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1.
Wang Q Barclay JE Blake AJ Davies ES Evans DJ Marr AC McInnes EJ McMaster J Wilson C Schröder M 《Chemistry (Weinheim an der Bergstrasse, Germany)》2004,10(14):3384-3396
A novel [NiS4Fe2(CO)6]cluster (1: 'S(4)'=(CH(3)C(6)H(3)S(2))(2)(CH(2))(3)) has been synthesised, structurally characterised and has been shown to undergo a chemically reversible reduction process at -1.31 V versus Fc(+)/Fc to generate the EPR-active monoanion 1(-). Multifrequency Q-, X- and S-band EPR spectra of (61)Ni-enriched 1(-) show a well-resolved quartet hyperfine splitting in the low-field region due to the interaction with a single (61)Ni (I=3/2) nucleus. Simulations of the EPR spectra require the introduction of a single angle of non-coincidence between g(1) and A(1), and g(3) and A(3) to reproduce all of the features in the S- and X-band spectra. This behaviour provides a rare example of the detection and measurement of non-coincidence effects from frozen-solution EPR spectra without the need for single-crystal measurements, and in which the S-band experiment is sensitive to the non-coincidence. An analysis of the EPR spectra of 1(-) reveals a 24 % Ni contribution to the SOMO in 1(-), supporting a delocalisation of the spin-density across the NiFe(2) cluster. This observation is supported by IR spectroscopic results which show that the CO stretching frequencies, nu(CO), shift to lower frequency by about 70 cm(-1) when 1 is reduced to 1(-). Density functional calculations provide a framework for the interpretation of the spectroscopic properties of 1(-) and suggest that the SOMO is delocalised over the whole cluster, but with little S-centre participation. This electronic structure contrasts with that of the Ni-A, -B, -C and -L forms of [NiFe] hydrogenase in which there is considerable S participation in the SOMO. 相似文献
2.
Jaime Pacheco-Arjona Pablo Rodriguez-Gonzalez Manuel Valiente David Barclay 《International journal of environmental analytical chemistry》2013,93(13):923-932
A new self-tuning single-mode-focused microwave technology has been evaluated in this work to perform the quantitative routine extraction of organometallic species from solid matrices of environmental interest. Species-specific isotope dilution analysis has been employed to better investigate the real influence of the microwave-assisted extractions on the final results. The advantages of such methodology in comparison with other established microwave units for the routine speciation analysis of organomercury and organotin compounds are discussed (such as the capability of using disposable glass vials, a self-tuning mode to provide an accurate control of the temperature and pressure inside of the vials, and the possibility of performing automated sequence of extractions with low sample size). The results obtained in this work demonstrated that such technology provides a fast and reliable quantitative extraction of the organometallic species in a wide range of extraction conditions even when the multi-elemental (Sn and Hg) species-specific determination is carried out. 相似文献
3.
4.
Barclay TM Hicks RG Lemaire MT Thompson LK Xu Z 《Chemical communications (Cambridge, England)》2002,(16):1688-1689
The synthesis of a verdazyl radical with a carboxylate substituent renders the radical highly soluble in water, thereby permitting the aqueous synthesis of Ni(II) and Co(II) verdazyl complexes which have been structurally and magnetically characterized. 相似文献
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6.
W.C. Ma A.V. Ramayya J.H. Hamilton S.J. Robinson M.E. Barclay K. Zhao J.D. Cole E.F. Zganjar E.H. Spejewski 《Physics letters. [Part B]》1984,139(4):276-278
The energy levels of 182Hg have been identified for the first time through comparison of in-beam studies of the reactions 156,154Gd(32S, 4n)184,182Hg and γ-X-ray coincidences. Levels up to 12+ in 182Hg were established from γ-γ coincidences and singles measurements. The data establish that the ground state shape is near spherical, and that the ground band is crossed by a well-deformed band at 4+. In contrast to IBA model predictions that the deformed band will rise in energy in 182Hg compared to 184Hg, the energies of the deformed levels in 182Hg continue to drop. 相似文献
7.
Barclay GL Quiclet-Sire B Sanchez-Jimenez G Zard SZ 《Organic & biomolecular chemistry》2005,3(5):823-835
In model studies towards the synthesis of kirkine, the carbon skeleton was constructed using a radical cascade reaction. Two different approaches towards the synthesis have been examined as well as the regioselectivity of the radical cyclisation. 相似文献
8.
Mojumdar SC Becker DA DiLabio GA Ley JJ Barclay LR Ingold KU 《The Journal of organic chemistry》2004,69(9):2929-2936
The rate constants, k(inh), for reaction of stilbazulenyl-bis-nitrone (STAZN, 1) with peroxyl radicals and the number of radicals trapped, n, are compared with those of phenolic antioxidants 2,2,5,7,8-pentamethyl-6-hydroxychroman (PMHC, 4a), 2,5,7,8-tetramethyl-6-hydroxychroman-2-carboxylic acid (Trolox, 4b), and 2,6-di-tert-butyl-4-methoxyphenol (DBHA, 5). The behavior of STAZN depended markedly on the media and type of initiator used, water-soluble or lipid-soluble. In styrene/chlorobenzene and initiation by azo-bis(isobutyronitrile) (AIBN), k(inh) (STAZN) = 0.64 k(inh) (5) = 0.02k(inh) (4a). On addition of methanol, the k(inh) of STAZN increased 6-fold to be four times that of 5 while that of 4a decreased 6-fold. In aqueous SDS-micelles containing methyl linoleate and initiation with water-soluble azo-bis(amidinopropane)2HCl, ABAP, the relative k(inh) values were 1 >or= 4b > 5. In dilinoleoylphosphatidyl choline (DLPC) bilayers and initiation with lipid-soluble azo-bis-2,4(dimethylvaleronitrile) (DMVN), the k(inh) order was 5 > 4b > 1. During initiation with ABAP in micelles and bilayers, the calculated values of k(inh) for STAZN changed during the induction period. The experimental results are interpreted in terms of the conformation of STAZN, which is transoid in homogeneous solution but cisoid in aqueous dispersions of lipids. In such dispersions, the STAZN lies at the lipid-water interface where it traps water-soluble peroxyl radicals by a single electron-transfer mechanism. The cisoid conformation at lipid-water interfaces is supported by theoretical calculations. 相似文献
9.
Oganesyan VS Barclay JE Hardy SM Evans DJ Pickett CJ Jayasooriya UA 《Chemical communications (Cambridge, England)》2004,(2):214-215
The potential of NIS spectroscopy to study the iron-sulfur clusters in metalloproteins is illustrated using model compounds. The origin of the intense low energy transfer bands is discussed. 相似文献
10.
Continuity of the Spectral Factorization Mapping 总被引:2,自引:0,他引:2
It is shown that the matrix spectral factorization mapping issequentially continuous from Lp to H2p (where 1 p<), underthe additional assumption of uniform integrability of the logarithmsof the spectral densities to be factorized. It is shown, moreover,that this condition is necessary for continuity, as well assufficient. 相似文献