900783)) Evaluation of the performance of single-walled carbon nanohorns in capillary electrophoresis ((10.1002/elps.200900628)) The inter- and intra-operator variability in manual spot segmentation and its effect on spot quantitation in two dimensional electrophoresis analysis. ((10.1002/elps.200900674)) [source]

    Cover Picture: Electrophoresis 8'2010

    ELECTROPHORESIS, Issue 8 2010
    Article first published online: 20 APR 2010
    Issue no. 8 is a regular issue comprising19 manuscripts distributed over four distinct parts. Part I is on proteins and proteomics and has 5 articles; Part II is on nucleic acids with 5 articles on DNA purification, sequencing, genotyping and differential gene expression; Part III has 4 articles on droplet dispensing and particle separation; Part IV is on various methodologies and applications assembling 5 articles on improved sample preparation method for glycan analysis by CE, measurement of intracellular accumulation chemotherapeutic drugs in cancerous cells, metabolic monitoring in microfluidic cell arrays, microchip electrophoresis for continuous monitoring of microdialysis samples, and determination of glyphosate and its metabolites in plant materials by CE. Featured articles include: Delta2D and Proteomweaver: Performance evaluation of two different approaches for two-dimensional electrophoresis analysis. ((10.1002/elps.200900766)) A Multidimensional Electrophoretic System of Separation for the Analysis of Gene Expression (MESSAGE). ((10.1002/elps.200900624)) Particle trapping using dielectrophoretically patterned carbon nanotubes. ((10.1002/elps.200900717)) [source]

    Isolation and properties of methanesulfonate-degrading Afipia felis from Antarctica and comparison with other strains of A. felis

    S. Azra Moosvi
    Summary Three novel strains of methylotrophic Afipia felis were isolated from several locations on Signy Island, Antarctica, and a fourth from estuary sediment from the River Douro, Portugal. They were identified as strains of the ,-2 proteobacterium A. felis by 16S rRNA gene sequence, analysis., Two, strains, tested, were, shown to contain the fdxA gene, diagnostic for A. felis. All strains grew with methanesulfonate (and two strains with dimethylsulfone) as sole carbon substrate. Growth on methanesulfonate required methanesulfonate monooxygenase (MSAMO), using NADH as the reductant and stimulated by reduced flavin nucleotides and Fe(II). Polymerase chain reaction amplification of DNA from an Antarctic strain showed a typical msmA gene for the ,-hydroxylase of MSAMO, and both Antarctic and Portuguese strains contained mxaF, the methanol dehydrogenase large subunit gene. This is the first report of methanesulfonate-degrading bacteria from the Antarctic and of methylotrophy in Afipia, and the first description of any bacterium able to use both methanesulfonate and dimethylsulfone. In contrast, the type strain of A. felis DSM 7326T was not methylotrophic, but grew in defined mineral medium with a wide range of single simple organic substrates. Free-living Afipia strains occurring widely in the natural environment may be significant as methylotrophs, degrading C1 -sulfur compounds, including the recalcitrant organosulfur compound methanesulfonate. [source]

    Novel Enantioselective Synthesis of Functionalized Pyridylarsanes by a Chiral Palladium Template Promoted Asymmetric Hydroarsanation Reaction

    Fengli Liu
    Abstract The asymmetric hydroarsanation reactions between diphenylarsane and (E)-1-phenyl-3-(pyridin-2-yl)-2-propenone and (E)-1-methyl-3-(pyridin-2-yl)-2-propenoate have been achieved by use of the organopalladium complex containing ortho -metalated (R)-[1-(dimethylamino)ethyl]naphthalene as the chiral reaction template in high regio- and stereoselectivities under mild conditions. Hydroarsanation of (E)-1-phenyl-3-(pyridin-2-yl)-2-propenone with diphenylarsane generated two stereoisomeric products in the ratio of 3:1 as five-membered As,N bidentate chelates on the chiral naphthylamine palladium template. Using the same chiral metal template, the corresponding hydroarsanation reaction with (E)-1-methyl-3-(pyridin-2-yl)-2-propenoate gave only one product as a six-membered As,N bidentate chelate. The naphthylamine auxiliary could be removed chemoselectively by treatment with concentrated hydrochloric acid to form the corresponding optically pure neutral complexes. Subsequent ligands displacement from the palladium using aqueous potassium cyanide generated the optically pure keto- and ester-functionalized chiral pyridylarsane ligands. The absolute configuration and the coordination properties of the pyridylarsanes have been established by single-crystal X-ray analysis.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source]

    Synthesis and Structure of Aminopyridinato-Stabilized Yttrium and Lanthanum Amides and Their Reactivity towards Alkylaluminium Compounds

    Christian Döring
    Abstract A series of aminopyridinato-stabilized (amido)lanthanide complexes has been synthesized and characterized. The bulky aminopyridines (2,6-diisopropylphenyl)[6-(2,4,6-triisopropylphenyl)pyridin-2-yl]amine (1a) and [6-(2,4,6-triisopropylphenyl)pyridin-2-yl](2,4,6-trimethylphenyl)amine (1b) were introduced by amine elimination reaction with [Ln{N(SiHMe2)2}3(thf)2] (Ln = Y, La, thf = tetrahydrofuran, Me = methyl) to obtain the corresponding mono(aminopyridinato) complexes. Single-crystal X-ray analyses were carried out for the yttrium derivatives. The complexes are not able to undergo coordinative chain transfer polymerization with ethylene in the presence of alkylaluminium compounds as the corresponding dialkyl complexes do. Investigations of the reactions of the lanthanide aminopyridinato complexes with triethylaluminium or diisobutylaluminium hydride reveal a fast transfer of the aminopyridinato ligand to the aluminium atom. The products of this transfer reaction are aminopyridinato-stabilized dialkylaluminium compounds. One example of these aluminium complexes was characterized by X-ray crystal structure analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source]

    Unprecedented Rearrangement of Molybdenum(VI) Oxide to (,2 -Oxido)bis[dioxidomolybdenum(VI)] Hexamolybdate

    María R. Pedrosa
    Abstract MoO2(acac)2 reacts with water, amides, sulfoxides, and phosphane oxides in aqueous methanol, under mild conditions, to afford a new family of molybdates of composition [Mo2O5L6][Mo6O19] (L = H2O, dimethylformamide, dimethylacetamide, dimethyl sulfoxide, dibutyl sulfoxide, tributylphosphane oxide, triphenylphosphane oxide, hexamethylphosphoramide). The crystal and molecular structures of the two first structurally characterized (,2 -oxido)bis[dioxidomolybdenum(VI)] hexamolybdates were established by X-ray diffraction analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source]

    Reactivity of InCp* Towards Transition Metal Carbonyl Clusters: Synthesis and Structural Characterization of the Rh6(CO)16,x(InCp*)x Mixed-Metal Cluster Compounds, x = 1,2

    Elena V. Grachova
    Abstract With [Rh6(CO)15(InCp*)], the first example of a transition metal carbonyl cluster with a coordinated InCp* (Cp* = C5Me5) fragment in the ligand environment is reported. This cluster with direct Rh,In bonds forms in the reaction of the hexanuclear carbonyl rhodium cluster Rh6(CO)15(NCMe) with InCp* under mild conditions. This is characterized by means of IR and NMR spectroscopy and crystal structure analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source]

    An Unusual Reaction of (,-Dimethylaminoethoxy)triethyltin with Phenyltin Trichloride.

    Aryl; X, Symmetrical Dimers [R2SnXY], The First X-ray Structural Evidence of the Existence of Complexes R2SnXY·R2SnXY (R = Alkyl, Y = Hal, Y) Both as Unsymmetrical Adducts [R2SnX2·R2SnY2]
    Abstract The substituent exchange reaction of PhSnCl3 with [Et3Sn(OCH2CH2NMe2)] gives rise unexpectedly to the unsymmetrical adduct [Ph2SnCl2·Ph2Sn(OCH2CH2NMe2)2] (2). It has been unambiguously proved for the first time that compounds of the RSnX3 type are able to undergo the hydrocarbon substituent redistribution reaction. The analogous tin complexes [Et2SnCl2·Et2Sn(OMe)2] (5) and [Bu2Sn(OAc)2·Bu2Sn(OMe)2] (6), which have ligands other than ,-dimethylaminoethoxy and could be considered as "organotin analogs of Grignard reagents" have symmetrical dimeric structures, i.e., can be formulated as [Bu2Sn(OMe)(OAc)]2 and [Et2Sn(OMe)Cl]2, respectively. Both types of structures, viz., unsymmetrical adduct (2) and symmetrical dimer (5, 6), have been characterized by X-ray diffraction analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006) [source]

    Single-Electron-Transfer Reactions of ,-Diimine dpp-BIAN and Its Magnesium Complex (dpp-BIAN)2,Mg2+(THF)3

    Igor L. Fedushkin
    Abstract The reactions of (dpp-BIAN)Mg(THF)3 (1) {dpp-BIAN = 1,2-bis[(2,6-diisopropylphenyl)imino]acenaphthene} with ethyl halides EtX (X = Cl, Br, I) in hexane proceed by single-electron transfer (SET) from the metal complex to the organic halide. Complexes [(dpp-BIAN)(Et)]MgX(THF)n [X = Cl, n = 0 (2); X = Br, n = 2 (3); X = I, n = 1 (4)] are the products of ethyl transfer to an imine carbon atom of a coordinated diimine ligand. The compound [(dpp-BIAN)(Et)]MgBr (3a) was obtained from the reaction of free dpp-BIAN with ethylmagnesiumbromide in hexane. In this case SET from the Grignard reagent to the neutral diimine takes place. Compounds 2,4 and 3a were isolated as crystals and characterized by 1H NMR spectroscopy. The molecular structure of 3 was determined by single-crystal X-ray analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006) [source]

    The Synthesis and Characterisation of Bis(phosphane)-Linked (6 - p -Cymene)ruthenium(II),Borane Compounds

    Adrian B. Chaplin
    Abstract The reaction of [(,6 - p -cymene)RuCl2]2 with some bis(phosphane) ligands (dppm, dppe, dppv, dppa, dpp14b, dppf) has been investigated. In general mixtures of products were obtained, although the pendant phosphane complexes [(,6 - p -cymene)RuCl2(,1 -dppv)] and [(,6 - p -cymene)RuCl2(,1 -dppa)] were isolated and characterized in the solid state by X-ray diffraction. The later complex was obtained in lower yield and undergoes an equilibration reaction resulting in the formation of a dimeric species, where the dppa bridges two ruthenium centres, and uncoordinated phosphane; the bridging species was also structurally characterised in the solid state. In contrast, the reaction of [(,6 - p -cymene)RuCl2(PPh3)] with dppa in the presence of [NH4]PF6 results in the formation of [(,6 - p -cymene)RuCl(PPh3)(,1 -dppa)]PF6, which is stable in solution. A series of linked ruthenium,borane complexes, viz. [(,6 - p -cymene)RuCl2(,1 -phosphane-BH3)] (phosphane = dppm, dppe, dppv, dppa, dpp14b, dppf) and [(,6 - p -cymene)RuCl(PPh3)(,1 -dppa-BH3)]PF6 have been prepared from isolated pendant phosphane complexes, those generated in situ, or from a preformed phosphane,borane adduct. The solid-state structures of [(,6 - p -cymene)RuCl2(,1 -dppm-BH3)], [(,6 - p -cymene)RuCl2(,1 -dppe-BH3)] and [(,6 - p -cymene)RuCl2(,1 -dppv-BH3)] have been determined by X-ray diffraction analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2005) [source]

    Lithium and Potassium Amides of Sterically Demanding Aminopyridines

    Natalie M. Scott
    Abstract The reaction of Grignard compounds of 1-bromo-2,4,6-diisopropylbenzene (1) or 1-bromo-2,6-dimethylbenzene (2), formed in situ, with 2,6-dibromopyridine in the presence of a catalytic amount of [(dme)NiBr2] (dme = 1,2-dimethoxyethane) and tricyclohexylphosphane (1:2 ratio) leads to the corresponding monoarylated bromopyridines. These bromopyridines undergo Pd-catalysed aryl amination (Buchwald,Hartwig amination) with 2,6-diisopropylaniline giving rise to (2,6-diisopropylphenyl)[6-(2,4,6-triisopropylphenyl)pyridin-2-yl]amine (Ap*H) and (2,6-diisopropylphenyl)[6-(2,6-dimethylphenyl)pyridin-2-yl]amine (Ap,H) (Ap = aminopyridinate). Deprotonation of Ap*H in diethyl ether using BuLi results (after workup in hexane) in a colourless crystalline material. X-ray structural analysis reveals it to be a monomeric three-coordinate lithium aminopyridinate. In toluene solution, an equilibrium between [(Ap*Li)2] (in excess at room temperature) and [Ap*Li(OEt2)] (prominent at low temperature) is observed. Reaction of Ap,H with BuLi in diethyl ether gives rise to [Ap*LiAp*Li(OEt2)]. Deprotonation of Ap*H and Ap,H using KH leads to [Ap*K]n and [Ap,K],, respectively. [Ap,K], is a rare example of a crystalline organometallic polymer, as determined by X-ray analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004) [source]

    Novel Phosphovanadate Layered Structure Assembled from a Tetrametallic Cubane-Like VV Cluster

    Fa-Nian Shi
    Abstract A novel phosphovanadate layered structure intercalated by 4,4,-bipyridinium cations, (C10H10N2)[(VO2)4(PO4)2], was synthesised under hydrothermal conditions and its crystal structure determined using single-crystal X-ray diffraction. The anionic [(VO2)4(PO4)2]n2n, perforated layers are strongly hydrogen bonded to the interlayer 4,4,-bipyridinium cations and are assembled by an unprecedented secondary tetrametallic VV building unit constructed from a distorted cubane-like {V4O4} cluster. The compound was further characterised by IR, Raman, 1H, 1H- 13C, 31P and 51V MAS NMR spectroscopy, and by thermal and elemental analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004) [source]

    Synthesis and Monitoring of ,-Bi2Mo3O12 Catalyst Formation using Thermo-Raman Spectroscopy

    Anil Ghule
    Abstract Thermo-Raman spectroscopy was used to monitor the dehydration and phase transformations of Bi2Mo3O12·5H2O. The hydrated forms Bi2Mo3O12·5H2O, Bi2Mo3O12·4.75H2O, Bi2Mo3O12·3H2O, Bi2Mo3O12·2H2O, and anhydrous Bi2Mo3O12 were observed during dehydration in the wavelength range from 200 to 1400 cm,1. Representative Raman spectra of these compounds are reported for the first time. The thermo-Raman intensity thermogram showed a systematic dehydration in four steps, and the differential thermo-Raman intensity thermogram confirmed this. Thermogravimetry, differential thermogravimetry, and differential scanning calorimetry results were in harmony with the results of the thermo-Raman spectroscopy. Additionally, the dehydration resulting in formation of anhydrous Bi2Mo3O12 (amorphous Bi2Mo3O12 phase) and the final transformation into the ,-Bi2Mo3O12 phase was observed to be a dynamic thermal process. The slow, controlled heating rate produced ,-Bi2Mo3O12 catalyst with a particle size averaging 200 nm. The catalyst formed was further characterized by Fourier transform infrared spectroscopy, X-ray diffraction, time of flight SIMS, transmission electron microscopy, and energy-dispersive X-ray analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004) [source]

    Synthesis, Structures and Reactions of Novel 9,10-Dihydro-9,10-distannaanthracenes

    Masaichi Saito
    Abstract A method for the synthesis of 9,10-dihydro-9,10-distannaanthracenes has been improved and applied to the synthesis of novel unsymmetrical 9,10-dihydro-9,10-distannaanthracenes. The first 9,9,10,10-tetrahalo-9,10-dihydro-9,10-distannaanthracenes were successfully synthesized by halogenation of 9,9,10,10-tetrakis(p -methoxyphenyl)-9,10-dihydro-9,10-distannaanthracene. The structures of the newly obtained 9,10-dihydro-9,10-distannaanthracenes were determined by X-ray analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004) [source]

    First Examples of Ternary Lanthanide 2,2,-Diphenyldicarboxylate Complexes: Hydrothermal Syntheses and Structures of Lanthanide Coordination Polymers of 2,2,-Diphenyldicarboxylic Acid and 1,10-Phenanthroline

    Yibo Wang
    Abstract In the four new lanthanide coordination polymers {[La2(2,2,-dpdc)3(phen)(H2O)]·2H2O}n (1), [Eu2(2,2,-dpdc)3(phen)(H2O)2]n (2), {[Ln2(2,2,-dpdc)3(phen)2(H2O)2]·4H2O}n [Ln = Tb (3), Yb (4)] (2,2,-dpdc = 2,2,-diphenyldicarboxylate, phen = 1,10-phenanthroline), prepared by hydrothermal synthesis, the 2,2,-dpdc dianion affords tetradentate, pentadentate, and hexadentate coordination modes. Complex 1 is a two-dimensional network of infinite 1-D chains assembled through ,,, interactions, with nine- and ten-coordinate La3+, and arranged in wave-like layers. In 2, Eu3+ possesses nine- and ten-coordinate geometries bridged by 2,2,-dpdc ligands to give a 3-D structure. The isomorphous complexes 3 and 4, in which Tb3+ and Yb3+ ions are both nine-coordinate, have two-dimensional structures of 1-D zigzag chains stacked via hydrogen bonds and ,,, interactions of phen molecules. The high-resolution emission spectrum of 2 shows two Eu3+ ion sites, which is consistent with the results of the X-ray crystal structure analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003) [source]

    Syntheses and Coordination Chemistry of Aminomethylphosphine Derivatives of Adenine

    Qingzhi Zhang
    Abstract Two aminomethylphosphane derivatives of adenine 9-(2-{bis[(diphenylphosphanyl)methyl]amino}ethyl)adenine (La) and 9-(3-{bis[(diphenylphosphanyl)methyl]amino}propyl)adenine (Lb) were synthesised. Oxidation of La and Lb with H2O2, elemental sulfur or elemental selenium led to the corresponding oxidized products 4a/b,6a/b. Both La and Lb behave as didentate ligands towards late transition metals. Reaction of La or Lb with [MX2(cod)] (M = Pd, Pt; X = Cl, Me) gave chelate complexes 7a/b,10a/b. Reaction of La or Lb with [AuCl(tht)] or [{RuCl(,-Cl)(p -MeC6H4iPr)}2] gave the didentate bridging complexes 11a/b and 12a. All compounds have been fully characterised by microanalysis, IR, 1H and 31P{1H} NMR spectroscopy, and EI/CI/FAB mass spectrometry. 1H{31P} NMR and 1H- 13C correlation experiments were used to confirm the spectral assignments where necessary. Two compounds were structurally characterised by X-ray crystallographic analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003) [source]

    Synthesis and Structure of Two New High Nuclearity Ru/Pt Mixed-Metal Clusters

    Brian F. G. Johnson
    Abstract The reaction of the dianion [Ru5C(CO)14]2, with [PtCl2(MeCN)2] in the presence of silica yields [Ru5PtC(CO)16] (1) and the new compound [PPN]2[Ru10Pt2C2(CO)28] (2), while, in a related reaction, [Ru6C(CO)16]2, undergoes addition of [PtCl2(MeCN)2] to yield the cluster [Ru12PtC2(CO)32(MeCN)2] (3). The high nuclearity compounds 2 and 3 have been fully characterized and their structures determined by single crystal X-ray analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003) [source]

    Direct Synthesis of (PhSe)4Ge and (PhTe)4Ge from Activated Hydrogenated Germanium , Crystal Structure and Twinning of (PhTe)4Ge

    Sabine Schlecht
    Abstract The germanium chalcogenolates (PhSe)4Ge and (PhTe)4Ge were synthesized from activated hydrogenated germanium (Ge*) and diphenyldiselenide or diphenylditelluride, respectively. (PhTe)4Ge is the first homoleptic organotellurolate of germanium. It was characterized spectroscopically and by X-ray crystal structure analysis. (PhTe)4Ge crystallizes in the monoclinic space group P21/c with a = 12.8018(14), b = 9.1842(9), c = 23.690(3) Å and , = 105.458(8)°. The molecules show a tetrahedral GeTe4 core. Weak Te-Te interactions connect neighbouring tetrahedra to infinite helices along [010]. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003) [source]

    Synthesis of a Hexadentate Hexameric Aluminum Imide and Its Metathesis Reactions

    N. Dastagiri Reddy
    Abstract The reaction of AlH3·NMe3 with one equivalent of 2-cyanothiophene in toluene afforded [HAlNCH2(C4H3S)]6 (2) in good yield. Treatment of 2 with SiMe3Br and SiMe3Cl in toluene under refluxing conditions resulted in the formation of compounds [BrAlNCH2(C4H3S)]6 (3) and [ClAlNCH2(C4H3S)]6 (4), respectively. In a similar way [PhC,CAlNCH2(C4H3S)]6 (5) was readily obtained from the reaction between 2 and PhC,CH. When 2 was treated with PhSH the Al-N cluster core dissociated and a four-membered ring compound [(PhS)2AlNHCH2(C4H3S)]2 (6) was formed. In contrast, a similar hexameric aluminum imide (HAlNCH2Ph)6 (1) retains its Al-N network when treated with PhSH to yield (PhSAlNCH2Ph)6 (7). An exchange of ethyl groups and hydrides occurred when 2 was treated with excess of ZnEt2, forming [EtAlNCH2(C4H3S)]68. Compounds 2,4 and 6,8 were characterized by X-ray single-crystal analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003) [source]

    Diastereoselective Synthesis of Heteroaromatic Glycine Derivatives

    Trygve Andreassen
    Abstract A TMSOTf promoted addition of an N - tert -butanesulfinyl ,-imino ester to five-membered aromatic heterocycles furnishes optically active heteroaromatic glycine derivatives with moderate-to-good yield in diastereomeric ratios up to 99,%. The absolute configuration of two of the addition products were solved by X-ray analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008) [source]

    Asymmetric Homoaldol Reactions with Cyclohex-2-enyl N,N -Diisopropylcarbamate: Kinetic Resolution, Elucidation of the Stereochemical Course and Applications in the Synthesis of Hexahydroisobenzofuran-4-(1H)-ones

    Jochen Becker
    Abstract Enantio-enriched cyclohex-2-enyl N,N -diisopropylcarbamate (5) is stereospecifically deprotonated by sec -butyllithium/(,)-sparteine (9) to form the configurationally stable lithium complex 7·9. A kinetic resolution of rac - 5 by n -butyllithium/(,)-sparteine (9) yielded (R)- 5 with up to 99,% ee. Electrophilic substitution with tin electrophiles proceeds in a anti -SE, fashion as shown by chemical correlations. The synthesized allylstannanes 10 undergo a highly stereospecific TiCl4 -mediated homoaldol reaction with various aldehydes, yielding syn -configured homoaldol products 12. These were transferred into all - cis -configured hexahydroisobenzofuran-4(1H)-ones 22 by BF3·OEt2 -mediated reactions with aldehydes. The configurations of several products were determined by X-ray structure analysis. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source]